CN101993784A - Method for preparing biodiesel from hogwash oil catalyzed by solid super acid - Google Patents
Method for preparing biodiesel from hogwash oil catalyzed by solid super acid Download PDFInfo
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- CN101993784A CN101993784A CN2010105681415A CN201010568141A CN101993784A CN 101993784 A CN101993784 A CN 101993784A CN 2010105681415 A CN2010105681415 A CN 2010105681415A CN 201010568141 A CN201010568141 A CN 201010568141A CN 101993784 A CN101993784 A CN 101993784A
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- sewer oil
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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 hogwash oil catalyzed by solid super acid, which is characterized by comprising the following steps: after the hogwash oil is pretreated, enabling the hogwash oil catalyzed by the solid super acid to carry out esterification reaction with methanol; in the reaction process, removing by-products (glycerol and water) in time; after the reaction, filtering the catalyst; then, in the presence of pressure reduction, adding water into the reaction products for refining and distilling; and discoloring and filtering by activated carbon to obtain the biodiesel. By using the solid super acid as the catalyst for catalyzing the hogwash oil to carry out the esterification reaction, the catalyst can not corrode the equipment, has high catalytic activity, can be separated from the reaction system easily, can be recycled and can not cause the environment pollution; and by adding the water for refining and distilling in the presence of pressure reduction, low-boiling point by-products and residual acid can be effectively pumped, the content of the by-products and the residual acid in finished products can be lowered, and the overall performance of the finished products can be improved.
Description
Technical field:
The present invention relates generally to a kind of preparation method of bio-diesel oil, particularly relates to a kind ofly preparation method of bio-diesel oil with the solid superacid as catalyst sewer oil, belongs to technical field of synthesis of ester compounds in the organic compound.
Background technology:
Sewer oil is the waste grease that reclaims from catering trade, main component is the product that waste oil oxidative rancidity and hydrolysis are become sour, harmful and the contaminate environment to HUMAN HEALTH, must be to its reasonable resource utilization in addition, utilize sewer oil production biofuel, can effectively solve environmental pollution, energy starved problem, be a kind of reasonable use mode.Existing sewer oil prepares method of bio-diesel oil alcoholic acid esterification method and ester-interchange method, and the alcoholic acid esterification method is catalyzer with sulfuric acid, and the esterification products color is dark, and by product is many, and is serious to equipment corrosion, aftertreatment waste liquor contamination environment.Ester-interchange method is many based on basic catalyst, complex process, and speed of response is slow, owing to introduce basic catalyst, produces the saponification phenomenon, and aftertreatment is complicated.
Summary of the invention:
1, goal of the invention:
The invention provides a kind of solid superacid as catalyst sewer oil and prepare method of bio-diesel oil, its purpose is to overcome defective of the prior art, reduces by product, improves product color, improves speed of response and reaction esterification yield.
2, technical scheme:
The present invention is achieved through the following technical solutions:
A kind of solid superacid as catalyst sewer oil prepares method of bio-diesel oil, it is characterized in that: formed by following feedstock production: carry out according to the following steps:
(1) sewer oil is filtered, comes unstuck, dewaters and decolour pre-treatment;
(2) with above-mentioned be that the ratio of 1:1 adds in the reactor in mass ratio through pretreated sewer oil and methyl alcohol, stir and add solid super acid catalyst down, heat up then, carried out esterification 3～5 hours under 70～80 ℃ of conditions of control reaction temperature, 4 hours best results of esterification are in time removed the byproduct of reaction G ﹠ W in reaction process under 75 ℃ of conditions, after reaction finishes, be cooled to 60 ℃, filter and remove solid super acid catalyst;
(3) add entry and stir, under reduced pressure, carry out refining and distilling after, be cooled to 80 ℃, add activated carbon decolorizing and filter, promptly get biofuel.
The add-on of solid super acid catalyst described in the above-mentioned steps (2) is through 1 ‰ of pretreated sewer oil and methanol feedstock total amount.
The amount that adds entry in the above-mentioned steps (3) is through 35～45% of pretreated sewer oil quality.
Above-mentioned steps adds the water underpressure distillation described in (3), is to be to be warming up to 120 ℃ under the 0.09MPa in vacuum tightness, and stripping extracts low-boiling point material and residual sour 1 hour.
Esterification yield reaches more than 96%, and yield reaches more than 75%.
3, advantage and effect:
This solid superacid as catalyst sewer oil of the present invention prepares method of bio-diesel oil, compared with prior art, has following advantage:
1, adopting solid super-strong acid is catalyzer, compared with prior art, has reduced by product, has improved product color, and processing unit is simple, has improved speed of response and reaction esterification yield.
2, in reaction process, in time remove the byproduct of reaction G ﹠ W by a minute water operation, improved the esterification yield of reaction.
3, adopt and under reduced pressure, to add the crystal and make distillation procedure, can effectively extract lower boiling by product and residual acid, reduced the content of by product and residual acid in the finished product, improve the overall performance of product.
