A production method for improving the yield and purity of dimethyl isophthalate-5-sulfonic acid for synthesizing three monomers

A technology of dimethyl isophthalate and isophthalic acid is applied in the synthesis field of intermediate dimethyl isophthalate-5-sulfonic acid, and can solve the problems of high reaction temperature, high content, low purity and the like , to reduce the consumption of methanol, improve the reaction speed, and improve the economic benefits.

Active Publication Date: 2021-06-22
SHANDONG FIRST MEDICAL UNIV & SHANDONG ACADEMY OF MEDICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] In view of the low yield, low purity, high reaction temperature, long reaction time and large amount of methanol used in the existing production of dimethyl isophthalate-5-sulfonic acid in China, resulting in the cost of the three monomers of the final product High, many types of impurities and high content, the present invention has carried out in-depth research and optimization on the existing process, forming a new synthetic process

Method used

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  • A production method for improving the yield and purity of dimethyl isophthalate-5-sulfonic acid for synthesizing three monomers
  • A production method for improving the yield and purity of dimethyl isophthalate-5-sulfonic acid for synthesizing three monomers
  • A production method for improving the yield and purity of dimethyl isophthalate-5-sulfonic acid for synthesizing three monomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The weight of the sulfonated material used in this embodiment is 1670Kg, and the main component content (weight ratio) of the sulfonated material is as follows: isophthalic acid-5-sulfonic acid, 76.59%; isophthalic acid, 0.054%; sulfuric acid, 16.11%; SO 3 , 4.06%; the rest are sulfonated organic impurities and impurities brought in by raw materials.

[0057] 1. N 2 Gas purge

[0058] use N 2 The esterification kettle is purged with gas, and N 2 Adjust the pressure of the esterification kettle to 0.015 MPa to stop N 2 Through.

[0059] 2. Add sulfonated material

[0060] Add the sulfonated material to the esterification kettle.

[0061] 3. Add part of methanol

[0062] Put 700Kg of methanol into the methanol metering tank with a pump, and put 280Kg of methanol into the esterification kettle from the bottom of the esterification kettle with a plunger pump. After the methanol feeding is stopped, the agitator is turned by manual cranking, and then the motor switch ...

Embodiment 2

[0076] The weight of the sulfonated material used in this embodiment is 1675Kg, and the main component content (weight ratio) of the sulfonated material is as follows: isophthalic acid-5-sulfonic acid, 76.59%; isophthalic acid, 0.054%; sulfuric acid, 16.11%; SO 3 , 4.06%; the rest are sulfonated organic impurities and impurities brought in by raw materials. 1. N 2 Gas purge

[0077] use N 2 The esterification kettle is purged with gas until the pressure of the esterification kettle reaches 0.025 MPa to stop N 2 Through.

[0078] 2. Add sulfonated material

[0079] Add the sulfonated material to the esterification kettle.

[0080] 3. Add part of methanol

[0081] Use a pump to pump 735Kg methanol into the methanol metering tank, and use a plunger pump to pump 355Kg methanol into the esterification kettle from the bottom of the esterification kettle. After the methanol feeding is stopped, the agitator is turned by manual cranking, and then the motor switch of the agitator...

Embodiment 3

[0096] The weight of the sulfonated material used in this embodiment is 1680Kg, and the main component content (weight ratio) of the sulfonated material is as follows: isophthalic acid-5-sulfonic acid, 76.59%; isophthalic acid, 0.054%; sulfuric acid, 16.11%; SO 3 , 4.06%; the rest are sulfonated organic impurities and impurities brought in by raw materials. 1. N 2 Gas purge

[0097] use N 2 The esterification kettle is purged with gas until the pressure of the esterification kettle reaches 0.04 MPa to stop N 2 Through.

[0098] 2. Add sulfonated material

[0099] Add the sulfonated material to the esterification kettle.

[0100] 3. Add part of methanol

[0101] Put 760Kg of methanol into the methanol metering tank with a pump, and put 310Kg of methanol into the kettle from the bottom of the esterification kettle with a plunger pump. After the methanol feeding is stopped, the agitator is turned by manual cranking, and then the motor switch of the agitator is jogged, and ...

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Abstract

The invention provides a kind of production method that improves three monomer synthesis dimethyl isophthalate-5-sulfonic acid yield and purity, described production method, comprises N 2 Gas purging, adding sulfonated material, adding part of methanol, temperature rise and pressure reaction, adding remaining methanol and catalyst, step temperature rise reaction. The invention reduces the unit consumption of methanol and improves the economic benefits of the product; equivalent to 413-439Kg of methanol consumed per ton of three monomers; the feed amount of methanol is 20% less than that of the existing process; the unit consumption of methanol per ton of three monomers is lower than that of the existing process more than 30%; the purity of dimethyl isophthalate-5-sulfonic acid exceeds 96%, reaching 96.85-97.05%, and the yield exceeds 97%, reaching 97.18-97.42%; the subsequent production of the three-monomer product The rate exceeds 84%; the reaction time is shortened; the esterification reaction operation cycle is shortened by 2 hours compared with the existing production process.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and is especially suitable as an important intermediate for synthesizing dimethyl isophthalate-5-sodium sulfonate (commonly known as: three monomers, English abbreviated as SIPM) with isophthalic acid as the starting material Synthesis of dimethyl isophthalate-5-sulfonic acid. Background technique [0002] The synthesis of three monomers with isophthalic acid as the starting material has been produced for decades at home and abroad. The production process is basically divided into the following types: (1) Isophthalic acid is first sulfonated, and then esterified and neutralized , refined, and dried to obtain SIPM, in which the sulfonating agent used is SO 3 , different concentrations of oleum, etc.; the neutralizer used is Na 2 CO 3 , NaOH, sodium sulfite, etc.; (2) esterification sulfonation method, isophthalic acid is first esterified with methanol to produce dimethyl isophthalate,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/22C07C309/58
CPCC07C303/22C07C309/58
Inventor 杨荣华张秀玲汪海李忠浩
Owner SHANDONG FIRST MEDICAL UNIV & SHANDONG ACADEMY OF MEDICAL SCI
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