CN103436369A - Method for synchronously preparing biodiesel and glycerol carbonate under acceleration action of methanol - Google Patents
Method for synchronously preparing biodiesel and glycerol carbonate under acceleration action of methanol Download PDFInfo
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- CN103436369A CN103436369A CN2013103968363A CN201310396836A CN103436369A CN 103436369 A CN103436369 A CN 103436369A CN 2013103968363 A CN2013103968363 A CN 2013103968363A CN 201310396836 A CN201310396836 A CN 201310396836A CN 103436369 A CN103436369 A CN 103436369A
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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Abstract
The invention relates to a method for synchronously preparing biodiesel and glycerol carbonate under the acceleration action of methanol, which comprises the following steps: adding natural grease, dimethyl carbonate and methanol into a reaction kettle, adding alkali into the reaction kettle while stirring, heating while stirring, cooling to room temperature, filtering the reaction product in the reaction kettle, and washing with dimethyl carbonate until the filter residue is white, thereby obtaining a filtrate; evaporating the filtrate to remove excessive dimethyl carbonate and methanol under reduced pressure to obtain a light yellow liquid which is a biodiesel crude product; extracting the biodiesel crude product with methanol 2-3 times, wherein the residue is purified biodiesel; and merging the methanol solution, and evaporating to remove methanol to obtain the glycerol carbonate. The invention solves the problem of glycerol residues in the traditional biodiesel production process, and obtains the glycerol carbonate with high added value, thereby being beneficial to upgrading the biodiesel preparation technique; and the invention enhances the economic benefit of the biodiesel industry, and has the advantages of lower technical difficulty and lower processing cost.
Description
Technical field
The present invention relates to technical field of biodiesel preparation, be specifically related to the method that methyl alcohol promotes the standby biofuel of interlock system and carbonic acid glyceride.
Background technology
China's diesel oil consumption is about 9,000 ten thousand ton/years at present, to a great extent dependence on import.Estimate, within 2012, China's diesel oil demand will break through 100,000,000 tons.The biofuel sale price is about 5000 yuan/tons, if by the blending ratio 80:20 (being the B20 standard) of diesel oil and biofuel estimation, and consumption market year 1800 ten thousand tons of the demands of China's biofuel so, the potential market total value is 90,000,000,000 yuan.And China's actual output does not also surpass 1,000,000 ton/years at present, according to national planning, to the year two thousand twenty, will reach 1,500 ten thousand tons.
The deep development of Biodiesel by-product glycerin is also the important factor that promotes this industrial harmonization development.The whole world is to the demand of glyceryl ester with nearly 10% speed increment, and within 2010, the consumption to glyceryl ester reaches nearly 4,000,000 tons, and China is the consumption big country of glyceride product, annually all needs a large amount of imports to make up the breach of domestic production.Wherein carbonic acid glyceride (GC) can be used as high polar solvent or valuable superpolymer intermediate composition, it is the composition of preparation table surface-active agent, dress material, stain remover, new coating, be also the important component part of a kind of new gas separatory membrane and polyurethane expanded particle, purposes is very extensive simultaneously.Carbonic acid glyceride can also carry out the cyclic carbonate alkene ester that transesterification reaction can be used for preparing other by the derivative with relative acid, ester or acid.At present the preparation method of carbonic acid glyceride has glycerine and phosgene, dialkyl carbonate, alkylene carbonate, urea, CO
2reaction, all there are problem in various degree in its transformation efficiency and selectivity, and at present domestic also not large-scale industrial produce carbonic acid glyceride, mainly rely on import.The report that adopts natural fats and oils and the standby biofuel of dimethyl carbonate interlock system and carbonic acid glyceride has been arranged at present, but the reaction times is longer, the very easily saponification of raw material and product, ultimate yield is not high, and saponified being difficult to separates.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide methyl alcohol to promote the method for the standby biofuel of interlock system and carbonic acid glyceride, reactant is natural fats and oils, methyl alcohol and methylcarbonate, in the preparation biofuel, the glycerine of generation synchronously is converted into to carbonic acid glyceride, both can solve the problem of glycerine remnants in the traditional biological diesel production, can obtain the carbonic acid glyceride of high added value again simultaneously, and adopt methyl alcohol as promotor, consumption is few, improve speed of response, reduce the saponification degree of raw material and product, make the separation of biofuel and by product thereof, a plurality of step height such as deep processing are integrated, be conducive to biofuel preparation technology's upgrading, improve the economic benefit of Biodiesel.
