CN101870927A - Method and device for preparing fatty acid methyl ester from oil residue - Google Patents
Method and device for preparing fatty acid methyl ester from oil residue Download PDFInfo
- Publication number
- CN101870927A CN101870927A CN201010209489A CN201010209489A CN101870927A CN 101870927 A CN101870927 A CN 101870927A CN 201010209489 A CN201010209489 A CN 201010209489A CN 201010209489 A CN201010209489 A CN 201010209489A CN 101870927 A CN101870927 A CN 101870927A
- Authority
- CN
- China
- Prior art keywords
- methyl ester
- fatty acid
- methanol gas
- acid methyl
- methanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 235000019387 fatty acid methyl ester Nutrition 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 123
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005886 esterification reaction Methods 0.000 claims abstract description 16
- 230000032050 esterification Effects 0.000 claims abstract description 11
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 6
- 229930195729 fatty acid Natural products 0.000 claims abstract description 6
- 239000000194 fatty acid Substances 0.000 claims abstract description 6
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 30
- 235000019198 oils Nutrition 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000011084 recovery Methods 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003377 acid catalyst Substances 0.000 claims description 4
- 150000002632 lipids Chemical class 0.000 claims description 4
- 241001048891 Jatropha curcas Species 0.000 claims description 2
- 229920000263 Rubber seed oil Polymers 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 239000007792 gaseous phase Substances 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 230000002378 acidificating effect Effects 0.000 claims 1
- 239000003054 catalyst Substances 0.000 claims 1
- 210000000582 semen Anatomy 0.000 claims 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- 150000004702 methyl esters Chemical class 0.000 abstract description 2
- 238000005903 acid hydrolysis reaction Methods 0.000 abstract 2
- 238000007670 refining Methods 0.000 abstract 2
- 239000003921 oil Substances 0.000 description 16
- 210000002683 foot Anatomy 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 239000002283 diesel fuel Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002551 biofuel Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- -1 fatty acids methyl esters Chemical class 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 240000001866 Vernicia fordii Species 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000004434 industrial solvent Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 235000009973 maize Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
Images
Classifications
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a method and a device for preparing fatty acid methyl ester from oil residue. The method comprises the following steps of: 1) acid hydrolysis of the oil residue, 2) esterification reaction and 3) methanol reclamation. The device consists of an oil residue acid hydrolysis reaction kettle, a separation tower, an esterification reactor, a methanol gas generator, a methanol gas condenser, a glycerol reclamation system and a residue discharge port. Fatty acid esterification, product refining and separation are performed at the same time so as to improve the esterification reaction rate, realize synchronization of preparation and refining of fatty methyl ester and improve the efficiency. The method has the advantages of simple flow, low equipment investment cost, pollution-free production process and environment friendliness.
Description
Technical field
The present invention relates to prepare the method and the device of fatty acid methyl ester, particularly a kind of method and apparatus of preparing fatty acid methyl ester from oil residue belongs to the oil chemical technology field.
Background technology
Fatty acid methyl ester claims biofuel again, and its physical and chemical performance is similar to diesel oil, is the high-quality substitute of diesel oil.Simultaneously, also a kind of important chemical material intermediate of fatty acid methyl ester is mainly as industrial solvent, synthetic fatty alcohol and derivative such as softening agent and lubricant etc.75% is raw materials cost in the fatty acid methyl ester preparation cost, and the price height is the commercial major obstacle of fatty acid methyl ester alternative fuel, and seeking cheap raw material becomes fatty acid methyl ester and substitute the key that can diesel oil fuel practicability.All can produce oil foot in raw material production grease processes such as the little seeds of a tung oil tree, rubber seed, rice bran, maize germ, cottonseed, environment has been polluted in the discharging of these oil foots on the one hand, has also wasted resource simultaneously.If they are used for the production biofuel, both can reduce production costs, protected environment again.
Summary of the invention
The objective of the invention is defective, a kind of method and apparatus of the preparing fatty acid methyl ester from oil residue that is suitable for commercially producing is provided at the prior art existence.The present invention finishes by following technical scheme:
A kind of device of preparing fatty acid methyl ester from oil residue is made up of oil foot acidolysis reaction still, knockout tower, esterifier, methanol gas producer and condenser etc.With the oil foot is raw material, utilizes the process of this device preparation fatty acid methyl ester as follows:
1) oil foot acidolysis: oil foot is added in the acidolysis reaction still, add 20～25% hydrochloric acid solns simultaneously, reflux 3～4 hours; Then lower floor's acid solution is disposed to glycerine recovery system recovery glycerine wherein, the upper strata croude fatty acids enters knockout tower, leaves standstill, and further separates, and acid solution is incorporated into to the glycerine recovery system, and upper strata lipid acid enters esterifier.Control condition: acidolysis reaction still pressure is 0.095～0.11MPa, and temperature is 90～100 ℃.
