CN112094720A

CN112094720A - System and method for accelerating aging and purifying wine by supercritical fluid fractionation technology

Info

Publication number: CN112094720A
Application number: CN202010036598.5A
Authority: CN
Inventors: 林士尧
Original assignee: Minnan Normal University
Current assignee: Minnan Normal University
Priority date: 2020-01-14
Filing date: 2020-01-14
Publication date: 2020-12-18

Abstract

The invention discloses a system and a method for accelerating aging and purifying wine by supercritical fluid fractionation technology, wherein a supercritical solvent is introduced into wine, the wine is mixed by an extraction tank and then is input into a reaction tank, so that alcohols and organic acid in the wine are subjected to esterification reaction by using lipase in the reaction tank to synthesize lipid compounds in wine beverage, and finally the lipid compounds are rapidly separated and purified in a separation tank by a fractionation tank, so that the standardization of qualitative and quantitative wine compounds can be realized. The invention uses supercritical carbon dioxide to extract the fragrant component reactant in the immature wine, and then uses the supercritical carbon dioxide to carry out esterification, so as to improve the ester component concentration of the koji wine, shorten the maturation time, improve the fragrance and the taste of the wine, and uses the fractionation technology to separate and purify the wine compounds according to the requirements, thereby producing high-quality koji wine new products and distilled wine, removing harmful low-boiling point substances and other undesirable components, shortening the manufacturing process, improving the plant health care effect, and conforming to the healthy consumption trend of times.

Description

System and method for accelerating aging and purifying wine by supercritical fluid fractionation technology

Technical Field

The invention relates to a device and a method for ripening and purifying wine, in particular to a system and a method for ripening and purifying wine by supercritical fluid fractionation technology.

Background

Esterification and ripening of wine

The liquor just distilled contains toxic Aldehydes (Aldehydes) and non-ethanol Alcohols (Fusel Alcohols) besides alcohol (ethanol), has unpleasant odor and taste such as pungent and pungent taste, is harmful to human health and low in public acceptance, needs to be stored to reduce irritation and pungent taste, and removes harmful substances, and the process is called ripening. The definition of ripening refers to that the taste of the wine changes from mild stimulation to mild, the fragrance is increased and the taste is more harmonious during the storage process of the new wine after the primary distillation, and the organic acid and the alcohol substances in the wine form ester compounds with fragrance due to esterification reaction during the storage process.

The aging process of wine mainly comprises removing aldehydes and forming organic acids and esters with special fragrance. During the curing process, a series of oxidation effects can be generated due to the action of alcohol and oxygen, the alcohol is oxidized into aldehyde, the aldehyde is oxidized into acid, the acid is esterified with ethanol to generate fragrant ethyl ester, and the alcohol and the aldehyde are condensed to synthesize acetal, so that the whole body reaches a new balance. The addition of organic acids and esters in the wine can improve the fragrance of the wine and make the wine mellow in taste.

Wines are ripened in many ways, most often and most time-consuming "cellaring", i.e. natural ripening, with the disadvantage of requiring a lot of time and space for storage. Because the esterification reaction rate of the higher alcohol and the acetic acid is very slow, the higher alcohol and the acetic acid are generally cellared for more than five years. Therefore, in recent years, there are other methods for performing artificial ripening by means of high-pressure homogenization, temperature, microwave, ultrasonic wave, etc., which are as follows:

1. high pressure homogeneous ripening method

The high-pressure homogenization has three effects of shearing force, impact force, cavitation and the like, can crush and refine the sample, change the particle size of the sample and the rheological property of sample particles, and also change a plurality of physical properties such as surface potential, conductivity, interfacial tension and the like. It promotes the ripening of alcoholic beverages by vigorously stirring and dispersing air.

2. Ultrasonic maturation method

Ultrasonic waves have the advantages of strong shearing force, particle breakage, increased heat transfer, mass transfer and cavitation, and are widely used in food processing. The ultrasonic wave accelerates the movement of water molecules in the wine, promotes the association of the water molecules and the ethanol molecules, reduces the clustering of the water molecules and the ethanol molecules and is more compact, so that the irritation and the spicy taste of the ethanol molecules are reduced, and the wine is more fragrant and smooth.

3. Microwave ripening method

The microwave energy generates high-frequency oscillation to destroy the original association structure of water molecules and ethanol molecules in the wine body, and the water molecules and the ethanol molecules are associated into a stable molecular group again; after the wine body absorbs microwave energy, the internal energy of the molecules is increased, and the reactions of oxidation reduction, esterification and the like are accelerated, so that the aim of accelerating ripening is fulfilled.

