* GB784843 (A)

Description: GB784843 (A) ? 1957-10-16

New basic phthalocyanine dyestuffs and a process for their production

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PATENT SPECIFICATION 784,843 Date of Application and filing Complete Specification: Dec 21, 1954. No 36945154. Application made in Germany on Dec 21, 1953. Application made in Germany on June 14, 1954. Complete Specification Published: Oct 16, 1957. Index at acceptance:-Class 2 ( 4), DIT. International Classification:-C 09 b. COMPLETE SPECIFICATION New Basic Phthalocyanine Dyestuffs and a process for their Production We, FARBENFABRIKEN BAYER AKTIENGESELLSCHAFT, of Leverkusen Bayerwerk, Germany, a body corporate organised under the laws of 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 b paeformedi, to be particularly described in and by the following statement: This invention relates to new basic phthalocyanine dyestuffs and to a process of making the same. The present invention provides new basic phthalocyanine dyestuffs having from one to four radicals of the general formula R /3 -N _R 2 3 R 2 R 4 attached to a phthalocyanine radical, wherein R, is a hydrogen atom or an allkyl radical, R, is an acyclic bivalent radical, and R 3

and R, are aliphatic radicals or together with the D X + HN R -X 2 ' R/3 D N R 2 X + HN wherein D is a phthalocyanine radical, R 1 is hydrogen or an alkyl radical, R 2 is an acyclic bivalent radical, R, and R 4 are aliphatic radicals or together with the adjacent nitrogen atom form a heterocyclic ring, and X is a halogen atom If R 1 is an acyclic bivalent radical carrying a halogen atom, a product is obtained in which there are two acyclic biadjacent nitrogen atom form a heterocyclic ring. The present invention also provides a process for the production of these new basic dyestuffs, which comprises reacting a phthalo 25 cyanine dyestuff containing one to four replaceable halogen atoms with a tertiary amine of the general formula R /3 H -N-R -N 2 R 1 R wherein R 1 to R 4 have the aforementioned meanings. The phthalocyanine dyestuff containing one to four replaceable halogen atoms can alternatively be reacted with an aliphatic primary or secondary amine containing at least one halogen atom, the halogen compound obtained in this reaction being subsequently reacted with a secondary amine The reaction underlying this process in accordance with the invention can be illustrated by the following equation: D N R 2 X + HX 21 R 1 / R 3 D N R 2 N R 1 R + HX R 3 valent radicals carrying -N< radicals. R, According to the invention, also, in the dyestuff produced R, can be an acyclic bivalent R a radical which contains an -N< radical. R 4 d Instead of using phthalocyanine dyestuffs it is possible to usg dyestuff intermiz diates containing a replaceable halogen atom, which upon completion of the above reactions are converted into the final phthalocyanine dyestuff. Examples of dyestuff derivatives containing replaceable halogen which are suitable as starting materials for the processes of the invention are phthalocyanine dyestuffs containing a carboxylic acid halide, or a sulphonic acid halide group, or a halogenoalkyl group, such as an w-chloromethyl group. Examples of suitable aliphatic tertiary amines containing primary or secondary amino groups are 1-amino 2 dimethyl-aminoethane, 1-amino-3-dimethylamino-propane, 1diethylamino 3 amino-n-pentane and the amide of methylaminoacetic acid and 1-diethylamino-4-amino-n-pentane. Examples of suitable aliphatic primary or secondary amines containing halogen atoms are (,-chloro-ethylamine, Jf,y-dibromopropylamine, 1-amino-4-chlorobutane, and 3 88 'odichloro-diethylamine. Among the secondary amines which can be reacted with the halogen atom to form the tertiary amine grouping are all common secondary amines, as for example dimethylamine, diethylamine, diethanolamine, piperidine, pyrrolidine and pyrroline.

An excess of the crgandc base employed in the reaction, or an inert organic solvent, such as benzene or acetone, can be used as a reaction medium It is often of advantage to carry out the reaction in an aqueous suspension. The hydrogen halide set free in the reaction can be bound by using an excess of the base or by adding another acid binding agent to the reaction mixture, such as an alkali metal carbonate, sodium hydroxide or sodium, bicarbonate. If the reaction is carried out in an aqueous suspension it may be of advantage to add a catalytic amount of pyridine The reaction then proceeds more quickly. Temperatures of 0-100 C have proved to be advantageous for obtaining the best results. The invention can be carried out by mixing the halogen-containing dyestuff, for example copper phthalocyanine-( 3)-di and tri-sulphochloride, with the amine, as for example 1amino-2-dimethylaminoethane, while stirring. Examples of suitable reaction media are water, an inert organic solvent or an excess of the organic base Preferably the reaction mixture is stirred for some hours at room temperature while the basic phthalocyanine dyestuff formed is precipitating To complete the reaction the mixture can be heated for a short time to 60 C The basic dyestuff formed can be recovered from the reaction mixture by filtration. Some of the basic phthalocyanine dyestuffs obtainable by the process of this invention are soluble in organic solvents, such as ethyl alcohol, benzyl alcohol, esters, aromatic hydrocarbons and dimethyl formamide, and can be used for dyeing plastics and varnishes or in 70 offset printing. The high affinity of the new basic phthalocyanine dyestuffs to fibres derived from various raw materials makes these dyestuffs, especially in form of their water-soluble salts, extremely 75 suitable for dyeing cotton, wool, cellulose, regenerated cellulose, fibres of polyamides or polyacrylonitrile, paper, or paper raw materials such as paper pulp The basic phthalocyanine dyestuffs take on these materials very easily 80 from a dilute acid solution and the resulting dyeings show extremely good wet fastness. It is very surprising that phthalocyanine dyestuffs will become readily soluble in dilute acids such as acetic acid if at least one tertiary 85 amino group is introduced into the molecule. The following Examples, in which all parts are by weight, further illustrate the invention. EXAMPLE 1: To a solution of 10 parts of copper phthalo 90 cyanine in 100 parts of

