CN101508904A - Method for producing biodiesel - Google Patents
Method for producing biodiesel Download PDFInfo
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- CN101508904A CN101508904A CNA2009100644614A CN200910064461A CN101508904A CN 101508904 A CN101508904 A CN 101508904A CN A2009100644614 A CNA2009100644614 A CN A2009100644614A CN 200910064461 A CN200910064461 A CN 200910064461A CN 101508904 A CN101508904 A CN 101508904A
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- esterification
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- methyl alcohol
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- 0 *[C@]1C#CCCC1 Chemical compound *[C@]1C#CCCC1 0.000 description 1
- GDOPTJXRTPNYNR-UHFFFAOYSA-N CC1CCCC1 Chemical compound CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 description 1
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
- 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
- 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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- Fats And Perfumes (AREA)
- Liquid Carbonaceous Fuels (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a production method of biodiesel which can efficiently solve the problems of producing biodiesel and meeting the requirement for fuels, and the solved technical proposals are as follows: biological oil is heated, filtered, dehydrated and dried, and then primary esterification reaction and secondary esterification reaction are carried out; vacuum drying of transesterification reactant is then carried out; secondary esterification reactant after vacuum drying is heated and distilled so as to generate the finished product biodiesel; methanol liquid after biodiesel is separated by distilling is redistilled to obtain methanol; and after cooling, the methanol is in cycle use. In the invention, the complete plant of biodiesel has stable technical performance, simple operation, less equipment investment and great economic and social benefits, and the rate of conversion reaches 85%.
Description
One, technical field
The present invention relates to chemical field, particularly a kind of production method of biofuel.
Two, background technology
Along with world economy and industrial expansion, the energy scarcity problem that become international is to solve energy scarcity, is all trying every means in countries in the world.China is the country of an agricultural and livestock industry prosperity, and the high acid value waste oil (general designation bio oil) that abundant agriculture herding resource, particularly vegetables oil, animal oil is arranged and form with mistake has abundant source.At present, the existing bio oil of utilizing is made biofuel as make raw material with vegetables oil, and biofuel both can be used as a kind of biofuel, can be used as diesel-dope again.Over nearly 20 years, prepare biofuel as oil-fired surrogate, caused the extensive concern of countries in the world by vegetables oil.At present, Europe and North America mainly are the feedstock production biofuel with the vegetables oil, and Japan then prepares biofuel by reclaiming waste edible oil.Several tame biofuel factory has been set up in Europe, and largest factory is in Italy, and yearly capacity reaches 250,000 tons.Biofuel has been applied in tractor, automobile, the car as motor spirit.In Germany, the automobile that benz, BMW, masses and Adui manufacturer produce all allows to use biofuel, and need not refiting engine.After 1991, European and American countries is set up the biofuel standard of having issued in succession.1996, the biofuel council based on the production biofuel was also set up in Europe, and this has shown the formation of another infant industry.
So far, China is in the starting stage to the exploitation of biofuel, and especially the acidifying oil that transforms with refining oil factory refining leftover bits and pieces (soap stock, oil foot, deodorization slip out thing, useless carclazyte etc.) is the more rarely seen report of exploitation of raw material production biofuel suite of equipment.The value of acidifying oil is about 1/3~1/4 of vegetables oil, therefore, with acidifying oil or croude fatty acids for the raw material production biofuel than having more advantage with vegetables oil.He not only has price advantage, but also will remove the problem of environmental pollution of refining oil factory from, is a good thing of killing two birds with one stone.But at present for various reasons, utilize bio oil to make biofuel and also have many technical difficult problems, therefore, how to solve effectively that to utilize bio oil production biofuel be the technical barriers that the crowd is concerned about.
