CN101397236A - Rectification technique for separating ethanol, acetone and butanol fermentation mash - Google Patents
Rectification technique for separating ethanol, acetone and butanol fermentation mash Download PDFInfo
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- CN101397236A CN101397236A CNA2008101531498A CN200810153149A CN101397236A CN 101397236 A CN101397236 A CN 101397236A CN A2008101531498 A CNA2008101531498 A CN A2008101531498A CN 200810153149 A CN200810153149 A CN 200810153149A CN 101397236 A CN101397236 A CN 101397236A
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Abstract
The invention relates to a distillation process method for separating ethanol-acetone-butanol fermentation mash. The distillation process method comprises the following steps: the fermentation mash is added from the middle part of a mash tower, a total solvent with the content of 93 percent discharged from the top of the tower enters the upper half part of a butanol tower, the waste mash discharged from the bottom of the tower enters a flash tank; a side mining section is arranged at the middle-upper part of the mash tower, the phase separation is carried out, heavy phases return to the mash tower, ight phases enter the middle-upper part of the butanol tower; the flash evaporation is carried out on the waste mash to 85 DEG C through a heat pump, secondary steam and fresh steam are mixed and then enter the bottom part of the mash tower for heating; the side mining section is arranged at the middle part of the butanol tower, the cooling phase separation is carried out, light phases return to the mash tower, and heavy phases return to the mash tower; and the follow-up section adopts the ordinary distillation process method for carrying out the separation. The distillation process method improves the working efficiency and the stability, greatly reduces the energy consumption during the distillation process of the ethanol, acetone and butanol mash and has significant practicality and economic benefits.
Description
Technical field
The present invention relates to the rectification process of fermentation liquid, the rectification technique of particularly a kind of separating alcohol, acetone and butanol fermentation mash specifically is to utilize heat pump techniques, the side technology of adopting to combine to pass through the processing method of rectifying separating alcohol-acetone-butanol fermentation mash from fermentation liquid.
Background technology
Ethanol, acetone and butanols are good organic solvents, and are the main raw materials of coating, plastics and products such as rubber, biofuel, are widely used in organic synthesis, plastics, resin, paint, medicine and national defense industry.Especially be that starting material production second third fourth (ethanol, acetone and butanols) solvent is the direction of future development with the non-grain crop.Common process adopts a plurality of towers such as wine with dregs tower, butanols tower, ethanol tower, acetone tower to carry out rectifying separation.Because of the third fourth content of second in the mash very low, be about about 2% (weight), and through the solvent behind wine with dregs tower and the butanols tower only is about 75%, therefore cause downstream section separation task heavier, mainly be to have portion water in a lot of towers, to carry out vaporization and condensation repeatedly, make that whole still-process energy consumption is higher; In the useless mash more dissolvent residual is arranged, the second stage employ degree is low.
Summary of the invention
The rectification technique that the purpose of this invention is to provide a kind of separating alcohol, acetone and butanol fermentation mash, this processing method can overcome the shortcoming of prior art, can reduce the energy consumption in the second third fourth mash still-process significantly, have significant practicality and economic benefit.
The step that the rectification technique of a kind of separating alcohol provided by the invention, acetone and butanol fermentation mash comprises:
1) fermentation liquid a adds from the middle part of wine with dregs tower 101, and it is that 93% total solvent enters butanols tower 102 first halves that cat head goes out content, and the mash that goes out to give up at the bottom of the tower enters flash tank 103.
2) offer side in wine with dregs tower 101 middle and upper parts and adopt, and the cooling phase-splitting, heavy phase is returned wine with dregs tower 101, gently enters butanols tower 102 middle and upper parts mutually.
3) flash tank 103 connection heat pumps 106 suitable for reading, the negative pressure that produces by heat pump 106 makes useless mash be flashed to 85 ℃, the secondary steam of generation with enter wine with dregs tower 101 bottoms after the live steam of heat pump 106 ingress mixes and heat.Useless mash enters environmental protection workshop section or second stage employ.
4) butanols tower 102 medial side are adopted, and the cooling phase-splitting, gently return tower mutually, and heavy phase is gone back to wine with dregs tower 101 middle and lower parts.
5) follow-up workshop section adopts common rectification technique to separate.Comprise butanols treating tower, acetone tower, aldehydes removal tower and ethanol tower.
6) butanols tower 102 tower still extraction fuel butanols b1 or enter butanols treating tower 201 bottoms, at the refining butanols b2 of butanols treating tower 201 middle and upper part extraction, the overhead product tundish v1 that packs into handles again, and the bottom product tundish v2 that packs into handles again.
