CN101486923A - Environment friendly process for biodiesel - Google Patents
Environment friendly process for biodiesel Download PDFInfo
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- CN101486923A CN101486923A CNA2009100103172A CN200910010317A CN101486923A CN 101486923 A CN101486923 A CN 101486923A CN A2009100103172 A CNA2009100103172 A CN A2009100103172A CN 200910010317 A CN200910010317 A CN 200910010317A CN 101486923 A CN101486923 A CN 101486923A
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- esterification
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- methanol
- methyl esters
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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
Abstract
The invention discloses environmental protection technology for bio-diesel production, which comprises the following units: 1) raw material preparation; 2) pre-esterification; 3) fine esterification; 4) washing desulphurization esterification; 5) refined methyl ester separation; 6) low-temperature dewaxing; 7) emission recovery; and 8) wastewater treatment. The environmental protection technology has the advantages that: 1. energy saving and emission reduction: the low temperature is served as technology heat and reduces the consumption of the energy; after the unit separation and purification, the produced exhaust gas and waste liquid can be reused in the technology, thus reducing the pollution emissions; 2. rapid esterification speed: high esterification rate; the hydrous grease is separated promptly by a liquid separating tank, thus avoiding a reverse reaction and reducing the esterification time to 1 hour; the acid value recovery problem is solved, so that the esterification is more thorough; the esterification rate can reach more than 98%; 3.output improving: the environmental protection technology has compact technology and reasonable procedure and can realize continuous and large-scale flowing production; and 4. low bio-diesel solidifying point: the wax in the bio-diesel is removed effectively by using a jacketed crystallizer and a full-automatic pressing filter, and the solidifying point is reduced.
Description
One, technical field
The invention belongs to art biodiesel technology field, be specifically related to a kind of environment-protective process that utilizes lipid acid production biofuel.
Two, background technology
Along with the rising violently of oil price, energy scarcity, the exhaustion day by day of petroleum resources and the raising of people's environmental consciousness, the research and development of biofuel is subjected to extensive concern in recent years.Biofuel is meant that with lipid acid be the liquid fuel that raw material is produced, all be close to or higher than ordinary diesel oil at aspects such as total calorific value, low-temperature fluidity, stability in storage, combustionproperty, rubber compatibility and environmental protection, can satisfy the service requirements of high-end vehicle and equipment.At present, the production method of biofuel is ester-interchange method.But there is following deficiency in process of production in this method: 1, discharge amount of pollution is big: the sulfuric acid behind this method esterification process, esterification water, alcohol and oily mixed solution can't effectively be handled, and major part is directly discharging all, causes environmental pollution; 2, esterification rate is slow, and esterification yield is low: owing to can't solve the backward reaction problem, the water that makes esterification produce can not in time be got rid of, and causes esterification time to reach about 6 hours.Simultaneously, pyrogenic distillation also can cause secondary oxidation, has greatly reduced esterification yield, and esterification yield has only between 80%-90% in the actual production, is difficult to reach national BD100 standard-required; 3, energy consumption is big: owing to adopt high temperature esterification and pyrogenic distillation, energy consumption is huge, produces 1 ton of biofuel coal consumption up to more than 200 kilograms; 4, yield poorly: because existing production method exhausts formula or semibatch between all being, can't form the continuous large-scale operation, output capacity is relatively poor continuously, and output is lower, and day output has only 10-30 tons, is difficult to meet the demands; 5, condensation point height: at present the biofuel of producing is because wax content is many, and condensation point is higher, generally all between 5-15 ℃, can't use as practicality diesel oil at all.
Three, summary of the invention
The environment-protective process that the purpose of this invention is to provide the production biofuel that a kind of discharge amount of pollution is little, esterification yield is high, energy consumption is little, output is high, condensation point is low.
