CN114014755B - Production process of methyl acetate in organic chemical industry - Google Patents
Production process of methyl acetate in organic chemical industry Download PDFInfo
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- CN114014755B CN114014755B CN202111483768.5A CN202111483768A CN114014755B CN 114014755 B CN114014755 B CN 114014755B CN 202111483768 A CN202111483768 A CN 202111483768A CN 114014755 B CN114014755 B CN 114014755B
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- Prior art keywords
- tower
- liquid material
- methyl acetate
- reaction
- acetic acid
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- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 title claims abstract description 30
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 239000000126 substance Substances 0.000 title claims abstract description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000011344 liquid material Substances 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000010517 secondary reaction Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000003860 storage Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000004064 recycling Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 239000003153 chemical reaction reagent Substances 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 10
- 238000007670 refining Methods 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 238000004806 packaging method and process Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- 230000032050 esterification Effects 0.000 claims description 4
- 238000005886 esterification reaction Methods 0.000 claims description 4
- 238000004065 wastewater treatment Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
- 238000009717 reactive processing Methods 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 9
- 238000000066 reactive distillation Methods 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- KYWXRBNOYGGPIZ-UHFFFAOYSA-N 1-morpholin-4-ylethanone Chemical compound CC(=O)N1CCOCC1 KYWXRBNOYGGPIZ-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000002649 leather substitute Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of methyl acetate production process, and discloses an organic chemical methyl acetate and a production process thereof, wherein the production process comprises the following production steps of: mixing, reacting, recycling, purifying and cooling for storage, wherein the operation pressure of the reactive rectifying tower is 101.33kPa, the temperature of the tower top is 57 ℃, the temperature of the tower kettle is 106 ℃, the reactive processing before purification is carried out, the reacted liquid material is rectified by the light component removing tower, the rectified liquid material is discharged into the heavy component removing tower, acetic acid is added into the liquid material by the heavy component removing tower, the liquid material is discharged into the reactive rectifying tower again after acetic acid is added into the liquid material, the reactive rectifying tower carries out secondary reaction, the liquid material after the secondary reactive processing is also subjected to the secondary rectifying processing by the light component removing tower, the rectified liquid material is discharged into the dehydrating tower, the liquid material is separated by the dehydrating tower, the high-purity methyl acetate and water are obtained, the purity of the obtained methyl acetate can reach 99.28%, and the purifying effect is good.
Description
Technical Field
The invention relates to the technical field of methyl acetate production processes, in particular to a production process of methyl acetate in organic chemical industry.
Background
Methyl acetate is a raw material of methyl ester, acetic acid and water, and is commonly used for manufacturing solvents, essence, artificial leather, reagents and the like after being generated.
The traditional production of the organic chemical methyl acetate is to add an acetyl morpholine organic ligand, a metal stabilizer, potassium acetate, sodium chloride and aqueous solution of potassium chloride into the generated methyl acetate to achieve high-purity methyl acetate, but the mode has higher requirements on temperature, pressure and the proportion of the added reagent in production and preparation, if the control is not strictly forbidden in operation, the purity of the methyl acetate is easily reduced, the operation requirement is higher, and the obtained methyl acetate reagent also contains a certain proportion of moisture, so that the problem of relatively lower purity is solved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a production process of methyl acetate in organic chemical industry, which aims to solve the problems in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions: the production process of methyl acetate in organic chemical industry includes the following steps:
S1, mixing: adding a certain proportion of methanol, a certain proportion of acetic acid and a certain proportion of water into a synthesizer;
S2, reaction: pouring the catalyst into a synthesizer, and carrying out esterification synthesis after catalyzing methanol, acetic acid and water through the catalyst;
s3, recycling: recovering alcohol in the synthesized reagent and performing wastewater treatment;
s4, purifying: refining and purifying the synthesized and dealcoholized reagent to obtain high-purity methyl acetate liquid material;
S5, cooling and storing: and cooling the purified liquid material, and storing the liquid material.
Preferably, the refining and purifying in the step S4 comprises a reaction rectifying tower, a light component removing tower, a heavy component removing tower and a dehydrating tower, wherein the operation pressure of the reaction rectifying tower is 101.33kPa, the tower top temperature is 57 ℃, the tower bottom temperature is 106 ℃, and the reaction processing before the purifying is carried out.
Preferably, the reacted liquid material is rectified through a light component removal tower.
