CN114525177A - Enzymatic deacidification method for high-acid-value oil - Google Patents
Enzymatic deacidification method for high-acid-value oil Download PDFInfo
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- CN114525177A CN114525177A CN202210181864.2A CN202210181864A CN114525177A CN 114525177 A CN114525177 A CN 114525177A CN 202210181864 A CN202210181864 A CN 202210181864A CN 114525177 A CN114525177 A CN 114525177A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/06—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils with glycerol
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/16—Refining fats or fatty oils by mechanical means
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention discloses an enzymatic deacidification method for high-acid-value grease, belonging to the technical field of grease processing. When the high-acid-value oil is catalyzed by using lipase in a eutectic solvent consisting of betaine and glycerol for esterification deacidification, on one hand, the eutectic solvent can effectively extract free fatty acid in the high-acid-value oil, and on the other hand, the esterification reaction carried out in the eutectic solvent can efficiently convert the free fatty acid into glyceride. Under the synergistic effect of eutectic extraction and enzymatic esterification in eutectic solvent, the acid value of high acid value grease can be quickly reduced to below 0.5mg KOH/g. The method has the advantages of high deacidification speed, simple product separation, environmental protection, and good economic and ecological benefits and industrial application prospects.
Description
Technical Field
The invention belongs to the technical field of oil processing, and particularly relates to an enzymatic deacidification method for high-acid-value oil.
Background
The high acid value grease generally refers to grease with the acid value of more than 10mg KOH/g. The high acid value of fats and oils presents great difficulties in their storage, processing and utilization. At present, the common high acid value grease mainly comprises: high-acid-value rice bran oil, high-acid-value wheat germ oil, high-acid-value fish oil, high-acid-value waste cooking oil, acidified oil, deodorized distillate and the like. The deacidification and reutilization of the high acid value grease can realize the high-value utilization of resources and is beneficial to environmental protection.
The traditional chemical alkali refining can generate a large amount of soap, so that a large amount of neutral oil is lost, and the traditional chemical alkali refining is not suitable for deacidification of high-acid-value grease; physical distillation deacidification has the problems of high energy consumption, high requirement on phosphorus content of raw materials and the like although the deacidification effect is good; solvent extraction and membrane separation deacidification are novel deacidification technologies developed in recent years, but have the problems of low deacidification efficiency, poor effect, high application cost and the like. Compared with the deacidification methods, the enzyme deacidification method has the advantages of mild reaction conditions, high catalytic specificity, good deacidification effect, safety, environmental protection and the like, and is a main development direction in the field of oil deacidification in recent years. Zhao Chengwei and the like (the technological optimization of deacidification of rice bran crude oil by an enzyme method, Chinese oil, 2019, 44 (4): 17-20) adopt immobilized lipase CALB to catalyze deacidify the rice bran oil with high acid value under the condition of high vacuum (<1000Pa) for reaction for 6 hours, and the acid value of the rice bran oil with high acid value is reduced from 20.52mg KOH/g to 1.54mg KOH/g; wancong et al (optimization research of enzyme method esterification deacidification process of solvent-free system high acid value rice bran oil, 2016, 41 (4): 10-13) adopt Lipozyme 435 to catalyze deacidify the high acid value rice bran oil under the condition of 0.09MPa, the reaction lasts for 10 hours, and the acid value of the high acid value rice bran oil is reduced from 39.81mg KOH/g to 2.06mg KOH/g; li et al (Journal of Agricultural and Food Chemistry,2016,64(35):6730-6737) used immobilized partial high glyceride lipase SMG1-F278N to catalyze deacidification of high acid value rice bran oil by adding ethanol in batches under n-hexane system for 6h, and the acid value of the high acid value rice bran oil is reduced from 50.12mg KOH/g to 0.10mg KOH/g. In conclusion, the existing enzymatic deacidification technology has mild reaction conditions and good deacidification effect, but the deacidification efficiency and effect are still improved by means of high vacuum or organic solvents and the like in the deacidification process, and the deacidification time is still long.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide an enzymatic deacidification method for high-acid-value oil, which can greatly improve the deacidification efficiency and realize the rapid deacidification of the high-acid-value oil.
