Device and method for shortening ketalation time in ibuprofen synthesis process

A technology of reaction time and synthesis process, applied in organic chemistry, chemical industry, sustainable manufacturing/processing, etc., can solve problems such as restricting ibuprofen production cycle, limiting ibuprofen production capacity, long reaction time, etc., and achieves easy washing Effects of operation, increasing reaction contact area and shortening reaction time

Active Publication Date: 2014-01-22
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems of this process are long reaction time, high energy consumption, and the steamed water contains neopentyl glycol with a mass content of about 17-20%, which needs to be recycled
[0006] Ketalization is an important intermediate chemical in the production of ibuprofen, and ketalization is a control step in the production of ibuprofen, which restricts the production cycle of ibuprofen and limits the production capacity of ibuprofen

Method used

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  • Device and method for shortening ketalation time in ibuprofen synthesis process
  • Device and method for shortening ketalation time in ibuprofen synthesis process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Feeding: 200g of petroleum ether, 105.3g of ketone, 71.3g of neopentyl glycol, and 9.3mL of 30% dilute sulfuric acid. After being heated by the steam in the jacket of the reaction kettle and the reboiler (E1), the temperature of the liquid in the reaction kettle (R) rises from 50°C to 85°C, the temperature at the bottom of the tower is 70°C, and the mass content of ketone in the bottom of the tower is 1.6%. The temperature at the top of the tower was 62°C, the mass content of neopentyl glycol in the bottom water layer of the reflux tank (A) was 0.8%, and the ketalization reaction time was 8 hours.

Embodiment 2

[0041] Feeding: 300g of petroleum ether, 158g of ketone, 107g of neopentyl glycol, 14mL of 30% dilute sulfuric acid. After being heated by the steam in the jacket of the reactor (R) and the reboiler (E1), the temperature of the liquid in the reactor (R) rises from 50°C to 92°C, the temperature at the bottom of the tower is 79°C, and the mass content of ketone in the bottom of the tower is 1.4%, the temperature at the top of the tower is 69°C, the mass content of neopentyl glycol in the water layer at the bottom of the reflux tank (A) is 0.5%, and the ketalization reaction time is 7.8 hours.

Embodiment 3

[0043] Feed: 3kg of petroleum ether, 1.6kg of ketone, 1.1kg of neopentyl glycol, 145mL of 30% dilute sulfuric acid. After being heated by the steam in the jacket of the reactor (R) and the reboiler (E1), the temperature of the liquid in the reactor (R) rises from 50°C to 97°C, the temperature at the bottom of the tower is 88°C, and the mass content of ketone in the bottom of the tower is 1.3%, the temperature at the top of the tower is 80°C, the mass content of neopentyl glycol in the water layer at the bottom of the reflux tank (A) is 0.83%, and the ketalization reaction time is 7.2 hours.

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Abstract

The invention relates to a device for shortening ketalation time in an ibuprofen synthesis process through reactive rectification, and a method for shortening ketalation time in an ibuprofen production process. The device consists of a reaction kettle (R), a rectification tower (T), a reboiler (E1), a condenser (E2), a reflux tank (A) and a circulating pump (P). The method comprises the following steps: adding a certain amount of chlorone-containing petroleum ether solution, neopentyl glycol and dilute sulfuric acid into the reaction kettle (R); heating the liquor in the reaction kettle (R) by use of steam in a jacket; introducing gas phase of the heated liquor into the rectification tower (T) to separate; feeding tank liquor of the reaction kettle (R) into the reboiler (E1) through the circulating pump (P) to heat; feeding into the reaction kettle (R); condensing the steam withdrawn on the tower top into condensation water through the condenser (E2) to obtain petroleum ether and water; layering the solution in the reflux tank (A), taking the upper layer of petroleum ether as overhead reflux, and withdrawing and recovering the lower layer of water.

Description

【Technical field】 [0001] The invention belongs to the field of chemical reaction rectification, and relates to the separation of water generated by the reaction of ketone and neopentyl glycol in a system in which dilute sulfuric acid is used as a catalyst and petroleum ether is used as a water-carrying agent, in particular a reaction rectification device and A method of shortening the reaction time of ketalization using this device. 【Background technique】 [0002] The production of ibuprofen is synthesized by the 1,2-transposition rearrangement method. It uses isobutylbenzene as a raw material to prepare ketone through Friedel-Crafts acylation with 2-chloropropionyl chloride, and then dilute sulfuric acid as a catalyst. Then it can be ketalized with neopentyl glycol, and then the product can be catalyzed rearrangement, hydrolysis and so on. [0003] The ketalization process uses ketone and neopentyl glycol as raw materials, dilute sulfuric acid as a catalyst, and petroleum ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/06
CPCC07D319/06Y02P20/10
Inventor 朱兆友王英龙张玲刘永太朱庆书汝绍刚孟庆信崔培哲朱峰
Owner QINGDAO UNIV OF SCI & TECH
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