For achieving the above object, the present invention's technical scheme of adopting is: this technology comprises as lower unit:
1) raw material is prepared: lipid acid, anhydrous methanol esterifying agent and the mass concentration that will be heated to 50-60 ℃, acid number and be 190-210mgkoh/g is the sulfuric acid catalyst more than 98%, mixes in tubular static mixer according to the mass ratio of 80-85:10-20:1-2;
2) pre-esterification: will go up the step mixture and send into reactor, at reaction conditions: under the rotating speed of 60-70 ℃ of temperature, pressure≤4Mpa and 60-100 rev/mins stirs, carry out 30 minutes esterifications, the reaction after product enters liquid separating tank to be separated, and getting the upper strata acid number is the material of 60-70mgkoh/g.Just can form streamline operration when operating for the third time by this step;
3) smart esterification: will go up the step obtain material, repeat step 2, acid number be the material of 3-6mgkoh/g;
4) washing removes thioesterification: upwards go on foot the methanol wash agent that adds quality of material 10-20% in the gained material, after static mixer mixes, send into the first horizontal washing esterification device, under the reaction conditions of 60-70 ℃ of temperature, pressure≤4Mpa, after the liquid hourly space velocity 30 minutes, send into liquid separating tank and separate, the upper materials that obtains is sent into the second horizontal washing esterification again think highly of multiple aforesaid operations, obtain thick methyl esters.Whole washing process is under the effect of earthquake fresh feed pump, relies on the interior tower tray resistance of pipe to finish, and makes material be washed esterification fully;
5) smart methyl esters separates: will go up the step in the thick methyl esters adding scraper evaporator of washing, and distill under 130-140 ℃ temperature, isolated gas-phase methanol and trace amounts of water vapor are reused as esterifying agent and washing composition after condensation.Isolated liquid phase is that acid number is that 0.3-0.7mgkoh/g, condensation point are 5-15 ℃ smart methyl esters;
6) low temperature pour point depression: will go up the smart methyl esters of step gained and send into double-pipe crystallizer, contained wax crystallization is separated out, again with full-automatic pressing filter machine with the removal of wax crystallization body, remove 3%-6% wax after, promptly get condensation point and be-5--25 ℃ methyl esters.Above-mentioned crystallisation process should carry out under the speed slowly, so that form bigger xln, avoids small wax grain to stop up the filter opening crack, thereby improves filtration velocity;
7) waste gas reclaims: contain the container top of methyl alcohol boil-off gas at all, the automatic exhaust steam valve through the pipeline parallel connection all is installed, the waste gas that is used to collect, and after the waste gas of collecting is cooled to liquid is sent into methanol rectifying tower and is separated and purify, and gained methyl alcohol is reused;
8) liquid waste disposal: with pre-esterification, the isolated lower floor of the liquid separating tank of smart esterification mixed solution, sending into liquid separating tank separates, after the methanol wash of gained upper strata waste oil with waste oil quality 10-30%, steam behind the methyl alcohol as boiler oil, for this technology provides 60-70 ℃ hot water and 130-140 ℃ water vapor.Gained lower floor sulfuric acid, methyl alcohol and esterification water mixed liquid, sending into scraper evaporator distills under 130-140 ℃, after isolated gas-phase methanol and water vapor were sent into methanol rectifying tower separation purification, gained methyl alcohol was reused, and gained water uses as process water; Isolated liquid phase sulfuric acid is reused as catalyzer.Replace removing as containing the available methyl alcohol of precipitation in the sulfuric acid.
The lipid acid that lipid acid described in the above-mentioned steps 1 is produced for the animal and plant offal.
Technology of the present invention has following advantage:
1, energy-saving and emission-reduction: this technology as esterification, washing heat energy, as fractionation by distillation heat energy, has reduced the consumption of the energy with 130-140 ℃ water vapors with 60-70 ℃ hot water greatly, and 1 ton of biofuel of every production only needs 5-10 kilograms of fuel oils.Simultaneously; the waste gas that produces obtains separating purification with waste liquid through waste gas recovery and liquid waste disposal unit; and put in the technology and reuse; not only reduced discharge amount of pollution; protect environment, but also reduced the raw material input, reduced raw materials cost; 1 ton of biofuel of every production can be saved 20-40 kilograms in sulfuric acid, 100-300 kilograms of methyl alcohol.
2, esterification rate is fast, esterification yield height: adopt two sections esterifications, and in time separate the water mixed liquid that contains that influences esterification, avoided the generation of backward reaction by liquid separating tank, make esterification time by the reducing to more than 6 hours about 1 hour of past, improved esterification rate greatly; Simultaneously, this process using methyl alcohol carries out twice washing as washing composition, has solved to wash the acid number rise problem that causes with water, makes esterification more thorough.Adopt low-temperature distillation to avoid the generation of secondary oxidation and processing loss again, esterification yield can reach more than 98%.
3, improved output: each unit compactness of this technology, flow process is reasonable, can realize the continuous large-scale straight-lined manufacturing, has improved output, and day throughput can reach more than 300 tons.
