CN104560411A - Technique for preparing fatty acid methyl ester by biological process - Google Patents
Technique for preparing fatty acid methyl ester by biological process Download PDFInfo
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- CN104560411A CN104560411A CN201410802813.2A CN201410802813A CN104560411A CN 104560411 A CN104560411 A CN 104560411A CN 201410802813 A CN201410802813 A CN 201410802813A CN 104560411 A CN104560411 A CN 104560411A
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- esterification
- reaction
- fatty acid
- methyl ester
- acid methyl
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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
- C11C3/10—Ester interchange
-
- 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
- C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
-
- 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
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a technique for preparing fatty acid methyl ester by a biological process, which comprises the following steps of esterification reaction and ester exchange reaction and adopts waste oil, methanol, concentrated sulfuric acid and sodium hydroxide as raw materials. The technique specifically comprises the following steps: esterification reaction, esterification reaction after-treatment, ester exchange reaction and ester exchange reaction after-treatment. The kitchen waste, such as waste oil and the like, is used as the raw material, thereby effectively utilizing the waste as the raw material; and thus, the technique has high environment friendliness. By adopting the two-step reaction process (including esterification reaction and ester exchange reaction), the reaction process is simple and efficient, and has high conversion rate. The produced fatty acid methyl ester is biodiesel, and thus, has the advantages of environment-friendly use effect, low pollution and broad market prospects.
Description
Technical field
The present invention relates to chemical production technology, particularly adopt biological process to produce the processing method of fatty acid methyl ester.
Background technology
The progressively increase of diesel and gasoline ratio, constantly the improving of soaring again and again and modern diesel engine of gas price is just impelling the trend of automotive type diesel oil to accelerate.Increasing newly over half in vehicle in Europe is diesel vehicle, the commercial car of the U.S. 90% is diesel vehicle, the current heavy truck of China and light truck are diesel vehicle substantially, in passenger vehicle, the ratio of diesel engine improves day by day, car also starts to produce diesel vehicle, therefore the demand of diesel oil is significantly increased, and the supply wretched insufficiency of worldwide diesel oil, therefore to the wide development space that biofuel stays.
The composition of biofuel is fatty acid methyl ester, along with the improvement of fatty-acid methyl ester producing process and quality product, use the engine of ordinary diesel oil that biofuel also can be used as supplying raw material when not doing any change, and biofuel and ordinary diesel oil can realize arbitrary proportion mixing in fuel tank.In addition Alternative Diesel Fuel raw materials used along with scale plantation price increasingly cheap, the production cost of Alternative Diesel Fuel is progressively declined, reduces with the price variance of common diesel.And biofuel is as the petroleum diesel substitute of high-quality, its maximum advantage is environmental friendliness, pollutes low.
In addition, fatty acid methyl ester also has certain chemical industry purposes, if epoxy aliphatic acid methyl ester is as epoxy soybean oil substitute products, not only cheap, purposes and quality all reach requirement, simultaneously, produce fatty alcohol with fatty acid methyl ester, technical maturity, can substitute the fatty alcohol that petrification is produced completely.Therefore, exploitation biofuel and fatty acid methyl ester agree with mutually with the direction that current petrochemical industry adjusts oil product structure, improve diesel and gasoline ratio, have broad prospects.
Therefore, the problems referred to above be the technique adopted in the producing process of fatty acid methyl ester design and use should pay attention to and the problem solved.
Summary of the invention
For above-mentioned Problems existing, the invention provides the processing method that biological process produces fatty acid methyl ester.
Technical solution of the present invention is: biological process produces the processing method of fatty acid methyl ester, adopts two-step approach, is respectively esterification and transesterification reaction, and raw material adopts waste grease, methyl alcohol, the vitriol oil and sodium hydroxide, specifically carries out according to following technique:
A. esterification: will eat in the waste grease suction reaction kettle of the esterification such as kitchen with oil pump, and add the vitriol oil as catalyzer in reaction kettle of the esterification, then adopt and take out pump methyl alcohol is squeezed in reaction kettle of the esterification, carry out esterification;
B. esterification aftertreatment: after esterification terminates, residue methanol rectification reclaims, and sulfuric acid residual in reactor and part water discharge process;
C. transesterification reaction: the head product formed in reaction kettle of the esterification is thick methyl esters, adds sodium hydroxide as catalyzer in the reaction kettle of the esterification through aftertreatment, and thick methyl esters carries out transesterification reaction with the methyl alcohol newly inputted;
D. transesterification reaction aftertreatment: after transesterification reaction terminates, catalyzer sodium hydroxide generates soap with raw material reaction, soap and glycerine are discharged from reaction kettle of the esterification, the end product generated enters in vacuum rectification tower and carries out distillation operation from reaction kettle of the esterification, vacuum rectification tower is warming up to 250 DEG C ~ 290 DEG C and carries out rectified purified under condition of negative pressure, obtains fatty acid methyl ester.