chlorosulphonic acid, 21 parts of thionyl chloride are slowly added at a temperature of 60-70 C The reaction mixture is then heated for 4-5 hours to 112113 C until a sample is soluble in a 10 % 95 solution of pyridine and is insoluble in aqueous diethylamine The reaction mixture is ccoled and pour-e on to ice The precipitated copper phthalocyanine-( 3)-di and tri-sulphochloride is filtered off with suction and washed 100 with ice water until it gives a neutral reaction. The paste of the sulphochloride thus obtained is added to a solution of 10 72 parts of 1-amino-2-dimethylaminoethane in 38 5 parts of water, stirred for 12 hours at room tern 105 perature and then for one hour at 60 C The basic dyestuff formed is filtered off and washed with hot water It dissolves in dilute acetic acid to give a clear greenish-blue solution 110 By using the nickel phthalocyanine instead of the copper phthalocyanine a dyestuff is formed which is soluble in dilute acetic acid to give a more greenish-blue solution (To obtain the sulphochloride of the nickel phthalo 115 cyanine the reaction mixture has to be heated for 5 hours to 117-118 C). Instead of the 1-amino-2-dimethylaminoethane there may be used equimolecular amounts of 1-amino-3-dimethylamino-propane, 120 1-diethylamino 4 amino-n-pentane, or the amide of methylaminoacetic acid and 1-diethylamino 4 amino-n-pentane The basic dyestuffs obtained are soluble in dilute acetic acid to give a clear greenish-blue solution 125 EXAMPLE 2: To a solution of 9 96 parts of the sodium salt of copper phthalocyanine 4,4 disulphonic acid (obtained by the reaction of two mols of phthalic acid anhydride and two mols 130 784,843 solves in dilute acetic acid to give a bluishgreen solution. EXAMPLE 5: To a solution of 10 parts of 4,41,411,4111tetraphenyl-copper phthalocyanine in 100 parts of chlorosulphonic acid 5 5 parts of thionyl chloride are added drop by drop at 20-25 C while stirring Stirring is continued for 12 hours at room temperature The reaction mixture is cooled and poured on to ice. The precipitated sulphochloride is separated by suction and washed with ice water until it gives a neutral reaction The paste obtained is added to 21 8 parts of 1-diethylamino-4amino-n-pentane and stirred for 12 hours at room temperature and thereafter for one hour at 60 C The basic dyestuff obtained in good yield is filtered off and washed with water It dissolves in dilute acetic acid to give a clear green solution. of the sodium salt of 4-sulphophthalic acid in a urea melt) in 100 parts of chlorosulphonic acid, 6 2 parts of thionyl chloride are added drop by drop at a temperature of 60-70 C.