4. Heating ripening method

The high temperature can increase the intermolecular kinetic energy and accelerate the esterification reaction. The fresh feeling and the fruit fragrance of the new wine can be kept after low-temperature ripening.

5. Nano gold ripening method

The gold has the characteristics of high oxidation resistance and high corrosion resistance, so the gold is regarded as a passive metal with very low activity, and the catalytic activity of the nano gold can accelerate the synthesis of an aroma component, namely ethyl acetate, in the wine so as to achieve the effect of accelerating maturation.

6. Electrocatalytic ripening

Electrocatalysis generally uses a set of catalytically active electrodes, and when a current passes through the electrodes, electron transfer phenomena and chemical and physical changes of some substances occur between the electrodes and the solution interface. Electrons are used as oxidation reducing agent to accelerate the reactions of oxidation, reduction, association, esterification and the like in the ripening process.

7. Infrared ray

Infrared is an electromagnetic wave, and there are two mechanisms for accelerating ripening: firstly, a large amount of energy is provided to raise the temperature of the wine; secondly, when the frequency of radiation is the same as the frequency of wine molecules, resonance absorption can occur, so that molecules such as ethanol or water and the like are subjected to strong vibration and rotation, ethanol molecules, water molecules and other polar molecules are excited, hydrogen bonds connecting the ethanol molecules, the water molecules and the other polar molecules are destroyed to become free-state molecules, the re-association probability is increased, and the repeated operation is carried out, so that a stable association molecule group is formed, the chemical stability of the wine body is further improved, the pungency is reduced, the fragrance in the wine is improved, and the purpose of ripening is achieved.

8. Supercritical carbon dioxide extraction technology

Carbon dioxide is a colorless, nontoxic and nonflammable substance, can be recovered after extraction, cannot damage nature, has low critical pressure and temperature, and can save a large amount of energy. The technology is used for accelerating the conversion of the esterification reaction of the wine, so that ester substances are gradually accumulated to generate mellow taste, and trace fusel, hetero ketone, hetero aldehyde, furan aldehyde and other health-harming components which are easy to cause hangover and headache can be reduced or removed, and the technology has obvious effects on improving the quality and shortening the maturation time. Can greatly improve the wine ripening technology.

9. Esterification reaction catalyzed by lipase

The esterification is a process of reacting an organic acid with an alcohol to remove a molecule of water and produce an ester compound having a relatively small molecular weight. Lipase is an important biocatalyst with potential applications in the field of biotechnology, and recently, lipase has been widely used with the progress of biotechnology and the development of new functions. In organic solvent (including supercritical fluid), reverse hydrolysis reaction can be catalyzed, such as esterification, cross-esterification, ammonolysis, cross-thioesterification and peptization, so the lipase has wide application.

Purification and separation of wine

Besides the aging method, the separation and purification technique is also important key. Although the latest transesterification technology can achieve high conversion rate in a short time, the wine must be further purified and separated, and the standardization of the wine can be qualitatively and quantitatively determined. CN101591612A discloses a method and an apparatus for aging wine, which utilizes supercritical technology to promote the aging of wine, but does not relate to the further purification of wine. There are no other reports on the apparatus and method of purification.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provides a system and a method for accelerating aging and purifying wine by a supercritical fluid fractionation technology, wherein esterification is carried out by supercritical carbon dioxide to shorten the aging time, improve the fragrance and the taste of the wine, remove harmful substances with low boiling point and other undesirable components, shorten the manufacturing process, and purify ester compounds from the aged mixed wine by the supercritical carbon dioxide fractionation technology, so that the fragrance and the taste of the wine can be improved, the cellaring time is shortened, and the quality of the wine is improved.