4, biodiesel congealing point is low: use double-pipe crystallizer and full-automatic pressing filter machine that the wax in the biofuel of producing is removed, wax content effectively reduced, remove 3%-6% wax after, promptly get condensation point and be-5--25 ℃ practicality biofuel.
Four, embodiment
Embodiment one:
1, raw material is prepared: PALM FATTY ACID, anhydrous methanol esterifying agent and the mass concentration that will be heated to 50-60 ℃, acid number and be 195mgkoh/g is the sulfuric acid catalyst more than 98%, mixes at tubular static mixer according to the mass ratio of 83:15:2;
2, pre-esterification: will go up the step mixture and send into reactor, at reaction conditions: the rotating speed of 65 ℃ of temperature, pressure 3Mpa and 60 rev/mins stirs down, carries out 30 minutes esterifications, and the reaction after product enters liquid separating tank to be separated, and gets upper materials;
3, smart esterification: will go up the step obtain material, repeat step 2, acid number be the material of 3.4mgkoh/g;
4, washing removes thioesterification: upwards go on foot the methanol wash agent that adds quality of material 10% in the gained material, after static mixer mixes, send into the first horizontal washing esterification device, under the reaction conditions of 65 ℃ of temperature, pressure 4Mpa, after the liquid hourly space velocity 30 minutes, send into liquid separating tank and separate, the upper materials that obtains is sent into the second horizontal washing esterification again think highly of multiple aforesaid operations, obtain thick methyl esters.
5, smart methyl esters separates: will go up the step in the thick methyl esters adding scraper evaporator of washing, and distill under 130 ℃ temperature, isolated gas-phase methanol and trace amounts of water vapor are reused as esterifying agent and washing composition after condensation.Isolated liquid phase is that acid number is that 0.31mgkoh/g, condensation point are 15 ℃ smart methyl esters;
6, low temperature pour point depression: will go up the smart methyl esters of step gained and send into double-pipe crystallizer, contained wax crystallization is separated out, with full-automatic pressing filter machine the wax crystallization body be removed again, remove 6% wax after, promptly get condensation point and be-5 ℃ methyl esters;
7, waste gas reclaims: contain the container top of methyl alcohol boil-off gas at all, the automatic exhaust steam valve through the pipeline parallel connection all is installed, the waste gas that is used to collect, and after the waste gas of collecting is cooled to liquid is sent into methanol rectifying tower and is separated and purify, and gained methyl alcohol is reused;
8, liquid waste disposal: with the isolated lower floor of the liquid separating tank of pre-esterification, smart esterification mixed solution, send into liquid separating tank and separate, gained upper strata waste oil is with the methanol wash of waste oil quality 20%, steams behind the methyl alcohol as boiler oil.Gained lower floor sulfuric acid, methyl alcohol and esterification water mixed liquid are sent into scraper evaporator and are distilled under 130 ℃, and after isolated gas-phase methanol and water vapor were sent into methanol rectifying tower separation purification, gained methyl alcohol was reused; Isolated liquid phase sulfuric acid is reused as catalyzer.
Embodiment two:
1, raw material is prepared: cottonseed lipid acid, anhydrous methanol esterifying agent and the mass concentration that will be heated to 50-60 ℃, acid number and be 210mgkoh/g is the sulfuric acid catalyst more than 98%, mixes at tubular static mixer according to the mass ratio of 84:15:1;
2, pre-esterification: will go up the step mixture and send into reactor, at reaction conditions: the rotating speed of 65 ℃ of temperature, pressure 3Mpa and 60 rev/mins stirs down, carries out 30 minutes esterifications, and the reaction after product enters liquid separating tank to be separated, and gets upper materials;
3, smart esterification: will go up step gained material, and repeat step 2, getting acid number is the material of 4.5mgkoh/g;
4, washing removes thioesterification: upwards the step obtains adding in the material methanol wash agent of quality of material 10%, after static mixer mixes, send into the first horizontal washing esterification device, under the reaction conditions of 65 ℃ of temperature, pressure 4Mpa, after the liquid hourly space velocity 30 minutes, send into liquid separating tank and separate, the upper materials that obtains is sent into the second horizontal washing esterification again think highly of multiple aforesaid operations, obtain thick methyl esters.
