Patent GB-456151-A (GB)
Title: Improvements in or relating to the manufacture of derivatives of hydrocyanic acid
IPC: C09B59/00
Filed: 1935-05-03
Abstract: Conversion products of hydrocyanic acid useful as activators in chemical reactions and in particular in the metal treating industry are prepared by treating hydrocyanic acid with water in the presence of a catalyst, the concentration of the acid being below 57 per cent. Materials suitable as catalysts are ammonium salts, and alkaline reacting compounds.  Ammonium salts specified p  are the chloride, cyanide, nitrate and sulphate, and alkaline substances specified are sodium cyanide, sodium acetate, sodium carbonate, sodium borate and their potassium equivalents, together with alkaline - earth carbonates hydroxides and cyanides, and primary, secondary and tertiary aromatic or aliphatic amines. Examples of the latter compounds are methyl, ethyl and n-propyl amine, aniline, toluidine, benzylamine, and the naphthylamines. Of all the above catalysts, however, caustic soda, soda ash, and in particular an aqueous solution of ammonia are the preferred examples.  The preferred amount of catalyst is 6 per cent of the hydrocyanic acid used.  The reaction vessel is furnished with a stirrer, reflux condenser, and a water jacket through which water is circulated first at about 130 DEG  F. to start the reaction, and later at a lower temperature to carry away excess heat and prevent the reaction from becoming too violent.  The character of the conversion product depends on the concentration of the reactants and the temperature of the reaction.  A high concentration and a high reaction temperature produce a hard black material with an igneous appearance, and lower concentrations produce a dull black amorphous mass.  This latter form is the more desirable product. The concentration of the catalyst does not appear to affect the character of the product, only the reaction time.  At the end of the reaction (about 8 hours) the solid is filtered off and the catalyst recovered from the filtrate.  In examples: (1) ammonium hydroxide, liquid hydrocyanic acid and water is warmed to start the reaction, which then proceeds for 4 hours.  The dull black product is removed by filtration; (2) commercial hydrocyanic acid, sodium hydroxide and water are reacted together for 190 minutes at 145 DEG F. to give an 89 per cent yield of amorphous dull black product; (3) commercial hydrocyanic acid, sodium carbonate and water are reacted at 135 DEG  F. for 255 minutes to give an 87 per cent yield of dull black product.  The Specification as open to inspection under Sect. 91 comprises also the information that the character of the product changes from the dull black to the igneous type of product at 56--57 per cent HCN concentration, and at about 80 per cent HCN concentration the product is about 80 per cent igneous type of product.  This subject-matter does not appear in the Specification as accepted.ALSO:Conversion products of hydrocyanic acid (probably polymers thereof) useful as activators in chemical reactions and in particular in the metal treating industry are prepared by treating hydrocyanic acid with water in the presence of a catalyst, the concentration of the acid being below 57 per cent.  Materials suitable as catalysts are ammonium salts and alkaline reacting compounds.  Ammonium salts specified are the chloride, cyanide, nitrate and sulphate, and alkaline substances specified are sodium cyanide, sodium acetate, sodium carbonate, sodium borate and their potassium equivalents, together with alkaline-earth carbonates hydroxides and cyanides, and primary, secondary and tertiary aromatic or aliphatic amines.  Examples of the latter compounds are methyl, ethyl and n-propyl amine, aniline, toluidine, benzylamine, and the naphthylamines.  Of all the above catalysts, however, caustic soda, soda ash, and in particular an aqueous solution of ammonia are the preferred examples.  The preferred amount of catalyst is 6 per cent of the hydrocyanic acid used. The reaction vessel is furnished with a stirrer, reflux condenser, and a water jacket through which water is circulated first at about 130 DEG  F. to start the reaction, and later at a lower temperature to carry away excess heat and prevent the reaction from becoming too violent.  The character of the conversion product depends on the concentration of the reactants and the temperature of the reaction.  A high concentration and a high reaction temperature produce a hard black material with an igneous appearance, and lower concentrations produce a dull black amorphous mass.  This latter form is the more desirable product. The concentration of the catalyst does not appear to affect the character of the product, only the reaction time.  At the end of the reaction (about 8 hours) the solid is filtered off and the catalyst recovered from the filtrate.  In examples: (1) ammonium hydroxide, liquid hydrocyanic acid and water is warmed to start the reaction, which then proceeds for 4 hours.  The dull black product is removed by filtration; (2) commercial hydrocyanic acid, sodium hydroxide and water are reacted together for 190 minutes at 145 DEG  F. to give an 89 per cent yield of amorphous dull black product; (3) commercial hydrocyanic acid, sodium carbonate and water are reacted at 135 DEG F. for 255 minutes to give an 87 per cent yield of dull black product.  The Specification as open to inspection under Sect. 91 comprises also the information that the character of the product changes from the dull black to the igneous type of product at 56--57 per cent HCN concentration, and at about 80 per cent HCN concentration the product is about 80 per cent igneous type of product.  This subject-matter does not appear in the Specification accepted.