One of the technical schemes adopted by the invention for solving the technical problems is as follows:

a system for accelerating aging and purifying wine by supercritical fluid fractionation technology comprises:

an extraction tank, which comprises a tank body, a raw material leading-in device and a supercritical fluid leading-in device, wherein the raw material leading-in device is used for leading the raw material into the tank body of the extraction tank, the supercritical fluid leading-in device is used for leading the supercritical fluid into the tank body of the extraction tank, and the tank body of the extraction tank is used for containing the led-in raw material and the supercritical fluid and enabling the led-in raw material and the supercritical fluid to form a substantially uniform solution;

the reaction tank comprises a tank body and a product guiding device, wherein the tank body of the reaction tank contains a catalyst, the tank body of the reaction tank is communicated with the tank body of the extraction tank and is used for enabling the uniform solution to enter the tank body of the reaction tank and to contact with the catalyst to generate esterification reaction under a supercritical state, and the product guiding device of the reaction tank is used for guiding a product after the esterification reaction to the fractionating tank;

a fractionating tank which comprises a tank body and a product leading-out device, wherein the tank body of the fractionating tank is communicated with the tank body of the reaction tank and is used for leading in the product after the esterification reaction, and the product leading-out device of the fractionating tank is used for leading out the product with stable temperature and pressure to the distinguishing tank after the temperature and the pressure are adjusted to set values and are stable in the tank body of the fractionating tank;

the three-zone tank comprises three tank bodies, the temperature and the pressure of the three-zone tank are different, the introduced product is purified and separated by supercritical fluid under different pressures and temperatures to obtain the finished distilled liquor of ester compounds with different concentrations, the standard mixture combination can be obtained qualitatively and quantitatively, and the processes of synthesis and separation can be simultaneously achieved.

In one embodiment, the system is a continuous supercritical maturation purification system or a batch supercritical maturation purification system. Wherein, a continuous supercritical ripening and purification system is preferred, which comprises continuous supercritical ripening and continuous supercritical fractionation and purification. When the supercritical ripening and purification system is a continuous supercritical ripening and purification system, the raw material introduction device may be any known continuous raw material introduction device, or a simple opening and closing device (opening the opening, pouring the raw material, and then closing the closing device).

In one embodiment, the maturation purification system includes one or more control valves to assist in temperature control, pressure control, and flow control.

In one embodiment, the fractionation tank is configured as a continuous supercritical fluid single column fractionation apparatus, and generally, further comprises control valves, preferably for assisting pressure control and flow control.

In one embodiment, the extraction tank of the system may further be provided with a temperature control device for controlling the temperature in the extraction tank.

In one embodiment, the reaction tank of the system may further include a temperature control device for controlling the temperature in the reaction tank.

In one embodiment, the three separation tanks of the system may be further provided with temperature control devices respectively for controlling the temperatures in the three separation tanks.

In one embodiment, the extraction tank is provided with a filler. The filler may be any filler that increases the number of theoretical plates (or plates) used to increase the reaction rate and reduce the relative size of the extraction tank.

The second technical scheme adopted by the invention for solving the technical problems is as follows:

a method for aging and purifying wine by supercritical fluid fractionation technology comprises mixing raw materials and supercritical fluid uniformly in an extraction tank, allowing the uniformly mixed supercritical solution to enter a reaction tank to contact with a catalyst, performing esterification reaction in a supercritical state, allowing the obtained mixed solution after the esterification reaction to enter a partition tank through a fractionation tank, and separating and purifying by supercritical carbon dioxide separation; wherein the pressure in the extraction tank is 5-40 Mpa, and the temperature is 30-100 ℃; the pressure in the reaction tank is 5-40 Mpa, and the temperature is 30-100 ℃; the pressure in the fractionating tank is 5-40 Mpa, and the temperature is 30-100 ℃; the pressure in the distinguishing groove is 5-40 MPa, the temperature is 30-100 ℃, the flow rate of the supercritical fluid is 7-30L/hr, and the fractionation time in the distinguishing groove is 30-90 min.

The pressure in the extraction tank is determined by the need of maintaining carbon dioxide as supercritical fluid, and is preferably maintained at 5-40 MPa, more preferably 10-35 MPa, and most preferably 15-30 MPa, in the case of aging reaction of wine. The temperature in the extraction tank is determined by different ripening reactions, such as wine ripening reaction, and is preferably maintained at 30-100 deg.C, more preferably 40-90 deg.C, and most preferably 45-65 deg.C, with carbon dioxide maintained as the supercritical fluid. When the extraction tank body is larger, in order to maintain the temperature of the extraction tank, it is preferable to further include a temperature control device.

The pressure in the reaction tank is preferably maintained at 5 to 40MPa, more preferably 10 to 35MPa, and still more preferably 15 to 30 MPa. The temperature in the reaction tank is preferably maintained at 30 to 100 ℃, more preferably 40 to 90 ℃, and most preferably 45 to 65 ℃. Generally, it is preferable that the pressure in the reaction tank is substantially the same as the pressure in the extraction tank, and the temperature in the reaction tank is substantially the same as the temperature in the extraction tank.

