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Method for extracting p-tertbutyl benzaldehyde from oxidation reactant of p-tertbutyl methylbenzene through integration of liquid-liquid extraction crystallization and decompression sidetrack rectification

A technology of p-tert-butyltoluene and tert-butyl benzoic acid, applied in the field of p-tert-butyl benzaldehyde, can solve the problems of inconvenient control of product quality, large equipment investment, long technological process, etc., and achieve convenient product quality and equipment investment. Reduced, no impact on the environment

Inactive Publication Date: 2014-01-01
江苏沿江化工资源开发研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Using the above method, there are the following problems: the process is long and complicated, and the investment in equipment is large; intermittent operation is inconvenient to control product quality; multiple washings and alkali washings seriously waste resources and affect the environment

Method used

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  • Method for extracting p-tertbutyl benzaldehyde from oxidation reactant of p-tertbutyl methylbenzene through integration of liquid-liquid extraction crystallization and decompression sidetrack rectification
  • Method for extracting p-tertbutyl benzaldehyde from oxidation reactant of p-tertbutyl methylbenzene through integration of liquid-liquid extraction crystallization and decompression sidetrack rectification
  • Method for extracting p-tertbutyl benzaldehyde from oxidation reactant of p-tertbutyl methylbenzene through integration of liquid-liquid extraction crystallization and decompression sidetrack rectification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1, liquid-liquid extraction crystallization and vacuum side stream rectification integrated separation method for p-tert-butyltoluene, p-tert-butylbenzaldehyde and p-tert-butylbenzoic acid, refer to figure 1 The process diagram shown and figure 2 and image 3 The device shown, the specific flow of the integrated process of extraction crystallization and vacuum side stream rectification is: at room temperature, raw materials ② For p-tert-butyltoluene, p-tert-butylbenzaldehyde and p-tert-butylbenzoic acid mixed solution at first enter extraction crystallization tower 1, extractant ① Benzene enters the extraction and crystallization tower 1 below the raw materials, and is fully stirred with the raw materials. The temperature of the extraction and crystallization tower is controlled at 28.3°C, and the layers are separated and crystallized. See Table 2 for the content of each component of the remaining phase ④. The extraction phase enters the vacuum distillati...

Embodiment 2

[0030] Embodiment 2 is basically the same as Example 1, but the raw materials in step (1) consist of: 37.1% p-tert-butyltoluene, 52.23% p-tert-butylbenzaldehyde and 10.67% p-tert-butylbenzoic acid. In step (2), the mass ratio of raw material / extractant toluene is 1:0.7-1.0; the actual number of stages in the extraction and crystallization section is 4 stages.

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Abstract

The invention discloses a method for extracting p-tertbutyl benzaldehyde from an oxidation reactant of p-tertbutyl methylbenzene through integration of liquid-liquid extraction crystallization and decompression sidetrack rectification. The method comprises the steps of putting a raw material into an extraction crystallization tower from the upper part of the extraction crystallization tower to reversely contact with an extracting agent methylbenzene which flows into the extraction crystallization tower from the lower part of the extraction crystallization tower; controlling the temperature and the mass ratio of the raw material to the extracting agent; putting the push-out material of the extraction crystallization tower into an extraction phase standing section at the upper part of the extraction crystallization tower; treating the material in a decompression sidetrack rectification tower to obtain p-tertbutyl benzaldehyde of which the concentration is more than 99.1% at the bottom of the decompression sidetrack rectification tower and a mixture of p-tertbutyl benzoic acid crystal and methylbenzene at the bottom of the extraction crystallization tower; standing the mixture of p-tertbutyl benzoic acid crystal and methylbenzene through extraction residual phases at the bottom of the extraction crystallization tower, and filtering in a pressure reducing filter to obtain p-tertbutyl benzoic acid crystal of which the concentration is 99.3%; circulating the methylbenzene into a liquid-liquid extraction crystallization tower. By adopting the method disclosed by the invention, water resources are saved, the discharge of wastewater is reduced, the production process flow is shortened, the equipment investment is reduced by about 35%, and continuous operations are adopted to ensure that the product quality can be controlled conveniently.

Description

technical field [0001] The invention relates to a chemical separation process, in particular to a method for extracting p-tert-butylbenzaldehyde in p-tert-butyltoluene oxidation reactants through the integration of liquid-liquid extraction crystallization and vacuum side line rectification. technical background [0002] 4-tert-butylbenzaldehyde is an important intermediate for the preparation of flavors, fragrances and medicinal products. As a raw material for the preparation of lyral, lyral is mainly used in daily chemicals and pesticide intermediates. The methods for preparing p-tert-butylbenzaldehyde mainly include oxygen catalysis and manganese dioxide oxidation production process. The preparation of p-tert-butylbenzaldehyde by manganese dioxide oxidation method has many by-products and serious environmental pollution. The oxygen oxidation method is cleaner . [0003] Use p-tert-butyltoluene as raw material to produce p-tert-butylbenzaldehyde and p-tert-butylbenzoic aci...

Claims

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Application Information

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IPC IPC(8): C07C27/34C07C27/28C07C45/80C07C47/542C07C51/43C07C51/48C07C63/04
CPCC07C45/81C07C51/43C07C47/542C07C63/04
Inventor 顾正桂詹其伟顾小艳
Owner 江苏沿江化工资源开发研究院有限公司
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