CN1325840A - Process for preparing ethyl acetate - Google Patents
Process for preparing ethyl acetate Download PDFInfo
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- CN1325840A CN1325840A CN 01115328 CN01115328A CN1325840A CN 1325840 A CN1325840 A CN 1325840A CN 01115328 CN01115328 CN 01115328 CN 01115328 A CN01115328 A CN 01115328A CN 1325840 A CN1325840 A CN 1325840A
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Abstract
A process for preparing ethyl acetate includes such steps as preparing extractant in solvent recovery tower, loading acetic acid and solid acid catalyst to esterifying tower, loading solid acid catalyst to pre-reactor, pre-reacting of acetic acid on alcohol, introducing the resultant to lower part of esterifying tower, introducing alocohol and acetic acid to esterifying tower to obtain binary azeotropic mixture of ethyl acetate and water from top of esterifying tower, introducing said mixture and extractant to rectifying tower, and obtain ethyl acetate. Its advantages include less environmental pollution, low cost, simple process and high utilization rate of heat.
Description
The present invention relates to a kind of method of production ethyl acetate, belong to chemical technology field.
Ethyl acetate is colourless and dulcet liquid, and ethyl acetate is the main component of varnish, spices etc., is many resinoid efficient solvents, is a kind of purposes fine chemical product very widely.
Produce both at home and abroad at present and mainly contain two kinds of methods: be that raw material, the vitriol oil are the direct esterification method of catalyzer 1. with acetate and ethanol; 2. be catalyzer with aluminum alkoxide, acetaldehyde carried out condensation reaction generate ethyl acetate.Domestic main employing direct esterification method production ethyl acetate, there is nearly over one hundred family in manufacturer, scale from 10,000 tons/year to not waiting in 1 kiloton/year, the main drawback of its Production Flow Chart is the energy consumption height, vitriol oil corrosion production unit and spent acid emission of serious pollution of environment.
The objective of the invention is to release a kind of method of production ethyl acetate, at vitriol oil contaminate environment in the traditional technology, the shortcoming that etching apparatus and energy consumption are high, on the basis of development of new on-macromolecular solid acid catalyst PMB-II and high score subclass solid acid catalyst storng-acid cation exchange resin THNK-9, in conjunction with the high efficient separation technology-extractive distillation with salt technology of this teaching and research group, developed new green energy conservation technical process-solid acid continuous catalysis esterification reaction rectification-extractive distillation with salt integrated process.
The method of the production ethyl acetate that the present invention releases comprises following each step:
1, prepare extraction agent in advance at the tower still of solvent recovery tower, extraction agent wherein is ethylene glycol and composite salt, and composite salt accounts for 10%～15% of tower still capacity;
2, in the esterification column still, preset acetate and solid acid catalyst, ratio between two: acetate: solid acid catalyst=1: 0.005～0.01, be heated to 95 ℃～105 ℃, make tower still material enter the opening for feed of tower epimere through interchanger;
3, filling solid acid catalyst in pre-reactor, loading height is 0.8～1.2 meter, make mol ratio be 1: 1 acetate and ethanol in this reactor, under 70～85 ℃, reacted 25～35 minutes, finish pre-reaction after, enter esterification column hypomere opening for feed;
4, feeding simultaneously mol ratio continuously in esterification column is 1: 1 ethanol and acetate, and making the internal circulating load of still liquid in the esterification column is 1/3～1/5 of esterification column hypomere inlet amount, obtains the binary azeotrope of ethyl acetate and water at the esterification column cat head;
5, above-mentioned binary azeotrope steam directly enters extractive distillation with salt tower hypomere opening for feed, make extraction agent enter extractive distillation column epimere opening for feed simultaneously, wherein extraction agent is 1～2: 1 with the ratio of binary azeotrope inlet amount, and cat head promptly obtains ethyl acetate of the present invention.
Portioned product of the present invention is back to the esterification column cat head, is used for taking out of the water of ethanol and esterification generation; The diluted extraction agent of extracting rectifying Tata still extraction recycles after entering in the extraction agent recovery tower rectification under vacuum dehydration.
