* GB784778 (A)

Description: GB784778 (A) ? 1957-10-16

Improvements in and relating to three-heat electric switches

Description of GB784778 (A)

PATENT SPE Ci FICATION 784 778 Date of Application and filing Complete Specification: May 16 1956. No 15265/56 Complete Specification Published: October 16, 1957 Index at acceptance:-Class 38 ( 5), BMP 2, 12 (B 3:B 6:Bll:E). International Classification:-',101 n H 02 c COMPLETE SPECIFICATION Improvements in and relating to Three-Heat Electric Switches We, WARMEX LIMITED, a British Company, of 375, Milton Road, Cambridge, and ARTH Up R GOLDSTEIN, a British Subject, of the same address, 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 electric switches and particularly such switches for electric blankets, of the type which have a miniature tell-tale lamp located in the switch casing visually to indicate through the transparent or translucent material thereof or a window therein, when the current is switched on and the blanket in circuit. Hitherto such switches which include tell-tale lamps, for electric blankets, have only been constructed for use with and in the circuit of electric blankets having a single heating wire or element which allows for no variation of heat to be given to the blanket. Electric blankets however are known having two heating wires or elements, connected by a triple conductor to a so-called " three-heat" switch, which also has terminals for connection to the usual double conductor to the mains. In addition to the position or positions into which the parts of this three-heat switch are set when the blanket is out of circuit, it can be set into three other positions in which the blanket is in circuit In one of these, both heating wires or elements of the blanket, connected in series, are in circuit; in another, one wire or element

alone is in circuit; whilst in the third position the two wires or elements connected in parallel are in circuit Consequently, three variations of heat can be given to the blanket at the choice of the user. Multi-position electric switches of the kind comprising a rotary member carrying a lPrice 3 s 6 d l plurality of axially-spaced contacts cooperating with a plurality of series of angularly spaced fixed contacts provided within a housing and arranged in different transverse planes, are known for controlling the 50 connections of heating resistance means employed with electric heating apparatus, such as electric stoves, electric heaters, and like electric heating appliances and apparatus, and which include a " pilot light," pilot 55 light circuit, and switch means for controlling said circuit, wholly within the switch casing, and wherein the pilot light is energised only during the actual circuit closure on each and all of the several heats, the pilot light being 60 visible through an opening in the switch guarded by a transparent cover. According to the present invention, a three-heat switch for an electric blanket having two heating wires or elements, in 65 cludes in its construction a tell-tale lamp the light from which is visible when the blanket is switched on through the material of the switch casing or a window therein, the said lamp being connected to two exist 70 ing contacts of the switch provided for the said triple conductor and mains supply, which are at different potentials when the switch is in any one of the " on " positions. Preferably, the tell-tale lamp is a glow 75 lamp and is in series with a resistance, and the lamp and resistance are arranged in parallel with the terminals to which they are connected, that is, in effect they are in parallel across one or both of the heating 80 wires or elements. In a preferred arrangement one connection to the lamp is always to a terminal in the switch connected to one lead of the mains, whilst the other connection to the 85 lamp is always to the terminal in the switch of the lead of the triple conductor which is connected to the junction between the two heating elements of the blanket. The invention is particularly suitable for 90 J a-Jc d 784,778 use with the known type of three-heat electric switches for electric blankets having a rotary member carrying a plurality of circumferentially spaced and grouped contacts, co-operating with fixed contacts having terminal connections to the leads for the supply and to the blanket. In certain constructions and especially to adapt the present invention to such existing three-heat switches for electric blankets, the lamp and its associated resistance can be carried by a shaped member of

insulating material having contacts on one surface connected to the lamp and resistance circuit, which is fitted between the switch cover and body so that, when the parts are assembled, the contacts connect up with the requisite terminals, contacts and connections in the switch body to hold the lamp in position for its glow to be seen through the transparent or translucent switch cover or a window therein. In order that the invention may be better understood, it will now be described with reference to the accompanying drawings which are given by way of example only and in which:Fig 1 is a front elevation of one form of three-heat switch for an electric blanket constructed according to the invention. Fig 2 is a top plan of Fig 1. Fig 3 is a similar view to Fig 2 but with the cover removed and parts broken away. Fig 4 is a top plan of a component of the switch according to the invention, to be fitted on the switch body shown in Fig 3, before the cover is attached in position. Fig 5 is a plan of the cover, with the component shown in Fig 4 in position, taken from below. Figs 6 and 7 are sectional elevations, to a somewhat larger scale, of details shown in Fig 3. Fig 8 is an electrical diagram of the switch shown in Fig 3 and the blanket heating wires or resistances, in one "switched-off" position. Figs 9, 10 and 11 are similar views of the switch in the three "switched-on" positions, and Fig 12 a similar view of the switch in the other "switched-off " position. The drawings show a three-heat switch for electric blankets, of known type, with certain additions and modifications to constitute a switch according to the present invention. In the drawings, 13 is the body of the switch formed from insulating material and go consisting of an outer casing 14 with an integral upstanding annular platform or ridge 15, surrounded by a groove 16 opening into the axial half sockets 17 and having a central cylindrical cavity 18 in which is mounted a central spindle 19 on which turns a cylindrical rotor or drum 34 of insulating material by means of the handle 20 which projects to the exterior where it has an operating thumb-piece 21 This handle is shown broken away in Fig 3 but it has five 70 definite positions of setting, viz VIII, IX, X, XI and XII, spaced 30 ' apart and which correspond to the diagrams Figs 8 to 12 to be hereafter described. The ridge 15 has mounted therein termi 75 nals 22 and 23 in Fig 3 spaced at 120 ' apart, 22 being 600 on one side of the horizontal axis and 23 being 600 on the other side These are the terminals for the

supply or main leads 24 and 25 which pass 80 as a duplex cable into the socket at this end and then into the groove 16. The ridge 15 also carries terminals 26, 27 and 28, the first 26 spaced at 30 ' from the terminal 22 and being spaced at 60 from 85 27, which is spaced 600 from 28; thus, the terminals 27 and 28 are located at 300 on each side of the horizontal axis The terminals 26, 27 and 28 are for the leads to constitute the triple conductor to the blanket, 90 and 66 is hereafter termed the " common " lead, 67 the " outer " lead and 68 the "'central " lead The terminals 22, 23, 26, 27 and 28 have contact tongues 29, 30, 31, 32 and 33, respectively, connected thereto which 95 project down into the cavity 18 of the casing which forms part of the body of the switch. The rotor 34 carries on its cylindrical face two groups of strip contacts One group of four-35, 36, 37 and 38-are spaced at 300 100 apart and connected at the end by an integral portion 39 (Fig 8) The other group of five -40, 41, 42, 43 and 44-have 40, 41 and 42 at 30 ' spacing, 42 and 43 at 60 ' apart, and 43 and 44 at 30 ' spacing; these are con 105 nected at the end by an integral portion 45 (Fig 8) The two groups at their ends are spaced at 30 ' apart. The mounting and arrangement is as shown in Fig 3, where the switch is in one 110 extreme out-of-circuit position represented by the handle position VIII and is such that when the handle is moved in a counterclockwise direction to the position IX the contact 35 connects with the terminal 26 115 and the contact 40 with the terminal 23, whilst the other contacts connect with other terminals to be more fully explained hereafter. As thus far particularly described the 120 switch is as hitherto constructed and it is completed by a cover having complementary half sockets for the duplex cable and triple conductor, which cover is secured in position by screws 46 engaging threaded bores 125 47 in the ridge 15. In the case of the particular switch according to the present invention being described, the cover 48 is either of transparent material and is lined on its flat inner 130 784,778 surface with a sheet 49 of opaque material with a rectangular slot 50 to leave a transparent window 51 to the interior, or it can be moulded in a translucent plastic, leaving for a window a thinned-out portion of the plastic Further, this cover on the interior has such volume and shape that it can accommodate the component shown in Fig. 4 between itself and the switch body when the cover is screwed into position. This component comprises a somewhat crescent-shaped carrier 52 of insulating material, the end portions of which are thinned and apertured at 53 to coincide with j 5 the threaded bores 47 The central