In order to achieve the above object, the technical solution used in the present invention is:
Methyl alcohol promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, comprises the following steps:
The first step, by natural fats and oils, methylcarbonate and methyl alcohol, according to volume ratio, be 1:(1-5): (1-10) add in reactor, natural fats and oils is Vegetable oil lipoprotein, animal grease or both mixture after deacidification, dehydration, and methylcarbonate and methyl alcohol are the reagent through chemical pure and the above purity of Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 5-20% in the downhill reaction still, after 60-90 ℃ of lower stirring heating 4-8 hour, cool to room temperature, the salt of wormwood that described alkali is technical grade and above purity, sodium carbonate, sodium hydroxide, potassium hydroxide, hydrated barta and composition thereof;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 2-3 time for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Resulting carbonic acid glyceride can be industry through being further purified.
Because the present invention has adopted common commercially available mineral alkali as catalyzer, before using, without processing, the solubleness in organic solvent is little, easily by filtering separation, removes after reaction, thereby has advantages of the technology difficulty of reduction and processing cost.The present invention can be applicable to prepare biofuel by natural fats and oils and methylcarbonate.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
Methyl alcohol promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, comprises the following steps:
The first step, be that 1:1:5 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, and natural fats and oils is the soybean oil after deacidification, dehydration, and methylcarbonate and methyl alcohol are the chemically pure reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 10% in the downhill reaction still, 90 ℃ of lower stirring heating after 6 hours, and cool to room temperature, the sodium hydroxide that described alkali is technical grade;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 3 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Embodiment 2
Methyl alcohol promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, comprises the following steps:
The first step, be that 1:1.1:6 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, and natural fats and oils is the rapeseed oil after deacidification, dehydration, and methylcarbonate and methyl alcohol are the analytical reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 10% in the downhill reaction still, 90 ℃ of lower stirring heating after 5 hours, and cool to room temperature, the mixture that described alkali is technical grade salt of wormwood and potassium hydroxide mass ratio 1:1;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 3 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Embodiment 3
Methyl alcohol promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, comprises the following steps:
The first step, be that 1:2:10 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, and natural fats and oils is the Oleum Gossypii semen after deacidification, dehydration, and methylcarbonate and methyl alcohol are the chemically pure reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 8% in the downhill reaction still, 70 ℃ of lower stirring heating after 5 hours, and cool to room temperature, described alkali is chemical pure hydrated barta product;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 2 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Embodiment 4
Methyl alcohol promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, comprises the following steps:
The first step, be that 1:1.5:8 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, and natural fats and oils is the butter after deacidification, dehydration, and methylcarbonate and methyl alcohol are the chemically pure reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 20% in the downhill reaction still, 80 ℃ of lower stirring heating after 6 hours, and cool to room temperature, described alkali is analytical pure potassium hydroxide;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 3 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Embodiment 5
Methyl alcohol promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, comprises the following steps:
The first step, by natural fats and oils, methylcarbonate and methyl alcohol, according to the ratio of amount, be that 1:1.6:9 adds in reactor, natural fats and oils is the rapeseed oil that is 1:1 of the mass ratio after deacidification, dehydration and the mixture of soybean oil, and methylcarbonate and methyl alcohol are the analytical reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 20% in the downhill reaction still, 60 ℃ of lower stirring heating after 6 hours, and cool to room temperature, described alkali is the chemical pure hydrated barta;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 3 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Embodiment 6
Methyl alcohol promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, comprises the following steps:
The first step, by natural fats and oils, methylcarbonate and methyl alcohol, according to the ratio of amount, be that 1:3:10 adds in reactor, natural fats and oils be through the deacidification, the dehydration after rapeseed oil and the mixture of lard, methylcarbonate and methyl alcohol are the analytical reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 8% in the downhill reaction still, 85 ℃ of lower stirring heating after 6 hours, and cool to room temperature, described alkali is analytical pure sodium hydroxide;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, subtract methylcarbonate excessive in filtrate with methyl alcohol and press and boil off, and obtains light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 2 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Claims (7)
1. methyl alcohol promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, it is characterized in that, comprises the following steps:
The first step, by natural fats and oils, methylcarbonate and methyl alcohol, according to volume ratio, be 1:(1-5): (1-10) add in reactor, natural fats and oils is Vegetable oil lipoprotein, animal grease or both mixture after deacidification, dehydration, and methylcarbonate and methyl alcohol are the reagent through chemical pure and the above purity of Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 5-20% in the downhill reaction still, after 60-90 ℃ of lower stirring heating 4-8 hour, cool to room temperature, the salt of wormwood that described alkali is technical grade and above purity, sodium carbonate, sodium hydroxide, potassium hydroxide, hydrated barta and composition thereof;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 2-3 time for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