Composite salt in the used extraction agent of the above-mentioned the first step can be: NaOH, sodium-acetate or K
2CO
3In any; Used solid acid catalyst can be in above-mentioned the second, three step: any in D001, Phenylsulfonic acid, D72, D61, phenylformic acid or the toluene sulfonic acide, D001 wherein, D72 and D61 are provided by Tianjin resin processing plant of Nankai University.
Compared with the prior art the present invention has following characteristics:
1, optimize the esterification condition, in the past liquid-phase esterification is improved in vapour-liquid mixed phase esterification, its equilibrium constant of reaction K will exceed 4 times than reactive liquid solution equilibrium constant K under the similarity condition, has improved esterification efficient greatly;
2, developed solid acid catalyst, this new catalyst catalyzer with traditional on catalytic effect is identical, and etching apparatus is neither exempted the N-process of aftertreatment, and is free from environmental pollution;
3, introduce high efficient separation technology-extractive distillation with salt, simplified technology and equipment greatly, reduced energy consumption and working cost; This technology once was successfully applied to produces dehydrated alcohol, technology maturation.
Advantage of the present invention is: improved esterification reaction rate to greatest extent; Develop the novel ester catalysts, reduced environmental pollution, saved maintenance of equipment and maintenance cost; Simplify reaction and separation process, improved heat utilization efficiency, reduced energy consumption, reduced facility investment expense and working cost, reduced production cost; The production equipment operability is good, stable process conditions; Quality product can reach the standard of GB top grade product.All be better than domestic original technology at aspects such as technical indicator, economic benefit, operations.
Description of drawings:
Fig. 1 is the process flow sheet of the inventive method.
Below introduce embodiments of the invention.
Embodiment 1:
At internal diameter is Φ 30mm, stripping section is 500mm, the esterification section is 1000m, rectifying section is Glacial acetic acid and catalyzer Phenylsulfonic acid 50 grams of the interior 500ml of adding of esterification column still of 300m, 95% (volume ratio) ethanol and Glacial acetic acid were mixed back speed with 5ml/min in 1: 1 in molar ratio to be entered in the fixed bed pre-reactor of filling 270 gram D001 catalyzer, 80 ℃ of temperature through behind the initial action, enter esterification column underfeed mouth and enter esterification column; The circulation acetic acid that contains catalyzer in the tower still is mixed into esterification column top opening for feed and enters in the esterification column, tower still internal circulating load is 1/5 of charging, cat head obtains the binary azeotrope steam of ethyl acetate and water, tower top temperature is 71.5 ℃, reflux ratio is 1.5, do not need condensation to enter extractive distillation with salt tower bottom, the extraction agent that enters with cat head extractant feed mouth contacts, cat head obtain the ethyl acetate partial reflux to the esterification column cat head as trim the top of column, remainder is a product, purity is greater than more than 99.5%, product ethyl acetate yield is greater than 90%, the solvent ratio of extractive distillation with salt tower is 1.2, and tower top temperature is 77 ℃, about 110 ℃ of tower still temperature, extraction agent is ethylene glycol+NaOH, the stripping section 500mm of extractive distillation with salt tower, the extracting rectifying section is 1000mm, the extraction agent washing section is 200mm; The extraction agent that the tower still obtains diluting, enter solvent recovery tower and carry out rectification under vacuum, removed overhead moisture content, obtain the extraction agent that can be recycled at the bottom of the tower, the top vacuum degree of solvent recovery tower is 700mmHg, and tower top temperature is 40 ℃～50 ℃, tower still temperature is about 120 ℃, reflux ratio is 2, solvent recovery tower stripping section 600mm, rectifying section 1000mm.
