CN102965203A - Method for preparing biodiesel through catalysis of natural biomass solid acid catalyst - Google Patents
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- CN102965203A CN102965203A CN2012104270778A CN201210427077A CN102965203A CN 102965203 A CN102965203 A CN 102965203A CN 2012104270778 A CN2012104270778 A CN 2012104270778A CN 201210427077 A CN201210427077 A CN 201210427077A CN 102965203 A CN102965203 A CN 102965203A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a method for preparing biodiesel through catalysis of a natural biomass solid acid catalyst. The method comprises the following steps: 1, washing, drying and crushing the natural biomass, weighing and impregnating the crushed biomass, and taking out and drying the biomass; 2, impregnating acidified biomass in a metal salt solution, taking out and drying; 3, placing the biomass loaded with metal salt in a muffle furnace for roasting to obtain a natural biomass solid acid catalyst; and 4, adding the prepared biomass solid acid catalyst, short chain alcohol and oil into a batch reactor for esterification and an ester exchange reaction; after the reaction, conducting reduced pressure distillation to remove excessive short chain alcohol; and standing to delaminate glycerol and biodiesel produced in the reaction, wherein the biodiesel product is on an upper layer. According to the invention, natural renewable biomass is used as a raw material for direct acidification, without carbonization, so as to realize low cost and high biological diesel oil yield; besides, the prepared catalyst has advantages of good mechanical strength, particle size conducive to recovery, and no secondary pollution.
Description
Technical field
The present invention relates to biofuel, be specifically related to a kind of method of the solid acid catalyst catalysis for preparing biodiesel oil take natural biomass as raw material.
Background technology
Biofuel is recovered oil.In recent years, along with the day by day exhaustion of petroleum resources and the progressively deterioration of environment, this renewable resources of biofuel comes into one's own day by day.Now be widely accepted gradually the substitute of the petrifaction diesel that becomes high-quality, low-sulfur, low toxicity.At present originally used catalyzer is acid solution catalysis in the process of production biofuel, and such as the vitriol oil, but its product separates with the catalyzer difficulty, and to the seriously corroded of conversion unit, side reaction is many, and environmental pollution is large.Afterwards, introduced the solid acid alkali catalytic agent, and solved the problem that catalyzer and product are difficult to separate, but also had problems simultaneously.The patent CN of Dalian University of Technology 200810012062.9 has proposed a kind of method for preparing carbon-based solid acid and biofuel with natural biomass such as wood chips through carbonization, sulfonation.The patent CN102247888A of Beijing University of Chemical Technology, the patent CN102125874A of South China Science ﹠ Engineering University, the patent CN101396668A of Fujian Normal University and the patent CN102218342A of East China University of Science etc. also proposed to use different biomass, with the carbonization of diverse ways elder generation, sulfonation prepares the method for carbon-based solid acid again.Yet above-mentioned preparation method has slatterned the most of organic matter in the natural biomass, charcoal base material after the carbonization not only volume, weight all significantly reduces, and the relative natural biomass of its physical strength also has significantly reduction, after using, catalyzer forms extremely small carbon powder, industrial being difficult to reclaims, and very easily causes secondary pollution.
Summary of the invention
Purpose of the present invention provides a kind of method of natural biomass solid acid catalyst catalysis for preparing biodiesel oil for the problem that above-mentioned prior art exists, and it does not carry out carbonizing treatment take the biomass of natural reproducible as the direct acidifying of raw material.It is low to reach cost, and the biofuel yield is high, and the catalyzer physical strength of preparation is good, and granular size is beneficial to recovery, does not cause the purpose of secondary pollution.
