CN102586027A - Continuous production method of biodiesel from waste oil/fat - Google Patents
Continuous production method of biodiesel from waste oil/fat Download PDFInfo
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- CN102586027A CN102586027A CN2012100440303A CN201210044030A CN102586027A CN 102586027 A CN102586027 A CN 102586027A CN 2012100440303 A CN2012100440303 A CN 2012100440303A CN 201210044030 A CN201210044030 A CN 201210044030A CN 102586027 A CN102586027 A CN 102586027A
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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
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- 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 discloses a continuous production method of biodiesel from waste oil/fat. The method includes mixing waste oil/fat with water at volume ratio of (3-4):1, and hydrolyzing; naturally settling obtained crude fatty acid for 0.5-1.5 hr to remove water and impurities and collect dewatered fatty acid; injecting the dewatered fatty acid and concentrated sulfuric acid into esterification kettle, introducing compressed methanol gas, stepwise esterifying, and alternately removing alcohol after esterification to give crude ester; neutralizing the crude ester with sodium carbonate under stirring; and performing multi-stage distillation to give biodiesel. The method obviates mechanical vacuum distillation for water removal, reduces occurrence of reverse reaction, reduces investment of cooling equipment, improves utilization efficiency, lowers labor intensity, guarantees safe and stable production, and reduces sewage generation.
Description
Technical field
The present invention relates to chemical production field, relate in particular to a kind of method of utilizing the waste grease continuously producing biodiesel.
Background technology
Biofuel is claimed fatty acid methyl ester again, mainly is to utilize animal-plant oil, waste grease etc. to obtain through esterification as raw material and methyl alcohol.Biofuel becomes the substitute of fossil oil with its recyclability, the low pollution, by the exploitation direction of a lot of countries as Future New Energy Source.
China's " 15 development outline " is clear and definite encourage growth oil substitutes in advance, and will develop biofuel and confirm as the new industry developing direction.Yet the R and D insufficient investment of China's biofuel still is in the starting stage, many manufacturing enterprises small scale, and production technology falls behind with device, makes production cost higher relatively, and technical target of the product can not satisfy biofuel fully and use standard.
Industriallization is made method of bio-diesel oil and is mainly contained two kinds: the one, and the direct alcoholysis of grease; Promptly utilize methyl alcohol directly to carry out transesterification reaction generation fatty acid methyl ester and glycerine with grease; Reaction times is shorter; But the specification of quality to raw oil material is higher, if its acid value is too high, then need carry out preparatory esterification; The 2nd, waste grease is carried out hydrolysis earlier, generate lipid acid, under the acid catalysis effect, react generation fatty acid methyl ester and water with methyl alcohol again after the dehydration then.Water-content in this reaction pair lipid acid has certain requirement, and water-content low reaction more is abundant more.
For food and drink and other waste grease production biofuel, because its composition is complicated, quality is difficult to guarantee, adopts the technology that is hydrolyzed into the lipid acid resterification earlier comparatively reasonable.Traditional esterification technology, employing be the intermittently esterification of single esterifying kettle, every independent esterification of reaction kettle, dealcoholysis separately.Adopt liquid methanol to add mode, the lipid acid water cut of hydrolysis is had strict demand, the height that this directly affects esterification yield influences the yield of product.
Summary of the invention
Technical problem to be solved by this invention provides a kind of shortcoming to traditional industry manufacturing biofuel, the method for utilizing the waste grease continuously producing biodiesel that energy consumption is low, production efficiency is high, product yield is high, level of automation is high.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of method of utilizing the waste grease continuously producing biodiesel comprises step:
1) waste grease hydrolysis
With waste grease and water according to 3～4: 1 volume ratio is mixed, and is hydrolyzed;
2) produce the lipid acid that anhydrates
With the croude fatty acids natural subsidence 0.5～1.5h that obtains of said hydrolysis, remove water and impurity, obtain the lipid acid that anhydrates; Behind the natural subsidence 1h, the emptying bottom water need not mechanical underpressure distillation and dewaters in slurry tank;
3) esterification, dealcoholysis
The said lipid acid that anhydrates, the vitriol oil are injected in the esterifying kettle, feed compression methyl alcohol gas, esterification step by step, after the esterification, alternately dealcoholysis makes thick ester; Adopt gas-phase methanol esterification mode, methyl alcohol gas is back to back, and the water that reaction generates is in time taken out of; Reduced the generation of backward reaction, improved esterification efficient, continuously methyl alcohol gas esterification; Avoided needing independent dealcoholysis after single the esterifying kettle reaction, reduced the cooling apparatus investment, improved the heat energy utilization rate; Improve the utilising efficiency of methyl alcohol simultaneously, realized the continuous operation of esterification, reduced operation labour intensity; Improve the automated operation level of esterification technique, better guaranteed safety, stably manufactured;
4) neutralization
In with said thick ester, add the soda ash powder, and under agitation neutralize;
5) rectifying
Thick ester after the above-mentioned neutralization is made said biofuel through two-stage rectification.
