* GB785613 (A)

Description: GB785613 (A) ? 1957-10-30

New diazoamino-compounds and process for making them

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PATENT SPECIFICATION 785,613 w pi Date of Application and filing Complete Specification: Aug 27, 1954. a r k R No 25021/54. Application made in Switzerland on Aug 28, 1953. Application made in Switzerland on July 5, 1954. Complete Specification Published: Oct 30, 1957. Index at acceptance:-Classes 2 ( 3), C 114, C 1 C( 3: 4: 5: 8: 10: 11 J), C 2 D( 2: 6); and 15 ( 2), B 2 A 2, B 2 C 1 D 2 A, B 2 C 2 (D 1 A: DIB: H: K), B 2 C 7 C. International Classification:-CO 7 c D 06 p. COMPLETE SPECIFICATION New Diazoamino-Compounds and process for making them We, CIBA LIMITED, a body corporate organised according to the laws of Switzerland, of Basle, Switzerland, 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 provides valuable new diazoamino-compounds which, like the compound of the constitution ( 1) /=V g O A correspond to the general formula X # //OOC ( 2) \ A'W-y H X R-NH, H which is free from groups imparting solubility in water and of which the p A-ivalue

differs by at most 0 7 from the value c (x;z), where the latter value is one of the following c (X=H;Z=V) = 48, c (X=H;Z=w) = 42, c (x=u;z=v) = 4 0, c (x=u;z=w) = 35, C (X=Cl;Z=V) = 36, c (X=C 1;Z=W) = 29. The invention also provides a process for making the above new diazoamino-compounds wherein a 1-aminobenzene-2-carboxylic acid4-sulphonic acid of the formula mooc AI O OC z C 53 ( 3) in which R represents a benzene residue, X and H are each in ortho-position relatively to the -N = N group, X represents a methyl, methoxy or ethoxy group (U) or a hydrogen or chlorine atom, and Z represents a methyl or benzyl group (V) or a straight chain alkyl residue (W) containing 2 to 4 carbon atoms and bound to the nitrogen atom by an end carbon atom, and in which formula the residue X R-N = NH is the residue of an amine of the constitution in which Z has the meaning given above, is 40 condensed wih a diazo-compound of an amine free from groups imparting solubility in water and having the formula ( 4) X R-NH, H in which R and X have the meanings given above, and X and H are each in ortho-position relatively to the -NH, group, and wherein the starting materials are so chosen that the p KA-value of the latter amine and the value c (x;z) fulfil the above requirements. s 5 lPric Q -rb 1 4 S 64 The 1-aminobenzene-2-carboxylic acid -4sulphonic acids of the formula ( 3) contain a secondary amino group, of which the nitrogen atom is bound either to a methyl or benzyl group (Z =V) or to an end carbon atom of a straight chain, that is to say, unbranched, alkyl group having 2 4 carbon atoms (Z=W) In the latter case Z is therefore an ethyl, n-propyl or n-butyl group As examples of such compounds there may be mentioned: (Z =V): 1 Methylaminobenzene 2 carboxylic acid 4 sulphonic acid, 1 Benzylaminobenzene 2 carboxylic acid 4 sulphonic acid, (Z W): 1 Ethylaminobenzene 2 carboxylic acid 4 sulphonic acid, 1 N Butylaminobenzene 2 carboxylic acid 4 sulphonic acid. The amines of the formula ( 4), of which diazo-compounds are used as starting materials in the present process, are amines of the benzene series They contain no substituents in one of the ortho-positions relatively to the diazotisable amino group and in the other of these ortho-positions they may be unsubstituted or contain a chlorine atom or a methyl, methoxy or ethoxy group The benzene nucleus may contain further substituents which do not impart solubility in water and are present in positions other than an orthoposition relatively to the amino group, for example, halogen atoms such as chlorine, or methyl, ethyl, methoxy or ethoxy groups, trifluoromethyl groups or nitro groups Thus, the amines may be unsubstituted in paraposition relatively to the amino group or may contain in that position a chlorine atom, a methyl, methoxy or acylamino group for example, a

benzoylamino group There come into consideration, for example, the following amines: 1-Amino-3-chlorobenzene, 1-amino-2-methyl-4 chlorob-enzene, 1-amino-2-methyl-5-chlorobenzene, 1-amino-4-methylbenzene, 1-amino-4-methoxybenzene 1-amino-2-methoxy-5-chlorobenzene, 1 amino 2 methoxy 4 chloro-5-methylbenzene, 1 amino 2 methoxy-4 benzoylarnino-5methylbenzene, 1-amino 2:5 dimethoxy-4-benzoylaminobenzene, 1 amino 2:5 diethoxy-4-benzoylaminobenzene, 1-amino-2-chloro-4-methoxybenzene. The 1-aminobenzene-2-carboxylic acid-4sulphonic acids of the formula ( 3) and the diazo-compounds of the amines of the formula ( 4) cannot be chosen at random for combination with one another, but the amine must be so chosen thats its p KA-value is not more than 0 7 higher or lower than the value c (x;z) The value c (x;z) depends on the nature of the substituent in orthoposition relatively to the amino group of the amine (X=H, Cl, CII, OCH, or OCG) and on the nature of the substituent in the amino group of the amino-benzene carboxylic acid sulphonic acid (Z = V or W). In order to determine whether a particular combination of starting materials falls within the invention, the p KA-value of the selected amine must be known, and then it can easily be determined whether this value differs by at most 0 7 from the value c (x:z, given above for the particular substituents X and Z of the chosen combination Thus, for example, the p KA-value of 1-amino-4-methoxybenzene is 5 3, in which case X is a hydrogen atom If this amine is combined with 1-methylaminoor 1-benzylamino-benzene-2-carboxylic acid4-sulphonic acid (Z =V), the value c (x;z) =c x=H;z=v) = 4 8 The latter value differs from 5 3 by less than 0 7, so that this combination falls within the invention If, on the other hand, the same amine is combined with 1-ethylaminobenzene-2-carboxylic acid-4-sulphonic acid (Z=W) the value c (X;Zj = c(x=H z w) = 4 2, which differs from 53 by more than 0 7, so that this combination or the compound obtainable thereby does not fall within the invention. According to recent textbooks the p KIvalue of the amine R-NH is derived from the equilibrium (+) RNH 3 < R-NH + H (+) of which the acidity constant is KA (R-NH) (H) (R-NH 3, the symbols for the components of the equilibrium enclosed within curved brackets repre 105 senting the activities of these components. The p KA-value is defined by the relationship p KA = -log K,. Fuller information with regard to the p K, 110 value and its determination, which may be carried out by an acidimetric, conductometric or calorimetric method, may be obtained, for example, from "Physical Chemistry of Electrolytic Solutions " by H S Harned and B B 115 Owen, Chapter 15/4, 1943 Edition, pages 480 et seq.

