CN101781609A - Method for preparing biodiesel from hemp plant oil - Google Patents
Method for preparing biodiesel from hemp plant oil Download PDFInfo
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- CN101781609A CN101781609A CN201010116729A CN201010116729A CN101781609A CN 101781609 A CN101781609 A CN 101781609A CN 201010116729 A CN201010116729 A CN 201010116729A CN 201010116729 A CN201010116729 A CN 201010116729A CN 101781609 A CN101781609 A CN 101781609A
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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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Abstract
The invention relates to a method for preparing biodiesel from hemp plant oil; and a co-solvent is adopted to fully dissolve alcohol and oil to be homogeneous, is added with a solid catalyst, and is pumped into a tubular reactor to carry out continuous reaction. A static mixer is arranged in the reactor. The reaction temperature is 60 to 300DEG C, the reaction pressure is 1 to 30MPa, the molar ratio of methanol to oil is 3 to 100, the molar ratio of the co-solvent to oil is 1 to 30, the consumption of the catalyst is 0.5 to 5 percent of the mass of the oil, and the reaction time is 10 to 120min. After reaction, through cooling, the catalyst is filtered and recovered, and then enters a flash tank to recover the alcohol and the co-solvent, and crude biodiesel is prepared by staying still and being layered; and after distillation, a biodiesel product is prepared, and the quality yield is more than 95 percent. The process is simple, the reaction can be carried out continuously, the catalyst, the alcohol and the co-solvent can be recycled, the equipment investment is low, and the production cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of biofuel, relate in particular to a kind of fibre of flax for textile material grease that utilizes and be the feedstock production method of bio-diesel oil, belong to biology and technical field of chemical engineering.
Background technology
Biofuel is the fatty acid methyl ester that animal and plant grease and methyl alcohol prepare through transesterification reaction, and method commonly used has acid catalysis, base catalysis, solid acid alkali catalytic, enzyme catalysis, supercritical methanol technology etc.Usually be catalyzer with KOH, methyl alcohol and grease mol ratio are 6: 1,65 ℃ of down reactions 1 hour, treat the product layering after, upper strata liquid obtains fatty acid methyl ester after through processing such as distillating carbinol, pickling, washing, drying, rectifying.Chinese patent CN 101138737A discloses a kind of molecular sieve solid alkaline catalysts and the application in producing biofuel, with the MCM-41 mesopore molecular sieve is carrier, the carrying alkali metal oxide compound, preparing biodiesel by catalyzing oil using can overcome the problem of homogeneous catalyst separation difficulty.Chinese patent CN 101225323A discloses a kind of supercritical extraction-transesterification reaction coupled method and has directly prepared method of bio-diesel oil by raw material, at 10～30MPa, 30～70 ℃ high-pressure carbon dioxide and a certain amount of low-carbon alcohol are carried out supercritical extraction, the mixed solution that extraction obtains is delivered in the fixed bed high-pressure reactor that catalyzer is housed and is carried out transesterification reaction, and product obtains biofuel after separating.Chinese patent 200610114033.4 discloses the method and apparatus of a kind of grease or lipid acid preparing low-carbon olefin by catalytically cracking, adopt fluidized-bed reactor, temperature of reaction is 400～700 ℃, reaction process need add water vapour, catalyst levels is 5～25 times of oil quality, catalyst reaction is once with regard to inactivation, and split product comprises C
1, C
2, C
3, C
4, CO, CO
2Deng, complicated component, severe reaction conditions, production cost height.The main products of high temperature pyrolytic cracking is a biogasoline, and biofuel is its byproduct, and the thermo-cracking equipment costs an arm and a leg.Chinese patent 200710065393.4 discloses a kind of integrated hydrogenation and has prepared method of bio-diesel oil, soybean wet goods vegetables oil is mixed with petroleum base diesel oil such as straight-run diesel oils, at 250～450 ℃ of temperature, hydrogen partial pressure is to carry out hydrofining or hydrocracking reaction under the condition that exists of 3.0～20.0MPa and catalyzer, vegetables oil is converted into biofuel, by-product propane and a small amount of lower carbon number hydrocarbons.Chinese patent 200810105647.5 discloses a kind of hydrogenation deoxidation catalyst that is used for the production biofuel, the mixture of vegetable and animals oils or vegetable and animals oils and fossil oil oil transforms through hydrogenation deoxidation and generates biofuel, 250～450 ℃ of temperature of reaction, hydrogen partial pressure are 1.0～10.0MPa, hydrogen to oil volume ratio 100～1000, diesel yield reaches more than 80%, yield of gasoline only 2%, gaseous product is the above component of propane, methane, ethane and C6.