while stirring -Stirring is continued at a temperature of 75-80 C until a sample is insoluble in aqueous diethylamnine Then the reaction mixture is cooled and poured on to ice The precipitated sulphochloride is filtered off and washed until it gives a neutral reaction. It is added to a solution of 7 84 parts of 1amino-3-dimethylamino-propane in 8 parts of water while stirring By following the procedure of Example 1 a clear reddish-blue basic dyestuff is obtained which is readily soluble in dilute acetic acid. A similar dyestuff may be obtained by using 1-amino-2-dimethylaminoethane as the basic compound. EXAMPLE 3: To a solution of 10 parts of the sodium salt of 3,3 ' diaza copper phthalocyanine 4,4 'disulphonic acid (obtained by the reaction of two mols of pyridine-2,3-dicarboxylic acid and two mols of the sodium salt of 4-sulphophthalic acid in a urea melt) in 150 parts of chlorosulphonic acid, 12 4 parts of thionyl chloride are added drop by drop at a temperature of 60-70 C while stirring Stirring is continued for 8 hours at 75-80 C until a sample is insoluble in aqueous diethylamine. After cooling, the reaction mixture is poured on to a mixture of ice and sodium chloride solution The precipitated sulphochloride is sucked off, mixed with ice-cold sodium chloride solution and neutralized with sodium hydroxide solution Thereafter 32 parts of 1diethylamino 4 amino-n-pentane are added. By following the procedure of Example 1 a reddish-blue basic dyestuff is obtained which is readily soluble in dilute acetic acid. EXAMPLE 4: To a solution of 14 3 parts of the sodium salt of 4,41-diphenyl-copper phthalocyanine41 l,4 '1-disulphonic acid (obtained by the reaction of two mols of diphenyl-3,4-dicarboxylic acid and two mols of the sodium salt of 4sulphophthalic acid in a urea melt) in 100 parts of chlorosulphonic acid, 24 9 parts of thionyl chloride are added drop by drop at a temperature of 60-70 C while stirring. Stirring is continued for about 20 minutes at C until a sample is insoluble in aqueous diethylamine The reaction mixture is cooled, poured on to ice and the precipitated sulphochloride is filtered off with suction and washed with ice water until it gives a neutral reaction. The paste obtained is added to a mixture of 19 parts of water, 7 6 parts of sodium bicarbonate and 9 5 parts of 1-amino-3-dimethylamino-propane and stirred for 12 hours at room temperature and for half an hour at C The precipitated basic dyestuff is filtered off and washed with hot water It is obtained in nearly quantitative yield and disEXAMPLE 6:

To a solution of 30 4 parts of the sodium salt of cobalt phthalocyanine-4,41,4 ",4 l"tetrasulphonic acid in 300 parts of chlorosulphonic acid, 90 3 parts of thionyl chloride 90 are added drop by drop at a temperature of 60-70 C while stirring Stirring is continued for 10 hours at 80-90 C until a sample is insoluble in aqueous diethylamine After cooling, the reaction mixture is poured on to a 95 mixture of ice and sodium chloride solution. The precipitated sulphochloride is then filtered off with suction and washed with ice water until the filtrate shows a neutral reaction The neutral paste is added to a mixture of 38 parts 100 of water, 15 2 parts of sodium bicarbonate and 19 parts of 1-amino-3-dimethylamino-propane, stirred for 12 hours at room temperature and for half an hour at 80 C Upon addition of a small amount of sodium chloride solution the 105 dyestuff is separated by suction and washed with water It dissolves in dilute acetic acid to give a greenish-blue solution. A similar dyestuff can be obtained when an equivalent amount of 1-diethylamino-4-amino 110 n-pentane is used instead of the above 1amino-3-dimethylamino-propane. EXAMPLE 7: Parts of a copper phthalocyanine, which contains 3 or 4 chloromethyl groups, are dis 115 solved in a mixture of 20 parts of 1-diethylamino-4-amino-n-pentane and 20 parts of water, and heated for about 15 hours to 90 C Upon addition of water the precipitated dyestuff is filtered off and washed with water 120 It is dissolved in 1 5 litres of 3 % acetic acid, filtered in the presence of active carbon, and recovered from the solution by the addition of sodium hydroxide solution and filtration It is soluble in dilute acetic acid to give 125 a clear greenish-blue solution. EXAMPLE 8: 11.9 Parts of a copper phthalocyanine obtained from diphenylsulphone-3,4-dicarboxylic-acid-31-sulphonic acid are dissolved in 130 784,843 56 parts of chlorosulphonic acid and reacted with 3 04 parts of thionyl chloride while stirring for 2 hours at 80 C To obtain the sulphochloride the reaction mixture is cooled and poured on to ice The precipitate is separated by suction and washed with ice water until the filtrate shows a neutral reaction The paste of the sulphochloride is mixed with a small amount of 1-amino-2-dimethylaminoethane Upon stirring for 10-12 hours at room temperature the excess of 1-amino-2dimethylamino-ethane is removed by steam distillation and the precipitated basic dyestuff filtered off and washed with hot water It is obtained in good yield as a clear turquoise dyestuff which is readily soluble in acetic acid. EXAMPLE 9:

