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Method and device for preparing tert-butyl acetate

A technology of tert-butyl acetate and acetic acid, which is applied in the field of preparing tert-butyl acetate, can solve the problems of low recovery rate of tert-butyl acetate, low recovery rate of tert-butyl acetate, low recovery rate of tert-butanol, etc., and achieve the purpose of suppressing side effects reaction, increase selectivity and yield, and suppress pyrolysis effects

Active Publication Date: 2021-06-08
HUNAN ZHONGCHUANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The mixed ester contains water, C8, tert-butanol and tert-butyl acetate. To recycle the tert-butanol in the mixed ester, rectification separation is usually used. The top material contains water, C8, tert-butanol and tert-butyl acetate. , the materials in the bottom of the tower are tert-butanol and tert-butyl acetate, the bottom materials can be returned to the reactor, and the tert-butanol can be reused, but the tert-butanol in the tower top materials cannot be reused, and are directly discharged as mixed esters to the mixed Ester tank, low recovery rate of tert-butanol in the whole system
[0013] Simultaneously, in the existing technology of preparing tert-butyl acetate, side reaction is more, causes the impurity content in the reaction product to be higher, and in the separation process, tert-butyl acetate pyrolysis, this also causes the yield of tert-butyl acetate to be relatively low. Low
[0014] In order to solve the problems of low recovery rate of tert-butyl acetate in the prior art, many reaction by-products, and low recovery rate of tert-butanol, a technical scheme for segmentally controlling the reaction temperature of the reactor is proposed. By controlling the reaction temperature, especially the first The reaction temperature of the second stage reduces the occurrence of side reactions and reduces the by-products after the reaction

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  • Method and device for preparing tert-butyl acetate
  • Method and device for preparing tert-butyl acetate
  • Method and device for preparing tert-butyl acetate

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Experimental program
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Effect test

Embodiment 1

[0049] Acetic acid and isobutylene are sent into the esterification reactor, and the polymerization inhibitor tert-butanol is added to react under the esterification reaction conditions. The esterification reactor is divided into two sections to control the reaction temperature respectively, and the temperature of the first section of the reaction is controlled to be 18°C, the temperature of the second stage reactor is controlled to be 18°C, the reaction pressure is 0.6MPa, the acid-ene ratio is 3:1, the reaction residence time is 80min, and the addition amount of polymerization inhibitor tert-butanol is 10wt% of the amount of acetic acid addition . The content of the mixture obtained after the reaction is: tert-butyl acetate 20.45wt%, tert-butanol 5.12wt%, acetic acid 68.54wt%, C8 2.12wt%, isobutylene 2.55wt%, water 1.22wt%. Enter the light component removal tower for separation. The top pressure of the light component removal tower is normal pressure, the top temperature is ...

Embodiment 2

[0052] Acetic acid and isobutylene are sent into the esterification reactor, and the polymerization inhibitor tert-butanol is added to react under the esterification reaction conditions. The esterification reactor is divided into two sections to control the reaction temperature respectively, and the temperature of the first section of the reaction is controlled to be 19°C, the temperature of the second stage reactor is controlled to be 20°C, the reaction pressure is 0.7MPa, the acid-to-ene ratio is 4:1, the reaction residence time is 70min, and the amount of polymerization inhibitor tert-butanol added is 8wt% of the amount of acetic acid added . The content of the mixture obtained after the reaction is: tert-butyl acetate 22.12wt%, tert-butanol 3.56wt%, acetic acid 64.77wt%, C8 2.89wt%, isobutylene 5.45wt%, water 1.21wt%. Enter the light component removal tower for separation. The top pressure of the light component removal tower is normal pressure, the top temperature is -8°C...

Embodiment 3

[0055]Acetic acid and isobutylene are sent into the esterification reactor, and the polymerization inhibitor tert-butanol is added to react under the esterification reaction conditions. The esterification reactor is divided into two sections to control the reaction temperature respectively, and the temperature of the first section of the reaction is controlled to be 20°C, control the temperature of the second stage reactor to be 22°C, the reaction pressure is 0.8MPa, the acid-ene ratio is 5:1, the reaction residence time is 60min, and the addition amount of polymerization inhibitor tert-butanol is 6wt% of the amount of acetic acid addition . The content of the mixture obtained after the reaction is: tert-butyl acetate 24.14wt%, tert-butanol 6.45wt%, acetic acid 65.21wt%, C8 1.81wt%, isobutylene 1.22wt%, water 1.17wt%, the mixture after the reaction was sent to Enter the light component removal tower for separation. The top pressure of the light component removal tower is norma...

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Abstract

The invention relates to a method and device for preparing tert-butyl acetate. The method mainly comprises the following steps: feeding a mixture of tert-butyl acetate, C8 and tert-butyl alcohol obtained at the top of a tert-butyl acetate refining tower into an extraction tower for extraction, extracting C8 and tert-butyl acetate from the top of the extraction tower, and extracting a mixture of tert-butyl alcohol and water from the bottom of the extraction tower; and feeding the mixture of the tert-butyl alcohol and water extracted from the bottom of the extraction tower into a rectifying tower for separation, extracting the tert-butyl alcohol containing water from the top of the rectifying tower, and extracting the water from the bottom of the rectifying tower. The method provided by the invention successfully solves the problems of low tert-butyl acetate recovery rate, considerable reaction byproducts and low tert-butyl alcohol recovery rate in the prior art, can effectively inhibit the occurrence of side reactions, reduces byproducts after the reactions, inhibits the high-temperature decomposition of tert-butyl acetate at the same time, and improves the selectivity and the yield of the tert-butyl acetate. The method is simple in process, easy to operate and low in energy consumption.

Description

technical field [0001] The invention relates to a method and a device for preparing tert-butyl acetate, in particular to a method and a device for preparing tert-butyl acetate with acetic acid and isobutene or mixed C4 containing isobutene. Background technique [0002] Tert-Butyl Acetate is a colorless liquid with a fruity aroma, is a low toxicity solvent, and is listed by the US Environmental Protection Agency as an exempt restricted volatile solvent and a non-hazardous air pollutant. Due to its unique molecular structure (big steric hindrance), mixing with other solvents can greatly improve the compatibility of solvents. Such as: nitrocellulose, acrylic, alkyd, polyester and polyurethane resins. As an oxygen-containing solvent, it can produce synergistic effects with other solvents (toluene, trichloroethane, etc.). As an environmentally friendly solvent, it can significantly reduce the atmospheric photochemical reactivity of the target product, the volatility at room te...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/04C07C67/54C07C29/74C07C29/80C07C31/12
CPCC07C67/04C07C67/54C07C29/74C07C29/80C07C69/14C07C31/12
Inventor 王坤刘郁东肖云飞刘良会
Owner HUNAN ZHONGCHUANG CHEM