CN106831471A - A kind of method for removing a small amount of acid or glacial acetic acid and refining DMF - Google Patents
A kind of method for removing a small amount of acid or glacial acetic acid and refining DMF Download PDFInfo
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- CN106831471A CN106831471A CN201710040321.8A CN201710040321A CN106831471A CN 106831471 A CN106831471 A CN 106831471A CN 201710040321 A CN201710040321 A CN 201710040321A CN 106831471 A CN106831471 A CN 106831471A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses the process that DMF and acid or glacial acetic acid in a kind of production of Sucralose are separate, the process is that methyl alcohol is added into pre-reactor together with DMF mixed liquors and solid acid catalyst containing acid or glacial acetic acid, enter reactive distillation column after pre-reaction, solid acid catalyst is inserted in reactive distillation column, unreacted acid or glacial acetic acid further reacts with methyl alcohol in reactive distillation column, reactive distillation tower top obtains methyl alcohol, the mixture of water and methyl acetate or methyl formate, deliver to existing methyl esters and equipment for separating methanol in Sucralose production, the DMF and aqueous mixtures of bottom of towe enter DMF dehydrating towers, bottom of towe reclaims the DMF for obtaining high-purity.The present invention can solve maximum azeotrope thing DMF and the problem of acid or glacial acetic acid separation in actual production, acetic acid is converted into useful methyl acetate or methyl formate, improve economic benefit；Recovery obtains DMF of the purity more than 99%, greatly reduces production cost.
Description
Technical field
The invention belongs to chemical technology field, and in particular to using in the method separation Sucralose industry of reactive distillation
N,N-dimethylformamide（DMF）And acid or glacial acetic acid.
Background technology
DMF abbreviation DMF, is the polar solvent of aprotic, is the fine solvent of many reactions.
The mixed solution of substantial amounts of DMF and acetic acid, and DMF can be produced in Sucralose production can be hydrolyzed as formic acid and dimethylamine.
All it is highly polar material due to DMF, acetic acid and formic acid, there is stronger interaction force between DMF and acid or glacial acetic acid, can
Form maximum azeotrope thing（156 DEG C of DMF and acetic acid normal pressure azeotropic temperature, acetic acid quality fraction 27%；DMF and formic acid normal pressure azeotropic temperature
153 DEG C of degree, formic acid mass fraction 8%）, it is difficult to realize separating by common method.
The separation method of report mainly has liquid-liquid extraction and azeotropic distillation at present.
Patent CN101977664, US20090259034 is disclosed and a kind of carboxylic is removed from the liquid comprising tertiary amide solvent
The method of acid, and in particular to use organic amine（Such as Alamine 304）Or organic amine and higher alcohol（Lauryl alcohol）Mixture from containing
Method in the DMF solution of cane sugar-6-acetic ester by liquid-liquid extraction separates acetic acid and DMF.Patent CN104774224 is introduced
A kind of method that carboxylic acid is removed from the sucrose-6-ester solution containing carboxylic acid, specially using TNA trinonylamine, tridecylamine, trioctylamine,
Alamine 304 class tertiary amine passes through multistage liquid-liquid extraction from formamide, N,N-dimethylformamide, N containing sucrose-6-ester, N- bis-
Acetic acid, benzoic acid, phenoxy propionic acid carboxylic acid are extracted in methylacetamide or dimethyl sulfoxide solvent.United States Patent (USP) US8796446 is disclosed
Acetic acid is extracted from the DMF solution containing cane sugar-6-acetic ester using organic tin compound, it is molten by DMF after repeatedly extraction
Acetic acid in liquid can be reduced to considerably less amount, but the organotin after extraction acetic acid is needed by NaOH neutralisation treatment,
Extractant could be reused, the acetic acid of such organotin extraction has then changed into acetate, increased the burden of solids treatment.
Japan Patent JP2002363150A discloses the method and apparatus that azeotropic distillation separates acetic acid and DMF.The method profit
With toluene as entrainer, toluene can form the lower azeotropic mixture of azeotropic point with acetic acid, without with DMF azeotropic, realize acetic acid
Separated with DMF azeotropic mixtures, but the method needs to add water simultaneously, and also required reflux ratio is also larger（30）, therefore from
The energy and economic angle consider it is unfavorable.
