5761 5765.output

* GB786169 (A)

Description: GB786169 (A) ? 1957-11-13

New photographic sensitisers

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The EPO does not accept any responsibility for the accuracy of data and information originating from other authorities than the EPO; in particular, the EPO does not guarantee that they are complete, up-to-date or fit for specific purposes.

7 r v, PATENT SPECIFICATION Inventor: GEORGE DE WINTER ANDERSON 786,1 69 Date of filing Complete Specification: Oct 28, 1955. Application Date: Nov 4, 1954. No 31910/54. Complete Specification Published: Nov 13, 1957. Index at acceptance: -Classes 2 ( 4), D 1 Q; and 98 ( 2), C 3. International Classification:-C O 9 b G 03 c. COMPLETE SPECIFTC ATTO Nx PATENTS ACT, 1949 SPECIF'ICATICN NO, 1786,169 In accordance with the Decision of the Superintending Examiner, acting for the Comptroller-General, dated the twentysecond day of October, 1958, this Specification has been amended under Section 14 In the following manner:, line se, delete "hlydrogen atoms or fore. Page 2, line es, delete Ohydrogen atoms or for". TSE PATENT OFFICE, othll November, 1 g 58 t 41;:;)n = Cc c -= Cow -SR where D 1 is the residue of a five-membered or six-membered heterocyclic nitrogen ring, R is a hydrogen atom or an alkyl, aryl, or aralkyl group, R, is an alkyl or aralkyl group, Rk is an alkyl, aryl or aralkyl group, X is an acid radicle and N is nought or one with (as second reactant) a compound containing a reactive CH group or a

reactive NH group, in the presence of a base and a solvent for the reactants It is stated in the Specification that the second reactant may be malonic dinitrile and that D 1 in the above formula may be a residue of inter alia a diazole (for example thio-Af 3-diazole) but there is no specific disclosure that D, can be an iminazole or benziminazole residue. According to our invention we provide new photographic sensitisers of the formula:l || o C CH CH C-CN 5-C-N lPnrice Ci 6 l 14 S 6 d DB 08539/1 ( 3)/3699 150 11/58 R U 1 ULL LN-a Zyi aenvatve tflereot, wherein R, A and B have the significance given above and X stands for halogen, sulphonic acid or sulphuric ester, in the presence of an organic amine. As suitable quaternary salts of the stated formula and their acyl derivatives there may be mentioned for example 2-/8-acetanilidovinyl-l: 3-dimethylbenzimidazolium iodide. The reaction is preferably carried out in a solvent for example ethanol (when triethylamine is conveniently used as the organic amine) or pyridine (when piperidine is conveniently used as the organic amine) The product may be isolated by cooling the reaction mixture and filtering, and it may be purified by crystallisation from a suitable solvent for example glacial acetic acid. When the new sensitisers of our invention are added to gelatino-silver halide emulsions they produce very powerful second order " sensitisation of the emulsions This "second order " sensitisation obtained with the sensitisers of our invention is much more powerful than that obtained with analogous sensitisers in which the atoms of the terminal nitrogencontaining radical are not symmetrically arranged about the plane of the double bond joining this radical to the polymethine chain. According to a further feature of our invenPATENT SPECIFICATION Inventor: GEORGE DE WINTER ANDERSON 7863169 Date of filing Complete Specification: Oct 28, l' l a i r 20 Application Date: Nov4, 1954 1 ______ Complete Specification Published: Nov13, 1957 Index at acceptance:-Classes 2 ( 4), D 1 Q; and 98 ( 2), C 3. International Classification:-CO 9 b G 03 c. COMPLETE SPECIFICATION New Photographic Sensitisers 955. No: 31910/54. We, IMPERIAL CHEMICAL INDUSTRIES LIMITED, of Imperial Chemical House, Millbank, London, S W 1, a British Company, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement -

This invention relates to new photographic sensitisers and more particularly to new photographic sensitisers of the merocyanine series. In British Specification No 555,936 there is described and claimed a process for the production of dyestuffs which comprises condensing (as first reactant) a compound of the general formula: /N = CW)-= C C = CW5 R 2 R 9 X where D, is the residue of a five-membered or six-membered heterocyclic nitrogen ring, R is a hydrogen atom or an alkyl, aryl, or aralkyl group, R, is an alkyl or aralkyl group, R, is an alllyl, aryl or aralkyl group, X is an acid radicle and N is nought or one with (as second reactant) a compound containing a reactive C 112 group or a reactive NH group, in the presence of a base and a solvent for the reactants It is stated in the Specification that the second reactant may be malonic dinitrile and that D, in the above formula may be a residue of inter alia a diazole (for example thio-,/,61-diazole) but there is no specific disclosure that D, can be an iminazole or benziminazole residue. According to our invention we provide new photographic sensitisers of the formula: R A-C-No \ 1 11 C g CH -CHC -CN P-C-r Ni lPrice Byio W 14 6 < 1 wherein R stands for an alkyl radical, and A and B stand for hydrogen atoms or for the atoms necessary to complete a benzene ring which is fused to the heterocyclic ring. According to a further feature of the invention we provide a process for the manufacture of new photographic sensitisers which comprises heating malonic dinitrile with a quaternary salt of the formula:R A-C C-CR CH-NH C 6 H 5 R or an N-acyl derivative thereof, wherein R, A and B have the significance given above and X stands for halogen, sulphonic acid or sulphuric ester, in the presence of an organic amine. As suitable quaternary salts of the stated formula and their acyl derivatives there may be mentioned for example 2-ft-acetanilidovinyl-i: 3-dimethylbenzimidazolium iodide. The reaction is preferably carried out in a solvent for example ethanol (when triethylamine is conveniently used as the organic amine) or pyridine (when piperidine is conveniently used as the organic amine) The product may be isolated by cooling the reaction mixture and filtering, and it may be purified by crystallisation from a suitable solvent for example glacial acetic acid. When the new sensitisers of our invention are added to gelatino-silver halide emulsions they produce very powerful " second order " sensitisation of the emulsions This "second order " sensitisation obtained with the sensirisers of our invention is much more powerful than that obtained with analogous sensitisers in which the atoms of the terminal nitrogencontaining radical are not symmetrically arranged

about the plane of the double bond joining this radical to the polymethine chain. According to a further feature of our invention therefore we provide a gelatino-silver halide emulsion sensitised with a photographic sensitiser as hereinbefore defined. The invention is illustrated but not limited by the following Examples in which the parts are by weight: EXAMPLE 1. 14.5 parts of 2-,J-acetanilidovinyl-1: 3-dimethylbenzimidazolium iodide, 2 8 parts of malonic dinitrile and 80 parts of ethanol are heated together under a reflux condenser and 3.8 parts of triethylamine are added The mixture is boiled under a reflux condenser for minutes The reaction mixture is then cooled and filtered, and the residue on the filter is washed thoroughly with hot water and dried at 1100 C The yellow crystalline solid so obtained is recrystallised from 780 parts of glacial acetic acid and the product obtained in the form of fine yellow needle-shaped crystals of melting point 324-325 C The absorption maximum of the product in methanol is at a wavelength of 413 millimicrons. EXAMPLE 2. 1 part of a 0 05 % solution of the sensitiser of Example 1 in 2-ethoxyethanol is added to parts of a gelatino-silver halide emulsion containing 8 8 % of gelatine, 1 7 % of silver chloride and 0 55 % of silver bromide The mixture is stirred for 30 minutes at 40 C and then coated onto a glass plate (A) A second plate (B) is coated with the same gelatinosilver halide emulsion sensitised with 10 parts of the above sensitiser solution The two plates are then exposed in a wedge spectrograph, developed and fixed, alongside a plate coated with the same gelatino-silver halide emulsion which had not been optically sensitised and a plate (C) coated with the same gelatino-silver halide emulsion sensitised with 10 parts of a 0.05 % solution of 4-( 3-ethyl-5-phenyl-benzoxazolylidene-2)-2-cyano-2-butenonitrile in 2ethoxyethanol. The optically-unsensitised plate showed a maximum inherent sensitivity at a wavelength of 405 millimicrons and a range of sensitisation up to 450 millimicrons. The sensitivity maximum, range of sensitivity and relative sensitivity at the maximum conferred sensitisation, as compared with the maximum inherent sensitivity, are shown in Table 1, where it is seen that the second order sensitisation with the dyestuff of Example 1 is in the blue region of the spectrum and is much more powerful than the sensitisation with the unsymmetrical dyestuff used in plate C. TABLE 1 Sensitivity Range of Relative Sensitivity Plate maximum sensitisation at maximum conferred (millimicrons) (millimicrons) sensitisation A

405,435 up to 470 1 B 460 up to 490 4 C 405,455 up to 495 1 5

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* GB786170 (A)

Description: GB786170 (A) ? 1957-11-13

Processes for treating fusible material

Description of GB786170 (A)

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BE533921 (A) CH333698 (A) DE1053194 (B) FR1112171 (A) NL97193 (C) US2739045 (A) BE533921 (A) CH333698 (A) DE1053194 (B) FR1112171 (A) NL97193 (C) US2739045 (A) less Translate this text into Tooltip



PATENT SPECIFICATION 7869170 Date of Application and filing Complete Specification Dec 7, 1954. No 35413 54. Application mode in United States of America on Dec 8, 1953.