Three, summary of the invention
At above-mentioned situation, for overcoming the prior art defective, the present invention's purpose just provides a kind of production method of biofuel, can effectively solve the production of biofuel, satisfy needs problem to fuel, the technical scheme of its solution is to be realized by following steps: 1. bio oil pre-treatment, 2. dry workshop section, 3. esterification, 4. secondary esterification, 5. vacuum-drying, 6. distillation, 7. seven operations of methanol rectification are finished, wherein:
1, bio oil pre-treatment: bio oil is heated to 65-70 ℃, removes by filter impurity;
2, dry workshop section: the bio oil that will remove behind the impurity is heated to 110 ℃ under the 0.085-0.09Mpa vacuum, changes with per minute 30-60 and stirs and heated 30 minutes, dehydrates;
3, esterification: the bio oil after will dehydrating adds and contains in the 3% vitriolic methyl alcohol, carry out the esterification first time, containing 3% vitriolic methyl alcohol (being that sulfuric acid and methanol quality per-cent are 3: 97) add-on is 10% ± 0.5% of biological weight of oil, be warming up to 65-70 ℃, change stirring down with per minute 30-60, the about 1.5-2.5 of esterification hour, make the bio oil acid value after the esterification drop to 70% of a preceding biological oleic acid valency of esterification, get a reactant of esterification;
4, secondary esterification: will fall a reactant of esterification after the acid value and add 40% ± 5% methyl alcohol of its weight and 3% sulfuric acid, stir, carry out the secondary esterification, esterification time is 9-12 hour, temperature is controlled at 65-70 ℃, survey an acid value in per 3 hours, and made acid value reduce to 5-10, get the secondary reactant of esterification;
5, vacuum-drying: with the vacuum-drying of secondary reactant of esterification, under the 0.085-0.09Mpa vacuum, be heated to 120 ℃, change stir and heated 30 minutes, remove moisture, water ratio≤3% with per minute 30-60.
6, distillation: with the secondary reactant of esterification after the vacuum-drying, be heated to 220 ℃ under the 0.085-0.09Mpa vacuum, the biofuel that is evaporated becomes liquid state through cooling, i.e. the finished product biofuel;
7, methanol rectification: fractionation by distillation goes out the methanol solution after the biofuel, distills out methyl alcohol again under 60-70 ℃, and after the cooling, methanol loop is used, and its purity is 98% ± 0.5%.
Said bio oil is any of vegetables oil, animal oil or high acid value waste oil.
Biofuel suite of equipment processing performance of the present invention is stable, and simple to operate, facility investment is few, and transformation efficiency reaches 85%, and economic and social benefit is huge.
Four, description of drawings
Accompanying drawing is a production unit process flow sheet of the present invention.
Five, embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is elaborated.
Provided by accompanying drawing, the present invention is realized by following steps:
1, bio oil pre-treatment: bio oil animal oil or vegetables oil or high acid value waste oil (or claiming stock oil) are heated to 68 ℃, remove by filter impurity;
2, dry workshop section: the bio oil that will remove behind the impurity is heated to 110 ℃ under the 0.088Mpa vacuum, changes with per minute 45 and stirs and heated 30 minutes, dehydrates the bio oil after must dehydrating;
3, esterification: the bio oil after will dehydrating adds and contains in the 3% vitriolic methyl alcohol, carry out the esterification first time, containing 3% vitriolic methyl alcohol (being that sulfuric acid and methanol quality per-cent are 3: 97) add-on is 10% of biological weight of oil, be warming up to 68 ℃, change stirring down with per minute 45, about 2 hours of esterification makes the bio oil acid value after the esterification drop to 70% of a preceding biological oleic acid valency of esterification, gets a reactant of esterification;
4, secondary esterification: will fall a reactant of esterification after the acid value and add 40% methyl alcohol of its weight and 3% sulfuric acid, stir, carry out the secondary esterification, esterification time is 10 hours, temperature is controlled at 68 ℃, survey an acid value in per 3 hours, and made acid value reduce to 9, get the secondary reactant of esterification;
5, vacuum-drying: with the vacuum-drying of secondary reactant of esterification, under the 0.088Mpa vacuum, be heated to 120 ℃, change with per minute 45 and stir and heated 30 minutes, remove moisture, water ratio 2.5%.
6, distillation: with the secondary reactant of esterification after the vacuum-drying, be heated to 220 ℃ under the 0.088Mpa vacuum, the biofuel that is evaporated becomes liquid state through cooling, i.e. the finished product biofuel;
7, methanol rectification: fractionation by distillation goes out the methanol solution after the biofuel, distills out methyl alcohol again under 64.5 ℃, and after the cooling, methanol loop is used, and its purity is 98%.