Additionally, DMF hydrolysis produce dimethylamine, dimethylamine dissociate in aqueous generation organic amine radical ion and hydroxyl from
Son and be in alkalescent, carry out ion exchange with tradable hydrogen ion on solid acid catalyst, solid acid catalytic can be caused
Agent is inactivated.This technique mainly suppresses DMF hydrolysis by three aspects causes catalyst to inactivate, and first, entering reactive distillation
Pre-reactor is set before, and the solid acid catalyst activating and regenerating in pre-reactor is simple and quick, but by balanced reaction
Limitation, still some unreacted acid or glacial acetic acid in reactive distillation column, it is necessary to further convert after pre-reaction.
Second, the mixed material after pre-reaction is sent into the rectifying section of reactive distillation column, most of water is produced from reactive distillation tower top, drop
Low amount of the water in conversion zone, reduces hydrolysis of the DMF in conversion zone, so as to suppress solid acid catalyst because being hydrolyzed with DMF
The dimethylamine of generation is acted on and inactivated.3rd, increase inlet amount of the methyl alcohol in reactive distillation column, methyl alcohol charging increases and can play
Diluting effect, reduces concentration of the water in reactive distillation column, equally reduces the hydrolysis of DMF, it is suppressed that solid acid catalyst
Inactivation.
Many acetic acid removed by the way of alkali neutralisation treatment in DMF solution in existing Sucralose production, but this
Sample is had to increase solids treatment device, and DMF can be hydrolyzed under alkalescence condition.
Therefore, present technology and factory's present situation are analyzed, it is proposed that a kind of technique side of new recovery DMF
Method.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, there is provided DMF solvent is returned in a kind of sucrose trichloride production process
The process of receipts.
The process that the DMF solvent that the present invention is provided is reclaimed be using the method for reactive distillation separate DMF and acetic acid or
Formic acid, specific operation process is as follows：
（1）By in the DMF solution of acid or glacial acetic acid, methyl alcohol and solid acid catalyst simultaneously addition pre-reactor；
（2）By in the mixed liquor feeding reactive distillation column upper end rectifying section charging aperture after pre-reaction, solid acid catalyst is reclaimed
Recycling；
（3）And by methyl alcohol feeding reactive distillation column lower end charging aperture, insert solid acid catalyst in reactive distillation column, acetic acid or
Further reaction is complete in reactive distillation column for formic acid；
（4）The overhead fraction of reactive distillation column is the mixture of methyl alcohol, water and methyl acetate or methyl formate, into Sucralose
Existing methyl esters and equipment for separating methanol in production；The tower reactor cut of reactive distillation column is DMF, water and a small amount of acid, and feeding DMF takes off
Water tower；
（5）DMF product of the purity more than 99% is obtained from the tower reactor of DMF dehydrating towers, waste water of the overhead extraction containing a small amount of DMF is delivered to
Sewage treatment plant.
The feeding temperature of DMF and acid or glacial acetic acid mixed liquor is 20 ~ 50 DEG C in described pre-reactor, and described methyl alcohol enters
Material temperature degree is 20 ~ 50 DEG C.
Described step（1）Acetic acid content is 5 ~ 40% in middle DMF and acetic acid mixed liquor.
Described step（1）Middle acid or glacial acetic acid is 1 with methanol molar ratio:1~1:5, catalyst amount is vinegar in raw material
Acid or the 5 ~ 30% of formic acid weight, pre-reaction temperature range is 30 ~ 80 DEG C.
Described step（1）Middle solid acid catalyst is NKC-9, Amberlyst15, D072 or D061, preferably NKC-
9。
Described step（3）Mixed liquor charging after the feed rate of middle reactive distillation column lower end charging aperture methyl alcohol and pre-reaction
Flow-rate ratio is 0.1:1~1:1.
The tower body part of described reactive distillation column from top to bottom includes three sections of rectifying section, conversion zone and stripping section successively.
The number of theoretical plate of described reactive distillation column is 30 ~ 60, atmospheric operation, and reflux ratio is 0.5 ~ 5.
Described DMF dehydrating towers number of theoretical plate is 15 ~ 50, decompression operation, and reflux ratio is 1~6.