Complete Specification Published Nov 13, 1957. Index at Acceptance: -Classes 82 ( 1), I 3 B; and 90, K 10. International Classification: -CO 1 b C 22 b. CO.Ml PLETE SPECIFICATION SPECIFICATION iw O 73 e,170 In pursuance of Section 9 of the Patents Act, 1949, the Specificatlon hrs teen amended in the following manner:Page 1, line e 2, after "o 1953 " 1, insert "i Zore-refining processes in which at least one:nolten zone is caused to traverse a body or material in order to produce a redlstribution of ingredients therein, forms the subject of our Patent No 71 g 9,673 and, hawring regard to the provisions of Section 9 of the Patents Act, 149, attention is directed to the claims of this patent 1 THE PATENT OFFICE, 29th Yay, l gav DB 05139/l( 8)/362 i i SO 5/53 R i,,> J LUA UC u CZI Dea In terms of a blaary solvent-solute system in which it will be assumed that the solute is the impurity to be removed and that k, the distribution coefficient, defined as the ratio of the solute concentration in the solid freezing out of a molten zone to that in the liquid in the zone is constant and less than 1 It is to be understood that the solute could just as well be considered to be the product which it is desired to recover, that the processes work equally well for systems having a k value greater than 1 and further that the invention is not to be limited to its application to binary systems It should be noted that the constant k is identical to and is here used in place of the lower case Greek letter gamma (y) which latter symbol has been heretofore used. Where the system undergoing treatment is a semi-conductive material such as, for example, silicon or germanium alloyed with small portions of solute or solutes to which lPrice 3 s 6 d l impurity toward the end of the charge in the direction of travel of the zone It has been shown that extremly high purity can be attained by this process For example, by batch zone-refining, a concentration of significant donor impurities in germanium has been reduced to less than 2 x 1012 atoms per cubic centimetre of germanium which, in this example, was less than one donor atom per atoms of germanium (W G Pfann and K M Olsen, Physical Review, Volume 89, page 322, 1953). According to the invention a process of treating fusible material comprising at least two ingredients, the material being enclosed in a column includes the steps of causing alternately spaced relatively hot and cold regions to progress in one direction from one end of the column to the other, the material being molten within the hot regions and solid within the cold regions, removing from at least one end of the column an arrount of material less Mu 8 u 1 IPATENT SPECIFICATION 786,170 Date of Application and filing Complete Specification Dec 7, 1954.

No 35413 '54. Application made in United States of America on Dec 8, I 523; Complete Specification Published Nov 13, 1957. Index at Acceptance:-Classes 82 ( 1), B 3 B; and 90, K 10. International Classification: -C Obb C 22 b. COMPLETE SPECIFICATION Processes for Treating Fusible Material We, WESTERN ELECTRIC COMPANY, INCORPORATED, of 195, Broadway, New York City, New York State, United States of America, a corporation of the State of New York, United States of America, do hereby declare the invention for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement: - This invention relates to processes for treating fusible material, and is particularly concerned with redistributing ingredients of fusible solvent-solute systems for the purpose of producing material of desired cornposition In their more usual applications the processes of this invention utilize variations in solute solubility in adjacent solid and liquid phases in the material being treated to segregate solutes and may be applied to systems of 2 ( metals and their alloys, to salts and salt solutions, both organic and inorganic, and to other solvent-solute systems which can be caused to undergo a liquid-solid transformation. For convenience the processes of this invention will be described in terms of a b nary solvent-solute system in which it will be assumed that the solute is the impurity to be removed and that k, the distribution coefficient, defined as the ratio of the solute concentration in the solid freezing out of a molten zone to that in the liquid in the zone, is constant and less than 1 It is to be understood that the solute could just as well be considered to be the product which it is desired to recover, that the processes work equally well for systems having a k value greater than 1 and further that the invention is not to be limited to its application to binary systems It should be noted that the constant k is identical to and is here used in place of the lower case Greek letter gamma (y) which latter symbol has been heretofore used. Where the system undergoing treatment is a semi-conductive material such as, for example, silicon or germanium alloyed with small portions of solute or solutes to which lPrice 3 s 6 d 1 present theory ascribes the extrinsic semiconductive properties of the aforesaid materials, these solutes are known as " significant impurities " or " significant solutes " Due to 50 the high order of purity required in the production of semiconductive materials such as those above set forth, and due to the favourable separation constants which characterize such

systems, the processes of this invention 55 are particularly well adapted to the purification of these materials for use in rectifiers, transistors and other semiconductive transducers. The processes of this invention utilize the 60 principles of what will be herein referred to as " batch zone-refining " which principles are amply set forth in the article " Principles of Zone-Refining " by W G Pfann in Journal of Metals, Volume 4, page 747, 1952 In one 65 form, batch zone-refining consists of slowly passing a series of molten zones through a long solid ingot or charge of impure substance, each molten zone, for a system having a k value less than 1, causing a net transfer of 70 impurity toward the end of the charge in the direction of travel of the zone It has been shown that extremly high purity can be attained by this process For example, by batch zone-refining, a concentration of signi 75 ficant donor impurities in germanium has been reduced to less than 2 X 102 atoms per cubic centimetre of germanium which, in this example, was less than one donor atom per 1010 atoms of germanium (W G Pfann and 80 K M Olsen, Physical Review, Volume 89, page 322, 1953). According to the invention a process of treating fusible material comprising at least two ingredients, the material being enclosed in 85 a column includes the steps of causing alternately spaced relatively hot and cold regions to progress in one direction from one end of the column to the other, the material being molten within the hot regions and solid within 90 the cold regions, removing from at least one end of the column an amount of material less HAS 786,170 than that which is contained in a hot region each time the material at that end of the column is molten, and adding at a point in the column an amount of feed material equal to the amount of treated material removed It will be appreciated that this process is capable of continuous operation, and in general a continuous process is more advantageous than a batch refining process from a manufacturing point of view. A particular aspect of zone separation with respect to which the use of a continuous method increases the scope or field of the application of zone processes, is as follows: In crystallization work, it is common practice to remove an impurity B from a crystalline substance A, by dissolving both A and B in solvent C Upon crystallizing solid from the solution of A and B in C a separation between A and B greater than that which would be obtained by crystallization in a binary system AB frequently results If one were desirous of using a common solvent C in order to improve the separation generally obtainable in batch zone-refining the binary system AB, it would generally be necessary to introduce a fresh supply of solvent C each time a heated region entered the beginning of a charge and as a result the operation of the process would become more complicated In a continuous process,

however, such as for example, any one of those of the present invention, the solvent may be continuously introduced as part of the feed and may be continuously withdrawn with the top and bottom products. Thus, insofar as operation of the refiner is concerned, handling such a ternary or higher order system is just as simple as handling a binary system. Since the processes of the present invention are considered to be the counterpart in the field of crystallization of the continuous fractionation column in the field of distillation, it is convenient to make reference to terminology and methods used in continuous fractional distillation processes It should be noted, however, that although a similarity exists between distillation methods and zone-refining methods, there are basic differences between the two processes These differences will become evident as the description proceeds. In batch zone-refining, molten zones slowly travel through a solid charge or ingot carrying imprities with them (for a system having a k value less than 1) and thereby effecting a separation of solutes and solvent In general, no material flows into or out of the apparatus in which the charge is contained during the separation process. The present process accomplishes the result of separating solute and solvent just as in batch zone-refining, but in addition superimposes, on the motion of the zones, the flows of feed, waste and product The container for the material undergoing treatment may now be considered to be a practical distillation column having an enriching section and a stripping section, feed being introduced intermediate the two sections, and product and waste, or first and second product, being 70 drawn out at either end In such a process net material flow is away from the feed inlet in both sections It will be shown below that the motion of the molten zolits constitutes reflux and that reflux ratios can be defined 75 and controlled during the operation of the process. The processes of the present invention accomplish both forward and counter current flow without the use of any mechanical means 80 except for the moving of heating sources in a simple one-channel column. Although the continuous fractionation column contains a rectification section, a stripping section and a provision for feed 85 introduction intermediate the two, and although product and waste are continuously withdrawn from either end of the column, it is apparent that the principles of continuous fractionation may not be directly applied to 90 the process of zone melting In liquid-vapour transfer processes, such as fractional distillation, feed may be readily introduced at any desired plate or position in the column due to the compressibility Or the vapour phase of the 95 system and the non-adherence ot the liquid