The pressure in the fractionating tank is determined by the different ripening reactions, for example, the wine ripening reaction, under the condition that carbon dioxide is maintained as a supercritical fluid, and preferably, the pressure in the fractionating tank is maintained at 5 to 40MPa, more preferably, 10 to 35MPa, and still more preferably, 15 to 30 MPa. The temperature in the fractionating tank is maintained at 30 to 100 ℃, preferably 40 to 90 ℃, and most preferably 45 to 65 ℃ as a necessary condition for maintaining carbon dioxide as a supercritical fluid.

The pressure in the separation tank is preferably maintained at 5 to 40MPa, preferably 10 to 35MPa, more preferably 15 to 30MPa, depending on the purification standards. The temperature in the separation tank is preferably maintained at 30 to 100 ℃, more preferably 40 to 90 ℃, and still more preferably 45 to 80 ℃.

In one embodiment, the pressure design of the three dividing grooves is preferably a gradient reduction.

In one embodiment, the supercritical fluid is a supercritical carbon dioxide fluid.

In one embodiment, the catalyst is a lipase.

In the above method, the esterification reaction may be a batch reaction or a continuous reaction, and the continuous reaction is preferred. In the continuous reaction, the wine flow in the extraction tank is not limited, the ripening effect is relatively low when the flow is large, and the ripening effect is relatively high when the flow is small.

The size of the extraction tank is not limited, and the capacity is large, the productivity is large, and the capacity is small, the productivity is small. The flow rate of carbon dioxide in the extraction tank depends on the size of the extraction tank.

The catalyst in the reaction tank is subjected to ripening esterification reaction. The amount of the catalyst is not limited, and if the amount of the catalyst is large, the ripening effect is relatively high, and if the amount of the catalyst is small, the ripening effect is relatively low.

Generally, the extraction tank and the reaction tank have a large capacity and a high productivity, and a small capacity and a low productivity. The flow of the wine is small, the dosage of the catalyst is large, the esterification effect is high, otherwise, the esterification effect is low.

In the method, the esterification reaction is to carry out the esterification of the wine in the supercritical carbon dioxide environment so as to greatly shorten the maturation time, and the best compound combination is found out by purifying and separating through fractionation equipment, so that the standard of the wine can be qualitatively and quantitatively measured.

The conditions of use of the supercritical maturation purification system of the present invention depend on the maturation reaction. The present invention is exemplified by a maturation reaction of alcoholic liquors under the conditions described in the above maturation purification method of alcoholic liquors.

The supercritical maturation purification system of the present invention has been confirmed to accelerate the maturation of wine, but those skilled in the art of food and drug technology can perform various maturation reactions of brewed foods or drugs, such as vinegar maturation reaction, using the same or similar devices.

It should be noted that the single processing procedure of each apparatus according to the present invention is common knowledge, and those skilled in the art can complete the processing procedures by using the apparatus according to the above description. The invention is based on the combined use of individual devices, so that the specific operating steps of these devices are not described in detail.

Compared with the background technology, the technical scheme has the following advantages:

the invention uses the supercritical fluid fractionation technology to accelerate the aging of the wine, further separates and purifies, and uses high technology to replace the wine year time, thereby reducing the storage cost of the traditional wine cellar, further improving the content of esters in the wine after the purification and separation of the fractionation equipment, and improving the fragrance and the taste of the wine. The invention can increase the wine age by 30 years in a very short time, and the miscellaneous aldehydes, miscellaneous ketones, miscellaneous acids and long-short chain fatty acids in the wine are all removed, so that the body and the liver are not hurt after drinking. Can be applied to the ripening of various high-grade wines, can also be applied to the process of further purification after the manufacture of esterification ripening, and has high market value.

The esterification reaction is equivalent to that in the traditional cellaring ten years after the wine is matured for half a day.

And (3) esterification and ripening standardization:

storing for 1 year in a cellar for 2 hours

Storing for 3 years in a cellar for 5 hours

Storing for 5 years after 8 hours

Storing for 10 years in a cellar for 12 hours

Drawings

The invention is further illustrated by the following figures and examples.

FIG. 1 is a comparison spectrum of a commercial Jinmen kaoliang spirit before and after esterification, wherein (a) in FIG. 1 is a GC/MS spectrum of the commercial Jinmen kaoliang spirit, and (b) in FIG. 1 is a GC/MS spectrum of the Jinmen kaoliang spirit after supercritical carbon dioxide extraction; peaks in the spectrum from left to right are ethyl acetate, ethyl caprate, and ethyl lactate.