Description of drawings:
Fig. 1 is the diesel oil infrared spectrum with the inventive method preparation.
Embodiment:
The present invention is described further below in conjunction with embodiment:
A kind of solid superacid as catalyst sewer oil prepares method of bio-diesel oil, it is characterized in that: formed by following feedstock production: carry out according to the following steps:
(1) sewer oil is filtered, comes unstuck, dewaters and decolour pre-treatment;
(2) with above-mentioned be that the ratio of 1:1 adds in the reactor in mass ratio through pretreated sewer oil and methyl alcohol, stir and add solid super acid catalyst down, heat up then, carried out esterification 3～5 hours under 70～80 ℃ of conditions of control reaction temperature, in reaction process, in time remove the byproduct of reaction G ﹠ W, after reaction finishes, be cooled to 60 ℃, filter and remove solid super acid catalyst;
(3) add entry and stir, under reduced pressure, add the distillation of crystal's system after, be cooled to 80 ℃, add activated carbon decolorizing and filter, promptly get biofuel.
The add-on of solid super acid catalyst described in the above-mentioned steps (2) is through 1 ‰ of pretreated sewer oil and methanol feedstock total amount.
The amount that adds entry in the above-mentioned steps (3) is through 35～45% of pretreated sewer oil quality.
Above-mentioned steps adds the water underpressure distillation described in (3), is to be to be warming up to 120 ℃ under the 0.09MPa in vacuum tightness, and stripping extracts low-boiling point material and residual sour 1 hour.
Esterification yield reaches more than 96%, and yield reaches more than 75%.
Embodiment 1:
At first the sewer oil that reclaims from catering trade is filtered, come unstuck, dehydration, pre-treatment such as decolouring, in reactor, add 200 parts then through pretreated sewer oil, 200 parts of methyl alcohol are raw material, stir the solid super acid catalyst that adds down through pretreated sewer oil and methanol feedstock total amount 1 ‰, heat up then, reaction is 4 hours under 75 ℃ of conditions of control reaction temperature, in reaction process, in time remove the byproduct of reaction G ﹠ W, after reaction finishes, be cooled to 60 ℃, filtering and remove solid super acid catalyst, add under 80 parts of water stirrings and add crystal's system, is to be warming up to 120 ℃ under the 0.09MPa in vacuum tightness, stripping extracts low-boiling point material and residual sour 1 hour, be cooled to 80 ℃, add activated carbon decolorizing and filter, promptly get biofuel.Esterification yield reaches 98.5%, and yield reaches 80%, the esterification best results.
The esterification equation:
Experimental data 1:
Embodiment 2:
At first the sewer oil that reclaims from catering trade is filtered, come unstuck, dehydration, pre-treatment such as decolouring, in reactor, add 200 parts then through pretreated sewer oil, 200 parts of methyl alcohol are raw material, stir the solid super acid catalyst that adds down through pretreated sewer oil and methanol feedstock total amount 1 ‰, heat up then, reaction is 3 hours under 70 ℃ of conditions of control reaction temperature, in reaction process, in time remove the byproduct of reaction G ﹠ W, after reaction finishes, be cooled to 60 ℃, filtering and remove solid super acid catalyst, add under 70 parts of water stirrings and add crystal's system, is to be warming up to 120 ℃ under the 0.09MPa in vacuum tightness, stripping extracts low-boiling point material and residual sour 1 hour, be cooled to 80 ℃, add activated carbon decolorizing and filter, promptly get biofuel.Esterification yield reaches 96%, and yield reaches 75%, and the esterification effect is preferable.
Experimental data 2:
Embodiment 3:
At first the sewer oil that reclaims from catering trade is filtered, come unstuck, dehydration, pre-treatment such as decolouring, in reactor, add 200 parts then through pretreated sewer oil, 200 parts of methyl alcohol are raw material, stir the solid super acid catalyst that adds down through pretreated sewer oil and methanol feedstock total amount 1 ‰, heat up then, reaction is 5 hours under 80 ℃ of conditions of control reaction temperature, in reaction process, in time remove the byproduct of reaction G ﹠ W, after reaction finishes, be cooled to 60 ℃, filtering and remove solid super acid catalyst, add under 90 parts of water stirrings and add crystal's system, is to be warming up to 120 ℃ under the 0.09MPa in vacuum tightness, stripping extracts low-boiling point material and residual sour 1 hour, be cooled to 80 ℃, add activated carbon decolorizing and filter, promptly get biofuel.Esterification yield reaches 97%, and yield reaches 77%, and the esterification effect is preferable.
Experimental data 3:
Product detects:
The effective ingredient of biodiesel esterification is lipid acid triglyceride, lipid acid two sweet esters, fatty acid monoglyceride, fatty acid methyl ester etc., can confirm by infrared or chromatogram spectrogram as shown in fig. 1.
