CN101475889B - Method for extracting spirit natural fermentation by-product by supercritical carbon dioxide - Google Patents
Method for extracting spirit natural fermentation by-product by supercritical carbon dioxide Download PDFInfo
- Publication number
- CN101475889B CN101475889B CN2009103003157A CN200910300315A CN101475889B CN 101475889 B CN101475889 B CN 101475889B CN 2009103003157 A CN2009103003157 A CN 2009103003157A CN 200910300315 A CN200910300315 A CN 200910300315A CN 101475889 B CN101475889 B CN 101475889B
- Authority
- CN
- China
- Prior art keywords
- product
- extracting
- carbon dioxide
- supercritical carbon
- spirit
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The invention relates to a method for extracting white spirit natural fermentation byproducts through supercritical carbon dioxide, which belongs to the field of reclaiming of the white spirit fermentation byproducts. The technical problem to be solved by the invention is to provide the method for extracting the white spirit natural fermentation byproducts through the supercritical carbon dioxide with good separation effect. The method for extracting the white spirit natural fermentation byproducts through the supercritical carbon dioxide comprises the steps of extraction, primary separation, secondary separation and the like. The method has good separation effect, can realize continuous production, improves the production efficiency, and has wide application prospect.
Description
Technical field
The present invention relates to the method for extracting spirit wild fermentation by-product by supercritical carbon dioxide, belong to the recovery field of liquor fermentation by product.
Background technology
Supercritical CO
2As a kind of novel extraction solvent, it has, and dissolving power is good, the extraction time is short, nontoxic, pollution-free, no solvent residue, extraction temperature lower (near room temperature), safe in utilization, multiple advantage such as cost is low, therefore, and supercritical CO in recent years
2Abstraction technique is all being obtained very big progress aspect the degree of depth of fundamental research and practical application and the range.
Spirit wild fermentation by-product be rich in acid, ester, alcohol, aldehyde etc. special be fragrance matter, for a long time, each brewery generally to the liquid by product as: yellow waters etc. are recycled with distillation method, but its utilization ratio is lower, solid by-product then uses as feed as: vinasse etc., and the fragrance matter that is wherein can not get effective utilization.In recent years, along with supercritical CO
2The development of abstraction technique has the employing supercritical CO
2Abstraction technique is to being that fragrance matter extracts, isolating relevant report in the spirit wild fermentation by-product.
As: the patent application of CN1970722 discloses the supercritical CO of fragrance matter in a kind of brewed spirit solid thing
2Extracting process, this method key step comprise that extraction, flash trapping stage, secondary separate, three grades of separation, during soon the brewed spirit solid thing will be packed extraction kettle into, pump into supercritical CO
2Fluid also adds the edible ethanol entrainment agent, and the pressure of rising extraction kettle extracts, and regulates different pressure and temperatures then respectively and carries out one, two, three separation and obtain isolate.But this method can not realize continuous production, and production efficiency is low; This method separating effect is relatively poor, and the purity of flash trapping stage gained Ester is lower, and two, three grades of separation gained acid content are on the low side.
Summary of the invention
Technical problem to be solved by this invention provides a kind of separating effect method of extracting spirit wild fermentation by-product by supercritical carbon dioxide preferably.
The method of extracting spirit wild fermentation by-product by supercritical carbon dioxide comprises the steps:
A, extraction: heating, pressurization CO
2, make CO
2Reach supercritical state, the raw material spirit wild fermentation by-product enters in the column extractor and supercritical CO
2Carry out counter-current extraction, obtain extraction product and raw material waste liquid, wherein, during counter-current extraction, supercritical CO
2Flow be 6～7t/h, pressure is 18～24Mpa, the preferred 20Mpa of pressure;
B, flash trapping stage: extraction product enters the parsing post, and the pressure that post is resolved in control is 6.5～7.0Mpa, and resolving the column top temperature is 40～50 ℃, and temperature of lower is 25～30 ℃, and heating parsing column bottom, obtains resolving product 1 and CO
2Fluid; Resolve product 1 and be mainly Ester and other flavour ingredient;
C, secondary separate: CO
2Fluid is heated to 50～55 ℃, and control pressure and CO
2Storage tank keeps balance, is 4.0～4.5Mpa generally speaking, enters separating still then and resolves, and obtains resolving product 2 and CO
2Gas.Resolve product 2 and be mainly acid.CO
2After heating of fluid process and the decompression, CO
2Residual organic in the fluid is because CO
2Solubleness reduces and all separates in separating still.