FIG. 2a is a GC/MS spectrum of a commercial Jinmen kaoliang spirit which is further purified and separated after esterification, FIG. 2b is a GC/MS spectrum of a component F1 in FIG. 2a, FIG. 2c is a GC/MS spectrum of a component F2 in FIG. 2a, and FIG. 2d is a GC/MS spectrum of a component F3 in FIG. 2 a; peaks in the spectrum from left to right are ethyl acetate, ethyl caprate, and ethyl lactate.

FIG. 3a is a GC/MS spectrum of further purification and separation of a commercial Jinmen kaoliang spirit after Esterification with a lipase catalyst, FIG. 3b is a GC/MS spectrum of a component SFE authentication F1 in FIG. 3a (i.e., a component obtained after purification and separation by a fractionating device after the lipase catalyst is added to a reaction tank), and FIG. 3c is a GC/MS spectrum of a component SFE authentication F2 in FIG. 3 a; peaks in the spectrum from left to right are ethyl acetate, ethyl caprate, and ethyl lactate.

FIG. 4a is a GC/MS spectrum of the wine of example 2 before and after esterification and purification separation, FIG. 4b is a GC/MS spectrum of component F1 in FIG. 4a, FIG. 4c is a GC/MS spectrum of component F2 in FIG. 4a, and FIG. 4d is a GC/MS spectrum of component F3 in FIG. 4 a.

FIG. 5 is a schematic diagram of the aging and purifying system for aging wine by supercritical fluid fractionation technology of the present invention.

Reference numerals:

a carbon dioxide steel cylinder

B raw material storage barrel

C supercritical carbon dioxide pump

D high-pressure liquid phase pump

E carbon dioxide precooling exchanger

F1-F2 power supply controller

G1-G14 high pressure valve

H total temperature controller

I1-I3 backpressure valve

P1 extraction tank

P2 reaction tank

P3 fractionating tank

P4 first partition groove

P5 second partition groove

P6 third divided groove

Detailed Description

The present invention will be described in detail with reference to the following examples:

a system for aging and purifying wine by supercritical fluid fractionation technology, as shown in FIG. 5, comprises:

an extraction tank P1, which comprises a tank body, a raw material leading-in device and a supercritical fluid leading-in device, wherein the raw material leading-in device comprises a raw material storage barrel B, a high-pressure liquid phase pump D and the like, and is used for leading the wine of the raw material into the tank body of the extraction tank;

and the reaction tank P2 comprises a tank body and a product guiding device, wherein the tank body of the reaction tank contains lipase, the tank body of the reaction tank is communicated with the tank body of the extraction tank and is used for enabling a uniform solution in the tank body of the extraction tank to enter the tank body of the reaction tank and contact with the lipase catalyst to generate esterification reaction under a supercritical state, and the product guiding device of the reaction tank is used for guiding the product after the esterification reaction out of the separation and fractionation tank P3.

And the fractionating tank P3 comprises a tank body and a product leading-out device, wherein the tank body of the fractionating tank is communicated with the tank body of the reaction tank P2 and is used for leading in the wine mixture after the esterification reaction, and the product leading-out device of the fractionating tank is used for leading out the wine mixture from the connecting section tanks P4-P6 after the temperature and the pressure of the wine mixture in the fractionating tank reach set values and are stable.

The three-zone groove P4, P5 and P6 comprises three groove bodies and three product leading-out devices, the temperature and the pressure of the three-zone groove are different, supercritical fluid purification and separation are carried out on the led-in wine mixture under different pressure gradients and temperatures to obtain distilled wine of ester compounds with different concentrations, and standard mixture combination is obtained qualitatively and quantitatively.

The temperature of the aging purification system is controlled by a total temperature controller H, and temperature controllers may be provided in the extraction tank, the reaction tank, the fractionation tank, and the separation tank, respectively. One or more pressure control valves and flow control valves may also be provided as desired.

The extraction tank, the reaction tank, the fractionating tank and the separating tank may be commercial supercritical extraction equipment.