According to the processing unit schema, the present invention also can be realized by following steps:
1, bio oil pre-treatment: will contain the more bio oil of solid impurity and in head tank 1, be heated to 65-70 ℃, and get to flame filter press 3 with pump 2-1 and remove by filter impurity, and be put in temporary jar 4;
2, dry workshop section: the bio oil in temporary jar 4 utilizes vacuum to be admitted in the vacuum-drying still 5, under the 0.085-0.09Mpa vacuum, be heated to 110 ℃, change to stir and heated 30 minutes with per minute 30-60, moisture content is eliminated substantially, open recirculated water, during with oil cooling to 65 ℃, close water coolant, prepare esterification;
3, esterification: dried bio oil is transported in the esterifying kettle 6 with pump 2-2 from vacuum-drying still 5, squeeze in esterifying kettle 6 containing 3% vitriolic methyl alcohol among the compounding kettle 7-1, it is heavy by 10% that add-on is about oil, intensification 65-70 ℃, change stirring down with per minute 30-60, about 2 hours of esterification, acid value drops to 70% of stock oil acid value, one time esterification is finished, a reactant of esterification, the methyl alcohol that is evaporated in the reaction process continues to participate in reaction by being back to after the water cooler 8-1 cooling in an esterifying kettle 6, after reaction finishes, precipitate 60 minutes, emit waste water;
4, secondary esterification a: reactant of esterification in esterifying kettle 6 is squeezed in the secondary esterifying kettle 9 with pump 2-3, reactant of esterification is weighed 40% ± 5% methyl alcohol and squeeze into (methyl alcohol proportion 0.79g/mm among the compounding kettle 7-2
3), and reactant of esterification is weighed 3% ± 0.2% sulfuric acid squeeze into and stir, be pressed in the secondary esterifying kettle 9 with air compressor machine 10 and react, esterification time 9-12 hour, temperature is controlled at 65-70 ℃, survey an acid value in the time of per 3, grasp extent of reaction, when treating that acid value is reduced to 5-10, illustrate to react and finish substantially, the secondary reactant of esterification, the methyl alcohol that is evaporated in the reaction process continues to participate in reaction by being back to after the water cooler 8-2 cooling in the secondary esterifying kettle 9, the reaction back that finishes is rising to the methyl esters temperature about 80 ℃ under the stirring state always, the methyl alcohol that has neither part nor lot in reaction in the methyl esters is recovered in the dilute methanol jar 11 after by water cooler 8-2 cooling, treat to continue after the rectifying to use, after the methyl alcohol Ex-all, with oily temperature control at 70 ℃, put into the oily same warm saline that weighs about 15%, stir the companion at a slow speed and wash, after water injection stir 4-5 minute static, approximately after 20-30 minute, waste water is bled off, wash 2-3 time, secondary reactant of esterification pH value is washed till neutrality substantially, washing is finished;
5, vacuum-drying: the secondary reactant of esterification in the secondary esterifying kettle 9 is inhaled in the vacuum-drying pot 12, be heated to 120 ℃ under the 0.085-0.09Mpa vacuum, change with per minute 30-60 and stir and heated 30 minutes, the basic Ex-all of moisture content makes water ratio≤3%;
6, distillation: the oil of the vacuum-drying in the dry still is got in the still kettle 13 with pump 2-4, be heated to 220 ℃ under the 0.085-0.09Mpa vacuum, biological bavin is evaporated out, after condenser 14 coolings, becomes liquid state, enters in the finished product storage tank 15;
7, methanol rectification: the methyl alcohol in the dilute methanol jar is squeezed into the rectifying tower 16 from the middle part with pump 2-5, and the control tower top temperature is at 60-70 ℃, distills out to enter in the methyl alcohol storage tank 18 after methyl alcohol cools off with condenser 17 to recycle, and methanol purity is 98% ± 0.5%.
Product of the present invention after testing, reach country fully to the diesel oil set quota, specifically be, (1) density: (20 ℃) kg/m≤0.84GB/T1884, (2) sulphur content % :≤0.2GB/T380, (3) cetane value :≤45GB/T386, (4) ash content: % (m/m)≤0.01GB/T508, (5) kinematic viscosity: (20 ℃ of mm2/s3.0~8.0GB/T265, (6) condensation point ℃ :≤0GB/T510, (7) cold filter clogging temperature ℃ :≤4SH/T248, (8) acidity: mgKOH/100ml≤7GB/T258, (9) 10% steam excess carbon residue %:(m/m)≤0.3GB/T268.
Of the present invention succeeding in developing, efficiently solve and utilize bio oil, the problem that comprises animal oil, vegetables oil and high acid value waste oil production biofuel, opened up the new way of fuel energy, realized animal oil, the comprehensive utilization of vegetables oil and the utilization again of high acid value waste oil, production cost is low, production cost can reduce more than 40%, can reduce facility investment more than 50%, transformation efficiency can reach 85%, and huge economic and social benefit is arranged.