Common method for producing biodiesel is intermittently to carry out, if raw material acid value height also needs grease is carried out pre-esterification, and complex process, pollutant emission is many; All there are severe reaction conditions in Pintsch process and hydrogenation technique, the shortcoming that product yield is low.
Summary of the invention
For overcoming defective described in the prior art, the invention provides a kind of method by the fibre of flax for textile material preparing biodiesel from lipid, may further comprise the steps:
(1) makes grease, short chain alcohol, cosolvent and solid catalyst uniform mixing, and under certain temperature and pressure, react;
(2) reaction product is filtered to reclaim solid catalyst;
(3) liquid product after the filtration enters flash tank and reclaims short chain alcohol and cosolvent;
(4) product of step (3) is clarified separation, the upper strata obtains coarse biodiesel, and lower floor obtains raw glycerine;
(5) coarse biodiesel is carried out obtaining biofuel after rectified purified.
Preferably, described short chain alcohol is the alcohol of C1-6, and cosolvent is the trimethyl carbinol, normal hexane, tetrahydrofuran (THF) or ethyl acetate, and solid catalyst is solid acid catalyst or solid base catalyst.
Preferably, wherein the reaction conditions of step (1) is: pressure 1～30MPa, 60～350 ℃ of temperature of reaction, short chain alcohol and greasy mol ratio 3～100, cosolvent and greasy mol ratio 1～30, solid catalyst consumption be oil quality 0.5～5%, the reaction times is 10～120 minutes.
Preferably, wherein said solid acid catalyst is the ZrSO after the acidifying
4, or the TiSO after the acidifying
4Solid base catalyst is an alkaline earth metal oxide, the alkaline-earth alkoxides compound, or active ingredient is the loaded catalyst of alkaline-earth metal.
Preferably, described alkaline earth metal oxide is MgO, CaO, SrO, and BaO.
Preferably, described grease is: oleum lini, Viscotrol C, hemp oil, jute oil, bluish dogbane oil, cannabis oil or sisal hemp oil.
Preferably, being reflected in the tubular reactor of step (1) carried out, and described tubular reactor inside has outside static mixer, the pipe electrically heated and heat insulation module are arranged, outlet band reducing valve.
Feature of the present invention and effect:
1) reaction can be carried out continuously, operates easylier, and technology is simpler;
2) adopt cosolvent to promote dissolving each other of pure oil phase, simplified reaction conditions, yield height, reduced product cost, and do not need preheater before the mixing of alcohol oil;
3) adopt solid catalyst, can recycling use, no neutralization, pickling, water-washing step, non-pollutant discharge;
4) static mixer in the tubular reactor helps the mixing of liquid-solid two-phase.
Description of drawings
Fig. 1 is preparation method's of the present invention schema.
The 1-grease storage tank
2-alcohol storage tank
3-cosolvent storage tank
4-glycerine storage tank
5-biofuel storage tank
The 6-rectifying tower
The 7-flash tank
The 8-clarifying tank
The 9-strainer
The 10-water cooler
The 11-reactor
The 12-ram pump
The 13-mixer
Embodiment
The following examples are used to further specify the present invention rather than are used for limiting the present invention.
Embodiment 1
With the oleum lini is raw material, and methyl alcohol oleum lini mol ratio is 9: 1, the trimethyl carbinol: the oleum lini mol ratio is 6: 1, and CaO is a catalyzer, and catalyst levels is 2.5% of an oleum lini quality.After mixing in stirring mixer, liquid phase is dissolved each other fully.With ram pump material is pumped into tubular reactor then, pipe range is 1.5m, and caliber is Φ 20 * 1mm, and material is a stainless steel.Reaction conditions is 12MPa, 250 ℃, and 50 minutes reaction times.Enter the water cooler cooling after the reducing valve discharging, product reclaims solid base catalyst through strainer, obtains the biofuel product through after flash distillation, standing demix and the rectifying again, and the mass yield of biofuel is 95.4%.