Embodiment 2:
At internal diameter is Φ 30mm, stripping section is 500mm, the esterification section is 1000m, rectifying section is Glacial acetic acid and catalyzer Phenylsulfonic acid 50 grams of the interior 500ml of adding of esterification column still of 300m, 95% (volume ratio) ethanol and Glacial acetic acid were mixed back speed with 5ml/min in 1: 1 in molar ratio to be entered in the fixed bed pre-reactor of filling 300 gram D72 catalyzer, 85 ℃ of temperature through behind the initial action, enter esterification column underfeed mouth and enter esterification column; The circulation acetic acid that contains catalyzer in the tower still is mixed into esterification column top opening for feed and enters in the esterification column, tower still internal circulating load is 1/4 of charging, cat head obtains the binary azeotrope steam of ethyl acetate and water, tower top temperature is 71.5 ℃, reflux ratio is 1.5, do not need condensation to enter extractive distillation with salt tower bottom, the extraction agent that enters with cat head extractant feed mouth contacts, cat head obtain the ethyl acetate partial reflux to the esterification column cat head as trim the top of column, remainder is a product, purity is greater than more than 99.5%, product ethyl acetate yield is greater than 89%, the solvent ratio of extractive distillation with salt tower is 1.2, and tower top temperature is 77 ℃, about 110 ℃ of tower still temperature, extraction agent is ethylene glycol+NaOH, the stripping section 500mm of extractive distillation with salt tower, the extracting rectifying section is 1000mm, the extraction agent washing section is 200mm; The extraction agent that the tower still obtains diluting, enter solvent recovery tower and carry out rectification under vacuum, removed overhead moisture content, obtain the extraction agent that can be recycled at the bottom of the tower, the top vacuum degree of solvent recovery tower is 700mmHg, and tower top temperature is 40 ℃～50 ℃, tower still temperature is about 120 ℃, reflux ratio is 2, solvent recovery tower stripping section 600mm, rectifying section 1000mm.
Embodiment 3:
At internal diameter is Φ 30mm, stripping section is 500mm, the esterification section is 1000m, rectifying section is Glacial acetic acid and catalyzer Phenylsulfonic acid 50 grams of the interior 500ml of adding of esterification column still of 300m, 95% (volume ratio) ethanol and Glacial acetic acid were mixed back speed with 5ml/min in 1: 1 in molar ratio to be entered in the fixed bed pre-reactor of filling 320 gram D61 catalyzer, 91 ℃ of temperature through behind the initial action, enter esterification column underfeed mouth and enter esterification column; The circulation acetic acid that contains catalyzer in the tower still is mixed into esterification column top opening for feed and enters in the esterification column, tower still internal circulating load is 1/4.5 of charging, cat head obtains the binary azeotrope steam of ethyl acetate and water, tower top temperature is 71.5 ℃, reflux ratio is 1.5, do not need condensation to enter extractive distillation with salt tower bottom, the extraction agent that enters with cat head extractant feed mouth contacts, cat head obtain the ethyl acetate partial reflux to the esterification column cat head as trim the top of column, remainder is a product, purity is greater than more than 99.5%, product ethyl acetate yield is greater than 87%, the solvent ratio of extractive distillation with salt tower is 1.2, and tower top temperature is 77 ℃, about 110 ℃ of tower still temperature, extraction agent is ethylene glycol+NaOH, the stripping section 500mm of extractive distillation with salt tower, the extracting rectifying section is 1000mm, the extraction agent washing section is 200mm; The extraction agent that the tower still obtains diluting, enter solvent recovery tower and carry out rectification under vacuum, removed overhead moisture content, obtain the extraction agent that can be recycled at the bottom of the tower, the top vacuum degree of solvent recovery tower is 700mmHg, and tower top temperature is 40 ℃～50 ℃, tower still temperature is about 120 ℃, reflux ratio is 2, solvent recovery tower stripping section 600mm, rectifying section 1000mm.
Embodiment 4:
At internal diameter is Φ 30mm, stripping section is 500mm, the esterification section is 1000m, rectifying section is Glacial acetic acid and catalyzer phenylformic acid 75 grams of the interior 500ml of adding of esterification column still of 300m, 95% (volume ratio) ethanol and Glacial acetic acid were mixed back speed with 5ml/min in 1: 1 in molar ratio to be entered in the fixed bed pre-reactor of filling 270 gram D72 catalyzer, 85 ℃ of temperature through behind the initial action, enter esterification column underfeed mouth and enter esterification column; The circulation acetic acid that contains catalyzer in the tower still is mixed into esterification column top opening for feed and enters in the esterification column, tower still internal circulating load is 1/3 of charging, cat head obtains the binary azeotrope steam of ethyl acetate and water, tower top temperature is 71.5 ℃, reflux ratio is 1.5, do not need condensation to enter extractive distillation with salt tower bottom, the extraction agent that enters with cat head extractant feed mouth contacts, cat head obtain the ethyl acetate partial reflux to the esterification column cat head as trim the top of column, remainder is a product, purity is greater than more than 99.5%, product ethyl acetate yield is greater than 90%, the solvent ratio of extractive distillation with salt tower is 1.2, and tower top temperature is 77 ℃, about 110 ℃ of tower still temperature, extraction agent is ethylene glycol+NaOH, the stripping section 500mm of extractive distillation with salt tower, the extracting rectifying section is 1000mm, the extraction agent washing section is 200mm; The extraction agent that the tower still obtains diluting, enter solvent recovery tower and carry out rectification under vacuum, removed overhead moisture content, obtain the extraction agent that can be recycled at the bottom of the tower, the top vacuum degree of solvent recovery tower is 700mmHg, and tower top temperature is 40 ℃～50 ℃, tower still temperature is about 120 ℃, reflux ratio is 2, solvent recovery tower stripping section 600mm, rectifying section 1000mm.