phase to the walls of the column This is not, however, so easily achieved in some liquidsolid transfer processes in which the liquid phase is not compressible to any appreciable 10 t extent and in which the solid phase, due to adhesion to the walls of the column, may not be caused, with facility, to slide away from the feed inlet and so make room for the addition of the new material Methods of accommodat 10 ' ing introduction of feed material include the process by which the solid material is caused to adhere, not to a fixed portion of the apparatus, but to a moving track and in which a separate counter flow of molten material is 11 ( maintained Another means of accomplishing such a result is by causing the processing to take place in separate stages with each stage in a separate enclosure. According to a further aspect of this inven Ii' tion, material to be treated is enclosed in a receptacle having openings at either end and means for inserting feed material, the treatment including the steps of causing alternately spaced relatively hot and cold regions to tra 12 ( verse the receptacle from one end to the other, the material being molten within the hot regions and solid within the cold regions, removing from an end of the receptacle an amount of material less than that contained in 12 ' a hot region each time the material at that end of the column is molten, thereby causing a void, causing this void to traverse the receptacle in the same direction and at the same rate as the hot regions, and filling the void with 13 ( 7 g 6,170 3 fresh feed material each time it reaches the feed inlet. These voids may be gaseous or substantially evacuated regions or may be filled with displaceable and substantially immiscible fluids The voids, which are generally associated with molten zones so that there is one void for each molten zone generated, will then accommodate a predetermined amount of feed which may be allowed to flow in as the void passes the feed inlet If the void has been substantially evacuated, feed simply flows in and fills up the entire space If, on the other hand, the void is actually a fluid region, this fluid is displaced by feed In the processes of the present invention this displacement is accomplished by virtue of a difference in density between the molten material of the feed and the fluid in the void. For convenience, the following description is in terms of processes in which the molten material introduced at the feed is of greater density than that contained in the void so that in the general case the fluid in the void will bubble through and will, therefore, be displaced by the molten feed material The process in which feed material is caused to rise through and thereby displace a heavier immiscible void fluid, however, also operates according to principles of this invention and is considered to be part of it. In the description of this invention, the term "void" is used to

connote a substantial absence of material undergoing treatment Voids may, therefore, be evacuated regions or may contain material which is liquid or gaseous at the operating temperatures It is a general requirement of the material in the void that it be substantially immiscible, if a liquid, with the molten phase of the system undergoing treatment However, where it is desired that the void fluid have some effect on the composition of the system, for example, as a doping medium, it may be partially miscible or soluble in the molten material undergoing treatment. These and other features of the invention will be more readily understood from the following detailed description when read with reference to the accompanying drawings, in which:Figs 1 A, 1 B, 1 C, ID, l E and IF are front elevations of the bottom section of a rectification or enriching section, of one type of apparatus in which the processes of this invention may be carried out depicting void generation and travel. Figs 2 A, 2 B, 2 C, 2 D, 2 E and 2 F are similar front elevations of a bottom section of a stripping section of an apparatus in which material is undergoing treatment according to the teaching of this invention and showing the manner in which a void is generated and caused to travel. Fig 3 is a front elevation of the enriching section of a similar piece of apparatus. Figs 4 A and 4:1 are front and side elevations of a column apparatus containing an enriching and a stripping section together with a suitable mechanical arrangement for con 70 trolling the motion of the heaters which are responsible for the molten regions. Fig 5 is a front elevation of a modified column-type continuous refiner in which the motion of the heaters is rotary 75 Figs 6 A, 6 B, 6 C and 6 D are cross-sectional views of various column and heater configurations. Fig 7 is a perspective view of a column zone refiner using strip heaters 80 Figs 8 A, SB, 8 C, 8 D, 8 E, 8 F, 8 G and 8 H are diagrammatic views of various types of void generators. Fig 9 A is a diagrammatic front view of a spiral type zone void refiner containing both 85 enriching and stripping sections Fig 9 B is a diagrammatic end view of the apparatus of Fig 9 A. Fig 10 is an end view of a spiral drum void refiner showing one type of void gener 90 ator. Figs 11 A, 11 B and 11 C, showing an end view of the stripping section of a spiral drum void refiner, depict the motion of a void during one complete revolution of the 95 refiner. Fig 12 is a diagrammatic front elevation of a column process in which the apparatus designed is such as to permit varying reflux ratios as

the material progresses through the 100 column; and Fig 13 is a diagrammatic front elevation of a section of an enriching or stripping column process which like that of Fig 12 has provision for varying the rate of reflux as the 105 feed inlet is approached. Referring again to Figs 1 A to i F, the equipment depicted is a front elevation of a portion of the enriching section of a column apparatus 110 In the enriching section depicted, heaters 1 continually move, in effect, in an upward dire-tion along column 2 so as to create molten zones 3 within the apparatus The material of regions 4 within column 2 and not within 115 heaters 1 is solid. In these figures and also in Figs 2 A to 2 F, Fig 3 and Fig 13, heating elements have been depicted schematically as bars corresponding with non-solid regions within the columns 120 Physically the heaters generally encompass the column and for a column having a circular cross-section are annular in cross-section. Further, the correspondence of non-solid regions within the column to heaters without 125 is not generally as exact as shown, the former usually lagging behind the latter The heaters depicted may, therefore, be considered to be the effective heating elements as seen from within the column The regular flat 130 7 06,170 786,170 interfaces shown are not to be expected in operation and are not essential, the idealized schematics being intended merely for ease of description. The heating elements themselves may consist of any conventional heating means such as resistance or high frequency windings, or burners, or for a normally liquid material may represent positions not occupied by cooling elements. By means of the re-entrant outlet tube 5, liquid is restrained from running out until the top of the lowest heater 1 is above the top of the re-entrant tube 5 Thereafter, since heaters 1 are longer than re-entrant tube 5, liquid flows out as lowest heater 1 advances until the lower extremity of heater 1 coincides with the lower extremity of column 2. Further travel causes the lower end of outlet tube 5 to freeze over and to prevent further flow until the next cycle Were it not for re-entrant tube 5, all of the molten material within a heater would ran out of column 2 at the bottom of the column until the lower extremity of each heater 1 coincided with the lower extremity of coiumn 2 or until the lower opening of the column was otherwise blocked by solid material This would result in a series of voids travelling through the rectification section, but since no molten material would be present in the column there would be no interphase segregation of solute The result would be a flow of matter from the feed inlet, caused by the displacement of the material inside of each void by material undergoing treatment, to the outlet with no

segregation of ingredients. In Fig 1 A the apparatus is just being started and the lowest heater 1 has advanced sufficiently to produce some liquid in the annular section about re-entrant tube 5, but has not advanced far enough to permit any of the molten material in the lowest molten zone 3 to flow out through the outlet tube. In Fig 1 B, first heater 1 has advanced sufficiently so that its lower extremity coincides with the lower extremity of column 2. It is seen that a portion of the molten material within this heater is allowed to flow out through tube 5 so as to create void 6, having a height equal to that of heater 1 minus that of re-entrant tube 5 As has been discussed, for the purpose of this description, this void represents either an evacuated region or one containing material which is fluid at the operating temperature of the apparatus and which has a lower specific gravity than that of the molten material contained in molten zones 3. In Fig 1 C, heaters 1 have advanced still further up the column so that a portion of the material within re-entrant tube 5 has frozen over, thereby preventing the escape of any more of the molten material within lower molten zone 3. In Fig ID, travel of heaters 1 up column 2 has progressed so that an additional heater is about to encompass tube 2 It is seen that passage of molten region 3 and void 6 is coincidental with travel of heaters 1 so that 70 both regions are within the heater and so that there are at all times interfaces 7 between the trailing edges of molten zones 3 and leading edges of solid regions 4 which are the interfaces at which liquid-solid transfer takes 75 place As the heaters 1 advance, melting material from solid regions 4 drops through voids 6 and into molten zones 3 This material then mixes with the material already present in molten zones 3 which material is frozen 80 out at interface 7, thereby meeting the requirements for zone-refiung. In Fig 1 E another heater 1 is now in a position corresponding with that of the lower heater shown in Fig 1 A 85 In Fig IF this heater has advanced so that its lower extremity is coincident with the lower extremity of tube 2 and so that a second void 6 has been produced The liquid flowing out of re-entrant tube 5 in Figs IB and 90 IF and for the system having a k value less than 1, represents material which is richer in solvent than that material at the upper portion of the column. Whereas, in the enriching section molten 95 zones travel toward and net flow of matter is away from the feed inlet, as shown in Figs. 1 A to IF, in the stripping section both the motion of the molten zones and the net flow of matter are in the direction of the outlet 101 Voids in the stripping section may be created by a void generator

