CN103436371B - Novel technology for preparing biodiesel by virtue of low-temperature enzyme fermentation method - Google Patents
Novel technology for preparing biodiesel by virtue of low-temperature enzyme fermentation method Download PDFInfo
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- CN103436371B CN103436371B CN201310378061.7A CN201310378061A CN103436371B CN 103436371 B CN103436371 B CN 103436371B CN 201310378061 A CN201310378061 A CN 201310378061A CN 103436371 B CN103436371 B CN 103436371B
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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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- 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
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Abstract
The invention discloses a novel technology for preparing biodiesel by a low-temperature enzyme fermentation method. The novel technology comprises the following steps of: S1. placing raw oil in a drying room, and heating the raw oil to be at a flowing liquid state; S2. pumping the liquefied raw oil into a reaction kettle I, adding a biological enzyme composite catalyst I, and reacting to obtain a liquid A; S3. centrifuging the liquid A to obtain a liquid B; S4. pumping the liquid B into a reaction kettle II, adding a biological enzyme composite catalyst II and methanol, and reacting to obtain crude biodiesel; S5. centrifuging the crude biodiesel to obtain liquid C; S6. pumping the liquid C into a reaction kettle III, decoloring, and filtering by a sheet frame to obtain the biodiesel. The novel technology has the advantages that the biodiesel can be rapidly produced by using the low-temperature enzyme fermentation method, waste is turned into treasure, reaction conditions are mild, the pressurization is not needed, the reaction temperature of the biological enzyme fermentation is not higher than 78 DEG C, and the production period is short; the novel technology has the characteristics of low cost, high efficiency, no toxicity, simplicity in operation and strong practicability.
Description
Technical field
The invention belongs to field of grease chemical technology, be specifically related to cold-adapted enzyme ferment legal system for biological diesel-oil technique.
Background technology
Biofuel is the one of biomass energy, and it is the mono alkyl ester of a kind of longer chain fatty acid that the technology such as biological utilisation thermo-cracking obtain.Biofuel is the mixture of the high complicated organic composition of oxygen level, and these mixtures organism that mainly number molecular weight is large, almost comprises the oxygen-bearing organic matter of all kinds.Biofuel not sulfur-bearing and aromatic hydrocarbons substantially, cetane value is higher, biodegradable, nontoxic, environmental sound.Its height is extremely conducive to the trouble-free burning of compressing ignition engine containing oxygen CN value thus reduces tail gas discharge of poisonous waste, so be called as low-pollution fuel.
The production method of biofuel mainly contains chemical method, biological enzyme and supercritical alcohols method.The method of the current suitability for industrialized production biofuel of China remains chemical method, namely animal and plant grease and the low-carbon alcohol such as methyl alcohol or ethanol is used to carry out transesterification under acid or basic catalyst and high temperature (230 ~ 250 DEG C), generate corresponding fatty acid methyl ester or ethyl ester, be drying to obtain biofuel through washing.And prepare biofuel with chemical method and still there is many technical barriers, be mainly reflected in: 1. use base catalysis method production biofuel, owing to having soap stock to generate in reaction, formation flocks, makes biodiesel oil product not easily separated; The soap stock produced in reaction process, glycerine are easy to the emulsification such as biofuel, methyl alcohol, cause biofuel yield low; Easy waste discharge in reaction, is formed " secondary pollution "; 2. use the vitriol oil as catalyzer, although have the advantages such as catalytic efficiency is higher, the reaction times is shorter, but deposit equally and easily discharge sulfuric acid wastewater containing in the reaction, formed " secondary pollution ", esterification products is difficult to be separated, catalyzer can not be recycled, thus causes a production cost comparatively high-technology difficult problem.
For solving the problem that chemosynthesis produces, people utilize biological enzyme biodiesel synthesis, namely carry out transesterification by animal grease and low-carbon alcohol by lipase, prepare corresponding fatty acid methyl ester and ethyl ester.Enzymatic Synthesis of Biodiesel has that mild condition, alcohol consumption are little, the advantage of non-pollution discharge.But at present technology is to the low conversion rate of methyl alcohol and ethanol, is generally only 40% ~ 60%, because current lipase is to the esterification of long chain aliphatic alcohol or effectively transesterification, and to short chain fatty alcohol as the low conversion rate such as methyl alcohol or ethanol.And short chain alcohol has certain toxicity to enzyme, the work-ing life of enzyme is short.By-product glycerin and shipwreck are in recovery, and not only formed product and suppress, the existence of chain rupture fatty alcohol and glycerine all affects reactive behavior and the stability of enzyme, and the work-ing life of harden monitoring is shortened greatly.