The technical solution adopted in the present invention is: a kind of method of natural biomass solid acid catalyst catalysis for preparing biodiesel oil may further comprise the steps:
1. natural biomass is washed, dry, pulverize, taking by weighing biomass after the pulverizing, to be immersed in massfraction be 1.5 ~ 5h in 15% ~ 75% the acid solution, takes out rear 80 ℃ ~ 100 ℃ lower oven dry;
2. the biomass after the acidifying are immersed in 1 ~ 5h in the metal salt solution, 80 ~ 100 ℃ of lower oven dry after taking out;
3. the biomass with loading metal-salt place 100 ~ 270 ℃ of lower roasting 2h of retort furnace, naturally cool to room temperature, obtain the natural biomass solid acid catalyst;
4. prepared biomass solid acid catalyst, short chain alcohol and grease are dropped in the batch reactor, heating under 60 ~ 120 ℃, stirring, carry out esterification and transesterification reaction, reaction times is 2 ~ 10h, the unnecessary short chain alcohol of pressure reducing and steaming after reaction finishes, leave standstill glycerine and delamination of biodiesel that reaction is produced, the upper strata is the biofuel product; The consumption of described biomass solid acid catalyst accounts for 3 ~ 7% of grease gross weight, and the mol ratio of described short chain alcohol and grease is 3 ~ 12:1.
Step of the present invention batch reactor 4. also can be fixed-bed reactor, this moment continuous the flowing through of the mixed solution of short chain alcohol and grease is filled with the fixed bed of biomass solid acid catalyst, carry out esterification and transesterification reaction 4 ~ 6h under 60 ℃ ~ 120 ℃, the reaction solution that flows out is carried out underpressure distillation, remove short chain alcohol and water, leave standstill or centrifugation glycerine after, obtain biofuel.The mol ratio of described short chain alcohol and grease is 3 ~ 12:1, and the consumption of described biomass solid acid catalyst accounts for 10% ~ 15% of fixed bed volume.
Described natural biomass is at least a in wood chip, bamboo bits, cotton and cotton products, xylogen, Mierocrystalline cellulose, shell, rice husk, crop stem, the bagasse.
Step 1. described acid solution comprise the inorganic or organic acid such as sulfuric acid, phosphoric acid, nitric acid, perchloric acid and Phenylsulfonic acid any one.
Step 2. described metal salt solution for containing K
+, Na
+, Mg
2+, Cu
2+(or Cu
+), Zn
2+, Ti
2+(or Ti
4+) and Fe
2+(or Fe
3+) in the salts solution of any one metal ion, concentration is 0.01 ~ 0.1mol/L.
Step 4. described short chain alcohol is a kind of in methyl alcohol, ethanol, propyl alcohol and the Virahol.
The step 4. mol ratio of described short chain alcohol and grease is 3-5:1.
The method of described a kind of natural biomass solid acid catalyst catalysis for preparing biodiesel oil may further comprise the steps:
1. will clean, to be immersed in massfraction be 3h in 45% the perchloric acid solution to the crop stem particle 10kg after the drying and crushing, takes out rear 90 ℃ of lower oven dry;
2. the crop stem after the acidifying is immersed in 4h in the copper-bath of 0.05mol/L, takes out rear 70 ℃ of lower oven dry;
3. the crop stem with load copper sulfate places 135 ℃ of lower calcination activation 2h of retort furnace, naturally cools to room temperature, obtains the crop stem solid acid catalyst;
4. drop in the batch reactor with prepared crop stem solid acid catalyst 5kg, ethanol 26kg and through the sewer oil 100kg that predrainage, removing impurities are processed, be heated with stirring to 90 ℃, carry out esterification and transesterification reaction, reaction times 6h, the unnecessary ethanol of pressure reducing and steaming after reaction finishes, standing separation is removed crop stem solid acid catalyst and glycerine, and the upper strata is the biofuel product.
Grease of the present invention can be crude vegetal, animal grease, sewer oil and all kinds of acidification oil, natural animal-plant lipid acid.To dewater in advance when preparing biofuel take sewer oil as raw material, removing impurities processes.
Biomass solid acid catalyst of the present invention is take the biomass of natural reproducible as raw material, and environmental protection is cheap.The preparation of catalyzer is directly carried out acidifying to raw material, does not carry out carbonizing treatment, and the catalyzer physical strength that makes is high, and granular size is suitable, is beneficial to recovery, can not cause secondary pollution; Repeatedly flood, to reach preferably charge capacity.
The biomass of the present invention after to acidifying are carried out again the dip loading of metal-salt, have further improved the catalytic activity of catalyzer.Reacted solid acid catalyst is convenient to separate with product.
