CN105925451B - A kind of green liquor deacidification and the method except fusel oil - Google Patents
A kind of green liquor deacidification and the method except fusel oil Download PDFInfo
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- CN105925451B CN105925451B CN201610395491.3A CN201610395491A CN105925451B CN 105925451 B CN105925451 B CN 105925451B CN 201610395491 A CN201610395491 A CN 201610395491A CN 105925451 B CN105925451 B CN 105925451B
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- extraction
- fusel oil
- green liquor
- deacidification
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
- C12G3/00—Preparation of other alcoholic beverages
- C12G3/08—Preparation of other alcoholic beverages by methods for altering the composition of fermented solutions or alcoholic beverages not provided for in groups C12G3/02 - C12G3/07
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
- C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
- C12H1/12—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation
- C12H1/16—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation
Abstract
The present invention provides a kind of green liquor deacidification and the method except fusel oil, comprises the following steps：S1 supercritical COs2Extraction：Green liquor is sent into supercritical CO2In device, raffinate is collected after extraction；The pressure of extraction be 8~15MPa, temperature be 20~35 DEG C, the time be 20~40min；S2 is parsed for the first time：CO after extraction2Fluid enters in the first extraction-container, and the pressure of parsing is 6~10MPa, and temperature is 15~22 DEG C, collects the first desorbed solution, and the first desorbed solution is incorporated into the raffinate, obtains deacidification and except the green liquor after fusel oil.The invention belongs to food processing technology field, the method that the present invention is provided deacidification and except fusel oil in the case where reducing loss of effective components, removed while realizing acid and fusel oil, it is easy to operate quick, pollutant component will not be introduced, obtained deacidification and except the green plum Quality of Liquors after fusel oil and in good taste.
Description
Technical field
The invention belongs to food processing technology field, more particularly to a kind of green liquor deacidification and the method except fusel oil.
Background technology
Green plum is also known as fruit plum, smoked plum, green plum not only rich in nutrition content, includes citric acid, tannic acid, sitosterol, Qi Dun
Tartaric acid and flavonoids isoreactivity composition, are typical basic foods, with regulation stomach, promote the production of body fluid to quench thirst, the function such as beautifying face and moistering lotion.
The characteristics of fresh green plum has peracid low sugar, sugar-acid ratio is about 0.2, and storage endurance should not eaten raw directly yet, is typical processing
Type fruit.
Green liquor is exactly one of main converted products of green plum, and unique flavor is cardiovascular, anti-ageing with anti-oxidant, protection
Wait for a long time effect.The preparation method of green liquor includes fermentation method and infusion method.Fermentation method：Fresh Green plum flesh is smashed, ferment is accessed
Thick wine is made in mother liquor for fermentation, is then made again by techniques such as precipitation, filtering, clarification, ageings.Infusion method：Using rice wine or Huang
Wine soaks fresh green plum, is then made through techniques such as precipitation, filtering, clarification, seasoning, ageings.Acidity and production by green plum
The influence of technique etc., especially the problem of obtained green liquor often has acidity and higher fusel oil, soak type green liquor.Leaching
The citric acid content of alveolitoid green liquor is usually 35g/L or so, and malic acid content is usually 5g/L or so, therefore acidity is higher,
Mouthfeel is drunk in influence.Fusel oil is carbon atoms 3 or the alcohols material of more than 3, is one of aroma-producing substance of drinks, including just
Propyl alcohol, isopropanol, isobutanol, isoamyl alcohol etc., mainly protein, amino acid are obtained by the reaction such as deamination, decarboxylation in raw material,
Content can produce harm when higher to nerve system of human body, cause " top " etc. to react.
The acid reduction method of green liquor mainly includes：Chemical acid lowering method, physics acid lowering method and bio-deacidification method.Chemical deacidification
Method：Using in the alkaline salt of addition and organic acid, so as to reduce acidity and improve mouthfeel.Chemical acid lowering method deacidification speed is fast,
Effect significantly, but easily has salts substances residual after deacidification, may influence the quality and stability of fruit wine.Physics acid lowering method：It is main
To include freezing processing, electrodialysis, ion-exchange etc., but the equipment for generally requiring specialty, operate cumbersome.Biological acid reduction
Method：Act on adjusting acid using the own metabolism of microorganism, this method often has selectivity, and metabolite is more difficult
Control.
Chinese patent 201310564272.X discloses a kind of green liquor deacidification and the method except fusel oil, using anion
Exchanger resin D314 deacidifications, 28kHz and 45kHz ultrasonic continuous alternate treatment remove fusel oil, the green liquor acidity after processing
There is the larger range of decrease with fusel oil content, but operating procedure is more complicated, and the cycle is longer.
