CN103805343A - Method for continuously producing biodiesel by using two segments of fixed beds - Google Patents
Method for continuously producing biodiesel by using two segments of fixed beds Download PDFInfo
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- CN103805343A CN103805343A CN201210450361.7A CN201210450361A CN103805343A CN 103805343 A CN103805343 A CN 103805343A CN 201210450361 A CN201210450361 A CN 201210450361A CN 103805343 A CN103805343 A CN 103805343A
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Abstract
The invention relates to a method for continuously producing aliphatic ester type biodiesel by adopting two segments of fixed bed reactors by taking animal grease and plant grease or waste grease as a raw material. The method comprises the following steps: mixing the raw material grease with lower alcohol like methanol or ethanol, and allowing the mixture to successively pass through two fixed bed reactors which are connected in series and filled with a solid catalyst; performing an ester exchange reaction and an esterification reaction in the first reactor, separating glycerinum generated in the reaction from the mixture flowing out from the first reactor, then replenishing the lower alcohol into the second reactor for the esterification reaction, and separating the lower alcohol and glycerinum from the mixture flowing out from the second reactor to obtain the aliphatic ester type biodiesel. Through the method disclosed by the invention, the two reactors can be selectively filled with a solid acid catalyst or a solid alkali catalyst according to the quality of the raw material grease, and a glycerinum byproduct is removed in midway of the reaction so as to break chemical balance, so that efficient conversion of the raw material grease is realized, the production efficiency is improved, and a high-purity glycerinum byproduct can be produced.
Description
Technical field
The present invention relates to biochemical industry technical field of new energies, specifically relate to one and utilize double-fixed bed series connection, take animal-plant oil or waste grease as raw material, produce continuously the processing method of fatty acid ester biofuel.
Background technology
Due to the day by day shortage of fossil energy and the environmental problem of being brought by it, the exploitation of renewable and clean energy resource has been accelerated in countries in the world.Wherein, biofuel is exactly a kind of well fossil oil substitute.Biofuel is a kind of take animal-plant oil or waste grease as raw material, through the low alkane monoesters of longer chain fatty acid generating with the esterification of low-carbon alcohol or transesterification reaction.Compared with fossil diesel fuel, CO, NO that burning biofuel is discharged
xand the amount of particle dust all greatly reduces.In addition, compared with fossil diesel fuel, its high lubricity, high hexadecane value, high flash point all make it become a kind of well fossil diesel fuel substitute.
The method of production biofuel is mainly to be undertaken by transesterification reaction at present, and the animal-plant oil that is glycerin fatty acid ester by main component or waste grease react with low-carbon alcohol.Transesterification reaction is made up of a series of reversible reactions, and acid or alkali all can be used as its catalyzer (Renew.Sust.Energ.Rev.10,248-268,2006).When take homogeneous phase alkali as catalyzer, as NaOH, first be to generate sodium alkoxide with alcohol, then be alkoxyl group negative ion forms tetrahedral structure intermediate as the carbonyl carbon of nucleophilic reagent attack triglyceride level, alcohol as electrophilic reagent again attack tetrahedron intermediate obtain the intermediate of electroneutral tetrahedral structure, it produces fatty acid monoester and triglyceride by rearrangement again, triglyceride is converted into monoglyceride and fatty acid monoester by same mechanism again, is finally all converted into fatty acid monoester and glycerine.When take homogeneous acid as catalyzer, proton is first combined with the carbonyl of triglyceride level, forms carbocation intermediate.Protophilic methyl alcohol is combined with carbocation and is formed the intermediate of tetrahedral structure, and then it resolves into fatty acid monoester and triglyceride, and produces the reaction of proton catalysis next round.Triglyceride and monoglyceride are also by this process reaction.