7) the 102 cat head extraction of butanols tower enter acetone tower 202 middle and lower parts, and the 202 cat head extraction of acetone tower enter aldehydes removal tower 203 middle and upper parts, aldehydes removal tower 203 middle and lower part extraction acetone c, and aldehydes removal tower 203 bottom products return acetone tower 202 middle parts, and cat head not condensing h decyclization is protected processing.
8) extraction enters ethanol tower 204 middle and lower parts at the bottom of acetone tower 202 towers, ethanol tower 204 towers middle part extraction ethanol d, and overhead product goes back to acetone tower 202 middle and lower parts, and bottom product postbacks ferment mash opening for feed.
The feeding temperature of said wine with dregs tower 101 is 95 ℃, and 78 of stage number, reflux ratio are 6, and cat head extraction temperature is 65 ℃, and column bottom temperature is 105 ℃;
It is 95 ℃ that said side is adopted temperature, is cooled to 50 ℃.
Said heat pump ingress live steam pressure is 0.5-0.6Mpa, and top hole pressure is 0.13Mpa.
78 of said butanols tower 102 stage number, reflux ratio is 4, and cat head extraction temperature is 65 ℃, and it is 98 ℃ that medial side is adopted temperature, and side is adopted liquid and is cooled to 60 ℃ of phase-splittings, gently returns tower mutually, and heavy phase is gone back to wine with dregs tower 101 middle and lower parts.Adopt atmospheric operation.
50 of said butanols treating tower 201 stage number, total reflux operation, atmospheric operation, feed entrance point is apart from 7-8 blocks of column plates of tower still.At 3-8 Board positions of distance cat head 3 extraction mouths are set, butanols b is made with extra care in extraction.When refining butanols quality descended, suitably extraction overhead condensation product was handled to tundish v1 again.When tower still butanol content descended and have influence on refining butanols quality, the suitable extraction of bottom product was handled to tundish v2 again.
Said acetone tower 202 stage number 75, feed entrance point is apart from 20-22 blocks of column plates of tower still, reflux ratio 3-4, atmospheric operation.The cat head produced quantity is 70%-75% of an inlet amount, and extraction liquid enters aldehydes removal tower 203 tops.Extraction enters ethanol tower 204 middle and lower parts at the bottom of acetone tower 202 towers.The opening for feed position is apart from 20-25 blocks of column plates of ethanol tower 204 tower stills.
Said aldehydes removal tower 203 stage number 64, total reflux operation, cat head not condensing h decyclization is protected processing.Feed entrance point is apart from 2-4 blocks of plates of cat head.Aldehydes removal tower 203 middle part extraction acetone c, the extraction position is apart from 30-35 blocks of column plates of cat head, produced quantity is more than 95% of inlet amount, acetone tower 202 middle parts are gone back in the extraction of tower still after vaporizing, feed entrance point apart from acetone tower 202 towers at the bottom of 25-30 blocks of column plates.
Said ethanol tower 204 stage number 70, total reflux operation, feed entrance point is apart from 20-22 blocks of column plates of tower still.23-27 column plate places are provided with the extraction mouth at the distance cat head, and extraction ethanol d, produced quantity are that inlet amount is more than 90%.When the ethanol downgrade of extraction, suitably the extraction overhead product is to acetone tower 202, and suitably extraction tower kettle product to wine with dregs tower inlet enters wine with dregs tower 101 with fermentation liquid a simultaneously.Adopt atmospheric operation.
The present invention's advantage compared with prior art and the positively effect of generation:
Why energy consumption is bigger for former technology, and an important reasons is exactly dealing with improperly of wine with dregs tower 101 and 102 pairs of fermentation liquids of butanols tower, makes that about 25% water has entered follow-up workshop section, has carried out multiple condensation and vaporization in a plurality of towers.The present invention disposes the moisture more than 97% making full use of the side excavating technology, has alleviated the working load of follow-up tower greatly.Utilize heat pump techniques simultaneously, useless mash is carried out flash distillation, can fully reclaim remaining solvent wherein, and produce a large amount of available secondary steams, save live steam consumption, reduce discharging.Simultaneously, compare, under the situation of same treatment amount,, can significantly dwindle tower diameter, reduced heat lost by radiation and the facility investment of tower to external environment because of having reduced the treatment capacity of tower in the follow-up workshop section with former technology.