portion is thickened and on its upper side is recessed at 54 to accommodate a miniature glow lamp 55 which on the assembly is so positioned that it comes beneath the transparent window 51 so that when alight this fact is readily visible. At one end the recess 54 opens into another recess 56 for a resistance 57 in series with the lamp 55 The ends of the lamp and resistance circuit are connected to pins 58 and 59 passing through and held in the thickened part of the carrier 52 and terminating in slightly projecting contacts 60 and 61 on the flat underside of the carrier (Fig. 5) When the parts are assembled, these contacts 60 and 61 come above the terminal 22 and another free terminal 62 mounted on the ridge 15. The terminal 22 is shown in Fig 6 and the head of the screw serves to secure a spring contact 63 in position above the terminal, as shown Similarly, as shown in Fig 7, the head of the screw of the terminal 62 serves to secure a spring contact 71 in position above the terminal These spring contacts are slightly and forcibly depressed by the contacts 60 and 61 when the parts are assembled and hold the lamp 55 and resistance 57 in the required circuit. 64 is a conducting wire which connects the terminals 62 and 28 In Fig 3 the wire is shown as a dotted line on the exterior of the switch casing, for the sake of clearness. Actually, it is disposed in the groove 16 so beneath the insulated leads 66 and 68. In the operation of the switch according to the invention, it is pointed out that Fig. 8 and also Fig 3 show one position in which the blanket is out of circuit and consequently the lamp 55 not lit This is due to the fact that although the contact 60 (Fig 5) is in connection with the terminal 22 and supply lead 24, yet the contact 61 (Fig 5) although connected to the group of contacts 40 to 44, through the terminal 62, wire 64 and terminal 28, is not "live" as the contact 40 is at 30 spacing from the terminal 23 for the other supply lead 25. The other position in which the blanket is out of circuit is the position of the parts when the handle is set into the position XII, Fig 3 This is set out in Fig 12 where although the contact 60 is above and connected to the terminal 22 and the contact 61 above and in connection with the termi 70 nal 62, the supply lead 25 is isolated. In the other three positions of the switch, that is, the " on " positions, shown in Figs. 9, 10 and 11 and corresponding to the positions IX, X and XI of the handle in Fig 75 3, the blanket is switched into the circuit, the contact 60, as in Figs 8 and 12, remaining connected to the input lead 24.

In Fig 9 the connections to the blanket are via the common lead 66 and the outer 80 lead 67 so that both of the heating wires or elements 69 (Fig 8) connected in series, are in the heating circuit The central lead 68, however, is " live " due to its connection to the junction between the two heating ele 85 ments 69 and 70, and consequently its connection via the wire 64, terminal 62 and contact 61 completes the circuit through the lamp, in parallel with part of the heater circuit 90 In Fig 10 the connected contacts 35 and 36 bridge the gap between the terminals 22 and 26 and the connected contacts 41 and 43 the gap between the terminals 28 and 23. The common lead 66 and central lead 68 95 are thus the conveyors of current to the heating wire or element 69 alone, and the lamp is lit owing to its associated contacts and 61 being connected in parallel with the live terminals 22 and 28 In this case it 100 should be appreciated that the outer lead 67 to the blanket is cut out as its terminal contact 32 comes in the gap between the two groups of moving contacts of the rotor. In Fig 11 the group of four contacts con 105 nect the common lead 66 and the outer lead 67 to the supply line 24 and the group of five contacts the central lead 68 to the supply line 25 As a result, both heating wires or elements 69 and 79 are in circuit arranged 110 in parallel and the lamp 55 is alight by the same connections as set forth for Fig 10. Obviously, switches for electric blankets in accordance with the invention can take many forms other than that particularly 115 described For instance, in place of the lamp and resistance being mounted in a separate component, this structure could be integral with the cover and in this case the recesses for the lamp and resistance would be open 120 from below Care would also be necessary to arrange that the closed top of the lamp recess was thin enough for the glow to be seen from the exterior In this last-mentioned form, in place of a contact such as 61 being 125 located above a terminal such as 62, provided for the purpose, it could come above a terminal such as 28 for the outer lead 68, and the terminal 62 dispensed with The wire 64 would then be replaced by a wire 130 784,778 in the cover leading to its associated contact 61. In other variations the moving part of the switch could have a rectilinear path and the other parts be modified accordingly. The invention is not limited to the precise forms or details of construction herein described, as these may be varied to 3 wit particular requirements.

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* GB784779 (A)

Description: GB784779 (A) ? 1957-10-16

Dynamo-electric machine rotor spider

Description of GB784779 (A)

PATENT SPECIFICATION Date of Application and filing Complete Specification: June 1, 1956. Application made in Sweden on June 18, 1955 Complete Specification Published: October 16, 1957 784,779 No 16944/56 Index at acceptance:-Classes 35, A 13 X; and 83 ( 2), A 44. International Classification:-B 23 p H 02 k. COMPLETE SPECIFICATION Dynamo-Electric Machine Rotor Spider We, ALLMANNA SY PNSKA ELEKTRISKA AKTIEBOLAGET, a Swedish Company of Visteras, Sweden, 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: - The present invention relates to a l O dynamo-electric machine rotor spider of thekind comprising a hub and arms extending from the hub for carrying an annular armature core made from magnetic stampings. According to the invention a dynamoelectric machine rotor spider is characterised in that it consists of a number of thick rectangular sheets each of which along one edge is welded to the side of its adjacent sheet with the sheets arranged in such a way that the parts of the sheets between the welded joints form a hub in the form of a tube of polygonal section and the other parts of the sheets form arms extending from said tube for carrying the armature The said tube of polygonal section, the inscribed circle of which has a smaller diameter than the shaft intended to carry the rotor spider, is turned

internally to fit the said shaft and is provided with a key groove, and thus forms a hub The arms. which preferably leave the hub tangentially, are turned at their ends remote from the hub to fit inside the annular armature core of the machine. The spider according to the invention is very suitable for mounting the rotor of a direct-coupled exciter for a large electric generator Such generators are usually designed, and made in accordance with, the wishes of the purchaser and are very seldom standardised The auxiliary machinery, however, is very often constructed from standardised parts Thus, for example, the exciter may be constructed from a standard annular armature core made from stampings which is fixed to the generator shaft by means of a spider adapted to fit the shaft in question. An advantage of the invention is that no 50 separate hub is necessary as in the case of spiders used at present Due to this it is a simple and inexpensive matter to construct a spider to fit inside a standard annular armature core and onto a non-standard 55 generator shaft Hitherto the cost of the separate hub has been a considerable part of the total cost of the spider. A spider according to the invention will now be described with reference to the ac 60 companying drawing, in which Figure 1 is a end elevational view of the spider and Figure 2 is a longitudinal section along the line A-A of Figure 1 65 Referring to the drawing, 1 designates plane thick rectangular sheets and 2 the welded joints joining the sheets together. The parts 3 of the sheets 1 between the welded joints form the sides of a tube or 70 hub of polygonal section which is turned internally to fit a shaft 5, and is provided with a key-groove The hub is secured against rotation relative to the shaft 5 by a key 6 The outer parts 4 of the sheets 1 75 form arms carrying an annular armature core (not shown).