Wherein, above-mentioned spirit wild fermentation by-product is at least a in yellow water, wine tail, the residual water.
Further, in order to save cost, the method for above-mentioned extracting spirit wild fermentation by-product by supercritical carbon dioxide also comprises the steps:
D, CO
2The recovery of gas: CO
2Gas is recycled after being liquid state through condenser condenses.
Wherein, the column extractor in the above-mentioned a step is that conventional column extractor gets final product, and that the stopping composition in the column extractor need meet is high temperature resistant, high pressure and acidproof requirement.
Further, in order to realize continuous production, also be provided with liquidometer in the column extractor in a step with liquid level in the automatic control column extractor, and the raw material waste liquid is at the uniform velocity discharged.Raw material discharging of waste liquid excessive velocities then can be wasted CO
2And the increase cost, raw material discharging of waste liquid speed is crossed slowly and then can be reduced production efficiency, and the height of the column extractor described in a step is preferably 1200mm, and when liquidometer control liquid level was 1150mm, discharging of waste liquid speed was preferably 360kg/h.
Further, more even for the parsing post is heated, the b step is preferably resolved the column bottom with 100～120 ℃ steam heating.
Further, for the flash trapping stage better effects if, the pressure of resolving post in the b step is preferably 6.8Mpa, resolves the column top temperature and is preferably 45 ℃, resolves the post temperature of lower and is preferably 27 ℃.
The beneficial effect of the inventive method is: the inventive method can realize continuous production, has improved production efficiency; The inventive method separating effect is better, fragrance matter extraction yield height such as ester, acid, the purity of flash trapping stage gained Ester higher (being about 90%), the separating obtained acid content of secondary height; The separating obtained parsing product 1 of the inventive method is conciliate division product 2 and is added the whole local flavor that can significantly improve finished wine in the finished wine, and it is given off a strong fragrance, and aftertaste is more sweet.
Description of drawings
Fig. 1 is the process flow sheet of the inventive method.
1 is raw material among the figure, and 2 is raw material storage tank, and 3 is feeding pump, 4 is column extractor, and 5 is waste tank, and 6 is the waste liquid remover, 7 is primary heater, and 8 for resolving post, and 9 for resolving product 1 storage tank, 10 for resolving product 1 remover, and 11 is well heater, and 12 is separating still, 13 for resolving product 2 storage tanks, 14 for resolving product 2 removers, and 15 is main condenser, and 16 is CO
2Storage tank, 17 is main high-pressure pump.
Embodiment
Below in conjunction with embodiment the specific embodiment of the present invention is further described, does not therefore limit the present invention among the described scope of embodiments.
Embodiment 1 adopts the fragrance matter that is in the inventive method extraction yellow water
The high 12.2m of the used column extractor of present embodiment, the stopping composition in the column extractor is a stainless steel ring, the design pressure of column extractor is 25Mpa.
Process flow sheet as shown in Figure 1, CO
2By CO
2Storage tank bottom under meter enters main high-pressure pump and boosts to 20Mpa, is heated to 55 ℃ through primary heater, makes CO
2Reach supercritical state.The raw material yellow water is entered in the column extractor from column extractor top by feeding pump through the raw material storage tank heated and stirred, simultaneously, and supercritical CO
2Enter from the column extractor bottom, carry out counter-current extraction.Supercritical CO
2Flow control is 6～7t/h, and pressure is 20Mpa.The liquidometer control liquid level that the column extractor top is provided with is 1150mm, and the raw material waste liquid is put to waste tank from the column extractor bottom valve, got rid of by the waste liquid remover, and control discharging of waste liquid flow is 360kg/h again.Extraction product is by supercritical CO
2The dissolving back is taken out of from the top, by the variable valve expenditure and pressure, enters the parsing post from the middle part.
Resolve post control pressure 6.8Mpa, resolving the column top temperature is 45 ℃, and resolving the post temperature of lower is 27 ℃, at this moment, the control vapor temperature is 100～120 ℃, and the column bottom is resolved in heating, separate out and resolve product 1 and put to resolving product 1 storage tank, get rid of through resolving product 1 remover then by valve.CO
2Fluid enters well heater through the automatic regulating valve expenditure and pressure and changes and be heated to about 52 ℃ from resolving the column top, enters separating still then.