Remarkable advantage of the invention：
By the way of reactive distillation, the acid or glacial acetic acid in DMF solution is converted into commercially valuable methyl esters, promote
Acid or glacial acetic acid is separated with DMF, and combines existing methyl alcohol and methyl esters separator in factory, is simplified and was operated
Journey.And the deactivation prob of acidic catalyst is fully taken into account, the hydrolysis of DMF has been reduced by technological design, so as to suppress solid
Body acidic catalyst is inactivated because of the dimethylamine effect produced with DMF hydrolysis.Purity is refining to obtain by dehydrating tower be more than 99%
DMF products, solve the current common problem of Sucralose industry, reduce production cost, reduce energy consumption, reduce
Pollution, improves economic worth and social value.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of process of the present invention.
1 is pre-reactor in figure, and 2 is mixed liquor feed pump after pre-reaction, and 3 is reactive distillation column overhead condenser, and 4 is anti-
Rectifying column rectifying section is answered, 5 is reactive distillation column, and 6 is the conversion zone of filled solid acidic catalyst in reactive distillation column, and 7 is anti-
The stripping section of rectifying column is answered, 8 is reactive distillation column tower reactor reboiler, and 9 is DMF dehydrating tower feed pumps, and 10 is the tower of DMF dehydrating towers
Top condenser, 11 is DMF dehydrating towers, and 12 is the tower reactor reboiler of DMF dehydrating towers.
Specific embodiment
1 couple of present invention elaborates below in conjunction with the accompanying drawings.
For the present invention is better described, technical scheme is readily appreciated, it is of the invention typical but non-limiting
Embodiment is as follows：
As shown in figure 1, a kind of a small amount of acetic acid of removing（Or formic acid）And the method for refining DMF, the described method comprises the following steps：
（1）The DMF solution of quantitative acid or glacial acetic acid, methyl alcohol and solid acidic resin catalyst are added in pre-reactor simultaneously
1, carry out pre-reaction；Wherein, acid content is 5 ~ 40%, acid or glacial acetic acid and methyl alcohol in charging in DMF and acid or glacial acetic acid mixed liquor
Mol ratio is 1:1~1:5, solid acid catalyst consumption is 5 ~ 30%, DMF and the acid or glacial acetic acid mixing of sour weight in raw material
The feeding temperature of liquid is 20 ~ 50 DEG C, and methyl alcohol feeding temperature is 20 ~ 50 DEG C, and pre-reaction temperature range is 30 ~ 80 DEG C；
（2）Mixture after pre-reaction sends into the rectifying section charging aperture of the epimere of reactive distillation column 5, reactive distillation column through feed pump 2
Hypomere pumps into methyl alcohol with the flow for setting, and unreacted acid or glacial acetic acid reacts complete in reactive distillation column；Wherein, methyl alcohol
Mixed liquor feed rate ratio is 0.1 after feed rate and pre-reaction:1~1:1, insert solid in the conversion zone 6 of reactive distillation column 5
Acidic catalyst is NKC-9, Amberlyst15, D072 or D061, and the number of theoretical plate of reactive distillation column is 30 ~ 60, normal pressure behaviour
Make, reflux ratio is 0.5 ~ 5；
（3）After the condensed device 3 of the overhead vapours of reactive distillation column 5 is condensed, partial reflux to reactive distillation column, part extraction is obtained
The mixture of methyl alcohol and methyl esters and water, delivers to existing methyl alcohol and methyl esters separator in Sucralose production；
（4）The tower reactor cut of reactive distillation column 5 is DMF, water and a small amount of acid, through the feeding DMF of feed pump 9 dehydrating towers 11；Wherein,
The number of theoretical plate of DMF dehydrating towers 11 is 15 ~ 50, decompression operation, and reflux ratio is 1~6；
（5）After the condensed device 10 of the overhead vapours of DMF dehydrating towers 11 is condensed, partial reflux to DMF dehydrating towers, part extraction is obtained
The mixture of water and a small amount of DMF, delivers to sewage treatment plant, and tower reactor is reclaimed and obtains DMF of the purity more than 99%.