785,613 p Kl,&value of a particular base may vary for given substituents X in ortho-position to the amino group of the amine and for given nitrogen-substituents Z in the 1-aminobenzene-2carboxylic acid-4-sulphonic acid. In order to facilitate determination of the permissible deviations of the p KA-values from the basic values for c (x;z) the following Table may be used From this Table direct readings can be obtained of the limits within which the Permissible p K Arrange of the amine -GCH 3 Z X=H X=U-OCG 13 X=Cl -OCH. Z=V 4 1 to 5 5 3 3 to 4 7 2 9 to 4 3 Z=W 3 5 to 4 9 2 8 to 4 2 2 2 to 3 6 The preparation of the diazo-compounds of the amines of the formula ( 4) and the reaction of these amines with the 1-aminobenzene-2carboxylic acid-4-sulphonic acids of the formula ( 3) may be carried out by methods in themselves known The condensation to form the diazoamino-compounds is advantageously carried out in an alkaline medium It has been found that the diazoamino-compounds so obtained cannot be isolated satisfactorily from the reaction mixture by the usual methods It is surprising, however, that these reaction mixtures can be worked up very successfully, if desired after filtering them to remove undissolved impurities, by subjecting the resulting solutions of the diazoamino-compounds to a rapid drying process As a rapid drying process there is to be understood one in which the material to be dried is subjected to a high temperature in the aqueous condition only for a short time, advantageously a period of the order of a few seconds, but it is permissible once the material is dried, to maintain it at a high temperature for a long period Accordingly, there are suitable drying or evaporation methods in which the solution to be evaporated to dryness is continuously exposed in la finely divided state to a powerful source of heat, and advantageously care is taken that the water vapour evolved is continuously and efficiently removed. Especially advantageous for this purpose is spray drying The term " spray drying" is used in its ordinary sense to mean a treatment in which the aqueous solution or suspension to be dried is finely sprayed or atomised and simultaneously exposed to a current of warm air The heat of the current of air is used to evaporate the solvent, especially water In this manner the air-solvent vapour-dry material system undergoes cooling For drying aqueous solutions or suspensions to produce a dry preparation it is generally necessary to maintain the outlet temperature of the said system at at least about 70 C, advantageously between and 1000 C, and for the same reason it is necessary that the inlet temperature of the air should be above 1000 C, advantageously within the range of 130-180 C in order to 65 avoid having to heat uneconomically large amounts of air.

Instead of spray drying, there may be used another rapid drying process, for example, a drying process in which the cold solution or 70 suspension is applied in a thin layer to a hot roller or moving band In this case also it is preferable, on the one hand, by heating to a sufficiently high temperature the moving surface, for example, the roller, and, on the other, 75 by finely distributing the material to be dried, for example, by breaking it up into droplets or by spraying it, to ensure that a thin uniform film of the material to be dried is formed from which the solvent can be completely distilled 80 in a short time After a short time the dry layer is completely removed from the hot surface by means of a knife or other suitable apparatus, the material being removed in any event before fresh solution is applied to the 85 place it occupies. It is surprising that during such rapid drying processes there is at most only a very slight decomposition of the diazo-compound or diazoamino-compound, and even in cases 90 where, owing to an unfavourable equilibrium between the starting materials and the diazoamino-compound being established when the condensation was carried out, a not inconsiderable amount of the temperature-sensitive 95 diazo compound is still present. The new diazoamino-compounds of the formula ( 2) can be worked up in the usual manner together with suitable coupling components (co-called naphthols), for example, 100 acetoacetylamino-compounds, 2-oxynaphthalene-3-carboxylic acid arylides, oxydiphenylene oxide carboxylic acid arylides, oxycarbazole carboxylic acid arylides or oxyanthracene carboxylic acid arylides, to form valuable pre 105 parations and printing pastes, which do not require acid steaming for developing the prints and therefore need no addition serving to pro785,613 duce an acid reaction It will be understood, however, that development may be carried out by acid steaming, in which case only a very short period of acid steaming is usually necessary for complete development. The following Examples illustrate the invention, the parts and percentages being by weight unless otherwise stated, and the relationship of parts by weight to parts by volume being the same as that of the kilogram to the litre: EXAMPLE 1. 17.8 parts of the hydrochloride of 1-amino2-methylh 4-chlorobenzene (p KA = 3 8) are diazotised in the usual manner at 0-7 C in parts of hydrochloric acid of 10 per cent. strength with 6 9 parts of sodium nitrite dissolved in 25 parts of water The volume of the diazo solution should be 150-200 parts by volume At the same time there is prepared a solution of 23 1 parts of 1-methylaminobenzene-2-carboxylic acid-4-sulphonic acid in 200 parts

of water with the addition of a sufficient quantity of a sodium hydroxide solution of 30 per cent strength to maintain the clear solution at a p H value of 7-8 There are then added 2 parts of anhydrous sodium carbonate and 2 parts of sodium bicarbonate, and the whole is cooled to _ 4 C in an ice-sodium chloride bath, and, if necessary, by the addition of ice The diazo solution is run in below the surface while stirring vigorously, and at the same time a sufficient quantity of a sodium hydroxide solution of 30 per cent strength is introduced dropwise to maintain the mixture at a p H value of 9 5 to 10 and to give a final p H value of 10. After the addition of diatomaceous earth, the mixture is filtered to remove a small amount of flocculent material, and the solution is then sprayed in a spray dryer, in which the inlet temperature of the air is between 130 and 1800 C., the outlet temperature is not less than 70 C and does not substantially exceed 1000 C. There is obtained a pale brown very fine powder which dissolves easily in water and has a content of about 50 per cent of the diazoaminocompound. EXAMPLE 2. 10 7 parts of 1-amino-4-methylbenzene (p Kl = 5 0) are diazotised in the usual manner in 75 parts of hydrochloric acid of 10 per cent strength with 6 9 parts of sodium nitrite dissolved in 25 parts of water At the same time there is prepared a solution of 23 1 parts of 1methylaminobenzene-2-carboxylic acid-4-sulphonic acid in the manner described in Example 1 The diazo solution is run in beneath the surface at 00 to -4 C, and at the same time a sufficient quantity of a sodium hydroxide solution of 30 per cent strength is added to maintain the mixture at a p H value of 9 5 to 10 Finally the p H value is adjusted to 10 with a solution of sodium hydroxide, and the mixture is filtered with the aid of diatomaceous earth to remove a small amount of impurities. The clear solution is worked up in a spray dryer as described in Example 1 There is obtained a pale powder having a content of about 45 per cent of the diazoamino-compound and in a yield of approximately 80 per cent of the theoretical yield. By using, instead of 10 7 parts of 1-amino4-methyl-benzene, 12 3 parts of 1-amino-4methoxybenzene (p KA = 5 3) and otherwise proceeding in the same manner, the corresponding diazoamino-compound is obtained in the form of a pale brown powder having a content of about 45 per cent and in the same yield. EXAMPLE 3. 17.1 parts of 1-amino-2-methoxy-4-chloro5-methylbenzene (p K &= 4 1) are diazotised as described in Example 1 and filtered The volume of the diazo-solution should be 150 85 parts by volume At the same time