The content of the invention
For solve problems of the prior art, inventor to deacidification and except fusel oil method carry out numerous studies,
Unexpected discovery：By using supercritical CO2Extraction, and analysis condition is controlled, the situation of active ingredient can retained
Under, while deacidification and except fusel oil.Based on above-mentioned discovery, so as to complete the present invention.
The purpose of the present invention will be further described in detail below reflect and description.
The present invention provides a kind of green liquor deacidification and the method except fusel oil, comprises the following steps：
S1 supercritical COs2Extraction：Green liquor is sent into supercritical CO2In device, raffinate is collected after extraction；Extraction
Pressure be 8~15MPa, temperature be 20~35 DEG C, the time be 20~40min；
S2 is parsed for the first time：CO after extraction2Fluid enters in the first extraction-container, and the pressure of parsing is 6~10MPa, temperature
Spend for 15~22 DEG C, collect the first desorbed solution, and the first desorbed solution is incorporated to the raffinate, obtain deacidification and except fusel oil after
Green liquor.
Supercritical CO2Extraction is using factors such as pressure and temperatures to supercritical CO2The influence of fluid solvent power and carry out thing
The separation of matter, has the advantages that safe noresidue.Using above-mentioned technical proposal, the CO after extraction2Have in fluid containing more
Composition is imitated, therefore, after being screened by many experiments, by controlling supercritical CO2Extraction and for the first time condition of parsing, are being reduced
Deacidification and except fusel oil in the case of loss of effective components, energy consumption is low, easy to operate quick, obtained deacidification and except fusel oil after
Green plum Quality of Liquors and in good taste, the loss of fragrance component is few.Supercritical CO2The time of extraction is unsuitable long, to reduce effectively
The loss of composition.Inventor has surprisingly found that, the supercritical CO after extraction2Fluid is in low pressure and low temperature (6~10MPa, 15~22
DEG C) under conditions of parsing can realize that the content of citric acid in the recovery of active ingredient, desorbed solution and fusel oil is low, i.e., in reality
Existing deacidification and the loss of active ingredient is reduced while except fusel oil.
Preferably, the pressure of the extraction be 10~15MPa, temperature be 28~32 DEG C, the time be 25~35min.It is more excellent
Selection of land, CO2The flow velocity of fluid is 180~240L/h.
It is highly preferred that the pressure of the extraction is 12MPa, temperature is 30 DEG C, the time is 30min.
Preferably, the pressure of first extraction-container is 7~9MPa, and temperature is 16~20 DEG C.The composition of first desorbed solution
Based on lactone component and aldehyde ketone constituents, the content of citric acid is few.
It is highly preferred that the pressure of first extraction-container is 8MPa, temperature is 18 DEG C.
Preferably, the green liquor is immersion green liquor.
Preferably, the present invention is provided green liquor deacidification and the method except fusel oil, also comprise the following steps：
Second of parsing of S3：CO after being parsed through first time2Fluid enters in the second extraction-container, and pressure is 4~6MPa, temperature
Spend for 30~40 DEG C, remove the second desorbed solution, reclaim CO2.Obtained desorbed solution is parsed for the second time with citric acid, isopropanol and different
Butanol etc. is main component.
Preferably, the pressure of second extraction-container is 5MPa, and temperature is 38 DEG C.
Preferably, the supercritical CO2Device includes the extraction column equipped with filler.It is highly preferred that filler is stainless steel ring.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention provides a kind of green liquor deacidification and except fusel oil
Method, by controlling supercritical CO2Extraction and for the first time condition of parsing, the deacidification in the case where reducing loss of effective components
Removed with while except fusel oil, realizing acid and fusel oil, it is easy to operate quick, pollutant component will not be introduced, obtained drop
Acid and except the green plum Quality of Liquors after fusel oil and in good taste, color and luster is good, and the loss of fragrance component is few.
Embodiment
Below by specific embodiment, the present invention is described in further detail.
In the present invention, the citric acid content of undressed soak type green liquor is 32.8mg/mL, and malic acid content is
5.2mg/mL, fusel oil content is 364.5mg/mL.
The green liquor deacidification of embodiment one and except fusel oil
Green liquor deacidification and the method except fusel oil, comprise the following steps：
S1 supercritical COs2Extraction：Soak type green liquor is sent into supercritical CO2In device, raffinate is collected after extraction；
The pressure of extraction be 12MPa, temperature be 30 DEG C, the time be 30min；CO2The flow velocity of fluid is 200L/h；
S2 is parsed for the first time：CO after extraction2Fluid enters in the first extraction-container, and the pressure of parsing is 8MPa, and temperature is
18 DEG C, the first desorbed solution is collected, and the first desorbed solution is incorporated to the raffinate, deacidification is obtained and except the green plum after fusel oil
Wine.