Embodiment 5:
At internal diameter is Φ 30mm, stripping section is 500mm, the esterification section is 1000m, rectifying section is Glacial acetic acid and catalyzer phenylformic acid 75 grams of the interior 500ml of adding of esterification column still of 300m, 95% (volume ratio) ethanol and Glacial acetic acid were mixed back speed with 5ml/min in 1: 1 in molar ratio to be entered in the fixed bed pre-reactor of filling 270 gram D001 catalyzer, 80 ℃ of temperature through behind the initial action, enter esterification column underfeed mouth and enter esterification column; The circulation acetic acid that contains catalyzer in the tower still is mixed into esterification column top opening for feed and enters in the esterification column, tower still internal circulating load is 1/4.3 of charging, cat head obtains the binary azeotrope steam of ethyl acetate and water, tower top temperature is 71.5 ℃, reflux ratio is 1.5, do not need condensation to enter extractive distillation with salt tower bottom, the extraction agent that enters with cat head extractant feed mouth contacts, cat head obtain the ethyl acetate partial reflux to the esterification column cat head as trim the top of column, remainder is a product, purity is greater than more than 99.5%, product ethyl acetate yield is greater than 90%, the solvent ratio of extractive distillation with salt tower is 1.2, and tower top temperature is 77 ℃, about 110 ℃ of tower still temperature, extraction agent is ethylene glycol+NaOH, the stripping section 500mm of extractive distillation with salt tower, the extracting rectifying section is 1000mm, the extraction agent washing section is 200mm; The extraction agent that the tower still obtains diluting, enter solvent recovery tower and carry out rectification under vacuum, removed overhead moisture content, obtain the extraction agent that can be recycled at the bottom of the tower, the top vacuum degree of solvent recovery tower is 700mmHg, and tower top temperature is 40 ℃～50 ℃, tower still temperature is about 120 ℃, reflux ratio is 2, solvent recovery tower stripping section 600mm, rectifying section 1000mm.
Embodiment 6:
At internal diameter is Φ 30mm, stripping section is 500mm, the esterification section is 1000m, rectifying section is Glacial acetic acid and catalyzer toluene sulfonic acide 65 grams of the interior 500ml of adding of esterification column still of 300m, 95% (volume ratio) ethanol and Glacial acetic acid were mixed back speed with 5ml/min in 1: 1 in molar ratio to be entered in the fixed bed pre-reactor of filling 282 gram D001 catalyzer, 80 ℃ of temperature through behind the initial action, enter esterification column underfeed mouth and enter esterification column; The circulation acetic acid that contains catalyzer in the tower still is mixed into esterification column top opening for feed and enters in the esterification column, tower still internal circulating load is 1/4.6 of charging, cat head obtains the binary azeotrope steam of ethyl acetate and water, tower top temperature is 71.5 ℃, reflux ratio is 1.5, do not need condensation to enter extractive distillation with salt tower bottom, the extraction agent that enters with cat head extractant feed mouth contacts, cat head obtain the ethyl acetate partial reflux to the esterification column cat head as trim the top of column, remainder is a product, purity is greater than more than 99.5%, product ethyl acetate yield is greater than 90%, the solvent ratio of extractive distillation with salt tower is 1.2, and tower top temperature is 77 ℃, about 110 ℃ of tower still temperature, extraction agent is ethylene glycol+NaOH, the stripping section 500mm of extractive distillation with salt tower, the extracting rectifying section is 1000mm, the extraction agent washing section is 200mm; The extraction agent that the tower still obtains diluting, enter solvent recovery tower and carry out rectification under vacuum, removed overhead moisture content, obtain the extraction agent that can be recycled at the bottom of the tower, the top vacuum degree of solvent recovery tower is 700mmHg, and tower top temperature is 40 ℃～50 ℃, tower still temperature is about 120 ℃, reflux ratio is 2, solvent recovery tower stripping section 600mm, rectifying section 1000mm.
