CN102766020A - Method for producing ethanol, acetone and butanol by permeabilization, vaporization, coupling and rectification of ABE (Acetone, Butanol and Ethanol) fermentation liquor - Google Patents
Method for producing ethanol, acetone and butanol by permeabilization, vaporization, coupling and rectification of ABE (Acetone, Butanol and Ethanol) fermentation liquor Download PDFInfo
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- CN102766020A CN102766020A CN201210225327XA CN201210225327A CN102766020A CN 102766020 A CN102766020 A CN 102766020A CN 201210225327X A CN201210225327X A CN 201210225327XA CN 201210225327 A CN201210225327 A CN 201210225327A CN 102766020 A CN102766020 A CN 102766020A
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Abstract
The invention provides a method for producing bulk biologic chemicals: ethanol, acetone and butanol by permeabilization, vaporization, coupling and rectification of an ABE (Acetone, Butanol and Ethanol) fermentation liquor. The method comprises the steps of: step A, separating and condensing the ABE fermentation liquor containing ethanol, acetone, butanol and butyric acid through a permeabilization and vaporization film, and obtaining a gas mixture containing ethanol, acetone, butanol, butyric acid and water on the permeable side; and step B, enabling the gas mixture to enter a rectification device directly to be subjected to rectification and separation without condensation so as to obtain ethanol, acetone and butanol products. According to the method provided by the invention, the ABE mixture on the permeable side after permeabilization and vaporization is enabled to enter the rectifying tower directly in form of gas, therefore, the energy consumption of product in the production process is greatly reduced, and the production efficiency is improved.
Description
Technical field
The invention belongs to infiltration evaporation coupling rectification separating and purifying technology field, be specifically related to a kind of ABE fermented liquid is produced ethanol, acetone and butanols through the infiltration evaporation coupling rectification method.
Background technology
Butanols, acetone and ethanol are important Organic Chemicals.Butanols is mainly used in the production of propenoate, methacrylic ester and n-butyl phthalate, also can be used as the solvent of resin, paint and tackiness agent simultaneously, and skimmer is used in the extraction agent and the ore dressing of grease, spices and pharmaceutical industry.In addition, research shows that butanols still is a kind of liquid biofuel efficiently, and its character is very near hydro carbons, and is good with the compatibleness of gasoline, has high energy density and fuel value, and lower vp and corrodibility are easy to carry.Acetone is widely used in plastics, coating and pharmaceutical industries, is the main raw material of producing dihydroxyphenyl propane, methyl methacrylate.Ethanol has good dissolving ability, can be used as the production of medical disinfectant, automobile fuel and multiple industrial chemicals.
Acetone butanol fermentation is meant that mikrobe (normally clostridium acetobutylicum or Bai Shi clostridium and mutant strain thereof) under anaerobic utilizes the process of biomass material fermentation production of acetone (Acetone), butanols (Butanol) and the ethanol (Ethanol) of starch, glucide and rich cellulose and semicellulose, is called for short the ABE fermentation.
Compare with chemical synthesis, the Production by Microorganism Fermentation butanols is still lacked competitiveness relatively, and its major cause is that production cost is too high.Cause the too high reason of fermentative Production cost to mainly contain following several respects: one, raw materials cost is high; Two, the principal product butanols has toxicity, forms product and suppresses; Three, production concentration is low, and the separation and Extraction energy consumption is big.
In ABE industrial fermentation process, generally comprise and produce acid (acetate and butyric acid) and product two stages of solvent (ethanol, acetone and butanols); When butanol concentration reached 14.5g/L, the generation of solvent will stop, and had a strong impact on conversion of raw material and usage ratio of equipment; Simultaneously, lower solvent strength makes the later separation extraction process become the maximum process of energy consumption in the butylic fermentation production process, therefore, how to seek effective means and reduces the product inhibition, reduces the sepn process cost and becomes the focus in the butylic fermentation research.Wherein the ABE fermented liquid separates through infiltration evaporation that to concentrate be one of technology of paying close attention to the most of vast researcher.Like patent CN102304106 a kind of method that the semicellulose biomass ferment is produced butanols, acetone, butyric acid and furfural that is rich in has been described.This technology is compared with traditional butylic fermentation production technique, greatly reduces the energy consumption of raw materials cost and separated from solvent leaching process, thereby has reached the purpose that reduces the industrial production cost.But the component that infiltration evaporation sees through side in this patent needs make with extra care through getting into rectifying tower again after the condensation earlier, and it is still higher that wherein infiltration evaporation sees through the heat-processed energy consumption of feed liquid in condensation and the rectifying tower of side feed liquid.