2) esterification: add acid catalyst and heating in esterifier, feed methanol gas simultaneously, methanol gas and lipid acid generation gaseous phase esterification reaction generate fatty acid methyl ester and water; React remaining methanol gas and under this hot conditions, take fatty acid methyl ester and water out of esterifier, make esterification carry out to positive dirction fast, after condensation, be back in the methanol gas producer, when the reactant primitive reaction in the esterifier is complete, stop heating, residue is discharged from discharge outlet.Control condition: esterifier pressure is 0.09～0.12MPa, and temperature is 180～200 ℃, and methanol gas producer pressure is 0.10～0.13MPa, and temperature is 65～80 ℃, and the methanol gas flow is 80～120m
3/ h.
3) Methanol Recovery: continue the heating methanol producer gas generator and reclaim methyl alcohol, after Methanol Recovery is complete, after methanol gas producer discharge outlet separation water outlet, obtain the fatty acid methyl ester product.Control condition: methanol gas producer pressure is 0.10～0.13MPa, and temperature is 65～90 ℃.
Advantage of the present invention and positively effect:
1) the present invention improves esterification reaction rate with fatty acid esterification, product purification with separate simultaneously and carry out, and realizes the preparation of fatty methyl esters and refiningly carries out synchronously, has improved efficient.
2) flow process of the present invention is simple, and equipment investment cost is low, and the production process cleaning has environment friendly.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment: followingly further specify flesh and blood of the present invention, but content of the present invention is not limited to this with example.
Embodiment 1: processing condition, material input and output situation with the Jatropha curcas oil preparing fatty acid methyl ester from oil residue are as follows:
1) acidolysis reaction: acidolysis reaction still pressure is 0.095MPa, and temperature is 90 ± 5 ℃, concentration of hydrochloric acid 20%.
2) esterification: reaction kettle of the esterification pressure is 0.1MPa, and temperature is 180 ± 5 ℃, and methanol gas producer pressure is 0.12MPa, and temperature is 65 ± 5 ℃, and the methanol gas flow is 80m
3/ h.
3) Methanol Recovery: methanol gas producer pressure is 0.11MPa, and temperature is 75 ± 5 ℃.
The material input and output: drop into 100 parts of oil foots, 50 parts of 20% hydrochloric acid solns, 1.2 parts of acid catalysts, the methanol gas flow is 80m
3/ h.75 parts of output fatty acid methyl esters (total fatty acids methyl esters content is 98.76%).
Embodiment 2: processing condition, material input and output situation with the rubber seed oil preparing fatty acid methyl ester from oil residue are as follows:
1) acidolysis reaction: acidolysis reaction still pressure is 0.10MPa, and temperature is 100 ± 5 ℃, concentration of hydrochloric acid 25%.
2) esterification: reaction kettle of the esterification pressure is 0.12MPa, and temperature is 200 ± 5 ℃, and methanol gas producer pressure is 0.13MPa, and temperature is 70 ± 5 ℃, and the methanol gas flow is 100m
3/ h.
3) Methanol Recovery: methanol gas producer pressure is 0.12MPa, and temperature is 85 ± 5 ℃.
The material input and output: drop into 100 parts of oil foots, 50 parts of 25% hydrochloric acid solns, 1.0 parts of acid catalysts, the methanol gas flow is 120m
3/ h.78 parts of output fatty acid methyl esters (total fatty acids methyl esters content is 97.96%).
Claims (5)
1. method with preparing fatty acid methyl ester from oil residue is characterized in that finishing by following technological step:
1) oil foot acidolysis: oil foot is added in the acidolysis reaction still, add 20～25% hydrochloric acid solns simultaneously, reflux 3～4 hours; Then lower floor's acid solution is disposed to glycerine recovery system recovery glycerine wherein, the upper strata croude fatty acids enters knockout tower, leaves standstill, and further separates, and acid solution is incorporated into to the glycerine recovery system, and upper strata lipid acid enters esterifier;
2) esterification: add acid catalyst and heating in esterifier, feed methanol gas simultaneously, methanol gas and lipid acid generation gaseous phase esterification reaction generate fatty acid methyl ester and water; React remaining methanol gas and under this hot conditions, take fatty acid methyl ester and water out of esterifier, make esterification carry out to positive dirction fast, after condensation, be back in the methanol gas producer, when the reactant primitive reaction in the esterifier is complete, stop heating, residue is discharged from discharge outlet;
3) Methanol Recovery: continue the heating methanol producer gas generator and reclaim methyl alcohol, after Methanol Recovery is complete, after methanol gas producer discharge outlet separation water outlet, obtain the fatty acid methyl ester product.
