CN104560412A - Preparation method for biodiesel - Google Patents
Preparation method for biodiesel Download PDFInfo
- Publication number
- CN104560412A CN104560412A CN201410814292.2A CN201410814292A CN104560412A CN 104560412 A CN104560412 A CN 104560412A CN 201410814292 A CN201410814292 A CN 201410814292A CN 104560412 A CN104560412 A CN 104560412A
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- China
- Prior art keywords
- temperature
- fatty acid
- vacuum
- production method
- biofuel
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Classifications
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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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
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- 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
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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
-
- 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)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Fats And Perfumes (AREA)
- Liquid Carbonaceous Fuels (AREA)
Abstract
The invention discloses a preparation method for biodiesel. The production method comprises the following steps: adding waste grease and glycerine in a reaction still according to a mass ratio of 100:(18-20); adding an acid catalyst under a vacuum stirring condition; conducting catalytic reaction for 2-3 h at a temperature of 110-150 DEG C; separating the generated fatty glyceride and water; conducting circulating reflux transesterification reaction on the fatty glyceride methanol according to a mass ratio of 100:(13-15) for 0.5-1 h at a temperature of 70-110 DEG C under an alkali catalyst vacuum condition; separating crude fatty acid methyl ester and a by-product regenerative glycerine in the supernatant liquor obtained from transesterification; collecting methanol and water in vacuum; adding the crude fatty acid methyl ester into a rectification tower; controlling cooling water temperature at 40-60 DEG C under a vacuum condition; carrying out rectification at 210-230 DEG C to obtain refined fatty acid methyl ester, that is, the biodiesel.
Description
Technical field
The present invention relates to the production method of biofuel, belong to Biomass Energy Utilization field.
Background technology
Not low because market raw material waste grease acid value is high, methyl alcohol easily consumes the huge height of valency at present, the industrialization of existing enterprise of China utilizes waste grease and methyl alcohol direct esterification transesterify, utilize waste grease and methanol production biofuel cost to improve constantly, reason uses a large amount of methyl alcohol to consume completely in the esterification reaction cannot regenerate.
Summary of the invention
The object of the invention is: the production method that a kind of biofuel is provided,
With the high acid value waste animal and vegetable oil of cheapness for raw material, the biofuel of the renewable recycling of cyclic production.
Technical solution of the present invention is that this production method comprises the following steps: join in reactor in 100:18 ~ 20 in mass ratio by waste grease and glycerol, an acidic catalyst is added under vacuum stirring condition, temperature 110 ~ 150 DEG C of catalyzed reaction 2 ~ 3h, are separated the glycerin fatty acid ester and water that generate; By glycerin fatty acid ester and methyl alcohol in mass ratio 100:13 ~ 15 under basic catalyst vacuum condition, temperature 70 ~ 110 DEG C of pump around circuit transesterification reaction 0.5 ~ 1h, fatty acid methyl ester and by product glycerol is isolated from transesterify gained clarified liq, and vacuum collection methyl alcohol and water; Crude fatty acid methyl ester adds rectifying tower, and controlled cooling model water temperature 40 ~ 60 DEG C, temperature 210 ~ 230 DEG C of rectifying obtain refined fat acid methyl esters, i.e. biofuel under vacuum.
Wherein, the consumption of described an acidic catalyst is 0.2 ~ 0.25% of waste grease and glycerol total mass, and an acidic catalyst is methylsulphonic acid, tosic acid.
Wherein, basic catalyst consumption is 0.15 ~ 0.20% of glycerin fatty acid ester and methyl alcohol total mass, and basic catalyst is sodium methylate.
Wherein, vacuum tightness 0.08-0.095mpa, mixing speed 70 revs/min.
The invention has the beneficial effects as follows:
1, a kind of biofuel of the present invention, refining transparent, its cold filter clogging temperature, close flash point, normal temperature kinematic viscosity and acid value all meet the related request of GB GB/T20828-2014 biodiesel technology performance after testing.
2, biofuel of the present invention utilizes waste grease, not only turns waste into wealth, and decreases environmental pollution.
3, biofuel of the present invention utilizes waste grease and glycerol to generate a large amount of by product glycerol and water under an acidic catalyst, basic catalyst condition, by product glycerol is by collection and treatment Reusability, trans-utilization rate is high, reduce the security risk using methyl alcohol in production process, favourable guarantee Manufacturing Worker and environmental safety, and production process uses vacuum successive reaction, shorten and produce the reaction times, save production cost.
4, the production technique operation steps of biofuel of the present invention is simple, and safe ready, is convenient to scale operation.
5, utilize cheap high acid value waste animal and vegetable oil to carry out esterification and transesterification reaction by glycerol at an acidic catalyst and generate the important substitute products of petrifaction diesel that fatty acid methyl ester is desirable low in price, there is the feature of environmental protection and recyclability, economic worth is high, meets national sustainable development policy.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described further, but protection scope of the present invention is not limited in this.