The green liquor deacidification of embodiment two and except fusel oil
Green liquor deacidification and the method except fusel oil, comprise the following steps：
S1 supercritical COs2Extraction：Soak type green liquor is sent into supercritical CO2In device, raffinate is collected after extraction；
The pressure of extraction be 14MPa, temperature be 28 DEG C, the time be 35min；CO2The flow velocity of fluid is 200L/h；
S2 is parsed for the first time：CO after extraction2Fluid enters in the first extraction-container, and the pressure of parsing is 9MPa, and temperature is
20 DEG C, the first desorbed solution is collected, and the first desorbed solution is incorporated to the raffinate, deacidification and the green liquor except fusel oil is obtained.
The green liquor deacidification of embodiment three and except fusel oil
Green liquor deacidification and the method except fusel oil, comprise the following steps：
S1 supercritical COs2Extraction：Soak type green liquor is sent into supercritical CO2In device, raffinate is collected after extraction；
The pressure of extraction be 12MPa, temperature be 30 DEG C, the time be 30min；CO2The flow velocity of fluid is 200L/h；
S2 is parsed for the first time：CO after extraction2Fluid enters in the first extraction-container, and the pressure of parsing is 8MPa, and temperature is
18 DEG C, the first desorbed solution is collected, and the first desorbed solution is incorporated to the raffinate, deacidification and the green liquor except fusel oil is obtained；
Second of parsing of S3：CO after being parsed through first time2Fluid enters in the second extraction-container, and pressure is 5MPa, temperature
For 38 DEG C, the second desorbed solution is removed, CO is reclaimed2。
After testing, the citric acid content in the first desorbed solution is higher, obtained deacidification and except in the green liquor after fusel oil
Citric acid content be 5.7mg/mL, malic acid content is 0.9mg/mL, and fusel oil content is 143.0mg/mL, deacidification and removal of impurities
Green liquor after alcohol oil accounts for the 97.5% of before processing soak type green liquor volume.Ethyl acetate content in second desorbed solution is
32.9mg/mL, fragrance component loss is less.
The green liquor deacidification of comparative example one and except fusel oil
Green liquor deacidification and the method except fusel oil, comprise the following steps：
S1 supercritical COs2Extraction：Soak type green liquor is sent into supercritical CO2In device, raffinate is collected after extraction,
Obtain deacidification and the green liquor except fusel oil；The pressure of extraction be 12MPa, temperature be 30 DEG C, the time be 30min；CO2Fluid
Flow velocity is 200L/h；
S2 is parsed：CO after extraction2Fluid enters in extraction-container, and the pressure of parsing is 5MPa, and temperature is 38 DEG C, removes solution
Liquid is analysed, CO is reclaimed2。
The difference of this comparative example and embodiment three is essentially consisted in：Lack the step of parsing for the first time.After testing, the drop obtained
Acid and except the citric acid content in the green liquor after fusel oil be 8.4mg/mL, malic acid content is 1.5mg/mL, and fusel oil contains
Measure for 152.9mg/mL, deacidification and except the green liquor after fusel oil accounts for the 93.6% of before processing soak type green liquor volume.Parsing
Ethyl acetate content in liquid is 172.1mg/mL, and fragrance component loss is more.
The green liquor deacidification of comparative example two and except fusel oil
Green liquor deacidification and the method except fusel oil, comprise the following steps：
S1 supercritical COs2Extraction：Soak type green liquor is sent into supercritical CO2In device, raffinate is collected after extraction；
The pressure of extraction be 12MPa, temperature be 30 DEG C, the time be 30min；CO2The flow velocity of fluid is 200L/h；
S2 is parsed for the first time：CO after extraction2Fluid enters in the first extraction-container, and the pressure of parsing is 8MPa, and temperature is
25 DEG C, the first desorbed solution is collected, and the first desorbed solution is incorporated to the raffinate, deacidification and the green liquor except fusel oil is obtained；
Second of parsing of S3：CO after being parsed through first time2Fluid enters in the second extraction-container, and pressure is 5MPa, temperature
For 38 DEG C, the second desorbed solution is removed, CO is reclaimed2。
The difference of this comparative example and embodiment three is essentially consisted in：The temperature of parsing is changed into 25 DEG C from 18 DEG C for the first time.Through inspection
Survey, the citric acid content in the first desorbed solution is higher, obtained deacidification and except the citric acid content in the green liquor after fusel oil
For 12.4mg/mL, malic acid content is 1.9mg/mL, and fusel oil content is 171.3mg/mL, deacidification and except the green grass or young crops after fusel oil
Plum wine accounts for the 97.8% of before processing soak type green liquor volume.Ethyl acetate content in second desorbed solution is 57.1mg/mL, fragrant
Gas component damages are less.