2. according to the method for right 1 described a kind of preparing fatty acid methyl ester from oil residue, it is characterized in that: described oil foot is Jatropha curcas oil pin, rubber seed oil foot or Oleum Gossypii semen; Acidolysis reaction still pressure is 0.095～0.11MPa described in the step (1), and temperature is 90～100 ℃.
3. according to the method for right 1 described a kind of preparing fatty acid methyl ester from oil residue, it is characterized in that: described an acidic catalyst is sulfuric acid, hydrochloric acid or tosic acid; Esterifier pressure is 0.09～0.12MPa described in the step (2), and temperature is 180～200 ℃, and methanol gas producer pressure is 0.10～0.13MPa, and temperature is 65～80 ℃, and the methanol gas flow is 80～120m
3/ h
4. according to the method for right 1 described a kind of preparing fatty acid methyl ester from oil residue, it is characterized in that: methanol gas producer pressure is 0.10～0.13MPa described in the step (3), and temperature is 65～90 ℃;
5. the device of a preparing fatty acid methyl ester from oil residue, it is characterized in that: this device comprises oil foot acidolysis reaction still, knockout tower, esterifier, methanol gas producer and condenser, glycerine recovery system, residue discharge outlet; Wherein, knockout tower connects acidolysis reaction still and esterifier, and esterifier connects the methanol gas producer, and the methanol gas producer connects condenser.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102094895A CN101870927B (en) | 2010-06-25 | 2010-06-25 | Method and device for preparing fatty acid methyl ester from oil residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102094895A CN101870927B (en) | 2010-06-25 | 2010-06-25 | Method and device for preparing fatty acid methyl ester from oil residue |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101870927A true CN101870927A (en) | 2010-10-27 |
| CN101870927B CN101870927B (en) | 2012-09-05 |
Family
ID=42996014
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102094895A Expired - Fee Related CN101870927B (en) | 2010-06-25 | 2010-06-25 | Method and device for preparing fatty acid methyl ester from oil residue |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101870927B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676302A (en) * | 2012-06-04 | 2012-09-19 | 昆明理工大学 | Method and device for preparing biodiesel by oil with high acid value |
| CN109563424A (en) * | 2016-08-18 | 2019-04-02 | 道达尔销售服务公司 | The manufacturing method of oiliness additive for the fuel with low sulfur content |
| CN112850997A (en) * | 2021-01-25 | 2021-05-28 | 茂名市凯跃特种油剂有限公司 | Wastewater treatment process for producing bunker fuel oil based on glycerol esterification reaction |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970694A (en) * | 2006-12-07 | 2007-05-30 | 张以光 | Production process of biological diesel oil |
| CN101003740A (en) * | 2007-01-18 | 2007-07-25 | 鲁希诺 | Method for making biologic diesel oil |
-
2010
- 2010-06-25 CN CN2010102094895A patent/CN101870927B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970694A (en) * | 2006-12-07 | 2007-05-30 | 张以光 | Production process of biological diesel oil |
| CN101003740A (en) * | 2007-01-18 | 2007-07-25 | 鲁希诺 | Method for making biologic diesel oil |
Non-Patent Citations (1)
| Title |
|---|
| 《农业工程学报》 20070228 苏有勇等 皂脚制备生物柴油的试验研究 184 1-4 第23卷, 第02期 2 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676302A (en) * | 2012-06-04 | 2012-09-19 | 昆明理工大学 | Method and device for preparing biodiesel by oil with high acid value |
| CN109563424A (en) * | 2016-08-18 | 2019-04-02 | 道达尔销售服务公司 | The manufacturing method of oiliness additive for the fuel with low sulfur content |
| CN112850997A (en) * | 2021-01-25 | 2021-05-28 | 茂名市凯跃特种油剂有限公司 | Wastewater treatment process for producing bunker fuel oil based on glycerol esterification reaction |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101870927B (en) | 2012-09-05 |
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