CN103146517A - Method for extracting high-ester seasoning liquid from after-run - Google Patents
Method for extracting high-ester seasoning liquid from after-run Download PDFInfo
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- CN103146517A CN103146517A CN2012101892204A CN201210189220A CN103146517A CN 103146517 A CN103146517 A CN 103146517A CN 2012101892204 A CN2012101892204 A CN 2012101892204A CN 201210189220 A CN201210189220 A CN 201210189220A CN 103146517 A CN103146517 A CN 103146517A
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Abstract
The invention discloses a method for extracting a high-ester seasoning liquid from after-run and belongs to the field of recovering a white spirit fermentation by-product. The method comprises the following steps of selecting after-run raw materials, pretreating the after-run raw materials and extracting and separating the high-ester seasoning liquid. The high-ester seasoning liquid is complex liquid comprising a plurality of flavor components such as ethyl caproate as a main flavor component, has the advantages of high ethyl caproate content above 250g/L, low long-chain higher fatty acid ethyl ester content, no color, transparent character, and thick, pure and appropriate fragrance, and can be used for white spirit blending thereby obviously improving white spirit quality. The high-ester seasoning liquid is extracted from after-run obtained by special material selection of a white spirit fermentation by-product. In the whole method, the high-ester seasoning liquid does not contact with any chemical reagents and is a natural seasoning liquid.
Description
Technical field
The present invention relates to a kind of wine separating and extracting method of high-ester flavouring liquid, belong to the recovery field of liquor fermentation by product.
Background technology
The wine tail is that conventional solid-state white liquor distilling process is interrupted the low alcohol that Hua Housuo plucks, and alcoholic strength generally between 14～20 °, contains a large amount of esters of gallic acid compositions in the wine tail.Most brewery still adopts returns the wine tail to the mode that end pot string steams, and extracts remaining part alcohol and part esters of gallic acid material in the wine tail.This traditional way exist damage wine, only can Extraction parts the also drawback such as volatile acid Ester, a large amount of beneficiating ingredients in the wine tail still can not effectively be extracted.Indivedual producers have adopted the supercritical extraction mode to extract effective constituent in the wine tail.As patent CN100415866C, at first the wine tail is carried out rectifying, obtain the extremely low rectifying still liquid of ethanol content, and then adopt supercritical extraction mode to extract wherein beneficiating ingredient this mixed solution, but its shortcoming is that the component that extracts is high boiling point organic compound mostly, be not the skeletal substances such as acid esters in white wine, and component concentration is lower.
In traditional aroma daqu liquor is produced, vinosity improves by the mode that extends fermentation period in most families that produce, extend fermentation period and can improve product ester ability in the cellar for storing things, especially the content near Ester in the wine unstrained spirits of a rice steamer at the bottom of the pond is very high, and then make the content of the Ester in the former wine of distillation raise, fermentation time is longer, and the Ester in the former wine especially content of ethyl hexanoate is just higher.But by distillation, only can extract the ester class of a small part, most Ester is dissolved in the wine tail or remains in poor unstrained spirits.Find through observing, fermentation period was at the Jiao Chi of 4～6 months, the wine tail of the rice steamer wine unstrained spirits at the bottom of close pond is through a standing night, and the surface meeting of wine tail produces a large amount of oily matter, and this oily matter contains the materials such as a large amount of ethyl hexanoates, caproic acid and ethyl palmitate after testing.If but with this oily matter wine blending, due to the existence that higher fatty acid ethyl esters is arranged, be easy to make the wine body muddy.
That supercritical carbon dioxide extraction method has is pure, safety, no solvent residue, extraction yield is high, flow process is simple, solvent carbonic acid gas relative low price and the plurality of advantages such as can be recycled, and is widely used in the food medicine and other fields.The stagnation point of carbonic acid gas is 31.06 ℃, 7.39Mp, and its critical temperature and pressure are all lower, be easy to industrialization, and that carbonic acid gas has is non-combustible, nontoxic, chemical stability is good, easily separated, therefore the advantage such as cheap and easy to get is widely used in supercritical extraction process.The density of supercritical carbon dioxide fluid can be regulated by changing pressure, the change of density directly affects its dissolving power, therefore supercritical extraction can be controlled with pressure the dissolving power of supercutical fluid, i.e. extracting effective components or remove objectionable constituent selectively.Carbonic acid gas is a kind of non-polar solvent, for nonpolar small-molecule substance, have higher extraction yield as volatile small molecule materials such as the lower aliphatic acetoacetic esters such as ethyl hexanoate, ethyl lactate, ethyl acetate and alcohol, caproic acid, butyric acid, extraction yield is very low for the larger acidic substance of polarity or macromolecular substance such as higher fatty acid ethyl esters etc.Therefore can selectively extract needed effective constituent by the control of supercritical process parameter.
