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A method for neutralizing an esterified material containing dimethyl isophthalate-5-sulfonic acid to prepare a three-monomer

A technology of dimethyl isophthalate and isophthalic acid, which is applied in the field of organic synthesis, can solve the problems of high cost of three monomers, many impurities, many side reactions, etc., so as to improve the economic benefit of the product and simplify the operation. process, the effect of shortening the reaction time

Active Publication Date: 2021-06-18
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

[0015] Aiming at the low conversion rate of dimethyl isophthalate-5-sulfonic acid, many side reactions, and the yield of finished tri-monomer in the existing neutralization process of synthesizing the three-monomer by neutralizing the esterification material with lye Not high, long reaction time, high cost of the final product three monomers, low purity, large number and high content of impurities, etc., the present invention improves the existing process and forms a new production process

Method used

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  • A method for neutralizing an esterified material containing dimethyl isophthalate-5-sulfonic acid to prepare a three-monomer
  • A method for neutralizing an esterified material containing dimethyl isophthalate-5-sulfonic acid to prepare a three-monomer
  • A method for neutralizing an esterified material containing dimethyl isophthalate-5-sulfonic acid to prepare a three-monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] The weight of the esterification material used in this example is 2285kG, and the contents (weight ratio) of each main component of the esterification material are as follows: dimethyl isophthalate-5-sulfonic acid, 80.21%; monomethyl isophthalate-5- Sulfonic acid, 1.32%; isophthalic acid, 0.053%; sulfuric acid, 15.51%; methanol, 12.45%; the rest are sulfonated organic impurities, esterified organic impurities and impurities brought in by raw materials.

[0051] 1. Add process water and esterification material

[0052] First add 4920Kg of measured process water to the neutralization tank, start stirring, feed cooling water into the jacket of the first neutralization tank, and put all the esterified materials in the esterification tank into the first neutralization tank.

[0053] 2. Add part of soda ash

[0054] When the temperature of the material in the first neutralization tank drops to 18°C, start the screw feeder and start adding solid soda ash to the neutralization...

Embodiment 2

[0066] The weight of the esterification material used in this example is 2285kG, and the contents (weight ratio) of each main component of the esterification material are as follows: dimethyl isophthalate-5-sulfonic acid, 80.21%; monomethyl isophthalate-5- Sulfonic acid, 1.32%; isophthalic acid, 0.053%; sulfuric acid, 15.51%; methanol, 12.45%; the rest are sulfonated organic impurities, esterified organic impurities and impurities brought in by raw materials.

[0067] With the process parameter of embodiment 1, steps 1-3 are identical, and different operation is in step 4.

[0068] Step 4. When the total amount of soda ash added is 570Kg, the online digital display pH meter shows that the pH value of the neutralization material is 6.9, and continue to add 35Kg of soda ash to the neutralization kettle. At this time, the pH value data shows 7.0, and it can be sampled after about 10 minutes after stabilization , the saponification value of the rapid analysis sample sample (liquid...

Embodiment 3

[0075] The weight of the esterification material used in this embodiment is 2360kG, and the content (weight ratio) of each main component of the esterification material is as follows: dimethyl isophthalate-5-sulfonic acid, 80.78%; monomethyl isophthalate-5- Sulfonic acid, 1.02%; isophthalic acid, 0.047%; sulfuric acid, 14.72%; methanol, 11.48%; the rest are sulfonated organic impurities, esterified organic impurities and impurities brought in by raw materials.

[0076] 1. Add process water and esterification material

[0077] First add 5200Kg of measured process water to the neutralization tank, start stirring, pass cooling water into the jacket of the first neutralization tank, and put all the esterified materials in the esterification tank into the first neutralization tank.

[0078] 2. Add part of soda ash

[0079] When the temperature of the material in the first neutralization tank drops to 20°C, start the screw feeder and start adding solid soda ash to the neutralizatio...

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Abstract

The invention provides a method for neutralizing an esterification material containing dimethyl isophthalate-5-sulfonic acid to prepare a three-monomer, the method comprising adding process water and esterification material, adding part of soda ash, and transferring , Control of the reaction end point. In the application of industrial devices, the conversion rate of isophthalic acid-dimethyl 5-sulfonic acid exceeds 97%, reaching 97.15-97.65%, and the yield of the three monomer crude products in the neutralization process (based on dimethyl isophthalate ‑5‑sulfonic acid) is 96.09‑96.77%, and the yield of the three-monomer product prepared by the subsequent refining and drying process exceeds 84%; the neutralization reaction cycle is shortened to 435‑475min; due to the effective control of the neutralization end point and the combination of other Neutralize process parameters, reduce side reactions, especially reduce the amount of monomethyl isophthalate-5-sodium sulfonate that is hydrolyzed into the finished product of the three monomers, and the quantity and amount of other by-products are all reduced.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and is especially suitable for using an inorganic basic compound to neutralize the esterification product in the production process of a trimonomer (chemical name: dimethyl isophthalate-5-sodium sulfonate, abbreviated as SIPM). (based on dimethyl isophthalate-5-sulfonic acid) to prepare the three-monomer process. Background technique [0002] The existing three-monomer production process, no matter which process route is adopted, uses dimethyl isophthalate-5-sulfonic acid, the main component in the esterification material, as the starting material, and prepares the three-monomer by neutralization with lye It is a necessary operation step in the production process. The alkali used generally includes soda ash, sodium hydroxide, sodium sulfite, etc. Due to the inevitable occurrence of numerous side reactions during the synthesis of dimethyl isophthalate-5-sulfonic acid, there is a certain...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/32C07C309/58
CPCC07C303/32C07C309/58
Inventor 杨荣华张秀玲徐昊彤陈永政
Owner SHANDONG FIRST MEDICAL UNIV & SHANDONG ACADEMY OF MEDICAL SCI