The separating still temperature is controlled at about 52 ℃, pressure and CO
2Storage tank keeps balance, is 4.2Mpa.CO after the heating
2Fluid enters from separating still top, makes CO
2After residual organic heats through decompression in the fluid, because CO
2Solubleness reduces and all carries out secondary and resolve and separate in separating still, obtains resolving product 2 and puts to resolving product 2 storage tanks by valve, gets rid of through resolving product 2 removers then.
The high temperature CO of coming out by the separating still top
2Gas turns back to CO after being condensed into liquid state through main condenser
2Storage tank recycles.
After testing, the main chemical compositions and the content of resolving product 1 see Table 1, and the main chemical compositions and the content of resolving product 2 see Table 2.
Table 1 is resolved the main chemical compositions and the content of product 1
| Chemical ingredients | Content (mg/ml) | Extraction yield |
| 3-hydroxyl-2-butanone | 96.28 | 95.30％ |
| Ethyl lactate | 1949.97 | 86.10％ |
| 2,3-top glycol (meso) | 64.16 | 65.30％ |
| Bata-phenethyl alcohol | 12.41 | 91.00％ |
Detected result shows to resolve in the product 1 and contains acid hardly.
Table 2 is resolved the main chemical compositions and the content of product 2
| Chemical ingredients | Content (mg/ml) | Extraction yield |
| Acetate | 612.66 | 56.70％ |
| Butyric acid | 5335.79 | 75.20％ |
| Caproic acid | 44006.40 | 95.00％ |
| Lactic acid | 1430.47 | 92.00％ |
Detected result shows to resolve in the product 2 and contains Ester hardly.
In a word, the inventive method separating effect is better, and each component extraction yield height is resolved the product purity height in addition, can directly add to be adjusted to the local flavor of sampling wine in the finished wine.
Claims (8)
1. the method for extracting spirit wild fermentation by-product by supercritical carbon dioxide comprises the steps:
A, extraction: heating, pressurization CO
2, make CO
2Reach supercritical state, the raw material spirit wild fermentation by-product enters in the column extractor and supercritical CO
2Carry out counter-current extraction, obtain extraction product and raw material waste liquid, wherein, during counter-current extraction, supercritical CO
2Flow be 6～7t/h, pressure is 18～24Mpa;
B, flash trapping stage: extraction product enters the parsing post, and the pressure that post is resolved in control is 6.5～7.0Mpa, and resolving the column top temperature is 40～50 ℃, and temperature of lower is 25～30 ℃, and heating parsing column bottom, obtains resolving product 1 and CO
2Fluid;
C, secondary separate: CO
2Fluid is heated to 50～55 ℃, and control pressure is 4.0～4.5Mpa and and CO
2Storage tank keeps balance, enters separating still then and resolves, and obtains resolving product 2 and CO
2Gas.
2. the method for extracting spirit wild fermentation by-product by supercritical carbon dioxide according to claim 1 is characterized in that: also comprise the steps: d, CO
2The recovery of gas: CO
2Gas is recycled after being liquid state through condenser condenses.
3. the method for extracting spirit wild fermentation by-product by supercritical carbon dioxide according to claim 1, it is characterized in that: described spirit wild fermentation by-product is at least a in yellow water, wine tail, the residual water.
4. the method for extracting spirit wild fermentation by-product by supercritical carbon dioxide according to claim 1 is characterized in that: also be provided with liquidometer in the column extractor in a step.
5. the method for extracting spirit wild fermentation by-product by supercritical carbon dioxide according to claim 4, it is characterized in that: the height of the column extractor described in a step is 1200mm, liquidometer control liquid level is 1150mm, and discharging of waste liquid speed is 360kg/h.
6. the method for extracting spirit wild fermentation by-product by supercritical carbon dioxide according to claim 1 is characterized in that: in a step during counter-current extraction pressure be 20Mpa.
7. the method for extracting spirit wild fermentation by-product by supercritical carbon dioxide according to claim 1 is characterized in that: the heating of the described parsing of b step column bottom is to adopt 100～120 ℃ steam heating.