In the embodiment of the present invention, the testing method of flash-point is carried out according to " GB/T261-2008 testing method foundation ".
In the embodiment of the present invention, the testing method of cold filter clogging temperature is carried out according to " testing method of SH/T0248-2006 diesel oil and domestic heating oil cold filter clogging temperature ".
In the embodiment of the present invention, the testing method of kinematic viscosity is carried out according to " GB/T265-2008 petroleum products kinematic viscosity testing method ".
In the embodiment of the present invention, the testing method of acid number is carried out according to " GB/T264-2008 petroleum products acid number testing method ".
The present invention is raw materials used: waste grease, glycerol (analytical pure), methyl alcohol (analytical pure), sodium methylate (analytical pure), potassium hydroxide (analytical pure), all purchased from traditional Chinese medicines chemical reagent company limited.
embodiment 1:by waste grease and glycerol in mass ratio 100:18 join in reactor, under the condition of vacuum tightness 0.085mpa, mixing speed 70 revs/min, add methylsulphonic acid, temperature 110 DEG C of catalyzed reaction 3h, the glycerin fatty acid ester of generation and water; By glycerin fatty acid ester and methyl alcohol in mass ratio 100:13 under sodium methylate, vacuum tightness 0.085mpa condition, temperature 70 C pump around circuit transesterification reaction 1h, crude fatty acid methyl ester and by product glycerol is isolated from transesterify gained clarified liq, and vacuum collection methyl alcohol and water; Crude fatty acid methyl ester adds rectifying tower, and under vacuum tightness 0.08mpa condition, controlled cooling model water temperature 40 DEG C, temperature 215 DEG C of rectifying obtain refined fat acid methyl esters, i.e. biofuel; Wherein the consumption of methylsulphonic acid is 0.2% of waste grease and glycerol total mass, and wherein sodium methylate consumption is 0.15% of croude fatty acids glyceryl ester and methyl alcohol total mass.
Gained biofuel (refined fat acid methyl esters) is after tested: its cold filter clogging temperature is 0 DEG C, close flash point 145 DEG C, normal temperature kinematic viscosity 4 ㎜/s, acid value is 0.46 ㎎ koH ∕ g, and indices value all meets GB GB/T20828-2014 biodiesel technology performance related request.
embodiment 2:by waste grease and glycerol in mass ratio 100:19 join in reactor, under the condition of vacuum tightness 0.09mpa, mixing speed 70 revs/min, add tosic acid, temperature 130 DEG C of catalyzed reaction 2.5h, the glycerin fatty acid ester of generation and water; By glycerin fatty acid ester and methyl alcohol 100:14 in mass ratio, under sodium methylate, vacuum tightness 0.09mpa condition, temperature 105 DEG C of pump around circuit transesterification reaction 45min, isolate crude fatty acid methyl ester and by product regeneration glycerol from transesterify gained clarified liq, and vacuum collection methyl alcohol and water; Crude fatty acid methyl ester adds rectifying tower, and under vacuum tightness 0.09mpa condition, controlled cooling model water temperature 50 DEG C, temperature 220 DEG C of rectifying obtain refined fat acid methyl esters, i.e. biofuel; Wherein the consumption of tosic acid is 0.225% of waste grease and glycerol total mass, and wherein sodium methylate consumption is 0.175% of croude fatty acids glyceryl ester and methyl alcohol total mass.
Gained biofuel (refined fat acid methyl esters) is after tested: its cold filter clogging temperature is 0 DEG C, close flash point 145 DEG C, normal temperature kinematic viscosity 3.8 ㎜/s, acid value is 0.41 ㎎ koH ∕ g, and indices value all meets GB GB/T20828-2014 biodiesel technology performance related request.
embodiment 3:by waste grease and glycerol in mass ratio 100:20 join in reactor, under the condition of vacuum tightness 0.095mpa, mixing speed 70 revs/min, add methylsulphonic acid, temperature 150 DEG C of catalyzed reaction 2h, the glycerin fatty acid ester of generation and water; By glycerin fatty acid ester and methyl alcohol 100:15 in mass ratio, under sodium methylate, vacuum tightness 0.095mpa condition, temperature 110 DEG C of pump around circuit transesterification reaction 0.5h, isolate crude fatty acid methyl ester and by product regeneration glycerol from transesterify gained clarified liq, and vacuum collection methyl alcohol and water; Crude fatty acid methyl ester adds rectifying tower, and under vacuum tightness 0.095mpa condition, controlled cooling model water temperature 60 DEG C, temperature 230 DEG C of rectifying obtain refined fat acid methyl esters, i.e. biofuel; Wherein the consumption of methylsulphonic acid is 0.25% of waste grease and glycerol total mass, and wherein sodium methylate consumption is 0.20% of croude fatty acids glyceryl ester and methyl alcohol total mass.
Embodiment gained biofuel (refined fat acid methyl esters) is after tested: its cold filter clogging temperature is 0 DEG C, close flash point 145 DEG C, normal temperature kinematic viscosity 3.8 ㎜/s, acid value is 0.39 ㎎ koH ∕ g, and indices value all meets the related request of GB GB/T20828-2014 biodiesel technology performance.