The defective of prior art maximum is: fermentation liquid enters from cat head through wine with dregs tower 101 backs that total solvent content is about 50% the feed liquid of butanols tower 102, after 102 processing of butanols tower, moisture about 25% moisture enters follow-up workshop section, causes very big load for the tower of back.And, this part moisture can not well be separated in the rectifying of back, the waste liquid of some carrier's a small amount of solvent comes back to wine with dregs tower 101 and butanols tower 102 carries out circular treatment, greatly reduce the operational stability and the efficient of wine with dregs tower 101 and butanols tower 102, caused the condensation vaporescence that moves in circles.
Process using side of the present invention is adopted cooling phase-splitting and heat pump techniques, moisture with 97% is disposed in wine with dregs tower 101 and butanols tower 102, make butanols tower 102 bottom butanol content reach fuel butanols rank (content is more than 98%), the top contains the extraction liquid of total solvent more than 97% and enters next workshop section.Owing to enter the feed liquid purity height of follow-up workshop section, the waste liquid that need return wine with dregs tower 101 and 102 processing of butanols tower again is few simultaneously, has improved the working efficiency and the stability of these two towers.Because follow-up workshop section treatment capacity is dwindled, and makes tower diameter dwindle, steam consumption reduces.Simultaneously add flash tank 103, utilize heat pump 106 to carry out flash distillation, can from useless mash, extract the content of remaining solvent in secondary steam and the useless wine with dregs of reduction the useless mash that comes out from wine with dregs tower 101 bottoms in wine with dregs tower 101 bottoms.
Description of drawings:
Fig. 1 is an invented technology flow path device synoptic diagram.
Embodiment.
Specific embodiments of the present invention is described in detail as follows with reference to accompanying drawing, but for illustrative purposes only rather than the restriction the present invention.
The step that a kind of separating alcohol-acetone provided by the invention-rectification technique of butanol fermentation mash comprises is described in detail as follows:
Total solvent content is that the fermentation liquid of 2% (weight ratio) is entered by the middle and upper part of wine with dregs tower 101, feeding temperature is 95 ℃, to be stabilized to tower top temperature be that 65 ℃, column bottom temperature begin extraction when being 105 ℃ in operation under the total reflux situation, the trim the top of column ratio is 6, produced quantity is 1% of an inlet amount, extraction liquid enters butanols tower 102 middle and upper parts, atmospheric operation.Side is adopted the position at 1/4 place, cat head middle and upper part, and produced quantity is 7% of an inlet amount, is cooled to 50 ℃ through supercooler 107 and enters phase separation tank 104, and heavy phase is returned wine with dregs tower 101,5 blocks of column plates of distance below the extraction column plate.Gently enter butanols tower 102 middle parts mutually on the top.105 ℃ of wine with dregs tower 101 bottom temps keep suitable liquid level, and useless mash enters flash tank 103, flash distillation to 85 ℃ discharge under the negative pressure state that heat pump 106 produces.Heat pump 106 bleeding points and 103 suitable for reading connections of flash tank.Heat pump 106 live steam inlet pressure 0.5MPa, top hole pressure 0.15MPa.
The 102 middle and upper part chargings of butanols tower, plate is several 78, reflux ratio 4.60 ℃ of tower top temperatures, produced quantity are 30% of total feed, and this moment, water-content was about 3%, and cat head extraction liquid enters next workshop section.Add side from tower bottom at 40% column plate of tower height and adopt, produced quantity is 85-90% of an inlet amount, and the extraction liquid temp is 98 ℃, after being cooled to 60 ℃, interchanger 108 enters phase separation tank 105, heavy phase enters wine with dregs tower 101 middle and lower parts, gently returns butanols tower 102 mutually, 2 blocks of column plates of distance under the extraction mouth.123 ℃ of butanols tower 102 tower still temperature, produced quantity is 50% of an inlet amount.Extraction liquid can reach fuel butanols rank, directly extraction b1 or to enter next workshop section refining.
Follow-up workshop section adopts the conventional rectification method to separate.
Application Example:
Undertaken by above-mentioned technology, the live steam consumption of former technology wine with dregs tower is 8.25 tons/hour, and the live steam consumption of butanols tower is 2.75 tons/hour, and follow-up workshop section live steam consumption is 3.15 tons/hour.Corresponding steam consumption is under the novel process: the wine with dregs tower is 5.1 tons/hour, and the butanols tower is 0.9 ton/hour, and follow-up workshop section is 2.4 tons/hour.Per hour saving the live steam consumption altogether is 5.75 tons/hour.By 130 yuan of calculating of steam per ton, 46000 tons of year saving steam, nearly 6,000,000 yuan of economic benefit.Simultaneously, through heat pump techniques, remaining solvent content in the useless mash at the bottom of the tower is dropped to below 0.0004% by original 0.0007%, significantly reduced and make when disposal of pollutants improves production capacity that environment is friendly more.