similar to the re-entrant tube 5 shown in Figs 1 A to IF Here the relative motions of voids and molten regions are different, the molten regions being caused 105 to travel in a downward direction and voids bubbling up through them as they come into contact with each other Again the volume of the voids is determined by the relative lengths of the heater and re-entrant tube or 110 other type of void generator Void volume in the stripping and rectification sections may be controlled independently. The creation and travel of voids in the stripping section may be seen more clearly by 115 reference to Figs 2 A to 2 F These views all depict the lower portion of a stripping column with succeeding views showing the manner in which the first and second voids are produced within the equipment as it is first 120 put into operation In all of these views the motion of the heaters 8 is downward The voids are produced by an external outlet tube type of void generator 9 which will be discussed in detail in connection with Figs 8 A 125 to 8 H. In Fig 2 A, as the equipment is started up, there are present only solid regions 10 and molten regions 11, the latter coinciding with heaters 8 No voids are present, the molten 130 with feed liquid constitutes a net flow of matter through the column in the direction of the void generators The rate of flow is controlled by the size, number and rate of travel of the voids; 70 The columnar section 13 depicted in Fig 3 serves as an enriching section if the motion of heaters 14 is upward Assuming the heater length h in the direction of travel and sufficient heat interchange so that any solid within 75 the heater is molten and any material outside of the heater is solid, it is seen that the upward motion of heaters produces molten regions 14 a, solid regions 15 and voids 16, the latter of a height equal to h-i, where 1 is the 80 length of a molten zone Where re-entrant tube 121 is of negligible cross-sectional area as compared with that of the column, the length of this tube may be considered to be equal to that of a molten zone This sim 85 plifying assumption will be made throughout this description so that the symbol 1 will be used to denote either molten zone length or void generator tube length As each void 16 passes under feed inlet 17, molten 90 material of the system undergoing treatment flows into and fills the void, any material in the void, being of lesser density than the feed material, bubbling up through the feed inlet. With heaters 14 moving in a downward 95 direction, the section depicted in Fig 3 functions as a stripping section and voids 16 behave in the manner described in connection with Figs 2 A to 2 F, bubbling through molten zones 14 a in intermittent fashion, rising 100 toward feed inlet 17 and being filled in turn by molten material passing through that orifice.

Figs 4, 5 and 7 depict three different types of column zone-void refiners Before des 105 cribing these in detail, various general requirements of such zone-void apparatus will be briefly noted Since flow of material from the feed inlet into the voids is usually brought about by the influence of gravity, the column 110 is either vertical or inclined In general, if the void is evacuated or contains material of a lesser density than that of the molten material undergoing treatment at the operating temperature, the feed inlet is higher than 115 the product and waste outlets If, on the other hand, the density of the material in the voids is greater than that of the molten material undergoing treatment at the operating temperature, the feed inlet must be lower 120 than the two outlets and the feed material will rise through the void fluid instead of falling through it at the entrant point. In the design of any apparatus suitable for carrying out the process of this invention, it 125 is necessary that the exit flows of molten material be limited in such a way as to maintain molten zones in the column at all times. Means by which this may be accomplished have been discussed briefly and will be con 130 material in lower region 11 being restrained by the solid material in the lower extremity of tube 9. In Fig 2 B, the heater has advanced so that its lower extremity coincides with the bottom. of tube 9 thereby allowing a portion of molten material to run out of the column and thereby creating first void 12. In Fig 2 C the heaters 8 have advanced in their downward direction It is seen that the only change that has occurred is the downward advancement of molten zones 11 and the consequent reduction in height of solid region 10 immediately above the first void 12 which void, being unable to pass through tlhe solid region immediately above it, remains stationary. In Fig 2 D the bridge of solid above void 12 of Fig 2 C has been melted through and void 12 has bubbled through the molten region 11 immediately above it so that in the view shown the void is directly above the molten material of lower zone 11. In Fig 2 E it is seen that further downward motion of the heater causes void 12 to be entrapped within a solid region 10 but that the lowest molten zone 11 has continued to proceed in a downward direction. In view 2 F the heater has again proceeded sufficiently far to permit the escape of a portion of molten material through tube 9 thereby creating a second void 12 Further advance of heaters 8 causes successive advances of liquid down and voids up the column in this section The broken views of Figs 1 and 2 combine to show material rich

in solvent leaving the enriching section and material rich in solute leaving the stripping section, all for asystem having a k value less than 1, that is, for one in which the solute concentration is greater in the molten phase than in the solid phase at the interface at equilibrium. Fig 3 is an elevation of either an enriching or stripping section depending on the direction of motion of the heaters and also shows a feed inlet In the processes herein described, there must be a net flow of matter from the feed inlet to each of the enriching and stripping outlets It will now be assumed that it is desired to recover purified solvent so that the outlet in the enriching section will be considered to be the product outlet and the outlet of the stripping section, the waste outlet It is, of course, understood that the outlet roles could well be reversed or that they could both be considered to be product outlets Liquid flow is brought about by creating voids in the column at the waste and product ends and by causing these voids to travel to the feed inlet where they are filled with feed liquid As has been discussed in connection with Figs 1 and 2, voids are created by allowing liquid to flow out of the iefinr The cycle of creating a void, causing it to flow to the feed inlet and filling it 786,170 786,170 sidered in more detail in connection with the views of Fig 8. In general, since it is desired to maintain any of the material undergoing treatment within the heaters in a molten state and any such material not within the heaters in a solid state, the walls of the column are uniformly thin and the heaters are closely fitted It may be found advantageous to cool the surfaces of the column not within the heaters where columns of large diameter are used, where the melting point of the material undergoing treatment approximates the ambient temperature or where heat transfer is otherwise inefficient. In describing the operation of the various types of apparatus herein described, it is assumed not only that the material undergoing treatment within a heater is molten and that the other material within the column is solid, but also that the material in the feed inlet is at all times in a molten state or, in any event, that it is in a molten state during a period sufficient to allow feed to flow into each void as it passes under the inlet It is also necessary that all zone-void apparatus be designed so that the walls of the outlet tube do no permanently remain cool and thereby block the system. It may be here noted that it is not necessary that a void occupy the entire cross-section of the column as has been indicated in Figs. 1, 2 and 3 In general, in a vertical column of circular cross-section, a small void will tend to be annular in shape Where the column is inclined the major portion of the void containing material which is lighter than thz.

molten material on which it floats in the enriching section and through which it bubbles in the stripping section will tend to travel adjacent that portion of the columnar waid which is uppermost in displacing its own volume from the top portion of any given molten zone. Fig 4 A is a front elevation and Fig 4 B a side elevation of a simple column-type zone void refiner described and claimed in Application 182/57 (Serial No 786,171) divided out of this application, comprising rectification section 18, stripping section 19, feed tank 122 with associated heater windings 123, product outlet 20, waste outlet 21, heaters 22, and means of actuating these heaters It is seen from Fig 4 A that there are two sets of four heaters each, each set being attached in fixed positions on a heater plate 23 or 24 In operation, heater plate 23 is actuated in a gradual upward motion and plate 24 in a downward motion by virtue of belt 25 which belt passes over pulleys 26, being driven by motor 27 and motor pulley 28 In operation, heaters 22 move upward in the enriching section and downward in the stripping section of the apparatus. When the heaters have advanced an integral number of intervals, where an interval is the distance equal to the spacing between corresponding portions of adjacent heaters, arm 29, shown in Fig 4 B and attached to heater plate 23, actuates clutch release switch 30 thereby 70 releasing magnetic clutch 31 Load weight 32 causes a rapid reverse travel until arm 29 actuates clutch bind switch 33 thereby causing the clutch to engage again whereupon the cycle is repeated In order for the appara 75 tus of Figs 4 A and 4 B to be operative, it is necessary that there be molten material in feed tank 122 and that the uppermost position of top heater 22 in each of the columns 18 and 19 be close enough to tank 122 so that 80 there is free interchange of the molten material within the heater with the feed material, and so that the voids within these heaters may pass into the feed tank The feed tank may be heated by means of heater windings 123 85 and a current source not showvn or by other conventional means If the material being processed is easily contaminated and if the feed tank is open, a protective layer may be floated on the molten feed In the process 90 ing of tin, a layer of lamp-black has proved to be adequate. In apparatus of the type depicted in Figs. 4-A and 4 B, which forms the subject matter of our beforementioned Application 182/57 95 (Serial No 786,171) corresponding points on the heaters are spaced at equal intervals and advance slowlly a total distance equal to an integral number of these intervals When the heaters have advanced an integral number 100 of intervals, for example 1, they are reversed rapidly an equal distance so that each heater coincides with a molten region which was previously behind it after

which forwar 4 travel is then resumed The heater should 105 reverse rapidly enough to prevent substantial freezing of the material within the molten zones. The minimum number of heaters in which a complete column of the type shown in Figs 110 4 A and 4 B can be operated is two, one for the enriching section and one for the stripping section As will be described below, it is possible with extremely simple apparatus to obtain the effect of a large number of stages 115 of separation with this minimum number. A saving in time is obtained, however, by placing a maximum number of heaters as close together as is feasible, the spacing being determined by the efficiency of heat transfer 120 within the column In the enriching section, the minimum spacing between heaters is determined by the requirement that a bridge of solid material be controllably maintained between the molten zones corresponding witix 125 adjacent heaters In the stripping section, however, it is necessary that two solid bridges with a void between them be maintained between successive molten zones during part of the cycle so that the minimum heater spac 130 786,170 ing in this section of the apparatus is greater than for the enriching section, ranging in the order of twice the void height. The practical number of heaters is a matter of design economics and is usually a compromise between minimum separation time and minimum apparatus cost. When reciprocating heaters are used there must be a sufficient number so that extreme positions of the first and last heaters in either section in a given direction are separated by at least the length of the section. An advantage of this reciprocating type of