Further improvement of the present invention is: in the aftertreatment of step b esterification, also comprise methanol rectifying tower, after esterification terminates, reaction system in reaction kettle of the esterification is heated, be warming up to 100 DEG C reclaim the moisture excessive useless methyl alcohol of part enter into methanol rectifying tower, methyl alcohol after rectifying tower rectifying again through tertiary effluent is cold be back to use after batch esterification in.
Further improvement of the present invention is: in the aftertreatment of step b esterification, and sulfuric acid residual in reactor and part water enter in oil trap after oil removal from reaction kettle of the esterification, and the sewage of generation enters Sewage treatment systems and processes.
Further improvement of the present invention is: the massfraction that the amount of the vitriol oil added in step a esterification accounts for the total material of esterification is 0.4% ~ 0.8%, and the massfraction that the amount of the sodium hydroxide added in step c transesterification reaction accounts for the total material of transesterification reaction is 0.2% ~ 0.5%.
Further improvement of the present invention is: in the aftertreatment of steps d transesterification reaction, glycerine and soap are discharged from reactor, the soap of discharging and glycerine are processed, by in glycerine and soap input reduction kettle, and in reduction kettle, add a small amount of hydrochloric acid, soap is reduced into grease, grease can continue for esterification as raw material after layering, and in reduction kettle remaining G & W and trace salt input alkali mixing tank in mix with sodium hydroxide after again through vacuum hydro-extraction, enter in glycerol distillation tower after filtering out salinity, in still-process, adopt batch distillation method to be discharged by the salt of separating out, cut obtains the glycerine that content is 90% ~ 99%, the colourless glycerine of 90% ~ 99% is formed again through activated carbon decolorizing, can be used as other production to glycerine demand.
Biological process of the present invention produces the processing method of fatty acid methyl ester, the present invention adopts biological process to produce fatty acid methyl ester, raw material adopts the waste greases such as meal kitchen, main containing triglyceride level and free lipid acid in waste grease, reacted by two-step approach, be respectively esterification and transesterification reaction, mainly react in a kettle. according to following equation:
Esterification:
Transesterification reaction:
It is rectified purified by vacuum rectification tower that reaction terminates rear crude product, and crude product is warming up to 250 DEG C ~ 300 DEG C and carries out rectified purified under condition of negative pressure, obtains final product fatty acid methyl ester.
The invention has the beneficial effects as follows: the present invention adopts biological process to produce fatty acid methyl ester, raw material adopts waste grease, effectively make use of waste as raw material, there is high-strength environmental protection efficacy, and reaction process is simply efficient, the crude product finally obtained carries out distillation operation by vacuum rectification tower, and make end reaction transformation efficiency reach more than 98%, in the finished product obtained, fatty acid methyl ester is higher than 90%.End product is fatty acid methyl ester, is biofuel, and the biofuel of producing in this way is as the petroleum diesel substitute of high-quality, environmental friendliness, pollute low, without sulfurous gas, particulate emissions after burning, carbon monoxide, Carbon emission are only 10% ~ 20% of petroleum diesel.There are extraordinary result of use and wide market outlook.
Accompanying drawing explanation
Fig. 1 is the schema that biological process of the present invention produces the processing method of fatty acid methyl ester.
Embodiment
In order to deepen the understanding of the present invention, be described in further detail the present invention below in conjunction with embodiment, this embodiment, only for explaining the present invention, not forming protection scope of the present invention and limiting.
The present embodiment provides biological process to produce the processing method of fatty acid methyl ester, adopts two-step approach, is respectively esterification and transesterification reaction, and raw material adopts waste grease, methyl alcohol, the vitriol oil and sodium hydroxide, specifically carries out according to following technique:
A. esterification: will eat in the waste grease suction reaction kettle of the esterification such as kitchen with oil pump, and add the vitriol oil as catalyzer in reaction kettle of the esterification, then adopt and take out pump methyl alcohol is squeezed in reaction kettle of the esterification, carry out esterification;
B. esterification aftertreatment: after esterification terminates, residue methanol rectification reclaims, and sulfuric acid residual in reactor and part water discharge process;
C. transesterification reaction: the head product formed in reaction kettle of the esterification is thick methyl esters, adds sodium hydroxide as catalyzer in the reaction kettle of the esterification through aftertreatment, and thick methyl esters carries out transesterification reaction with the methyl alcohol newly inputted;
D. transesterification reaction aftertreatment: after transesterification reaction terminates, catalyzer sodium hydroxide generates soap with raw material reaction, soap and glycerine are discharged from reaction kettle of the esterification, the end product generated enters in vacuum rectification tower and carries out distillation operation from reaction kettle of the esterification, vacuum rectification tower is warming up to 250 DEG C ~ 290 DEG C under condition of negative pressure, be preferably 270 DEG C, carry out rectified purified, obtain fatty acid methyl ester.