Claims (9)
1, the rectification technique of a kind of separating alcohol, acetone and butanol fermentation mash, this processing method are to produce ethanol, acetone and butanols by rectifying from fermentation liquid, it is characterized in that the step that it comprises:
1) fermentation liquid adds from the middle part of wine with dregs tower (101), and it is that 93% total solvent enters butanols tower (102) first half that cat head goes out content, and the mash that goes out to give up at the bottom of the tower enters flash tank (103);
2) offer side and adopt in wine with dregs tower (101) middle and upper part, and the cooling phase-splitting, heavy phase is returned wine with dregs tower (101), gently enters butanols tower (102) middle and upper part mutually;
3) flash tank (103) connection heat pump suitable for reading (106), the negative pressure that produces by heat pump (106) makes useless mash be flashed to 85 ℃, the secondary steam that produces heats bottom entering wine with dregs tower (101) after the live steam of heat pump 106 ingress mixes, and useless mash enters environmental protection workshop section or second stage employ;
4) butanols tower (102) medial side is adopted, and the cooling phase-splitting, gently returns tower mutually, and heavy phase is gone back to wine with dregs tower (101) middle and lower part.
5) follow-up workshop section adopts common rectification technique to separate, and comprises butanols treating tower, acetone tower, aldehydes removal tower and ethanol tower;
6) butanols tower (102) tower still extraction fuel butanols or enter butanols treating tower (201) bottom, at the refining butanols of butanols treating tower (201) middle and upper part extraction, the overhead product tundish v1 that packs into handles again, and the bottom product tundish v2 that packs into handles again;
7) butanols tower (102) cat head extraction enters acetone tower (202) middle and lower part, acetone tower (202) cat head extraction enters aldehydes removal tower (203) middle and upper part, aldehydes removal tower (203) middle and lower part extraction acetone, aldehydes removal tower 203) bottom product returns acetone tower (202) middle part, and cat head not condensing decyclization is protected and handled;
8) extraction enters ethanol tower (204) middle and lower part at the bottom of acetone tower (202) tower, ethanol tower (204) tower middle part extraction ethanol, and overhead product goes back to acetone tower (202) middle and lower part, and bottom product postbacks ferment mash opening for feed.
2, according to the said processing method of claim 1, the feeding temperature that it is characterized in that said wine with dregs tower (101) is 95 ℃, and 78 of stage number, reflux ratio are 6, and cat head extraction temperature is 65 ℃, and column bottom temperature is 105 ℃.
3,, it is characterized in that it is 95 ℃ that said side is adopted temperature, is cooled to 50 ℃ according to the said processing method of claim 1.
4, according to the said processing method of claim 1, it is characterized in that said heat pump ingress live steam pressure is 0.5-0.6Mpa, top hole pressure is 0.13Mpa.
5, according to the said processing method of claim 1, it is characterized in that 78 of said butanols tower (102) stage number, reflux ratio is 4, cat head extraction temperature is 65 ℃, it is 98 ℃ that medial side is adopted temperature, and side is adopted liquid and is cooled to 60 ℃ of phase-splittings, gently returns tower mutually, heavy phase is gone back to wine with dregs tower (101) middle and lower part, adopts atmospheric operation.
6, according to the said processing method of claim 1, it is characterized in that 50 of said butanols treating tower (201) stage number, total reflux operation, atmospheric operation, feed entrance point is apart from 7-8 blocks of column plates of tower still, at 3-8 Board positions of distance cat head 3 extraction mouths are set, butanols is made with extra care in extraction, when refining butanols quality descends, suitably extraction overhead condensation product is handled to tundish v1 again, when tower still butanol content descended and have influence on refining butanols quality, the suitable extraction of bottom product was handled to tundish v2 again.
7, according to the said processing method of claim 1, it is characterized in that said acetone tower (202) stage number 75, feed entrance point is apart from 20-22 blocks of column plates of tower still, reflux ratio 3-4, atmospheric operation, cat head produced quantity are 70%-75% of inlet amount, and extraction liquid enters aldehydes removal tower (203) top, extraction enters ethanol tower (204) middle and lower part at the bottom of acetone tower 202 towers, and the opening for feed position is apart from 20-25 blocks of column plates of ethanol tower (204) tower still.