there is prepared a solution of 23 1 parts of 1methyl-aminobenzene-2-carboxylic acid-4-sulfonic acid in 200 parts of water with a sufficient quantity of a sodium hydroxide solution 90 of 30 per cent strength to give the clear solution a p H value of 7-8 There are then added 2 parts of anhydrous sodium carbonate and 2 parts of sodium bicarbonate, and the mixture is cooled to -3 C The diazo-solution is 95 then run in beneath the surface and at the same time a sufficient quantity of a sodium hydroxide solution of 30 per cent strength is added to maintain the p H value between 9 5 and 10. When the mixing operation is finished, the p H 100 value is adjusted to 10 with a sodium hydroxide solution of 30 per cent strength, a small amount of diatomaceous earth is added, and the mixture is filtered to remove a small amount of impurities The diazoamino-compound is 105 isolated in a spray dryer as described in Example 1 There is obtained a pale beige powder having a content of diazoamino-compound of about 50 per cent and in a yield amounting to about 85 per cent of the theoretical yield 110 EXAMPLE 4. 25.6 parts of 1-amino-2-methoxy-4-benzoylamino-5-methylbenzene are stirred overnight at room temperature in 100 parts by volume of water with 30 parts of hydrochloric acid of 30 115 per cent strength and 2 parts of a solution of per cent strength of the hydrochloride of oleyl-diethyl-ethylenediamine, the mixture is then cooled to 0-5 C and diazotised with 6.9 parts of sodium nitrite in 25 parts of water 120 The filtered diazo-solution is coupled in the manner described in Example 1 with a solution, also prepared as described in that Example, of 23.1 parts of 1-methylamino-benzene-2-carboxylic acid-4-sulphonic acid, the p H value of 125 the reaction mixture being maintained between 8 and 9, and finally adjusted to 9 After filtering the mixture in the presence of a diatomaceous earth, the product is worked up in a spray dryer The diazoamino-compound is obtained 130 785,613 of 30 per cent strength to give a clear solution having a p H value between 7 and 8 2 parts of anhydrous sodium carbonate and 2 parts of sodium hydrogen carbonate are added, and the mixture is cooled to -30 C The diazo-solu 70 tion is run in beneath the surface, while stirring well, and at the same time there is added a sufficient quantity of a sodium hydroxide solution of 30 per cent strength to maintain the p H value of the reaction mixture between 75 and 11 The whole is stirred for a further -t hour at 0-5 C, and is then filtered with the addition of diatomaceous earth to remove a small amount of a flocculent precipitate The clear brown solution is evaporated in a spray 80 dryer as described in Example 1 The diazoamino-compound is obtained in the form of its sodium salt as a brown powder easily soluble in water. By using, instead of 1-ethylaminobenzene-2 85 carboxylic acid-4-sulphonic acid, 30 7 parts of 1-benzylaminobenzene-2-carboxylic

acid-4-sulphonic acid and otherwise proceeding in exactly the same manner, the corresponding diazoamino-compound is obtained in a yield of 80 90 -85 per cent in the form of a pale beige powder of good solubility and having a content of per cent. EXAMPLE 7. In the manner described in Example 6 there 95 is prepared the diazoamino-compound from diazotised 1-amino-2-methyl-5-chlorobenzene (p IK = 3 4) and 1-ethylaminobenzene-2-carboxylic acid-4-sulphonic acid. By using, instead of 1-ethylaminobenzene 100 2-carboxylic acid-4-sulphonic acid, 27 3 parts of l-n-butylaminobenzene-2-carboxylic acid-4sulphonic acid and otherwise proceeding in exactly the same manner, the new diazoaminocompound is obtained in the form of a pale 105 brown powder having a content of 55-60 per cent and an excellent solubility The yield amounts to about 85 per cent of the theoretical yield. EXAMPLE 8 110 19.4 parts of hydrochloride of 1-amino-2chloro-4-methoxybenzene (p KA = 3 5) are diazotised in the usual manner in 45 parts of hydrochloric acid of 10 per cent strength with 6.9 parts of sodium nitrite dissolved in 25 115 parts of water at 3-7 C At the same time there is prepared as described in Example 5 a solution of 24 5 parts of 1-ethylaminobenzene2-carboxylic acid-4-sulphonic acid and the solution is coupled with the diazo-solution at 120 -3 C, the p H value being maintained at 9.5-10 by the addition of a sodium hydroxide solution of 30 per cent strength and at the end of the coupling the p H value is adjusted to 11. l The product is worked up, as described in 125 the preceding Examples, in a spray dryer, after the solution has been filtered with the aid of a small amount of diatomaceous earth The diazoamino-compound is a very slightly yellow l coloured powder having a content of about 50 130 in the form of a pale brown powder which dissolves easily in water and has a content of per cent The yield amounts to -about 75 per cent of the theoretical yield. Instead of 1-amino-2-methoxy-4-benzoylamino-5-methylbenzene, there may be used 27.2 parts of 1-amino-4-benzoylamino-2: 5dimethoxybenzene or 30 0 parts of 1-amino-4benzoylamino-2: 5-diethoxybenzene The p H value of the reaction mixture is then maintained between 9 and 11 by the addition of a somewhat larger quantity of a sodium hydroxide solution of 30 per cent strength, and the p H value is finally adjusted to 11 By evaporating the solution in a spray dryer the corresponding diazoamino-compound is obtained in the form of a pale brown easily soluble powder having a content of 50-60 per cent and in a yield of 75-80 per cent of the theoretical yield.