* GB786171 (A)

Description: GB786171 (A) ? 1957-11-13

Processes for treating fusible material


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BE533921 (A) CH333698 (A) DE1053194 (B) FR1112171 (A) NL97193 (C) US2739045 (A) BE533921 (A) CH333698 (A) DE1053194 (B) FR1112171 (A) NL97193 (C) US2739045 (A) less Translate this text into Tooltip



m: m 7 b e a cis Z':, PATENT S PEII I 'N PATENT SPECIFICATION N 786,171 Date of Application and filing Complete Specification: Dec7, 1954 No 182 j 57. Application made in United States of America on Dec 8, 1953. (Divided out of No 786,170) Complete Specification Published: Nov 13, 1957. Index at acceptance:-Classes 82 ( 1), 13 B; and 90, K 10. International Classification:-CO 1 b, C 22 b. COMPLETE SPECIFICATION PAT Eil TS ACT, i SPECIFICATICN Y C 78264171 In pursuance of Section 9 of the Patents Act, 1949, the Spez-iflaticfl has been amended in the following manner:Page 1, line 90, after 11953) ', insert Zone-ref Sning processes in whichn at least one molten zone is caused to traverse a body of:; aterial in order to produce a redistrlbut 1 cn of 1 i Zredients therein, forms the subject of our Patent No 76-9,673 and, having regarl to the provisions of Section 9 of the Patents Act, 1949, attention is directed to the claims of this patent m. THE PAE'NT OFFICE, 29th -'ay, 1958 segregate solutes and may be applied to systems of metals and their alloys to salts and salt

solutions, both organic and inorganic and to other solvent-solute systems -which can be caused to undergo a liquid-solid transformation. For convenience the processes of this invention -will be described in terms of a binary solvent-solute system in which it will be assumed that the solute is the impurity to be removed and that A the distribu Ltionl coefficient defined as the ratio of the solute concentration in the solid freezing out of a molten zone to that in the liquid in the zone, is constant and less than 1 It is to be understood that the solute could Just as well be considered to be the product which it is desired to recover, that the processes work equally well for systems having a 7 value greater than 1 antd further that the invention is not to be limited to its application to binary systems It should be noted that the constant 1; is identical to and is here used in place of the lower case (reek letter DB 05339/1 (S) /5621 150 55/5 F The processes of this invention utilize the principles of what will be herein referred to as batch zone-refiningz" which principles are amply set forth in the article "Principles of Z:one-Refining" by W G 70 Pfann in Journal of Metals Volume 4. page 47 1952 In one form batch zone-refining consists of slowly passing a series of molten zones through a long solid ingot or charge of impure substance each 75 molten zone for a system having a A value less than 1 causing a net transfer of impurity toward the end of the charge in the direction of travel of the zone It has been shown that extremely high purity 80 can lie attained by this process For example by batch zone-refining, a concentration of significant donor impurities in germanium has been reduced to less than 2 x 1012 atoms per 'cubic centimetre of 85 germanium which in this example was less than one donor atom per 10 ' atoms of germanium (W G Pfann and K r M. Clsen Physical Review Volume 39 page 322 19 35 90 Yv 1 PATENT SPECIFICATION Date of Application and filing Complete Specification: Dec 7, 1954. Application made in United States of America on Dec 8, (Divided out of No 786,1170) Complete Specification Published: 1 ov% 13, 1957. 786,171 No 182157. 1953. Index at acceptance:-Classes 82 ( 1), X l International Classification:-C Olb, C 22 b. COMPLETE SPECI Fji j Q Processes for Treating Fusible Material We, WESTER N ELECTRIC COMPANY, INCORPORATED, of 195, Broadway, New York City, New York State, United States of Ameriea, a Corporation of the State of' New York, United States of America, do hereby declare the invention for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:-

This invention relates to processes for treating fusible materials, and is particularly concerned with redistributing ingredients of fusible solvent-solute systems for the purpose of producing material of desired composition In their more usual applications the processes of this intention utilize variations in solute solubility in adjacent solid and liquid phases in the material being treated to segregate solutes and may be applied to systems of metals and their alloys, to salts and salt solutions, both organic and inorganie, and to other solvent-solute systems which can be caused to undergo a liquid-solid transformation. For convenience the processes of this invention will be described in terms of a binary solvent-solute system in which it will be assumed that the solute is the impurity to be removed and that k, the distribution coefficient, defined as the ratio of the solute concentration in the solid freezing out of a molten zone to that in the liquid in the zone, is constant and less than 1 It is to be understood that the solute could just as well be considered to' be the product which it is desired to recover, that the processes work equally well for systems having a lb value greater than 1 and further that the invention is not to be limited to its application to binary systems It should be noted that the constant 7 k is identical to and is here used in place of the lower case Greek letter gamma (y) which latter symbol has been heretofore used. Where the system undergoing treatment is a semi-conductive material such as, for example, silicon or germanium alloyed 50 with small portions of solute or solutes to which present theory ascribes the extrinsic semiconductive properties of the aforesaid materials, these solutes are known as "significant impurities" or "significant 55 solutes" Due to the high order of purity required in the production of semiconductive materials such as those above set forth, and due to the favourable separation constants which characterize such systems, 60 the processes of this invention are particularly well adapted to the purification of these materials for use in rectifiers, transistors and other semiconductive transducers 65 The processes of this invention utilize the principles of what will be herein referred to as "batch zone-refining" which principles are amply set forth in the article "Principles of Zone-Refining" by W G 70 Pfann in Journal of Metals, Volume 4, page 747, 1952 In one form, batch zone-refining consists of slowly passing a series of molten zones through a long solid ingot or charge of impure substance, each 75 molten zone, for a system having a k value less than 1, causing a net transfer of impurity toward the end of the charge in the direction of travel of the zone It has been shown that extremely high purity 80 can be attained by this process For example, by batch zone-refining, a concentration of significant donor

impurities in germanium has been reduced to less than 2 x 1012 atoms per cubic centimetre of 85 germanium which, in this example, was less than one donor atom per 1010 atoms of germanium (W G Pfann and K >M. Olsen, Physical Review, Volume 89, page 322 1953) 90 786,171 According to one aspect of the present ing drawings. invention a process of treating a fusible Figs 1 A and 1 B are front and side material comprising at least two elevations of a column process containing ingredients, the material being enclosed an enriching and a stripping section s in a colhun, includes the steps of causing together with reciprocating heaters in 70 alternately spaced relatively hot and cold accordance with this invention; regions to progress in one direction from Fig 2 is a perspective view of a column one end of the eoliumn to the other, the refiner using strip heaters; material being molten within the hot Fig 3 is a diagranmmatic front view of regions and solid within the cold regions, a column process in which the column is 75 movement of the regions being caused by of non-uniform cross-section so that the motion of the heat sources producing the refluxi rate may he varied; and hot regions, these heat sources being Fig 4 is a diagrammatic front view oi caused to move in said one direction for a column apparatus using heaters of varya, distance equal to a digital nnmiber of ing size 80 cold region lengths after which the heat Referring now to the drawings Figs. sources are caused to travel the same dis 1 A and 1 B show a side elevation of a tance in the reverse direction at such a simple eolumn-type zone-void refiner Cowrate that the state of the material in the prising rectification section i S, stripping hot and cold regions at the beginning of section 19, feed tank 122 with associated ss said reverse travel is not substantially heater windings 122)3 produet outlet 2 ( 0. changed during the reverse travel, the waste outlet 21 heaters 22 and means of series of steps being repeated at least actuating these heaters It is seen from once Thus the effect of a continuous Fig l A that there are two sets of four succession of heaters can be obtained with heaters each, eaclh set being attached in 90 out having to resort to a column in the fixed positions on a heater plate 23 or form of a substantially continuous ring 24 In operation, heater plate 2:3 is Furthermore, where the material being actuated in a gradual upward motion and treated is of non-uniform cross-seetion, it plate 24 in a downward motion by virtue is possible to construct the heaters so that of belt 25 which belt passes over pulleys 95 they conform closely to the section which 26 heing driven by motor 27 and motor they traverse, pulley 28 In operation, heaters 22 move According to another aspect of the upward in the enriching section and invention a process of treating a fusible downward in the stripping section of the material

