CN114890888A - Method for extracting ultrahigh-concentration lactic acid from yellow wine brewing water based on tangential flow membrane technology - Google Patents
Method for extracting ultrahigh-concentration lactic acid from yellow wine brewing water based on tangential flow membrane technology Download PDFInfo
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- CN114890888A CN114890888A CN202210697436.5A CN202210697436A CN114890888A CN 114890888 A CN114890888 A CN 114890888A CN 202210697436 A CN202210697436 A CN 202210697436A CN 114890888 A CN114890888 A CN 114890888A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a method for extracting lactic acid with ultrahigh concentration from yellow water for brewing based on tangential flow membrane technology, which comprises the steps of firstly pretreating the yellow water by using a 200-mesh and 300-mesh screen, and filtering to remove insoluble substances; then, filtering the yellow water in series by adopting filter membranes with different pore diameters in a gradient manner, and removing color and smell of the obtained filtrate by using activated carbon; and then carrying out electrolytic impurity removal, and concentrating by using a rotary evaporator to obtain a high-concentration lactic acid solution, wherein the concentration of lactic acid is more than 600g/L, and the content of other substances is less than 5%. The method is simple to operate and easy to realize, and by means of the synergistic work of membrane filtration, activated carbon adsorption, electrolysis and rotary evaporation concentration reduction, the lactic acid solution with high concentration and less impurities is obtained, the resource utilization of the yellow water which is a brewing byproduct is realized, the emission of the yellow water with high COD is reduced, and the method has important significance for environmental protection.
Description
Technical Field
The invention relates to a method for extracting ultrahigh-concentration lactic acid from yellow wine brewing water based on a tangential flow membrane technology, and belongs to the technical field of wine brewing.
Background
The yellow water is a brownish yellow fluid liquid which is deposited at the bottom of a pit pool after the fermented grains are subjected to the catabolism of microorganisms and part of water is exuded in the process of brewing and producing the white spirit by a solid-state method, and belongs to a byproduct in the process of brewing the white spirit by the solid-state method. The yellow water is rich in aromatic flavor substances such as organic acid, alcohol and aldehyde, and also contains amino acids, saccharides, alcohol, humus, yeast autolysate, microbial thallus and living cells. The yellow water has the highest organic acid content, wherein the lactic acid content is the first and accounts for about 90 percent of the total organic acid content, the content can reach 40-80 g/L, meanwhile, the COD content in the yellow water is also very high, the yellow water is directly discharged without treatment, the environment is polluted, the resource waste can be caused, if the yellow water can be treated, substances such as lactic acid and the like which are rich in the organic matters are separated and extracted, the resources can be recycled, the discharge of the yellow water with high COD is also reduced, and the method has important significance for protecting the environment.
At present, the main methods for separating and extracting lactic acid from yellow water in fermentation liquor comprise an extraction method, a calcium salt method, an esterification hydrolysis method, a molecular distillation method, an adsorption method and the like. These methods generally have the disadvantages of complicated process, high cost, low lactic acid yield (not higher than 60%), etc., such as: the extractant in the extraction method is generally high in cost and toxic, so that the implementation of the method is restricted; the calcium salt method has the defects of low yield of calcium lactate crystallization process, large consumption of acid-base solution in the process, high energy consumption and labor waste; the lactic acid yield by the esterification hydrolysis method is low; the molecular distillation method has low product single-pass yield and higher equipment investment; most desorption processes of the adsorption method need chemical reagents, and the obtained product is difficult to further purify.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides a method for extracting lactic acid with ultrahigh concentration from yellow wine brewing water based on a tangential flow membrane technology. The method is simple to operate, easy to implement and environment-friendly, the membrane filtration, activated carbon adsorption, electrolysis and rotary evaporation concentration methods have synergistic effects, and the obtained lactic acid solution is high in concentration and few in impurities.