Summary of the invention
The purpose of this invention is to provide a kind of method of extracting high-ester flavouring liquid from the wine tail, utilize the method to extract the high Wine blending liquid of ethyl hexanoate content from this special wine tail, this Wine blending liquid ethyl hexanoate content is high, reaches 250g/L; Higher fatty acid ethyl esters content is few, is applicable to hook transfer low and middle-grade white wine, not only can not produce muddiness, and the cellar for storing things is fragrant pure, has the typical style of aromatic Chinese spirit.
The present invention extracts wine with the method for high-ester flavouring liquid from the wine tail, comprise the steps:
(1) selection of wine tail: selecting wine unstrained spirits fermentation period is the aromatic Chinese spirit fermentation pit of 4 to 6 months, and the wine unstrained spirits of selecting bottom, close Jiao Chi pond to divide, and the wine unstrained spirits obtains the lower concentration wine tail of alcoholic strength in 15%～20% scope through the distillation of rice steamer bucket.
(2) pre-treatment step of wine tail: with above-mentioned selected low boilers for low-proof wine standing demix, collect the floating oily matter in wine tail upper strata, obtain wine tail oily matter;
(3) extraction step: the wine tail oily matter of step 2 is placed in supercritical CO
2Extraction kettle in, regulating extraction kettle pressure is 7.5～8Mp, the extraction kettle temperature is 35～45 ℃; Extraction time is 1h～2h; Make that in the wine tail, the esters of gallic acid material is dissolved in supercritical CO
2In fluid;
(4) separating step: will carry the CO of esters of gallic acid material in step (3)
2Fluid successively enters separating still I and separating still II; Described separating still I pressure is 6.5～7Mp, and separating still I temperature is 35～40 ℃; Separating still II pressure is 4.5～5Mp, and separating still II temperature is 25～35 ℃, by reducing CO in separating still
2Pressure, make the esters of gallic acid material resolve in separating still; Collect the parsing thing of separating still II, this parsing thing is colourless transparent liquid, is high-ester flavouring liquid.
The parsing thing that obtains in separating still I in described step (4) is forwarded to carry out the cycling extraction separation in extraction kettle; To reach the high efficiente callback of active principle.
Foundation of the present invention and principle: the selected wine tail of the present invention be fermentation period the wine tail in the Chang Jiao pond of 4～6 months and only at the bottom of scavenger the wine unstrained spirits be object through the low boilers for low-proof wine of rice steamer bucket distillation.Thereby can improve and produce the ester ability in the cellar for storing things and improve vinosity owing to extending fermentation period, and at the bottom of the pond, in the wine unstrained spirits, the content of ester is just higher, especially the content of ethyl hexanoate is just higher.But by distillation, only have the part Ester to steam in former wine, most of flavour ingredient steams with the wine tail.
The alcohol number of degrees in general wine tail are 20 ° of left and right, and the component that in the wine tail, content is maximum is ethyl lactate, and content can reach the 10g/L left and right; The less ethyl hexanoate of content is because solubleness in the alcohol of 20 ° of left and right is extremely low, thereby with other hydrophobic components slowly polymerization together, separates out gradually, and floats on the water surface.This part material is wine tail oily matter.This oily matter is take ethyl hexanoate, caproic acid as main component, but still contain a large amount of long-chain components such as ethyl palmitate, and be directly used in to hook and transfer low and middle-grade wine, the impact because of the long-chain fat acetoacetic ester causes the wine body muddy, and assorted flavor is outstanding, makes this precious resources to use.For addressing this problem, the present invention utilizes supercritical extraction process to remove higher fatty acid ethyl esters.Ethyl hexanoate and higher fatty acid ethyl esters molecular weight differ larger in theory, thereby this two classes material is at supercritical CO
2In solubleness also have difference, according to this characteristic, by supercritical extraction method, ethyl hexanoate is separated with higher fatty acid ethyl esters; Thereby obtain the ethyl hexanoate Wine blending liquid of high density.
Therefore, the present invention chooses long Jiao Chi of solid state fermentation cycle, and it is high that such Jiao Chi produces ester content, and wine tail oily matter is more; Adopt supercritical CO
2Extraction process is removed the objectionable constituent in wine tail oily matter, keeps beneficiating ingredient, makes more than in extraction liquid, ethyl hexanoate content reaches 250g/L, and extraction liquid water white transparency, vinosity is strong, and the pure coordination of fragrance is used for the quality that wine blending can significantly promote white wine.This high-ester flavouring liquid extracts from the wine tail and obtains, and is natural microbial fermentation product, adopts again supercritical extraction process, has advantages of pure, safety, no solvent residue, meets the needs of food safety.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is the supercritical extraction process schema.