Foregoing is only enforcement basic explanation of the present invention, and all should belong to enforcement protection domain of the present invention according to any equivalent transformation that technical scheme of the present invention is done.
Claims (4)
1. the production method of biofuel, it is characterized in that this production method comprises the following steps: join in reactor in 100:18 ~ 20 in mass ratio by waste grease and glycerol, an acidic catalyst is added under vacuum stirring condition, temperature 110 ~ 150 DEG C of catalyzed reaction 2 ~ 3h, are separated the glycerin fatty acid ester and water that generate; By glycerin fatty acid ester and methyl alcohol in mass ratio 100:13 ~ 15 under basic catalyst vacuum condition, temperature 70 ~ 110 DEG C of pump around circuit transesterification reaction 0.5 ~ 1h, crude fatty acid methyl ester and by product regeneration glycerol is isolated from transesterify gained clarified liq, and vacuum collection methyl alcohol and water; Crude fatty acid methyl ester adds rectifying tower, and controlled cooling model water temperature 40 ~ 60 DEG C, temperature 210 ~ 230 DEG C of rectifying obtain refined fat acid methyl esters, i.e. biofuel under vacuum.
2. the production method of biofuel according to claim 1, is characterized in that: the consumption of described an acidic catalyst is 0.2 ~ 0.25% of waste grease and glycerol total mass, and an acidic catalyst is methylsulphonic acid, tosic acid.
3. the production method of biofuel according to claim 1, is characterized in that: basic catalyst consumption is 0.15 ~ 0.20% of croude fatty acids glyceryl ester and methyl alcohol total mass, and basic catalyst is sodium methylate.
4. the production method of biofuel according to claim 1, is characterized in that: vacuum tightness 0.08-0.095mpa, mixing speed 70 revs/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410814292.2A CN104560412A (en) | 2014-12-24 | 2014-12-24 | Preparation method for biodiesel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410814292.2A CN104560412A (en) | 2014-12-24 | 2014-12-24 | Preparation method for biodiesel |
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| Publication Number | Publication Date |
|---|---|
| CN104560412A true CN104560412A (en) | 2015-04-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410814292.2A Pending CN104560412A (en) | 2014-12-24 | 2014-12-24 | Preparation method for biodiesel |
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| Country | Link |
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| CN (1) | CN104560412A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892809A (en) * | 2015-05-11 | 2015-09-09 | 江南大学 | Synthesized biodiesel sulfonic acid funtionalized polymer catalyst, and preparation method thereof |
Citations (7)
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| CN101108976A (en) * | 2007-09-10 | 2008-01-23 | 谢红翔 | Biological diesel oil and method of manufacturing the same |
| CN101346488A (en) * | 2005-12-23 | 2009-01-14 | Posco公司 | Bearing device for roll of hot dipping bath in continuous hot dip coating line |
| CN101451071A (en) * | 2007-12-05 | 2009-06-10 | 青岛生物能源与过程研究所 | Biodiesel preparation method and removable production apparatus thereof |
| CN101880602A (en) * | 2010-06-17 | 2010-11-10 | 暨南大学 | A method for preparing biodiesel from oil with high acid value |
| CN103160379A (en) * | 2011-12-09 | 2013-06-19 | 深圳市贝壳能源科技有限公司 | Method for producing biodiesel by virtue of high-acid-value oil raw material |
| CN103173293A (en) * | 2011-12-26 | 2013-06-26 | 北京石油化工学院 | Method for preparing biodiesel by utilizing high-acid value oil |
| US20130185991A1 (en) * | 2012-01-24 | 2013-07-25 | Maria Aparecida Cirone Taboada ME | Process for Producing High-Yield Biodiesel Applying High Acidity Triglycerides with Generation of Glycerin 90% Free of Salts |
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2014
- 2014-12-24 CN CN201410814292.2A patent/CN104560412A/en active Pending
Patent Citations (7)
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| CN101346488A (en) * | 2005-12-23 | 2009-01-14 | Posco公司 | Bearing device for roll of hot dipping bath in continuous hot dip coating line |
| CN101108976A (en) * | 2007-09-10 | 2008-01-23 | 谢红翔 | Biological diesel oil and method of manufacturing the same |
| CN101451071A (en) * | 2007-12-05 | 2009-06-10 | 青岛生物能源与过程研究所 | Biodiesel preparation method and removable production apparatus thereof |
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Non-Patent Citations (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892809A (en) * | 2015-05-11 | 2015-09-09 | 江南大学 | Synthesized biodiesel sulfonic acid funtionalized polymer catalyst, and preparation method thereof |
| CN104892809B (en) * | 2015-05-11 | 2017-01-25 | 江南大学 | A kind of synthetic biodiesel sulfonic acid functionalized polymer catalyst and preparation method thereof |
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Application publication date: 20150429 |
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