The invention relates to a method for extracting lactic acid with ultrahigh concentration from yellow water for brewing based on a tangential flow membrane technology, which comprises the steps of firstly pretreating the yellow water by using a 200-mesh and 300-mesh screen, and filtering to remove insoluble substances; then, filtering the yellow water in series by adopting filter membranes with different pore diameters in a gradient manner, and removing color and odor of the obtained filtrate by using activated carbon; and then carrying out electrolytic impurity removal, and concentrating by using a rotary evaporator to obtain a high-concentration lactic acid solution, wherein the concentration of lactic acid is more than 600g/L, the content of other substances is less than 5%, and compared with the initial content of lactic acid in yellow water, the concentration of the lactic acid solution is improved by about 16 times.
Preferably, a 250-mesh screen is selected to pretreat the yellow water stock solution.
Preferably, three filter membranes with different pore diameters are adopted for filtration treatment in series ladder filtration. Specifically, in the tangential flow membrane device, yellow water is firstly coarsely filtered through a large-aperture filter membrane, then filtered through a medium-aperture filter membrane, and finally filtered through a small-aperture filter membrane to obtain final filtrate.
Furthermore, the parameters of the large-aperture filter membrane are 5000D-10000D, the parameters of the medium-aperture filter membrane are 500D-1000D, and the parameters of the small-aperture filter membrane are 100D-200D.
Furthermore, the pressure of the tangential flow membrane equipment is 1.8-3MPa when the tangential flow membrane equipment is used, and circulating water is used for cooling feed liquid, so that the membrane is prevented from being overheated and damaged.
Preferably, the granular activated carbon with the mesh number of 40-80 is selected, so that the granular activated carbon is easy to clean and has a good adsorption effect, and the dosage is 2-8 g of activated carbon per 100mL of final filtrate for adsorption.
Preferably, the area is selected to be 0.3-0.5cm during the electrolytic impurity removal 2 The graphite electrode has good conductivity, certain adsorption effect and current densityIs 0.1-0.5A/cm 2 And the electrolysis is carried out for 0.25-1 h.
Preferably, the conditions of use of the rotary evaporator are: the pressure is 30-50mbar, the temperature is 40-50 ℃, and the rotating speed is 20-25 rpm.
The invention has the beneficial effects that:
the invention provides a method for extracting high-concentration lactic acid from yellow wine water based on a tangential flow membrane technology, and the method has the advantages of simple operation, easy realization, environmental friendliness, high purity of the obtained lactic acid, less impurities and the like. Lactic acid solution with concentration of more than 600g/L is obtained through the synergistic effect of membrane filtration, activated carbon adsorption, electrolysis and rotary evaporation concentration technology.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1:
the method for extracting the ultrahigh-concentration lactic acid from the yellow wine brewing water based on the tangential flow membrane technology comprises the following steps of:
pretreating a certain amount of yellow water stock solution with a 250-mesh screen, filtering to remove impurities, filtering with a tangential flow membrane device, roughly filtering with a large-aperture membrane, filtering with a medium-aperture membrane to obtain filtrate, filtering with a 200D membrane to obtain final filtrate, wherein the pressure is set to 1.8MPa, cooling the feed solution with circulating water, adding 2% of activated carbon into the filtrate for adsorption, filtering to remove the activated carbon with a filter, transferring the adsorbed solution into a self-made electrolytic cell for electrolysis, and controlling the current density to be 0.3A/cm 2 Electrolyzing for 0.5h, transferring the electrolyzed solution into a rotary evaporator, and concentrating by using the rotary evaporator at the pressure of 40mbar and the temperature of 50 ℃, at the rotating speed of 20rpm, wherein the concentration time is about 3h to obtain a concentrated solution, and measuring the content of the lactic acid to be 650 g/L.
Example 2:
pretreating a certain amount of yellow water stock solution with a 250-mesh screen, and filteringRemoving impurity substances, filtering with tangential flow membrane equipment, coarse-filtering with a large-aperture membrane, filtering with a medium-aperture membrane, filtering with a 200D membrane to obtain final filtrate, wherein the pressure is set to 1.8MPa, and cooling the feed liquid with circulating water. Transferring the obtained filtrate into an electrolytic cell for electrolysis, and controlling the current density to be 0.3A/cm 2 Electrolyzing for 0.5h, transferring the electrolyzed solution into a rotary evaporator, and concentrating by using the rotary evaporator at the pressure of 40mbar and the temperature of 50 ℃, at the rotating speed of 20rpm, wherein the concentration time is about 3h to obtain a concentrated solution, and measuring the content of the lactic acid to be 520 g/L.