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* GB784780 (A)

Description: GB784780 (A) ? 1957-10-16

Method of dissolving or dispersing metal naphthenates in liquidhydrocarbons, especially lubricating oils

Description of GB784780 (A)

A high quality text as facsimile in your desired language may be available amongst the following family members:

CH323327 (A) DE1006564 (B) FR1076375 (A) NL111902 (C) FR66722 (E) CH323327 (A) DE1006564 (B) FR1076375 (A) NL111902 (C) FR66722 (E) less Translate this text into Tooltip

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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.

PATENT 8 PECIFICAT 1 784,780 Date of Application and filing Complete Specification April 13, 1953. /& ue No 10082/53. Application made in Germany on April 12, 1952. Application made in Germany on May 2, 1952. Application made in Germany on May 16, 1952. Complete Specification Published Oct 16, 1957. Index at Acceptance:-Class 91, F 1. International Classification: -CI O m. COMPLETE SPECIFICATION Method of Dissolving or Dispersing Metal Naphthenates in Liquid Hydrocarbons, especially Lubricating Oils We, RHEIN-CHEMIE GESELLSCHAFT MIT BESCHRINKTER HAFTUNG, a body corporate organised according to the laws of Germany, of Heidelberg, Germany, 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: It is known to add oil-soluble soaps or salts of sulphonic acids to mineral oils in order to bind sulphurous or sulphuric acid formed during the combustion of fuels containing sulphur This is necessary because the free acids lead to the formation of resinifying or coking products on the pistons, piston rings and oil wiping rings The use of metal salts of naphthenic acids, especially barium or aluminium naphthenate, has been proposed for this purpose As is known, salts of naphthenic acid are also used in admixture with organic solvents, especially liquid hydrocarbons, for various purposes in chemical technology, for example, in the fields of impregnation, pest control, and plastics However, they are difficult to use owing to their physical properties. They form gels with liquid hydrocarbons or are insoluble or sparingly soluble in liquid hydrocarbons In consequence they considerably increase the viscosity of the liquid hydrocarbons with which they are mixed This increase in viscosity does not permit, for example, large amounts of metal salts of naphthenic acids having polyvalent cations to be incorporated with engine oil, so that in the case of high power engines, which are driven with fuels containing considerable amounts of sulphur, insufficient cations are present to bind sulphuric acid formed and to prevent undesired attack on lubricating oil films and on engine parts. In order to enable the metal naphthenates, which in the pure state are solid and in some case brittle substances, to mix easily with solvents, especially liquid hydrocarbons and hydrocarbon oils, it has been proposed to use solution promoters of various kinds, for example, glycols, glycol esters of lower acids and glycol ether with alcohols of low molecular weight. The present invention is based on the observation that the solvent action of solution promoters can be combined with other actions which are favourable to the properties of the solutions produced therewith and to the purposes for which the solutions are used. An object of the invention is to provide for use in dissolving metal salts of naphthenic acids in liquid hydrocarbons solution promoters which lower the viscosity of hydrocarbon oils containing metal naphthenates and at the same time exert a solvent or dispersing action on resinfication products and other decomposition products of the oil. A further object of the invention is to provide, in addition to the solution promoter which is hereinafter referred to as " solvent A ", a second substance, referred to as " solvent B ", which supplements the action of solvent A. The invention also includes special procedures for preparing mixtures of metal naphthenates with liquid hydrocarbons or hydrocarbon oils with the aid of solvent A and, if desired, also solvent B It has been

found that in many cases it is of advantage first to prepare a solution or mixture of the metal naphthenate with the solvents A and B, and then to mix the resulting solution or mixture with the liquid hydrocarbon Solutions consisting of the metal naphthenate, a solvent A and a solvent B have been found especially valuable as additives to hydrocarbon lubricating oils, in particular engine oils Accordingly, the invention also includes the preparation of metal naphthenate-containing compositions having special properties and their use as additives to hydrocarbon lubricating oils. In accordance with the invention liquid solutions or liquid dispersions of metal salts of _ 784,780 naphthenic acids, especially barium naphthenate or aluminium naphthenate, in liquid hydrocarbons or hydrocarbon oils, such as mineral oils, and especially lubricating oils, are prepared with the aid of an etherified or esterified polyaliylene glycol of the general formula XO-RP-O),-R-OY, in which R represents an alkylene radical 2 or 3 carbon atoms, N represents a whole number from 2 to 20 or higher, and especially from 2 to 7, X represents a hydrocarbon or acyl radical containing more than 6 carbon atoms, and advantageously more than G carbon atoms, and Y represents a hydrogen atom or a hydrocarbon or acyl radical containing any desired number of carbon atoms The etheriie-d or esterified polyalkylene glycol of the above general formula constitutes the solvent A referred to above. As etherified polyalkcylene derivatives there come into consideration, for example, the following:Dodecyl pentaethylene glycol, octadecenyl hexaethylene glycol, lauryl pentapropylene glycol (the term " jauryl" throughout the specification denotes the hydrocarbon radical of the fatty alcohols obtained from coconut oil fatty acids), 2-ethylhexyl pentaethylene glycol, nonyl heptaethylene glycol, phenylethyl pentaethylene glycol, methyl-cyclohexyl octaethylene glycol, para-actyl-phenyl tetrapropylene glycol, dodecyl cyclohexyl hexapropylene glycol, hexylnaphthyl tetraethylene or tetrapropylene glycol. As polyalkylene glycols etherified on both sides there may be used, for example, the following: Dodecy I or lauryl pentaethylene glycol methyl ether, para-octylphenyl tetraethylene glycol isopropyl ether, octadecenyl hexaefnylene glycol ethyl-hexyl ether, 2-ethylhexyl heptaethylene glycol benzyl ether As alcohols for the etherification there may also be used those which are obtainable by the reduction of natural or synthetic fatty acids, by the hydrogenation of carbon monoxide under atmospheric or superatmospheric pressure, by the oxo-synthesis or by the oxidation of paraffin wax. Among the polyallylene glycols esterified on one or both sides there are suitable, inter aia, pentaethylene glycol rnonostearate,