p IK,-values of the bases. 1-amino-2-methoxy-4-benzoylamino5-methyl benzene = 4 5 1-amino-4-benzoylamino-2: 5dimethoxybenzene = 4 0 1-amino-4-benzoylamino-2: 5diethoxybenzene = 3 9. EXAMPLE 5. 12.75 parts of 1-amino-3-chlorobenzene (p RA = 3 6) are diazotised in the usual manner, the volume of the mixture amounting to 150parts by volume At the same time there is prepared a solution of 24 5 parts of 1-ethylamino-benzene-2-carboxylic acid-4-sulphonic acid in 200 parts of water with a sufficient quantity of a sodium hydroxide solution of 30 per cent strength to give a clear solution having a p H value of 7-8 2 parts of anhydrous sodium carbonate and 2 parts of sodium bicarbonate are added, and the mixture is then cooled to -3 C The whole is then mixed with the diazo solution as described in Example 1, and the solution is worked up in a spray dryer There is obtained a pale powder which dissolves easily in water and has a content of about 50 per cent of the diazoaminocompound The yield amounts to 80-85 per cent of the theoretical yield. By using, instead of 1-ethylaminobenzene2-carboxylic acid-4-sulphonic acid, 27 3 parts of l-n-butylamino-benzene-2-carboxylic acid4-sulphonic acid and proceeding otherwise in exactly the same manner, there is obtained in the same yield a powder having similar properties. EXAMPLE 6. 19.4 parts of the hydrochloride of 1-amino2-methoxy-5-chlorobenzene (pl, = 3 5) are diazotised as described in Example 1 The volume of the filtered diazo-solution should be 150-200 parts by volume At the same time there is prepared a solution of 24 5 parts of 1ethylamino-benzene-2-carboxylic acid-4-sulphonic acid in 300 parts of water with a sufficient quantity of a sodium hydroxide solution 785,613 per cent The yield amounts to 75-80 per cent of the theoretical yield. EXAMPLE 9. In the manner described in Example 1 there is prepared a solution of the diazoamino-compound from 17 8 parts of the hydrochloride of 1-amino-2-methyl-4-chloro-benzene and 23 1 parts of 1-methylaminobenzene-2-carboxylic acid-4-sulphonic acid After being filtered the solution is charged into an externally cooled pressure vessel and maintained therein at a temperature of -2 to O C In order to isolate the diazoamino-compound the following apparatus is used: An externally chromium plated and polished hollow steel roller is horizontally mounted for free rotation It has a connection for superheated steam at a maximum of 6 atmospheres gauge pressure A brass knife is pressed against the roller by means of weights at

approximately the level of its axis At a distance of 20-25 centimetres from the roller surface there is arranged perpendicularly with respect to the centre of the axis a nozzle connected to the pressure vessel, the nozzle being so adjusted that the supply of the solution under 2-5 atmospheres gauge pressure suffices, without the special air supply, to atomise the solution finely and spray it on the roller With a roller 20 centimetres in radius and 20-25 centimetres long and at a speed of rotation of about 6 revolutions per minute, the nozzle and knife are so adjusted that the two planes which they form with the roller axis are at an angle of The residence time on the roller of the material to be dried is then 3-4 seconds, the roller rotating from the nozzle to the knife in the direction of the shorter distance between them The quantity of the solution sprayed is 3-4 litres per hour, and the surface temperature of the roller is 115-140 C (corresponding to 2-5 atmospheres gauge pressure of steam). The finished diazoamino-compound is removed from the roller in the form of a pale brown powder, and must be ground for a short time in order to attain a uniform fine grain size The product so obtained does not differ in its content, yield or properties from the product obtained by spray drying in Example 1. The solutions obtained as described in Examples 2-7 can be worked up in the same manner There are then obtained diazoaminocompounds which do not differ substantially from the products obtained by spray drying. EXAMPLE 10. The diazoamino-compounds described in Examples 1-9 can be worked up into printing preparations in accordance with the following Table: For 100 parts of printing preparation A B C Sodium di-isoDiazoamino-compound from Accor propyl 1 ' ding naphDiazo Stabiliser Con to Ex Parts Coupling thalene Tint Parts component tent ample component sulphonate 71.2 69.1 74.5 1-amino2-methyl4-chlorobenzene 1-amino4-methylbenzene 1-amino2-methoxy-4chloro-5methylbenzene 1-methylamino-2carboxybenzene4-sulphonic acid % % % 27.8 29.9 24.5 2:3-oxynaphthoicacid-21methylanilide Nasalt 3-oxycarbazole-2carboxylic acid-41chloranilide 1-acetoacetylamino2:5-dimethoxy4-chlorobenzene 1.0 1.0 1.0 bluish red redbrown yellow 785,618 TABLE-continued For 100 parts of printing preparation _ Sodium di-isoDiazoamino-compound from Accor propyl ding naphDiazo Stabiliser Con to Ex Parts Coupling thalene Tint Parts component tent ample component sulphonate E 5:-x 10 bu % % % % % % 22.2 2:3-oxynaphthoic acid anilide Na-salt 26.5 2:3-oxynaphthoic acid-2:61dimethylanilide Nasalt 25.7 2:3-oxynaphthoic 30.9 21.8 28.2 methylanilide Na-salt 2:3-oxynaphthoic acid-21ethoxyanilide Na-salt

1-acetylamino-2methoxy4-acetoacetylamino-5chlorobenzene 2:3-oxy naphthoic acid-21ethoxyanilide Na-salt 1.0 1.0 1.0 1.0 1.0 reddish violet yellow orange scarlet yellow red I I With these preparations printing pastes may be prepared as follows: 1 4 a d -amino-benzoylmino-2:5iethoxybenzene E F G H I 76.8 72.5 73.3 68.1 77.2 70.8 1-amino4-benzoyl 4 amino2:5-dimethoxybenzene 1-amino3-chlorobenzene 1-amino2-methyl5-chlorobenzene 1-amino2-methoxy5-chlorobenzene l-amino2-chloro4-methoxybenzene 1-ethylamino-2carboxybenzene4-sulphonic acid 1-benzylamino-2carboxybenzene4-sulphonic acid 1-ethylaminobenzene-2carboxylic acid-4sulphonic acid a 1 1 I l 785,613 blue 1.0 785,613 A B c D E F G H I Printing preparation 80 80 60 70 50 50 80 60 60 Urea 50 30 Glycerine 30 30 Alcohol 30 30 30 50 Thiodiethylene glycol 30 50 50 50 30 30 50 30 Sodium diisopropyl 20 naphthalene sulphonate, 10 % solution Water 260 320 355 310 285 310 280 310 250 Sodium hydroxide 20 20 15 20 15 10 10 10 10 solution of 30 per cent strength Starch-tragacanth 600 500 500 500 550 550 550 500 550 thickening Sodium chlorate 10 10 10 10 10 10 10 10 10 Terpentine oil 10 10 10 10 10 10 10 10 10 1000 1000 1000 1000 1000 1000 1000 1000 1000 A cotton fabric is printed with these printing pastes The printed material is dried at 50600 C, and then steamed under neutral conditions in a Mather-Platt apparatus for 5-8 minutes at 100 C The material is rinsed in the cold, and treated with an enzyme preparation for 10 minutes at 40-50 C in order to remove the starch It is then rinsed in the cold, soaped at the boil for 10 minutes and dried after being again rinsed There are obtained pure strong prints The same strong prints are also obtained by steaming under acid conditions for 2-3 minutes at 100 C instead of under neutral conditions.