8, according to the said processing method of claim 1, it is characterized in that said aldehydes removal tower (203) stage number 64, total reflux operation, cat head not condensing decyclization protect to be handled, and feed entrance point is apart from 2-4 blocks of plates of cat head, aldehydes removal tower (203) middle part extraction acetone, the extraction position is apart from 30-35 blocks of column plates of cat head, produced quantity is more than 95% of inlet amount, and acetone tower (202) middle part is gone back in the extraction of tower still after vaporizing, feed entrance point apart from acetone tower (202) tower at the bottom of 25-30 blocks of column plates.
9, according to the said processing method of claim 1, it is characterized in that said ethanol tower (204) stage number 70, total reflux operation, feed entrance point is apart from 20-22 blocks of column plates of tower still, 23-27 column plate places are provided with the extraction mouth at the distance cat head, extraction ethanol, produced quantity is that inlet amount is more than 90%, when the ethanol downgrade of extraction, suitably the extraction overhead product is to acetone tower (202), suitably extraction tower kettle product to wine with dregs tower inlet enters wine with dregs tower (101) with fermentation liquid simultaneously, adopts atmospheric operation.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101941888A (en) * | 2009-07-06 | 2011-01-12 | 中国科学院过程工程研究所 | Method for fermentation and differential pressure distillation of butanol by stalk dilute acid hydrolyzate |
| CN102432462A (en) * | 2011-10-25 | 2012-05-02 | 河北工业大学 | Method for extracting, rectifying and separating methylene dichloride, ethanol and ethyl acetate |
| CN102766020A (en) * | 2012-06-29 | 2012-11-07 | 北京化工大学 | Method for producing ethanol, acetone and butanol by permeabilization, vaporization, coupling and rectification of ABE (Acetone, Butanol and Ethanol) fermentation liquor |
| WO2014023136A1 (en) * | 2012-08-06 | 2014-02-13 | 南通醋酸纤维有限公司 | Low-density organic solvent aqueous solution recycling heat pump assisted distillation device and process |
| CN104086391A (en) * | 2014-06-16 | 2014-10-08 | 华南理工大学 | Ethanol, acetone and n-butanol salting-out composite rectification separation recovery method and apparatus |
| CN104844437A (en) * | 2015-05-12 | 2015-08-19 | 辽宁省石油化工规划设计院有限公司 | Method and device for separating solvent in nine-tower continuous rectification method |
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2008
- 2008-11-19 CN CN2008101531498A patent/CN101397236B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941888A (en) * | 2009-07-06 | 2011-01-12 | 中国科学院过程工程研究所 | Method for fermentation and differential pressure distillation of butanol by stalk dilute acid hydrolyzate |
| CN101941888B (en) * | 2009-07-06 | 2014-11-05 | 中国科学院过程工程研究所 | Method for fermentation and differential pressure distillation of butanol by stalk dilute acid hydrolyzate |
| CN102432462A (en) * | 2011-10-25 | 2012-05-02 | 河北工业大学 | Method for extracting, rectifying and separating methylene dichloride, ethanol and ethyl acetate |
| CN102432462B (en) * | 2011-10-25 | 2014-01-15 | 河北工业大学 | Method for extracting, rectifying and separating methylene dichloride, ethanol and ethyl acetate |
| CN102766020A (en) * | 2012-06-29 | 2012-11-07 | 北京化工大学 | Method for producing ethanol, acetone and butanol by permeabilization, vaporization, coupling and rectification of ABE (Acetone, Butanol and Ethanol) fermentation liquor |
| CN102766020B (en) * | 2012-06-29 | 2014-11-05 | 北京化工大学 | Method for producing ethanol, acetone and butanol by permeabilization, vaporization, coupling and rectification of ABE (Acetone, Butanol and Ethanol) fermentation liquor |
| WO2014023136A1 (en) * | 2012-08-06 | 2014-02-13 | 南通醋酸纤维有限公司 | Low-density organic solvent aqueous solution recycling heat pump assisted distillation device and process |
| CN104086391A (en) * | 2014-06-16 | 2014-10-08 | 华南理工大学 | Ethanol, acetone and n-butanol salting-out composite rectification separation recovery method and apparatus |
| CN104086391B (en) * | 2014-06-16 | 2016-01-06 | 华南理工大学 | The method of the compound rectifying separation recovery of saltouing of ethanol, acetone and propyl carbinol and device |
| CN104844437A (en) * | 2015-05-12 | 2015-08-19 | 辽宁省石油化工规划设计院有限公司 | Method and device for separating solvent in nine-tower continuous rectification method |
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