CN113636930A - Production process of acetic anhydride - Google Patents
Production process of acetic anhydride Download PDFInfo
- Publication number
- CN113636930A CN113636930A CN202111056694.7A CN202111056694A CN113636930A CN 113636930 A CN113636930 A CN 113636930A CN 202111056694 A CN202111056694 A CN 202111056694A CN 113636930 A CN113636930 A CN 113636930A
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- CN
- China
- Prior art keywords
- acetic anhydride
- acid
- cracking
- acetic acid
- condensable gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 84
- 238000010521 absorption reaction Methods 0.000 claims abstract description 27
- 239000002253 acid Substances 0.000 claims abstract description 26
- 239000007789 gas Substances 0.000 claims abstract description 23
- 238000005336 cracking Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- CCGKOQOJPYTBIH-UHFFFAOYSA-N ethenone Chemical compound C=C=O CCGKOQOJPYTBIH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims abstract description 9
- 235000019838 diammonium phosphate Nutrition 0.000 claims abstract description 9
- 238000011084 recovery Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 230000008016 vaporization Effects 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000009835 boiling Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 239000000498 cooling water Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000019631 acid taste sensations Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/54—Preparation of carboxylic acid anhydrides
- C07C51/56—Preparation of carboxylic acid anhydrides from organic acids, their salts, their esters or their halides, e.g. by carboxylation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/54—Preparation of carboxylic acid anhydrides
- C07C51/573—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention relates to a production process of acetic anhydride, which comprises the steps of preparing 94% of cracking acid solution from acetic acid, vaporizing the cracking acid, adding 10% of diammonium hydrogen phosphate, mixing, feeding the mixture into a cracking furnace, cracking at a high temperature of 700-730 ℃ and a negative pressure of-0.06-0.08 MPa in the furnace under the action of a catalyst to generate ketene, water and non-condensable gas, cooling the water and unreacted acetic acid by water and salt, cooling and condensing in sections, discharging, feeding the cooled ketene and non-condensable gas into an absorption tower to perform absorption reaction with the acetic acid in the tower, absorbing the ketene and the acetic acid to generate crude acetic anhydride, and feeding the non-condensable gas into a subsequent absorption tower to perform subsequent recovery. The invention has the following advantages: can effectively improve the conversion rate of raw materials, thereby further improving the yield of acetic anhydride and improving the production efficiency.
Description
Technical Field
The invention relates to the technical field of acetic anhydride production, in particular to a production process of acetic anhydride.
Background
Acetic anhydride is an organic substance having the chemical formula C4H6O3Colorless transparent liquid, strong smell of acetic acid, acid taste, hygroscopicity, dissolving in chloroform and diethyl ether, slowly dissolving in water to form acetic acid, and reacting with ethanol to form ethyl acetate. Is inflammable and has corrosionSexual, lacrimatory.
The existing acetic anhydride production process has low raw material conversion rate, thus resulting in lower acetic anhydride yield and low production efficiency.
Disclosure of Invention
The invention aims to provide a production process of acetic anhydride, which aims to improve the conversion rate of raw materials and the yield of acetic anhydride and improve the production efficiency.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: preparing 94% of cracking acid solution from acetic acid, vaporizing the cracking acid, adding 10% of diammonium hydrogen phosphate, mixing, feeding the mixture into a cracking furnace, cracking at the high temperature of 700-730 ℃ and under the negative pressure of-0.06-0.08 MPa in the furnace under the action of a catalyst to generate ketene, water and non-condensable gas, cooling the water and unreacted acetic acid by water and salt, cooling and condensing in sections, discharging, feeding the cooled ketene and non-condensable gas into an absorption tower to perform absorption reaction with the acetic acid in the tower, generating crude acetic anhydride after the absorption reaction of the ketene and the acetic acid, and feeding the non-condensable gas into a subsequent absorption tower to perform subsequent recovery; when the concentration of the crude acetic anhydride reaches 85%, the crude acetic anhydride is sent into a rectifying tower for rectification, fractionated low boiling point returns to an absorption tower for absorption, a high boiling point part is extracted at regular time for centralized treatment, middle fraction is used as finished acetic anhydride, unabsorbed non-condensable gas is washed and absorbed through subsequent multi-stage circulation, and finally the middle fraction is exhausted out of a vacuum pump extraction system, a small amount of uncracked acetic acid and water generated by reaction are separated in a condensation process, namely weak acid is collected in a weak acid recovery tank through a gas-liquid separator, and the weak acid is recycled through a weak acid concentrating device and is reused.
As an improvement: the catalyst is diammonium hydrogen phosphate.
The beneficial effects obtained by the invention are as follows: the process can effectively improve the conversion rate of the raw materials, thereby further improving the yield of the acetic anhydride and improving the production efficiency.
