Process for the extraction of hops
阅读：978发布：2022-01-26
专利汇可以提供Process for the extraction of hops专利检索，专利查询，专利分析的服务。并且Process for extracting from hops the essential brewing ingredients thereof, viz., neutral substances, bitter substances and tannin, which process comprises subjecting a primary extract solution of hops, e.g., in alcohol or hydrocarbon solvents, said solution containing as ingredients the neutral substances, bitter substances and tannin, to a first liquid-liquid extraction, wherein either (i) the tannins or (ii) the neutral substances are separated off, leaving a solution of (i) neutral and bitter substances or (ii) tannins and bitter substances, and subjecting the latter solution to a second liquid-liquid extraction to separate said solution into its components; the first extractant is desirably an aliphatic, cycloaliphatic or aromatic hydrocarbon when the primary extract solvent is an alcohol or aqueousalcoholic solution, to result in extraction of the neutral and bitter substances in a hydrocarbon phase and leaving of the tannin in the alcoholic phase, whereafter the neutral and bitter substances are separated from each other by treating the extract with a second extractant, desirably aliphatic alcohol containing water.，下面是Process for the extraction of hops专利的具体信息内容。
1. PROCESS FOR SUBSTANTIALLY SEPARATING THE ESSENTIAL INGREDIENTS OF HOPS, WHICH PROCESS COMPRISES SUBJECTING A PRIMARY EXTRACT OF HOPS IN AN ORGANIC SOLVENT, CONTAINING AS COMPONENTS (I) NEUTRAL SUBSTANCES, (II) BITTER SUBSTANCES AND (III) TANNINS, TO A FIRST LIQUID-LIQUID EXTRACTION WITH A SECOND ORGANIC SOLVENT DIFFERENT FROM SAID PRIMARY EXTRACT SOLVENT WHEREBY EITHER (III) THE TANNINS OR (I) THE NEUTRAL SUBSTANCES ARE SUBSTANTIALLY SEPARATED OFF, LEAVING A RESIDUAL SOLUTION OF (I AND II) NEUTRAL AND BITTER SUBSTANCES OR (III AND II) TANNINS AND BITTER SUBSTANCES, AND SUBJECTING THE RESIDUAL SOLUTION TO A SECOND LIQUID-LIQUID EXTRACTION WITH AN ORGANIC SOLVENT DIFFERENT FROM SAID SECOND ORGANIC SOLVENT TO SEPARATE SAID SOLUTION INTO ITS COMPONENTS.
2. ProcEss as claimed in claim 1, wherein the primary extract solution is a solution of the hops ingredients in alcohol, alcohol containing water, benzene, alkyl benzenes or halogenated hydrocarbons.
3. Process as claimed in claim 1, wherein the primary extract solution is a methanolic-aqueous or an ethanolic-aqueous solution.
4. Process as claimed in claim 3, wherein the alcoholic primary extract solution has a water content of from about 5 to 30% by volume.
5. Process as claimed in claim 1, wherein the primary extract solution is a solution of the hops ingredients in benzene.
6. Process as claimed in claim 1, wherein the primary extract solution is a solution of the hops ingredients in methylene chloride.
7. Process as claimed in claim 1, wherein the primary extract solution is subjected to the first liquid-liquid extraction in an extraction stage A, wherein the neutral and bitter substances (i and ii) are separated from the tannins (iii), and to the second liquid-liquid extraction in an extraction B, wherein the neutral substances (i) are separated from the bitter substances (ii).
8. Process as claimed in claim 7, wherein the primary extract solution is an alcoholic solution and the primary extract solution is subjected, in the extraction stage A, to extraction with a hydrocarbon extractant 1 comprising at least one of aliphatic hydrocarbons of from 5 to 10 carbon atoms, cyclo-aliphatic hydrocarbons of from 5 to 8 carbon atoms, and aromatic hydrocarbons selected from benzene and alkyl-substituted benzene derivatives, resulting in an extract of the neutral substances and bitter substances (i and ii) in a hydrocarbon phase and leaving the tannins (iii) in an alcoholic phase; subjecting the extract from said extraction stage A, containing (i and ii) in extraction stage B, to extraction with an alcohol extractant 2 comprising a mixture of at least one lower aliphatic alcohol with water, to result in an extract of the bitter substances (ii) in an alcohol/water phase and leaving the neutral substances (i) in the hydrocarbon phase.