Chinese patent CN102533450A discloses a kind of process for preparing biodiesel through supercritical methanol two-step method of hot integration coupling flash evaporation, and (1) first rich mixture is hydrolyzed into lipid acid and glycerine under sub-critical water extraction; (2) then there is esterification reaction of organic acid and obtain biofuel in lipid acid under supercritical methanol condition.Though supercritical fluid technology, flash evaporation technology and energy saving of chemical industry technology organically combine by this technique, effectively reduce the energy consumption of Preparation of Biodiesel by Supercritical Method, operational condition and methanol consumption, realize the high-efficiency and continuous stably manufactured of biofuel, but supercritical catalyst method needs to carry out under high-temperature and high-pressure conditions, facility investment is expensive, fire-fighting and safety check are difficult to reach a standard, are unfavorable for industrial production.
Chinese patent ZL200410100479.2 discloses a kind of coupling production biofuel and 1, the method of ammediol, lipase-catalyzed methyl alcohol or ethanol and grease are reacted and generates biofuel and microbial transformation glycerine is 1, ammediol two processes are got up by membrane filtration coupling, and two processes are carried out simultaneously.Though the present invention eliminates short chain alcohol and glycerine to the suppression of lipase, extend the work-ing life of immobilized enzyme, eliminate the technique of glycerine separation and Extraction simultaneously, reduce production cost, save the time, improve production efficiency, but because low-carbon alcohol is toxic to enzyme, cause enzyme process biodiesel conversion rate low, difference that lipase is high temperature resistant, in production process, high temperature is comparatively large on enzyme impact of living, and the separation and purification of enzyme and enzyme immobilization cost higher.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art, there is provided a kind of cold-adapted enzyme ferment legal system for biological diesel-oil technique, this technology utilization cold-adapted enzyme ferment method can fast producing bio-diesel, has that cost is low, efficiency is high, nontoxicity, simple to operate, practical characteristic.
Object of the present invention is achieved through the following technical solutions: cold-adapted enzyme ferment legal system is for biological diesel-oil technique, and it comprises the following steps:
S1. stock oil is placed in drying room, improves baking room temperature degree to 145 ~ 155 DEG C fast with hotblast stove, make stock oil become the liquid state of flowing, wherein, stock oil to be oil length be 95 ~ 98% the hogwash fat solidified, sewer oil, acidification oil;
S2. liquid raw material oil oil pump is squeezed in No. 1 reactor, No. 1 biological enzyme composite catalyst of 1.5 ~ 2.5% is added in No. 1 reactor, liquid raw material oil is 48 ~ 55:1 with the weight part ratio of No. 1 biological composite catalyst, reaction 50 ~ 80min, obtain A liquid, wherein, No. 1 biological enzyme composite catalyst is the mixture of lipase and ferric sulfate, its weight part ratio is 0.8 ~ 1.2:1, and described lipase is one or more composite curing enzyme in the lipase produced by bacterium, fungi, yeast or animal pancreatic;
S3. be separated by A liquid supercentrifuge, the rotating speed of whizzer is 11000 ~ 13000rmp, and centrifugation time is 30 ~ 40min, and remove dregs and free phosphoric acid, obtain B liquid, B liquid pH is 6.5 ~ 7.5;
S4. B liquid oil pump is squeezed in No. 2 reactors, heating up makes the B liquid temp in No. 2 reactors be 68 ~ 78 DEG C, add the methyl alcohol of No. 2 biological enzyme composite catalysts and 13 ~ 18%, B liquid, methyl alcohol, the weight part ratio of No. 2 biological enzyme composite catalysts is (38 ~ 42): (7 ~ 13): 1, circulating reaction 5.5 ~ 6.5h, temperature of reaction is 65 ~ 75 DEG C, obtain coarse biodiesel, wherein, No. 2 biological enzyme composite catalysts are the mixture of lipase and toluenesulphonic acids copper crystal, its weight part ratio is 1:2 ~ 3, described lipase is by bacterium, fungi, one or more composite curing enzyme in the lipase that yeast or animal pancreatic produce,
S5. use the centrifugal coarse biodiesel of supercentrifuge, the rotating speed of whizzer is 11000 ~ 13000rmp, and centrifugation time is 80 ~ 90min, removes glycerine and remaining catalyzer, obtains C liquid;
S6. be driven in No. 3 reactors by C liquid oil pump, being warming up to C liquid temp is after 105 ~ 115 DEG C, adds the discoloring agent dioxide peroxide of 2.5 ~ 3.5%, and the weight part ratio of C liquid and discoloring agent is 30 ~ 33:1, and reaction 28 ~ 40h, Plate Filtration, obtains biofuel.
The present invention has the following advantages: present invention utilizes hogwash fat, sewer oil, acidifying wet goods waste resource, compound biological enzyme is utilized to be converted into the biofuel of environment-friendly type for catalyst reaction, environmental pollution can be reduced and can save fossil energy again, non-edibility grease is turned waste into wealth, alleviates the situation that China's fossil diesel fuel is day by day in short supply; Present invention process reaction conditions is gentle, and without the need to pressurization, biological enzyme ferment temperature of reaction is not also higher than 78 DEG C, with short production cycle, has that cost is low, efficiency is high, nontoxicity, simple to operate, practical characteristic.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, and protection scope of the present invention is not limited to the following stated.
embodiment 1:cold-adapted enzyme ferment legal system is for biological diesel-oil technique, and it comprises the following steps:
S1. by oil length be 95% the hogwash fat solidified be placed in drying room, improve baking room temperature degree to 145 DEG C fast with hotblast stove, make hogwash fat become the liquid state of flowing;
S2. liquid hogwash fat oil pump is squeezed in No. 1 reactor, No. 1 biological enzyme composite catalyst of 1.5% is added in No. 1 reactor, the weight part ratio of liquid hogwash fat and No. 1 biological composite catalyst is 48:1, reaction 50min, obtain A liquid, wherein, No. 1 biological enzyme composite catalyst is the mixture of lipase and ferric sulfate, its weight part ratio is 0.8:1, and described lipase is by bacteriogenic lipase;
S3. be separated by A liquid supercentrifuge, the rotating speed of whizzer is 11000rmp, and centrifugation time is 30min, and remove dregs and free phosphoric acid, obtain B liquid, B liquid pH is 6.5;
S4. B liquid oil pump is squeezed in No. 2 reactors, heating up makes the B liquid temp in No. 2 reactors be 68 DEG C, add the methyl alcohol of No. 2 biological enzyme composite catalysts and 13%, the weight part ratio of B liquid, methyl alcohol, No. 2 biological enzyme composite catalysts is 38:7:1, circulating reaction 5.5h, temperature of reaction is 65 DEG C, obtain coarse biodiesel, wherein, No. 2 biological enzyme composite catalysts are the mixture of lipase and toluenesulphonic acids copper crystal, its weight part ratio is 1:2, and described lipase is by bacterium and mycetogenetic composite curing enzyme;
S5. use the centrifugal coarse biodiesel of supercentrifuge, the rotating speed of whizzer is 11000rmp, and centrifugation time is 80min, removes glycerine and remaining catalyzer, obtains C liquid;
S6. be driven in No. 3 reactors by C liquid oil pump, being warming up to C liquid temp is after 105 DEG C, adds the discoloring agent dioxide peroxide of 2.5%, and the weight part ratio of C liquid and discoloring agent is 30:1, and reaction 28h, Plate Filtration, obtains biofuel.
embodiment 2:cold-adapted enzyme ferment legal system is for biological diesel-oil technique, and it comprises the following steps:
S1. by oil length be 98% the acidification oil solidified be placed in drying room, improve baking room temperature degree to 155 DEG C fast with hotblast stove, make acidification oil become the liquid state of flowing;
S2. liquid acids carburetion oil pump is squeezed in No. 1 reactor, No. 1 biological enzyme composite catalyst of 2.5% is added in No. 1 reactor, the weight part ratio of liquid acids carburetion and No. 1 biological composite catalyst is 55:1, reaction 80min, obtain A liquid, wherein, No. 1 biological enzyme composite catalyst is the mixture of lipase and ferric sulfate, its weight part ratio is 1.2:1, and described lipase is the lipase produced by animal pancreatic;
S3. be separated by A liquid supercentrifuge, the rotating speed of whizzer is 13000rmp, and centrifugation time is 40min, and remove dregs and free phosphoric acid, obtain B liquid, B liquid pH is 7.5;
S4. B liquid oil pump is squeezed in No. 2 reactors, heating up makes the B liquid temp in No. 2 reactors be 78 DEG C, add the methyl alcohol of No. 2 biological enzyme composite catalysts and 18%, the weight part ratio of B liquid, methyl alcohol, No. 2 biological enzyme composite catalysts is 42:13:1, circulating reaction 6.5h, temperature of reaction is 75 DEG C, obtain coarse biodiesel, wherein, No. 2 biological enzyme composite catalysts are the mixture of lipase and toluenesulphonic acids copper crystal, its weight part ratio is 1:3, and described lipase is the lipase produced by yeast;
S5. use the centrifugal coarse biodiesel of supercentrifuge, the rotating speed of whizzer is 13000rmp, and centrifugation time is 90min, removes glycerine and remaining catalyzer, obtains C liquid;
S6. be driven in No. 3 reactors by C liquid oil pump, being warming up to C liquid temp is after 115 DEG C, adds the discoloring agent dioxide peroxide of 3.5%, and the weight part ratio of C liquid and discoloring agent is 33:1, and reaction 40h, Plate Filtration, obtains biofuel.
embodiment 3:cold-adapted enzyme ferment legal system is for biological diesel-oil technique, and it comprises the following steps:
S1. by oil length be 97% the sewer oil that solidifies be placed in drying room, improve baking room temperature degree to 150 DEG C fast with hotblast stove, make sewer oil become the liquid state of flowing;
S2. liquid sewer oil oil pump is squeezed in No. 1 reactor, No. 1 biological enzyme composite catalyst of 2% is added in No. 1 reactor, the weight part ratio of liquid sewer oil and No. 1 biological composite catalyst is 50:1, reaction 60min, obtain A liquid, wherein, No. 1 biological enzyme composite catalyst is the mixture of lipase and ferric sulfate, its weight part ratio is 1:1, and described lipase is the composite curing enzyme produced by bacterium, fungi and animal pancreatic;
S3. be separated by A liquid supercentrifuge, the rotating speed of whizzer is 12000rmp, and centrifugation time is 35min, and remove dregs and free phosphoric acid, obtain B liquid, B liquid pH is 7;
S4. B liquid oil pump is squeezed in No. 2 reactors, heating up makes the B liquid temp in No. 2 reactors be 72 DEG C, add the methyl alcohol of No. 2 biological enzyme composite catalysts and 15%, the weight part ratio of B liquid, methyl alcohol, No. 2 biological enzyme composite catalysts is 40:10:1, circulating reaction 6h, temperature of reaction is 70 DEG C, obtain coarse biodiesel, wherein, No. 2 biological enzyme composite catalysts are the mixture of lipase and toluenesulphonic acids copper crystal, its weight part ratio is 1:2.5, and described lipase is the composite curing enzyme produced by bacterium, fungi and yeast;
S5. use the centrifugal coarse biodiesel of supercentrifuge, the rotating speed of whizzer is 12000rmp, and centrifugation time is 85min, removes glycerine and remaining catalyzer, obtains C liquid;
S6. be driven in No. 3 reactors by C liquid oil pump, being warming up to C liquid temp is after 110 DEG C, adds the discoloring agent dioxide peroxide of 3%, and the weight part ratio of C liquid and discoloring agent is 31:1, and reaction 35h, Plate Filtration, obtains biofuel.
embodiment 4:cold-adapted enzyme ferment legal system is for biological diesel-oil technique, and it comprises the following steps:
S1. by oil length be 95% the hogwash fat solidified be placed in drying room, improve baking room temperature degree to 155 DEG C fast with hotblast stove, make stock oil become the liquid state of flowing;
S2. liquid hogwash fat oil pump is squeezed in No. 1 reactor, No. 1 biological enzyme composite catalyst of 2.3% is added in No. 1 reactor, the weight part ratio of liquid swill and No. 1 biological composite catalyst is 55:1, reaction 70min, obtain A liquid, wherein, No. 1 biological enzyme composite catalyst is the mixture of lipase and ferric sulfate, its weight part ratio is 0.8:1, and described lipase is by mycetogenetic lipase;
S3. be separated by A liquid supercentrifuge, the rotating speed of whizzer is 13000rmp, and centrifugation time is 30min, and remove dregs and free phosphoric acid, obtain B liquid, B liquid pH is 7;
S4. B liquid oil pump is squeezed in No. 2 reactors, heating up makes the B liquid temp in No. 2 reactors be 75 DEG C, add the methyl alcohol of No. 2 biological enzyme composite catalysts and 18%, the weight part ratio of B liquid, methyl alcohol, No. 2 biological enzyme composite catalysts is 42:10:1, circulating reaction 5.5h, temperature of reaction is 72 DEG C, obtain coarse biodiesel, wherein, No. 2 biological enzyme composite catalysts are the mixture of lipase and toluenesulphonic acids copper crystal, its weight part ratio is 1:2, and described lipase is the composite curing enzyme produced by yeast and animal pancreatic;
S5. use the centrifugal coarse biodiesel of supercentrifuge, the rotating speed of whizzer is 13000rmp, and centrifugation time is 80min, removes glycerine and remaining catalyzer, obtains C liquid;
S6. be driven in No. 3 reactors by C liquid oil pump, being warming up to C liquid temp is after 108 DEG C, adds the discoloring agent dioxide peroxide of 3%, and the weight part ratio of C liquid and discoloring agent is 33:1, and reaction 28h, Plate Filtration, obtains biofuel.
Claims (1)
1. cold-adapted enzyme ferment legal system is for biological diesel-oil technique, it is characterized in that, it comprises the following steps:
S1. stock oil is placed in drying room, improves baking room temperature degree to 145 ~ 155 DEG C fast with hotblast stove, make stock oil become the liquid state of flowing; Wherein, described stock oil to be oil length be 95 ~ 98% the hogwash fat solidified, sewer oil, acidification oil;
S2. liquid raw material oil oil pump is squeezed in No. 1 reactor, No. 1 biological enzyme composite catalyst of 1.5 ~ 2.5% is added in No. 1 reactor, liquid raw material oil is 48 ~ 55:1 with the weight part ratio of No. 1 biological composite catalyst, reaction 50 ~ 80min, obtain A liquid, wherein, No. 1 biological enzyme composite catalyst is the mixture of lipase and ferric sulfate, and its weight part ratio is 0.8 ~ 1.2:1; Wherein, described lipase is one or more composite curing enzyme in the lipase produced by bacterium, fungi, yeast or animal pancreatic;
S3. be separated by A liquid supercentrifuge, the rotating speed of whizzer is 11000 ~ 13000rmp, and centrifugation time is 30 ~ 40min, and remove dregs and free phosphoric acid, obtain B liquid, B liquid pH is 6.5 ~ 7.5;
S4. B liquid oil pump is squeezed in No. 2 reactors, heating up makes the B liquid temp in No. 2 reactors be 68 ~ 78 DEG C, add the methyl alcohol of No. 2 biological enzyme composite catalysts and 13 ~ 18%, the weight part ratio of B liquid, methyl alcohol, No. 2 biological enzyme composite catalysts is 38 ~ 42:7 ~ 13:1, circulating reaction 5.5 ~ 6.5h, and temperature of reaction is 65 ~ 75 DEG C, obtain coarse biodiesel, wherein, No. 2 biological enzyme composite catalysts are the mixture of lipase and toluenesulphonic acids copper crystal, and its weight part is 1:2 ~ 3; Described lipase is one or more composite curing enzyme in the lipase produced by bacterium, fungi, yeast or animal pancreatic;
S5. use the centrifugal coarse biodiesel of supercentrifuge, the rotating speed of whizzer is 11000 ~ 13000rmp, and centrifugation time is 80 ~ 90min, removes glycerine and remaining catalyzer, obtains C liquid;
S6. be driven in No. 3 reactors by C liquid oil pump, being warming up to C liquid temp is, after 105 ~ 115 DEG C, add the discoloring agent of 2.5 ~ 3.5%, reaction 28 ~ 40h, Plate Filtration, obtains biofuel, wherein, described discoloring agent is dioxide peroxide, and the weight ratio of C liquid and discoloring agent is 30 ~ 33:1.
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| CN1412278A (en) * | 2002-11-04 | 2003-04-23 | 宋庭礼 | Method for producing biological diesel oil by using high-acidity waste animal and vegetable oil |
| CN1303187C (en) * | 2005-10-08 | 2007-03-07 | 暨南大学 | Method for synthesizing biodiesel utilizing swill water oil |
| CN100451088C (en) * | 2006-12-07 | 2009-01-14 | 张以光 | Production process of biological diesel oil |
| CN101696372B (en) * | 2009-11-03 | 2012-12-26 | 合肥工业大学 | Method for preparing biodiesel by solid acid-base two-step method |
| CN102925287A (en) * | 2012-11-19 | 2013-02-13 | 北京化工大学 | Method for preparing biodiesel by biological-chemical catalytic coupling |
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