Patent GB-341000-A (GB)
Title: Process for recovering valuable products from cocoa by-products
IPC: C07D473/12
Filed: 1929-10-07
Abstract: Fats and fatty acids are extracted, together with alkaloids, from cocoa by-products such as cocoa press cake, cocoa expeller cake, and cocoa shells by means of ethylene dichloride.  The by-products are preferably subjected to a preliminary treatment with water or steam at temperatures of 50-120 DEG  C.  The material thus opened up is extracted a number of times with ethylene dichloride in suitable vessels with agitation at temperatures of 60-85 DEG  C.  The extraction may also be carried out continuously on the counter-current principle, and pressure may be employed.  The extract contains the fats and fatty acids together with alkaloids such as caffeine and theobromine; if desired, the extraction may be performed at lower temperatures, at which the theobromine is not removed.  The solvent is removed from the extract, for example, by distillation with or without the use of steam or reduced pressure.  From the concentrated fat solution remaining, the theobromine crystallizes almost completely and may be filtered off.  The caffeine may be removed from the filtrate by agitation with hot water.  The crude fat remaining may then be refined and the free fatty acids contained therein removed by known methods. In an alternative method of separation the extract is treated, preferably in the presence of a small amount of water, with a material forming a compound with theobromine insoluble in ethylene dichloride, for example an alkali or alkaline earth or other metal oxide or hydroxide.  By this means the salts of the fatty acids and of the theobromine mixed with or dissolved in water form a top layer on the extract and are separated. The extract is the clarified by known agents or by filtration, and the p  ethylene dichloride is distilled off, preferably in steam, in which case the steam is allowed to condense partially in the still and the caffeine is removed from the fat by extracting with the water condensate.  The fatty acids and theobromine in the water layer are set free from their salts by means of a suitable mineral acid such as hydrochloric acid.  If sufficient residual ethylene dichloride is not present to dissolve the fatty acids, more is added and the theobromine is then separated by filtration.ALSO:Fats, fatty acids, and alkaloids such as theobromine and caffeine are extracted from cocoa press cake, cocoa expeller cake, cocoa shells, and similar cocoa by-products by means of ethylene dichloride.  The by-products are preferably subjected to a preliminary treatment with water or steam at temperatures of 50-120 DEG  C. in order to set free the combined alkaloids.  The material thus opened up is extracted a number of times with ethylene dichloride in suitable vessels with agitation at temperatures of 60-85 DEG  C.  The extraction may also be carried out continuously on the counter-current principle.  If desired, the fat and caffeine may first be extracted at temperatures below 60 DEG  C. and the theobromine subsequently extracted at higher temperatures.  The extraction may be effected under pressure.  The solid residue from which the fat and alkaloids have been removed may be freed from ethylene dichloride by distillation with or without the aid of reduced pressure, steam, air, or other gases, and may then be used as food for cattle or as a fertilizer.  The extract is treated to separate the fats and alkaloids from the solvent, for example, by distilling off the latter with or without the use of steam or reduced pressure.  From the concentrated fat solution remaining, the theobromine crystallizes almost completely and may be filtered off. The caffeine may be removed from the filtrate by agitation with hot water and recovered from the water solution by evaporation.  The crude fat remaining may then be refined and the free fatty acids contained therein removed by known methods.  In an alternative method of separation the extract is treated, preferably in the presence of a small amount of water, with a substance forming a compound with theobromine insoluble in ethylene dichloride, for example, an alkali or alkaline earth or other metal oxide or hydroxide.  By this means the salts of the fatty acids and of the theobromine dissolved in or mixed with water form a top layer on the extract and are separated. The extract is then clarified with known agents or by filtration, and the ethylene dichloride is distilled off, preferably in steam, in which case the steam is allowed to condense partially in the still and the caffeine is recovered from the fat by extraction with the water condensate.  The fatty acids and theobromine in the water layer are set free from their salts by means of a suitable mineral acid such as hydrochloric acid.  If sufficient residual ethylene dichloride is not present to dissolve the fatty acids, more is added, and the theobromine is then separated by filtration.ALSO:The residues of cocoa bye-products such as cocoa press cake, cocoa expeller cake, and cocoa shells which are left after the fats and alkaloids contained therein have been extracted by means of ethylene dichloride are used as food for animals, or as fertilizers.ALSO:Fats, fatty acids, and alkaloids are extracted from cocoa press cake, cocoa expeller cake, cocoa shells, and similar cocoa bye-products by means of ethylene dichloride.  The bye-products are preferably subjected to a preliminary treatment with water or steam at a temperature of 50-120 DEG  C. in order to set free the combined alkaloids.  The material thus opened up is extracted a number of times with ethylene dichloride in suitable vessels with agitation at temperatures of 60-85 DEG  C.  The extraction may also be carried out continuously on the countercurrent principle.  If desired, the fat and caffeine may first be extracted at temperatures below 60 DEG  C. and the theobromine subsequently extracted at higher temperatures.  The extraction may be effected under pressure.  The solid residue from which the fat and alkaloids have been removed may be freed from ethylene dichloride by distillation with or without the aid of reduced pressure, steam, air, or other gases, and may then be used as a fertilizer or as food for animals.  The extract is treated to separate the fats and alkaloids from the solvents, for example, by distilling off the latter with or without the use of steam or reduced pressure.  From the concentrated fat solution remaining, the theobromine crystallizes out almost completely and may be filtered off.  The caffeine may be removed from the filtrate by agitation with hot water and recovered from the water solution by evaporation.  The crude fat remaining may then be refined and the free fatty acids contained therein removed by known methods.  In an alternative method of separation the extract is treated, preferably in the presence of a small amount of water, with a substance forming a compound with theobromine insoluble in ethylene dichloride for example, an alkali or alkaline earth or other metal oxide or hydroxide.  By this means the salts of the fatty acids and of the theobromine dissolved in or mixed with water form a top layer on the extract and are separated. The extract is then clarified with known agents or by filtration, and the ethylene dichloride is distilled off, preferably in steam, in which case the steam is allowed to condense partially in the still and the caffeine is recovered from the fat by extraction with the water condensate.  The fatty acids and theobromine in the water layer are set free from their salts by means of a suitable mineral acid such as hydrochloric acid.  If sufficient residual ethylene dichloride is not present to dissolve the fatty acids, more is added, and the theobromine is then separated by filtration.