The invention is realized by the following technical scheme:
an enzymatic deacidification method of high acid value grease comprises the following steps:
step 1: catalyzing high-acid-value grease to perform esterification reaction by adopting immobilized lipase in a eutectic solvent consisting of betaine and glycerol at a preset rotating speed;
step 2: and after the reaction is finished, performing centrifugal treatment to obtain deacidified grease.
Preferably, in step 1, the molar ratio of betaine to glycerol is 1: 4 to 8.
Preferably, in the step 1, the molar ratio of the glycerol to the free fatty acid in the high acid value grease is 2-6: 1.
preferably, in step 1, the immobilized lipase is Novozym 435 or Lipozyme 435.
More preferably, the addition amount of the immobilized lipase is 2 to 6% of the total mass of the substrate.
Preferably, in the step 1, the temperature of the esterification reaction is 40-70 ℃, and the time of the esterification reaction is 0.5-2 h.
Preferably, in the step 1, the preset rotating speed is 200-500 rpm.
Preferably, in the step 2, the rotation speed of the centrifugation is 8000-15000 rpm, and the time of the centrifugation is 1-2 min.
Compared with the prior art, the invention has the following beneficial technical effects:
the enzymatic deacidification method of the high-acid-value oil is carried out in the eutectic solvent composed of the betaine and the glycerol, and the eutectic solvent composed of the betaine and the glycerol has better solubility to free fatty acid, so that the free fatty acid in the high-acid-value oil can be efficiently extracted; in addition, free fatty acid in high-acid-value grease can be converted into glyceride through esterification reaction catalyzed by lipase in the eutectic solvent, and water generated in the esterification reaction process can be captured by the eutectic solvent consisting of betaine and glycerol through hydrogen bond formation, so that the conversion of the free fatty acid into the glyceride is promoted. Under the combined action of the extraction of the eutectic solvent and the esterification reaction catalyzed by lipase in the eutectic solvent, the acid value of the high-acid-value grease is rapidly reduced. The method has the advantages of high deacidification speed, good effect, simple product separation, environmental protection, and good economic and ecological benefits and industrial application prospects.
Further, the molar ratio of betaine to glycerol was 1: 4-8, not only is the free fatty acid extracted by the eutectic solvent facilitated, but also the free fatty acid is efficiently converted into glyceride by the lipase in the eutectic solvent.
Further, the molar ratio of the glycerol to the free fatty acid in the high-acid-value oil is 2-6: 1, can ensure higher fatty acid esterification rate.
Furthermore, Novozym 435 or Lipozyme 435 is adopted as the immobilized lipase, so that higher fatty acid selectivity and esterification rate can be ensured.
Furthermore, the temperature of the esterification reaction is 40-70 ℃, so that the eutectic solvent can be ensured to have higher extraction efficiency on fatty acid, and the lipase can be ensured to have higher reactivity and stability.
Furthermore, the rotating speed of the centrifugation is 8000-15000 rpm, the time of the centrifugation is 1-2 min, and the product can be rapidly recovered with high recovery rate.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention. All percentages are by mass, unless otherwise indicated.
Example 1
2Kg of a mixture of a eutectic solvent consisting of betaine and glycerol and a high acid value grease (56.48mg KOH/g) was added to a 5L reaction flask, in a molar ratio of 1: 4, the molar ratio of the glycerol in the eutectic solvent to the free fatty acid in the high-acid-value grease is 2: 1. after preheating the reaction mixture to 40 ℃ 40g of Novozym 435 were added and the reaction was carried out with a stirring speed of 200 rpm. After reacting for 2h, centrifuging at the rotating speed of 15000rpm for 1min to obtain the deacidified grease. The acid value of the deacidified oil is analyzed, and the acid value of the deacidified oil is reduced to 0.46mg KOH/g.