In industrial production, using more is homogeneous catalyst, and EP0523767A2 discloses a kind of main process take homogeneous phase alkali as Catalyst Production biofuel, and homogeneous phase alkali is mainly NaOH and NaOCH
3.Under the effect of homogeneous phase alkaline catalysts, at lesser temps (40-65 ℃) with that in the short period, transesterify just can be carried out is more complete, but this process but has following shortcoming: first, after reaction completes, catalyzer can remain in reaction product, at this moment after needing first to neutralize with acid, remove homogeneous phase alkali again with a large amount of water, this process not only makes catalyzer not recycle, and the waste water producing also can bring larger subsequent treatment cost; In addition, because glycerine and water dissolve each other, the introducing meeting of large water gaging brings difficulty to the purification process of follow-up glycerine.In the time that the acid number of stock oil is greater than 5mg KOH/g, homogeneous phase alkali can with free fatty acids generation saponification reaction, thereby consume catalyzer.For high-acid-value material oil, can use homogeneous acid as catalyzer.CN1412278A has reported use H
2sO
4as the method for catalysis high acid value vegetable and animals oils production biofuel.Homogeneous acid and homogeneous phase alkali have same shortcoming, in addition also can etching apparatus.Therefore, use solid catalyst to address these problems.For solid catalyst, one of them advantage is to use fixed-bed reactor.Than tank reactor, the back-mixing of fixed-bed reactor is little, the mechanical wear of catalyzer is little and do not need catalyzer to separate, can be continuous carry out production operation.
S.Furuta etc. (Catalysis Communications, 5,721-723,2004) have reported the transesterification reaction that uses solid acid catalysis soya-bean oil and methyl alcohol in single hop fixed bed.The solid acid using is WO
3/ ZrO
2, be that 250 ℃, pressure are that 1atm, alcohol oil rate are that 40:1, WHSV are that under 0.75 condition, the yield of biofuel reaches 90% in temperature of reaction.
The content of the fatty acid methyl ester in the EU 14214 standard regulation biofuel of European Union is greater than 96.5%, and biofuel is difficult to separate by conventional methods with stock oil, thereby best terms of settlement is that stock oil is transformed completely.Transesterification reaction is a reversible reaction, carries out being subject to the impact of thermodynamical restriction in single hop reactor, and glycerin fatty acid ester can not transform completely.If connect two sections of fixed-bed reactor, constantly shift out byproduct glycerine to break chemical equilibrium in reaction process, thereby can realize efficient transesterification reaction.For transesterification reaction, the activity of acid catalyst is less than alkaline catalysts (J.Am.Oil Chem., 63,1375-1380,1986).Therefore, in order to adapt to more stock oil, particularly for the higher stock oil of acid number, the mode that uses solid acid catalyst and solid base catalyst to combine by two sections of fixed beds, the greatly productive expense of the reduction biofuel of degree.
The present invention can be converted into biofuel by stock oil completely by transesterify or esterification under gentle reaction conditions, and this process can be carried out continuously.In addition, the present invention has expanded the source range that comes of stock oil, has improved production efficiency simultaneously, has reduced production cost.In process of production, there is no the discharge of " three wastes ", can be to environment, and glycerine that can by-product high-quality.Therefore, the present invention has good application prospect.
Summary of the invention
The object of the present invention is to provide a kind of processing method of two sections of fixed bed continuous production of biodiesels.
The present invention has taked following technical scheme:
1) animal-plant oil or waste grease raw material are mixed by a certain amount of with the low-carbon alcohol such as methyl alcohol or ethanol, then inject the first fixed-bed reactor that are filled with solid catalyst, transesterify and esterification occur under certain condition, and animal-plant oil or waste grease Partial Conversion are fatty acid ester biofuel;
2) glycerin layer in mixture after the reaction that in step a, the first fixed-bed reactor flow out is separated;
3) mixture after step b separation of glycerin layer is supplemented to the low-carbon alcohol such as a certain amount of methyl alcohol or ethanol, then inject the second fixed-bed reactor that are filled with solid catalyst, react under certain condition, raw oil material is converted into fatty acid ester biofuel completely;
4) glycerin layer in mixture after the reaction that in step c, the second fixed-bed reactor flow out is separated, obtain fatty acid ester biofuel.