Example 3:
taking a certain amount of yellow water stock solution, pretreating the yellow water stock solution by using a 250-mesh screen, filtering to remove impurity substances, filtering by using tangential flow membrane equipment, coarsely filtering by using a large-aperture membrane, filtering the obtained filtrate by using a medium-aperture membrane, filtering the obtained filtrate by using a 200D membrane to obtain a final filtrate, wherein the pressure is set to be 1.8MPa, cooling the feed liquid by using circulating water, adding 5% of activated carbon into the obtained filtrate for adsorption, filtering the activated carbon by using a suction filter, transferring the adsorbed solution into a rotary evaporator, concentrating by using the rotary evaporator, wherein the pressure is 40mbar, the temperature is 50 ℃, the rotating speed is 20rpm, and the concentration time is about 3 hours, so as to obtain a concentrated solution, and measuring the lactic acid content to be 480 g/L.
Example 4:
pretreating a certain amount of yellow water stock solution by using a 250-mesh screen, removing impurities, filtering the solution after coarse filtration in tangential flow membrane equipment, performing coarse filtration by using a large-aperture membrane, filtering the obtained filtrate by using a medium-aperture membrane, and finally filtering by using a 200D membrane to obtain a final filtrate, wherein the membrane filtration pressure is 1.8MPa, cooling the feed liquid by using circulating water, adding 4% of active carbon into the obtained filtrate for adsorption, filtering the active carbon by using a filter, transferring the adsorbed solution into a self-made electrolytic cell for electrolysis, and controlling the current density to be 0.3A/cm 2 Electrolyzing for 0.5h, transferring the electrolyzed solution to a rotary evaporator, and concentrating with the rotary evaporator at 45 deg.C and 30mbar and 24rpmThe shrinkage time was about 3 hours, and a concentrated solution was obtained, and the lactic acid content was measured at 620 g/L.
Example 5:
pretreating a certain amount of yellow water stock solution by using a 250-mesh screen, removing impurities, filtering the solution after coarse filtration in tangential flow membrane equipment, coarsely filtering the solution by using a large-aperture membrane, filtering the obtained filtrate by using a medium-aperture membrane, and finally filtering the filtrate by using a 200D membrane to obtain a final filtrate, wherein the membrane filtration pressure is 2.2MPa, cooling the feed liquid by using circulating water, adding 6% of active carbon into the obtained filtrate for adsorption, filtering the active carbon by using a filter, transferring the adsorbed solution into a self-made electrolytic cell for electrolysis, and controlling the current density to be 0.3A/cm 2 Electrolyzing for 0.5h, transferring the electrolyzed solution into a rotary evaporator, and concentrating by using the rotary evaporator at the pressure of 30mbar and the temperature of 40 ℃, at the rotating speed of 24rpm, wherein the concentration time is about 3h to obtain a concentrated solution, and measuring the content of the lactic acid to be 640 g/L.
Through the above embodiments, it is found that the content of lactic acid can be greatly increased by the synergistic effect of membrane filtration, activated carbon adsorption, electrolysis and rotary evaporation concentration techniques, and a lactic acid solution with ultrahigh concentration can be obtained.
The lactic acid product obtained by the invention can be applied to the fields of food, medicine, chemical industry, feed and the like.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A method for extracting ultra-high concentration lactic acid from yellow water for brewing wine based on a tangential flow membrane technology is characterized by comprising the following steps:
firstly, pretreating yellow water by using a 200-300-mesh screen, and filtering to remove insoluble substances; then, filtering the yellow water in series by adopting filter membranes with different pore diameters in a gradient manner, and removing color and odor of the obtained filtrate by using activated carbon; and then carrying out electrolytic impurity removal, and concentrating by using a rotary evaporator to obtain a high-concentration lactic acid solution, wherein the concentration of lactic acid is more than 600g/L, and the content of other substances is less than 5%.
