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Process for producing resorcinol by continuously hydrolyzing m-phenylenediamine

A technology of m-phenylenediamine and resorcinol, which is applied in the field of continuous hydrolysis of m-phenylenediamine to produce resorcinol, which can solve the problems of reduced reaction yield and product quality, long storage time of hydrolyzed materials, and high energy consumption of external input. problems, to achieve a high degree of device intensification, solve the problem of decomposition and deterioration, and enhance competitiveness

Active Publication Date: 2012-09-26
ZHEJIANG HONGSHENG CHEM IND +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is inhomogeneity in the mixing area of ​​the mechanical stirring mixer. In order to fully mix two or more liquid materials in the shortest time, the mixing intensity must be increased. The increase in the mixing intensity will inevitably lead to excessive external input energy consumption.
In order to ensure the use of subsequent processes, intermittent batching needs to be equipped with two sets of batching devices or a set of large-volume batching devices and storage containers at the same time, which will lead to long storage time of hydrolyzed materials, increased decomposition of raw materials, and reduced reaction yield and product quality.

Method used

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  • Process for producing resorcinol by continuously hydrolyzing m-phenylenediamine
  • Process for producing resorcinol by continuously hydrolyzing m-phenylenediamine
  • Process for producing resorcinol by continuously hydrolyzing m-phenylenediamine

Examples

Experimental program
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Effect test

Embodiment 1

[0049] The hydrolysis reaction and batching system use nitrogen to replace the air in the system device.

[0050] Continuously convey metered 98% sulfuric acid, molten m-phenylenediamine and demineralized water (or distilled water) with a booster pump, wherein, 98% sulfuric acid and water pass through a first-stage pipeline mixer to prepare 12% dilute sulfuric acid, dilute sulfuric acid Prepare m-phenylenediamine sulfate solution with m-phenylenediamine by secondary pipeline mixer, the flow of m-phenylenediamine, 98% sulfuric acid, water are respectively 0.77kg / min, 2.075kg / min, 10.21kg / min, determine The molar ratio of m-phenylenediamine, sulfuric acid and water is 1:2.0:60.

[0051] Hydrolysis using 2m 3 A tower reactor with an aspect ratio of 4.2 and five baffles inside. The m-phenylenediamine sulfate aqueous solution prepared by metering and pressurizing m-phenylenediamine, sulfuric acid and water is heated to 237°C through a heat exchanger, and then continuously pressed...

Embodiment 2

[0054] According to the method described in Example 1, the difference is that the molar ratio of m-phenylenediamine, sulfuric acid, and water is 1:1.8:80, the hydrolysis reaction temperature is 242° C., and the hydrolysis reaction residence time is 135 minutes. The product purity is 99.4%, and the yield is 90.0%.

Embodiment 3

[0056] According to the method described in Example 1, the difference is that the molar ratio of m-phenylenediamine, sulfuric acid, and water is 1:2:100, the hydrolysis reaction temperature is 230° C., and the hydrolysis reaction residence time is 200 minutes. The product purity is 99.5%, and the yield is 91.2%.

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Abstract

The invention discloses a process for producing resorcinol by continuously hydrolyzing m-phenylenediamine. The devices adopted by the process include a pipe mixer, a heat exchanger and a tower reactor, wherein baffle plates are distributed in the tower reactor from top down and the external wall of the tower reactor is provided with a heating pipe coil. The process comprises the following steps: 1, continuously preparing a hydrolysis raw material by using the pipe mixer to form homogeneous aqueous solution of m-phenylenediamine sulfate; 2, preheating the aqueous solution of m-phenylenediaminesulfate to 225 to 245 DEG C by the heat exchanger, continuously filling the aqueous solution of m-phenylenediamine sulfate to the tower reactor from the top part of the tower reactor, keeping the reaction and retention time of the reaction material in the tower reactor between 120 and 240 minutes, and performing continuous hydrolysis reaction; and 3, performing post-processing step of the hydrolysis reaction solution obtained by the hydrolysis reaction to obtain the resorcinol. The process has the characteristics of high equipment efficiency, short production period, high product yield, stable product quality and simple and convenient process control.

Description

(1) Technical field [0001] The invention relates to a process for producing resorcinol by continuous hydrolysis of m-phenylenediamine. (2) Background technology [0002] Resorcinol (Resorcinol), commonly known as Resorcinol, also known as 1,3-benzenediol, is an important organic chemical raw material, widely used in pesticides, dyes, paints, medicines, plastics, rubber, electronic chemicals It is mainly used in the preparation of impregnating agents for tire cords, adhesive resins for synthetic rubber, high-performance adhesives for wood plywood, synthetic benzophenone UV absorbers, m-aminophenol, etc. [0003] At present, the routes of industrial synthesis of resorcinol mainly include the sulfonation alkali fusion method using benzene as raw material, the oxidation method using m-dicumene as raw material, and the hydrolysis method of m-phenylenediamine. Domestically, the sulfonated alkali fusion method using benzene as raw material is mainly used. Due to the process and eq...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/08C07C37/05
Inventor 何旭斌王新武陶建国孟明朱敬鑫张桂香
Owner ZHEJIANG HONGSHENG CHEM IND
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