9. Process as claimed in claim 8, wherein the alcoholic primary extract solution contains water in such amount that, in extraction stage A, the water content of the alcoholic phase amounts to between about 10 and 30% by volume and the aromatic and cycloaliphatic hydrocarbon content of extractant 1 amounts to between about 10 and 60% by volume.
10. Process as claimed in claim 8, wherein the ratio by volume of extractant 1 to the alcoholic phase is in the range of from about 1 to 10.
11. Process as claimed in claim 8, wherein the hydrocarbon phase subjected to extraction in extraction stage B has a cycloaliphatic and/or aromatic hydrocarbon content of less than about 40% by volume, while the water content of extractant 2 is from about 10 to 30 % by volume.
12. Process as claimed in claim 8, wherein the hydrocarbon phase extracted in extraction stage B contains approximately 0 to 30 % by volume of cycloaliphatic and/or aromatic hydrocarbons, and the water content of extractant 2 is from about 10 to 20 % by volume.
13. Process as claimed in claim 8, wherein the ratio by volume of said hydrocarbon phase to extractant 2 is in the range of from about 0.1 to 1.0.
14. Process as claimed in claim 8, wherein the ratio by volume of said hydrocarbon phase to the alcohol phase in extraction stage B is reduced to at least one half to one third of the corresponding ratio of hydrocarbon phase to the alcoholic phase in extraction stage A.
15. Process as claimed in claim 8 wherein in extraction stage A the extractant is at least one halogenated hydrocarbon with from 1 to 3 carbon atoms and with up to 3 halogen atoms.
16. Process as claimed in claim 7, wherein the primary extract solution is a solution of the hops ingredients in benzene, alkyl benzenes, or halogenated hydrocarbons, and the primary extract solution is subjected, in extraction stage A, to extraction with an alcoholic extractant 1 comprising at least one of aliphatic alcohols of from 1 to 3 carbon atoms, or mixtures of such alcohols with water, whereby the neutral and bitter substances (i and ii) remain in the hydrocarbon or halogenated hydrocarbon phase as a raffinate, while the tannins (iii) are extracted into the alcoholic phase as a tannin extract; and subjecting, in extraction stage B, the raffinate from extraction stage A containing neutral and bitter substances (i and ii), to extraction with an alcohol extractant 2 comprising a mixture of lower aliphatic alcohol with water, to result in an extract of the bitter substances (ii) in an alcohol/water phase and leaving the neutral substances (i) in the hydrocarbon or halogenated hydrocarbon phase.
17. Process as claimed in claim 16, wherein methanol-water mixtures containing from 10 to 40 % by volume of water are used as extractant 1 in extraction stage A.
18. Process as claimed in claim 16, wherein, in extraction stage A, the ratio by volume of the hydrocarbon phase to the alcoholic phase is in the range of from about 1 to 10.
19. Process as claimed in claim 16, wherein, in extraction stage A, the ratio by volume of the halogenated hydrocarbon phase to the alcoholic phase is in the range of from about 0.1 to 2.
20. Process as claimed in claim 16, wherein the hydrocarbon phase used in extraction stage B has an aromatic hydrocarbon content of less than about 40% by volume, and the water content of extractant 2 is from about 10 to 30 % by volume.
21. Process as claimed in claim 20, wherein the ratio by volume of the hydrocarbon phase to extractant 2 is in the range of from about 0.1 to 1.0.
22. Process as claimed in claim 16, wherein the halogenated hydrocarbon phase used in extraction stage B is methylene chloride and extractant 2 is a methanol-water mixture containing from 30 to 40% by volume of water.