Description of the drawings:
FIG. 1 is a flow chart of a process for producing acetic anhydride according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1: preparing 94% of cracking acid solution from acetic acid, vaporizing the cracking acid, adding 10% of diammonium hydrogen phosphate, mixing, feeding the solution into a cracking furnace, cracking at a high temperature of 700 ℃ and under a negative pressure of-0.06 MPa in the furnace under the action of a catalyst to generate ketene, water and non-condensable gas, cooling the water and unreacted acetic acid by water and cooling salt, cooling and condensing in sections, discharging the ketene, the non-condensable gas and the cooled ketene, the cooled non-condensable gas and the cooled non-condensable gas enter an absorption tower to perform absorption reaction with the acetic acid in the tower, the ketene and the acetic acid generate crude acetic anhydride after the absorption reaction, and the non-condensable gas enters a subsequent absorption tower to perform subsequent recovery; when the concentration of the crude acetic anhydride reaches 85%, the crude acetic anhydride is sent into a rectifying tower for rectification, fractionated low boiling point returns to an absorption tower for absorption, a high boiling point part is extracted at regular time for centralized treatment, middle fraction is used as finished acetic anhydride, unabsorbed non-condensable gas is washed and absorbed through subsequent multi-stage circulation, and finally the middle fraction is exhausted out of a vacuum pump extraction system, a small amount of uncracked acetic acid and water generated by reaction are separated in a condensation process, namely weak acid is collected in a weak acid recovery tank through a gas-liquid separator, and the weak acid is recycled through a weak acid concentrating device and is reused.
The catalyst is diammonium hydrogen phosphate.
Example 2: preparing 94% of cracking acid solution from acetic acid, vaporizing the cracking acid, adding 10% of diammonium hydrogen phosphate, mixing, feeding the solution into a cracking furnace, cracking at 730 ℃ and under-0.08 MPa in the furnace under the action of a catalyst to generate ketene, water and non-condensable gas, cooling the water and unreacted acetic acid by water and cooling the salt, cooling and condensing the water and unreacted acetic acid in sections, discharging the cooled ketene and non-condensable gas, feeding the ketene and non-condensable gas into an absorption tower to perform absorption reaction with the acetic acid in the tower, performing absorption reaction on the ketene and the acetic acid to generate crude acetic anhydride, and feeding the non-condensable gas into a subsequent absorption tower to perform subsequent recovery; when the concentration of the crude acetic anhydride reaches 85%, the crude acetic anhydride is sent into a rectifying tower for rectification, fractionated low boiling point returns to an absorption tower for absorption, a high boiling point part is extracted at regular time for centralized treatment, middle fraction is used as finished acetic anhydride, unabsorbed non-condensable gas is washed and absorbed through subsequent multi-stage circulation, and finally the middle fraction is exhausted out of a vacuum pump extraction system, a small amount of uncracked acetic acid and water generated by reaction are separated in a condensation process, namely weak acid is collected in a weak acid recovery tank through a gas-liquid separator, and the weak acid is recycled through a weak acid concentrating device and is reused.
The catalyst is diammonium hydrogen phosphate.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (2)
1. A production process of acetic anhydride is characterized by comprising the following steps: preparing 94% of cracking acid solution from acetic acid, vaporizing the cracking acid, adding 10% of diammonium hydrogen phosphate, mixing, feeding the mixture into a cracking furnace, cracking ketene, water and non-condensable gas in the furnace at the high temperature of 700-730 ℃ under the action of a catalyst under the negative pressure of-0.06-0.08 MPa, cooling water and salt of the unreacted acetic acid by stages, cooling and condensing the water and unreacted acetic acid by stages, discharging the cooled ketene and non-condensable gas, feeding the ketene and non-condensable gas into an absorption tower to perform absorption reaction with the acetic acid in the tower, performing absorption reaction on the ketene and the acetic acid to generate crude acetic anhydride, and feeding the non-condensable gas into a subsequent absorption tower to perform subsequent recovery; when the concentration of the crude acetic anhydride reaches 85%, the crude acetic anhydride is sent into a rectifying tower for rectification, fractionated low boiling point returns to an absorption tower for absorption, a high boiling point part is extracted at regular time for centralized treatment, middle fraction is used as finished acetic anhydride, unabsorbed non-condensable gas is washed and absorbed through subsequent multi-stage circulation, and finally the middle fraction is exhausted out of a vacuum pump extraction system, a small amount of uncracked acetic acid and water generated by reaction are separated in a condensation process, namely weak acid is collected in a weak acid recovery tank through a gas-liquid separator, and the weak acid is recycled through a weak acid concentrating device and is reused.
2. The process for producing acetic anhydride according to claim 1, wherein: the catalyst is diammonium hydrogen phosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111056694.7A CN113636930A (en) | 2021-09-09 | 2021-09-09 | Production process of acetic anhydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111056694.7A CN113636930A (en) | 2021-09-09 | 2021-09-09 | Production process of acetic anhydride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113636930A true CN113636930A (en) | 2021-11-12 |
Family
ID=78425420
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111056694.7A Pending CN113636930A (en) | 2021-09-09 | 2021-09-09 | Production process of acetic anhydride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113636930A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101006041A (en) * | 2004-08-18 | 2007-07-25 | 塞拉尼斯国际公司 | Acetic anhydride and acetate ester co-production |
| CN102476988A (en) * | 2010-11-22 | 2012-05-30 | 中国石油化学工业开发股份有限公司 | Method for preparing carboxyl anhydride |
-
2021
- 2021-09-09 CN CN202111056694.7A patent/CN113636930A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101006041A (en) * | 2004-08-18 | 2007-07-25 | 塞拉尼斯国际公司 | Acetic anhydride and acetate ester co-production |
| CN102476988A (en) * | 2010-11-22 | 2012-05-30 | 中国石油化学工业开发股份有限公司 | Method for preparing carboxyl anhydride |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211112 |
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| RJ01 | Rejection of invention patent application after publication |