Preferably, the rectified liquid material is discharged into a heavy-removal tower, acetic acid is added into the liquid material in the heavy-removal tower, then the liquid material is discharged into a reaction rectifying tower again, secondary reaction is carried out through the reaction rectifying tower, and the liquid material after secondary reaction processing is also rectified again through a light-removal tower.
Preferably, the liquid material after rectification is discharged into a dehydration tower, and the liquid material is separated by the dehydration tower to obtain high-purity methyl acetate and water.
Preferably, in the step S5, the I-type dangerous goods are packaged by a plastic packaging barrel, a sealing ring is added at the opening of the barrel, the dangerous goods plastic packaging barrel meets the requirement of GB.18191, and the storage temperature is lower than 25 ℃.
Compared with the prior art, the invention provides a production process of methyl acetate in organic chemical industry, which has the following beneficial effects:
The operation pressure of the reactive distillation column is 101.33kPa, the temperature of the top of the column is 57 ℃, the temperature of the column bottom is 106 ℃, the reactive processing is carried out before purification, the reacted liquid material is rectified by a light component removal column, the rectified liquid material is discharged into a heavy component removal column, acetic acid is added into the liquid material by the heavy component removal column, the liquid material is discharged into the reactive distillation column again, the reactive distillation column is used for carrying out secondary reaction, the liquid material after the secondary reactive processing is also subjected to the reactive distillation processing by the light component removal column, the liquid material after the reactive distillation is discharged into the dehydration column, the separation treatment is carried out by the dehydration column, the high-purity methyl acetate and water are obtained, the purity of the obtained methyl acetate can reach up to 99.28%, and the purification effect is good.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a flow chart of refining and purifying of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a technical scheme, a production process of methyl acetate in organic chemical industry, referring to fig. 1, comprising methanol, acetic acid, a catalyst and water, wherein the production steps are as follows:
S1, mixing: adding a certain proportion of methanol, a certain proportion of acetic acid and a certain proportion of water into a synthesizer;
S2, reaction: pouring the catalyst into a synthesizer, and carrying out esterification synthesis after catalyzing methanol, acetic acid and water through the catalyst;
s3, recycling: recovering alcohol in the synthesized reagent and performing wastewater treatment;
s4, purifying: refining and purifying the synthesized and dealcoholized reagent to obtain high-purity methyl acetate liquid material;
S5, cooling and storing: and cooling the purified liquid material, and storing the liquid material.
Referring to fig. 2, the refining and purifying in step S4 includes a reactive rectifying tower, a light component removing tower, a heavy component removing tower and a dehydrating tower, wherein the reactive rectifying tower has an operating pressure of 101.33kPa, a tower top temperature of 57 ℃ and a tower bottom temperature of 106 ℃, and the reactive rectifying tower is subjected to reactive processing before purifying.
And rectifying the reacted liquid material through a light component removal tower.
Discharging the rectified liquid material into a heavy-removal tower, discharging the liquid material into a reaction rectifying tower again after acetic acid is added into the liquid material, performing secondary reaction through the reaction rectifying tower, and performing secondary rectification processing on the liquid material after secondary reaction processing through a light-removal tower.
And discharging the liquid material after rectification into a dehydration tower, and separating the liquid material through the dehydration tower to obtain high-purity methyl acetate and water.
And in the step S5, the I-type dangerous goods are packaged by using a plastic packaging barrel, a sealing ring is added at the opening of the barrel, the dangerous goods plastic packaging barrel meets the requirement of GB.18191, and the storage temperature is lower than 25 ℃.
