CN103436369B - 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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- CN103436369B CN103436369B CN201310396836.3A CN201310396836A CN103436369B CN 103436369 B CN103436369 B CN 103436369B CN 201310396836 A CN201310396836 A CN 201310396836A CN 103436369 B CN103436369 B CN 103436369B
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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
- 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 methyl alcohol and promote that interlock system is for the method for biofuel and carbonic acid glyceride.
Background technology
Current China diesel oil consumption is about 9,000 ten thousand tons/year, dependence on import to a great extent.Estimate, within 2012, China's diesel oil demand is by breakthrough 100,000,000 tons.Biofuel sale price is about 5000 yuan/ton, if the blending ratio 80:20 (i.e. B20 standard) pressing diesel oil and biofuel estimates, so consumption market year demand 1,800 ten thousand tons of China's biofuel, potential market total value is 90,000,000,000 yuan.And China's actual output, also more than 1,000,000 tons/year, according to national planning, will reach 15,000,000 tons to the year two thousand twenty at present.
The deep development of Biodiesel by-product glycerin is also the important factor promoting the development of this industrial harmonization.The whole world is to the demand of glyceryl ester with the speed increment of nearly 10%, and within 2010, reach nearly 4,000,000 tons to the consumption of glyceryl ester, China is the consumption big country of glyceride product, all needs a large amount of import to make up the breach of domestic production every year.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, also be 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 by carrying out with relative acid, ester or the derivative of acid the cyclic carbonate alkene ester that transesterification reaction can be used for preparing other.The preparation method of current carbonic acid glyceride has glycerine and phosgene, dialkyl carbonate, alkylene carbonate, urea, CO
2reaction, all there is problem in various degree in its transformation efficiency and selectivity, and domestic also non-large-scale industrial produces carbonic acid glyceride at present, mainly relies on import.Had at present the report adopting natural fats and oils and dimethyl carbonate interlock system for biofuel and carbonic acid glyceride, 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 is separated.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, interlock system is for the method for biofuel and carbonic acid glyceride to the object of the present invention is to provide methyl alcohol to promote, reactant is natural fats and oils, methyl alcohol and methylcarbonate, while preparation biofuel, the glycerine of generation is synchronously converted into carbonic acid glyceride, both the problem of glycerine remnants in traditional biological diesel production can have been solved, the carbonic acid glyceride of high added value can be obtained 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, multiple step such as deep processing height is integrated, be conducive to the upgrading of biofuel preparation technology, 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 that interlock system is for the method for biofuel and carbonic acid glyceride, comprises the following steps:
The first step, be 1:(1-5 by natural fats and oils, methylcarbonate and methyl alcohol according to volume ratio): (1-10) adds in reactor, natural fats and oils is Vegetable oil lipoprotein, animal grease or both mixtures after deacidification, dehydration, and methylcarbonate and methyl alcohol are the reagent of chemical pure through Non-aqueous processing and above purity;
Second step, stir the alkali adding natural fats and oils quality 5-20% in downhill reaction still, at 60-90 DEG C after stirring heating 4-8 hour, cool to room temperature, described alkali is the salt of wormwood, sodium carbonate, sodium hydroxide, potassium hydroxide, hydrated barta and composition thereof of technical grade and above purity;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 2-3 time, remaining as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and namely obtain carbonic acid glyceride.
Namely the carbonic acid glyceride obtained can be industry through being further purified.