hexaethylene glycol monostearate, dodecyl-benzyl pentapropylene glycol oleate, stearyl-pentaethylene glycol isopropyl ether, bzizoylpentaethylene glycol oleate, benzoyl-1 lieptaethylene or heptapropylene glycol cctyl ether or benzoyl-pentaethylene glycol methyl ether. in general there are advantageously used fatty alcohol polyglycol ethers of the foregoing formula, in which N advantageously represents 4 Of advantage are those ethers or esters of the above formula in which X represents a hydrocarbon or acyl radical containing 12 carbon atoms. The solutions of metal salts of naphthenic acids in liquid hydrocarbons can be made in accordance with the invention in various ways. The metlhod used depends on the particular metal naphthenate, polyglycol derivative and the hydrocarbon oil in which these substances are to be incorporated It is of advantage to work at a raised temperature, for example, at 90-150 C C For example, the aforesaid components may be mrixed together, advantageously while stirring at a raised temperature, or a solution, a gel or a suspension of a metal naphthenate in a liquid hydrocarbon may be mixed with the palyalkyiene glycol derivative Alternatively, the metal naphthenate may be added, while stirring, to a solution of a polyalkyleine glycol derivative in a liquid hydrocarbon Finally the two components may each be sepa-rately dissolved in the liquid hydrocarbon and the solutions subsequently muied together. The proportion of the polyalkylene glycol derivative required may vary within wide limits, for example, from 1 per cent by weight calculated on the metal naplhthenate up to an equal weight or higher 1 ihe proportion to be added depends on the nature of the metal naphthienate used and also of the liquid hydrocarbon and on the viscosity of the desired solution. The following examples illustrate the invention, the parts and percentages being by weight: EXAMPLE 1 100 The capacity of lauryl pentaethylene glycol ether for lowering the viscosity of mixtures ot mineral oils with various metal salts of naphthenic acid is strong This is shown by the table given blowv The parts by weight of the 105 naphlthenates given below are stirred into 159 parts by weight of a mineral oil (specific gravity at 20 C = O 882, viscosity index= 89, carbon number according to Gonradson= 0.11, constituents insoluble in benzene= 0) at 110 a temperature of 1 C 0-110 C until a homogeneous mixture is obtained, and the viscosities of -the resulting slutieons are determined at O C or 50 C The same solutions are mix-d with lauryl pentaethylene glycol ether 115 in the proportions by weight given in the table and the viscosity of the

solutions is determined at 80 C or 50 C. -784; 7 j 8 Parts by weight Parts by of lauryl penta Viscosity at of l a C y penta-tke Naphthenate weight glycol ether C centistokes Aluminium naphthenate l 80 27 59 ,, 1 0 4 80 19 80 Aluminium and calcium naphthenate 5 + 5 80 49 99 ,,, ,, 5 + 5 4 80 30 00 Zinc naphthenate 30 800 72 76 ,,, 30 4 80 37 04 Iron naphthenate 30 50 119 02 ,,, 30 4 500 108 20 Lead naphthenate 30 50 85 2 ,,> 30 4 50 78 EXAMPLE 2. The addition of polyalkylene glycol derivatives lowers the viscosity also in the case of naphthenate solutions which are themselves of low viscosity A solution of 30 parts by weight of calcium naphthenate in 100 parts by weight of a hydrocarbon oil having a boiling range of 150-270 C and resembling Diesel oil has a viscosity of 3 02 centi-stokes at 80 C By the addition of 8 parts of methyl heptaethylene glycol naphthenic acid ester to 100 parts of the aforesaid solution the viscosity is lowered to 2 74 centi-stokes at 80 C. EXAMPLE 3. The viscosity of a mineral oil having a viscosity of 18 7 centi-stokes at 80 C is increased to 29 5 centi-stokes at 80 C by dissolving therein 10 per cent of potassium naphthenate The addition of 20 per cent of decyl pentaethylene glycol ether to the solution lowers the viscosity to 21 26 centi-stokes at 80 C. The methyl ether of the aforesaid polyglycol ether or its benzoate has a similar action. EXAMPLB 4 parts of tetrahydronaphthalene and 20 parts of barium naphthenate have an average viscosity of 15 5 centi-stokes at 80 C By adding 10 parts of lauryl pentaethyleneglycol ether to 100 parts of the aforesaid solution, the viscosity falls to 1 76 centi-stokes at 80 C. EXAMPLE 5. The neutral barium naphthenate prepared from distilled naphthenic acids having an acid number of 180 is a brittle resin at ordinary temperature, which changes into a rubberlike condition at about 100 C and has a dropping point of over 230 C It is only very sparingly soluble in mineral oils and the solution yields a stiff jelly after cooling A fatty alcohol containing 6 8 per cent by weight of hydroxyl and obtained by hydrogenating under a high pressure a fatty acid obtained by the oxidation of paraffin wax, is oxyethylated in known manner with 5 mols of ethylene oxide with the use of an alkali as a catalyst, and there is obtained a polyglycol ether which is wax-like at room temperature and has a dropping point of 38 C. When 40 parts of the brittle barium naphthenate are mixed at about 100 C with 15 parts of the aforesaid polyglycol ether, while stirring

well, the rubber-like structure disappears, and after cooling there is obtained a syrup which can be drawn out into filaments and which is easily soluble without leaving any residue in liquid hydrocarbons. In many cases it has been found advan. tageous when incorporating a metal salt of a naphthenic acid in a liquid hydrocarbon with the aid of a polyglycol derivative (solvent A), also to use an ether (solvent B), which is free from polyglycol groups and contains at least one radical having 6 or more carbon atoms. The ethers may be of the aliphatic, aromatic, or alicyclic series or of a mixed character It has been found very advantageous to use high boiling ethers which are liquid at room temperature These ethers differ from solvent A in that they contain no polyalkylene glycol groups. It is surprising that ethers of this kind act as solution promoters with respect to both the naphthenate and the esterified or etherified polyalkylene glycol and mixtures thereof, and are moveover easily soluble in organic solvents, especially in liquid hydrocarbons and hydrocarbon oils. Among these high boiling ethers there may be used, for example, the following:Di-n-hexyl ether di-nr-octyl ether, di-nnonyl ether, di-2-ethylhexyl ether, dodecyl ethers, for example, a dodecyl octyl ether and especially dodecyl 2-ethyl-hexyl ether, dodecyl phenyl ether, dodecyl cyclohexyl ether, octadecen-( 9)-yl-1-isobutyl ether, octadecyl-Ptetrahydronaphthyl ether, nonyl-4-methylcyclohexyl ether, 4-octylphenyl-2-ethyl-hexyl ether,, tetrahydronaphthyl-methyl phenyl ether and also benzyl ethers or alkyl substituted benzyl ethers of aliphatic or alicyclic alcohols, for example, nonyl benzyl ether, octadecenyl4-methyl-benzyl ether, dibenzyl ether, tetrahydronaphthyl-methyl benzyl ether, and also tetrahydronaphthyl methyl-2-ethylhexyl ether, 784,780 butanediol-( 1: 3)-monooctyl ether, butane diol-( 1: 4)-dibenzyl ether and butane diol( 1:4)-isobutyl dodecyl ether. There can also be used with advantage the ethers of fatty alcohols prepared by the reduction of fatty acids obtained by the oxidation of paraffin wax or the alcohols of forerunnings or oxo or naphthene-alcohols, for example, paraffin wax fatty alkyl cyclohexyl ether, dodecyl fatty alkyl (forerunnings) ether, the alcohols of the forerunnings being a mixture of alcohols obtained by hydrogenating fatty acids from the oxidation of paraffin wax under a high pressure and then distilling the alcohols, the latter being obtained as forerunnings and contain a chain length of 6-9 carbon atoms From naphthenic acids, such as are obtained in the raffination of mineral oils, there can be made by reduction under high pressure or by the