Fig. 3 is the gas chromatographic analysis figure of high-ester flavouring liquid after diluting 100 times.
Embodiment
Below in conjunction with accompanying drawing and example, the present invention is described in further detail:
Embodiment: extract the method for high-ester flavouring liquid from the wine tail of fermentation period than Chang Jiao pond production, carry out as follows:
(1) selection of wine tail: select fermentation period to grow the Jiao Chi of (being generally 4 months to 6 months), and the low boilers for low-proof wine of selecting to pluck through the distillation of rice steamer bucket near wine unstrained spirits at the bottom of the pond is object; Alcoholic strength is generally 15%～20%.
(2) pre-treatment step of wine tail: the special wine tail of plucking is placed in storage tank standing night, the floating oily matter in wine tail upper strata in storage tank is collected, obtain wine tail oily matter.
(3) extracting and separating step: adopt supercritical CO
2(this device comprises CO to extraction plant
2, ice chest storage tank, high-pressure pump etc. partly form) heavy constituent (higher fatty acid ethyl esters) and the light constituent (own ester, caproic acid etc.) of wine tail oily matter separated; As shown in Figure 2, the wine tail oily matter with step 2 is placed in supercritical CO
2Extraction kettle in, regulating extraction kettle pressure is 7.5～8Mp, the extraction kettle temperature is 35～45 ℃; Separating still I pressure is 6.5～7Mp, and separating still I temperature is 35～40 ℃; Separating still II pressure is 4.5～5Mp, and separating still II temperature is 25～35 ℃.Extraction time is 1h～2h.
(4) high-ester flavouring liquid (4) high-ester flavouring liquid is collected step: after extraction finishes, open the valve of separating still II, collect the parsing thing of separating still II, this parsing thing is colourless transparent liquid, is the high-ester flavouring liquid take ethyl hexanoate as main ingredient.This high-ester flavouring liquid water white transparency, extraction yield is more than 10%, and each component concentration is as shown in table 1.This extracting solution adopts gas-chromatography detection method, CP-WAX57CB capillary column 50m * 0.25mm that its chromatographic column adopting U.S. Varian Chrompack company produces * 0.20 μ m.Column temperature: the second order temperature programming, 35 ℃ of initial temperatures keep 2min, are raised to 100 ℃ with 4 ℃/min, then are raised to 210 ℃ with 10 ℃/min, keep 15min; 230 ℃ of injector temperatures; 240 ℃ of detector temperatures; Carrier gas: High Purity Nitrogen; Column cap is pressed: 120kPa; Post flow: 1.0mL/min; Sample size: the gas chromatographic analysis figure that 1 μ L, Fig. 3 are high-ester flavouring liquid after 100 times of dilutions, in figure from the left side first large peak value be the etoh solvent peak that diluted sample is used, the 2nd large peak value is the ethyl hexanoate peak, the 3rd large peak value is the caproic acid peak.
(5) extract remainder is collected step: after extraction finishes, open the valve of extraction kettle, collect the raffinate of extraction kettle, this extraction liquid color is scarlet, makes waste liquid and processes, and enters the anaerobic methane fermentation vat.
(6) recycling step of the parsing thing of separating still I: after extraction time arrives, open the valve of separating still I, collect the parsing thing of separating still I, still contain a large amount of flavour ingredients such as ethyl hexanoate in this parsing thing, this is resolved thing squeezes into extraction kettle from the entrainment agent pump again, carry out cycling extraction again, reach the high efficiente callback of active principle.
The component concentration of table 1 high-ester flavouring liquid
Claims (2)
1. one kind is extracted wine with the method for high-ester flavouring liquid from the wine tail, it is characterized in that comprising the steps:
(1) selection of wine tail: selecting wine unstrained spirits fermentation period is the aromatic Chinese spirit fermentation pit of 4 to 6 months, and the wine unstrained spirits of selecting bottom, close Jiao Chi pond to divide, and the wine unstrained spirits obtains the lower concentration wine tail of alcoholic strength in 15%～20% scope through the distillation of rice steamer bucket;
(2) pre-treatment step of wine tail: with above-mentioned selected low boilers for low-proof wine standing demix, collect the floating oily matter in wine tail upper strata, obtain wine tail oily matter;
(3) extraction step: the wine tail oily matter of step 2 is placed in supercritical CO
2Extraction kettle in, regulating extraction kettle pressure is 7.5～8Mp, the extraction kettle temperature is 35～45 ℃; Extraction time is 1h～2h; Make that in the wine tail, the esters of gallic acid material is dissolved in supercritical CO
2In fluid;
(4) separating step: will carry the CO of esters of gallic acid material in step (3)
2Fluid successively enters separating still I and separating still II; Described separating still I pressure is 6.5～7Mp, and separating still I temperature is 35～40 ℃; Separating still II pressure is 4.5～5Mp, and separating still II temperature is 25～35 ℃, by reducing CO in separating still
2Pressure, make the esters of gallic acid material resolve in separating still; Collect the parsing thing of separating still II, this parsing thing is colourless transparent liquid, is high-ester flavouring liquid.