5.87 Parts of 4,41,411,4111, 5,51,51,511-octaphenyl copper phthalocyanine are dissolved in 58 7 parts of chlorosulphonic acid and 7 15 parts of thionyl chloride and stirred for 1012 hours at room temperature The sulphochloride is obtained as in the preceding example by pouring the reaction mixture on to ice, filtering off and washing. The paste of the sulphochloride is mixed with a small amount of ice water and reacted with 10 5 parts of 1-amino-2-dimethylaminoethane as described in Example 8. A basic dyestuff of a clear green colour, which is readily soluble in dilute acetic acid, is obtained in good yield. EXAMPLE 10: Parts of a paste of copper phthalocyanine-( 3)-di and tri (,3-chloroethyl)-sulphonamide containing about 25 % of the dyestuff are added to 40 parts of a 50 % solution of dimethylamine Upon addition of 6 parts of a 15 % solution of sodium hydroxide the reaction mixture is stirred for 20 hours at room temperature The reaction product formed is precipitated by heating for a short while and by addition of a solution of sodium acetate It is filtered off with suction and washed The dyestuff is obtained in nearly quantitative yield and is soluble in dilute acetic acid to give a clear blue solution. By using a solution of diethylamine in the above example the corresponding diethylamine derivative is obtained The copper phthalocyanine-( 3)-di and tri(BP-chloroethyl)-sulphonamide can be obtained by the following procedure: 14.6 Parts of the copper phthalocyanine-( 3)di and tri-sulphochloride are suspended in 80 parts of water at 5-10 C To this suspension 7 parts of '-chloroethylamine hydrochloride dissolved in 10 parts of water are added while stirring Stirring is continued for 4 hours while 39 parts of a 10 % solution of sodium hydroxide are added and the temperature gradually rises to 18 C Thereafter stirring is continued for 20 hours at room temperature. The reaction product obtained in a quantitative yield is filtered off and washed. EXAMPLE 11: Parts of a paste of copper phthalocyanine-( 3)-di and tri (-chloroethyl)-sulphonamide containing 25 % of the dyestuff are dissolved in 45 parts of a 50 % solution of 1-amino 3 dimethylamino-propane Upon addition of 6 parts of a 15 % solution of sodium hydroxide the reaction mixture is stirred for 20 hours at room temperature. Thereafter a sodium salt solution is added and the dyestuff precipitated by adding hydrochloric acid until the solution becomes neutral.

It is soluble in dilute acetic acid to give a clear blue solution. EXAMPLE 12: 80 Parts of a paste of copper phthalocyanine-( 3)-di and tri-(li,y-dibromopropyl)sulphonamide containing 25 % of the dyestuff are dissolved in 40 parts of an approximately % solution of dimethylamine Then 9 parts 85 of a 15 % solution of sodium hydroxide are added and the reaction mixture is stirred for hours at room temperature Thereafter the excess of dimethylamine is removed by steam distillation and the dyestuff precipitated by 90 adding sodium chloride solution (and eventually some hydrochloric acid) The reaction product obtained in excellent yield is readily soluble in acetic acid to give a clear blue solution 95 The above mentioned copper phthalocyanine-( 3)-di and tri-(,7 dibromopropyl)sulphonamide can be obtained as follows: 14.6 Parts of copper phthalocyanine-( 3)-di and tri-sulphochloride are suspended in 50 100 parts of water at 5-10 C To this suspension 19 parts of 2,3-dibromopropylamine hydrobromide dissolved in 50 parts of water are added while stirring Within 4 hours 4 2 parts of a 10 % solution of sodium hydroxide are 105 added while the temperature rises to 15 C. The reaction mixture is then stirred for another 20 hours The reaction product obtained in an excellent yield is separated by suction and washed 110 EXAMPLE 13: Parts of a paste of 4,4 ',4 '1,4111-tetra-(pf 8-chloroethyl sulphonamide phenyl)-copper phthalocyanine containing 25 % of the dyestuff are dissolved in 50 parts of an approxi 115 mately 50 % solution of dimethylamine and stirred for 20 hours at room temperature. During this time one part of sodium hydroxide dissolved in a small amount of water is added. Thereafter the excess of dimethylamine is 120 removed, and the dyestuff precipitated by adding sodium acetate solution It is separated by suction and washed The basic dyestuff obtained in nearly quantitative yield is soluble in dilute acetic acid to give a clear green 125 solution. The 4,4141,41411 tetra (p-,-chloroethylsulphonamide-phenyl)-copper phthalocyanine can be obtained as follows: 14,5 Parts of 4,414,41,41-copper phthalo 130 784,843 784,843 cyanine-tetra-(p phenyl sulphochloride) are suspended in 80 parts of a mixture of ice and ice water and reacted with 7 parts of P-chloroethylamine hydrochloride dissolved in 10 parts of water at a temperature of 0-5 C The mixture is stirred for one and a half hours at the same temperature while 4 2 parts of a % solution of sodium hydroxide are added. Stirring is then continued at a temperature of 20 C until the reaction

is finished The dyestuff is separated by suction and washed with water The yield is quantitative. Following the procedure of the above example a clear blue basic dyestuff can be obtained from 4,41,4 '1,4 '11-copper phthalocyanine tetra (p-chloroethyl)-sulphonamide (obtained from 4,41,4 x,4111-copper phthalocyanine-tetrasulphochloride and 13-chloroethylamine). EXAMPLE 14: Parts of copper phthalocyanine-( 3)-diand tri-(/-chloroethyl)-sulphonamide are dissolved in 25 parts of diethanolamine and 20 parts of pyridine Upon addition of one part of sodium hydroxide dissolved in 6 parts of water the reaction mixture is stirred for 20 hours at room temperature and then for 2 hours at 80-90 C The basic dyestuff is precipitated by the addition of sodium chloride solution It is obtained in good yield and dissolves in acetic acid to give a clear blue solution.