method of Bouveault-Blanc the corresponding naphthenic alcohols, which can easily be converted into ethers which can be used with advantage in the method of the invention As examples thzre may be mentioned, dinaphthenyl ether and also naphthenyl benzyl ether or naphthenyl-2-ethylhexyl ether. Instead of a single ether there may be used a mixture of two or more ethers or a solution of a single ether or a mixture of' thers in a liquid hydrocarbon or hydrocarbon oil. By the use of ethers of the kind described above (solvent B) in accordance with the invention there is obtained an improvement or acceleration in the solubility of metal salts of naphthenic acids in liquid hydrocarbons ot hydrocarbon oils in the presence of solvent A. Whereas, for example, a mixture of a metal naphthenate with a poly alkylene glycol derivative is a wax-like mass at room temperature, there is obtained a clear solution even after the addition of 20 per cent of an ether or mixture of ethers to the mixture of metal naphthenate and polyalkylene glycol derivative The resulting solution can easily be diluted with liquid hydrocarbons. The aforesaid ethers act not only as solution promoters, but they also lower the viscosity of solutions or mixtures in which a polyalkylene glycol derivative and a metal salt of a naphthenic acid are incorporated in a liquid hydrocarbon Furthermore they also act as solvents or dispersing agents for deposits of resins, lacquers or asphalts, when a mixture of a metal naphthenate, solvent A and solvent B is used as an addition to hydrocarbon engine oil. The proportion of solevnt B to be added to the mixture of a metal naphthenate and a polyalkylene glycol derivative may vary within wide limits, for example, up to 200 per cent. and higher The proportions are not dependent only on the nature and quantity of the metal naphthenate or mixtures of metal naphthenates or the polyalkylene glycol derivative added thereto, but also on the improvement desired in the solubility or msicibility of the metal naphthenates in liquid hydrocarbons or hydrocarbon oils and also on the viscosity desired in the solutions. Solutions of metal naphthenates in hydrocarbon oils in the presence of an ether (solvent B) and a polyalkylene glycol derivative can be prepared in various ways Thus, for example, the metal naphthenate may first be dissolved with the aid of heat in the ether (solvent B) or in the polyalkylene glycol derivative (solvent A) and the other of these solvents added to the resulting solution, and the solution so obtained diluted with the liquid hydrocarbon or hydrocarbons The metal naphthenate may first be thoroughly mixed or stirred, preferably after being melted, with the polyalkylene glycol derivative, and the ether added to the resulting mixture and the whole mixture added to the

liquid hydrocarbon or hydrocarbons Furthermore, a solution of the liquid hydrocarbon or hydrocarbons, ether and polyaikylene glycol derivative may first be prepared, and the metal naphthenate then dissolved in the solution. Finally, the metal naphthenate and the polyalkylene glycol derivative (solvent A) may each be dissolved separately in the ether, and the two solutions may then be united The resulting mixture dissolves easily in hydro. carbon oils. EXAMPLE 6 This example shows that by the addition of ethers used in the inevntion clear solutions of 100 metal naphthenates in the polyalkylene glycol derivatives are obtained. Various metal naphthenates having the cations mentioned below are melted with the polyalkylene glycol derivatives described 105 below in the ratio 10: 1 at a temperature of 40-80 C After cooling, there are, obtained wax-like substances These mixtures are mixed with the ethers given below in the ratio 1: 1, and in this manner there is 110 obtained in each case a thinly liquid solution which can be easily incorporated in hydrocarbon oils. z 4 784,780 Polyalkylene glycol Cation derivative Ether Potassium Naphthenic acid heptaethylene ethylhexyl benzyl glycol ester ether Zinc (divalent) Dodecyl pentaethylene glycol lauryl N butyl methyl ether ether Lead Benzyl pentaethylene glycol benzoate dioctyl ether Iron (trivalent) Para-octylphenyl tetraethylene glycol ether dibenzyl ether Aluminium/calcium Stearyl hexaethylene glycol tetradecyl methylbenzoate cyclohexyl ether EXAMPLE 7 Neutral aluminium naphthenate is very sparingly soluble in liquid hydrocarbons, for example, in a light petroleum fraction having a boiling range of 150-270 C and a viscosity of 2 centistokes at 80 C or in a higher boiling mineral oil boiling, for example, at 200-300 C and having a viscosity of 20 centistokes at 80 C A solution of aluminium napthenate in the higher boiling mineral oil produced by stirring for a long time at a raised temperature, for example C, is a thick gel which becomes nonhomogeneous upon cooling and from which a part of the oil used separates out The viscosity of the freshly prepared solution cannot be determined with accuracy, but it is approximately 6000 centistokes at 80 C. Such a gel cannot be used for technical purposes, for which a solution of aluminium naphthenate is desired An addition of 4 per cent of lauryl pentaethyleneglycol ether lowers the viscosity of the aluminium naphthenate solution in the oil from above 6000 to about 160 centistokes at 80 C. It is even more advantageous first to dissolve the aluminium

napbthenate in an ether Viscosity of the mixture at 80 C. + 20 % of dodecyl ethyl-hexyl ether + 40 %,, ,,,,, , + 60 %,,,,,,,, + 80 %, 3,, , + 100 % ',,,,,, , The solutions so obtained are easily miscible with hydrocarbon oils. EXAMPLE 10 A solution of 50 per cent strength of barium naphthenate in a liquid hydrocarbon, for 'example, of the type of spindle oil, could not be prepared hitherto or could be prepared only with very great difficulty, and could not be used for technical purposes It is relatively easy to prepare a solution of the same (solvent B) By dissolving 10 parts of aluminium naphthenate in 100 parts of dodecyl2-ethyl-hexyl ether there is obtained a solution haivng a viscosity of 1890 centi-stokes at C The viscosity is then lowered to 99 centi-stokes by the incorporation of 4 per cent of lauryl pentaethyleneglycol ether The resulting solution is easily miscible in all proportions with liquid hydrocarbons and thinly liquid solutions are always obtained. EXAMPLE 8 A solution of 50 per cent strength of calcium naphthenate in dodecyl octyl ether has a viscosity of 18 60 centi-stokes at 80 C, which is lowered by the addition of 10 per cent of dodecyl pentaethyleneglycol ether of 11.4 centi-stokes The solution so obtained is easily miscible with hydrocarbon oils. EXAMPLE 9 The following table shows the effect on the viscosity of a mixture of 60 parts of barium naphthenate and 30 parts of lauryl pentaethyleneglycol ether obtained by adding varying proportions of lauryl ethyl-hexyl ether. 122 0 centi-stokes 38.1,, 18.5,, 12.5,,,, 9.2,, 7.2, concentration of the naphthenate in lauryl ethyl-hexyl ether, and the solution has a viscosity of 2335 centi-stokes at 80 C By the addition of the polyethylene glycol derivatives named below the viscosity of the solution is very considerably reduced This reduction in viscosity is dependent on the degree of polymerisation of the polyalkylene glycol derivatives used, as will be seen from the following results:% of lauryl triethylene glycol ether= 11 80 centistokes at 80 C. % of lauryl pentaethylene glycol ether= 11 94,,,,, %' of lauryl heptaethylene glycol ether= 13 38 p,,, S 784,780 When the viscosity-lowering substance lauryl hexaethyleneglycol ether is further etherified with ethyl-hexanol to form lauryl hexaethyleneglycol ethyl-hexyl ethere, the viscosity i is lowered within the same limits and gives for an addition of 20 per cent a viscosity of 13.64 centistokes. The above solutions are easily miscible with hydrocarbon oils -EXAMPLE