In the aftertreatment of step b esterification, also comprise methanol rectifying tower, after esterification terminates, reaction system in reaction kettle of the esterification is heated, be warming up to 100 DEG C reclaim the moisture excessive useless methyl alcohol of part enter into methanol rectifying tower, methyl alcohol after rectifying tower rectifying again through tertiary effluent is cold be back to use after batch esterification in.In the aftertreatment of step b esterification, sulfuric acid residual in reactor and part water enter in oil trap after oil removal from reaction kettle of the esterification, and the sewage of generation enters Sewage treatment systems and processes.The massfraction that the amount of the vitriol oil added in step a esterification accounts for the total material of esterification is 0.4% ~ 0.8%, be preferably 0.5%, the massfraction that the amount of the sodium hydroxide added in step c transesterification reaction accounts for the total material of transesterification reaction is 0.2% ~ 0.5%, is preferably 0.3%.In the aftertreatment of steps d transesterification reaction, glycerine and soap are discharged from reactor, the soap of discharging and glycerine are processed, by in glycerine and soap input reduction kettle, and in reduction kettle, add a small amount of hydrochloric acid, soap is reduced into grease, grease can continue for esterification as raw material after layering, and in reduction kettle remaining G & W and trace salt input alkali mixing tank in mix with sodium hydroxide after again through vacuum hydro-extraction, enter in glycerol distillation tower after filtering out salinity, in still-process, adopt batch distillation method to be discharged by the salt of separating out, cut obtains the glycerine that content is 90% ~ 99%, the colourless glycerine of 90% ~ 99% is formed again through activated carbon decolorizing, can be used as other production to glycerine demand.
The present embodiment biological process produces the processing method of fatty acid methyl ester, the present invention adopts biological process to produce fatty acid methyl ester, raw material adopts the waste greases such as meal kitchen, main containing triglyceride level and free lipid acid in waste grease, reacted by two-step approach, be respectively esterification and transesterification reaction, mainly react in a kettle. according to following equation:
Esterification:
Transesterification reaction:
It is rectified purified by vacuum rectification tower that reaction terminates rear crude product, and crude product is warming up to 250 DEG C ~ 300 DEG C and carries out rectified purified under condition of negative pressure, obtains final product fatty acid methyl ester.
The beneficial effect of the present embodiment is: the present invention adopts biological process to produce fatty acid methyl ester, raw material adopts waste grease, effectively make use of waste as raw material, there is high-strength environmental protection efficacy, and reaction process is simply efficient, the crude product finally obtained carries out distillation operation by vacuum rectification tower, and make end reaction transformation efficiency reach more than 98%, in the finished product obtained, fatty acid methyl ester is higher than 90%.End product is fatty acid methyl ester, is biofuel, and the biofuel of producing in this way is as the petroleum diesel substitute of high-quality, environmental friendliness, pollute low, without sulfurous gas, particulate emissions after burning, carbon monoxide, Carbon emission are only 10% ~ 20% of petroleum diesel.There are extraordinary result of use and wide market outlook.
Claims (5)
1. biological process produces the processing method of fatty acid methyl ester, it is characterized in that: adopt two-step approach, be respectively esterification and transesterification reaction, and raw material adopts waste grease, methyl alcohol, the vitriol oil and sodium hydroxide, specifically carries out according to following technique:
A. esterification: will eat in the waste grease suction reaction kettle of the esterification such as kitchen with oil pump, and add the vitriol oil as catalyzer in reaction kettle of the esterification, then adopt and take out pump methyl alcohol is squeezed in reaction kettle of the esterification, carry out esterification;
B. esterification aftertreatment: after esterification terminates, residue methanol rectification reclaims, and sulfuric acid residual in reactor and part water discharge process;
C. transesterification reaction: the head product formed in reaction kettle of the esterification is thick methyl esters, adds sodium hydroxide as catalyzer in the reaction kettle of the esterification through aftertreatment, and thick methyl esters carries out transesterification reaction with the methyl alcohol newly inputted;
D. transesterification reaction aftertreatment: after transesterification reaction terminates, catalyzer sodium hydroxide generates soap with raw material reaction, soap and glycerine are discharged from reaction kettle of the esterification, the end product generated enters in vacuum rectification tower and carries out distillation operation from reaction kettle of the esterification, vacuum rectification tower is warming up to 250 DEG C ~ 290 DEG C and carries out rectified purified under condition of negative pressure, obtains fatty acid methyl ester.