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* GB784844 (A)

Description: GB784844 (A) ? 1957-10-16

Dyeing process

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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 SPECIFICATION 784,844 4 ' Date of Application and filing Complete Specification Dec 21, 1954. No 36946/54. Application made in Germany on Dec 21, 1953. Complete Specification Published Oct 16, 1957. Index at acceptance: -Class 15 ( 2), B 2 G, BZ 2 L( 1: 2: 5 D). International Classification: -D 06 p. COMPLETE SPECIFICATION Dyeing Process We, FARBENFABRIKEN BAYER AKTIENGESELLSCHAFT, of Leverkusen-Bayerwerk, Germany a body corporate organised under the laws of 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:- This invention relates to dyeings which have good to excellent wet fastness and to a process of producing the same. In accordance with the present invention fibres or fibrous materials are dyed in a slightly acid solution of a water-insoluble basic phthalocyanine dyestuff having from one to four radicals of the general formula R 3 / -N-R-N I \ R 1 R, attached to a phthalocyanine radical, wherein R, is a hydrogen atom or an alkyl radical, R 2 is an acyclic bivalent radical, and R, and R, are aliphatic radicals. The water-insoluble basic phthalocyanine dyestuffs and their production are described and claimed in our co-pending Application No 36945/54 (Serial No 784,843). Examples of fibres or fibrous materials which can be dyed by the process of the present invention are those derived from raw materials such as cotton, wool, regenerated cellulose, polyamides, polyacryls, paper and paper raw materials such as sulphite cellulose, soda cellulose, straw cellulose or wood pulp. In carrying out the process of the invention, the fibres or fibrous materials are dyed in a dilute acid solution of the above water-insoluble basic phthalocyanine dyestuffs Examples of slightly acid solutions which can be used are solutions of the phthalocyanine dyestuffs in aqueous acetic acid and formic acid, which can be prepared, for example, by mixing the waterinsoluble dyestuff with water to form a suspension or paste, and adding such an amount of acid as will give an aqueous solution of the dyestuff The dyeing process is not restricted lPrice 3 s 6 d l to the use of a specific temperature range but can be carried out at any temperature customarily employed in dyeing using an aqueous bath In general, the basic phthalocyanine dyestuff is completely extracted from the the dye bath, leaving a

water-clear solution. The dyeings produced by the process of the invention have good to excellent wet fastness. It is noteworthy that this wet fastness is obtained without any after-treatment. The process of the invention is further illustrated by the following examples. EXAMPLE 1. 1 gram of the blue copper phthalocyanine dyestuff produced as described in Example 3 of our co-pending Application No 36945/54 60 (Serial No 784,843) is mixed with a small amount of water to form a paste The dyestuff is dissolved by adding 1 millilitre of acetic acid and water is added until 100 milllitres of a dyestuff solution are obtained In this solu 65 tion 100 grams of polyacrylonitrile fibres are dyed while the temperature of the dye bath is slowly raised to the temperature of boiling water Care is taken that the dye bath always has a slight excess of acetic acid After 20 70 minutes the dyeing process is complete, and the dyeings are washed and dried The dyeings obtained are a clear blue colour and have excellent wet and light fastness. EXAMPLE 2. mililitres of a dyestuff solution are obtained from 1 gram of the green copper phthalocyanine produced as described in Example 4 of our co-pending Application No. 36945/54 (Serial No 784,843) by following the procedure of Example 3 of that application 100 grams of cotton are dyed in this solution while the temperature of the dye bath is slowly raised After about 10 minutes the dyeing process is complete and the dye bath contains scarcely any dyestuff The resulting clear bluish-green dyeings are washed and dried as usual; they possess excellent wet and light fastness. 2 784,344 EXAMPLE 3. grams of the green dyestuff which is produced as described in Example 5 of our co-pending Application No 36945/54 (Serial No 784,843) are dissolved as described in Example 7 of that application With the dyestuff solution thus obtained 1 kilogram of wood pulp is dyed in a beater or a blending vat. The pulp is sized with a phenol resin, dried in the usual manner, and pressed at 180-200 C and a pressure of 100 atmospheres to form a plate Since the dyestuff takes very readily on the wood pulp and has good light fastness it is specially suited for the manufacture of coloured hard fibre boards The waste water is nearly water-clear.