The method of biomass solid acid catalyst catalysis for preparing biodiesel oil of the present invention is applicable to grease take various acid numbers as the up-to-standard biofuel of raw material production.The biofuel product of producing meets the quality standard of national 0# diesel oil fully.
Embodiment
The method of a kind of natural biomass solid acid catalyst catalysis for preparing biodiesel oil of the present invention may further comprise the steps:
1. natural biomass is washed, dry, pulverize, taking by weighing biomass after the pulverizing, to be immersed in massfraction be 1.5 ~ 5h in 15% ~ 75% the acid solution, takes out rear 80 ℃ ~ 100 ℃ lower oven dry,
2. the biomass after the acidifying are immersed in 1 ~ 5h in the metal salt solution, 80 ~ 100 ℃ of lower oven dry after taking out,
3. the biomass with loading metal-salt place 100 ~ 270 ℃ of lower roasting 2h of retort furnace, naturally cool to room temperature, obtain the natural biomass solid acid catalyst,
4. prepared biomass solid acid catalyst, short chain alcohol and grease are dropped in the batch reactor, heating under 60 ~ 120 ℃, stirring, carry out esterification and transesterification reaction, reaction times is 2 ~ 10h, the unnecessary short chain alcohol of pressure reducing and steaming after reaction finishes leaves standstill glycerine and delamination of biodiesel that reaction is produced, and the upper strata is the biofuel product, the consumption of described biomass solid acid catalyst accounts for 3 ~ 7% of grease gross weight, and the mol ratio of described short chain alcohol and grease is 3 ~ 12:1.
Step of the present invention batch reactor 4. also can be fixed-bed reactor, this moment continuous the flowing through of the mixed solution of short chain alcohol and grease is filled with the fixed bed of biomass solid acid catalyst, carry out esterification and transesterification reaction 4 ~ 6h under 60 ℃ ~ 120 ℃, the reaction solution that flows out is carried out underpressure distillation, remove short chain alcohol and water, leave standstill or centrifugation glycerine after, obtain biofuel.The mol ratio of described short chain alcohol and grease is 3 ~ 12:1, and the amount of described biomass solid acid catalyst accounts for 10% ~ 15% of fixed bed volume.
Described natural biomass is at least a in wood chip, bamboo bits, cotton and cotton products, xylogen, Mierocrystalline cellulose, shell, rice husk, crop stem, the bagasse.
Step 1. described acid solution comprise the inorganic or organic acid such as sulfuric acid, phosphoric acid, nitric acid, perchloric acid and Phenylsulfonic acid any one, massfraction is 15 ~ 75%.
Step 2. described metal salt solution for containing K
+, Na
+, Mg
2+, Cu
2+(or Cu
+), Zn
2+, Ti
2+(or Ti
4+) and Fe
2+(or Fe
3+) in the salts solution of any one metal ion, concentration is 0.01 ~ 0.1mol/L.
Step 4. described short chain alcohol is a kind of in methyl alcohol, ethanol, propyl alcohol and the Virahol.
The preferred steps 4. mol ratio of described short chain alcohol and grease is that 3-5:1 is best.
Grease of the present invention can be crude vegetal, animal grease, sewer oil and all kinds of acidification oil, natural animal-plant lipid acid.To dewater in advance when preparing biofuel take sewer oil as raw material, removing impurities processes.
Embodiment: a kind of method of natural biomass solid acid catalyst catalysis for preparing biodiesel oil can have following a plurality of embodiment:
1, concrete steps are:
1. will clean, to be immersed in massfraction be 1.5h in 15% the sulphuric acid soln to the wood pellet 10kg after the drying and crushing, takes out rear 80 ℃ of lower oven dry;
2. the wood chip after the acidifying is immersed in 1h in the Klorvess Liquid of 0.01mol/L, takes out rear 80 ℃ of lower oven dry;
3. the wood chip with load Repone K places 100 ℃ of lower calcination activation 2h of retort furnace, naturally cools to room temperature, obtains the natural wood chip solid acid catalyst;
4. drop in the batch reactor with prepared solid acid catalyst 3kg, methyl alcohol 11kg and through the sewer oil 100kg that predrainage, removing impurities are processed, be heated with stirring to 60 ℃, carry out esterification and transesterification reaction, reaction times 2h, the unnecessary methyl alcohol of pressure reducing and steaming after reaction finishes, standing separation is removed catalyzer and glycerine, and the upper strata is the biofuel product.Product yield 71%.