2. biological process according to claim 1 produces the processing method of fatty acid methyl ester, it is characterized in that: in the aftertreatment of step b esterification, also comprise methanol rectifying tower, after esterification terminates, reaction system in reaction kettle of the esterification is heated, be warming up to 100 DEG C reclaim the moisture excessive useless methyl alcohol of part enter into methanol rectifying tower, methyl alcohol after rectifying tower rectifying again through tertiary effluent is cold be back to use after batch esterification in.
3. biological process according to claim 1 produces the processing method of fatty acid methyl ester, it is characterized in that: in the aftertreatment of step b esterification, sulfuric acid residual in reactor and part water enter in oil trap after oil removal from reaction kettle of the esterification, and the sewage of generation enters Sewage treatment systems and processes.
4. biological process according to claim 1 produces the processing method of fatty acid methyl ester, it is characterized in that: the massfraction that the amount of the vitriol oil added in step a esterification accounts for the total material of esterification is 0.4% ~ 0.8%, the massfraction that the amount of the sodium hydroxide added in step c transesterification reaction accounts for the total material of transesterification reaction is 0.2% ~ 0.5%.
5. biological process according to claim 1 produces the processing method of fatty acid methyl ester, it is characterized in that: in the aftertreatment of steps d transesterification reaction, glycerine and soap are discharged from reactor, the soap of discharging and glycerine are processed, by in glycerine and soap input reduction kettle, and in reduction kettle, add a small amount of hydrochloric acid, soap is reduced into grease, grease can continue for esterification as raw material after layering, and in reduction kettle remaining G & W and trace salt input alkali mixing tank in mix with sodium hydroxide after again through vacuum hydro-extraction, enter in glycerol distillation tower after filtering out salinity, in still-process, adopt batch distillation method to be discharged by the salt of separating out, cut obtains the glycerine that content is 90% ~ 99%, the colourless glycerine of 90% ~ 99% is formed again through activated carbon decolorizing, can be used as other production to glycerine demand.
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| CN201410802813.2A CN104560411A (en) | 2014-12-23 | 2014-12-23 | Technique for preparing fatty acid methyl ester by biological process |
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| CN201410802813.2A CN104560411A (en) | 2014-12-23 | 2014-12-23 | Technique for preparing fatty acid methyl ester by biological process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219973A (en) * | 2017-12-21 | 2018-06-29 | 山东大学深圳研究院 | The method for preparing biodiesel using kitchen or slaughterhouse animal solid waste |
| CN111542584A (en) * | 2017-11-14 | 2020-08-14 | 沙特阿拉伯石油公司 | Waste vegetable oil emulsifier for reverse emulsion drilling fluid |
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| CN101805671A (en) * | 2010-04-09 | 2010-08-18 | 上海中器环保科技有限公司 | Method for using waste oil for carrying out one-step method acid catalysis to prepare biodiesel |
| CN102021082A (en) * | 2010-12-02 | 2011-04-20 | 北京工商大学 | Method for preparing fatty acid methyl ester and glycerol from kitchen waste oil by utilizing acid-base two-step method |
| CN103421548A (en) * | 2012-05-14 | 2013-12-04 | 陕西德融新能源股份有限公司 | Preparation technology of biodiesel produced from non refined grease |
-
2014
- 2014-12-23 CN CN201410802813.2A patent/CN104560411A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805671A (en) * | 2010-04-09 | 2010-08-18 | 上海中器环保科技有限公司 | Method for using waste oil for carrying out one-step method acid catalysis to prepare biodiesel |
| CN102021082A (en) * | 2010-12-02 | 2011-04-20 | 北京工商大学 | Method for preparing fatty acid methyl ester and glycerol from kitchen waste oil by utilizing acid-base two-step method |
| CN103421548A (en) * | 2012-05-14 | 2013-12-04 | 陕西德融新能源股份有限公司 | Preparation technology of biodiesel produced from non refined grease |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111542584A (en) * | 2017-11-14 | 2020-08-14 | 沙特阿拉伯石油公司 | Waste vegetable oil emulsifier for reverse emulsion drilling fluid |
| US11427744B2 (en) | 2017-11-14 | 2022-08-30 | Saudi Arabian Oil Company | Waste vegetable oil-based emulsifier for invert emulsion drilling fluid |
| CN108219973A (en) * | 2017-12-21 | 2018-06-29 | 山东大学深圳研究院 | The method for preparing biodiesel using kitchen or slaughterhouse animal solid waste |
| CN108219973B (en) * | 2017-12-21 | 2021-08-03 | 山东大学深圳研究院 | Method for preparing biodiesel by utilizing kitchen or slaughterhouse animal solid waste |
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