Claims (4)
1, a kind of production method of biofuel is characterized in that, is realized by following steps:
(1), bio oil pre-treatment: bio oil is heated to 65-70 ℃, removes by filter impurity;
(2), dry workshop section: the bio oil that will remove behind the impurity is heated to 110 ℃ under the 0.085-0.09Mpa vacuum, change with per minute 30-60 and stir and heated 30 minutes, dehydrates;
(3), esterification: the bio oil after will dehydrating adds and contains in the 3% vitriolic methyl alcohol, carry out the esterification first time, containing 3% vitriolic methyl alcohol add-on is 10% ± 0.5% of biological weight of oil, be warming up to 65-70 ℃, change stirring down with per minute 30-60, esterification 1.5-2.5 hour, make the bio oil acid value after the esterification drop to 70% of a preceding biological oleic acid valency of esterification, get a reactant of esterification;
(4), secondary esterification: will fall a reactant of esterification after the acid value and add 40% ± 5% methyl alcohol of its weight and 3% sulfuric acid, stir, carry out the secondary esterification, esterification time is 9-12 hour, temperature is controlled at 65-70 ℃, survey an acid value in per 3 hours, and made acid value reduce to 5-10, get the secondary reactant of esterification;
(5), vacuum-drying: with the vacuum-drying of secondary reactant of esterification, under the 0.085-0.09Mpa vacuum, be heated to 120 ℃, change stir and heated 30 minutes, remove moisture, water ratio≤3% with per minute 30-60.
(6), distillation: with the secondary reactant of esterification after the vacuum-drying, be heated to 220 ℃ under the 0.085-0.09Mpa vacuum, the biofuel that is evaporated becomes liquid state through cooling, i.e. the finished product biofuel;
(7), methanol rectification: fractionation by distillation goes out the methanol solution after the biofuel, distills out methyl alcohol again under 60-70 ℃, and after the cooling, methanol loop is used, and its purity is 98% ± 0.5%.
2, the production method of biofuel according to claim 1 is characterized in that, said bio oil is any of vegetables oil, animal oil or high acid value waste oil.
3, the production method of biofuel according to claim 1 and 2 is characterized in that, is realized by following steps:
(1), bio oil pre-treatment: bio oil animal oil or vegetables oil or high acid value waste oil are heated to 68 ℃, remove by filter impurity;
(2), dry workshop section: the bio oil that will remove behind the impurity is heated to 110 ℃ under the 0.088Mpa vacuum, change with per minute 45 and stir and heated 30 minutes, dehydrates the bio oil after must dehydrating;
(3), esterification: the bio oil after will dehydrating adds and contains in the 3% vitriolic methyl alcohol, carry out the esterification first time, containing 3% vitriolic methyl alcohol add-on is 10% of biological weight of oil, be warming up to 68 ℃, change stirring down with per minute 45, esterification 2 hours makes the bio oil acid value after the esterification drop to 70% of a preceding biological oleic acid valency of esterification, gets a reactant of esterification;
(4), secondary esterification: will fall a reactant of esterification after the acid value and add 40% methyl alcohol of its weight and 3% sulfuric acid, stir, carry out the secondary esterification, esterification time is 10 hours, temperature is controlled at 68 ℃, survey an acid value in per 3 hours, and made acid value reduce to 9, get the secondary reactant of esterification;
(5), vacuum-drying: with the vacuum-drying of secondary reactant of esterification, under the 0.088Mpa vacuum, be heated to 120 ℃, change with per minute 45 and stir and heated 30 minutes, remove moisture, water ratio 2.5%.
(6), distillation: with the secondary reactant of esterification after the vacuum-drying, be heated to 220 ℃ under the 0.088Mpa vacuum, the biofuel that is evaporated becomes liquid state through cooling, i.e. the finished product biofuel;
(7), methanol rectification: fractionation by distillation goes out the methanol solution after the biofuel, distills out methyl alcohol again under 64.5 ℃, and after the cooling, methanol loop is used, and its purity is 98%.