The method for accelerating aging and purifying wine by utilizing the supercritical fluid fractionation technology of the device has the following specific operation modes:

starting the power supply of the equipment, setting the temperature of the electric heating controller according to the conditions of each group, confirming that all the high-pressure valves G1-G14 are closed, and opening SC-C0₂A booster pump and controller power supply F1-F2 sets the required pressure, sets the temperature of a carbon dioxide precooling exchanger, starts a carbon dioxide steel cylinder A when all the temperatures reach the set temperature and pressurizes the carbon dioxide steel cylinder A to a set amount, starts a high-pressure valve to pump the raw materials into an extraction tank P1 by a high-pressure liquid phase pump D in sequence, closes a valve G2 after the conveying is finished, then starts a supercritical carbon dioxide pump C to send the supercritical carbon dioxide into the extraction tank P1, and times the reaction time; setting the reaction time to complete the supercritical state. Keeping the wine in supercritical state, pumping the wine in supercritical state into reaction tank P2 through high pressure pump, contacting with lipase to react to promote esterification and ripening of wine, wherein the pressure and temperature in reaction tank P2 are the same as those in extraction tank P1.

The whole purification operation is carried out in a SC-C0₂The method is completed in the equipment of a fractionation system. The heating temperature of the fractionating tank P3 is set to 40-70 ℃, and the pressure required by pressurization is 10-30 MPa. The fractionating system has three separate tanks P4-P6 controlled by back pressure valves I1-I3 to form gradually decreasing pressure gradient. SC-C0₂The pressure of (2) is fed from the bottom into the fractionating tank P3 by using a high-pressure metering pump capable of setting the pressure and flow rate. The mixed liquid after the esterification reaction in the reaction tank P2 enters a fractionating tank P3 to adjust the temperature and the pressure until the required fractionating pressure is reached in a fractionating tank P3, the wine after the lactonization in the fractionating tank P3 is injected into a first separating tank P4 from the top end by a high-pressure liquid phase pump, and the SC-C0 at the bottom of the first separating tank P4 with 7-21L/hr is maintained₂The flow rate is maintained for a fractionation residence time of 30 to 90 minutes. The esterified wine is SC-C0 from the middle and the bottom of the first partition groove P4₂The esterified liquor can be dissolved in SC-C0 under the set pressure of the first partition groove P4₂Will be dissolved and carried and directed to the next second dividing tank P5 controlled at a different pressure. Continuing to separate and purify in the second separating tank P5, the components in the wine which are soluble in the second separating tank P5 under the set pressure will be dissolved and carried to the next third separating tank P6 with different pressure, and continuing to separate in the third separating tank P6And (5) separating and purifying. The solubility of each partition tank under different conditions will cause the separation of the primary components. And (4) timing the retention time, closing a communication valve between each partition groove P4-P6 after the operation is finished, opening a high-pressure valve at an outlet of each partition groove P4-P6 to release the pressure, and collecting the purified and separated refined wine.

Example 1

20 liters of 58 ℃ Kaoliang spirit commercially available was placed in a maturation purification system shown in FIG. 5, in which the capacity of the extraction tank P1 was 100 liters and the amount of lipase used in the reaction tank P2 was 1 kg. The extraction tank P1 has supercritical carbon dioxide pressure of 30Mpa, temperature of 50 deg.C, and kaoliang liquor flow rate of 20L/hr (20L per hour).

The pressure, temperature and flow rate of the supercritical carbon dioxide in the reaction tank P2 are the same as those of the extraction tank P1.

The temperature of the fractionating tank P3 is 40-70 ℃, and the pressure is 10-30 MPa.

The pressure of the first partition tank P4 is 30MPa, the temperature is 50 ℃, and the temperature is SC-C0₂The flow rate was 20L/hr (20 liters per hour) for a fractional residence time of 30 minutes.

The pressure of the second partition tank P5 is 25MPa, the temperature is 45 ℃, and the temperature is SC-C0₂The flow rate was 20L/hr (20 liters per hour) for a fractional residence time of 30 minutes.

The third dividing groove P6 has pressure of 20Mpa, temperature of 40 deg.C, and SC-C0₂The flow rate was 20L/hr (20 liters per hour) for a fractional residence time of 30 minutes.

The results of comparing the flavor, color and aroma of the esterified wine with those of a commercially available 58 ° jinmen kaoliang wine are shown in table 1. The flavor and aroma of the wine prepared in example 1 are far superior to those of the commercial Jinmen kaoliang wine.