11 This example illustrates the capacity of various polyalklylene glycol derivatives for lowering the viscosity of a solution of 50 per cent strength of barium naphthenate in lauryl ethyl-hexyl ether The initial solution has a viscosity of 3255 centistokes at 80 C The following 2 olyalkylene glycol derivatives when used in a proportion amounting to 20 per cent yield solutions having the following viscosities:Benzyl pentaethylene glycol ether 10 4 centistokes at 80 C. Octyl-phenol octaethylene glycol ether 15 5,,, ,, Stearic acid heptaethylene glycol ester 140,,,, ,, The solutions so obtained are easily miscible with hydrocarbon oils. The joint use of polyglycol derivatives (solvent A) and high boiling ethers (solvent B) in addition to metal naphtlhenates has been found to be especially effective in improving hydrocarbon engine lubricating oils In applying the invention for this purpose it is especially advantageous first to prepare a mixture of the metal naphthenate with the polyglycol ether or ester (solvent A) and the high boiling ether (solvent B), and to add the resulting mixture to the hydrocarbon oil, advantageously with the aid of heat These additions are suitable for all kinds of internal combust''on engines Even under severe conditions they retain their cleansing action on the engine. The new additions to hydrocarbon engine lubricating oils also act well in the case of cold engines, that is to say, at low oil temperatures of, for example, 40-50 C. The proportions in which the additionsa should be incorporated in hydrocarbon engine lubricating oils depends on various factors. These include the quality of the hydrocarbon engine lubricating oil, the period for which the engine is run without changing the oil, and the sulphur content of the fuel. The content of the added substances in the oil should be greater the poorer the quality of the engine oil,; the longer the period for which the engine is to be run without chang-' ing the oil, and the higher the sulphur content of the fuel. In general the proportion of the mixture of metal naphthenate, solvent A and solvent B added to the engine oil is advantageously within the range of 1 to 15 per cent on the weight of the oil Hlowever, smaller or higher proportions may be added. The substances, or mixtures or solutions ot substances, to be added to the engine oil, may be incorporated in the oil simukltaneously or in any desired order of succession. A good homogeneous distribution of the added substances, namely a mixture of a metal naphthenate with solvent A and solvent B, in hydrocarbon engine lubricating oils is obtained by incorporating these mixtures at temperatures of-about 40-60 C or higher.

For example, even temperatures up to 150 C may be used In many cases a homogeneous mixture is obtained even at lower temperatures. To the new additions for engine oils or to the mineral oil solutions made there-with there may also be added agents improving the pour point or viscosity and also age-protecting agents or oxidation inhibitors, for exampe, alkyl substituted phenols or cresolhn, compounds which contain divalent sulphur and also secondary aromatic amines, phenthiazines, phosphoric acid esters or thiophosphoric acid esters, or salts of thiophenols. The favourable action of these new additions for engine oils is illustrated by the following examples:EXAMPLE 12 The following mixture is prepared:parts of lauryl ethyl-hexyl ether, parts of a pentaethyleneglycol ether of a fatty alcohol, which has been obtained by hyd 95 rogenating under high pressure a fatty acid obtained by the oxidation of paraffin wax, and which has a hydroxyl number of 6 6, 49 parts of barium naphthmnate, parts of para-ethyllexyl-phenol 100 parts of the above mixture were added to parts of a paraffin base oil having the following characteristics: Specific graivty at 30 ' C = O 885 Ignition point = 225 C 105 Viscosity at 500 C = 65 8 centi-stokes. The above oil blend was tested as engine oil in a diesel engine under the following severe conditions of test:Oil temperature 160 C 110 Duration of test 120 hours working under full lead. There was used a Middle East diesel fuel which had a sulphur content of 1 per cent. At the end of the test all piston rings were 115 freely movable, the oil wiping rings had no deposits of sludge or coke thereon and both the outsides and insides of the pistons had a preponderantly metallic appearance. W 7 hen the used oil was tested for its lubri 120 cating property in an Almen-Wieland machine it gave /l-values (coe ficient of friction) rang: -g 784,780 ing between 0 2 and 0 1 at a load capacity of 28 plates ( 1400 kgs). EXAMPLE 13 rhe following mixture was tested: 65 parts of lauryl ethyl-hexyl ether, parts of lauryl-pentaethyleneglycol ether, 36 parts of barium naphthenate, parts of ethylhexyl-phenol A paraffin base oil as described in Example 13 was mixed with 10 parts of the above mixture and the mixture was tested as an engine oil in the engine of a travelling motor vehicle. The distance travelled was 6000 kilometres without changing the oil and merely making up the oil consumed. At the end of the test journey the piston rings and the oil wiping rings were freely movable and no deposits of coke or sludge had formed in the grooves carrying the rings The walls of the pistons and the

interiors thereof had an entirely lustrous metallic appearance. Tests on the lubricating property of the used oil in the Almen-Wieldand machine gave Ax-values between O 1 and 0 2 at a plate number of 20 '( 1000 kg). EXAMPLE 14 The following mixture in the form of a 10 per cent addition to upper cylinder lubricating oil was tested in a 2-stroke diesel engine:-parts of barium naphthenate, parts of calcium naphthenate, parts of naphthenic alcohol hexaethyleneglycol ether, parts of dioctyl ether, parts of di-tertiary-butyl-paracresol. As the upper cylinder lubricating oil there was used a paraffin base oil such as is described in Example 13. After a test period of 10 hours at 4500 revolutions per minute and a water temperature of 95 C, the piston rings were freely movable, and the pistons had a metallic appearance both inside and outside.

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* GB784781 (A)

Description: GB784781 (A) ? 1957-10-16

Manufacture of water-insoluble azo-dyestuffs

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PATENT SPECIFICATION 784781 Date of Application and filing Complete Specification: Dec 3, 1953. ' i' No 33695153. Ski /1 Application made in Germany on Dec 3, 1952. Complete Specification Published: Oct 16, 1957. Index at acceptance:-Classes 2 ( 4), P 1 (A 4 B: F 4), P 2 G 2 A, P 2 H( 3: 9:10:12:13), P( 2 J: 4 K), P 9 A 3 C 1, P 9 A 4 (B: C); and 15 ( 2), B 2 (A 2: C 1 D 2 C). International Classification:-C 09 b D 06 p. COMPLETE SPECIFICATION Manufacture of Water-Insoluble Azo-Dyestuffs We, FARBWERKE HOECHST AKTIENGESELLSCHAFT vormals Meister Lucius & Br Uning, a body corporate recognised under German law, of Frankfurt(M)-Hdchst, Germany, 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: According to this invention new, valuable, water-insoluble azo-dyestuffs are made by coupling in substance or on the fibre a diazocompound of an amino-azo-compound of the following general formula: 0 4 al/yl //_ v i,,=,v-e A-eo-,w-R t Co 0 A//kyl #2 z 1< dop in which R represents an aromatic, hydroaromatic, araliphatic or heterocyclic radical and R, represents a methyl or phenyl group, with an arylide of acetoacetic acid or terephthaloyl-bis-acetic acid, the dyestuff components being free from groups imparting solubility in water to the finished dyestuifs, such as sulphonic acid or carboxylic acid groups The azo-dyestuffs so obtained correspond to, the following general formula: in which N represents one of the numbers 1 or 2, R represents an aromatic, hydroaromatic, araliphatic or heterocyclic radical, R, represents a methyl or phenyl group, and R 2 represents the radical of an arylide of acetoacetic acid or terephthaloyl-bis-acetic acid the dyestuff components being free from groups imparting solubility in water to the finished dyestuffs, such as sulphonic acid and carboxylic acid groups. The new dyestuffs yield mainly clear red tints, and are of particular importance for use in print style for the following reason The 40 diazo-components of the present invention can produce on the so-called yellow naphthols of commerce (which term defines coupling components which either contain acylacetyl-aminogroups or are derived from pyrazolone), clear 45 yellowish-red to bluish red tints which have hitherto been unlmown in practice on the basis of an arylide of a /-ketocarboxylic acid, as compared with yellow tints produced by the