In technique scheme, in the time that the acid number of animal-plant oil or waste grease is less than 5mg KOH/g, the solid catalyst of two fixed-bed reactor fillings is solid base catalyst; When the acid number of animal-plant oil or waste grease is greater than 5mg KOH/g, the first fixed-bed reactor filling solid acid catalyst, the second fixed-bed reactor filling solid alkaline catalysts.
In technique scheme, between two fixed-bed reactor reactions, be provided with separating step, the glycerin layer after the reaction that the first fixed-bed reactor are flowed out in mixture separates.
In technique scheme, after the reaction that the first fixed-bed reactor flow out after mixture separation glycerin layer, press massfraction and supplement 1 ~ 10% low-carbon alcohol, then inject the second fixed-bed reactor reaction that is filled with solid catalyst, preferred massfraction is 0.5 ~ 5%.
In technique scheme, inject the reactant animal-plant oil of the first fixed-bed reactor or waste grease raw material and the low-carbon alcohol such as methyl alcohol or ethanol in mass ratio 2:1 ~ 10:1 mix, preferably mass ratio is 3:1 ~ 5:1.
In technique scheme, after the first fixed-bed reactor reaction, animal-plant oil or waste grease 40% ~ 80% are converted into fatty acid ester biofuel, and preferred transformation efficiency is 60% ~ 80%.
In technique scheme, the reaction conditions of the first reactor, temperature is 120 ~ 220 ℃, and pressure is 0.1 ~ 4.0MPa, and volume space velocity is 0.5 ~ 5.0h
-1; Preferred reaction conditions, temperature is 140 ~ 200 ℃, and pressure is 0.1 ~ 3.0MPa, and volume space velocity is 0.5 ~ 5.0h
-1.
In technique scheme, the reaction conditions of the second reactor is 120 ~ 220 ℃, and pressure is 0.1 ~ 4.0MPa, and volume space velocity is 0.5 ~ 5.0h
-1preferred reaction conditions, temperature is 140 ~ 200 ℃, and pressure is 0.1 ~ 3.0MPa, and volume space velocity is 0.5 ~ 5.0h
-1.
In above-mentioned technology water case, the glycerin layer in mixture is the thing that dissolves each other of glycerine and low-carbon alcohol, and it separates with oil reservoir by centrifugal separation or stratification method.
In technique scheme, unreacted low-carbon alcohol can recycle.
In technique scheme, animal-plant oil or waste grease raw material can be soybean oil, plam oil, rapeseed oil, peanut oil, little Chinese parasol tree oil, Oleum Gossypii semen, engineering algae oil, lard, food and drink abendoned oil, expired animal-plant oil, or their mixture.
In technique scheme, low-carbon alcohol is methyl alcohol or ethanol, preferably methyl alcohol.
In technique scheme, the solid acid using and solid alkali have active high, the feature of good stability.
Beneficial effect: the present invention utilizes the method production biofuel of two sections of fixed beds, can be applicable to various neutrality and acid animal-plant oil or waste grease.Than single fixed-bed process, owing to the glycerine producing in reaction process being discharged between two sections of fixed beds, break the equilibrium state of chemical reaction, impel reversible reaction to carry out to generating biofuel direction, not only improve the efficiency of transesterification reaction, also improved the quality of biofuel.The present invention can be continuous production biofuel, reaction conditions gentleness, and can by-product the glycerine of high-quality.Therefore, the present invention has good application prospect.
Embodiment:
Below in conjunction with specific embodiment, the invention will be further described, and embodiment is not limited.