Embodiment 7:
At internal diameter is Φ 30mm, stripping section is 500mm, the esterification section is 1000m, rectifying section is Glacial acetic acid and catalyzer toluene sulfonic acide 65 grams of the interior 500ml of adding of esterification column still of 300m, 95% (volume ratio) ethanol and Glacial acetic acid were mixed back speed with 5ml/min in 1: 1 in molar ratio to be entered in the fixed bed pre-reactor of filling 282 gram D001 catalyzer, 80 ℃ of temperature through behind the initial action, enter esterification column underfeed mouth and enter esterification column; The circulation acetic acid that contains catalyzer in the tower still is mixed into esterification column top opening for feed and enters in the esterification column, tower still internal circulating load is 1/4.6 of charging, cat head obtains the binary azeotrope steam of ethyl acetate and water, tower top temperature is 71.5 ℃, reflux ratio is 1.5, do not need condensation to enter extractive distillation with salt tower bottom, the extraction agent that enters with cat head extractant feed mouth contacts, cat head obtain the ethyl acetate partial reflux to the esterification column cat head as trim the top of column, remainder is a product, purity is greater than more than 99.5%, product ethyl acetate yield is greater than 90%, the solvent ratio of extractive distillation with salt tower is 2.0, and tower top temperature is 77 ℃, about 110 ℃ of tower still temperature, extraction agent is ethylene glycol+sodium-acetate, the stripping section 500mm of extractive distillation with salt tower, the extracting rectifying section is 1000mm, the extraction agent washing section is 200mm; The extraction agent that the tower still obtains diluting, enter solvent recovery tower and carry out rectification under vacuum, removed overhead moisture content, obtain the extraction agent that can be recycled at the bottom of the tower, the top vacuum degree of solvent recovery tower is 700mmHg, and tower top temperature is 40 ℃～50 ℃, tower still temperature is about 120 ℃, reflux ratio is 1.8, solvent recovery tower stripping section 600mm, rectifying section 1000mm.
Embodiment 8:
At internal diameter is Φ 30mm, stripping section is 500mm, the esterification section is 1200m, rectifying section is Glacial acetic acid and catalyzer toluene sulfonic acide 65 grams of the interior 500ml of adding of esterification column still of 300m, 95% (volume ratio) ethanol and Glacial acetic acid were mixed back speed with 5ml/min in 1: 1 in molar ratio to be entered in the fixed bed pre-reactor of filling 300 gram D72 catalyzer, 85 ℃ of temperature through behind the initial action, enter esterification column underfeed mouth and enter esterification column; The circulation acetic acid that contains catalyzer in the tower still is mixed into esterification column top opening for feed and enters in the esterification column, tower still internal circulating load is 1/4.6 of charging, cat head obtains the binary azeotrope steam of ethyl acetate and water, tower top temperature is 71.5 ℃, reflux ratio is 1.5, do not need condensation to enter extractive distillation with salt tower bottom, the extraction agent that enters with cat head extractant feed mouth contacts, cat head obtain the ethyl acetate partial reflux to the esterification column cat head as trim the top of column, remainder is a product, purity is greater than more than 99.5%, product ethyl acetate yield is greater than 90%, and the solvent ratio of extractive distillation with salt tower is 1.4, and tower top temperature is 77 ℃, about 110 ℃ of tower still temperature, extraction agent is ethylene glycol+K
2CO
3, the stripping section 500mm of extractive distillation with salt tower, the extracting rectifying section is 1000mm, the extraction agent washing section is 200mm; The extraction agent that the tower still obtains diluting, enter solvent recovery tower and carry out rectification under vacuum, removed overhead moisture content, obtain the extraction agent that can be recycled at the bottom of the tower, the top vacuum degree of solvent recovery tower is 700mmHg, and tower top temperature is 40 ℃～50 ℃, tower still temperature is about 120 ℃, reflux ratio is 1.6, solvent recovery tower stripping section 800mm, rectifying section 1000mm.