Embodiment 2
With the Viscotrol C is raw material, and the mol ratio of methyl alcohol and Viscotrol C is 6: 1, and the mol ratio of tetrahydrofuran (THF) and Viscotrol C is 12: 1, and SrO is a catalyzer, and catalyst levels is 2.0% of a Viscotrol C quality.Mix in stirring mixer, with ram pump material is pumped into tubular reactor then, pipe range is 1.5m, and caliber is Φ 20 * 1mm, and material is a stainless steel.Reaction conditions is 10MPa, 220 ℃, and 40 minutes reaction times.Enter the water cooler cooling after the reducing valve discharging, product reclaims solid base catalyst through strainer, obtains the biofuel product through after flash distillation, standing demix and the rectifying again, and the mass yield of biofuel is 96.4%.
Embodiment 3
With the oleum lini is raw material, and methyl alcohol oleum lini mol ratio is 12: 1, the trimethyl carbinol: the oleum lini mol ratio is 12: 1, and calcium methylate is a catalyzer, and catalyst levels is 2.0% of an oleum lini quality.After mixing in stirring mixer, liquid phase is dissolved each other fully.With ram pump material is pumped into tubular reactor then, pipe range is 1.5m, and caliber is Φ 20 * 1mm, and material is a stainless steel.Reaction conditions is 10MPa, 240 ℃, and 60 minutes reaction times.Enter the water cooler cooling after the reducing valve discharging, product reclaims solid base catalyst through strainer, obtains the biofuel product through after flash distillation, standing demix and the rectifying again, and the mass yield of biofuel is 95.2%.
It is pointed out that under the prerequisite that does not break away from spirit of the present invention those of ordinary skills can make various changes or change to the present invention, these changes or change fall within protection scope of the present invention equally.Protection scope of the present invention is as the criterion with appending claims.
Claims (7)
1. method by the fibre of flax for textile material preparing biodiesel from lipid may further comprise the steps:
(1) makes grease, short chain alcohol, cosolvent and solid catalyst uniform mixing, and under certain temperature and pressure, react;
(2) reaction product is filtered to reclaim solid catalyst;
(3) liquid product after the filtration enters flash tank and reclaims short chain alcohol and cosolvent;
(4) product of step (3) is clarified separation, the upper strata obtains coarse biodiesel, and lower floor obtains raw glycerine;
(5) coarse biodiesel is carried out obtaining biofuel after rectified purified.
2. the method for claim 1, described short chain alcohol is C
1-6Alcohol, cosolvent is the trimethyl carbinol, normal hexane, tetrahydrofuran (THF) or ethyl acetate, solid catalyst is solid acid catalyst or solid base catalyst.
3. method as claimed in claim 1 or 2, wherein the reaction conditions of step (1) is: pressure 1～30MPa, 60～350 ℃ of temperature of reaction, short chain alcohol and greasy mol ratio 3～100, cosolvent and greasy mol ratio 1～30, solid catalyst consumption be oil quality 0.5～5%, the reaction times is 10～120 minutes.
4. method as claimed in claim 2, wherein said solid acid catalyst are the ZrSO after the acidifying
4, or the TiSO after the acidifying
4Solid base catalyst is an alkaline earth metal oxide, the alkaline-earth alkoxides compound, or active ingredient is the loaded catalyst of alkaline-earth metal.
5. method as claimed in claim 4, described alkaline earth metal oxide are MgO, CaO, SrO, and BaO.
6. as claim 3 or 4 described methods, described grease is: oleum lini, Viscotrol C, hemp oil, jute oil, bluish dogbane oil, cannabis oil or sisal hemp oil.