Embodiment 1
Technical process is as shown in figure 1, DMF solution and acetic acid mol ratio containing acetic acid 15% are 1:1 methyl alcohol and acetic acid weight
20% NKC-9 catalyst is added in pre-reactor, 70 DEG C of reaction temperature.
Mixed liquor delivers to reactive distillation column epimere charging aperture after pre-reaction, reactive distillation column lower end methanol feed stream amount with it is upper
Section mixed liquor feed rate ratio is 0.3:1, reactive distillation column atmospheric operation, number of theoretical plate 30, reflux ratio is 0.5, overhead components
It is methyl acetate：34.1%th, methyl alcohol：59.3%th, water：6.6%, bottom of towe composition is DMF：98.9%th, acetic acid：0.1%th, water：1%.
Bottom of towe component enter DMF dehydrating towers, operating pressure 20kPa, number of theoretical plate 20, reflux ratio 3, tower top obtains water：
99.5%, bottom of towe obtains DMF：99.9%th, acetic acid 0.1%.
Embodiment 2
Technical process is as shown in figure 1, DMF solution and acetic acid mol ratio containing acetic acid 30% are 2:1 methyl alcohol and acetic acid weight
15% NKC-9 catalyst is added in pre-reactor, 65 DEG C of reaction temperature.
Mixed liquor delivers to reactive distillation column epimere charging aperture after pre-reaction, reactive distillation column lower end methanol feed stream amount with it is upper
Section mixed liquor feed rate ratio is 0.4:1, reactive distillation column atmospheric operation, number of theoretical plate 30, reflux ratio is 0.5, overhead components
It is methyl acetate：34.1%th, methyl alcohol：59.7%th, water：6.2%, bottom of towe composition is DMF：96.5%th, acetic acid：0.4%th, water：3.1%.
Bottom of towe component enter DMF dehydrating towers, operating pressure 20kPa, number of theoretical plate 20, reflux ratio 2, tower top obtains water：
99.8%, bottom of towe obtains DMF：99.6%th, acetic acid 0.4%.
Embodiment 3
Technical process is as shown in figure 1, DMF solution and acetic acid mol ratio containing acetic acid 40% are 3:1 methyl alcohol and acetic acid weight
15% NKC-9 catalyst is added in pre-reactor, 65 DEG C of reaction temperature.
Mixed liquor delivers to reactive distillation column epimere charging aperture after pre-reaction, reactive distillation column lower end methanol feed stream amount with it is upper
Section mixed liquor feed rate ratio is 0.4:1, reactive distillation column atmospheric operation, number of theoretical plate 30, reflux ratio is 0.5, overhead components
It is methyl acetate：29.7%th, methyl alcohol：64.7%th, water：5.6%, bottom of towe composition is DMF：95.4%th, acetic acid：0.4%th, water：4.2%.
Bottom of towe component enter DMF dehydrating towers, operating pressure 20kPa, number of theoretical plate 20, reflux ratio 1.5, tower top obtains water：
99.6%, bottom of towe obtains DMF：99.5%th, acetic acid 0.5%.
Embodiment 4
DMF solution and formic acid mol ratio containing formic acid 15% are 1:1 methyl alcohol and the NKC-9 catalyst of formic acid weight 20% add
Enter in pre-reactor, 60 DEG C of reaction temperature.
Mixed liquor delivers to reactive distillation column epimere charging aperture after pre-reaction, reactive distillation column lower end methanol feed stream amount with it is upper
Section mixed liquor feed rate ratio is 0.2:1, reactive distillation column atmospheric operation, number of theoretical plate 30, reflux ratio is 0.5, overhead components
It is methyl formate：43.4%th, methyl alcohol：46.8%th, water：9.8%, bottom of towe composition is DMF：98.2%th, formic acid：0.1%th, water：1.7%.
Bottom of towe component enter DMF dehydrating towers, operating pressure 20kPa, number of theoretical plate 20, reflux ratio 2, tower top obtains water：
99.5%, bottom of towe obtains DMF：99.8%th, formic acid 0.1%.
Embodiment 5
DMF solution and formic acid mol ratio containing formic acid 30% are 1.5:1 methyl alcohol and the NKC-9 catalyst of formic acid weight 15%
Add in pre-reactor, 50 DEG C of reaction temperature.