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* GB784845 (A)

Description: GB784845 (A) ? 1957-10-16

Improvements relating to liquid atomisers

Description of GB784845 (A)

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PATENT SPECIFICATION p 784,84 e 5 Date of Application and filing Complete Specification: Oct 10, 1955. No 28824/55. Complete Specification Published: Oct 16, 1957. Index at Acceptance:-Class 69 ( 3), I( 1: 5). International Classification:-BO 5. COMPLETE SPECIFICATION Improvements relating to Liquid Atomisers I, REGINALD PERCY FRASER, O B E a British Subject, of Tir-na-N'og, Kingston Hill, Surrey, 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:- This invention relates to liquid atomisers having spray nozzles both of the swirl-spray pressure type (in which the energy for atomisation of the liquid is derived from pressure on the liquid and swirling formations within the nozzle structure), and of the twin-fluid or blast type (in which a gaseous fluid under medium or high pressure is also utilised to take part in the atomisation of the liquid) Efficient atomisers of the last mentioned kind are already known and in use comprising a tubular casing within which is mounted a liquid supply member the front end piece of which constitutes a liquid swirl-spray pressure nozzle for forming an open cone of spray, the exit orifice of the said nozzle being surrounded laterally by a forwardly dished or cupped formation, whilst an annular stream of converging air or other gas or steam for atomisation of the liquid is supplied through the casing alongside or around the liquid supply member and issues through an annular passage provided between the rim of the said dished or cupped formation and the front end of the said casing so that the said annular gaseous stream strikes the open cone of liquid after it has formed Examples of atomisers of this kind may be seen in my Patent Specifications Nos 536,224, and 664,676 (Figure 4) Such atomisers may be referred to as vortex cup-type atomisers. The problem of atomisation of liquids by the use of atomisers becomes increasingly difficult with increase of discharge or output of the liquid from the nozzle, and the chief object of the present invention is to provide, in atomisers of the two kinds referred to, improvements both in performance and in construction when dealing with large volumes of liquid; lPrice 3 s 6 d l X Lj G O The present invention consists in providing a liquid atomiser of each of the types above referred to with a stationary hollow cylindrical or outwardly conical or flared tubular passage extending axially forward from the central 50 liquid exit orifice of the spray nozzle, and with tangential passages at or near the base of the said passage for enabling a gaseous stream such as air or steam under pressure to become whirled and issue as a gaseous liner to the said 55 passage, the inner diameter or smallest inner diameter of which is greater than the diameter of the liquid exit orifice In this way a substantially cylindrical vortex of the gaseous stream is created within the tubular passage, 60 and the liquid film leaving the nozzle is accelerated and rotated. A subsidiary feature of novelty consists in giving to the annular exit passage of atomisers of the aforesaid vortex cup-type, a shape which, 65 in section, is convergent-divergent Alternatively this annular exit

formation may be regarded geometrically as a two-dimensional convergent-divergent nozzle rotated about an axis to generate the improved annular exit 70 The supply pressure of the gaseous stream may be greater than fourteen pounds per square inch and the said annular exit passage may be designed for controlled gaseous expansion within it such as to create supersonic velocity 75 in the stream. Atomisers of the twin-fluid kind referred to, when of large size, necessarily have a large facial area exposed to radiation of heat from combustion chambers into which they may 80 project So long as the liquid and the atomising gaseous stream are flowing through the atomiser they are sufficient to cool the atomiser face, but when the supply is cut off the face of the atomiser may become excessively hot from the 85 heat in the chamber A further subsidiary feature, therefore, of the present invention consists in providing for positive cooling of the front plate or head of the atomiser. The invention will now be described more 90 fully with reference to the accompanying drawing which illustrates in longitudinal section one embodiment of a large capacity atomiser constructed according to the invention. The body or casing of the atomiser consists of a base or rear part 1 and a cylindrical open ended front or cap part 2, these parts being held together by bolts 3 Through the base 1 of the casing extends axially a liquid supply pipe 4 the front end of which carries a liquid swirl spray nozzle constituted by the hollow ported atomising member 5, and the overlying nozzle piece 6 in the centre of which is the central exit orifice 7. The atomising member 5 is formed with a depression 16 on its face and with slots 15 leading tangentially into the said depression which therefore acts as a swirl chamber. Liquid fed under pressure along the supply pipe 4 enters the chamber 13 constituted by the interior of the member 5 and thence outwardly through its ports into the annular space 14 existing between the said member 5 and the nozzle piece 6, then back through the tangential slots 15 into the swirl chamber 16, and thence forwardly through the orifice 7 of the nozzle piece. In the particular construction shown the nozzle piece 6 is formed with a flange 8 which is clamped between opposing flanges 9 on the parts 1 and 2 of the casing. Fitting over the face of the nozzle piece 6 is a plate 10, the front surface of which is inwardly dished or cupped as shown at 21 to constitute a vortex cup formnation, and the periphery of which is symmetrically disposed adjacent to but spaced from the rim 11 of the cap 2 so as to constitute an outer nozzle having the annular exit passage 12.