23. Process as claimed in claim 22, wherein the ratio by volume of the halogenated hydrocarbon phase to extractant 2 is in the range of from about 0.05 to 0.2.
24. Process as claimed in claim 1, wherein the neutral substances (i) are separated from the bitter substances and tannins (ii and iii) in the primary extract solution in an extraction stage C, while the tannins (iii) are separated from the bitter substances (ii) in an extraction stage D.
25. Process as claimed in claim 24, wherein the primary extract solution is an alcoholic solution and the primary extract solution is subjected, in extraction stage C, to extraction with a hydrocarbon extractant 3 comprising at least one of aliphatic hydrocarbons having from 5 to 10 carbon atoms, cycloaliphatic hydrocarbons having from 5 to 8 carbon atoms, and aromatic hydrocarbons selected from benzene and alkylsubstituted benzene derivatives, to result in extraction of the neutral substances (i) into a hydrocarbon phase as a neutral substance extract, while the bitter substances and tannins (ii) and (iii) are left in an alcoholic phase; and the alcoholic phase left after extraction stage C is subjected, in extraction stage D, to extraction with a hydrocarbon extractant 4 comprising at least one of aliphatic hydrocarbons of from 5 to 8 carbon atoms, aliphatic hydrocarbons of from 5 to 10 carbon atoms, cycloaliphatic hydrocarbons of from 5 to 8 carbon atoms, and aromatic hydrocarbons selected from benzene and alkyl-substituted benzene derivatives, to result in extraction of the bitter substances (ii) into the hydrocarbon phase while the tannins (iii) are left in the alcoholic phase.
26. Process as claimed in claim 25, wherein the primary extract solution in extraction stage C has a water content of from about 5 to 30% by volume.
27. Process as claimed in claim 25, wherein the ratio by volume of extractant 3 to the alcoholic phase is in the range of from 0.1 to 1.
28. Process as claimed in claim 24, wherein the primary extract solution is a solution of the hops ingredients in benzene, alkylbenzenes or halogenated hydrocarbons and the primary extract solution is subjected to, in extraction stage C, extraction with an alcoholic extractant 3 comprising at least one of aliphatic alcohols of from 1 to 3 carbon atoms or mixtures of such alcohols with water, to result in leaving the neutral substances (i) in a hydrocarbon or halogenated hydrocarbon phase while the tannins and the bitter substances (iii and ii) are extracted into the alcoholic phase; and the alcoholic extract phase from extraction stage C containing tannins and bitter substances (iii and ii) is subjected, in extraction stage D, to extraction with a hydrocarbon extractant 4 comprising at least one of aliphatic hydrocarbons of from 5 to 10 carbon atoms, cycloaliphatic hydrocarbons having from 5 to 8 carbon atoms, and aromatic hydrocarbons selected from benzene and alkyl-substituted benzene derivatives, to result in extraction of the bitter substances (ii) into the hydrocarbon phase while the tannins (iii) remain in the alcoholic phase.
29. Process as claimed in claim 28, wherein a methanol-water mixture containing from 10 to 40% by volume of water is used as extractant 3 in extraction stage C.
30. Process as claimed in claim 28, wherein the primary extract solution is a solution containing a halogenated hydrocarbon and the ratio by volume of the halogenated hydrocarbon phase to the alcoholic phase is in the range of from 0.1 to 0.4.
31. Process as claimed in claim 28, wherein the alcoholic phase used in extraction stage D has a water content of from about 10 to 40% by volume, and the hydrocarbon phase used as extractant 4 has an aromatic hydrocarbon content of from about 0 to 90 % by volume.
32. Process as claimed in claim 28, wherein the ratio by volume of extractant 4 to the alcoholic phase is in the range of from about 1 to 10.
33. Process as claimed in claim 28, wherein the ratio by volume of the hydrocarbon phase to the alcoholic phase in extraction stage D is increased by at least about 5 to 20 times in relation to the corresponding ratio in extraction stage C.
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