Claims (4)
1. a solid superacid as catalyst sewer oil prepares method of bio-diesel oil, it is characterized in that: formed by following feedstock production: carry out according to the following steps:
(1) sewer oil is filtered, comes unstuck, dewaters and decolour pre-treatment;
(2) with above-mentioned be that the ratio of 1:1 adds in the reactor in mass ratio through pretreated sewer oil and methyl alcohol, stir and add solid super acid catalyst down, heat up then, carried out esterification 3～5 hours under 70～80 ℃ of conditions of control reaction temperature, in reaction process, in time remove the byproduct of reaction G ﹠ W, after reaction finishes, be cooled to 60 ℃, filter and remove solid super acid catalyst;
(3) add entry and stir, under reduced pressure, carry out refining and distilling after, be cooled to 80 ℃, add activated carbon decolorizing and filter, promptly get biofuel.
2. solid superacid as catalyst sewer oil according to claim 1 prepares method of bio-diesel oil, it is characterized in that: the add-on of solid super acid catalyst described in the step (2) is through 1 ‰ of pretreated sewer oil and methanol feedstock total amount.
3. solid superacid as catalyst sewer oil according to claim 2 prepares method of bio-diesel oil, it is characterized in that: the amount that adds entry in the step (3) is through 35～45% of pretreated sewer oil quality.
4. solid superacid as catalyst sewer oil according to claim 2 prepares method of bio-diesel oil, it is characterized in that: step adds the water underpressure distillation described in (3), be to be to be warming up to 120 ℃ under the 0.09MPa in vacuum tightness, stripping extracts low-boiling point material and residual sour 1 hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105681415A CN101993784A (en) | 2010-12-01 | 2010-12-01 | Method for preparing biodiesel from hogwash oil catalyzed by solid super acid |
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| CN2010105681415A CN101993784A (en) | 2010-12-01 | 2010-12-01 | Method for preparing biodiesel from hogwash oil catalyzed by solid super acid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911794A (en) * | 2012-10-17 | 2013-02-06 | 海南大学 | Method for steadily preparing biodiesel by efficiently utilizing waste meal oil |
| CN104531364A (en) * | 2014-12-26 | 2015-04-22 | 华侨大学 | Method for catalytic esterification and deacidification of high-acid-value waste oil |
| CN108102765A (en) * | 2017-11-15 | 2018-06-01 | 孟庆桓 | It is a kind of to be acidified the method that gutter oil prepares antiwear additive |
| CN116836757A (en) * | 2023-08-14 | 2023-10-03 | 平湖市晨星科技实业有限公司 | Method for producing biodiesel by utilizing rare earth compound and solid super acidic catalyst |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580190A (en) * | 2004-05-21 | 2005-02-16 | 北京化工大学 | Method for preparing biodiesel by solid acid-base catalyst |
| CN1654601A (en) * | 2005-02-24 | 2005-08-17 | 浙江工业大学 | Method for preparing biological diesel oil |
| CN1986737A (en) * | 2005-12-19 | 2007-06-27 | 丁以钿 | Process of producing biodiesel oil with catering waste oil |
-
2010
- 2010-12-01 CN CN2010105681415A patent/CN101993784A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580190A (en) * | 2004-05-21 | 2005-02-16 | 北京化工大学 | Method for preparing biodiesel by solid acid-base catalyst |
| CN1654601A (en) * | 2005-02-24 | 2005-08-17 | 浙江工业大学 | Method for preparing biological diesel oil |
| CN1986737A (en) * | 2005-12-19 | 2007-06-27 | 丁以钿 | Process of producing biodiesel oil with catering waste oil |
Non-Patent Citations (4)
| Title |
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| 《中国油脂》 20071231 王志华等 固体超强酸SO2-4/Fe2O3催化制备生物柴油的研究 第59-62页 1-4 第32卷, 第8期 2 * |
| 《化工进展》 20091231 陈颖等 固体超强酸催化制备生物柴油研究进展 第383-389页 1-4 第28卷, 第3期 2 * |
| 《现代化工》 20081031 吴志鹏等 固体酸催化剂制备生物柴油研究进展 第126-129页 1-4 第28卷, 2 * |
| 《现代化工》 20081130 王仰东等 废油脂制备生物柴油新型固体酸催化剂研究 第45-47页 1-4 第27卷, 第11期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911794A (en) * | 2012-10-17 | 2013-02-06 | 海南大学 | Method for steadily preparing biodiesel by efficiently utilizing waste meal oil |
| CN104531364A (en) * | 2014-12-26 | 2015-04-22 | 华侨大学 | Method for catalytic esterification and deacidification of high-acid-value waste oil |
| CN104531364B (en) * | 2014-12-26 | 2017-07-21 | 华侨大学 | A kind of method for being catalyzed high acid value waste oil esterification acid reduction |
| CN108102765A (en) * | 2017-11-15 | 2018-06-01 | 孟庆桓 | It is a kind of to be acidified the method that gutter oil prepares antiwear additive |
| CN116836757A (en) * | 2023-08-14 | 2023-10-03 | 平湖市晨星科技实业有限公司 | Method for producing biodiesel by utilizing rare earth compound and solid super acidic catalyst |
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Application publication date: 20110330 |