TABLE 1 comparison of the flavor, color and aroma of Jinmen kaoliang spirit

	Flavor (I) and flavor (II)	Color and luster	Fragrance
				Commercial Jinmen kaoliang liquor	Spicy food	Transparent and colorless	Choking of food
Wine of example 1	Front opening	Golden yellow colour	Fragrant wine

A commercially available 58 ℃ Kaoliang spirit and a spirit prepared in example 1 were analyzed by GC/MS (Gas chromatography/Mass Spectroscopy) under instrumental analysis conditions of a flow rate of 1mL/min (1 mL/min), an initial temperature of 40 ℃, a temperature rise rate of 5 ℃/min, and a temperature maintenance after reaching 250 ℃. The spectra are shown in FIG. 1 (a) and FIG. 1 (b), wherein the spectrum of (a) in FIG. 1 is circled to 0.63mg/100mL of ethyl acetate, 7.53mg/100mL of ethyl hexanoate and 9.28mg/100mL of ethyl lactate in the commercially available Jingmen kaoliang spirit, and in FIG. 1 (b), it can be seen that the ethyl acetate, 85.48mg/100mL of ethyl hexanoate and 236.27mg/100mL of ethyl lactate in the case of lipase catalysis are obtained after supercritical extraction. The supercritical extraction reaction can increase the content of esters in the wine and make the wine more fragrant and mellow.

In FIGS. 2a to 2d, after purification and separation by a fractional distillation apparatus without lipase catalysis, ethyl acetate was 28.27mg/100mL, ethyl hexanoate was 66.71mg/100mL, and ethyl lactate was 191.48mg/100mL in fraction F1 obtained in first separation tank P4; in the fraction F2 obtained in the second separation tank P5, ethyl acetate was 43.41mg/100mL, ethyl hexanoate was 84.33mg/100mL, and ethyl lactate was 232.23mg/100 mL; in the fraction F3 obtained in the third separation tank P6, ethyl acetate was 58.95mg/100mL, ethyl caproate was 108.27mg/100mL, and ethyl lactate was 257.57mg/100 mL. The content of esters in the qualitative and quantitative wine is standardized after fractionation and purification.

As shown in fig. 3a to 3c, after the lipase catalyst is added to the reaction tank and purified and separated by the fractionating apparatus, in the fraction F1 (authentication F1) obtained in the first partition tank P4, ethyl acetate was 49.28mg/100mL, ethyl hexanoate was 88.54mg/100mL, and ethyl lactate was 248.69mg/100 mL; in fraction F2 (Escherichia F2) obtained in the second separation tank P5, ethyl acetate was 84.74mg/100mL, ethyl caproate was 128.95mg/100mL, and ethyl lactate was 298.32mg/100 mL. After the lipase catalyst is added, the content of esters in the wine is further improved after the purification and separation by a fractionating device.

Example 2

10L of a commercial wine was placed in an extraction tank as shown in FIG. 5, in which the capacity of the extraction tank was 100L and the amount of lipase used in the reaction tank was 0.5 kg. The supercritical carbon dioxide pressure in the extraction tank is 30Mpa, the temperature is 50 ℃, and the wine flow is 60L/h (60L per hour).

The supercritical carbon dioxide pressure, temperature and flow rate in the reaction tank are the same as those in the extraction tank.

The first dividing vessel P4 was set at a pressure of 30MPa, a temperature of 50 ℃ and a flow rate of 20L/hr (20 liters per hour) for a fractionation residence time of 30 minutes.

The second zone tank P5 was set at a pressure of 25MPa, a temperature of 45 ℃ and a flow rate of 20L/hr (20 liters per hour) for a fractionation residence time of 30 minutes.

The third fractionation tank P6 was set at a pressure of 20MPa, a temperature of 40 ℃ and a flow rate of 20L/hr (20 liters per hour) for a fractionation residence time of 30 minutes.

Commercially available wine was analyzed by GC/MS (Gas chromatography/Mass Spectroscopy) under instrumental analysis conditions of a flow rate of 1mL/min (1 mL per minute), an initial temperature of 40 ℃, a temperature rise rate of 5 ℃/min, and a temperature maintenance after reaching 250 ℃.

The obtained wine has a spectrum as shown in FIGS. 4a to 4d, wherein the commercially available wine (component F in FIG. 4) has ethyl acetate of 6.65mg/100mL, ethyl hexanoate of 8.72mg/100mL and ethyl lactate of 38.48mg/100mL, and after purification and separation by a fractionating apparatus by adding a lipase catalyst, the fraction F1 obtained in the first partition tank P4 has ethyl acetate of 18.21mg/100mL, ethyl hexanoate of 16.70mg/100mL and ethyl lactate of 91.47mg/100mL, the fraction F2 obtained in the second partition tank P5 has ethyl acetate of 23.40mg/100mL, ethyl hexanoate of 20.32mg/100mL, ethyl lactate of 71.22mg/100mL, and the fraction F3 obtained in the third partition tank P6 has ethyl acetate of 48.98mg/100mL, ethyl hexanoate of 72.17mg/100mL and ethyl lactate of 252.56mg/100 mL.

