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
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  • 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; interm

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

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Example Embodiment

[0028] Example 1, the method for the integrated separation of p-tert-butyl toluene, p-tert-butyl benzaldehyde and p-tert-butyl benzoic acid with liquid-liquid extraction crystallization and vacuum sideline distillation, refer to figure 1 Shown process diagram and figure 2 with image 3 In the device shown, the specific process of the integrated process of extractive crystallization and vacuum side-line distillation is: at room temperature, raw materials ② It is the mixed liquid of p-tert-butyltoluene, p-tert-butylbenzaldehyde and p-tert-butylbenzoic acid that first enters the extraction crystallization tower 1, the extractant ① Benzene enters the extraction crystallization tower 1 under the raw materials, fully stirs the raw materials, controls the temperature of the extraction crystallization tower to 28.3℃, separates and crystallizes by layers, the raffinate phase and the extraction phase reach equilibrium in the standing section, the extraction phase ③ and the extraction pha...

Example Embodiment

[0030] Example 2 is basically the same as Example 1, but the raw material composition in step (1) is: 37.1% p-tert-butyl toluene, 52.23% p-tert-butyl benzaldehyde and 10.67% p-tert-butyl benzoic acid. In step (2), the mass ratio of raw material / extractant toluene is 1:0.7-1.0; the actual number of stages of the extraction 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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