8. the method for extracting spirit wild fermentation by-product by supercritical carbon dioxide according to claim 1 is characterized in that: the pressure of resolving post in the b step is 6.8Mpa, and resolving the column top temperature is 45 ℃, and resolving the post temperature of lower is 27 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103003157A CN101475889B (en) | 2009-01-22 | 2009-01-22 | Method for extracting spirit natural fermentation by-product by supercritical carbon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103003157A CN101475889B (en) | 2009-01-22 | 2009-01-22 | Method for extracting spirit natural fermentation by-product by supercritical carbon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101475889A CN101475889A (en) | 2009-07-08 |
| CN101475889B true CN101475889B (en) | 2011-05-04 |
Family
ID=40836667
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009103003157A Active CN101475889B (en) | 2009-01-22 | 2009-01-22 | Method for extracting spirit natural fermentation by-product by supercritical carbon dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101475889B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321508B (en) * | 2011-09-01 | 2013-09-25 | 泸州品创科技有限公司 | Recycling method of pot-bottom water |
| CN112391259A (en) * | 2020-11-30 | 2021-02-23 | 湖南汉华京电清洁能源科技有限公司 | Edible white spirit processing method and processing device |
| CN113332741B (en) * | 2021-06-17 | 2023-02-10 | 四川剑南春（集团）有限责任公司 | Method for extracting acid substances in brewing tail water |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031110A (en) * | 1987-07-22 | 1989-02-15 | 农业合作公司 | The method and apparatus and the application thereof of fermentation |
| 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 |
-
2009
- 2009-01-22 CN CN2009103003157A patent/CN101475889B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031110A (en) * | 1987-07-22 | 1989-02-15 | 农业合作公司 | The method and apparatus and the application thereof of fermentation |
| CN1990851A (en) * | 2005-12-30 | 2007-07-04 | 郑州轻工业学院 | Method of extracting lees residual distilled spirit fragrance component |
| CN1970722A (en) * | 2006-11-28 | 2007-05-30 | 李家民 | Supercritical CO2 extraction method for aromatic matter in brewed spirit solid |
Non-Patent Citations (2)
| Title |
|---|
| 宋柯等.白酒发酵副产物丢糟、黄水、底锅水中提取香味成分在酒用香料中的应用.《酿酒科技》.2008,(第6期), * |
| 王国春等.利用超临界CO_2萃取技术从酿酒副产物中提取酒用呈香呈味物质的研究.《酿酒科技》.2008,(第1期), * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101475889A (en) | 2009-07-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101643796A (en) | Method for utilizing straw biomass by grades | |
| CN107129870A (en) | A kind of comprehensive method for extracting aroma component in agalloch eaglewood | |
| CN109294893B (en) | Resource utilization system and method for white spirit brewing byproduct yellow water | |
| CN108822967A (en) | A kind of preparation process of agilawood essential oil | |
| CN204702730U (en) | A kind of Novel steam distillation unit for liquor production by liquid fermentation | |
| CN108531342A (en) | A kind of production method and equipment of the neutral edible product that brews alcohol | |
| CN101475889B (en) | Method for extracting spirit natural fermentation by-product by supercritical carbon dioxide | |
| CN103013748A (en) | Brewing process of white wine | |
| CN101074258B (en) | Method for separating and extracting phytosterin and Vitamin E from soyabean deodorization distillate | |
| CN100441675C (en) | Method of extracting lees residual distilled spirit fragrance component | |
| CN102925311A (en) | Production method of grape wine | |
| CN1970722B (en) | Supercritical CO2 extraction method for aromatic matter in brewed spirit solid | |
| CN1900263A (en) | Method for extracting wine flavour and fragrance substance from yellow water by super critical CO2 technology | |
| CN102010357A (en) | Method for refining lutein by supercritical extraction | |
| Chetrariu et al. | Pre-treatments used for the recovery of brewer’s spent grain—A minireview | |
| CN100447230C (en) | Method for extracting wine flavour and fragrance substance from solid white spirit brewing semiproduct and by-product | |
| CN103146517B (en) | Method for extracting high-ester seasoning liquid from after-run | |
| CN102942445A (en) | Alcohol differential distillation production method | |
| CN101381279B (en) | Fuel ethanol dehydration apparatus and method | |
| CN110981696A (en) | Process and system for producing fuel ethanol by using double-coarse single-fine three-tower distillation low-concentration fermented mash | |
| US20100167367A1 (en) | Ethanol recovery system for cellulosic feedstocks | |
| CN107739655A (en) | A kind of microalgae grease extraction and separation method, equipment and application | |
| CN209243063U (en) | A kind of resource utilization system of brewed spirit by-product yellow water | |
| CN211522068U (en) | System for producing fuel ethanol by using double-coarse single-fine three-tower distillation low-concentration fermented mash | |
| CN100415866C (en) | Method for extracting wine flavour and fragrance substance from wine tail by super critical CO2 extracting technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |