CN101148600A - Method for preparing biological diesel oil from waste animals and plants grease - Google Patents
Method for preparing biological diesel oil from waste animals and plants grease Download PDFInfo
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- CN101148600A CN101148600A CNA2007101350093A CN200710135009A CN101148600A CN 101148600 A CN101148600 A CN 101148600A CN A2007101350093 A CNA2007101350093 A CN A2007101350093A CN 200710135009 A CN200710135009 A CN 200710135009A CN 101148600 A CN101148600 A CN 101148600A
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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
- 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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Abstract
The improved continuous esterification process of waste animal and vegetable oil and grease with low carbon alcohol to prepare biodiesel oil features that liquid low carbon alcohol is introduced into the liquid comprising liquid waste animal and vegetable oil and grease in 95-99.9 wt% and acid catalyst in 0.1-5 wt% to produce esterification reaction at normal pressure and the temperature from vaporizing temperature to 95 deg.c while the vapor mixture comprising the resultant, water vapor and low carbon alcohol vapor is discharged from the top of the reactor and separated in a fractionating tower to obtain product, separated water and liquid low carbon alcohol for reuse. The process has high reaction speed, high reaction conversion rate and other advantages, and the product has acid value capable of being controlled below 2 mgKOH/g.
Description
Technical field
The present invention relates to a kind of biodiesel oil preparing process, is raw material with the aste vegetable oil and animal fat particularly, and the low-carbon alcohol continuous esterification prepares the biofuel method.
Background technology
Biofuel is by to animal-plant oil, under the alkaline catalysts effect, carry out the fatty acid ester (mixing-in fat acid low carbon alcohol ester) that transesterification reaction makes with low-carbon alcohol (as methyl alcohol, ethanol, butanols etc.), have renewable, readily biodegradable, nontoxic, sulphur content is low and waste gas in advantages such as emissions figure is little, be environmentally friendly fuel.
With aste vegetable oil and animal fat (acidifying oil, sewer oil, hogwash fat, carclazyte wet goods) is the feedstock production biofuel, can reduce cost, and has found fine method of disposal for these waste oil again simultaneously.Yet because the waste oil main component comprises grease and lipid acid, the existence of abundant fatty acid can not directly adopt base catalysis and low-carbon alcohol to carry out transesterify.Therefore, preparing biological diesel oil from waste animals and plants grease, generally all adopt the two-step catalysis reaction, generate fatty acid ester of low-carbon alcohol by fatty acid esterification reaction in acid catalysis low-carbon alcohol and the aste vegetable oil and animal fat earlier, the grease in base catalysis low-carbon alcohol again and the aste vegetable oil and animal fat carries out transesterification reaction.The esterification of the first step acid catalysis lipid acid and low-carbon alcohol, major part are to adopt low-carbon alcohol once to add to carry out back flow reaction, as described in Chinese patent CN1743417, CN1958727.This deficiency that once adds back flow reaction is: the moisture of generation (reaction water, carry water) is all the time in reactor, and fatty acid response is a reversing process in low-carbon alcohol and the raw material, there is moisture to exist in the reaction system, can make the esterification of lipid acid and low-carbon alcohol be difficult to complete reaction, and then influence esterification reaction rate and equilibrium conversion, esterification produces the acid number height, influences the follow-up second step base catalyzed reactions, for example easily produces soap class byproduct in the base-catalyzed transesterification reaction process.