As optimized technical scheme, the hydrolysis pressure in the said waste grease hydrolysing step is 2.0～3.5MPa.
As optimized technical scheme, esterification pressure is 0.08～1.5MPa in said esterification, the dealcoholysis step, methyl alcohol gas pressurization esterification mode; Esterification is carried out under 0.08～1.5MPa pressure; Shorten esterification time, reduced esterification temperature, reduced production energy consumption.
As optimized technical scheme, said neutral temperature is 70～90 ℃, adopts solid soda ash 70～90 ℃ of neutralizations down, has reduced the generation of sewage, has also prevented that fatty acid methyl ester and alkali reaction from generating Chinese honey locust simultaneously.
As optimized technical scheme; Said multistage rectification is a two-stage rectification, contains small amount of moisture in the thick ester in neutralization back, and rectifying removes moisture and other low-boiling-point substances through one-level; Get into the two-stage rectification device then; The biofuel that obtains meets national correlated quality standard, if still contain moisture or other low-boiling-point substances through after the two-stage rectification, then through obtaining meeting the biofuel of national correlated quality standard after three rectifying even four rectifying.
Owing to adopted technique scheme, a kind of method of utilizing the waste grease continuously producing biodiesel comprises step: 1) waste grease hydrolysis, with waste grease and water according to 3～4: 1 volume ratio mixing is hydrolyzed; 2) produce the lipid acid that anhydrates,, remove water and impurity, obtain the lipid acid that anhydrates the croude fatty acids natural subsidence 0.5～1.5h that obtains of said hydrolysis; 3) esterification, dealcoholysis are injected the said lipid acid that anhydrates, the vitriol oil in the esterifying kettle, feed compression methyl alcohol gas, esterification step by step, and after the esterification, alternately dealcoholysis makes thick ester; 4) neutralization adds the soda ash powder, and under agitation neutralizes in said thick ester; 5) rectifying makes said biofuel with the thick ester after the above-mentioned neutralization through multistage rectification, in slurry tank behind the natural subsidence 1h, and the emptying bottom water; Need not mechanical underpressure distillation and dewater, adopt gas-phase methanol esterification mode, methyl alcohol gas is back to back; The water that reaction generates is in time taken out of, reduced the generation of backward reaction, improved esterification efficient; Methyl alcohol gas esterification has been avoided needing independent dealcoholysis after single the esterifying kettle reaction continuously, has reduced the cooling apparatus investment; Improve the heat energy utilization rate, improved the utilising efficiency of methyl alcohol simultaneously, realized the continuous operation of esterification; Reduce operation labour intensity, improved the automated operation level of esterification technique, better guaranteed safety, stably manufactured; Adopt solid soda ash 70～90 ℃ of neutralizations down, reduced the generation of sewage, also prevented that fatty acid methyl ester and alkali reaction from generating Chinese honey locust simultaneously.
Description of drawings
Accompanying drawing is the process flow sheet of the embodiment of the invention.
Embodiment
Shown in accompanying drawing, lipid acid and gas-phase methanol get into the 1# esterifying kettle by the esterifying kettle bottom, get into from 2# esterifying kettle bottom through riser again, get into the 3# esterifying kettle successively.Unnecessary methyl alcohol gas gets into methanol distillation column purifying continued by the 3# esterifying kettle and participates in esterification.The preliminary esterified prod that the 3# esterifying kettle is discharged gets into follow-up esterifying kettle again; Utilize more than the further esterification to 99% of refining methyl alcohol gas of methyl alcohol compressor injection; Unnecessary methyl alcohol gas gets into the 1# esterifying kettle and participates in the esterification circulation, so forms continuous esterification, and the final thick ester of esterification hockets in follow-up esterifying kettle after the dealcoholysis operation; Change neutralising arrangement over to, after the neutralization slagging-off, can carry out rectifying and make biofuel.