The evaluation of test example green liquor
Invite and evaluate the people of expert 15 of experience, the people of ordinary consumer 45 as evaluation personnel with fruit wine, evaluation personnel with
Machine is divided into 3 groups (two groups of three groups of embodiment, one group of comparative example and comparative examples), and every group includes the people of expert 5 and the people of ordinary consumer 15,
The deacidification that is obtained respectively to embodiment three, comparative example one and comparative example two and except the green liquor of fusel oil is evaluated and is given a mark,
Without exchange between evaluation personnel, evaluation index includes color and luster, mouthfeel, fragrance, total satisfactory grade, and each evaluation index expires
It is divided into 100 points, evaluation result is as shown in table 1 to table 3.
Deacidification and the green liquor evaluation result table except fusel oil that the embodiment three of table 1 is obtained
| Evaluation index | Average |
| Color and luster | 92 |
| Mouthfeel | 91 |
| Fragrance | 95 |
| Total satisfactory grade | 94 |
Deacidification and the green liquor evaluation result table except fusel oil that the comparative example one of table 2 is obtained
| Evaluation index | Average |
| Color and luster | 93 |
| Mouthfeel | 81 |
| Fragrance | 76 |
| Total satisfactory grade | 79 |
Deacidification and the green liquor evaluation result table except fusel oil that the comparative example two of table 3 is obtained
| Evaluation index | Average |
| Color and luster | 91 |
| Mouthfeel | 84 |
| Fragrance | 87 |
| Total satisfactory grade | 85 |
It was found from table 1 to table 3, deacidification that the embodiment of the present invention is obtained and except the green liquor of fusel oil is in color and luster, mouthfeel, perfume (or spice)
Higher evaluation is all obtained in terms of taste, total satisfactory grade, comparative example one is substantially better than in terms of mouthfeel, fragrance and total satisfactory grade
The deacidification obtained with comparative example two and the green liquor except fusel oil.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (6)
1. a kind of green liquor deacidification and the method except fusel oil, it is characterised in that：It is made up of following steps：
S1, supercritical CO2Extraction：Green liquor is sent into supercritical CO2In device, raffinate is collected after extraction；The pressure of extraction
Be 28~32 DEG C for 10~15MPa, temperature, the time be 25~35min；
S2, for the first time parsing：CO after extraction2Fluid enters in the first extraction-container, and the pressure of parsing is 8MPa, and temperature is 18 DEG C,
The first desorbed solution is collected, and the first desorbed solution is incorporated to the raffinate, deacidification is obtained and except the green liquor after fusel oil.
2. green liquor deacidification according to claim 1 and the method except fusel oil, it is characterised in that：The pressure of the extraction
Be 30 DEG C for 12MPa, temperature, the time be 30min.
3. green liquor deacidification according to claim 1 and the method except fusel oil, it is characterised in that：The green liquor is leaching
Steep green liquor.
4. green liquor deacidification according to any one of claim 1 to 3 and the method except fusel oil, it is characterised in that：Also
Comprise the following steps：
S3, second of parsing：CO after being parsed through first time2Fluid enters in the second extraction-container, and pressure is 4~6MPa, and temperature is
30~40 DEG C, the second desorbed solution is removed, CO is reclaimed2。
5. green liquor deacidification according to claim 4 and the method except fusel oil, it is characterised in that：Second extraction-container
Pressure be 5MPa, temperature be 38 DEG C.
6. green liquor deacidification according to claim 1 and the method except fusel oil, it is characterised in that：The supercritical CO2Dress
Put including the extraction column equipped with filler.
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| CN201610395491.3A CN105925451B (en) | 2016-06-06 | 2016-06-06 | A kind of green liquor deacidification and the method except fusel oil |
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| CN201610395491.3A CN105925451B (en) | 2016-06-06 | 2016-06-06 | A kind of green liquor deacidification and the method except fusel oil |
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| CN105925451B true CN105925451B (en) | 2017-08-25 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103571729A (en) * | 2013-11-14 | 2014-02-12 | 广东嘉豪食品股份有限公司 | Method for reducing acid and removing fusel oil of plum wine |
| CN104531433A (en) * | 2014-12-10 | 2015-04-22 | 惠州学院 | Method for increasing aroma of litchi liquor with help of supercritical CO2 fluid |
-
2016
- 2016-06-06 CN CN201610395491.3A patent/CN105925451B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103571729A (en) * | 2013-11-14 | 2014-02-12 | 广东嘉豪食品股份有限公司 | Method for reducing acid and removing fusel oil of plum wine |
| CN104531433A (en) * | 2014-12-10 | 2015-04-22 | 惠州学院 | Method for increasing aroma of litchi liquor with help of supercritical CO2 fluid |
Non-Patent Citations (1)
| Title |
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| 青梅酒降酸的阴离子交换树脂选择及动力学研究;高敏等;《食品与发酵工业》;20090630(第06期);全文 * |
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