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* GB785614 (A)

Description: GB785614 (A) ? 1957-10-30

Numeral storer for calculating, book-keeping or the like machines

Description of GB785614 (A)

PATENT SPECIFICATION Inventor: MARTIN HEBEL 785 c 614 4,' Date of Application and filing Complete Specification Sept25,1954. No 27743/54. Complete Specification Published Oct 30, 1957. Index at Acceptance:-Class 106 ( 1), L. International Classification: -GO 6 c. COMPLETE SPECIFICATION Numeral Storer for Calculating, Book-Keeping or the like Machines We, ELDI-FEINMECIIANIK G M si H, a German company, of Hechendorf am Pilsensee, 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:- The present invention relates to a numeral storer for incorporation in a calculating, bookkeeping or like machine wherein numerals introduced into the machine or arising in the course of arithmetic processes performed by the machine are each presented by a combination of the positions of a number of elements which each have two positions only and are movable through a predetermined distance from a first normal position to a second moved position An example of a machine of this kind is described in the specification of our Application No 7997/53 (Serial No 785,285). In conformity with the mode of operation of such a calculating, book-keeping or like machine, the storer to which the invention relates is of a type (to be referred to hereinafter as such) which includes (a) essentially resilient elements, each corresponding to a numeral or a component factor thereof, and each of which is retainable in a position displaced from the idle or free position to represent a stored numeral or factor; (b) control elements which co-operate respectively with each of the said resilient elements and are operable selectively to retain a displaced resilient element in its displaced position, and (c) coupling members respectively associated with each of the resilient elements and which are operable to take up a position interposed between an associated resilient element and projections on a co-operating feeler rail in such manner that the capability of movement of the feeler rail is determined in dependence on the displacement or non-displacement of the the resilient element.

In a construction of a calculating or bookkeeping machine which is mainly mechanical, lPrice 3 s 6 d l complete storers are mounted side by side in so-called book-keeping lines and, for economy, certain elements extend through the whole series of storers to co-operate with the mechanisms in all the storers in the line These 50 elements are, apart from the driving shafts:1 So-called transmission links which are connectable by means of notches with those swinging plates presenting or comprising the resilient elements which correspond to like 55 numerals or factors in different decimal orders so as to pivot only those swinging plates of that storer with which they are coupled, for the introduction for storing of the numerals; 2 Coupling plates for storer extraction 60 which are each composed of all the coupling members of like decimal order and which are inserted digit place by digit place by a selector shaft to bring the feeler rails into an operative relationship with those of the resilient 65 elements of the swinging plates which correspond to a particular decimal order; 3 Transmission rails which are crossed with respect to the feeler rails and, due to the teeth along one of their edges, can themselves exe 70 cute a movement or be blocked against moves ment depending on the position of the feeler rails, in order thus to transfer an extracted numeral into the actual calculating mechanisms for calculation 75 Even though this possibility of mechanical intergration of parts may appear valuable from the economic point of view it presents limitations particularly with a great number of storers, and there may be cases where the free 80 dom of disposition of the storers offered by a more electrical construction is of advantage. Thus, it is stated as a variation in the abovementioned specification that a cam shaft operating the control elements of a storer may be 85 rotated independently of other storers by a stepping electromagnet and that a separate magnet may be provided for the feeler rails in each storer but beyond 'that, preventing complete freedom of disposition, there must 90 a 785,614 still remain the interconnection of the storers through the three sets of continuous mechanical members listed above. The object of the present invention is a special construction of a storer which can be connected into the transmission system in a more electromagnetic form which renders each storer practically independent spatially. According to the description in the abovementioned specification, it has already been proposed that storing and extracting operations should eccur alternately at each digit place in the course of calculation and the storer shaft and the extraction selector shaft are constructed to operate in 20 steps for a ten digit storer capacity For

example, an operative step of the selector shaft is carried out, a coupling plate is inserted thereby, the numeral stored at the digit place concerned is extracted and transmitted to the actual calculating mechanism, then both shafts make a step simultaneously the selector shaft into the intermediate inoperative position where the coupling plate becomes disengaged, and the storer shaft into the operative position where the decade storer plate composed of the control elements is lifted, whereupon, by the transmission links, the swinging plate is pivoted and then the storer shaft rotated further into the intermediate position to lower the decade storer plate, while the selector shaft, on the other hand, proceeds into the operative position for the next higher place of digits. In contrast to this, a single cam shaft in a storer of the type set forth is provided, according to the present invention, with the two sets of cams for storing and extraction respectively and, on rotation, operates the control elements for storing, and the coupling members for extraction in alternating sequence This offers the advantage of positive action ensured by the form of the cam together with the omission of coupling plates common to several storers and the separate extraction selector shaft The device for connection of the swinging plates to the result rails need not be affected thereby. If the omission of continuous result rails is desired for the purpose of introducing numerals into the storers, the storer may also contain, according to a further feature of the invention, individual driving members for pivoting the swinging plates Usually these members will consist of small electromagnets each of which turn by their armatures, a swinging plate when they are excited by numeral or code factor characteristic circuits. The third set of continuous elements, the transmission rails, may be omitted according to a further feature of the invention, by the raised feeler rails closing contact pairs in electric numeral circuits. Even if the use of the single cam shaft for storing and extraction enlarges the usefulness of the storer for many special purposes, nevertheless the two further features of the indePendently pivotable swinging plates and a contact actuation by the feeler rails provide complete freedom of choice in the positioning of the numeral storers for calculation and printing on a more electrical embodiment of the 70 book-keeping machine. The invention will be particularly described with reference to an example shown in the accompanying drawings in which:Fig 1 shows a side elevation of the storer 75 frame with the arrangement of the common storing and extraction cam shaft of the electromagnet for the feeler rails and of the electromagnets for deflecting the swinging plates. Fig 2 shows a front elevation of the storer 80 with a stepping magnet