Owing to present invention employs common commercially available mineral alkali as catalyzer, without the need to process before using, solubleness is in organic solvent little, easily to be removed by filtering separation after reaction, thus has the advantage reducing technology difficulty 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 that interlock system is for the method for biofuel and carbonic acid glyceride, comprises the following steps:
Natural fats and oils, methylcarbonate and methyl alcohol are that 1:1:5 adds in reactor according to the ratio of amount by the first step, 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 adding natural fats and oils quality 10% in downhill reaction still, at 90 DEG C, stirring heating is after 6 hours, cool to room temperature, and described alkali is the sodium hydroxide of technical grade;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 3 times, remaining as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Embodiment 2
Methyl alcohol promotes that interlock system is for the method for biofuel and carbonic acid glyceride, comprises the following steps:
Natural fats and oils, methylcarbonate and methyl alcohol are that 1:1.1:6 adds in reactor according to the ratio of amount by the first step, 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 adding natural fats and oils quality 10% in downhill reaction still, at 90 DEG C, stirring heating is after 5 hours, cool to room temperature, and described alkali is the mixture of technical grade salt of wormwood and potassium hydroxide mass ratio 1:1;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 3 times, remaining as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Embodiment 3
Methyl alcohol promotes that interlock system is for the method for biofuel and carbonic acid glyceride, comprises the following steps:
Natural fats and oils, methylcarbonate and methyl alcohol are that 1:2:10 adds in reactor according to the ratio of amount by the first step, 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 adding natural fats and oils quality 8% in downhill reaction still, at 70 DEG C, stirring heating is after 5 hours, cool to room temperature, and described alkali is chemical pure hydrated barta product;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 2 times, remaining as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Embodiment 4
Methyl alcohol promotes that interlock system is for the method for biofuel and carbonic acid glyceride, comprises the following steps:
Natural fats and oils, methylcarbonate and methyl alcohol are that 1:1.5:8 adds in reactor according to the ratio of amount by the first step, 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 adding natural fats and oils quality 20% in downhill reaction still, at 80 DEG C, stirring heating is after 6 hours, cool to room temperature, and described alkali is analytical pure potassium hydroxide;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 3 times, remaining as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Embodiment 5
Methyl alcohol promotes that interlock system is for the method for biofuel and carbonic acid glyceride, comprises the following steps:
The first step, be that 1:1.6:9 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, natural fats and oils is the mass ratio after deacidification, dehydration is the rapeseed oil of 1:1 and the mixture of soybean oil, and methylcarbonate and methyl alcohol are the analytical reagent through Non-aqueous processing;
Second step, stir the alkali adding natural fats and oils quality 20% in downhill reaction still, at 60 DEG C, stirring heating is after 6 hours, cool to room temperature, and described alkali is chemical pure hydrated barta;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 3 times, remaining as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Embodiment 6
Methyl alcohol promotes that interlock system is for the method for biofuel and carbonic acid glyceride, comprises the following steps:
The first step, be that 1:3:10 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, natural fats and oils is rapeseed oil after deacidification, dehydration and the mixture of lard, and methylcarbonate and methyl alcohol are the analytical reagent through Non-aqueous processing;
Second step, stir the alkali adding natural fats and oils quality 8% in downhill reaction still, at 85 DEG C, stirring heating is after 6 hours, cool to room temperature, and described alkali is analytical pure sodium hydroxide;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, subtracts methylcarbonate excessive in filtrate and boils off with methyl alcohol pressure, obtain light yellow liquid, be biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 2 times, remaining as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
Claims (7)
1. methyl alcohol promotes that interlock system is for the method for biofuel and carbonic acid glyceride, is characterized in that, comprises the following steps:
The first step, be 1:(1-5 by natural fats and oils, methylcarbonate and methyl alcohol according to volume ratio): (1-10) adds in reactor, natural fats and oils is Vegetable oil lipoprotein, animal grease or both mixtures after deacidification, dehydration, and methylcarbonate and methyl alcohol are the reagent of chemical pure through Non-aqueous processing and above purity;
Second step, stir the alkali adding natural fats and oils quality 5-20% in downhill reaction still, at 60-90 DEG C after stirring heating 4-8 hour, cool to room temperature, described alkali is the salt of wormwood, sodium carbonate, sodium hydroxide, potassium hydroxide, hydrated barta and composition thereof of technical grade and above purity;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 2-3 time, remaining as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and namely obtain carbonic acid glyceride.