use of known diazo-components on yellow 50 naphthols. It is to be understood that no claim is made herein to the products of reacting a diazocomponent of the present invention with a yellow naphthol derived from pyrazolone 55 In a great number of cases, the new dyestuffs possess good properties of wet fastness and good fastness to light Therefore they constitute a valuable advance of the class of icecolours 60 The aminoazo-compounds used as diazocomponents can be obtained, for example, by coupling a diazotised 1-amino-2: 5-di-alkoxy4-nitrobenzene with an acylacetic acid anmide of the following formula 65 R 1-CO-CH,-CO-NH-R, in which R represents an aromatic, hydroaromatic, araliphatic or heterocyclic radical and R, represents a methyl or phenyl group, and subsequently reducing the nitro group to 70 the amino group. The following Examples illustrate the inver;iion, the parts being by weight, unless otherwise stated, and the relation between part by weight and part by volume being the 75 same as that between the kilogram and the litre: EXAM Pi LE 1. 38.6 parts of -( 41-amino-21: 5-dimnethoxybenzen:-1 '-azo) acetoacetic adi& 3-mthoxy 80 anilide of the following formula 1 cc 0 &A, Y/ 1 R, 784,781 oe HH 0 1 ce a C/I (obtainable by coupling diazotised 1-amino2:5-dimethoxy-4-nitro-benzene with acetoacetic acid-3-methoxy-anilide and subsequently reducing the nitro group to the amino group) are kneaded with 35 parts of hydrochloric acid of 35 per cent strength and 35 parts of water, the hydrochloride of the amina compound being formed 1000 parts of water are then run in, while stirring, and the mixture is diazotised at room temperature by adding dropwise, in the course of about 10 minutes, 17 5 parts of a sodium nitrite solution of 40 per cent strength The mixture is then stirred further for a few minrutes The diazo-solution is clarified by filtering with suction and the filtrate is run, while stirring, into a suspension of acetoacetyl-aminobenzene, which is prepared as follows:17 7 parts of acetoacetylaminobenzene are stirred with 250 parts of water, 15 parts of a sodium hydroxide solution of 38 B 6 and 5 parts of Turkey Red oil until dissolution is complete The anilide is thnl precipitated again, while stirring, by adding dropwise an acetic acid of 30 per cent strength, until a neutral reaction is attained. The excess of mineral acid in the coupling mixture is then neutralised by adding dropwise 230 parts of a sodium acetate solttion of per cent strength The whole is stirred until the diazonium-salt can no longer be detected The precipitate is then filtered with suction and washed well with water A red pigment dyestuff of good fastness to light is obtained. EXAMPLE 2.

Cotton fabric is padded on the foulard with a solution containing per litre 20 grams of 1acetoacetylamino 2:5 dimethoxy-4-chlorobenzene, 20 cc of a sodium hydroxide solution of 38 Be and 15 grams of Mononol Brilliant Oil The fabric is dried and printed with a paste containing in 1000 grams 50 grams of a dyeing salt consisting of the diazonium chloride of -( 4-amnino-2: 5 '-dimethoxybenzene- 11-azo)-acetoacetic acid anilide having a content of the base of 25 per cent, 480 grams cf water, 450 grams of starch-tragacanth thickening and 20 grams of acetic acid of 50 per cent strength After drying, the material is passed through a boiling bath containing per litre 10 grams of anhydrous sodium carbonate, rinsed and after-treated at the boil for some minutes with a solution containing 3 grams of soap and 2 grams of sodium carbonate per litre of liquor An intense scarlet red print of very good fastness to light and good properties of wet fastness is obtained. A bluish red tint of the same good fastness properties is obtained when the printing is applied to cotton fabric which has been padded with a corresponding amount of 1acetoacetylamino-3-ethoxybenzene or of acetoacetyl-arminobenzene. The above printing process can also be applied to fabrics of other kinds, for example staple fibres of regenerated cellulose or viscose. EXAMPLE 3 70 Cotton yarn which has been well boiled and dried is treated for about half an hour at a ratio of goods to liquor of 1:20 in a solution containing per litre 1 gram of terephthaloylbis-acetic acid-2-methoxy-4-chloro-5-methyl 75 anilide, 7 5 cc of a sodium hydroxide solution of 38 Be and 10 cc of Turkey red oil After being squeezed, the impregnated material is introduced into a developing bath which has been prepared as follows: 1 5 parts of the 80 hydrochloride of -( 4 '-amino-21: 51-diethoxybenzene-l'-azo)-acetoacetic acid anilide are added, while stirring, to a mixture of 150 parts of water and 1 5 parts of hydrochloric acid of 20 per cent strength The mixture is 85 diazotised, by adding dropwise 1 3 parts of a sodium nitrite solution of 20 per cent strength. The excess of mineral acid is then neutralised by the addition of 5 parts of a sodium acetate solution of 10 per cent strength, 5 parts of 90 acetic acid of 30 per cent strength are then added and the solution of the diazonium salt is made up to 1000 parts by volume. The: dyeing is developed for 20-30 minutes, rinsed and after-treated at the boil 95 for half an hour with a solution containing per litre 3 grams of soap and 2 grams of sodium carbonate A clear yellowish-red dyeing of medium fastness to light and good properties of wet fastness is obtained 100 When the same diazo-compound is coupled on cotton yam

which has been impregnated with a solution containing per litre 4 grams of 4:4 ' di(acetoacetylamino) 3: 31 dimethyldiphenyl, 3 cc of a sodium hydroxide solution 105 of 38 Be and 10 cc of Turkey red oil, a kluish-red dyeing is obtained. By using other diazotised aminoazo-compounds of the above constitution and other arylides of ( 8-keto-carboxylic acids in the usual 110 dyeing or printing processes, dyestuffs having similar good properties of fastness are obtained. In the following Table are given the tints obtained after subjecting the material to an 115 after-treatment with a boiling solution of soap ard sodium carbonate The samz tints are obtained when the dyestuffs are produced in substance as opposed to on the fibre. Diazo, Component: K, 4 ' amino-21: 51dimethoxybenzene-l'-azo) -acetoacetic acid 1) -anilide 4) 3 784,781 Coupling Component: 1-acetoacetylamino-4ethoxybenzene 1-acetoacetylamino2: 5-dimethylbenzene terephthaloyl-bis-acetic acid-2-methoxyw-4chloro-5-methylanilide 4: 41-di-(acctoacetylamino)-3: 31-dimethyldiphenyl 11) 5 12) -4-methoxy-anilide terephthaloyl-bis-acetic acid-2-methoxy-4chloro-5-methylanilide 1-acetoacetylamino2: 5-dimethoxy-4chlorobenzene 4: 41-di-(acetoacetylamino)-3: 3 ' -dimethyldiphenyl yellow-red bluish-red brick-red bluish-red clear blue-red yellowish-red yellow-red bluish-red 13) 14) 15) -2: 3-dimethyl-anilide -2: 5-dimethyl-anilide -2: 5-dimethyl-anilide 16) 3 17) -3-trifluoromethylanilide dimethoxybenzene-1 'azo)-acetoacetic acid 18) -2-trfifuoromethyl4-chlaranilide 1-acetoacetylamino2: 5-dimnethoxy-4-chlorobenzene tereplhthaloyl-bis-aceticacid-2-methoxy-4chloro-5-m-ethyl-anilide 4: 41-di(acetoacetylamino)-3: 31-dimethyldiphenyl 4: 4 '-di-(acetoacetylamino)-3: 3 '-dimethyldiphenyl Tint: bluish-red scarlet bright red bluish-red 10) red yellowish-red orange clear red yellow-red brick-red Diazo Component: 19) -cyclohexylamide 784,781 Coupling Component: 4: 4 '-di-(acetoacetylaminy)-3: 31-dimethyldiphenyl 20) -naphthyl-2-amide,, 21) -6-methoxy-benz thiazole-2-amide 22) -N-ethylcarbazolyl,, 3-amide 23) -benzimidazole-5,, amide o.-( 41-amino-2 ': 51dimethoxybenzene- 11-azo) -benzoylacetic acid 24) -anilide,, -( 41-amino-21: 51diethoxy-benzene- 11-azo) -acetoacetic acid 25) -3-methyl-anilide 26) -benzylamide,, 27) -2-methoxy-anilide 28) -4-chloranilide x.-( 41-amino-21: 51diethoxy-benzene-1 '-azo) -benzoylacetic acid 29) -anilide terephthaloyl-bis-acetic acid-2-methoxy-4chloro-5-methylanilide bright scarlet