intended for rotating the cam shaft. Fig 3 is an enlarged section through the storer to show the decade storer plate and the engagement thereof with one of the storing 85 cams Moreover, Fig 3 shows the lever arms of the swinging plates extending rearwardly for actuation by the armatures of the pivoting magnets. Fig 4 shows an enlarged section through the 90 storer on such a level that the coupling plate with a rearward extension thereof may be seen in engagement with the corresponding extraction cam. A separate detailed representation of the 95 electromagnetic drive for the swinging plates is not shown as this does not represent any problem to one skilled in the art. In Fig 1, 1 is the storer frame in which a cam shaft 4 is journalled at 2 and 3 for rota 100 tion, in the present embodiment cf the invention, by means of a ratchet wheel 5, a pawl 6 and a magnet 7 together constituting a known step by step drive Over a hexagonal length of the cam shaft 4 storer cams 8,, 8 &, 8, 105 8 i,, and extracter cams 9,I 9 are uniformly distributed Their angular position is determined by the hexagonal profile of the shaft, their position lengthwise of the shaft by the distance pieces 10 110 A toothed feeler rail 11, which is actuated by an individual supporting leaf spring 12 and the armature 13, 14 of an electromagnet 15 is provided for transmitting extracted factors If actuation of the storer is not to rely on its 115 position in space, the supporting springs 12 will not be moved by a cam shaft, but by such an electromagnet The teeth 16 of the rail 11 co-operate with the teeth of the coupling plates 40 to indicate the storage position of the 120 teeth of the swinging plates 19 A contact 18 is closed with a complementary contact strip together constituting a contact pair when the feeder rail rises to indicate a stored numeral by an insulating element 17 on the feeler rail 125 acting on the contact strip The interior of the storer may be seen from Figs 3 and 4 Only one swinging plate 19 with the teeth 20, 20,Q is shown in Fig 1 Magnets 21, 22, 23 and the magnet 24 obscured by 23 in Fig 1 130 785,614 act on the rearwardly extending lever arms of the swinging plates in order to turn them The manner of this action is not shown in detail, but the armatures thereof are connected to exert a pull through intermediate springs 32 respectively on the rearwardly extending lever arms 30 ( 1)-30 ( 5) of the four swinging plates in the direction indicated by arrows against the springs 32 so that the teeth 20 of the swinging plates 19 are deflected into the storing position The decade storer plate 33 which provides the control elements and is rotatably mounted at 34 and 35 in holes in the frame 1 has a lever 36 extending rearwardly and on the lever is an inclined track surface 37 against which a chamfered end of the associated

storing cam 8 ( 1)-( 10) strikes so that the decade storer plate at the place of digits concerned is raised to such an extent at the front, by pressing down the respective lever 36, that the teeth 20 of the swinging plate 19 concerned can move past the teeth 39 to be retained in notches 391 in the plate 33 to represent a stored numeral or factor when this plate is lowered again This operation is already described in the above-mentioned specification. A coupling plate 40, which is mounted for lateral displacement axially of the rod 43 fixed in the housing at 41, 42, is now displaced from the position seen in Fig 4 against the force of a leaf spring 44 until it abuts the frame 1 by engagement of a rotating cam 9 ( 1)-( 10) with an abutment 46 of an arm 45 of the coupling plate In this displacement of individal coupling members in the form of tongues of the plate 40 are shifted into alignment with the teeth 16 of the feeler rails and are raised when the latter are raised in order to sense the respective positions of the teeth of the swinging plates 19. The front elevation in Fig 2 gives an approximate indication of the relative proportions and the positions of the feeler rails 11. Similarly, actuation of the contacts 18 may be seen by the magnet 15. The present description shows that by means of the apparatus according to the invention, it is possible to make a numeral storer completely independent as such, so that it may be. disposed at any point.

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* GB785615 (A)

Description: GB785615 (A) ? 1957-10-30

Improvements in or relating to brake linings

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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.

I, ARTHUR SAMY, a British Subject of, 10 Ice House Street, Hong Kong, 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 complete brake linings for brake shoes of the type made of the same material throughout the body of the lining and in which a dry lubricant, such as graphite, is incorporated in the body of the lining to prevent screeching noises and it has for its object a brake lining in which the dry lubricant is incorporated in the body of the lining in an improved manner. According to the present invention, a brake lining of the type set forth is constructed in which a dry lubricant is in granular form and the individual granules formed of graphite or mica are disseminated in the body of the brake lining during the manufacture of the lining, so that a supply of lubricant in a finely powdered form from the separated individual granules is maintained and evenly spread over the friction surface as the lining wears down, the individual granules wearing down to lubricate the friction surfaces at small spaced apart intervals The lubricant is graphite or mica and is not in powdered form or block form but in granular form intermixed in the body of the lining and which can wear down into powdered form. Granular graphite or mica is incorporated in the brake lining material, so that it is evenly disseminated in the body of the lining in order that a predetermined quantity is presented at the wearing surface and sufficient only to prevent high frequency vibration without detrimentally affecting the efficiency of the braking power of the lining. The granular graphite or mica is incor785,615 porated during the manufacture of a moulded or other brake shoe lining and as the lining 45 wears, fresh granules of graphite or mica will be presented to the surface of the lining and gradually wear down so that graphite or mica powder removed from the granules lubricates the friction surfaces in sufficient 50 quantity as required.

It has previously been proposed in Patent Specification No 656,324 to make brake blocks of two or more braking surface elements of different materials and to make 55 cast iron elements of such a brake block of supercarburated cast iron obtained by sintering an intimate mixture of iron, steel or cast iron in powdered state with the calculated amount of finely subdivided graphite 60 Preferably in this case, the graphite is selected of finer subdivision than the metal powder It should, for instance, pass entirely through a 6400 mesh per cm 2 sieve.

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* GB785616 (A)

Description: GB785616 (A) ? 1957-10-30

Improvements in and relating to the production of artificial filaments,threads, andthe like

Description of GB785616 (A)

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PATENT SPECIFICATION Inventor: ERNEST EDWARD TALLIS Date of filing Complete Specification: Jan 2, 1956. Application Date: Jan3, 1955 No 43/55. Complete Specification Published: Oct 30, 1957. 785,616 Index at acceptance:-Class 2 ( 2), B 2 V( 1 C 2 A; 1 C 2 C; 7). International Classification;-D Olf. COMPLETE SPECIFICATION Improvements in and relating to the Production of Artificial Filaments, Threads, and the like We, COURTAULDS LIMITED, a British Company, of 16, St Martin's-le-Grand, in the City of London, England, do hereby declare the invention, for which we pray that a patent may be granted to us, and themethod by which it is to be performed, to be particularly described in and by the following statement: - This invention relates to the production of artificial filaments, threads, fibres and the like, hereinafter referred to as filaments from viscose. In U K Patent Specification No 375,842 there is described a process for the manufacture and production of derivatives of polyhydric alcohols which consists in etherifying or esterifying part of the hydroxyl groups in hydroxyalkyl ethers of aliphatic, polyhydric alcohols, free from carbonyl groups, which alcohols contain at least 3 carbon atoms in the molecule, with aliphatic substances which contain at least 6, and preferably from 10 to 18 carbon atoms, in the molecule, the final product containing at least two free hydroxyl groups The products are stated to be " wetting, cleansing and dispersing agents". U.K Patent Specification No 380,431 describes the production of products suitable as assistants for the textile and related industries which consists in esterifying or etherifying a water-insoluble organic compound other than a water-insoluble carbohydrate but containing at least one hydroxyl or carboxylic acid group, or a group reacting like a carboxylic acid group under the conditions of working, with polyethylene glycols containing a chain of at least four ethenoxy groups, or with mono-ethers or-esters of such polyethylene glycols And in U K Patent Specification No 541,099 is described a process for the production of threads which comprises extruding viscose into an aqueous coagulating solution of sulphuric acid and at least one metallic salt, which may be zinc sulphate, in the presence of a non-ionogenic Pdice 3 s 6 d l water-soluble compound obtainable by the action of an alkylene oxide on a monohydroxy compound containing at least 8 carbon atoms in a chain The products serve to re 50 duce the

