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Preparation method of isophthalic acid

A technology of isophthalic acid and m-xylene, which is applied in the field of preparation of isophthalic acid, can solve problems such as difficult control of oxygen partial pressure and air intake, oxygen content safety risk and combustion side reactions, etc., to reduce combustion side effects Reaction, increased operational safety, enhanced catalytic activity and selectivity effects

Inactive Publication Date: 2018-04-27
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the difficulty in controlling the oxygen partial pressure and air intake in the prior art, and the resulting oxygen content in the tail gas is either too large to cause safety risks, or too small to cause serious combustion side reactions. And provide a kind of preparation method of isophthalic acid

Method used

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  • Preparation method of isophthalic acid
  • Preparation method of isophthalic acid
  • Preparation method of isophthalic acid

Examples

Experimental program
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Effect test

Embodiment 1A

[0041] Mix m-xylene, acetic acid, water, cobalt acetate, manganese acetate, and hydrobromic acid evenly according to a certain ratio, and then pump them into the oxidation reaction kettle. At the beginning of the experiment, the rotating speed of the stirring paddle and the temperature of the heating jacket were set. At the same time, the O 2 , CO 2 , N 2 According to a certain ratio, the gas mixture is introduced into the reactor to initiate the oxidation reaction. The oxidation reaction conditions are that the rotation speed of the stirring blade is 800ppm, the temperature is 180°C, the reaction pressure is 2.0MPa, the reaction time is 90min based on the average residence time of the solvent, the mass ratio of the feed solvent to m-xylene is 10:1, and the H 2 O / HAc=5%, in terms of ion concentration, the catalyst concentration Co is 800ppm, Mn is 400ppm, Br is 1200ppm, and O in the gas mixture 2 The content is 17.9%, N 2 The content is 67.4%, CO 2 The content is 14.7%. ...

Embodiment 2A

[0043] Mix m-xylene, acetic acid, water, cobalt acetate, manganese acetate, and hydrobromic acid evenly according to a certain ratio, and then pump them into the oxidation reaction kettle. At the beginning of the experiment, the rotating speed of the stirring paddle and the temperature of the heating jacket were set. At the same time, the O 2 , CO 2 , N 2 According to a certain ratio, the gas mixture is introduced into the reactor to initiate the oxidation reaction. The oxidation reaction conditions are that the rotation speed of the stirring blade is 800ppm, the temperature is 180°C, the reaction pressure is 2.0MPa, the reaction time is 90min based on the average residence time of the solvent, the mass ratio of the feed solvent to m-xylene is 10:1, and the H 2 O / HAc=5%, in terms of ion concentration, the catalyst concentration Co is 800ppm, Mn is 400ppm, Br is 1200ppm, and O in the gas mixture 2 The content is 12.6%, N 2 The content is 47.4%, CO 2 The content is 40.0%. ...

Embodiment 3A

[0045] Mix m-xylene, acetic acid, water, cobalt acetate, manganese acetate, and hydrobromic acid evenly according to a certain ratio, and then pump them into the oxidation reaction kettle. At the beginning of the experiment, the rotating speed of the stirring paddle and the temperature of the heating jacket were set. At the same time, the O 2 , CO 2 , N 2 According to a certain ratio, the gas mixture is introduced into the reactor to initiate the oxidation reaction. The oxidation reaction conditions are that the rotation speed of the stirring blade is 800ppm, the temperature is 180°C, the reaction pressure is 2.0MPa, the reaction time is 90min based on the average residence time of the solvent, the mass ratio of the feed solvent to m-xylene is 10:1, and the H 2 O / HAc=5%, in terms of ion concentration, the catalyst concentration Co is 800ppm, Mn is 400ppm, Br is 1200ppm, and O in the gas mixture 2 The content is 8.4%, N 2 The content is 31.6%, CO 2 The content is 60.0%. T...

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Abstract

The invention discloses a preparation method of isophthalic acid. The preparation method comprises the steps of: in an m-xylene oxidation system, subjecting m-xylene to primary oxidation reaction to obtain isophthalic acid; wherein the m-xylene oxidation system includes a catalyst, an oxidizing agent and a solvent, the catalyst is Co-Mn-Br catalyst, the oxidizing agent contains, by volume percent,5-21% of O2, 0.04%-79% of CO2, and N2, and the oxygen partial pressure in the tail gas is 1.21%-6% at the end of the primary oxidation. The preparation method provided by the invention is conducive to the formation of active peroxy carbonic ester, can effectively accelerate the reaction speed, weaken combustion side reaction, and control the O2 content of the tail gas within a safety range, and increases the operation safety of the reaction.

Description

technical field [0001] The present invention relates to a kind of preparation method of isophthalic acid. Background technique [0002] A series of commercial oxidized compounds usually use air or oxygen to directly oxidize petroleum or natural gas derivatives, such as the oxidation of toluene to produce benzaldehyde and benzoic acid, the oxidation of p-xylene to produce terephthalic acid and cumene phenol, m-xylene ( MX) oxidation to produce isophthalic acid (IPA), etc. This oxidation usually occurs in the presence of air or oxygen to form peroxides and hydroxides. In addition, as an autoxidation reaction, an oxidation reaction occurs even under low temperature conditions. [0003] Generally speaking, MX oxidation is directly related to the oxygen content in the liquid phase. Within a certain limit, the greater the oxygen partial pressure, it means that under a certain air flow, more bubbles are sealed below the liquid surface, which is conducive to the reaction. speed i...

Claims

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Application Information

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IPC IPC(8): C07C51/265C07C51/487C07C63/24B01J31/04B01J31/22
CPCB01J31/04B01J31/2239C07C51/265C07C51/487C07C63/24
Inventor 孙伟振赵玲吕全明董健
Owner EAST CHINA UNIV OF SCI & TECH