Embodiment 1
1, acidifying plant oil foot highly pressured hydrolysis is produced lipid acid: acidifying plant oil foot and hot water inject hydrolysis tower in proportion at 4: 1, utilize the 2.0MPa steam pressurized to heat up, and make the croude fatty acids of percent hydrolysis more than 98%, and natural subsidence 0.5h removal water is assorted in slurry tank.
2, esterification, dealcoholysis: the lipid acid that anhydrates, the vitriol oil inject in the esterifying kettle, feed compression methyl alcohol gas, under 0.08MPa pressure, and esterification step by step, after the esterification, alternately dealcoholysis.
3, neutralization: thick ester after the dealcoholysis, be cooled to 70 ℃ with still in changing over to, add the soda ash powder under stirring and be neutralized to the regulation acid value, alkaline residue is removed in sedimentation.
4, rectifying: neutralized crude esters gets into secondary level rectifying tower, through underpressure distillation, obtains refining biodiesel, and acid value is less than 0.8mg/g.
Embodiment 2
1, acidifying plant oil foot and sewer oil mixture highly pressured hydrolysis are produced lipid acid: acidifying plant oil foot and hot water inject hydrolysis tower in proportion at 3: 1; Utilize the 3.0MPa steam pressurized to heat up; Make the croude fatty acids of percent hydrolysis more than 96%, natural subsidence 1h removal water is assorted in slurry tank.
2, esterification, dealcoholysis: the lipid acid that anhydrates, the vitriol oil inject in the esterifying kettle, feed compression methyl alcohol gas, esterification step by step under 0.55MPa pressure, and after the esterification, alternately dealcoholysis.
3, neutralization: thick ester after the dealcoholysis, be cooled to 80 ℃ with still in changing over to, add the soda ash powder under stirring and be neutralized to the regulation acid value, alkaline residue is removed in sedimentation.
4, rectifying: neutralized crude esters gets into the two-stage rectification tower, through underpressure distillation, obtains refining biodiesel, and acid value is less than 0.8mg/g.
Embodiment 3
1, acidifying plant oil foot highly pressured hydrolysis is produced lipid acid: acidifying plant oil foot and hot water inject hydrolysis tower in proportion at 3.5: 1; Utilize the 3.5MPa steam pressurized to heat up; Make the croude fatty acids of percent hydrolysis more than 98%, natural subsidence 1.5h removal water is assorted in slurry tank.
2, esterification, dealcoholysis: the lipid acid that anhydrates, the vitriol oil inject in the esterifying kettle, feed compression methyl alcohol gas, under 1.5MPa pressure, and esterification step by step, after the esterification, alternately dealcoholysis.
3, neutralization: thick ester after the dealcoholysis, be cooled to 90 ℃ with still in changing over to, add the soda ash powder under stirring and be neutralized to the regulation acid value, alkaline residue is removed in sedimentation.
4, rectifying: neutralized crude esters gets into secondary level rectifying tower, through underpressure distillation, obtains refining biodiesel, and acid value is less than 0.8mg/g.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; The present invention is not restricted to the described embodiments; That describes in the foregoing description and the specification sheets just explains principle of the present invention; Under the prerequisite that does not break away from spirit and scope of the invention, the present invention also has various changes and modifications, and these variations and improvement all fall in the scope of the invention that requires protection.The present invention requires protection domain to be defined by appending claims and equivalent thereof.
All are from design of the present invention, and the structural transformation of having done without creative work all drops within protection scope of the present invention.
Claims (5)
1. a method of utilizing the waste grease continuously producing biodiesel is characterized in that, comprises step:
1) waste grease hydrolysis
With waste grease and water according to 3～4: 1 volume ratio is mixed, and is hydrolyzed;
2) produce the lipid acid that anhydrates
With the croude fatty acids natural subsidence 0.5～1.5h that obtains of said hydrolysis, remove water and impurity, obtain the lipid acid that anhydrates;
3) esterification, dealcoholysis
The said lipid acid that anhydrates, the vitriol oil are injected in the esterifying kettle, feed compression methyl alcohol gas, esterification step by step, after the esterification, alternately dealcoholysis makes thick ester;
4) neutralization
In with said thick ester, add the soda ash powder, and under agitation neutralize;
5) rectifying
Thick ester after the above-mentioned neutralization is made said biofuel through multistage rectification.
2. a kind of method of utilizing the waste grease continuously producing biodiesel as claimed in claim 1 is characterized in that: the hydrolysis pressure in the said waste grease hydrolysing step is 2.0～3.5MPa.