Example 2
2Kg of a mixture of a eutectic solvent consisting of betaine and glycerol and a high acid value grease (56.48mg KOH/g) was added to a 5L reaction flask, in a molar ratio of 1: 6, the molar ratio of the glycerol in the eutectic solvent to the free fatty acid in the high-acid-value grease is 4: 1. after preheating the reaction mixture to 60 ℃ 120g of Novozym 435 were added and the reaction was carried out with a stirring speed of 300 rpm. After the reaction is carried out for 0.5h, the mixture is centrifuged for 2min at the rotating speed of 8000rpm to obtain the deacidified grease. And analyzing the acid value of the deacidified oil, and finding that the acid value of the deacidified oil is reduced to 0.10mg KOH/g.
Example 3
2Kg of a mixture of a eutectic solvent consisting of betaine and glycerol and a high acid value grease (56.48mg KOH/g) was added to a 5L reaction flask, in a molar ratio of 1: and 8, the molar ratio of the glycerol in the eutectic solvent to the free fatty acid in the high-acid-value grease is 6: 1. after the reaction mixture was preheated to 70 ℃ 100g of Lipozyme 435 were added and the reaction was carried out with a stirring speed of 500 rpm. After the reaction is carried out for 0.5h, the mixture is centrifuged for 1.5min at the rotating speed of 12000rpm to obtain the deacidified grease. And analyzing the acid value of the deacidified oil, and finding that the acid value of the deacidified oil is reduced to 0.10mg KOH/g.
Example 4
2Kg of a mixture of a eutectic solvent consisting of betaine and glycerol and a high acid value grease (56.48mg KOH/g) was added to a 5L reaction flask, in a molar ratio of 1: 5, the molar ratio of the glycerol in the eutectic solvent to the free fatty acid in the high-acid-value grease is 5: 1. after preheating the reaction mixture to 50 ℃ 60g of Lipozyme 435 were added and the reaction was carried out with a stirring speed of 400 rpm. After reacting for 1h, centrifuging for 1min at the rotating speed of 15000rpm to obtain deacidified grease. And analyzing the acid value of the deacidified oil, and finding that the acid value of the deacidified oil is reduced to 0.13mg KOH/g.
Example 5
2Kg of a mixture of a eutectic solvent consisting of betaine and glycerol and a high acid value grease (56.48mg KOH/g) was added to a 5L reaction flask, in a molar ratio of 1: and 4, the molar ratio of the glycerol in the eutectic solvent to the free fatty acid in the high-acid-value grease is 3: 1, after preheating the reaction mixture to 45 ℃ 50g of Lipozyme 435 were added and the reaction was carried out with a stirring speed of 500 rpm. After reacting for 1h, centrifuging for 1min at the rotating speed of 15000rpm to obtain deacidified grease. And analyzing the acid value of the deacidified oil, and finding that the acid value of the deacidified oil is reduced to 0.48mg KOH/g.
Example 6
2Kg of a mixture of a eutectic solvent consisting of betaine and glycerol and a high acid value grease (56.48mg KOH/g) was added to a 5L reaction flask, in a molar ratio of 1: 7, the molar ratio of the glycerol in the eutectic solvent to the free fatty acid in the high-acid-value grease is 6: 1, after preheating the reaction mixture to 65 ℃ 60g of Novozym 435 were added and the reaction was carried out with a stirring speed of 300 rpm. After reacting for 1h, centrifuging for 2min at the rotating speed of 8000rpm to obtain deacidified grease. And analyzing the acid value of the deacidified oil, and finding that the acid value of the deacidified oil is reduced to 0.11mg KOH/g.
Claims (8)
1. An enzymatic deacidification method of high acid value grease is characterized by comprising the following steps:
step 1: catalyzing high-acid-value grease to perform esterification reaction by adopting immobilized lipase in a eutectic solvent consisting of betaine and glycerol at a preset rotating speed;
step 2: and after the reaction is finished, performing centrifugal treatment to obtain deacidified grease.