Summary of the invention
The present invention provides a kind of ABE fermented liquid infiltration evaporation coupling rectification to produce the method for ethanol, acetone and butanols; Comprise: steps A; Contain ethanol, acetone, butanols and butyro-ABE fermented liquid and separate concentratedly through infiltrating and vaporizing membrane, see through the gaseous mixture that side obtains containing ethanol, acetone, butanols, butyric acid and water; With step B, said gaseous mixture directly gets into rectifier unit and carries out rectifying separation without condensation, obtain ethanol, acetone and butanols product.
In embodiments of the invention, rectifier unit described in the preferred steps B comprises first rectifying tower, second rectifying tower and the 3rd rectifying tower.Wherein, In a concrete embodiment, after the rectifying separation, cat head obtains acetone and the alcoholic acid mixture gets into second rectifying tower in first rectifying tower for said gaseous mixture; Tower middle part side line recovered water obtains butanols at the bottom of the tower and butyro-mixture gets into the 3rd rectifying tower; At the bottom of the cat head of second rectifying tower and tower, obtain acetone and ethanol respectively; At the bottom of the cat head of the 3rd rectifying tower and tower, obtain butanols and butyric acid respectively.And in another concrete embodiment, after the rectifying separation, cat head obtains acetone to said gaseous mixture and the alcoholic acid mixture gets into second rectifying tower in first rectifying tower, obtains water, butanols and butyro-mixture at the bottom of the tower and gets into the 3rd rectifying tower; At the bottom of the cat head of second rectifying tower and tower, obtain acetone and ethanol respectively; At the bottom of the cat head of the 3rd rectifying tower and tower, obtain water and butyric acid respectively, tower middle part side line extraction butanols.
In the present invention, infiltration evaporation feed liquid side feed temperature is between 30 ~ 75 ℃ among the preferred steps A, and seeing through wall pressure is 50 ~ 650Pa.More preferably, infiltration evaporation feed liquid side feed temperature is between 55 ~ 60 ℃, and seeing through wall pressure is 100 ~ 550Pa.
In the present invention, the infiltration evaporation technology is under the promotion of vapor partial pressure difference, and is interactional different according to solvent and mould material, optionally reaches through the purpose component and separates spissated purpose, has the characteristics energy-conservation, efficient, that selectivity is high.Infiltrating and vaporizing membrane in the aforesaid method can be any one infiltrating and vaporizing membrane that can play materials such as concentrating butanols and acetone; As with octamethylcyclotetrasiloxane, tetramethyl-tetrem thiazolinyl cyclotetrasiloxane, YSR 3286, gather trimethyl silicane propine, Vestolen PP 7052, PS, pvdf, tetrafluoroethylene and Mierocrystalline cellulose, and the infiltrating and vaporizing membrane of one or more making in said material material modified.Wherein, more preferably, infiltrating and vaporizing membrane described in the steps A is for being the Zylox/polyvinylidene fluoride permeable vaporizing composite package of solvent preparation with water, and wherein Zylox is above-mentioned YSR 3286.
Description of drawings
Fig. 1 is the schematic flow sheet of the embodiment of the invention 1, and wherein each Reference numeral is explained as follows: 1-fermentor tank, 2-micro-filtration, 3-feed pump, 4-infiltration evaporation storage tank; The 5-feed pump, 6-infiltration evaporation membrane separation apparatus, 7-first rectifying tower, 8-feed pump, 9-second rectifying tower; The 10-feed pump, 11-the 3rd rectifying tower, 12-acetone storage tank, 13-ethanol storage tank; 14-butanols storage tank, 15-butyric acid storage tank, 16-surge tank, 17-vacuum pump.
Embodiment
Embodiment 1
With the Semen Maydis powder is that fermentation substrate carries out the ABE fermentation, the infiltration evaporation coupling rectification is produced acetone, butanols and ethanol; It is specific as follows to describe production stage in conjunction with accompanying drawing 1.
Fermentation: this step is carried out in fermentor tank as shown in Figure 11; Be that Clostridium acetobutylicumABE1101 bacterial strain is that carbon source is carried out anaerobically fermenting and obtained containing acetone, butanols and alcoholic acid fermented liquid with the Semen Maydis powder.Wherein this fermentation step comprises two steps of culture medium preparation and inoculation again.Culture medium preparation: with the Semen Maydis powder is fermentation substrate preparing natural substratum, and Semen Maydis powder is 60g/L in the substratum; The natural medium of preparation is transferred to high-temperature sterilization in the fermentor tank, treats that feeding aseptic nitrogen after temperature is reduced to 40 ℃ in the fermentor tank makes up oxygen-free environment.Inoculation: under aseptic technique, in above-mentioned substratum, insert activatory bacterial classification; Inoculum size is 1:10 (volume of the volume of bacteria culture fluid/substrate cultivation base); Under 37 ℃ of constant temperatures, ferment, timing sampling is analyzed the variation and the product solvent variation of substrate in the fermented liquid in the fermenting process.