Mixed liquor delivers to reactive distillation column epimere charging aperture after pre-reaction, reactive distillation column lower end methanol feed stream amount with it is upper
Section mixed liquor feed rate ratio is 0.4:1, reactive distillation column atmospheric operation, number of theoretical plate 30, reflux ratio is 0.5, overhead components
It is methyl formate：35.0%th, methyl alcohol：56.6%th, water：8.4%, bottom of towe composition is DMF：96.5%th, formic acid：0.3%th, water：3.2%.
Bottom of towe component enter DMF dehydrating towers, operating pressure 20kPa, number of theoretical plate 20, reflux ratio 1.5, tower top obtains water：
99.6%, bottom of towe obtains DMF：99.7%th, formic acid 0.3%.
Embodiment 6
DMF solution and formic acid mol ratio containing formic acid 35% are 2:1 methyl alcohol and the NKC-9 catalyst of formic acid weight 15% add
Enter in pre-reactor, 50 DEG C of reaction temperature.
Mixed liquor delivers to reactive distillation column epimere charging aperture after pre-reaction, reactive distillation column lower end methanol feed stream amount with it is upper
Section mixed liquor feed rate ratio is 0.3:1, reactive distillation column atmospheric operation, number of theoretical plate 30, reflux ratio is 0.5, overhead components
It is methyl formate：34.9%th, methyl alcohol：56.7%th, water：8.4%, bottom of towe composition is DMF：95.5%th, formic acid：0.5%th, water：4.0%.
Bottom of towe component enter DMF dehydrating towers, operating pressure 20kPa, number of theoretical plate 20, reflux ratio 1.2, tower top obtains water：
99.6%, bottom of towe obtains DMF：99.4%th, formic acid 0.6%.
Embodiment 7
The present embodiment is with the difference of embodiment 1：
Solid acid catalyst is Amberlyst 15, and addition is 22% in pre-reaction.
Embodiment 8
The present embodiment is with the difference of embodiment 2：
Solid acid catalyst is Amberlyst 15, and addition is 18% in pre-reaction.
Embodiment 9
The present embodiment is with the difference of embodiment 3：
Solid acid catalyst is Amberlyst 15, and addition is 15% in pre-reaction.
Embodiments of the invention are the foregoing is only, is not intended to limit the invention, it is all in thought of the invention and principle
Within any modification, equivalent and the improvement made etc., should be included within the scope of the present invention.
Claims (8)
1. a kind of method for removing a small amount of acid or glacial acetic acid and refining DMF, it is characterised in that comprise the following steps：
（1）By the DMF solution of acid or glacial acetic acid, methyl alcohol and solid acid catalyst simultaneously add pre-reactor in, it is described pre-
Solid acid catalyst is provided with reactor；
（2）Mixed liquor after pre-reaction is sent into the rectifying section charging aperture of reactive distillation column, and methyl alcohol is sent into reactive distillation column
Lower end charging aperture, makes acid or glacial acetic acid further be reacted in reactive distillation column, and solid acid is filled with the reactive distillation column
Property catalyst；
（3）Methyl esters and separating methanol will be sent into from the methyl alcohol of reactive distillation column overhead extraction, water and methyl acetate or methyl formate
Device, and DMF, water and a small amount of acid mixed liquor feeding DMF dehydrating towers that reactive distillation tower reactor is produced；
（4）DMF product of the purity more than 99% is obtained from the tower reactor of DMF dehydrating towers, waste water of the overhead extraction containing a small amount of DMF is delivered to
Sewage treatment plant.
2. a kind of method for removing a small amount of acid or glacial acetic acid and refining DMF according to claim 1, it is characterised in that institute
The feeding temperature of the DMF solution of acid or glacial acetic acid is 20 ~ 50 DEG C in the pre-reactor stated, described methyl alcohol feeding temperature for 20 ~
50℃。
3. a kind of method for removing a small amount of acid or glacial acetic acid and refining DMF according to claim 1, it is characterised in that institute
The step of stating（1）Acid or glacial acetic acid content range is 5 ~ 40wt% in middle DMF solution.
4. a kind of method for removing a small amount of acid or glacial acetic acid and refining DMF according to claim 1, it is characterised in that
In the pre-reactor, acid or glacial acetic acid is 1 with the mol ratio of methyl alcohol:1~1:5, solid acid catalyst consumption is in raw material
The 5 ~ 30% of acid or glacial acetic acid weight, pre-reaction temperature range is 30 ~ 80 DEG C.