It is the feedstock production biodiesel processes that Chinese patent CN1995288 discloses with oil from high acid value waste animal and plant fat and neutral grease, adopt " sealing continuous esterification-transesterify-methanol vapor distillation " technology, continuous esterification, tape loop water and methanol rectification dehydration are organically combined, make the aqueous methanol steam of generation enter the methanol fractionation system of forming by methanol rectification post and reboiler, the anhydrous methanol vapour condensation that rectifying obtains is after bumper post returns esterification device, water then stays in reboiler, realizes that circulation divides water and continuous esterification.Though the moisture that this method can produce reaction is taken out of by methanol vapor and is separated, shortcoming is: esterification adopts the band press operation, and the reactor methanol vapour phase is leaked easily, has increased unsafe factor; Secondly, methyl alcohol is added by reactor top, because reactor temperature is higher than the methyl alcohol vaporization temperature, in fact methyl alcohol enter behind the reactor major part and vaporize, have only the part methanol steam to be inhaled in the reaction system with bubble form like this and carry out the gas-liquid two-phase reaction with grease (liquid phase) by stirring, owing to have resistance to mass transfer between gas-liquid two-phase, reaction mainly takes place on gas liquid film, causes the esterification effect to reduce; Besides, enter the methyl alcohol vaporization of reactor, also suppressed the aqueous methanol steam of inside reactor generation and discharged fast, cause moisture to take weak effect out of, also reduced the speed of esterification to a certain extent, and influence the follow-up second step base catalyzed reactions.
Chinese patent CN100999680 is disclosed to prepare biodiesel esterification technology with waste oil, waste oil with 97～99.8% and 0.2～3% porous support solid acid catalyst, under temperature of reaction 95-130 ℃, normal pressure, feed vapour phase methyl alcohol continuously by reactor bottom or bottom, stir and carried out esterification in 1～4 hour, reaction is isolated solid acid catalyst after finishing.This method advantage is that the methyl alcohol vapour phase enters from the bottom, and discharges from reactor continuously, makes moisture that the fatty acid response in methyl alcohol and the waste oil generates, reaches in the waste oil original moisture and take reactor out of.But shortcoming is with above-mentioned CN1995288, methyl alcohol also is to enter in the reaction system with gas form, the methyl alcohol of vapour phase and liquid phase grease form gas-liquid two-phase, because of catalyzer is a solid acid catalyst, the real reaction system is gas-liquid-solid phase reaction, because the gas-liquid-solid three alternate resistance to mass transfers that exist also can reduce esterification reaction rate, cause the esterification effect to reduce; Secondly, temperature of reaction is higher relatively, and energy consumption is bigger, and needs to increase methyl alcohol vaporizer and control corresponding system, and equipment multioperation inconvenience causes the technology controlling and process difficulty.
Summary of the invention
The object of the invention is to overcome the deficiency of above-mentioned prior art, provides a kind of simple to equipment requirements, esterification efficient height, and speed is fast, sufficient reacting, the high method for preparing biological diesel oil from waste animals and plants grease of conversion rate of fatty acid in the aste vegetable oil and animal fat.
The object of the invention realizes, the main improvement is to adopt the liquid phase low-carbon alcohol to be supplied with continuously by reactor bottom, and the lipid acid in vaporization and the aste vegetable oil and animal fat carries out continuous esterification, and takes moisture in the reaction system out of, overcome the deficiencies in the prior art, realize the object of the invention.Specifically, method for preparing biological diesel oil from waste animals and plants grease of the present invention, comprise low-carbon alcohol acid catalyzed esterification and base-catalyzed transesterification optionally, it is characterized in that the low-carbon alcohol acid catalyzed esterification is the liquid phase aste vegetable oil and animal fat by 95～99.9wt%, 0.1%～5wt% an acidic catalyst, in normal pressure and low-carbon alcohol vaporization temperature～95 ℃, in the reactor liquid phase, feed the esterification of liquid phase low-carbon alcohol continuously, reaction produces moisture in water and the aste vegetable oil and animal fat, discharge from the reactor upper top continuously with low carbon alcohol vapor, mix vapour phase directly or be condensed into liquid phase and enter pure rectifying tower, after isolating moisture, liquid phase low-carbon alcohol cyclically utilizing, detection reaction product acid number is reduced to 2mgKOH/g or following, finish esterification, isolate catalyzer.
The inventive method if the raw material aste vegetable oil and animal fat is high acid value (for example greater than 160mgKOH/g or more than), needn't be carried out transesterification reaction because fat content is very low, then can omit follow-up base catalyzed reactions; Otherwise after the esterification, need to carry out for second step and under alkaline catalysts catalysis, carry out transesterification reaction by prior art.
The inventive method better is that the liquid phase low-carbon alcohol is fed by reactor bottom, is more conducive to and the abundant esterification of liquid phase aste vegetable oil and animal fat.Low-carbon alcohol feeding amount is looked fatty acid content and esterification transformation efficiency in the aste vegetable oil and animal fat, by detecting the control of esterification acid number.
Acid-catalyzed esterification reaction temperature of the present invention, lower limit only need reach the low-carbon alcohol vaporization temperature, and the liquid phase low-carbon alcohol that enters so just can be vaporized in the liquid phase aste vegetable oil and animal fat and be taken moisture out of; Its upper limit is lower than the grease safety temperature for 95 ℃, can prevent that grease from decomposing variation.
More preferably a kind of, the low-carbon alcohol that reactor comes out, the vapour mixture of water are without condensation, directly entering methanol rectifying tower separates, can save low-carbon alcohol, the water required heat of in pure rectifying tower, vaporizing, help reducing the rectifying energy consumption, also saved the low-carbon alcohol of coming out in the reactor, the required water of condensation of vapour mixture condensation of water.
An acidic catalyst and basic catalyst among the present invention for known biodiesel manufacture catalyzer, have no special requirements.For example solid acid catalyst can be Fe
2O
3/ SO
4 2-/ carrier, loading type sulfuric acid/carclazyte, TiO
2/ SO
4 2-/ carrier, heteropolyacid, resin cation (R.C.) etc.; Or liquid acid catalyst, as sulfuric acid, phosphoric acid, hydrochloric acid etc.Basic catalyst comprises existing solid alkali and liquid alkali catalyst equally.If adopt liquid acid catalyst, after reaction finished, by the reaction product sedimentation, after liquid acid catalyst and small amount of impurities separated, reaction product was that available alkaline catalysts catalysis low-carbon alcohol and grease carry out preparing biodiesel by ester exchange; If make catalyzer with solid acid, after reaction finishes, overanxious go out catalyzer and small amount of impurities after, reaction product can be carried out transesterification reaction with alkaline catalysts catalysis low-carbon alcohol and grease equally and be prepared biofuel.
Method for preparing biological diesel oil from waste animals and plants grease of the present invention, use the liquid phase low-carbon alcohol instead and add mode in the reaction liquid phase continuously, liquid phase low-carbon alcohol and liquid phase waste oil mix, under the effect of an acidic catalyst, carry out esterification, owing to be homogeneous reaction, so esterification reaction rate is accelerated thoroughly, reaction time of esterification can be reduced to 0.5～2 hour, the esterification transformation efficiency of lipid acid reaches more than 99% in the waste grease raw material, and acid number can be controlled below the 2mgKOH/g, and it is few to produce soap class byproduct in the base-catalyzed transesterification reaction process.The liquid phase low-carbon alcohol is both as reactant, vaporization is simultaneously carried agent as moisture again, can take moisture out of reactor equally, and the liquid phase low-carbon alcohol is at inside reactor vaporization band water, not only with aste vegetable oil and animal fat in the fatty acid esterification sufficient reacting, speed up, but also need not set up additional methyl alcohol vaporising device, low equipment investment is operated also simple.
Description of drawings
Accompanying drawing is a kind of optimization schematic flow sheet of the inventive method.
Embodiment
Embodiment 1: at 3M
3In the reactor, (main component is a lipid acid to add acidifying oil, acid number 189.3mgKOH/g oil, fat content is very low and needn't carry out transesterification reaction,) 2000KG, about about 65 ℃ of stirring heating, add catalyst sulfuric acid 20KG, liquid phase methyl alcohol pumps into from reactor bottom continuously, and temperature of reactor is increased to and carries out esterification about 75 ℃, vapour phase (the methyl alcohol that comes out from reactor head, water) directly enter methanol rectifying tower, separate the liquid phase methyl alcohol behind the moisture, return from reactor bottom and add, when react drop to 0.75mgKOH/g to acid number after, esterification finishes (about 2 hours), lower floor's sulfuric acid catalyst and small amount of impurities are isolated in reaction solution sedimentation 4 hours (or direct centrifugal treating), get upper strata coarse biodiesel (acid number is a 0.75mgKOH/g oil), after the washing decolouring is handled, promptly get biofuel.
Embodiment 2: at 3M
3In the reactor, (main component is a Vegetable oil lipoprotein to add carclazyte oil, little fat acid, acid number 14.21mgKOH/g oil) 2000KG, stirring heating adds catalyst sulfuric acid 18KG for about about 65 ℃, liquid phase methyl alcohol is carried out esterification from the reactor bottom adding continuously, and temperature of reactor progressively is elevated to about 75 ℃, and the vapour phase of coming out from reactor (methyl alcohol, water) directly enters methanol rectifying tower.When react drop to 1mgKOH/g to acid number after, esterification finishes (about 0.5 hour), lower floor's sulfuric acid catalyst and small amount of impurities are isolated in reaction solution sedimentation 4 hours, the upper strata is that acid number is a 0.92mgKOH/g oil.
Again the carclazyte after this esterification oil and methyl alcohol are carried out transesterification reaction under the catalysis of alkaline catalysts, sedimentation 8 hours, or after centrifugation goes out glycerine, can obtain biofuel after the processing.
Embodiment 3: at 3M
3In the reactor, add refining sewer oil (main component is animal-plant oil, lipid acid, acid number 65.86mgKOH/g oil) 2000KG, add solid catalyst Fe
2O
3/ SO
4 2-/ carrier 40KG, about about 70 ℃ of stirring heating, liquid phase methyl alcohol carries out esterification from the reactor bottom adding continuously, and temperature of reactor progressively is elevated to about 100 ℃, and the vapour phase of coming out from reactor (methyl alcohol, water) directly enters methanol rectifying tower.When react drop to 2mgKOH/g to acid number after, esterification finishes (about 1.5 hours), lower floor's catalyst sulfuric acid iron and small amount of impurities are isolated in reaction solution sedimentation 4 hours, upper strata reactant acid number is a 0.82mgKOH/g oil.
Again sewer oil after this esterification and methyl alcohol are carried out transesterification reaction under the catalysis of alkaline catalysts, sedimentation 8 hours, or after centrifugation goes out glycerine, can obtain biofuel after the processing.
Embodiment 4: at 3M
3In the reactor, (main component is animal-plant oil, lipid acid to add refining sewer oil, acid number 105.6mgKOH/g oil) 2000KG, add loading type heteropoly phosphorus molybdenum tungstic acid 40KG, about about 70 ℃ of stirring heating, liquid phase methyl alcohol carries out esterification from the reactor bottom adding continuously, and temperature of reactor progressively is elevated to about 100 ℃, and the vapour phase of coming out from reactor (methyl alcohol, water) directly enters methanol rectifying tower.When react drop to 2mgKOH/g to acid number after, esterification finishes (about 1.5 hours), lower floor's catalyst sulfuric acid hydrogen sodium and small amount of impurities are isolated in reaction solution sedimentation 6 hours, upper strata reactant acid number is a 0.93mgKOH/g oil.
Again sewer oil after this esterification and methyl alcohol are carried out transesterification reaction under the catalysis of alkaline catalysts, sedimentation 8 hours, or after centrifugation goes out glycerine, can obtain biofuel after the processing.
Embodiment 5: at 3M
3In the reactor, add hogwash fat (main component is animal-plant oil, lipid acid, acid number 12.4mgKOH/g oil) 2000KG, add solid catalyst TiO
2/ SO
4 2-/ carrier 40KG, about about 65 ℃ of stirring heating, liquid phase methyl alcohol carries out esterification from the reactor bottom adding continuously, temperature of reactor progressively is elevated to about 90 ℃, and the vapour phase of coming out from reactor (methyl alcohol, water) directly enters methanol rectifying tower, after the acid number of reactant drops to 2mgKOH/g, esterification finishes (about 0.5 hour), lower floor's solid catalyst and small amount of impurities are isolated in reaction solution sedimentation 6 hours, and upper strata reactant acid number is a 0.77mgKOH/g oil.
Again sewer oil after this esterification and methyl alcohol are carried out transesterification reaction under the catalysis of alkaline catalysts, sedimentation 8 hours, or after centrifugation goes out glycerine, can obtain biofuel after the processing.
In addition, the present invention can also be with ethanol, butanols instead of methanol.
Claims (3)
1. method for preparing biological diesel oil from waste animals and plants grease, comprise low-carbon alcohol acid catalyzed esterification and base-catalyzed transesterification optionally, it is characterized in that the low-carbon alcohol acid catalyzed esterification is the liquid phase aste vegetable oil and animal fat by 95～99.9wt%, 0.1%～5wt% an acidic catalyst, in normal pressure and low-carbon alcohol vaporization temperature～95 ℃, in the reactor liquid phase, feed the esterification of liquid phase low-carbon alcohol continuously, reaction produces moisture in water and the aste vegetable oil and animal fat, discharge from the reactor upper top continuously with low carbon alcohol vapor, mix vapour phase directly or be condensed into liquid phase and enter pure rectifying tower, after isolating moisture, liquid phase low-carbon alcohol cyclically utilizing, detection reaction product acid number is reduced to 2mgKOH/g or following, finishes esterification, isolates catalyzer.
2. according to the described method for preparing biological diesel oil from waste animals and plants grease of claim 1, it is characterized in that the liquid phase low-carbon alcohol is fed by reactor bottom.
3. according to claim 1 or 2 described method for preparing biological diesel oil from waste animals and plants grease, the vapour mixture that it is characterized in that low-carbon alcohol that reactor comes out, water directly enters methanol rectifying tower and separates without condensation.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101350093A CN101148600B (en) | 2007-10-18 | 2007-10-18 | Method for preparing biological diesel oil from waste animals and plants grease |
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|---|---|---|---|
| CN2007101350093A CN101148600B (en) | 2007-10-18 | 2007-10-18 | Method for preparing biological diesel oil from waste animals and plants grease |
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| CN101148600A true CN101148600A (en) | 2008-03-26 |
| CN101148600B CN101148600B (en) | 2012-08-15 |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747182A (en) * | 2008-12-01 | 2010-06-23 | 浙江东江能源科技有限公司 | Low acid value esterification novel process |
| CN101338214B (en) * | 2008-08-08 | 2012-05-09 | 贵州大学 | Method for preparing biodiesel using acidizing oil as raw material under normal pressure |
| CN102465058A (en) * | 2010-11-04 | 2012-05-23 | 朱建军 | Production process for preparing biodiesel |
| CN102580977A (en) * | 2011-12-31 | 2012-07-18 | 福建广汇龙环保科技有限公司 | System for transforming kitchen waste into new energy |