Employed during the fermentation microbial strains can be aforesaid clostridium acetobutylicum, also can be Bai Shi clostridium and mutant strain thereof, can also be the product butanols bacterial strain that obtains through other approach screenings.The fermentation substrate of fermenting process can be the biomass of glucide such as glucose, wood sugar, molasses or cassava, wheat, corn or other rich in starch, also can be that sweet sorghum stalk, sweet corn stem stalk, corn cob, bagasse, apple residue, jerusalem artichoke or other are rich in juice after the squeezings such as semicellulose and cellulosic biomass or the liquid glucose that obtains through methods such as acidolysis, enzymolysis.Fermentation mode in the aforesaid method can be a batch fermentation, and fed-batch fermentation also can be to continuously ferment.
The micro-filtration degerming: this step is carried out in micro-filtration as shown in Figure 12; In a last step,, detect that the butanols massfraction reaches 0.82% in the fermented liquid through after the 40h fermentation; At this moment; Open the fermentor tank bleeder valve; The fermented liquid of multiple compositions such as mycetome, carbohydrate and solvent goes out fermentor tank entering micro-filtration with the velocity flow of 70L/h in the fermentor tank; Return fermentor tank after thalline is concentrated in micro-filtration 2, the fermented liquid of removing behind thalline and other solid substances gets into infiltration evaporation storage tank 4.The microfiltration membrane of in micro-filtration 2, using can be that any one can play and filters microfiltration membrane of removing thalline, like the microfiltration membrane with one or more making in the inorganic materials such as organic materials such as Mierocrystalline cellulose, Vilaterm, Vestolen PP 7052, PS, tetrafluoroethylene, pvdf, polyacrylonitrile, polyester, polysulfones or zirconium white, titanium oxide, aluminum oxide, silicon-dioxide.
Infiltration evaporation separates concentrated: this step is carried out in infiltration evaporation membrane separation apparatus 6 as shown in Figure 1; Acetone in the fermented liquid, butanols and ethanol equal solvent are through being concentrated behind the infiltrating and vaporizing membrane; Feed temperature maintains 60 ℃ in the infiltration evaporation storage tank; The system vacuum degree maintains about 450Pa; The infiltrating and vaporizing membrane that uses in the infiltration evaporation membrane separation apparatus after feed liquid gets into the infiltration evaporation membrane separation apparatus, returns infiltration evaporation storage tank 4 through the feed liquid of film for the Zylox/polyvinylidene fluoride permeable vaporizing composite package of water as the solvent preparation; See through the gas that side obtains containing acetone, butanols, ethanol, butyric acid and water, wherein be rich in acetone, butanols and ethanol.
Rectifying: this step is carried out in rectifying tower as shown in Figure 17,9 and 11; Infiltration evaporation directly gets into first rectifying tower 7 through be rich in acetone, butanols and the alcoholic acid gas that side obtains without condensation; Cat head is provided with condensing surface; Overhead condensation is taked the mode of total reflux during beginning, the mode of taking partial condensation to reflux behind the 0.5h, and the liquid of trim the top of column crosses with the gaseous mixture that sees through the rising of side from infiltration evaporation; Constantly carry out the mass-and heat-transfer effect, thereby accomplish the fine separation process; First rectifying tower, 7 tower top temperatures are 23 ℃, and reflux ratio is 3:1, and cut is the mixture of ethanol and acetone, and it is refining that overhead fraction gets into second rectifying tower 9; Second rectifying tower is also taked the refining mode of partial reflux, and reflux ratio is 2:1, and tower top temperature is 15 ℃, and tower still temperature is 45 ℃, cat head extraction acetone, and purity is 98.2%, tower still extraction ethanol, purity is 95.5%; The side line recovered water (not shown in figure 1) at the tower middle part of first rectifying tower 7; The tower still temperature of first rectifying tower 7 is 58 ℃, and component is butanols and butyro-mixture at the bottom of the tower, and it is refining that it gets into the 3rd rectifying tower 11; The 3rd rectifying tower is also taked the partial reflux mode, and its reflux ratio is 3:2, and tower top temperature is 25 ℃, and tower still temperature is 95 ℃, cat head extraction butanols, and its purity is 99.5%, and the tower still obtains butyric acid, and butyric acid is as the by product among the present invention, and its output is very little.