The working principle of the device is as follows: adding a certain proportion of methanol, a certain proportion of acetic acid and a certain proportion of water into a synthesizer, pouring a catalyst into the synthesizer, carrying out catalytic esterification synthesis on the methanol, the acetic acid and the water through the catalyst, recovering alcohol in synthesized reagents, carrying out wastewater treatment on the reagents after synthesis and alcohol removal, refining and purifying the reagents to obtain high-purity methyl acetate liquid, wherein the refining and purifying steps comprise a reaction rectifying tower, a light component removing tower, a heavy component removing tower and a dehydrating tower, the operating pressure of the reaction rectifying tower is 101.33kPa, the temperature of the top of the tower is 57 ℃, the temperature of the tower kettle is 106 ℃, carrying out reaction processing before purification, rectifying the reacted liquid through the light component removing tower, discharging the rectified liquid into the heavy component removing tower again, such as the reaction rectifying tower, carrying out secondary reaction on the liquid after secondary reaction processing, carrying out rectification processing again through the light component removing tower, discharging the liquid after rectification again into the dehydrating tower, carrying out separation processing on the liquid through the dehydrating tower, obtaining high-purity methyl acetate and the water, cooling the liquid after the reaction rectifying tower, and the liquid is cooled and the liquid is packaged to meet the dangerous condition of a dangerous condition of being stored in a plastic packaging barrel, and the dangerous condition meeting the requirements of a packing, namely, the dangerous condition of a plastic packaging barrel is stored in a packing container is cooled package, and the dangerous condition is stored at a temperature of a dangerous condition of a storage container is required to be 25 GB is stored at 25.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (2)
1. A production process of methyl acetate in organic chemical industry is characterized in that: comprises methanol, acetic acid, a catalyst and water, and the production steps are as follows:
S1, mixing: adding a certain proportion of methanol, a certain proportion of acetic acid and a certain proportion of water into a synthesizer;
S2, reaction: pouring the catalyst into a synthesizer, and carrying out esterification synthesis after catalyzing methanol, acetic acid and water through the catalyst;
s3, recycling: recovering alcohol in the synthesized reagent and performing wastewater treatment;
s4, purifying: refining and purifying the synthesized and dealcoholized reagent to obtain high-purity methyl acetate liquid material;
s5, cooling and storing: cooling the purified liquid material, and storing the liquid material;
The refining and purifying in the step S4 comprises a reaction rectifying tower, a light component removing tower, a heavy component removing tower and a dehydrating tower, wherein the operation pressure of the reaction rectifying tower is 101.33kPa, the tower top temperature is 57 ℃, the tower bottom temperature is 106 ℃, and the reaction processing before the purifying is carried out;
Rectifying the reacted liquid material through a light component removal tower;
Discharging the rectified liquid material into a heavy-removal tower, discharging the liquid material into a reaction rectifying tower again after acetic acid is added into the liquid material by the heavy-removal tower, performing secondary reaction by the reaction rectifying tower, and performing secondary rectification processing on the liquid material after secondary reaction processing by a light-removal tower;
and discharging the liquid material after rectification into a dehydration tower, and separating the liquid material through the dehydration tower to obtain high-purity methyl acetate and water.
2. The process for producing methyl acetate in organic chemical industry according to claim 1, wherein the process comprises the following steps: and in the step S5, the I-type dangerous goods are packaged by using a plastic packaging barrel, a sealing ring is added at the opening of the barrel, the dangerous goods plastic packaging barrel meets the requirement of GB.18191, and the storage temperature is lower than 25 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111483768.5A CN114014755B (en) | 2021-12-07 | 2021-12-07 | Production process of methyl acetate in organic chemical industry |
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|---|---|---|---|
| CN202111483768.5A CN114014755B (en) | 2021-12-07 | 2021-12-07 | Production process of methyl acetate in organic chemical industry |
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| Publication Number | Publication Date |
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| CN114014755A CN114014755A (en) | 2022-02-08 |
| CN114014755B true CN114014755B (en) | 2024-06-25 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306994A (en) * | 2008-06-18 | 2008-11-19 | 河北工业大学 | Technological process for producing high-purity methyl acetate and device |
| 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 |
| CN113651695A (en) * | 2021-08-17 | 2021-11-16 | 天津天南同创科技发展有限公司 | Separation and refining method for preparing methyl acetate from industrial tail gas |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186575B (en) * | 2007-12-04 | 2010-04-14 | 南京工业大学 | Methyl acetate catalytic rectification hydrolysis process |
| CN102060655A (en) * | 2010-12-13 | 2011-05-18 | 陈越峰 | Hydrolysis method of methyl acetate |
| CN205821214U (en) * | 2016-07-06 | 2016-12-21 | 湖北三里枫香科技有限公司 | A kind of production technology device of high-purity methyl acetate |
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2021
- 2021-12-07 CN CN202111483768.5A patent/CN114014755B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306994A (en) * | 2008-06-18 | 2008-11-19 | 河北工业大学 | Technological process for producing high-purity methyl acetate and device |
| 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 |
| CN113651695A (en) * | 2021-08-17 | 2021-11-16 | 天津天南同创科技发展有限公司 | Separation and refining method for preparing methyl acetate from industrial tail gas |
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