5, smart methyl esters separates: will go up the step in the thick methyl esters adding scraper evaporator of washing, and distill under 130 ℃ temperature, isolated gas-phase methanol and trace amounts of water vapor are reused as esterifying agent and washing composition after condensation.Isolated liquid phase is that acid number is that 0.46mgkoh/g, condensation point are 5 ℃ smart methyl esters;
6, low temperature pour point depression: will go up the smart methyl esters of step gained and send into double-pipe crystallizer, contained wax crystallization is separated out, with full-automatic pressing filter machine the wax crystallization body be removed again, remove 4% wax after, promptly get condensation point and be-25 ℃ methyl esters;
7, waste gas reclaims: contain the container top of methyl alcohol boil-off gas at all, the automatic exhaust steam valve through the pipeline parallel connection all is installed, the waste gas that is used to collect, and after the waste gas of collecting is cooled to liquid is sent into methanol rectifying tower and is separated and purify, and gained methyl alcohol is reused;
8, liquid waste disposal: with the isolated lower floor of the liquid separating tank of pre-esterification, smart esterification mixed solution, send into liquid separating tank and separate, gained upper strata waste oil is with the methanol wash of waste oil quality 20%, steams behind the methyl alcohol as boiler oil.Gained lower floor sulfuric acid, methyl alcohol and esterification water mixed liquid are sent into scraper evaporator and are distilled under 130 ℃, and after isolated gas-phase methanol and water vapor were sent into methanol rectifying tower separation purification, gained methyl alcohol was reused; Isolated liquid phase sulfuric acid is reused as catalyzer.
Embodiment three:
1, raw material is prepared: soya fatty acid, anhydrous methanol esterifying agent and the mass concentration that will be heated to 50-60 ℃, acid number and be 203mgkoh/g is the sulfuric acid catalyst more than 98%, mixes at tubular static mixer according to the mass ratio of 83.5:15:1.5;
2, pre-esterification: will go up the step mixture and send into reactor, at reaction conditions: the rotating speed of 65 ℃ of temperature, pressure 3Mpa and 60 rev/mins stirs down, carries out 30 minutes esterifications, and the reaction after product enters liquid separating tank to be separated, and gets upper materials;
3, smart esterification: will go up step gained material, and repeat step 2, getting acid number is the material of 5.1mgkoh/g;
4, washing removes thioesterification: upwards the step obtains adding in the material methanol wash agent of quality of material 10%, after static mixer mixes, send into the first horizontal washing esterification device, under the reaction conditions of 65 ℃ of temperature, pressure 4Mpa, after the liquid hourly space velocity 30 minutes, send into liquid separating tank and separate, the upper materials that obtains is sent into the second horizontal washing esterification again think highly of multiple aforesaid operations, obtain thick methyl esters.
5, smart methyl esters separates: will go up the step in the thick methyl esters adding scraper evaporator of washing, and distill under 130 ℃ temperature, isolated gas-phase methanol and trace amounts of water vapor are reused as esterifying agent and washing composition after condensation.Isolated liquid phase is that acid number is that 0.69mgkoh/g, condensation point are 8 ℃ smart methyl esters;
6, low temperature pour point depression: will go up the smart methyl esters of step gained and send into double-pipe crystallizer, contained wax crystallization is separated out, with full-automatic pressing filter machine the wax crystallization body be removed again, remove 5% wax after, promptly get condensation point and be-17 ℃ methyl esters;
7, waste gas reclaims: contain the container top of methyl alcohol boil-off gas at all, the automatic exhaust steam valve through the pipeline parallel connection all is installed, the waste gas that is used to collect, and after the waste gas of collecting is cooled to liquid is sent into methanol rectifying tower and is separated and purify, and gained methyl alcohol is reused;
8, liquid waste disposal: with the isolated lower floor of the liquid separating tank of pre-esterification, smart esterification mixed solution, send into liquid separating tank and separate, the useless formicester in gained upper strata is with the methanol wash of useless formicester quality 20%, steams behind the methyl alcohol as boiler oil.Gained lower floor sulfuric acid, methyl alcohol and esterification water mixed liquid are sent into vaporizer and are distilled under 130 ℃, and after isolated gas-phase methanol and water vapor were sent into methanol rectifying tower separation purification, gained methyl alcohol was reused; Isolated liquid phase sulfuric acid is reused as catalyzer.