2. methyl alcohol according to claim 1 promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, it is characterized in that, comprises the following steps:
The first step, be that 1:1:5 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, and natural fats and oils is the soybean oil after deacidification, dehydration, and methylcarbonate and methyl alcohol are the chemically pure reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 10% in the downhill reaction still, 90 ℃ of lower stirring heating after 6 hours, and cool to room temperature, the sodium hydroxide that described alkali is technical grade;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 3 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
3. methyl alcohol according to claim 1 promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, it is characterized in that, comprises the following steps:
The first step, be that 1:1.1:6 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, and natural fats and oils is the rapeseed oil after deacidification, dehydration, and methylcarbonate and methyl alcohol are the analytical reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 10% in the downhill reaction still, 90 ℃ of lower stirring heating after 5 hours, and cool to room temperature, the mixture that described alkali is technical grade salt of wormwood and potassium hydroxide mass ratio 1:1;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 3 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
4. methyl alcohol according to claim 1 promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, it is characterized in that, comprises the following steps:
The first step, be that 1:2:10 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, and natural fats and oils is the Oleum Gossypii semen after deacidification, dehydration, and methylcarbonate and methyl alcohol are the chemically pure reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 8% in the downhill reaction still, 70 ℃ of lower stirring heating after 5 hours, and cool to room temperature, described alkali is chemical pure hydrated barta product;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 2 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
5. methyl alcohol according to claim 1 promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, it is characterized in that, comprises the following steps:
The first step, be that 1:1.5:8 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, and natural fats and oils is the butter after deacidification, dehydration, and methylcarbonate and methyl alcohol are the chemically pure reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 20% in the downhill reaction still, 80 ℃ of lower stirring heating after 6 hours, and cool to room temperature, described alkali is analytical pure potassium hydroxide;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 3 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
6. methyl alcohol according to claim 1 promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, it is characterized in that, comprises the following steps:
The first step, by natural fats and oils, methylcarbonate and methyl alcohol, according to the ratio of amount, be that 1:1.6:9 adds in reactor, natural fats and oils is the rapeseed oil that is 1:1 of the mass ratio after deacidification, dehydration and the mixture of soybean oil, and methylcarbonate and methyl alcohol are the analytical reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 20% in the downhill reaction still, 60 ℃ of lower stirring heating after 6 hours, and cool to room temperature, described alkali is the chemical pure hydrated barta;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtain light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 3 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
7. methyl alcohol according to claim 1 promotes the method for the standby biofuel of interlock system and carbonic acid glyceride, it is characterized in that, comprises the following steps:
The first step, by natural fats and oils, methylcarbonate and methyl alcohol, according to the ratio of amount, be that 1:3:10 adds in reactor, natural fats and oils be through the deacidification, the dehydration after rapeseed oil and the mixture of lard, methylcarbonate and methyl alcohol are the analytical reagent through Non-aqueous processing;
Second step, stir the alkali that adds natural fats and oils quality 8% in the downhill reaction still, 85 ℃ of lower stirring heating after 6 hours, and cool to room temperature, described alkali is analytical pure sodium hydroxide;
The 3rd step, filter the reactant in reactor, with the methylcarbonate adopted in the first step, washs to filter residue white, obtains filtrate;
The 4th step, subtract methylcarbonate excessive in filtrate with methyl alcohol and press and boil off, and obtains light yellow liquid, is the biofuel crude product;
The 5th step, by isopyknic methanol extraction 2 times for the biofuel crude product, remain as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
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Cited By (5)
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CN105038997A (en) * | 2015-09-01 | 2015-11-11 | 中国科学院广州能源研究所 | Method for synchronously preparing biodiesel and glycerol carbonate through ionic liquid and catalytic grease |
CN105586149A (en) * | 2014-11-13 | 2016-05-18 | 中国石油天然气股份有限公司 | Separation method for carbonic acid glyceride and biodiesel |
CN105642266A (en) * | 2014-11-13 | 2016-06-08 | 中国石油天然气股份有限公司 | Glycerin-free prepared biodiesel composite solid base catalyst and preparation method |
CN108484564A (en) * | 2018-05-02 | 2018-09-04 | 西安石油大学 | A kind of method that complex solid base catalysis quickly prepares carbonic acid glyceride |
CN114214120A (en) * | 2021-12-21 | 2022-03-22 | 常州市金坛区维格生物科技有限公司 | Method for co-producing fatty acid methyl ester and glycerol carbonate |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN105586149A (en) * | 2014-11-13 | 2016-05-18 | 中国石油天然气股份有限公司 | Separation method for carbonic acid glyceride and biodiesel |
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CN108484564A (en) * | 2018-05-02 | 2018-09-04 | 西安石油大学 | A kind of method that complex solid base catalysis quickly prepares carbonic acid glyceride |
CN114214120A (en) * | 2021-12-21 | 2022-03-22 | 常州市金坛区维格生物科技有限公司 | Method for co-producing fatty acid methyl ester and glycerol carbonate |
CN114214120B (en) * | 2021-12-21 | 2023-08-18 | 常州市金坛区维格生物科技有限公司 | Co-production method of fatty acid methyl ester and glycerin carbonate |
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