5. a kind of method for removing a small amount of acid or glacial acetic acid and refining DMF according to claim 1, it is characterised in that institute
State step（1）With（2）In solid acid catalyst be NKC-9, Amberlyst15, D072 or D061.
6. a kind of method for removing a small amount of acid or glacial acetic acid and refining DMF according to claim 1, it is characterised in that anti-
Answer in rectifying column that mixed liquor feed rate ratio is 0.1 after methanol feed stream amount and pre-reaction:1~1:1.
7. a kind of method for removing a small amount of acid or glacial acetic acid and refining DMF according to claim 1, it is characterised in that anti-
It is 30 ~ 60 to answer the number of theoretical plate of rectifying column, and normal pressing operation, reflux ratio is 0.5~5.
8. a kind of method for removing a small amount of acid or glacial acetic acid and refining DMF according to claim 1, it is characterised in that DMF
Dehydrating tower number of theoretical plate is 15 ~ 50, decompression operation, and reflux ratio is 1~6.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107459540A (en) * | 2017-08-28 | 2017-12-12 | 山东三和维信生物科技有限公司 | Method for the saving DMF and the raising ester yield of sucrose 6 of Sucralose production |
| CN107903183A (en) * | 2017-11-15 | 2018-04-13 | 福州大学 | Method of comprehensive utilization and device containing sour DMF solution |
| CN109503409A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | Sucralose is esterified reaction acid DMF processing method and processing device |
| CN111592469A (en) * | 2020-05-22 | 2020-08-28 | 安徽金禾实业股份有限公司 | Method for recovering DMAC (dimethylacetamide) residual liquid in sucralose production |
| CN111606822A (en) * | 2020-05-25 | 2020-09-01 | 安徽金禾实业股份有限公司 | Method for recovering acidic DMF (dimethyl formamide) in sucralose production |
| CN112933636A (en) * | 2021-03-04 | 2021-06-11 | 安徽金禾实业股份有限公司 | Scraper type sucrose-6-ester continuous production equipment and production process flow |
| CN113636951A (en) * | 2021-09-22 | 2021-11-12 | 安徽金禾实业股份有限公司 | Method for treating waste DMF in sucralose production |
| CN113666838A (en) * | 2021-09-22 | 2021-11-19 | 安徽金禾实业股份有限公司 | Method for recovering low-concentration DMF (dimethyl formamide) through double-tower coupling in sucralose production |
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Cited By (9)
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|---|---|---|---|---|
| CN107459540A (en) * | 2017-08-28 | 2017-12-12 | 山东三和维信生物科技有限公司 | Method for the saving DMF and the raising ester yield of sucrose 6 of Sucralose production |
| CN107903183A (en) * | 2017-11-15 | 2018-04-13 | 福州大学 | Method of comprehensive utilization and device containing sour DMF solution |
| CN107903183B (en) * | 2017-11-15 | 2019-11-12 | 福州大学 | Method of comprehensive utilization and device containing sour DMF solution |
| CN109503409A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | Sucralose is esterified reaction acid DMF processing method and processing device |
| CN111592469A (en) * | 2020-05-22 | 2020-08-28 | 安徽金禾实业股份有限公司 | Method for recovering DMAC (dimethylacetamide) residual liquid in sucralose production |
| CN111606822A (en) * | 2020-05-25 | 2020-09-01 | 安徽金禾实业股份有限公司 | Method for recovering acidic DMF (dimethyl formamide) in sucralose production |
| CN112933636A (en) * | 2021-03-04 | 2021-06-11 | 安徽金禾实业股份有限公司 | Scraper type sucrose-6-ester continuous production equipment and production process flow |
| CN113636951A (en) * | 2021-09-22 | 2021-11-12 | 安徽金禾实业股份有限公司 | Method for treating waste DMF in sucralose production |
| CN113666838A (en) * | 2021-09-22 | 2021-11-19 | 安徽金禾实业股份有限公司 | Method for recovering low-concentration DMF (dimethyl formamide) through double-tower coupling in sucralose production |
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