Embodiment 1: product inspection method
The acid number of sample detects according to GB/T5530-2005 method;
Product gas chromatographic analysis, chromatographic condition: capillary column (DB-5ht); Fid detector; Adopt programmed temperature method, since 50 ℃, keep 1min; Be warming up to 180 ℃ with the speed of 15 ℃/min, keep 0min; Be warming up to 230 ℃ with the speed of 10 ℃/min again, constant temperature 0min; Be warming up to 360 ℃ with the speed of 20 ℃/min again, constant temperature 19min.
Embodiment 2: the soybean oil take acid number as 0.8mg KOH/g and methyl alcohol are prepared biofuel as raw material
(1) by soybean oil and methyl alcohol in mass ratio 10:1 mix, then inject the first fixed-bed reactor that are filled with solid base catalyst, be 120 ℃ in temperature, pressure is 4.0MPa, volume space velocity is 5.0h
-1condition under there is transesterify and esterification, 40.8% soybean oil is converted into fatty acid ester biofuel;
(2) glycerin layer in mixture after the reaction that in step 1, the first fixed-bed reactor flow out is separated by stratification method;
(3) mixture after step 2 separation of glycerin being pressed to massfraction and supplemented 10% methyl alcohol, then inject the second fixed-bed reactor that are filled with solid base catalyst, is 120 ℃ in temperature, and pressure is 4.0MPa, and volume space velocity is 0.1h
-1under condition, react, soybean oil is converted into fatty acid ester biofuel completely;
(4) glycerin layer in mixture after the reaction that in step 3, the second fixed-bed reactor flow out is separated by centrifugal method, obtained fatty acid ester biofuel.
Embodiment 3: the rapeseed oil take acid number as 1.0mg KOH/g and ethanol are prepared biofuel as raw material
(1) by rapeseed oil and ethanol in mass ratio 5:1 mix, then inject the first fixed-bed reactor that are filled with solid base catalyst, be 140 ℃ in temperature, pressure is 3.0MPa, volume space velocity is 4.0h
-1condition under there is transesterify and esterification, 61.2% rapeseed oil is converted into fatty acid ester biofuel;
(2) glycerin layer in mixture after the reaction that in step 1, the first fixed-bed reactor flow out is separated by centrifuging;
(3) mixture after step 2 separation of glycerin being pressed to massfraction and supplemented 5% ethanol, then inject the second fixed-bed reactor that are filled with solid base catalyst, is 160 ℃ in temperature, and pressure is 3.0MPa, and volume space velocity is 0.5h
-1under condition, react, rapeseed oil is converted into fatty acid ester biofuel completely;
(4) glycerin layer in mixture after the reaction that in step 3, the second fixed-bed reactor flow out is separated by stratification method, obtained fatty acid ester biofuel.
Embodiment 4: the cottonseed crude oil take acid number as 5mg KOH/g and methyl alcohol are prepared biofuel as stock oil
(1) by cottonseed crude oil and methyl alcohol in mass ratio 4:1 mix, then inject the first fixed-bed reactor that are filled with solid base catalyst, be 160 ℃ in temperature, pressure is 0.1MPa, volume space velocity is 0.1h
-1condition under there is transesterify and esterification, 79.5% cottonseed crude oil is converted into fatty acid ester biofuel;
(2) glycerin layer in mixture after the reaction that in step 1, the first fixed-bed reactor flow out is separated by centrifuging;
(3) mixture after step 2 separation of glycerin being pressed to massfraction and supplemented 0.1% methyl alcohol, then inject the second fixed-bed reactor that are filled with solid base catalyst, is 220 ℃ in temperature, and pressure is 0.1MPa, and volume space velocity is 5.0h
-1under condition, react, cottonseed crude oil is converted into fatty acid ester biofuel completely;
(4) glycerin layer in mixture after the reaction that in step 3, the second fixed-bed reactor flow out is separated by stratification method, obtained fatty acid ester biofuel.