2, concrete steps are:
1. will clean, jointly to be immersed in massfraction be 5h in 75% the phosphoric acid solution for xylogen particle 6kg, cellulose grain 4kg after the drying and crushing, takes out rear 100 ℃ of lower oven dry;
2. the 5h in the metabisulfite solution of 0.1mol/L with the xylogen after the acidifying and cellulosic impregnation mixture takes out rear 80 ℃ of lower oven dry;
3. xylogen and the cellulosic mixture with load sodium sulfate places 270 ℃ of lower calcination activation 2h of retort furnace, naturally cools to room temperature, obtains the biomass solid acid catalyst;
4. prepared solid acid catalyst 3kg, ethanol 62kg and crude vegetal 100kg are dropped in the batch reactor, be heated with stirring to 120 ℃, carry out esterification and transesterification reaction, reaction times 10h, the unnecessary ethanol of pressure reducing and steaming after reaction finishes, standing separation is removed catalyzer and glycerine, and the upper strata is the biofuel product.Product yield 73%.
3, concrete steps are:
1. will clean, to be immersed in massfraction be 1.5h in 15% the Phenylsulfonic acid solution to the shell particle 10kg after the drying and crushing, takes out rear 80 ℃ of lower oven dry;
2. the shell after the acidifying is immersed in 1h in the solution of ferrous chloride of 0.01mol/L, takes out rear 80 ℃ of lower oven dry;
3. the shell with the load iron protochloride places 100 ℃ of lower calcination activation 2h of retort furnace, naturally cools to room temperature, obtains natural shell solid acid catalyst;
4. continuous the flowing through of mixed solution of propyl alcohol 20kg and animal grease 100kg is filled with the fixed bed of biomass solid acid catalyst, the consumption of solid acid catalyst accounts for 10% of fixed bed volume, carry out esterification and transesterification reaction 4h under 60 ℃, the unnecessary propyl alcohol of reaction solution pressure reducing and steaming to flowing out after reaction finishes, standing separation is removed catalyzer and glycerine, and the upper strata is the biofuel product.Product yield 75%.
4, concrete steps are:
1. will clean, to be immersed in massfraction be 5h in 75% the salpeter solution to the bagasse particle 10kg after the drying and crushing, takes out rear 100 ℃ of lower oven dry;
2. the bagasse after the acidifying is immersed in 5h in the solution of zinc sulfate of 0.1mol/L, takes out rear 80 ℃ of lower oven dry;
3. the bagasse with load zinc sulfate places 270 ℃ of lower calcination activation 2h of retort furnace, naturally cools to room temperature, obtains natural bagasse solid acid catalyst;
4. continuous the flowing through of mixed solution of the sewer oil 100kg that processes with Virahol 81kg with through predrainage, removing impurities is filled with the fixed bed of biomass solid acid catalyst, the consumption of biomass solid acid catalyst accounts for 15% of fixed bed volume, carry out esterification and transesterification reaction 6h under 120 ℃, the unnecessary Virahol of reaction solution pressure reducing and steaming to flowing out after reaction finishes, standing separation is removed catalyzer and glycerine, and the upper strata is the biofuel product.Product yield 72%.
5, concrete steps are:
1. will clean, to be immersed in massfraction be 3h in 45% the perchloric acid solution to the crop stem particle 10kg after the drying and crushing, takes out rear 90 ℃ of lower oven dry;
2. the crop stem after the acidifying is immersed in 4h in the copper-bath of 0.05mol/L, takes out rear 70 ℃ of lower oven dry; 3. the crop stem with load copper sulfate places 135 ℃ of lower calcination activation 2h of retort furnace, naturally cools to room temperature, obtains the crop stem solid acid catalyst;
4. drop in the batch reactor with prepared solid acid catalyst 5kg, ethanol 26kg and through the sewer oil 100kg that predrainage, removing impurities are processed, be heated with stirring to 90 ℃, carry out esterification and transesterification reaction, reaction times 6h, the unnecessary ethanol of pressure reducing and steaming after reaction finishes, standing separation is removed catalyzer and glycerine, and the upper strata is the biofuel product.Product yield 83%.