A gaseous stream such as air or steam is supplied through a pipe 17 to the interior of the base 1 of the casing and passes forwardly along the inside la of the casing through holes 18 in flange 8 and past whirl-imparting vanes 19 to the annular exit passage 12 of the outer nozzle. As already stated the present invention consists in providing a hollow cylindrical or outwardly conical or flared tubular passage extending axially forward with respect to the central liquid exit orifice 7 of the swirl-spray nozzle This tubular passage is seen at 20 and in the particular construction shown it is constituted by the interior of a hollow forward projection from the vortex cupped or dished face 21 of the plate 10 Its inner diameter may be as much as, say, ten times the diameter of the liquid exit orifice 7 The rear face of the said plate 10 is formed with tangential slots 22 which at their outer ends are open to the interior la of the casing, thereby enabling some of the air or steam inside the casing to pass along the said slots and into the tubular passage 20 at the base thereof The said tubular passage can extend forwardly as far as or even beyond the transverse plane containing the edge of the forwardly dished or cupped formation 21 and the mouth of the annular exit passage 12. Consequently, the conical liquid film advancing from the central liquid exit orifice 7 is ac 70 celerated and rotated by the high velocity gaseous vortex advancing along the internal surface of the passage 20 so that as soon as the mixture reaches the mouth of the said tubular passage it expands radially outwards as a sub 75 stantially disc-like sheet and strikes the converging annular stream of air or steam issuing from the annular exit passage 12. The front plate 10 is shown as being hollow, this being so as to enable a cooling fluid to be 80 circulated within its annular cavity for cooling purposes as already ei:plainzd. One of the feed pipes for the cooling fluid is seen at 24, its front end being secured to and leading through the rear wall of the said hollow 85 plate 10. The above described tubular passage 20 may be provided with a detachable tubular liner 25, as shown, for ready inter-changeability when desired The rear rim of the said liner 25 may 90 reach to or slightly overlap the mouths of the tangential slots 22, as shown, this constituting one way of enabling the effective exit area of the said slots to be changed at will by interchanging the gasket or shim 26 for one of 95 different thickness. A feature of the construction illustrated, which is the particular subject of a separate Patent Application No 7738 of 1957 (Serial No. 784846) divided from this Application, resides 100 in the fact that the spaced walls of the annular exit passage 12 are not parallel but

are convergent at 12 ' and then divergent, and the length of the passage in the direction of travel of the air or steam is appreciable so that the 105 air or steam can undergo appreciable increase in velocity (above sonic) The width of the exit passage 12 is determined by the correct choice of a flat washer or shim 23 at the base of the cap 2 of the casing 110

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* GB784846 (A)

Description: GB784846 (A) ? 1957-10-16

Improvements relating to liquid atomisers

Description of GB784846 (A)

PATENT SPECIFICATION 78 42 S-4 6; Date of application and filing Complete Specification: Oct 10, 1955. No 7738157. (Divided out of No 784,845) ,,' Complete Specification Published: Oct16, 1957. Index at acceptance:-Class 69 ( 3), I( 1:5). International Classification:-1 805. COMPLETE SPECIFICATION Improvements relating to Liquid Atomisers I, REGINALD PERCY FRASER, a British Subject, of Tir-na-N'og, Kingston Hill, Surrey, 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:- This invention relates to liquid atomisers and has particular reference to liquid atomisers comprising a tubular casing within which

is axially mounted a liquid supply member the front end of which constitutes a spray nozzle having an end face or cap portion extending laterally around the nozzle orifice to near to the front end of the casing or to a terminal cap thereon, to form an annular passage for the exit of an annular converging stream of air or other gas or steam supplied through the interior of the casing. Examples of atomisers of this kind may be seen in my Patent Specifications Nos. 536,224 and 664,676 (Fig 4), and in my Patent Specification No 28,824 of 1955 (Serial No 784,485) from which the present application is derived as a Divisional Application therefrom. According to the present invention the aforesaid annular exit passage has a shape which, in section, is convergent-divergent If desired the degree of divergence of the stream of air or other gas or steam may be such as to enable supersonic velocity to be attained by the stream. The invention will now be described more fully with reference to the accompanying which illustrates the invention embodied in the improved atomiser described and claimed in my parent Patent Specification No 28,824 of 1955 (Serial No 784,845). The body or casing of the atomiser consists of a base or rear part 1 and a cylindrical open ended front or cap part 2, these parts being held together by bolts 3 Through the base 1 of the casing extends axially a liquid supply pipe 4 the front end of which carnies a liquid swirl-spray nozzle constilPrice 3 s 6 d l tuted by the hollow ported atomising member 5, and the overlying nozzle piece 6 in the centre of which is the central exit orifice 7 so The atomising member 5 is formed with a depression 16 on its face and with slots 15 leading tangentially into the depression -which therefore acts as a swirl chamber. Liquid fed under pressure along the 55 supply pipe 4 enters the chamber 13 constituted by the interior of the member 5 and thence outwardly through its ports into the annular space 14 existing between the said member 5 and the nozzle piece 6, then back 60 through the tangential slots 15 on the member 5 into the swirl chamber 16, and thence forwardly through the orifice 7 of the nozzle piece. Fitting over the face of the nozzle piece 6 65 is a plate 10, the front surface of which is inwardly dished or cupped as shown at 21 to constitute a vortex cup formation, and the periphery of which is symmetrically disposed adjacent to but spaced from the rim 11 of 70 the cap 2 so as to constitute the annular exit passage 12. A gaseous stream such as air or steam is supplied through a pipe 17 to the interior of the base 1 of the casing and passes forwardly 75 along the inside la of the casing through holes 18 in flange 8 and past whirl-imparting vanes 19 to the annular exit passage 12.