Embodiment 5: the plam oil take acid number as 11.2mgKOH/g and methyl alcohol are prepared biofuel as stock oil
(1) by plam oil and methyl alcohol in mass ratio 3:1 mix, then inject the first fixed-bed reactor that are filled with solid acid catalyst, be 180 ℃ in temperature, pressure is 2.0MPa, volume space velocity is 0.5h
-1condition under there is transesterify and esterification, 71.8% plam oil oil is converted into fatty acid ester biofuel;
(2) glycerin layer in mixture after the reaction that in step 1, the first fixed-bed reactor flow out is separated by centrifuging;
(3) mixture after step 2 separation of glycerin being pressed to massfraction and supplemented 0.5% methyl alcohol, then inject the second fixed-bed reactor that are filled with solid base catalyst, is 200 ℃ in temperature, and pressure is 2.0MPa, and volume space velocity is 3.0h
-1under condition, react, plam oil is converted into fatty acid ester biofuel completely;
(4) glycerin layer in mixture after the reaction that in step 3, the second fixed-bed reactor flow out is separated by centrifuging, obtained fatty acid ester biofuel.
Embodiment 6: the little Chinese parasol tree oil take acid number as 38.2mgKOH/g and methyl alcohol are prepared biofuel as stock oil
(1) by little Chinese parasol tree oil and methyl alcohol in mass ratio 4:1 mix, then injection is filled with the first fixed-bed reactor of solid acid catalyst, is 200 ℃ in temperature, pressure is 2.0MPa, volume space velocity is 2.5h
-1condition under there is transesterify and esterification, 78.8% little Chinese parasol tree oil is converted into fatty acid ester biofuel;
(2) glycerin layer in mixture after the reaction that in step 1, the first fixed-bed reactor flow out is separated by stratification method;
(3) mixture after step 2 separation of glycerin being pressed to massfraction and supplemented 4.0% methyl alcohol, then inject the second fixed-bed reactor that are filled with solid base catalyst, is 180 ℃ in temperature, and pressure is 1.0MPa, and volume space velocity is 3.0h
-1under condition, react, little Chinese parasol tree oil is converted into fatty acid ester biofuel completely;
(4) glycerin layer in mixture after the reaction that in step 3, the second fixed-bed reactor flow out is separated by stratification method, obtained fatty acid ester biofuel.
Embodiment 7: the waste grease take acid number as 45.1mgKOH/g and ethanol are prepared biofuel as stock oil
(1) by waste grease and ethanol in mass ratio 4:1 mix, then inject the first fixed-bed reactor that are filled with solid acid catalyst, be 220 ℃ in temperature, pressure is 1.0MPa, volume space velocity is 3.0h
-1condition under there is transesterify and esterification, 79.5% waste grease is converted into fatty acid ester biofuel;
(2) glycerin layer in mixture after the reaction that in step 1, the first fixed-bed reactor flow out is separated by centrifuging;
(3) mixture after step 2 separation of glycerin being pressed to massfraction and supplemented 4.0% ethanol, then inject the second fixed-bed reactor that are filled with solid base catalyst, is 200 ℃ in temperature, and pressure is 0.1MPa, and volume space velocity is 4.0h
-1under condition, react, waste grease is converted into fatty acid ester biofuel completely;
(4) glycerin layer in mixture after the reaction that in step 3, the second fixed-bed reactor flow out is separated by stratification method, obtain fatty acid ester biofuel.
Claims (10)
1. a method for two sections of fixed bed continuous production of biodiesels, step is as follows:
A) by animal-plant oil and/or waste grease raw material and methyl alcohol and/or ethanol in mass ratio 2:1 ~ 10:1 mix, then inject the first fixed-bed reactor that are filled with solid catalyst, be 120 ~ 220 ℃ in temperature, pressure is 0.1 ~ 4.0MPa, and volume space velocity is 0.1 ~ 5.0h
-1condition under there is transesterify and esterification, animal-plant oil or waste grease quality 40% ~ 80% are converted into fatty acid ester biofuel;
B) glycerin layer in mixture after the reaction that in step a, the first fixed-bed reactor flow out is separated;
C) mixture after step b separation of glycerin layer is pressed to massfraction and supplemented methyl alcohol or the ethanol of 0.1-10%, then inject the second fixed-bed reactor that are filled with solid catalyst, be 120 ~ 220 ℃ in temperature, pressure is 0.1 ~ 4.0MPa, and volume space velocity is 0.1 ~ 5.0h
-1under condition, react, raw oil material is converted into fatty acid ester biofuel completely;
D) glycerin layer in mixture after the reaction that in step c, the second fixed-bed reactor flow out is separated, obtained fatty acid ester biofuel.