tendency of the orifices of the jets to become partially or completely blocked and may be added to the viscose or coagulating bath in small quantities, for example of the order of 0 02 per cent or less cal 55 culated on the viscose. Viscose filaments produced by the normal spinning processes have la crenulated surface and a structure which consists of a skin and a core The presence of the skin and core 60 can be demonstrated by staining a cross-section cut from the filaments under specific conditions; such methods are described in the Textile Research Journal, 1945, page 443. Another method of differentiating between 65 the skin and core is by measuring the mate of axial diffusion of dyestuffs as described in the Textile Research Journal, 1948, page 9. In addition to the difference in dyeing affinity and in swelling property between the 70 skin and core the cellulose molecules of the skin are believed to be more highly orientated than those of the core and for this reason it is thought that the strength of viscose fibres resides mainly in the skin It is well-known, for 75 example, that industrial viscose yams such as are used in the manufacture of tyres have a much thicker skin than the normal textile fibres It has been proposed, for example in U.K Patent Specification No 723,435, to 80 obtain viscose filaments having a thick skin, a non-crenulated surface and a diffuse boundary between skin and core. The object of the present invention is to provide a further process for obtaining modified 85 viscose filaments. According to the present invention a process for the production of artificial filaments comprises spinning viscose in which is dissolved more than 0 02 grams of alkylene oxide-fatty 90 acid condensate per 100 grams of viscose into a coagulating bath containing sulphuric acid and zinc sulphate An example of such a compound is obtained by reacting ethylene oxide with a sperm oil. The upper limit of the amount of alkylene oxide-fatty acid condensate to be added is determined by the solubility of the compound in the medium used and is of the order of 2 per cewt of the viscose The preferred alkylene oxide is ethylene oxide and the compounds preferably contain 3-40 moles of ethylene oxide per average molecular equivalent of a sperm oil The coagulating bath may be of any desirable concentration, it may contain sulphuric acid, sodium sulphate and zinc sulphate, and the zinc sulphate concentration is preferably-between 0 5 per cent and 15 per cent The actual concentration of zinc sulphate used will depend on the type of filament being spun Other substances may be added to thte spinning bath, such as ammonium sulphate, magnesium sulphate and glucose. The invention includes viscose containing at least 0 02 per cent of a compound obtained by reacting an alkylene oxide with a fatty acid, or

source of fatty acid, such as a sperm oil The invention also includes modified regenerated cellulose filaments having a thick skin and a non-crenulated surface when produced by the process of the present invention. In addition to the thick skin and non-crenulated surface the filaments may have a beanshaped cross-section and a diffuse boundary between the skin and core In certain cases tthe core may be very small or non-existent The process of the present invention also tends to reduce the milkiness of the filaments and to lower the water-imbibition Tests may be necessary to determine the quantity of the compound to be added to give the desired characteristics to the filament. The process of the present invention enables unripened or so-called " green " viscoses to be spun When spinning according to the process of this invention the concentration of cellulose in the freshly spun rayon filaments is appreciably increased. The advantages of the process are realised to the greatest extent when it is used in conjunction with the so-called " hot stretch " process in which the freshly spun filaments are subjected to stretching while they are passing through a bath of hot dilute acid as described in U K Patent Specification No 467,500. When filaments are made by ithe combination of the hot stretch process and the process of the present invention for use in the manufacture of composite rubber rayon articles, for example tyres, the cords made from the filaments are of improved quality and have a greater fatigue life than similar cords produced without the process of the present invention. The invention is illustrated by the following Examples in which the percentages are by weight. EXAMPLE 1. To viscose containing 7 4 per cent of cellulose, 7 0 per ceezt of caustic soda and 33 per cent of carbon disulphide based on the weight of alpha-cellulose was added 0 1 per cent of 70 an ethylene oxide-sperm oil compound sold under the trade name " Cetrol " The compound contained 9 moles of ethylene oxide per average molecular equivalent of sperm oil. When the salt figure of the viscose had reached 75 7.3 the viscose was extruded through a jet having 750 holes each 0 0025 inch in diameter into a coagulating bath containing 7 2 per cent of sulphuric acid, 19 1 per cent of sodium sulphate and 6 85 per dent of zinc sulphate The 80 length of immersion of the filaments in the bath was 34 inches and the 750 filamentthread so formed was withdrawn from the bath at a rate of 53 metres per minute and stretched 75 per cent in a hot dilute acid bath at 95 C The 85 thread was subsequently washed, desulphurised, treated with a finish, dried and collected on a cap twister and had a

denier of f 700. The stained cross-sections of the filaments 90 obtain are shown in the drawing accompanying the provisional specification which shows the cross-section of filaments spun according to the example The filaments are bean-shaped in cross-section, have a non-crenulated surface 95 and a very thick skin Many of the filaments have no core Filaments spun under similar conditions but without the ethylene oxide sperm oil-compound were generally circular with a crenulated surface, a thinner skin and 100 a distinct core. EXAMPLE 2. A viscose was prepared having the same composition as that in Example 1 except that it contained 0 1 per cent of an ethylene oxide 105 sperm oil compound containing 33 moles of ethylene oxide per average molecular equivalent of sperm oil. The viscose was extruded at a salt figure of 7.5 through a jet having 750 holes each 0 0025 110 inch in diameter into a coagulating bath containing 6 96 per cent of sulphuric acid, 19 0 per cent of sodium sulphate and 7 83 per cent of zinc sulphate The length of immersion, withdrawal speed, and hot stretch conditions 115 and taftertreatment were the same as described in Example 1 and the filaments had similar characteristics to those shown in the drawing.

