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Purification method and device for continuous rectification separation of ibuprofen intermediate raw material

A purification method and rectification separation technology, which is applied in the purification field of continuous rectification separation of ibuprofen intermediate raw materials, and can solve the problems of insufficient recovery rate and low recovery rate of isobutylbenzene

Active Publication Date: 2022-07-22
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
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Problems solved by technology

[0003] At present, the commonly used raw materials for ibuprofen intermediates include isobutylbenzene and p-isobutylacetophenone, etc., wherein, the purification of isobutylbenzene adopts a staged purification process of a batch rectification tower, but the staged purification process of a batch rectification tower The recovery rate of isobutylbenzene in the purification process is very low
Chinese patent CN201822040975.3 discloses a continuous distillation and purification system for unqualified chlorothalonil. most of the chlorothalonil, which effectively removes the hazardous waste in unqualified chlorothalonil products, but there is still the problem that the recovery rate is not high enough

Method used

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  • Purification method and device for continuous rectification separation of ibuprofen intermediate raw material

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Experimental program
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Effect test

Embodiment 1

[0063] The feed flow rate of the synthesis liquid is 900kg / h, the feed temperature is 25°C, and the feed pressure is 2atm, which contains 50% by weight of isobutylbenzene, 35% by weight of toluene, 5% by weight of 4-methyl-1-pentene, and 5% by weight of n-butyl benzene. Benzene 5wt%, 1-ethyl-2-vinylbenzene 5wt%; the actual number of trays in the T301 detetramethyl tower is 25, and the best feeding position is the 13th tray in the order from top to bottom, reflux The ratio is 1, the pressure is 1MPa; the actual number of trays of the toluene recovery tower T302 is 50, the best feeding position is the 10th tray from top to bottom, the reflux ratio is 1.2, and the pressure is 0.015MPa; toluene The actual number of trays of tower T303 is 44, the best feeding position is the 40th tray in the order from top to bottom, the reflux ratio is 2.5, and the pressure is 0.07MPa; the actual number of trays of isobutylbenzene tower T304 There are 110 plates, the best feeding position is the 7...

Embodiment 2

[0065] The feed flow rate of the synthesis liquid is 2000kg / h, the feed temperature is 25°C, and the feed pressure is 2atm, which contains 55wt% of isobutylbenzene, 35wt% of toluene, 4wt% of 4-methyl-1-pentene, n-butyl 4wt% of benzene, 2wt% of 1-ethyl-2-vinylbenzene; the actual number of trays in the T301 detetramethyl tower is 30, and the best feeding position is the 15th tray in the order from top to bottom, reflux The ratio is 1, the pressure is 1MPa; the actual number of trays of the toluene recovery tower T302 is 60, the best feeding position is the 13th tray from top to bottom, the reflux ratio is 1.5, and the pressure is 0.01MPa; The actual number of trays of tower T303 is 42, the best feeding position is the 40th tray in the order from top to bottom, the reflux ratio is 2.8, and the pressure is 0.015MPa; the actual number of trays of isobutylbenzene tower T304 There are 102 plates, the best feeding position is the 82nd plate in the order from top to bottom, the reflux ...

Embodiment 3

[0067]The feed flow rate of the synthesis liquid is 5000kg / h, the feed temperature is 25°C, and the feed pressure is 2atm, which contains 53wt% of isobutylbenzene, 38wt% of toluene, 3wt% of 4-methyl-1-pentene, n-butylene 3 wt% of benzene, 3 wt% of 1-ethyl-2-vinylbenzene; the actual number of trays of the T301 detetramethyl tower is 22, and the best feeding position is the 12th tray from top to bottom, reflux The ratio is 1.2, the pressure is 1MPa; the actual number of trays of the toluene recovery tower T302 is 55, the best feeding position is the 15th tray in the order from top to bottom, the reflux ratio is 1.8, and the pressure is 0.01MPa; toluene The actual number of trays of tower T303 is 38, the best feeding position is the 35th tray in the order from top to bottom, the reflux ratio is 2.1, and the pressure is 0.05MPa; the actual number of trays of isobutylbenzene tower T304 The best feeding position is the 63rd plate from top to bottom, the reflux ratio is 3.9, and the ...

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Abstract

The invention belongs to the technical field of chemical separation and purification, and particularly relates to a purification method and device for continuous rectification separation of an ibuprofen intermediate raw material. The method comprises the following steps: carrying out primary rectification on a synthetic liquid to obtain a primary material and recycled 4-methyl-1-pentene; performing second-stage rectification on the first-stage material to obtain a second-stage material and a recycled toluene crude product; and carrying out third-stage rectification on the second-stage material to obtain isobutylbenzene and a recovered n-butylbenzene crude product. Results of the embodiment show that the purification method provided by the invention is high in product recovery rate and product purity, the purity of the isobutylbenzene is as high as 99.99 wt%, the recovery rate is as high as 99.9 wt%, the impurity content is not higher than 50ppm, the problem of separation of the isobutylbenzene from the 4-methyl-1-pentene, the toluene and the n-butylbenzene is solved, the steps are simple, and the purification method has the advantages of low cost and low energy consumption.

Description

technical field [0001] The invention belongs to the technical field of chemical separation and purification, and in particular relates to a purification method and device for continuous rectification and separation of ibuprofen intermediate raw materials. Background technique [0002] Ibuprofen is an anti-inflammatory, antipyretic and analgesic drug with good curative effect. The domestic demand for ibuprofen intermediate raw materials is increasing. The production process of the intermediate raw materials is backward, the product quality is not up to standard, the energy consumption is high and the cost is high. Many factors lead to the domestic demand for ibuprofen intermediate raw materials basically relying on imports. Therefore, it is important to strengthen the research on the refining process of ibuprofen intermediate raw materials, improve the process route for producing ibuprofen intermediate raw materials, improve the quality of ibuprofen intermediate raw materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/04C07C15/02C07C15/06C07C11/113B01D3/14
CPCC07C7/005C07C7/04B01D3/146C07C15/02C07C15/06C07C11/113Y02P20/10
Inventor 崔培哲李鑫王英龙朱兆友王凯广齐建光钟立梅郑忠辉徐文辉贾建波杜德平
Owner QINGDAO UNIV OF SCI & TECH
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