comprising at least two apparatus 100 ingredients, the material being enclosed in When the heaters have advanced an a column of inverted U-shape having a integral number of intervals, where an source of feed material at the junction of interval is the distance equal to the the limbs and an outlet for treated spacing' between corresponding portions of material at each open end of a limb, adjacent heaters arnl 29, shown in Fig 10 o includes the steps of producing a molten 1 B and attached to heater plate 2 '. region in each limb by means of a movable actuates clutch release switch 30 therelly heater, a heater being initially at the top releasing magnetic clutch 31 Load wveighlt of one limb and at the bottom of the other 32 caauses a rapid reverse travel until arm limb, simultaneously moving the heaters 29 actuates clutch bind switch 3 thereby lie so that the molten region travels down causing the cl Lutch to engage again wherethe said one limb and up the said other upon the cycle is repeated In order for limb until each limb has been completely the apparatus of Figs 1 A and l B to he traversed by the molten region, reversing operative, it is necessary that there be 50the direction of travel of the heaters so molten material in feed tank 122 and that 115 that they return to their starting positions the uppermost position of top heater 22 the reverse travel of the heaters being at in each of the columns 18 and 19 be lose such a rate that the state of the material enough to tank 122 so that there is free in the limbs does not substantially change interchange of the molten material within during such reverse travel, and repeating the beater with the feed material, and so 12 C the steps a plurality of times that the voids within these heaters Allay The invention is of particular utility in pass into the feed tank The feed tank connection with the'eontinuous zone melt may hbe heated by means of heater Wnding processes described and claimed in injus 123) and a current sourec not shown Application 33413/54 (Serial Qo 786,170 i or by other conventional' means I tie 12, from which this application is divided, material being processed is easily conand the following specific embodiments of taminated and if the feed tank is opel a the invention relate to apparatus suitable protective layer may e Po otedl onl tine for zone void melting as described in the molten feed In the pi ess 1 W Of t'ii a aforesaid application In the accompany-layer of larmpblacl has p 7 rned to he 134 786,171 adequate. In apparatus of the type depicted in Figs 1 A and 1 B, corresponding points on the heaters are spaced at equal intervals s and advance slowly a total distance equal to an integral number of these intervals. When the heaters have advanced an integral number of intervals, for example 1, they are reversed rapidly an equal distance so that each

heater coincides with a molten region which was previously behind it after which forward travel is then resumed The heater should reverse rapidly enough to prevent substantial freezing of the material within the molten zones. The minimum number of heaters in which a complete column of the type shown in Figs 1 A and 1 B can be operated is two, one for the elariching section and one for the stripping section It is possible with extremely simple apparatus to obtain the effect of a large number of stages of separation with this minimum number. A saving in time is obtained, however, by placing a maximum number of heaters as close together as is feasible, the spacing being determined by the efficiency of heat transfer within the column In the enrichingo section the minimum spacing between heaters is determined bv the requirement that a bridge of solid material be controllably maintained between the molten zones corresponding with adjacent heaters In the stripping section, however, it is necessary that two solid bridges with a void between them be maintained between successive molten zones during part of the cycle so that the minimum heater spacing in this section of the apparatus is greater than for the enriching section, ranging in the order of twice the void height. The practical number of heaters is a matter of design economics and is usually a compromise between minimum separation time and minimum apparatus cost. When reciprocating heaters are used in this wav there must be a sufficient number so that extreme positions of the first and last heaters in either section in a given direction are separated by at least the lenoth of the section. An advantage of this reciprocating type of heater is that the apparatus design is somewhat simpler than that in which a continuous heater path is established. Heaters may be rigidly and permanently attached to a heater plate as shown in Figs 1 A and 1 B and may be of any complete ring-type since there is no -necessity of passing them by the feed inlet By the use of voids in the above process it is possible to operate the apparatus in a continuous manner similar to that used in distillation processes For a full description of this use of voids reference is directed to the aforesaid Application 35413/54 (Serial No 786,170). A typical small apparatus suitable for 70 laboratory work may have, for example, a column of about 1/2 inch or more in diameter and an outlet tube or from 1/16 to 1/8 inch or more in diameter. Zone lengths may be about an inch in 75 length with spacing between zones of the same order. An apparatus of large cross-section is shown in Fig 2 It consists essentially of two concentric half-cylinders 52 and 53 80 with

strip-shaped heaters 54 mounted on a rotatable drum or frame not shown. Feed is passed in inlet 55 and with effeetiv-e continuous counterclockwise heater motion, produced by reciprocating travel 85 with controlled refining rate counterclockwise and rapid return an integral number of heater spacings in the opposite direction, product is drawn out of outlet and void generator 56 and waste out of out 90 let and void generator 57 By keeping the thickness of the column, that is, the space between half-cylinders 52 and 53 small, the zone lengths measured in the direction of travel may be kept small, thereby per 95 mitting a large number of zones or stages to exist concurrently. In the methods discussed herein, it may be advantageous to provide cooling between the zones especially for sub 100 stances having a low melting point or high thermal conductivity This may be accomplished by blowing cooling gas at the region between the heaters, by submerging the apparatus in a cool liquid, or by 105 providing heat exchangers in tubular form encircling the column If the latter is used, some of the heat may be returned to the system in ways well known to those skilled in the chemical fields '110 It is well known in the field of separation that when a desired component undergoes a high percentage of enrichment, the net flow through the various stages should differ for effective operation; see for 115 example, H D Smyth, "Atomic Energy for Military Purposes", Prineeton University Press, 1945, at page 167 Stated another way, the downflow should vary, being greater for successive stages 120 approaching the feed inlet The effect of variable downflow can be achieved quite simply in the zone-void process by varying the volume of the molten zones as they travel This may be done either by 125 varying the cross-section of the zones while keeping the zone length constant as in Fig 3, or by varying the zone length in a column of constant cross-section as in Fig 4 or by a combination of the two 130 a 786,171 methods. The apparatus of Fig 3 operates in a manner identical to that of Figs 1 A and l B, feed passing in through feed inlet 112, product passing out void generator 102 and waste being withdrawn through void generator 10:3 In the apparatus shown the motion of heaters 104 is reciprocating. travelling gradually up in enriching seetion 105 and down in stripping section 106 and then rapidly in the opposite direction to complete the cyc-le of heater motion Motion of -he heaters 104 iaiy be brought about by apparatus such as that shown in Figs 1 A and 1 B. The broken section shown in Fig -4 is of a column 107 having heaters 108 varying in surface area and containing solid regions 109, molten regions 110 and voids 111 produced b Ly v-oid generators not shown In such an

apparatus motion of the heaters 108 is reciprocal If travel is gradual in an upward direction, the section depicted is that of an enriching column, whereas if it is gradual in a downward direction the process represented is stripping for a system having a k value less than 1. It will be understood that the reciproeating heater arrangement of the invention can be used with other column arrangements than those described above, whilst the term "column" includes horizontal as well as vertical columns, those inclined at any intermediate angle to the horizontal, and to all types of chambers having openings at either end of any cross-sectional shape whatsoever.


* GB786172 (A)

Description: GB786172 (A) ? 1957-11-13

Improvements in shaft mountings for sheaves, pulleys, sprockets and othermachine elements

Description of GB786172 (A) Translate this text into Tooltip



PATENT SPECIFICATION Inventor: -KENNETH DAVID ZERNY. Date of filing Complete Specification: May 15, 1956.

Application Date: Feb 15, 1955 No 4503/55. Complete Specification Published: Nov 13, 1957. Index at Acceptance:-Class 80 ( 2), 52 B 6. International Classification:-FO 6 d. COMPLETE SPECIFICATION. Improvements in Shaft Mountings for Sheaves, Pulleys, Sprockets and other Machine Elements. We, THE ZERNY ENGINEERING COMPANY LIMITED, of Rickmansworth, Hertfordshire, a British Company, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement: - This invention relates to bush elements of the tapered, longitudinally split contractile type used for the mounting on shafts of sheaves or pulleys or other machine elements by a wedging action Bush elements of this type have been known for many years, being generally made of cast iron. According to the present invention, a bush element of the type referred to is made of hardenable steel, suitably mild steel, and provided in its bore with a plurality of longitudinal ribs such that, after a hardening treatment, the ribs will bite into and form a key in a suitable axle or shaft when the bush is wedged into the hub of a machine element. The ribs are preferably formed with a longitudinal sharp edge for biting into an axle or shaft They may be formed by serrating the interior of the bore longitudinally so as to be of zig-zag section, suitably with 20-80 ribs per inch In one convenient arrangement the faces of each rib are at 90 ' to one another, the faces of the valleys between the ribs likewise being inclined together at 90, although it will be understood that this angle can be varied. This invention is suitable for bushes of the type referred to of the most varied construction, including in particular that deslPrice 3 s 6 d l cribed in Application No 29374/53 (Serial No 750,186). Any appropriate hardening process may be applied to the bush before use, the degree of hardening required being readily determined by those skilled in the art Such process may be applied overall, or concentrated at or confined to the interior face of the bore. The outer face of the bush (or each bush in the case of those described in Application No 29374/53) may be formed with a keyway, suitably a socket for a Woodruff key. In a preferred arrangement two tapered longitudinally split contractile bushes are provided, one being tapped in an axial direction at circumferentially spaced positions, and the other being formed with registering boltholes so that the two can be drawn

together with the narrow ends facing inwards, towards one another, by suitable bolts The splits in the two bushes are not in register The radially inner face of each bush is serrated, the serrations running parallel with the axle at a pitch of about 25 to the inch, and defining a 90 zig-zag.