Claims (2)
1, a kind of environment-protective process of production biofuel is characterized in that: comprise as lower unit:
1) raw material is prepared: lipid acid, anhydrous methanol esterifying agent and the mass concentration that will be heated to 50-60 ℃, acid number and be 190-210mgkoh/g is the sulfuric acid catalyst more than 98%, mixes in tubular static mixer according to the mass ratio of 80-85:10-20:1-2;
2) pre-esterification: will go up the step mixture and send into reactor, at reaction conditions: under the rotating speed of 60-70 ℃ of temperature, pressure≤4Mpa and 60-100 rev/mins stirs, carry out 30 minutes esterifications, the reaction after product enters liquid separating tank to be separated, and getting the upper strata acid number is the material of 60-70mgkoh/g;
3) smart esterification: will go up the step obtain material, repeat step 2, acid number be the material of 3-6mgkoh/g;
4) washing removes thioesterification: upwards go on foot the methanol wash agent that adds quality of material 10-20% in the gained material, after static mixer mixes, send into the first horizontal washing esterification device, under the reaction conditions of 60-70 ℃ of temperature, pressure≤4Mpa, after the liquid hourly space velocity 30 minutes, send into liquid separating tank and separate, the upper materials that obtains is sent into the second horizontal washing esterification again think highly of multiple aforesaid operations, obtain thick methyl esters;
5) smart methyl esters separates: will go up the step in the thick methyl esters adding scraper evaporator of washing, under 130-140 ℃ temperature, distill, isolated gas-phase methanol and water vapor are after condensation, reuse as esterifying agent and washing composition, isolated liquid phase is that acid number is that 0.3-0.7mgkoh/g, condensation point are 5-15 ℃ smart methyl esters;
6) low temperature pour point depression: will go up the smart methyl esters of step gained and send into double-pipe crystallizer, contained wax crystallization is separated out, again with full-automatic pressing filter machine with the removal of wax crystallization body, remove 3%-6% wax after, promptly get condensation point and be-5--25 ℃ methyl esters;
7) waste gas reclaims: contain the container top of methyl alcohol boil-off gas at all, the automatic exhaust steam valve through the pipeline parallel connection all is installed, the waste gas that is used to collect, and after the waste gas of collecting is cooled to liquid is sent into methanol rectifying tower and is separated and purify, and gained methyl alcohol is reused;
8) liquid waste disposal: with pre-esterification, the isolated lower floor of the liquid separating tank of smart esterification mixed solution, sending into liquid separating tank separates, after the methanol wash of gained upper strata waste oil with waste oil quality 10-30%, steam behind the methyl alcohol as boiler oil, gained lower floor sulfuric acid, methyl alcohol and esterification water mixed liquid, sending into scraper evaporator distills under 130-140 ℃, after isolated gas-phase methanol and water vapor are sent into methanol rectifying tower separation purification, gained methyl alcohol is reused, and isolated liquid phase sulfuric acid is reused as catalyzer.
2, the environment-protective process of a kind of production biofuel according to claim 1 is characterized in that: the lipid acid that described lipid acid is produced for the animal or plant offal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100103172A CN101486923A (en) | 2009-02-05 | 2009-02-05 | Environment friendly process for biodiesel |
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| CNA2009100103172A CN101486923A (en) | 2009-02-05 | 2009-02-05 | Environment friendly process for biodiesel |
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| CN101486923A true CN101486923A (en) | 2009-07-22 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586032A (en) * | 2012-02-17 | 2012-07-18 | 临沂实能德环保燃料化工有限责任公司 | Production method for biodiesel |
| CN107001232A (en) * | 2014-12-11 | 2017-08-01 | Bdi-生物能国际股份公司 | Method for purification of fatty acid alkyl esters class |
| CN107286016A (en) * | 2016-03-30 | 2017-10-24 | 张开益 | New ester plasticizer production line and its application method |
-
2009
- 2009-02-05 CN CNA2009100103172A patent/CN101486923A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586032A (en) * | 2012-02-17 | 2012-07-18 | 临沂实能德环保燃料化工有限责任公司 | Production method for biodiesel |
| CN107001232A (en) * | 2014-12-11 | 2017-08-01 | Bdi-生物能国际股份公司 | Method for purification of fatty acid alkyl esters class |
| CN107286016A (en) * | 2016-03-30 | 2017-10-24 | 张开益 | New ester plasticizer production line and its application method |
| CN107286016B (en) * | 2016-03-30 | 2020-04-03 | 张开益 | Ester plasticizer production device and use method thereof |
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Application publication date: 20090722 |