2. a kind of wine that extracts from the wine tail according to claim 1 is with the method for high-ester flavouring liquid, it is characterized in that, the parsing thing that obtains in separating still I in described step (4) is forwarded to carry out the cycling extraction separation in extraction kettle, to reach the high efficiente callback of active principle.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104357299A (en) * | 2014-11-10 | 2015-02-18 | 江苏洋河酒厂股份有限公司 | Production method of high-acid high-ester flavoring liquor |
| CN106047577A (en) * | 2016-08-19 | 2016-10-26 | 四川远鸿小角楼酒业有限公司 | Method for producing flavor distilling wine blending liquid by using yellow water |
| CN109198578A (en) * | 2018-11-07 | 2019-01-15 | 广东石湾酒厂集团有限公司 | A method of high concentration esters blending liquor is prepared using soybean-flavor liquor by-product |
Citations (5)
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| SU889693A1 (en) * | 1979-06-07 | 1981-12-15 | Всесоюзный Заочный Институт Пищевой Промышленности | Method of producing brandy alcohol |
| CN1900262A (en) * | 2006-07-12 | 2007-01-24 | 四川省宜宾五粮液集团有限公司 | Method for extracting wine flavour and fragrance substance from wine tail by super critical CO2 extracting technology |
| CN1970722A (en) * | 2006-11-28 | 2007-05-30 | 李家民 | Supercritical CO2 extraction method for aromatic matter in brewed spirit solid |
| CN1990851A (en) * | 2005-12-30 | 2007-07-04 | 郑州轻工业学院 | Method of extracting lees residual distilled spirit fragrance component |
| RU2421510C1 (en) * | 2010-05-05 | 2011-06-20 | Общество с ограниченной ответственностью "Научно-внедренческое предприятие "Эффект-91" | Distillate production method |
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2012
- 2012-06-08 CN CN201210189220.4A patent/CN103146517B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU889693A1 (en) * | 1979-06-07 | 1981-12-15 | Всесоюзный Заочный Институт Пищевой Промышленности | Method of producing brandy alcohol |
| CN1990851A (en) * | 2005-12-30 | 2007-07-04 | 郑州轻工业学院 | Method of extracting lees residual distilled spirit fragrance component |
| CN1900262A (en) * | 2006-07-12 | 2007-01-24 | 四川省宜宾五粮液集团有限公司 | Method for extracting wine flavour and fragrance substance from wine tail by super critical CO2 extracting technology |
| CN1970722A (en) * | 2006-11-28 | 2007-05-30 | 李家民 | Supercritical CO2 extraction method for aromatic matter in brewed spirit solid |
| RU2421510C1 (en) * | 2010-05-05 | 2011-06-20 | Общество с ограниченной ответственностью "Научно-внедренческое предприятие "Эффект-91" | Distillate production method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104357299A (en) * | 2014-11-10 | 2015-02-18 | 江苏洋河酒厂股份有限公司 | Production method of high-acid high-ester flavoring liquor |
| CN104357299B (en) * | 2014-11-10 | 2016-08-24 | 江苏洋河酒厂股份有限公司 | A kind of production method of peracid ester flavouring wine |
| CN106047577A (en) * | 2016-08-19 | 2016-10-26 | 四川远鸿小角楼酒业有限公司 | Method for producing flavor distilling wine blending liquid by using yellow water |
| CN109198578A (en) * | 2018-11-07 | 2019-01-15 | 广东石湾酒厂集团有限公司 | A method of high concentration esters blending liquor is prepared using soybean-flavor liquor by-product |
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| CN103146517B (en) | 2014-07-16 |
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Owner name: ANHUI REITH WILL TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: GUJINGGONG SPIRITS CO., LTD., ANHUI PROV. Effective date: 20150908 |
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Effective date of registration: 20150908 Address after: 236820 Gujing Town, Bozhou City, Anhui Patentee after: ANHUI RUISIWEIER TECHNOLOGY CO., LTD. Address before: No. 26 236820 ancient town in Anhui province Bozhou City Qiaocheng District Three Avenue Patentee before: Gujinggong Spirits Co., Ltd., Anhui Prov. |