2. method according to claim 1, is characterized in that: when the acid number of animal-plant oil or waste grease is less than or equal to 5mg KOH/g, the solid catalyst of two fixed-bed reactor fillings is solid base catalyst; When the acid number of animal-plant oil or waste grease is greater than 5mgKOH/g, the first fixed-bed reactor filling solid acid catalyst, the second fixed-bed reactor filling solid alkaline catalysts.
3. method according to claim 1, is characterized in that: between two fixed-bed reactor reactions, be provided with separating step, the glycerin layer after the reaction that the first fixed-bed reactor are flowed out in mixture is separated;
After the reaction that the first fixed-bed reactor flow out, after mixture separation glycerin layer, supplement the low-carbon alcohol such as methyl alcohol or ethanol of 0.5-5% by massfraction, then inject the second fixed-bed reactor reaction that is filled with solid catalyst.
4. method according to claim 1, is characterized in that: the reactant animal-plant oil or waste grease raw material and methyl alcohol or the ethanol 3:1 ~ 5:1 in mass ratio that inject the first fixed-bed reactor.
5. according to method described in claim 1 or 3, it is characterized in that: after the first fixed-bed reactor reaction, animal-plant oil or waste grease 60% ~ 80% are converted into fatty acid ester biofuel.
6. according to method described in claim 1 or 2, it is characterized in that:
Vegetable and animals oils fat raw material can be one or two or more kinds mixture in soybean oil, plam oil, rapeseed oil, peanut oil, little Chinese parasol tree oil, Oleum Gossypii semen, engineering algae oil, lard;
Waste grease is food and drink abendoned oil or expired animal-plant oil.
7. according to method described in claim 1 or 2, it is characterized in that: the reaction conditions of the first reactor, temperature is 140 ~ 200 ℃, and pressure is 0.1 ~ 3.0MPa, and volume space velocity is 0.5 ~ 5.0h-1; The reaction conditions of the second reactor is 140 ~ 200 ℃, and pressure is 0.1 ~ 3.0MPa, and volume space velocity is 0.5 ~ 5.0h
-1.
8. method according to claim 1, is characterized in that: unreacted low-carbon alcohol can recycle.
9. method according to claim 1, is characterized in that:
Described solid base catalyst is lanthanum gahnite;
Described solid acid catalyst is iron zinc prussiate.
10. method according to claim 1, is characterized in that: the glycerin layer in mixture is the thing that dissolves each other of glycerine and low-carbon alcohol, and it separates with oil reservoir by centrifugal separation or stratification method.
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| CN104560226A (en) * | 2014-11-04 | 2015-04-29 | 华文蔚 | Preparation method of biodiesel |
| CN106221943A (en) * | 2016-09-14 | 2016-12-14 | 上海中器环保科技有限公司 | The production technology of high-quality biological diesel oil |
| CN108927171A (en) * | 2017-05-26 | 2018-12-04 | 中国科学院大连化学物理研究所 | A kind of catalyst of the transesterification prenol processed of prenyl acetate and its application |
| CZ308818B6 (en) * | 2019-12-20 | 2021-06-09 | Zdeněk Ing. Řičica | Method of producing alternative biofuel from waste fat sludge |
| CN114178292A (en) * | 2021-12-10 | 2022-03-15 | 西安建筑科技大学 | System and method for realizing co-production of multiple ester products by taking food waste as raw material |
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Application publication date: 20140521 |