4, the production method of biofuel according to claim 1 is characterized in that, is realized by following steps:
(1), bio oil pre-treatment: will contain the more bio oil of solid impurity and in head tank (1), be heated to 65-70 ℃, and get to flame filter press (3) with pump (2-1) and remove by filter impurity, and be put in temporary jar (4);
(2), dry workshop section: the bio oil in temporary jar (4) utilizes vacuum to be admitted in the vacuum-drying still (5), under the 0.085-0.09Mpa vacuum, be heated to 110 ℃, change to stir and heated 30 minutes with per minute 30-60, moisture content is eliminated substantially, open recirculated water, during with oil cooling to 65 ℃, close water coolant, prepare esterification;
(3), esterification: dried bio oil is transported in the esterifying kettle (6) with pump (2-2) from vacuum-drying still (5), squeeze in the esterifying kettle (6) containing 3% vitriolic methyl alcohol in the compounding kettle (7-1), add-on is that oil is heavy by 10%, about intensification 65-70 ℃, change stirring down with per minute 30-60, esterification 2 hours, acid value drops to 70% of stock oil acid value, one time esterification is finished, a reactant of esterification, the methyl alcohol that is evaporated in the reaction process continues to participate in reaction by being back to after water cooler (8-1) cooling in the esterifying kettle (6), react finish after, precipitate 60 minutes, emit waste water;
(4), secondary esterification a: reactant of esterification in the esterifying kettle (6) is squeezed in the secondary esterifying kettle (9) with pump (2-3), reactant of esterification being weighed 40% ± 5% methyl alcohol squeezes in the compounding kettle (7-2), and reactant of esterification is weighed 3% ± 0.2% sulfuric acid squeeze into and stir, be pressed in the secondary esterifying kettle (9) with air compressor machine (10) and react, esterification time 9-12 hour, temperature is controlled at 65-70 ℃, survey an acid value in the time of per 3, when treating that acid value is reduced to 5-10, get the secondary reactant of esterification, be back to after the methyl alcohol that is evaporated in the reaction process cools off by water cooler (8-2) and continue to participate in reaction in the secondary esterifying kettle (9), after finishing, reaction under the stirring state methyl esters temperature is being risen to about 80 ℃ always, the methyl alcohol that has neither part nor lot in reaction in the methyl esters is recovered in the dilute methanol jar (11) after by water cooler (8-2) cooling, treat to continue to use after the rectifying, after the methyl alcohol Ex-all, with oily temperature control at 70 ℃, put into oil and weigh 15% same warm saline, stirring the companion at a slow speed washes, after water injection stir 4-5 minute static, after 20-30 minute, waste water is bled off, wash 2-3 time, secondary esterification reaction thing pH value is washed till neutrality substantially, and washing is finished;
(5), vacuum-drying: the secondary reactant of esterification in the secondary esterifying kettle (9) is inhaled in the vacuum-drying pot (12), under the 0.085-0.09Mpa vacuum, be heated to 120 ℃, change with per minute 30-60 and stir and heated 30 minutes, make water ratio≤3%;
(6), distillation: the oil of the vacuum-drying in the dry still is got in the still kettle (13) with pump (2-4), 0.085-0.09Mpa be heated to 220 ℃ under the vacuum, biological bavin is evaporated out, after condenser (14) cooling, become liquid state, enter in the finished product storage tank (15);
(7), methanol rectification: the methyl alcohol in the dilute methanol jar is squeezed into the rectifying tower (16) from the middle part with pump (2-5), tower top temperature is at 60-70 ℃, distill out methyl alcohol and recycle with entering in the methyl alcohol storage tank (18) after condenser (17) cooling, methanol purity is 98% ± 0.5%.
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CNA2009100644614A CN101508904A (en) | 2009-03-24 | 2009-03-24 | Method for producing biodiesel |
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CNA2009100644614A CN101508904A (en) | 2009-03-24 | 2009-03-24 | Method for producing biodiesel |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101993778A (en) * | 2010-11-08 | 2011-03-30 | 浙江工业大学 | Multilayer evaporator-based system and process for removing methanol from biodiesel |
CN104694255A (en) * | 2015-03-09 | 2015-06-10 | 安徽增源生物能源有限公司 | Method for preparing biodiesel under low temperature and negative pressure |
ES2660207A1 (en) * | 2016-09-21 | 2018-03-21 | Bio-Oils Huelva, S.L. | High efficiency process for the production of alkyl esters of fatty acids by acid catalysis and treatment procedure (Machine-translation by Google Translate, not legally binding) |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101993778A (en) * | 2010-11-08 | 2011-03-30 | 浙江工业大学 | Multilayer evaporator-based system and process for removing methanol from biodiesel |
CN101993778B (en) * | 2010-11-08 | 2013-03-27 | 浙江工业大学 | Multilayer evaporator-based system and process for removing methanol from biodiesel |
CN104694255A (en) * | 2015-03-09 | 2015-06-10 | 安徽增源生物能源有限公司 | Method for preparing biodiesel under low temperature and negative pressure |
CN104694255B (en) * | 2015-03-09 | 2017-07-28 | 安徽增源生物能源有限公司 | A kind of method that low-temperature negative-pressure prepares biodiesel |
ES2660207A1 (en) * | 2016-09-21 | 2018-03-21 | Bio-Oils Huelva, S.L. | High efficiency process for the production of alkyl esters of fatty acids by acid catalysis and treatment procedure (Machine-translation by Google Translate, not legally binding) |
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