6, concrete steps are:
1. will clean, to be immersed in massfraction be 3h in 30% the salpeter solution for the rice husk particle 2kg after the drying and crushing and bamboo bits particle 8kg, takes out rear 100 ℃ of lower oven dry;
2. the 5h in the liquor zinci chloridi of 0.06mol/L with the rice husk after the acidifying and bamboo bits impregnation mixture takes out rear 80 ℃ of lower oven dry;
3. rice husk and the bamboo bits mixture with the load zinc chloride places 200 ℃ of lower calcination activation 2h of retort furnace, naturally cools to room temperature, obtains the natural biomass solid acid catalyst;
4. continuous the flowing through of mixed solution of propyl alcohol 54kg and tallow fatty acid 100kg is filled with the fixed bed of biomass solid acid catalyst, the consumption of biomass solid acid catalyst accounts for 12% of fixed bed volume, carry out esterification and transesterification reaction 5h under 80 ℃, the unnecessary propyl alcohol of reaction solution pressure reducing and steaming to flowing out after reaction finishes, catalyzer and glycerine are removed in centrifugation, and the upper strata is the biofuel product.Product yield 78%.
7, concrete steps are:
1. will clean, to be immersed in massfraction be 3h in 45% the perchloric acid solution to the crop stem particle 10kg after the drying and crushing, takes out rear 90 ℃ of lower oven dry;
2. the crop stem after the acidifying is immersed in 4h in the copper-bath of 0.05mol/L, takes out rear 70 ℃ of lower oven dry;
3. the crop stem with load copper sulfate places 135 ℃ of lower calcination activation 2h of retort furnace, naturally cools to room temperature, obtains the crop stem solid acid catalyst;
4. prepared biomass solid acid catalyst 5kg, methyl alcohol 14kg and acidification oil 100kg are dropped in the batch reactor, be heated with stirring to 90 ℃, carry out esterification and transesterification reaction, reaction times 6h, the unnecessary methyl alcohol of pressure reducing and steaming after reaction finishes, standing separation is removed catalyzer and glycerine, and the upper strata is the biofuel product.Product yield 79%.
Acidization of the present invention also can be carried out suitable heated and stirred, and its temperature control is conducive to the load of catalyst activity component at 30 ~ 150 ℃.
Claims (9)
1. the method for a natural biomass solid acid catalyst catalysis for preparing biodiesel oil is characterized in that: may further comprise the steps:
1. natural biomass is washed, dry, pulverize, taking by weighing biomass after the pulverizing, to be immersed in massfraction be 1.5 ~ 5h in 15 ~ 75% the acid solution, takes out rear 80 ℃ ~ 100 ℃ lower oven dry;
2. the biomass after the acidifying are immersed in 1 ~ 5h in the metal salt solution, 80 ~ 100 ℃ of lower oven dry after taking out;
3. the biomass with loading metal-salt place 100 ~ 270 ℃ of lower roasting 2h of retort furnace, naturally cool to room temperature, obtain the natural biomass solid acid catalyst;
4. prepared biomass solid acid catalyst, short chain alcohol and grease are dropped in the batch reactor, heating under 60 ~ 120 ℃, stirring, carry out esterification and transesterification reaction, reaction times is 2 ~ 10h, the unnecessary short chain alcohol of pressure reducing and steaming after reaction finishes, leave standstill glycerine and delamination of biodiesel that reaction is produced, the upper strata is the biofuel product; The consumption of described biomass solid acid catalyst accounts for 3 ~ 7% of grease gross weight, and the mol ratio of described short chain alcohol and grease is 3 ~ 12:1.