2. methyl alcohol according to claim 1 promotes that interlock system is for the method for biofuel and carbonic acid glyceride, is characterized in that, comprises the following steps:
Natural fats and oils, methylcarbonate and methyl alcohol are that 1:1:5 adds in reactor according to the ratio of amount by the first step, 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 adding natural fats and oils quality 10% in downhill reaction still, at 90 DEG C, stirring heating is after 6 hours, cool to room temperature, and described alkali is the sodium hydroxide of technical grade;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 3 times, remaining 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 that interlock system is for the method for biofuel and carbonic acid glyceride, is characterized in that, comprises the following steps:
Natural fats and oils, methylcarbonate and methyl alcohol are that 1:1.1:6 adds in reactor according to the ratio of amount by the first step, 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 adding natural fats and oils quality 10% in downhill reaction still, at 90 DEG C, stirring heating is after 5 hours, cool to room temperature, and described alkali is the mixture of technical grade salt of wormwood and potassium hydroxide mass ratio 1:1;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 3 times, remaining 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 that interlock system is for the method for biofuel and carbonic acid glyceride, is characterized in that, comprises the following steps:
Natural fats and oils, methylcarbonate and methyl alcohol are that 1:2:10 adds in reactor according to the ratio of amount by the first step, 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 adding natural fats and oils quality 8% in downhill reaction still, at 70 DEG C, stirring heating is after 5 hours, cool to room temperature, and described alkali is chemical pure hydrated barta product;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 2 times, remaining 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 that interlock system is for the method for biofuel and carbonic acid glyceride, is characterized in that, comprises the following steps:
Natural fats and oils, methylcarbonate and methyl alcohol are that 1:1.5:8 adds in reactor according to the ratio of amount by the first step, 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 adding natural fats and oils quality 20% in downhill reaction still, at 80 DEG C, stirring heating is after 6 hours, cool to room temperature, and described alkali is analytical pure potassium hydroxide;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 3 times, remaining 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 that interlock system is for the method for biofuel and carbonic acid glyceride, is characterized in that, comprises the following steps:
The first step, be that 1:1.6:9 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, natural fats and oils is the mass ratio after deacidification, dehydration is the rapeseed oil of 1:1 and the mixture of soybean oil, and methylcarbonate and methyl alcohol are the analytical reagent through Non-aqueous processing;
Second step, stir the alkali adding natural fats and oils quality 20% in downhill reaction still, at 60 DEG C, stirring heating is after 6 hours, cool to room temperature, and described alkali is chemical pure hydrated barta;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, by methylcarbonate excessive in filtrate and methyl alcohol pressure reducing and steaming, obtains light yellow liquid, is biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 3 times, remaining 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 that interlock system is for the method for biofuel and carbonic acid glyceride, is characterized in that, comprises the following steps:
The first step, be that 1:3:10 adds in reactor by natural fats and oils, methylcarbonate and methyl alcohol according to the ratio of amount, natural fats and oils is rapeseed oil after deacidification, dehydration and the mixture of lard, and methylcarbonate and methyl alcohol are the analytical reagent through Non-aqueous processing;
Second step, stir the alkali adding natural fats and oils quality 8% in downhill reaction still, at 85 DEG C, stirring heating is after 6 hours, cool to room temperature, and described alkali is analytical pure sodium hydroxide;
3rd step, filters the reactant in reactor, with the methylcarbonate washing adopted in the first step to filter residue white, obtains filtrate;
4th step, subtracts methylcarbonate excessive in filtrate and boils off with methyl alcohol pressure, obtain light yellow liquid, be biofuel crude product;
5th step, by biofuel crude product isopyknic methanol extraction 2 times, remaining as the biofuel after purifying, merges methanol solution, boils off methyl alcohol and obtain carbonic acid glyceride.
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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 of glycerol carbonate and biodiesel |
| CN105642266B (en) * | 2014-11-13 | 2019-01-18 | 中国石油天然气股份有限公司 | Composite solid base catalyst for preparing biodiesel by glycerol-free method and preparation method thereof |
| 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 |
| 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 |
| 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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Patent Citations (5)
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|---|---|---|---|---|
| CN1916114A (en) * | 2006-09-07 | 2007-02-21 | 中国林业科学研究院林产化学工业研究所 | Method for producing biological diesel oil through homogeneous successive reaction |
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