The equal National standard of the acetone that obtains among the present invention, butanols and alcohol concn; The present invention is that industrial production ethanol, acetone and butanols provide a good method.
The inventive method is compared with the method that existing ABE fermented liquid infiltration evaporation coupling rectification is produced ethanol, acetone and butanols, and not only energy consumption reduces by 30%, and facility investment reduces about 10%.
Embodiment 2
The mode of the rectifying part of this embodiment is different with embodiment 1, and this embodiment is not illustrated by drawings.Infiltration evaporation sees through the gaseous mixture that contains acetone, butanols, ethanol, butyric acid and water that side obtains in first rectifying tower after the rectifying separation; Cat head obtains acetone and the alcoholic acid mixture gets into second rectifying tower, obtains water, butanols and butyro-mixture at the bottom of the tower and gets into the 3rd rectifying tower; At the bottom of the cat head of second rectifying tower and tower, obtain acetone and ethanol respectively; At the bottom of the cat head of the 3rd rectifying tower and tower, obtain water and butyric acid respectively, tower middle part side line extraction butanols.
Claims (8)
1. an ABE fermented liquid infiltration evaporation coupling rectification is produced the method for ethanol, acetone and butanols; Comprise: steps A; Contain ethanol, acetone, butanols and butyro-ABE fermented liquid and separate concentratedly through infiltrating and vaporizing membrane, see through the gaseous mixture that side obtains containing ethanol, acetone, butanols, butyric acid and water; With step B, said gaseous mixture directly gets into rectifier unit and carries out rectifying separation without condensation, obtain ethanol, acetone and butanols product.
2. according to the said method of claim 1, it is characterized in that rectifier unit described in the step B comprises first rectifying tower, second rectifying tower and the 3rd rectifying tower.
3. according to the said method of claim 2; It is characterized in that after the rectifying separation, cat head obtains acetone and the alcoholic acid mixture gets into second rectifying tower in first rectifying tower for said gaseous mixture; Tower middle part side line recovered water obtains butanols at the bottom of the tower and butyro-mixture gets into the 3rd rectifying tower; At the bottom of the cat head of second rectifying tower and tower, obtain acetone and ethanol respectively; At the bottom of the cat head of the 3rd rectifying tower and tower, obtain butanols and butyric acid respectively.
4. according to the said method of claim 2; It is characterized in that; After the rectifying separation, cat head obtains acetone and the alcoholic acid mixture gets into second rectifying tower in first rectifying tower for said gaseous mixture, obtains water, butanols and butyro-mixture at the bottom of the tower and gets into the 3rd rectifying tower; At the bottom of the cat head of second rectifying tower and tower, obtain acetone and ethanol respectively; At the bottom of the cat head of the 3rd rectifying tower and tower, obtain water and butyric acid respectively, tower middle part side line extraction butanols.
5. according to any said method in the claim 1 ~ 4, it is characterized in that infiltration evaporation feed liquid side feed temperature is between 30 ~ 75 ℃ in the steps A, seeing through wall pressure is 50 ~ 650Pa.
6. according to the said method of claim 5, it is characterized in that infiltration evaporation feed liquid side feed temperature is between 55 ~ 60 ℃ in the steps A, seeing through wall pressure is 100 ~ 550Pa.
7. according to any said method in the claim 1 ~ 4; It is characterized in that; Infiltrating and vaporizing membrane described in the steps A for octamethylcyclotetrasiloxane, tetramethyl-tetrem thiazolinyl cyclotetrasiloxane, YSR 3286, gather trimethyl silicane propine, Vestolen PP 7052, PS, pvdf, tetrafluoroethylene and Mierocrystalline cellulose, and the infiltrating and vaporizing membrane of one or more making in said material material modified.
8. according to the said method of claim 7, it is characterized in that infiltrating and vaporizing membrane described in the steps A is for water being the Zylox/polyvinylidene fluoride permeable vaporizing composite package of solvent preparation.
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| CN103772144A (en) * | 2014-01-27 | 2014-05-07 | 南京工业大学 | Method for separating acetone-butanol-alcohol fermenting liquid by utilizing pervaporation-rectification coupling |
| CN103910605A (en) * | 2013-12-27 | 2014-07-09 | 江苏九天高科技股份有限公司 | Pervaporation system and technology for refining biological n-butanol by pervaporation system |
| CN104771924A (en) * | 2015-04-15 | 2015-07-15 | 中国科学院广州能源研究所 | Device and method for preparing coupled and rectified ethanol by furfural |
| CN110002960A (en) * | 2019-05-05 | 2019-07-12 | 北京化工大学 | A kind of device and method of separation ABE fermentation infiltration evaporation liquid |
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