3. a kind of method of utilizing the waste grease continuously producing biodiesel as claimed in claim 1 is characterized in that: esterification pressure is 0.08～1.5MPa in said esterification, the dealcoholysis step.
4. a kind of method of utilizing the waste grease continuously producing biodiesel as claimed in claim 1 is characterized in that: said neutral temperature is 70～90 ℃.
5. a kind of method of utilizing the waste grease continuously producing biodiesel as claimed in claim 1 is characterized in that: said multistage rectification is a two-stage rectification.
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| CN2012100440303A CN102586027A (en) | 2012-02-24 | 2012-02-24 | Continuous production method of biodiesel from waste oil/fat |
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| CN2012100440303A CN102586027A (en) | 2012-02-24 | 2012-02-24 | Continuous production method of biodiesel from waste oil/fat |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103540414A (en) * | 2013-10-22 | 2014-01-29 | 惠州市神州创宇低碳技术发展有限公司 | Method and equipment for refining biodiesel through palm oil residue and acidic oil |
| CN103865657A (en) * | 2014-01-21 | 2014-06-18 | 徐如思 | Production process for preparing biodiesel by adopting chemical synthesis |
| CN104086412A (en) * | 2014-06-30 | 2014-10-08 | 海盐县精细化工有限公司 | Process method for producing butyl oleate by using rape oil fatty acid |
| CN110172377A (en) * | 2019-06-20 | 2019-08-27 | 成都恒润高新科技股份有限公司 | A method of biodiesel is continuously prepared using waste animal and vegetable oil |
| CN113563977A (en) * | 2021-07-21 | 2021-10-29 | 湖北天基生物能源科技发展有限公司 | Waste grease treatment system and treatment method |
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| CN101230288A (en) * | 2007-01-24 | 2008-07-30 | 新疆协力新能源有限责任公司 | Method for producing biological diesel oil |
| CN101702916A (en) * | 2007-03-30 | 2010-05-05 | 利莱恩斯生命科学有限公司 | An integrated process for the preparation of fatty acid methyl ester (biodiesel) |
| CN101811964A (en) * | 2010-04-21 | 2010-08-25 | 潍坊市大明化工有限公司 | Method for synthesizing fatty acid methyl ester |
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2012
- 2012-02-24 CN CN2012100440303A patent/CN102586027A/en active Pending
Patent Citations (3)
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| CN101230288A (en) * | 2007-01-24 | 2008-07-30 | 新疆协力新能源有限责任公司 | Method for producing biological diesel oil |
| CN101702916A (en) * | 2007-03-30 | 2010-05-05 | 利莱恩斯生命科学有限公司 | An integrated process for the preparation of fatty acid methyl ester (biodiesel) |
| CN101811964A (en) * | 2010-04-21 | 2010-08-25 | 潍坊市大明化工有限公司 | Method for synthesizing fatty acid methyl ester |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103540414A (en) * | 2013-10-22 | 2014-01-29 | 惠州市神州创宇低碳技术发展有限公司 | Method and equipment for refining biodiesel through palm oil residue and acidic oil |
| CN103540414B (en) * | 2013-10-22 | 2016-01-06 | 惠州市神州创宇低碳技术发展有限公司 | The method and apparatus of a kind of palm dregs of fat and acidification oil refining biofuel |
| CN103865657A (en) * | 2014-01-21 | 2014-06-18 | 徐如思 | Production process for preparing biodiesel by adopting chemical synthesis |
| CN103865657B (en) * | 2014-01-21 | 2016-01-20 | 徐如思 | A kind of production technique adopting chemical synthesis to prepare biofuel |
| CN104086412A (en) * | 2014-06-30 | 2014-10-08 | 海盐县精细化工有限公司 | Process method for producing butyl oleate by using rape oil fatty acid |
| CN104086412B (en) * | 2014-06-30 | 2016-04-20 | 海盐县精细化工有限公司 | Produce oil with rape oil fatty acid the processing method of acid butyl ester |
| CN110172377A (en) * | 2019-06-20 | 2019-08-27 | 成都恒润高新科技股份有限公司 | A method of biodiesel is continuously prepared using waste animal and vegetable oil |
| CN113563977A (en) * | 2021-07-21 | 2021-10-29 | 湖北天基生物能源科技发展有限公司 | Waste grease treatment system and treatment method |
| CN113563977B (en) * | 2021-07-21 | 2022-08-16 | 湖北天基生物能源科技发展有限公司 | Treatment system and treatment method for waste grease |
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Application publication date: 20120718 |