| CN102851122A (en) * | 2011-06-30 | 2013-01-02 | 中国石油化工股份有限公司 | Method for preparation of fatty acid ester |
| CN102994235A (en) * | 2012-11-12 | 2013-03-27 | 江苏高科石化股份有限公司 | Method for preparing printing ink solvent and co-producing biodiesel by utilizing waste animal and plant oil |
| CN103013678A (en) * | 2011-09-20 | 2013-04-03 | 中国石油化工股份有限公司 | Method for reducing biodiesel crude product acid value, and biodiesel preparation method |
| CN104673502A (en) * | 2015-02-03 | 2015-06-03 | 江苏西方环保科技有限公司 | Continuous esterification technique for producing biodiesel from waste grease |
| CN105112168A (en) * | 2015-08-21 | 2015-12-02 | 中国石油大学(华东) | Biodiesel producing device and method |
| CN105542970A (en) * | 2016-01-20 | 2016-05-04 | 定陶县地元生化制品有限公司 | Method and device for continuously producing biological diesel oil |
| CN107837811A (en) * | 2017-11-28 | 2018-03-27 | 广西锟德能源科技有限公司 | A kind of esterification catalyst, catalyzing esterification system and the method for preparing esterification catalyst and Esterification catalytic reaction |
| CN108048224A (en) * | 2018-01-25 | 2018-05-18 | 南通金利油脂工业有限公司 | Aliphatic acid produces the device and method of aliphatic ester |
| CN115254143A (en) * | 2022-06-23 | 2022-11-01 | 北京科技大学 | Preparation method and application of carbon-based solid acid catalyst |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100500810C (en) * | 2006-12-25 | 2009-06-17 | 昆明理工大学 | Process for preparing biodiesel oil |
-
2007
- 2007-10-18 CN CN2007101350093A patent/CN101148600B/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338214B (en) * | 2008-08-08 | 2012-05-09 | 贵州大学 | Method for preparing biodiesel using acidizing oil as raw material under normal pressure |
| CN101747182A (en) * | 2008-12-01 | 2010-06-23 | 浙江东江能源科技有限公司 | Low acid value esterification novel process |
| CN102465058A (en) * | 2010-11-04 | 2012-05-23 | 朱建军 | Production process for preparing biodiesel |
| CN102851122A (en) * | 2011-06-30 | 2013-01-02 | 中国石油化工股份有限公司 | Method for preparation of fatty acid ester |
| CN103013678A (en) * | 2011-09-20 | 2013-04-03 | 中国石油化工股份有限公司 | Method for reducing biodiesel crude product acid value, and biodiesel preparation method |
| CN103013678B (en) * | 2011-09-20 | 2014-12-31 | 中国石油化工股份有限公司 | Method for reducing biodiesel crude product acid value, and biodiesel preparation method |
| CN102580977A (en) * | 2011-12-31 | 2012-07-18 | 福建广汇龙环保科技有限公司 | System for transforming kitchen waste into new energy |
| CN102994235A (en) * | 2012-11-12 | 2013-03-27 | 江苏高科石化股份有限公司 | Method for preparing printing ink solvent and co-producing biodiesel by utilizing waste animal and plant oil |
| CN104673502A (en) * | 2015-02-03 | 2015-06-03 | 江苏西方环保科技有限公司 | Continuous esterification technique for producing biodiesel from waste grease |
| CN105112168A (en) * | 2015-08-21 | 2015-12-02 | 中国石油大学(华东) | Biodiesel producing device and method |
| CN105112168B (en) * | 2015-08-21 | 2018-10-26 | 中国石油大学(华东) | A kind of device and method producing biodiesel |
| CN105542970A (en) * | 2016-01-20 | 2016-05-04 | 定陶县地元生化制品有限公司 | Method and device for continuously producing biological diesel oil |
| CN107837811A (en) * | 2017-11-28 | 2018-03-27 | 广西锟德能源科技有限公司 | A kind of esterification catalyst, catalyzing esterification system and the method for preparing esterification catalyst and Esterification catalytic reaction |
| CN108048224A (en) * | 2018-01-25 | 2018-05-18 | 南通金利油脂工业有限公司 | Aliphatic acid produces the device and method of aliphatic ester |
| CN115254143A (en) * | 2022-06-23 | 2022-11-01 | 北京科技大学 | Preparation method and application of carbon-based solid acid catalyst |
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