2. The enzymatic deacidification method of high acid value oil and fat according to claim 1, wherein in the step 1, the molar ratio of betaine to glycerol is 1: 4 to 8.
3. The enzymatic deacidification method of high acid value oil and fat according to claim 1, wherein in the step 1, the molar ratio of the glycerol to the free fatty acid in the high acid value oil and fat is 2-6: 1.
4. the enzymatic deacidification method of high acid value fats and oils according to claim 1, wherein in step 1, the immobilized lipase is Novozym 435 or Lipozyme 435.
5. The enzymatic deacidification method of high acid value oil and fat according to claim 4, characterized in that the addition amount of the immobilized lipase is 2-6% of the total mass of the substrate.
6. The enzymatic deacidification method of high acid value oil and fat according to claim 1, wherein in the step 1, the temperature of the esterification reaction is 40-70 ℃, and the time of the esterification reaction is 0.5-2 h.
7. The enzymatic deacidification method for high acid value oil and fat according to claim 1, wherein in the step 1, the preset rotating speed is 200-500 rpm.
8. The enzymatic deacidification method for high acid value oil and fat according to claim 1, wherein in the step 2, the rotation speed of the centrifugation is 8000-15000 rpm, and the time of the centrifugation is 1-2 min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210181864.2A CN114525177A (en) | 2022-02-25 | 2022-02-25 | Enzymatic deacidification method for high-acid-value oil |
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| CN202210181864.2A CN114525177A (en) | 2022-02-25 | 2022-02-25 | Enzymatic deacidification method for high-acid-value oil |
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| CN202210181864.2A Pending CN114525177A (en) | 2022-02-25 | 2022-02-25 | Enzymatic deacidification method for high-acid-value oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115261148A (en) * | 2022-08-29 | 2022-11-01 | 广东省农业科学院蚕业与农产品加工研究所 | Application of eutectic solvent in grease dehydration |
| CN115677757A (en) * | 2022-11-21 | 2023-02-03 | 江苏极易新材料有限公司 | Method for purifying tris (2,4-di-tert-butylphenyl) phosphite ester with low chloride ion content |
Citations (3)
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| US20080305531A1 (en) * | 2004-09-10 | 2008-12-11 | Verenium Corporation | Compositions and Methods for Making and Modifying Oils |
| CN106906194A (en) * | 2017-03-09 | 2017-06-30 | 华南理工大学 | A kind of enzyme process acid stripping method of partial glyceride lipase and the grease rich in PUFA |
| CN113061486A (en) * | 2021-04-09 | 2021-07-02 | 广东省农业科学院蚕业与农产品加工研究所 | Method for removing free fatty acid in grease through enzyme catalysis |
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2022
- 2022-02-25 CN CN202210181864.2A patent/CN114525177A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080305531A1 (en) * | 2004-09-10 | 2008-12-11 | Verenium Corporation | Compositions and Methods for Making and Modifying Oils |
| CN106906194A (en) * | 2017-03-09 | 2017-06-30 | 华南理工大学 | A kind of enzyme process acid stripping method of partial glyceride lipase and the grease rich in PUFA |
| CN113061486A (en) * | 2021-04-09 | 2021-07-02 | 广东省农业科学院蚕业与农产品加工研究所 | Method for removing free fatty acid in grease through enzyme catalysis |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115261148A (en) * | 2022-08-29 | 2022-11-01 | 广东省农业科学院蚕业与农产品加工研究所 | Application of eutectic solvent in grease dehydration |
| CN115261148B (en) * | 2022-08-29 | 2023-06-02 | 广东省农业科学院蚕业与农产品加工研究所 | Application of eutectic solvent in grease dehydration |
| CN115677757A (en) * | 2022-11-21 | 2023-02-03 | 江苏极易新材料有限公司 | Method for purifying tris (2,4-di-tert-butylphenyl) phosphite ester with low chloride ion content |
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