* GB786173 (A)

Description: GB786173 (A) ? 1957-11-13

Improvements in or relating to thread clamping and cutting devices for looms


PATENT SPECIFICATION 786,173 Date of filing Complete Specification (under Section 3 ( 3) of the Patents Act, 1949): Feb 22, 1956. Application Date: Feb 23, 1955. Application Date: April 4, 1955. Complete Specification Published: Nov 13 1957. No 5390/55. No 9738/55. Index at acceptance: -Class 142 ( 2), E( 9 D 1 l O 1 B), International Classification:-DO 3 d. COMPLETE SPECIFICATION Improvements in or relating to Thread Clamping and Cutting Devices for Looms I, WALTER VERNON {GLEDHILL, of Ty Bryn, Holmfirth, near Huddersfield, in the County of York, a British Subject, do hereby declare the invention, for which I pray that a patent may be granted

to me, and the method by which it is to be performed, to be particularly described in and by the following statement: In a weft replenishing loom in which the replenishment is controlled and initiated by a device known as a feeler, which ascertains the condition of the weft supply in the active shuttles and, when such supply is approaching exhaustion, operates to initiate the action of weft-changing mechanism, it is necessary to provide means to cut the weft extending from the eye of the shuttle to the fell of the cloth. This is usually achieved by a temple thread cutter, which is associated with the loom, temple at the weft change end of the loom, and which is arranged to cut the weft adjacent to the selvedge of the cloth at each weft change The temple thread cutter can only operate effectively if the weft thread extending from the fell of the cloth to the shuttle eye is held taut. For this purpose looms are sometimes provided with a weft grabber, which is adapted to catch and grab the weft thread between the shuttle eye and the temple thread cutter. Such grabbers, usually, have an opening at their rear end, and centrally of the front end of this opening there is formed a recess. This type of grabber is arranged to move rearwardly at each weft change, and the intention is that the weft thread will be caught between the upper and lower jaws of the grabber and guided into the recess at the front of the opening In some cases, there is also provided; a pivoted, clamping lever adapted to be turned to an open position when the grabber is projected rearwardly, but to be turned to a closed position where it co-operates with the lower jaw to nip any thread which lies on the lower jaw, when the grabber returns to h. its forward position, In other words, the clamping lever acts as a pivoted upper jaw cooperating with the fixed lower jaw The chief disadvantage of this arrangement is that the upper jaw instead of nipping a weft thread, sometimes pushes the thread off the lower jaw, thereby causing the thread to hang from the selvedge of the cloth in which position it is apt to be dragged into the fell 'of the cloth by a shuttle, thus producing a trailer in " It is the object of this invention to provide a grabber of an improved construction which is more efficient in operation than known types of grabber According to this invention, a weft grabber for a weft replenishing loom, is provided with a two edged fixed jaw, one edge of which co-operates with a pivoted clamping lever, and the other edge of which co-operates with a cutter operatively associated with the clamping lever The cutter is preferably arranged on the opposite face of the grabber to the clamping lever and, the arrangement is such that in addition to holding the weft thread taut for the temple thread cutter, the grabber also severs the thread at the side of the grabber nearest to the

shuttle, so that the piece of weft thread between the grabber and the shuttle eye falls away and cannot be dragged into the fell of the cloth by a shuttle. A preferred feature of this invention is the provision of serrations on either or both the jaws of the clamp to assist in catching the weft thread. According to a further preferred feature there is provided a fibrous member connected to the clamp so that weft threads caught in the clamp engage with, and are held 'by, the fibrous member. The construction, arrangement and operation of three types of weft grabber in accordance with this invention will now be described by way of examples, with reference to the accompanying drawings. Fig 1 shows a weft grabber connected to the shuttle protector arm of a loom, and the grabber opening device, with the grabber projected to the rear of the loom and with its jaws in the open position; Fig 2 is a side view of the grabber shown in Fig 1 to a larger scale; Fig 3 is a view similar to Fig 2, but with the jaws in the closed position; Fig 4 is a view of the opposite side of the grabber shown in Figs 2 and 3, with the jaws in the open position; Fig 5 is a plan view of the grabber shown in Figs 2, 3 and 4 with the jaws in the open position; Fig 6 is a section on the line VI-VI in Fig 4; Fig 7 is a section on the line VIII-VIII in Fig 4; Fig 8; is an enlarged view of the edge of the pivoted jaw of the grabber looking in the direction of the arrow VIII in Fig 4; Fig 9 is a side view of an alternative form of grabber showing the grabber in its projected position with its jaws open; Fig 10 is a side view of another alternative form, of grabber, again showing the jaws in the open position; and Fig 11 is a section on the line XI-XI in Fig 10. Referring firstly to Fig 1, which shows the positioning of a grabber in a loom, and Figs. 2 to 8 which show this particular grabber, 1 is the breast rail of the loom and 3 is the shuttle protector arm which is turned about a pivot point (not shown) each time the weft changing m 2 echanism is about to be actuated to project its upper end 5 rearwardly between the selvedge of the cloth and the shuttle in the shuttle box where weft replenishment is about to take place. The grabber 7 is fixed to the upper end 5 of the protector arm by means of a bolt 9 and nut 11, the bolt passing through a slot 13 in the forward end of the grabber body 15, which slot allows the position of the grabber relative to the protector arm to be adjusted. Pivoted about a stud 17 on' the rearward end of the grabber body, 15 is a clamping lever 19 the rear end of which forms the upper of a pair of jaws, the lower jaw 21 being fixed to, or made integral with the grabber body 15 As shown in Fig 5, the clamping lever is pressed

against the body 15 by a spring 23 between a washer 25 t and a nut 27 which retains the clamping lever 19 on the stud 17. On the opposite face of the body 15 to the clamping lever, there is mounted a cutter 29 pivoted about a screw which screws into a tapped hole in the stud 17 (It will be understood that the body 15 is drilled and tapped through to the cutter surface of the body to receive the stud 17, and that the latter is itself drilled and tapped at the end which screws into the body to receive the screw 31) A spring 33 situated between the head of the screw 31 and the cutter 29 presses the cutter against the face of the body 15 The screw 31 is locked by a wire 35 which enters the slot in the head 70 of the screw 31 and at its other end is fixed to the body by a screw 37. A peg 39 is screwed into the clamping lever 19, and is locked in position by a locknut 41, a reduced portion 43 of this peg project 75 ing across the body 15 and engaging with a hole in the cutter 29 By this arrangement the clamping lever 19 and cutter 29 are connected, so that when the clamping lever is turned, the cutter is also turned 80 As shown in Fig 1, there is provided, on the breast rail 1 of the loom, a grabber opening device comprising an arm 45 pivoted at 47 to a bracket 49 and formed with a catch 51 adapted to engage with the peg 39 when 85 the protector arm moves the grabber 7 rearwardly The arm 45 is pulled downwardly by a spring 53, one end of which is connected to the arm 45, and the other end of which (not shown in the drawings) is connected to a fixed 90 part of the loom An adjustable stop bar 55 is provided on the bracket 49, to adjust the position of the arm 45 relative to the bracket 49 and thereby to adjust the position of the catch 51 relative to the peg 39 Such a grabber 95 operating device is described and claimed in the Complete specification of Patent Application No 1356/55 (Serial No 781,991). A stop is provided on top of the body 15, comprising a screw 57 and locknut 59, the 1 OC purpose of this stop being to engage with the reduced portion 43 ' of the peg 39, and so limit forward movement of the peg 39 and hence also to limit the opening movement of the clamping lever 19 and cutter 29 10 o The forward end of the clamping lever 19 is formed with a curved projection 61, which is adapted to be struck by the loom sley or a part connected to the sley as the latter advances, after the grabber has been projected 1 li rearwardly It will be clear that when this happens, the clamping lever 19 is turned in an anti-clockwise direction, looking as in Figs. 2 and 3 into the closed position shown in Fig. 3 The closing movement of the clamping lever 11 ' 19 is limited by the end 63 of the projection 61 striking against the underside of a bearing block 65 which is fixed to the body 15 by screws 67. The bearing block 65 carries a stub shaft 69 121 which projects from