Embodiment 9:
At internal diameter is Φ 30mm, stripping section is 500mm, the esterification section is 1200m, rectifying section is Glacial acetic acid and catalyzer toluene sulfonic acide 65 grams of the interior 500ml of adding of esterification column still of 300m, 95% (volume ratio) ethanol and Glacial acetic acid were mixed back speed with 5ml/min in 1: 1 in molar ratio to be entered in the fixed bed pre-reactor of filling 275 gram D001 catalyzer, 80 ℃ of temperature through behind the initial action, enter esterification column underfeed mouth and enter esterification column; The circulation acetic acid that contains catalyzer in the tower still is mixed into esterification column top opening for feed and enters in the esterification column, tower still internal circulating load is 1/4.6 of charging, cat head obtains the binary azeotrope steam of ethyl acetate and water, tower top temperature is 71.5 ℃, reflux ratio is 1.5, do not need condensation to enter extractive distillation with salt tower bottom, the extraction agent that enters with cat head extractant feed mouth contacts, cat head obtain the ethyl acetate partial reflux to the esterification column cat head as trim the top of column, remainder is a product, purity is greater than more than 99.5%, product ethyl acetate yield is greater than 90%, and the solvent ratio of extractive distillation with salt tower is 1.4, and tower top temperature is 77 ℃, about 110 ℃ of tower still temperature, extraction agent is ethylene glycol+K
2CO
3, the stripping section 500mm of extractive distillation with salt tower, the extracting rectifying section is 1000mm, the extraction agent washing section is 200mm; The extraction agent that the tower still obtains diluting, enter solvent recovery tower and carry out rectification under vacuum, removed overhead moisture content, obtain the extraction agent that can be recycled at the bottom of the tower, the top vacuum degree of solvent recovery tower is 700mmHg, and tower top temperature is 40 ℃～50 ℃, tower still temperature is about 120 ℃, reflux ratio is 1.6, solvent recovery tower stripping section 800mm, rectifying section 1000mm.
Claims (3)
1, a kind of method of production ethyl acetate is characterized in that this method comprises following each step:
(1) prepare extraction agent in advance at the tower still of solvent recovery tower, extraction agent wherein is ethylene glycol and composite salt, and composite salt accounts for 10%～15% of tower still capacity;
(2) in the esterification column still, preset acetate and solid acid catalyst, ratio between two: acetate: solid acid catalyst=1: 0.005～0.01, be heated to 95 ℃～105 ℃, make tower still material enter the opening for feed of tower epimere through interchanger;
(3) filling solid acid catalyst in pre-reactor, loading height is 0.8～1.2 meter, make mol ratio be 1: 1 acetate and ethanol in this reactor, under 70～85 ℃, reacted 25～35 minutes, finish pre-reaction after, enter esterification column hypomere opening for feed;
(4) feeding simultaneously mol ratio continuously in esterification column is 1: 1 ethanol and acetate, and making the internal circulating load of still liquid in the esterification column is 1/3～1/5 of esterification column hypomere inlet amount, obtains the binary azeotrope of ethyl acetate and water at the esterification column cat head;
(5) above-mentioned binary azeotrope steam directly enters extractive distillation with salt tower hypomere opening for feed, make extraction agent enter extractive distillation column epimere opening for feed simultaneously, wherein extraction agent is 1～2: 1 with the ratio of binary azeotrope inlet amount, and cat head promptly obtains ethyl acetate of the present invention.
2, preparation method as claimed in claim 1 is characterized in that the composite salt in the used extraction agent of the first step wherein is NaOH, sodium-acetate or K
2CO
3In any.