According to the present invention the spaced walls of the annular exit passage 12 80 are not parallel but are convergent at 121 and then divergent, and the length of the passage in the direction of travel of the air or steam is appreciable so that the air or steam can undergo appreciable increase in 85 velocity The width of the exit passage 12 is determined by the correct choice of a flat washer or shim 23 at the base of the cap portion 2 of the casing. As the front end of the atomiser, if of 90 large size and exposed to radiation by heat from a combustion chamber into which it may project, may become excessively hot unless cooled I may provide means for keeping the said front end cool In the construction shown the front plate 10 is shown as being hollow, this being so as to enable a cooling fluid to be circulated within its annular cavity for cooling purposes One of the feed pipes for the cooling fluid is seen at 24, its front end being secured to and leading through the rear wall of the said hollow plate. Although the invention has been specifically described as embodied in the improved atomiser described and claimed in my parent Patent Specification, as aforesaid, it is to be understood that it is not limited to use in that particular construction but is also applicable to other constructions of atomisers of the kind specified, as for example, the atomisers of my Patents Nos 536,224 and 664,676 (Fig 4). In my present application I make no claim

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* GB784847 (A)

Description: GB784847 (A) ? 1957-10-16

Improvements in or relating to fused electrical plugs, sockets and adaptors

Description of GB784847 (A)

PATENT SPECIFICATION Inventor: RONALD FREDERICK LOEBL 7 4,847 Date of application and filing Complete Specification: Feb 7, 1956. 1 Nolk)3785/56. Complete Specification Published: Oct 16, 1957. Index at acceptance: -Class 38 ( 1), E 3 (A 4 A: A 15: B 4 A: D 2: D 5: D 8), E 24. International Classification:-HO 2 f. COMPLETE SPECIFICATION Improvements in or relating to Fused Electrical Plugs, Sockets and Adaptors We, LOBLITE LIMITED, a Body Corporate organised under the laws of Great Britain, of Third Avenue, Team Valley, Gatesheadon-Tyne 11, 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 electrical plugs and adaptors of the kind which incorporate a fuse in one or more of the terminal connections, the fuse being retained removably in the plug or adaptor by a removable contact pin. It is the object of the present invention to provide an improved construction wherein the fuse is releasably held in a housing provided in the plug or adaptor. According to the present invention we provide an electrical plug or adaptor comprising a body of insulating material, a housing in said body to receive a cartridge fuse, a contact member secured in one end of the housing, a contact pin removably threaded into the other end of the housing, and a cartridge fuse in the housing in electrical connection with said contact elements. By way of example one or both of the contact elements may include, or have mounted thereon, a compression spring adapted to seat between the contact element and an end of the cartridge fuse. In order that the nature of the invention may be readily understood, an embodiment of adaptor in accordance therewith is hereinafter particularly described with reference to the accompanying drawing which is a vertical section. In this drawing, the adaptor consists of a two-part housing 1, 2 secured together by any suitable means (not shown) The contact elements consist of the common arrangement of an earth pin and two supply pins arranged in roughly triangular formation. The earthing circuit consists of a socket 3 to receive the usual earthing pin of a three-pin plug inserted into the adaptor This socket is threaded into a boss 4 in the housing and makes contact with an

earthing pin 5 projecting beneath One of the current-carry 50 ing elements is constituted by a socket 6 to receive a pin of the inserted plug, this socket being integral with a contact element 7 secured in the top end of a fuse holder recess 8 The lower end of the recess 8 has 55 screw-threading 9 receiving a threaded contact pin 10 having at its upper end a seating 11 in which is held a spring 12 serving to contact the lower end of a cartridge fuse 13. The other of the two current-carrying ele 60 ments could be either a simple straightthrough connection, similar to the earthing pin as described, or a replica of the fused circuit described In this drawing it would appear directly in line behind the assembly 65 6-13 and has not been shown. With such a construction, the insertion and replacement of the cartridge fuse 13 only entails unscrewing of the pin 10 from its position at the end of the recess 8, whereafter 70 the fuse 13 will readily drop out The spring 12 ensures a firm and continuous contact of the fuse on the contact elements The contact pin 10 need only be finger-tight and thus no tools are required and the housing 1, 2 75 need not be taken apart when a blown fuse is to be changed.

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