7. the method for claim 1, being reflected in the tubular reactor of step (1) carried out, and described tubular reactor inside has that static mixer, pipe are outer electrically heated and heat insulation module, an outlet band reducing valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010116729A CN101781609A (en) | 2010-03-03 | 2010-03-03 | Method for preparing biodiesel from hemp plant oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010116729A CN101781609A (en) | 2010-03-03 | 2010-03-03 | Method for preparing biodiesel from hemp plant oil |
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| Publication Number | Publication Date |
|---|---|
| CN101781609A true CN101781609A (en) | 2010-07-21 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010116729A Pending CN101781609A (en) | 2010-03-03 | 2010-03-03 | Method for preparing biodiesel from hemp plant oil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250695A (en) * | 2011-06-23 | 2011-11-23 | 南昌大学 | Method for continuously converting oil into fatty acid short chain alcohol ester |
| CN102807922A (en) * | 2011-05-31 | 2012-12-05 | 中国石油化工股份有限公司 | Preparation method for fatty acid ester |
| CN103074162A (en) * | 2013-01-06 | 2013-05-01 | 盐城师范学院 | Method for preparing biodiesel |
| TWI493025B (en) * | 2013-09-26 | 2015-07-21 | Structure of a kind of solid diesel catalyst for solid diesel catalyst | |
| CN106467453A (en) * | 2016-08-31 | 2017-03-01 | 贝利化学（张家港）有限公司 | A kind of method that pipeline reactor synthesizes p-Methoxybenzoic acid |
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| CN2786122Y (en) * | 2005-05-19 | 2006-06-07 | 张�诚 | Production equipment for biological diesel oil |
| CN1928016A (en) * | 2006-09-28 | 2007-03-14 | 张海军 | Preparation method of biological diesel oil |
| CN1952047A (en) * | 2005-10-19 | 2007-04-25 | 中国石油化工股份有限公司 | Production process of biological diesel oil |
| CN1970692A (en) * | 2006-12-07 | 2007-05-30 | 天津大学 | Process for preparing biological diesel oil by using loop reactor |
| CN101012389A (en) * | 2007-02-02 | 2007-08-08 | 清华大学 | Method of preparing biological diesel oil catalyzed by solid base |
| CN101067091A (en) * | 2007-06-08 | 2007-11-07 | 清华大学 | Solid catalysis process of preparing biodiesel oil continuously with high acid value material |
-
2010
- 2010-03-03 CN CN201010116729A patent/CN101781609A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2786122Y (en) * | 2005-05-19 | 2006-06-07 | 张�诚 | Production equipment for biological diesel oil |
| CN1952047A (en) * | 2005-10-19 | 2007-04-25 | 中国石油化工股份有限公司 | Production process of biological diesel oil |
| CN1928016A (en) * | 2006-09-28 | 2007-03-14 | 张海军 | Preparation method of biological diesel oil |
| CN1970692A (en) * | 2006-12-07 | 2007-05-30 | 天津大学 | Process for preparing biological diesel oil by using loop reactor |
| CN101012389A (en) * | 2007-02-02 | 2007-08-08 | 清华大学 | Method of preparing biological diesel oil catalyzed by solid base |
| CN101067091A (en) * | 2007-06-08 | 2007-11-07 | 清华大学 | Solid catalysis process of preparing biodiesel oil continuously with high acid value material |
Non-Patent Citations (1)
| Title |
|---|
| 《安徽农业科学》 20091001 徐桂转等 用于制备生物柴油的固体催化剂研究进展 1-7 第37卷, 第28期 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807922A (en) * | 2011-05-31 | 2012-12-05 | 中国石油化工股份有限公司 | Preparation method for fatty acid ester |
| CN102250695A (en) * | 2011-06-23 | 2011-11-23 | 南昌大学 | Method for continuously converting oil into fatty acid short chain alcohol ester |
| CN103074162A (en) * | 2013-01-06 | 2013-05-01 | 盐城师范学院 | Method for preparing biodiesel |
| TWI493025B (en) * | 2013-09-26 | 2015-07-21 | Structure of a kind of solid diesel catalyst for solid diesel catalyst | |
| CN106467453A (en) * | 2016-08-31 | 2017-03-01 | 贝利化学（张家港）有限公司 | A kind of method that pipeline reactor synthesizes p-Methoxybenzoic acid |
| CN106467453B (en) * | 2016-08-31 | 2018-10-16 | 贝利化学（张家港）有限公司 | A kind of method of pipeline reactor synthesis P-methoxybenzoic acid |
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Application publication date: 20100721 |