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Method for continuously preparing sulfonated product of benzene series by microreaction device

A micro-reaction device and technology of benzene series, applied in chemical instruments and methods, sulfonic acid preparation, chemical/physical/physicochemical processes, etc., can solve the problems of severe direct sulfonation reaction of benzene and its derivatives, over-sulfonation, etc. , to achieve the effects of reducing the production of by-product sulfone and benzene disulfonic acid, complete reaction and simple refining process

Active Publication Date: 2018-03-23
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Purpose of the invention: In order to solve the problem of using SO in the prior art 3 For the problems of severe direct sulfonation reaction and oversulfonation of benzene and its derivatives, the present invention provides a method for continuously preparing sulfonated products of benzene series by using a micro-reaction device

Method used

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  • Method for continuously preparing sulfonated product of benzene series by microreaction device
  • Method for continuously preparing sulfonated product of benzene series by microreaction device
  • Method for continuously preparing sulfonated product of benzene series by microreaction device

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Experimental program
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Effect test

Embodiment 1

[0038] See microreaction device figure 1 , Benzene was pumped into the Corning reactor through a liquid feed pump at a flow rate of 5 mL / min. Meanwhile, open SO 3 Adjust the gas valve to adjust the pressure reducing valve to control the flow rate to 1.25L / min. Adjust the air valve so that the volume percentage of sulfur trioxide in the mixed gas is 6%, and the mixed gas is obtained by mixing the gas mixer, and the benzene and the mixed gas are respectively passed through the liquid preheater After preheating to 20°C with the gas preheater, it enters the reaction plate in the Corning reactor and mixes for reaction. Benzene and SO 3 The molar ratio is 1:1, the residence time in the heart-shaped reaction plate is 13min, and the backpressure value of the backpressure valve is set to 8bar. After the reaction was completed, the reaction solution was collected, cooled to room temperature, and the solid was collected by filtration. The solid was dissolved in water, the solid was fi...

Embodiment 2

[0040] Method is with embodiment 1, and difference is that benzene flow rate is 10ml / min, SO 3 The gas flow rate is 2.5ml / min, the residence time in the heart-shaped reaction plate is 6.5min, and the yield of refined benzenesulfonic acid is 93.4%.

Embodiment 3

[0042] Method is with embodiment 1, and difference is that benzene flow rate is 15ml / min, SO 3 The gas flow rate is 3.75ml / min, the residence time in the heart-shaped reaction plate is 4.0min, and the yield of refined benzenesulfonic acid is 92.1%.

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Abstract

The invention discloses a method for continuously preparing a sulfonated product of benzene series by a microreaction device. The method comprises following steps: (1), SO3 gas and air are mixed, andmixed gas is obtained; (2), liquid benzene series and the mixed gas are pumped into microreactors in the microreaction device respectively for a sulfonation reaction, and a reaction liquid is obtained; (3), the reaction liquid is subjected to solid-liquid separation after being cooled to the room temperature, solids are collected, and a crude product is obtained; 3), the crude product obtained inthe step (3) is dissolved in water, insoluble substances are removed, and the sulfonated product is obtained. The sulfonated product of the benzene series is prepared by the microreaction device, reaction conditions are milder, reaction rate can be effectively controlled and reaction time can be effectively shortened, so that continuous production is realized, byproducts such as sulfone and benzene disulfonic acid are reduced, the highest yield can reach 99.1%, the refining process is simpler, and product quality is improved; amplification effect is avoided basically, and industrial amplification is facilitated.

Description

technical field [0001] The invention relates to sulfonation of benzene and derivatives thereof, in particular to a method for continuously preparing sulfonation products of benzene series by using a micro-reaction device. Background technique [0002] The sulfonated products of benzene and its derivatives are an important raw material of organic compounds. It is a very important organic chemical intermediate, widely used in the dye industry, pharmaceutical industry, agricultural industry, etc. The traditional sulfonation technology mainly uses concentrated sulfuric acid azeotropic or fuming sulfuric acid. The disadvantage is that the reaction process is too violent and a large amount of waste acid is produced, which pollutes the environment. With the development of sulfonation technology, more and more attention has been paid to sulfur trioxide as a green sulfonating agent that is clean, pollution-free and of good product quality. The development and application of sulfur t...

Claims

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Application Information

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IPC IPC(8): C07C303/06C07C309/29C07C309/30C07C309/36C07C309/38B01J19/00
CPCB01J19/0093C07C303/06C07C309/29C07C309/30C07C309/36C07C309/38
Inventor 郭凯郑明卫万力袁鑫
Owner NANJING UNIV OF TECH
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