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* GB785617 (A)

Description: GB785617 (A) ? 1957-10-30

Spinneret plates

Description of GB785617 (A)

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PATENT SPECIFICATION Inventors: WILLIAM FRANCIS OSBOR JOHN WILDEY PHIPPS (z f EB Date of filing Complete Specification: Jan. 1) i i WJ Application Date: Feb4, 1955. \\ O Complete Specification Published: Oct30, 1 Index at acceptance:-Class 2 ( 2), Bl Bi. International Classification:-D Old. COMPLETE SPECIFICATION Spinneret Plates We, IMPERIAL CHEMICAL INDUSTRIES LIMITED, of Imperial Chemical House, Millbank, London, S W 1, England, a British Company, do hereby declare the invention, S 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 thin spinneret lo plates and their use in melt spinning apparatus. The spinnerets comonly used in the melt spinning of artificial filaments are made of thick metal plates so that they withstand the high melt pressures necessary for spinning the molten polymer. In order to produce fine orifices of accurate diameter and of a capillary length (of about 1 5 diameters) in the thick plates, it is necessary to drill deep counterbores of substantially larger diameters into the upper surface of the plates Furthermore the manufacture of such spinneret plates is expensive and a high degree of accuracy in dimensions and of smoothness of capillary walls, required to produce uniformity of dimensions in the extruded filaments, is difficult to attain. Usually the spinneret plate is supported at its periphery by shoulders at the end of a barrel-like spinning pack housing, the remaining components of the spinning pack resting on the spinneret plate, e g the filter gauzes and sand pack. According to our invention we provide a melt spinning apparatus

comprising a thin spinneret plate characterised in that the spinneret plate is less than 2 mm thick in at least that part where the holes are and that as well as being supported at its periphery it is also supported in at least one area away from the periphery Preferably the additional support is at the centre of the spinneret plate. Using this preferred support, the spinneret holes can advantageously be arranged in a circle round the spinneret centre. The addi$,qnal support enables the use of lPrice _ NE and 785,617 18, 1956 No 3328/55. 957. very thin spinneret plates Such thin spinneret plates can be made from a thin metal plate of uniform thickness, and the spinneret holes of a high degree of accuracy 50 are obtained by simple punching The thin spinnerets are therefore much less expensive than the thick spinneret plates hitherto used in melt spinning Furthermore the holes can be made with an accurately shaped bell 55 mouth on the upper side and cleaning and inspection is greatly simplified. When supporting the additional area the preferred form is to secure said additional area by suitable means to a support situated 60 above the upper or pressure side of the spinneret plate One way of achieving this is by securing the additional area to the spinning pack housing The preferred form consists in securing the additional area, e g the 65 centre of the spinneret to a perforated bridge plate substantially of the same shape as the spinneret which extends over the whole width of the spinning pack and is itself supported at its periphery, e g by shoulders on 70 the spinning pack housing The bridge plate must be provided with suitable apertures for the unimpaired flow of the molten polymer to the spinneret orifices. To assist the flow of the melt, a melt dis 75 tribution plate may be placed between the bridge plate and the melt source This melt distribution plate can support the filter pack and has a number of preferably intersecting grooves on that surface facing the filter pack, 80 said grooves covering as large an area as possible, consistent with the mechanical rigidity of said plate and leading to orifices in the bridge plate which conduct the melt to the spinneret 85 The drawings filed with the provisional specification illustrate but do not limit our invention. Fig 1 is a diagrammatic section through a spinning pack with a thin spinneret Fig 2 90 is a diagrammatic plan view of the spinneret shown in Fig 1. 2 785,617 In Fig 1 the thin spinneret ( 6) is used in the spinning pack housing ( 1) The spinning pack housing ( 1) is provided with a shoulder ( 2) which supports the thin spinneret through a shaped washer ( 10) The thin spinneret plate is shaped into a circular trough

and the spinneret holes ( 13) and ( 14) are punched into the base of the trough The holes are of a bell shape In the centre of the thin spinneret plate there is a hole through which passes a bolt ( 8) via a large shaped washer ( 9) The bolt ( 8) is threaded into a bridge plate ( 3) which rests on the thin spinneret plate and is supported by the shoulder ( 2) of the spinning 1, pack housing ( 1) The bridge plate ( 3) is provided with apertures ( 4) and ( 5) which lead to the spinneret holes ( 13) and ( 14) The number of apertures in the bridge plate correspond to the number of holes in the thin 2 o spinneret plate and the holes are placed to lead to each of the spinneret holes Above the bridge plate there is a melt distribution plate ( 15) which distributes the melt coming from a filter pack above the melt distribution plate. Fig 2 is a plan view of the thin spinneret plate, of a thickness of 1 5 mm, as used in the spinning pack of Fig 1 It is made of nickel steel The outside flange ( 11) is the peripheral Dart which rests on the shoulder ( 2) of the spinning pack housing ( 1) shown in Fig 1 Concentric with that flange is a circular trough bearing on its apex one circle of spinneret holes ( 12) which have been produced by punching small holes of the required size in the plate. During spinning a spinning pump pumps the molten material through filter packs, not shown, to the grooved melt distribution plate ( 15) which faces the filter pack and which contains a number of grooves leading to one or more apertures in the bridge plate ( 3) below The molten material passes through the apertures ( 4) and ( 5) in the bridge plate which lead it to the circular projecting trough of the thin supported spinneret plate ( 6) The hydraulic pressure of the melt is used to seal the spinneret against the shoulder ( 2) of the spinning pack housing by means of the shaped gasket ( 10) The centre aperture of the thin spinneret plate is sealed by the hydraulic pressure by pressing against the shaped washer ( 9) held by the bolt ( 8) which is screwed into the bridge plate ( 3). In the drawings the spinneret is supported on shoulders which are a part of the barrel forming the spinning pack housing In other forms of melt spinning apparatus the spinneret may be supported by a ring threaded into the spinning pack housing or by locking bolts or any other known means. While in the drawings a spinneret with an annular trough is illustrated this can be replaced by a flat plate if desired We prefer the annular troughed spinneret because the trough gives greater rigidity to the plate. The use of a single ring of holes enables the maximum area of spinneret to be supported using a centre supporting means. However other supporting means may be 70 used and, if so, different

hole patterns may be desired For example, struts projecting radially inwards from the wall of the spinning pack housing may support the spinneret In this case the spinneret holes should 75 be arranged between the radial struts. The spinnerets of our invention are easier to manufacture and maintain and rigorous inspection of the spinneret apertures in the thin plate is easily carried out Furthermore 80 the orifices in thin plate spinning have been found to be less liable to blockage by carbonized melt or by adventitious foreign matter In practice it has been found that a greater degree of uniformity in diameter of 85 the extruded filaments has been attained than has hitherto been found possible with thick plate spinnerets.

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