3, preparation method as claimed in claim 1 is characterized in that wherein used solid acid catalyst is in second and third step: any in D001, Phenylsulfonic acid, D72, D61, phenylformic acid or the toluene sulfonic acide.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01115328 CN1325840A (en) | 2001-04-20 | 2001-04-20 | Process for preparing ethyl acetate |
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|---|---|---|---|
| CN 01115328 CN1325840A (en) | 2001-04-20 | 2001-04-20 | Process for preparing ethyl acetate |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1294114C (en) * | 2004-05-21 | 2007-01-10 | 河北科技大学 | Method for producing acetic ether |
| CN102399130A (en) * | 2011-12-13 | 2012-04-04 | 西南化工研究设计院 | Method for simplifying rectification process for preparing ethanol through hydrogenation of acetic acid |
| CN103539663A (en) * | 2013-10-28 | 2014-01-29 | 江苏理工学院 | Separating method of ethyl acetate and cyclohexane |
| CN106693434A (en) * | 2015-08-05 | 2017-05-24 | 南通鸿志化工有限公司 | Salting extractive rectification device |
| CN107840808A (en) * | 2017-10-30 | 2018-03-27 | 烟台国邦化工机械科技有限公司 | Continuous reaction rectification production cyanoacetate compound, malonate compound device and its production technology |
| CN108083978A (en) * | 2017-12-25 | 2018-05-29 | 万华化学集团股份有限公司 | The preparation process and device of cyclohexanedimethanol |
| CN108675929A (en) * | 2018-03-23 | 2018-10-19 | 广西金茂生物化工有限公司 | A kind of production technology of ethyl acetate |
| CN109942358A (en) * | 2019-04-16 | 2019-06-28 | 营创三征(营口)精细化工有限公司 | A kind of solid acid catalysis low-boiling point alcohol continuous esterification technique |
| CN113493380A (en) * | 2020-04-01 | 2021-10-12 | 丹东明珠特种树脂有限公司 | Preparation method and preparation system of high-purity methyl acetate |
-
2001
- 2001-04-20 CN CN 01115328 patent/CN1325840A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1294114C (en) * | 2004-05-21 | 2007-01-10 | 河北科技大学 | Method for producing acetic ether |
| CN102399130B (en) * | 2011-12-13 | 2014-07-02 | 西南化工研究设计院 | Method for simplifying rectification process for preparing ethanol through hydrogenation of acetic acid |
| CN102399130A (en) * | 2011-12-13 | 2012-04-04 | 西南化工研究设计院 | Method for simplifying rectification process for preparing ethanol through hydrogenation of acetic acid |
| CN104829408B (en) * | 2013-10-28 | 2017-03-08 | 江苏理工学院 | A kind of ethyl acetate and the separation method of hexamethylene |
| CN103539663B (en) * | 2013-10-28 | 2015-05-13 | 江苏理工学院 | Separating method of ethyl acetate and cyclohexane |
| CN104829408A (en) * | 2013-10-28 | 2015-08-12 | 江苏理工学院 | Method for separation of ethyl acetate and cyclohexane |
| CN103539663A (en) * | 2013-10-28 | 2014-01-29 | 江苏理工学院 | Separating method of ethyl acetate and cyclohexane |
| CN106693434A (en) * | 2015-08-05 | 2017-05-24 | 南通鸿志化工有限公司 | Salting extractive rectification device |
| CN107840808A (en) * | 2017-10-30 | 2018-03-27 | 烟台国邦化工机械科技有限公司 | Continuous reaction rectification production cyanoacetate compound, malonate compound device and its production technology |
| CN108083978A (en) * | 2017-12-25 | 2018-05-29 | 万华化学集团股份有限公司 | The preparation process and device of cyclohexanedimethanol |
| CN108083978B (en) * | 2017-12-25 | 2021-01-29 | 万华化学集团股份有限公司 | Process and apparatus for the preparation of cyclohexanedimethanol |
| CN108675929A (en) * | 2018-03-23 | 2018-10-19 | 广西金茂生物化工有限公司 | A kind of production technology of ethyl acetate |
| CN109942358A (en) * | 2019-04-16 | 2019-06-28 | 营创三征(营口)精细化工有限公司 | A kind of solid acid catalysis low-boiling point alcohol continuous esterification technique |
| CN113493380A (en) * | 2020-04-01 | 2021-10-12 | 丹东明珠特种树脂有限公司 | Preparation method and preparation system of high-purity methyl acetate |
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