2. The method of claim 1, wherein:
and (4) pretreating the yellow water stock solution by using a 250-mesh screen.
3. The method of claim 1, wherein:
when the filtration is carried out in series echelon, three filter membranes with different apertures are adopted for filtration treatment.
4. The method of claim 3, wherein:
in the tangential flow membrane equipment, yellow water is firstly coarsely filtered by a large-aperture filter membrane, then filtered by a medium-aperture filter membrane, and finally filtered by a small-aperture filter membrane to obtain final filtrate.
5. The method of claim 4, wherein:
the parameters of the large-aperture filter membrane are 5000D-10000D, the parameters of the medium-aperture filter membrane are 500D-1000D, and the parameters of the small-aperture filter membrane are 100D-200D.
6. The method of claim 4, wherein:
the pressure of the tangential flow membrane equipment is 1.8-3MPa when in use.
7. The method of claim 1, wherein:
the mesh number of the active carbon is 40-80 meshes, and the dosage of the active carbon is 2-8 g per 100mL of filtrate for adsorption.
8. The method of claim 1, wherein:
selecting area of 0.3-0.5cm during electrolysis for removing impurities 2 The current density of the graphite electrode is 0.1-0.5A/cm 2 Electrolysis ofThe time is 0.25-1 h.
9. The method of claim 1, wherein:
the parameters of the rotary evaporator were set as: the pressure is 30-50mbar, the temperature is 40-50 ℃, and the rotating speed is 20-25 rpm.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5503750A (en) * | 1993-10-04 | 1996-04-02 | Russo, Jr.; Lawrence J. | Membrane-based process for the recovery of lactic acid by fermentation of carbohydrate substrates containing sugars |
| JPH09135698A (en) * | 1995-09-14 | 1997-05-27 | Sanei Touka Kk | Production of organic acid |
| CN106350419A (en) * | 2016-08-30 | 2017-01-25 | 宜宾五粮液股份有限公司 | Method for producing lactic acid-containing compound wine-blending liquid from wine-brewing yellow water |
| CN106565465A (en) * | 2016-10-27 | 2017-04-19 | 广西轻工业科学技术研究院 | Method for extracting lactic acid from yellow water as by-product of Daqu liquor |
| CN109294893A (en) * | 2018-10-30 | 2019-02-01 | 北京建筑大学 | A kind of resource utilization system and method for brewed spirit by-product yellow water |
| CN211963757U (en) * | 2020-03-02 | 2020-11-20 | 上海汉禾生物新材料科技有限公司 | A receive and strain multistage continuous filtration system of formula membrane of book for purifying lactic acid |
-
2022
- 2022-06-20 CN CN202210697436.5A patent/CN114890888A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5503750A (en) * | 1993-10-04 | 1996-04-02 | Russo, Jr.; Lawrence J. | Membrane-based process for the recovery of lactic acid by fermentation of carbohydrate substrates containing sugars |
| JPH09135698A (en) * | 1995-09-14 | 1997-05-27 | Sanei Touka Kk | Production of organic acid |
| CN106350419A (en) * | 2016-08-30 | 2017-01-25 | 宜宾五粮液股份有限公司 | Method for producing lactic acid-containing compound wine-blending liquid from wine-brewing yellow water |
| CN106565465A (en) * | 2016-10-27 | 2017-04-19 | 广西轻工业科学技术研究院 | Method for extracting lactic acid from yellow water as by-product of Daqu liquor |
| CN109294893A (en) * | 2018-10-30 | 2019-02-01 | 北京建筑大学 | A kind of resource utilization system and method for brewed spirit by-product yellow water |
| CN211963757U (en) * | 2020-03-02 | 2020-11-20 | 上海汉禾生物新材料科技有限公司 | A receive and strain multistage continuous filtration system of formula membrane of book for purifying lactic acid |
Non-Patent Citations (1)
| Title |
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