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* GB784782 (A)

Description: GB784782 (A) ? 1957-10-16

Improvements in or relating to processes for the production of seleniumrectifiers

Description of GB784782 (A)

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CH324326 (A) NL101501 (C) CH324873 (A) CH324326 (A) NL101501 (C) CH324873 (A) less Translate this text into Tooltip

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PATENT SPECIFICATION 7 $ 49782 Date of Application and filing Complete Specification: February 10 1954. t, t D Application made in Germany on February 10 1953 Complete Specification Published: October 16, 1957 Index at acceptance:-Class 37, I((AE:2). International Classification:-H Oll. COMPLETE SPECIFICATION

Improvements in or relating to Processes for the Production of Selenium Rectifiers We, SIEMENS-SCHUCKERTWERKE AKTIENGESELLSCHAFT, of Berlin and Erlangen. Germany, a German 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 a process for the production of selenium rectifiers Processes for the production of such rectifiers are known in which an addition is made to the semi-conductor (composed of selenium) for increasing the conductivity of the semiconductor, and hence of the finished rectifier. The addition for increasing the conductivity of the semi-conductor consists of a halogen, or halogens, or halogen compound(s) and will hereinafter be referred to as " the first addition " It is also known to make an addition for promoting the formation of the barrier layer In this specification the " barrier layer " is to be understood as that which produces the blocking resistance in the rectifier Thus, an addition which promotes the formation of the barrier layer is an addition which increases the blocking resistance of the finished rectifier, the blocking resistance of the rectifier being the resistance offered to the current resulting from an inverse voltage applied to the rectifier Known additions for promoting the formation of the barrier layer are, for example, metals such as antimony, bismuth, -35 tin, thallium, indium, gallium, cadmium, copper and lead, or non metals such as arsenic or sulphur or alloys or compounds of these substances The addition for promoting the barrier layer will hereinafter be -40 referred to as " the second addition " In known processes for the production of selenium rectifiers, the second addition in the form of thallium is applied with the counter electrode to the surface of the semiconductor, the thallium entering the semiI Price 3 s 6 d J conductor by diffusion This has the drawback that it is difficult to regulate the quantity and distribution of the diffused addition in the semi-conductor. According to the present invention there 50 is provided a process for the production of a selenium rectifier, wherein the semiconductor body is built up of a plurality of individually successively applied selenium layers, each of which layers is provided with 55 the first addition as herein defined, there being added to one layer in which the barrier layer is formed in the finished rectifier (and, in the case where the semi-conductor body is to consist of more than two layers, 60 also to the successive layers adjacent to said layer, with the exception of one or more of the last layers) the second addition as herein defined, the quantity of the second addition, in the case

where the semi-conductor body 65 is to consist of more than two layers, being made progressively greater in the layers approaching the barrier layer. As already stated, each of the layers contains the first addition for increasing con 70 ductivity It will of course be appreciated that different halogens or different mixtures thereof may be used in various layers As the first addition there is preferably employed chlorine, iodine, or bromine, 75 either in the elementary state or as halogen compounds, for example selenium chloride, selenium bromide, selenium tetrachloride or selenium tetrabromide The first addition, which serves to increase conductivity, will 80 have its effect modified by the presence of the second addition The latter, which primarily serves to promote the formation of the barrier layer, will also tend to reduce conductivity 85 For this reason therefore the semiconductor body is built up of a plurality of individually applied successive selenium layers, each of which may be prepared with a given quantity of the first addition, there 90 No 3963/54 2 784,782 being added to some of the layers neighbouring the barrier layer, the second addition in such a quantity that as a result of the combined action of the first addition and the second addition the final conductivity of each layer provided with both additions is less than a layer having only the first addition In this way the barrier effect of the rectifier is enhanced. J 0 Alternatively, the quantity of the first addition in the layer(s) provided with both the first and second additions may be made larger than that provided in the layers or layer having only the first addition, so that the conductivity of the layers having both additions is about the same as that of the layers having only the first addition A rectifier having a relatively low forward resistance is thus obtained. The present process may be carried out with, for example, a metallic carrier electrode which has been plated with another metal and which has been suitably preheated or otherwise prepared to ensure good adhesion of a subsequently applied selenium layer so that an electric junction without a barrier layer is formed between the carrier electrode and the semi-conductor body A first selenium layer containing the first addition is applied to the carrier electrode, the addition being, for example, chlorine, this layer being applied, for example, by evaporation, painting, pressure, pouring or in another known way A further selenium layer is then applied to the first mentioned selenium layer in one of the known ways, the further selenium layer containing the first addition again for example chlorine, and the second addition for example thallium The second selenium layer can be applied to the first selenium layer while the

first layer is still in the amorphous condition. Alternatively, the first layer may, prior to the application of the second layer, be subjected to a thermal pre-treatment by which it is converted entirely or partially into the better conducting or into the best conducting modification If desired, a final layer can be applied The layer may consist in known manner of cadmium selenide, cadmium sulphide or selenium dioxide The counter electrode consisting of the usual known materials, for example bismuth, tin or cadmium in elementary form or in the form of an alloy thereof, is then applied to the semiconductor layer or the final layer, for example by spraying or evaporation, if desired after the second layer has undergone thermal treatment, and the rectifier in this W O state is then thermally and/or electrically formed in the usual known manner until it reaches the finished state. For a better understanding of the invention and to show how the same may be carried into effect, reference will now bo 65 made to the accompanying drawing which shows diagrammatically a selenium rectifier. Referring now to the drawing, a rectifier is shown in which 1 is a carrier electrode, 2 a and 2 b are two layers of the semi 70 conductor body and 3 is the counter electrode of the rectifier The two layers 2 a and 2 b each consist of selenium with the first addition, the layer 2 b also having the second addition The counter electrode 3 is then 75 applied, this electrode being free from agents such as thallium which promote the building up of the barrier layer Such an agent, which is otherwise present in the counter electrode. thus cannot produce any disadvantageous 80 undesirable effect on the rectifier during operation which may result in ageing The usual thermal and electrical treatments may be employed in the present process in a manner which is well known 85

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