and is formed integral with a cam 73 A boss 71 is fixed on the shaft 69 by means of a screw 75 which also acts as an anchor for one end of a tension spring 77, the other end of which is fixed to a 12. screw 79 fixed in the body 15 By this arrangement, the cam 73, is urged into contact with the edge 81 of the clamping lever 19, as shown in Figs 2 and 7. A brush 83 comprising a twisted wire core 131 786,173 786,173 3 and thin phosphor bronze wires or fibres' 87 is fixed at one end in a hole in the cam 731, by means of a fixing screw 89. As can be clearly seen in, Fig 2, the phosphor bronze 'fibres'187 are inclined so that those on top of the brush point slightly forwardly. In Figure 3 the portion of the core 85 carrying the 'fibres' '87 has been broken away for the sake of clearness. The lower jaw 21 is formed with serrations 91 at the clamping lever side, and with a sharp cutting edge 93 at the cutter side The clamping lever 19 is formed with serrations at both sides as indicated in Fig 8 The purpose of these serrations on both the lower jaw and the clamping lever is to increase the tendency of the jaw and clamping lever to grip a weft thread, and the reason for the staggered relationship of the serrations 95 is that if a serration on the lever 19 extended completely across the edge of this lever it would form a slot, and a thread might engage with such a slot and therefore would not be pressed on to the brush Also by serrating both sides, the lever 19 ' can be used on a loom having the weft replenishing mechanism at either end The cutter 29 is formed with a sharp cutting edge 97, which is adapted to co-operate in scissors action with the cutting edge 93 on the lower jaw 21, and it will be seen from (Fig 4, that the clamping lever 19 and cutter 29 are so connected that the serrated edge of ithe lever 19 will nip a thread on the lower jaw just before the cutter 29 will cut that thread. The operation of the above described grabber will now be described In the nonoperative or set position, the grabber 7 is in a forward position out of the way of the loom sley, and the various parts of the grabber are in the positions shown in Fig 3 ' In this position the clamping lever 19 ' is in the closed position, the cam 73 pressing against the edge 81, of the lever 19 and pressing the end 63 of the projection 61 against the underside of the bearing block 65. When the weft changing mechanism is about to operate, the upper end 5 ' of the protector arm 3 moves rearwardly, and the peg 39 engages with the catch 51 on the arm 45 Further rearward movement of the grabber,7, causes the lever 19 to turn into the open position shown in Figs 1 and 2 During this turning movement, the cam 73 ' will be turned by virtue of its engagement with the 'edge 81 of the lever 19, and consequently the spring 77 is extended The grabber is projected rearwardly of the

catch 51 to the, position indicated in broken 'ines in Fig 1. As the sley moves forwardly the weft thread extending from the fell of the cloth to the shuttle in the box will enter the space between the lower jaw 21 and the lever 19 This can be made more certain in some cases if the loom is provided with a weft holding brush as described and claimed in the Complete specification of patent application No 37464/ 54 (Serial No 779,285) In this position part of the weft thread will lie across the top of 70 the brush 83, Further forward, movement of the sley causes pant of the sley to strike the projection 61, which turns the lever 19 to its closed position. The closing of the lever, 19 nips the weft 75 thread between the edge of the lever 19 and the lower jaw 2,1, and then severs the thread between the cutter 29 and the lower jaw 21. At the same time, the camn 73; will be turned by the spring 77, so that the brush 83 is 80 turned in a clockwise direction looking in the direction of the arrow "BR" in Fig 2 This twisting of the brush causes the weft thread to 'be pulled into the phosphor bronze 'fibres' 87 where it is held 85 The protector arm 3 ' then returns to its original position taking with it the weft thread which extends from the fell of the cloth and which is later cut at the selvedge by the temple thread cutter 90 An alternative form of grabber for use with a different type of loom is shown in Fig 9 A bracket 101 is pivoted on a shaft 103 which extends from the weft replenishing mechanism and this bracket carries a grabber 95 arm 105 which is pivoted on a stub shaft 107. The bracket 101 and arm 105 are normally positioned with the arm 105 ' inclined to the vertical, the lower end being forward of the upper end, Fig 9 shows the parts with the arm 100 bracket turned so that the arm is in the projected or rear position. A compression spring 109 is fixed in a hole 111 in the bracket 101, so that if the lower end of the grabber arm 105, or the parts it 105 carries, meet with any obstruction as the bracket 101 is turned, the spring 109 will be compressed. Fixed to the arm 105 by screws 151 and 1513 is an extension 113 from a grabber body 110 The grabber itself has a lower jaw 117, a clamping lever g 19 ' and a cutter (not shown) the construction and mounting of which are all similar to the corresponding parts of the grabber 7 described with reference to Figs 1 115 to 8 In this constructions however, the peg 121 (which is the same as the peg 3,9 on the grabber 17) engages with a hole in one end of a lever operating rod 123, and the rod 123 is retained on the peg 121 by a split pin 125 120 The other end of the rod 123 carries, a bracket 127 which is secured to the rod by a setscrew 129 This bracket 127 is pivotally mounted on a shaft 131 which projects from the weft re& plenishing

mechanismparallelwiththeshaft 103 125 Alsp pivotally mounted on the shaft 131 is a brush operating rod 133, the lower end 135 of which is bent at right angles to the main part of the rod, and projects through one of a series of holes 13,7 in a brush lever 139, 130 786,1,73 being secured in this hole by a nut 141 The brush operating red 133 is thus pivotally connected to the lever 139 which is itself pivoted to the body 115 'of a stud 143. A brush comprising a wire core 145 and phosphor bronze ' fibres'147 is fixed into a hole in the lever 139 by a screw 149 This brush is similar to that described in the arrangement shown in Figs 1 to 8 except that it will be noticed that the 'fibres'147 do not extend below the core 145, having been cut or ground away to present a smooth under surface of the brush to avoid catching loose weft threads on the underside where they might easily be dragged into the fell of the cloth by a shuttle. When a weft change is abouit to take place, the bracket 101 is turned from its inoperative position to the position shown in the drawing, where the lower jaw 117 will lie beneath the weft thread extending from the fell of the cloth to the eye of the shuttle in the shuttlebox when the sley moves forwardly on the beat-up During this turning movement of the bracket 101, the rods 123 and 133 cause the clamping lever 119 to move into the open position, and the brush to be lowered to the position shown in Fig 9. When the bracket 101 is turned back to its inoperative position in the direction of the arrow C, the rods 123, and 133 cause the clamping lever 119 and brush to be turned in the directions indicated by the arrows D and E respectively, to the position where the weft thread is clamped and' cut, and the part between the temple cutter and, the grabber is suspended on the brush. It will be appreciated, that various adjustments of the parts of this type of weft grabber are possible The extension 1139 and with it the body 115 of the grabber can be adjusted relative to the arm 105 by slackening the screw 151 and turning the extension 113 about the screw 153 (such a turning movement being permitted) by a slot 155 in the extension 113 through which slot the screw 151 passes The effective length of the lever operating rod 123 can be varied by slackening the screw 129 and sliding the rod'123 through the bracket 127 whilst the effective length of the 'brush lever 139 can be varied by fastening the lower end of the rod 1133, in a different hole in the series 137. A further alternative grabber is shown in Figs, 10 and, 11 in which construction, the grabber body 156 is formed integral with an arm 157 adapted to be secured to a part of the weft replenishing mechanism by a screw 159 and a further screw (not shown) which passes through the slot 161 By this fixing arrangement the body, 153 ' and arm 157 can be

adjusted relative to the part to which they are fixed by turning the arm 1517 about the screw 159. The lower jaw 163, clamping lever 165 and cutter (not shown) are all arranged similar to the corresponding parts on the grabber 7, and the clamping lever 165 is adapted to be turned by the rod 16,7 which is fixed at one end to a fixed part of the loom, and at its 70 other end is pivoted to the lever 165 at 168. The grabber is also provided with a cam operated brush 169 which is similar to that described with reference to Figs 1 to 8, the tension spring 171 being anchored at its upper 75 end to a screw hook 173 fixed to the body 156 In this case, however, the brush is smooth on the underside as in the arrangement shown in and described with reference to Fig 9. The cam 175 engages with the face of the 80 lever 165 which is chamfered at 177 as shown in Fig 11 to allow the cam to operate smoothly. Apart from the differences consequent upon the mounting of the grabber and the arrange 85 ment of the cam 175 and lever 165, the operation of this grabber is identical with that described with reference to Figs 1 to 8. It will be appreciated that various refinements described with reference to one of the 90 above three constructions may be used' with the others For instance the brush used on the grabber 7 may be smooth on the underside as are the brushes described in the two alternative arrangements 95 Also the clamping levers 119 (Fig 9) and (Fig 10) need only be serrated on the side which bears against the lower jaw as these grabbers are not intended to be applicable to either hand of loom as is the grabber 100 shown in Figs 1 to S. In describing the brushes used in the above exemplary descriptions, references to phosphor-bronze ' fibres' are intended to mean very thin phosphor-bronze wires, but it will 105 be appreciated that any other suitable fibre may be employed. It will also be noted that in Figs 9 and 10 the rods 123 and 167 are cranked This is to allow space for the weft threads which float 110 over the grabber as it is moved rearwardly, and to prevent these weft threads being broken by the rods 123 and 167.


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