2. the method for a kind of natural biomass solid acid catalyst catalysis for preparing biodiesel oil as claimed in claim 1, it is characterized in that: step 4. described batch reactor can be fixed-bed reactor, at this moment continuous the flowing through of the mixed solution of short chain alcohol and grease is filled with the fixed bed of biomass solid acid catalyst, carry out esterification and transesterification reaction 4 ~ 6h under 60 ℃ ~ 120 ℃, the reaction solution that flows out is carried out underpressure distillation, remove short chain alcohol and water, leave standstill or centrifugation glycerine after, obtain biofuel; The mol ratio of described short chain alcohol and grease is 3 ~ 12:1, and the consumption of described biomass solid acid catalyst accounts for 10% ~ 15% of fixed bed volume.
3. the method for a kind of natural biomass solid acid catalyst catalysis for preparing biodiesel oil as claimed in claim 1 is characterized in that: described natural biomass is at least a in wood chip, bamboo bits, cotton and cotton products, xylogen, Mierocrystalline cellulose, shell, rice husk, crop stem, the bagasse.
4. the method for a kind of natural biomass solid acid catalyst catalysis for preparing biodiesel oil as claimed in claim 1 is characterized in that: step 1. described acid solution comprise the inorganic or organic acid such as sulfuric acid, phosphoric acid, nitric acid, perchloric acid and Phenylsulfonic acid any one.
5. the method for a kind of natural biomass solid acid catalyst catalysis for preparing biodiesel oil as claimed in claim 1 is characterized in that: step 2. described metal salt solution for containing K
+, Na
+, Mg
2+, Cu
2+(or Cu
+), Zn
2+, Ti
2+(or Ti
4+) and Fe
2+(or Fe
3+) in the salts solution of any one metal ion.
6. the method for a kind of natural biomass solid acid catalyst catalysis for preparing biodiesel oil as claimed in claim 1, it is characterized in that: step 2. described metal salt solution concentration is 0.01 ~ 0.1mol/L.
7. the method for a kind of natural biomass solid acid catalyst catalysis for preparing biodiesel oil as claimed in claim 1 is characterized in that: step 4. described short chain alcohol is a kind of in methyl alcohol, ethanol, propyl alcohol and the Virahol.
8. such as the method for claim 1,2 described a kind of natural biomass solid acid catalyst catalysis for preparing biodiesel oil, it is characterized in that: the step 4. mol ratio of described short chain alcohol and grease is 3-5:1.
9. the method for a kind of natural biomass solid acid catalyst catalysis for preparing biodiesel oil as claimed in claim 1 is characterized in that: may further comprise the steps:
1. will clean, to be immersed in massfraction be 3h in 45% the perchloric acid solution to the crop stem particle 10kg after the drying and crushing, takes out rear 90 ℃ of lower oven dry;
2. the crop stem after the acidifying is immersed in 4h in the copper-bath of 0.05mol/L, takes out rear 70 ℃ of lower oven dry;
3. the crop stem with load copper sulfate places 135 ℃ of lower calcination activation 2h of retort furnace, naturally cools to room temperature, obtains the crop stem solid acid catalyst;
4. drop in the batch reactor with prepared crop stem solid acid catalyst 5kg, ethanol 26kg and through the sewer oil 100kg that predrainage, removing impurities are processed, be heated with stirring to 90 ℃, carry out esterification and transesterification reaction, reaction times 6h, the unnecessary ethanol of pressure reducing and steaming after reaction finishes, standing separation is removed crop stem solid acid catalyst and glycerine, and the upper strata is the biofuel product.
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| CN103468414A (en) * | 2013-09-29 | 2013-12-25 | 天津理工大学 | Method for preparing biodiesel by using composite solid acid catalyst |
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| CN109692690A (en) * | 2018-12-24 | 2019-04-30 | 华中科技大学 | It is a kind of for producing the catalyst and preparation method of levoglucosenone |
| US11414623B2 (en) * | 2019-05-29 | 2022-08-16 | King Fahd University Of Petroleum And Minerals | Efficient biomass carbon-based solid acid esterification catalyst for producing biodiesel |
| CN113019465A (en) * | 2021-03-24 | 2021-06-25 | 湖北碧美新能源科技有限公司 | Solid acid catalyst of biodiesel and method for preparing biodiesel |
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