The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents.

Claims

1. A system for accelerating aging and purifying wine by supercritical fluid fractionation technology is characterized in that: the method comprises the following steps:

the reaction tank comprises a tank body and a product guiding device, wherein the tank body of the reaction tank contains a catalyst, the tank body of the reaction tank is communicated with the tank body of the extraction tank and is used for enabling the uniform solution to enter the tank body of the reaction tank and to contact with the catalyst to generate esterification reaction in a supercritical state, and the product guiding device of the reaction tank is used for guiding out a product after the esterification reaction;

a fractionating tank which comprises a tank body and a product leading-out device, wherein the tank body of the fractionating tank is communicated with the tank body of the reaction tank and is used for leading in the product after the esterification reaction and adjusting the temperature and the pressure in the tank body of the fractionating tank, and the product leading-out device of the fractionating tank is used for leading out the product after the temperature and the pressure are stable;

and the three-region groove comprises three groove bodies, the temperature and the pressure of the three-region groove are different, and the introduced product is subjected to supercritical fluid purification and separation under different pressures and temperatures to obtain finished products of ester compounds with different concentrations.

2. The system for aging and purifying wine by supercritical fluid fractionation technology according to claim 1, wherein: the system is a continuous supercritical ripening and purifying system.

3. The system for aging and purifying wine by supercritical fluid fractionation technology according to claim 1, wherein: and the extraction tank is internally provided with a filler.

4. The system for aging and purifying wine by supercritical fluid fractionation technology according to claim 1, wherein: the system is also provided with a temperature control device, a pressure control device and a flow control device.

5. A method for aging and purifying wine by supercritical fluid fractionation technology using the aging and purifying system according to any one of claims 1 to 4, characterized in that: uniformly mixing the raw materials and the supercritical fluid in an extraction tank, allowing the uniformly mixed solution in a supercritical state to enter a reaction tank to contact with a catalyst and perform esterification reaction in the supercritical state, allowing the mixed solution obtained after the esterification reaction to enter a partition tank through a fractionation tank, and performing separation and purification by using the supercritical fluid; wherein the pressure in the extraction tank is 5-40 Mpa, and the temperature is 30-100 ℃; the pressure in the reaction tank is 5-40 Mpa, and the temperature is 30-100 ℃; the pressure in the fractionating tank is 5-40 Mpa, and the temperature is 30-100 ℃; the pressure in the distinguishing groove is 5-40 MPa, the temperature is 30-100 ℃, and the flow rate of the supercritical fluid is 7-30L/hr.

6. The method for aging and purifying wine by supercritical fluid fractionation technology according to claim 5, wherein: the pressure in the extraction tank is 10-35 Mpa, and the temperature is 40-90 ℃; the pressure in the reaction tank is 10-35 Mpa, and the temperature is 40-90 ℃; the pressure in the fractionating tank is 10-35 Mpa, and the temperature is 40-90 ℃; the pressure in the distinguishing groove is 10-35 Mpa, and the temperature is 40-90 ℃.

7. The method for aging and purifying wine by supercritical fluid fractionation technology according to claim 5, wherein: the pressure in the extraction tank is 15-30 Mpa, and the temperature is 45-65 ℃; the pressure in the reaction tank is 15-30 Mpa, and the temperature is 45-65 ℃; the pressure in the fractionating tank is 15-30 Mpa, and the temperature is 45-65 ℃; the pressure in the distinguishing groove is 15-30 Mpa, and the temperature is 45-80 ℃.

8. The method for aging and purifying wine by supercritical fluid fractionation technology according to claim 5, wherein: the pressure in the reaction tank is the same as the pressure in the extraction tank, and the temperature in the reaction tank is the same as the temperature in the extraction tank.

9. The method for aging and purifying wine by supercritical fluid fractionation technology according to claim 5, wherein: the pressure gradient decreases for three of the discriminating grooves.

10. The method for aging and purifying wine by supercritical fluid fractionation technology according to claim 5, wherein: the supercritical fluid is supercritical carbon dioxide fluid; the catalyst is lipase.