Unlock instant, AI-driven research and patent intelligence for your innovation.

A production method for increasing the yield of isophthalic acid-5-sulfonic acid for synthesizing three monomers

A technology of isophthalic acid and a production method, which is applied in the field of synthesis of an intermediate isophthalic acid-5-sulfonic acid, can solve the problems of unreasonable ratio of raw materials, high cost of three monomers, and high reaction temperature, and achieves reduction of Sulfur trioxide loss, reduced process dosage, good repeatability

Active Publication Date: 2021-04-16
SHANDONG FIRST MEDICAL UNIV & SHANDONG ACADEMY OF MEDICAL SCI +1
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] For the synthesis of isophthalic acid-5-sulfonic acid from isophthalic acid and oleum in China, the yield is low, the reaction temperature is high, the reaction time is long, and the ratio of raw materials is unreasonable, resulting in high cost of the final product three monomers , high impurity content, etc., the present invention conducts in-depth research on material ratio, reaction temperature and time, etc., optimizes the existing process, and forms a new process

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A production method for increasing the yield of isophthalic acid-5-sulfonic acid for synthesizing three monomers
  • A production method for increasing the yield of isophthalic acid-5-sulfonic acid for synthesizing three monomers
  • A production method for increasing the yield of isophthalic acid-5-sulfonic acid for synthesizing three monomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Embodiment 1 A kind of production method that improves three monomer synthesis isophthalic acid-5-sulfonic acid yields

[0071] Include the following steps:

[0072] (1) Feeding

[0073] Material ratio: 1900 kg of isophthalic acid; 1620 kg of 65% oleum; the reaction is carried out in a 3000L glass-lined kettle;

[0074] Measure 1620 kg of fuming sulfuric acid into the high-level tank, put 1300 kg of fuming sulfuric acid into the sulfonation tank, and start stirring; add 1900 kg of isophthalic acid into the sulfonation tank within 60 minutes.

[0075] (2) filled with nitrogen

[0076] After the addition of isophthalic acid is completed, nitrogen is charged into the sulfonation tank. When the nitrogen pressure reaches 0.01MPa, the nitrogen addition valve is closed and the temperature rises.

[0077] (3) The first stage heating reaction

[0078] Within 40 minutes, the temperature of the sulfonation kettle was raised from normal temperature to 120° C., and the reaction ...

Embodiment 2

[0091] Embodiment 2 A kind of production method that improves three monomer synthesis isophthalic acid-5-sulfonic acid yields

[0092] Include the following steps:

[0093] (1) Feeding

[0094] Ratio of materials: 1925 kg of isophthalic acid; 1645 kg of 65% oleum; the reaction is carried out in a 3000L glass-lined kettle.

[0095] Measure 1645 kg of fuming sulfuric acid into the high-level tank, put 1320 kg of fuming sulfuric acid into the sulfonation tank, and start stirring; add 1925 kg of isophthalic acid into the sulfonation tank within 50 minutes.

[0096] (2) filled with nitrogen

[0097] After the addition of isophthalic acid is completed, nitrogen is charged into the sulfonation tank. When the nitrogen pressure reaches 0.01MPa, the nitrogen addition valve is closed and the temperature rises.

[0098] (3) The first stage heating reaction

[0099] In the first stage, the temperature of the sulfonation tank was raised from normal temperature to 122°C within 50 minutes...

Embodiment 3

[0112] Embodiment 3 A kind of production method that improves three monomer synthesis isophthalic acid-5-sulfonic acid yields

[0113] Include the following steps:

[0114] (1) Feeding

[0115] Ratio of materials: 1950 kg of isophthalic acid; 1660 kg of 65% oleum; the reaction is carried out in a 3000L glass-lined kettle.

[0116] Measure 1660 kg of fuming sulfuric acid into the high-level tank, put 1330 kg of fuming sulfuric acid into the sulfonation tank, and start stirring; add 1950 kg of isophthalic acid into the sulfonation tank within 60 minutes.

[0117] (2) filled with nitrogen

[0118] After the addition of isophthalic acid is completed, nitrogen is charged into the sulfonation kettle. When the nitrogen pressure reaches 0.012MPa, the nitrogen addition valve is closed to start heating.

[0119] (3) The first stage heating reaction

[0120] In the first stage, the temperature of the sulfonation tank was raised from normal temperature to 124° C. within 60 minutes, an...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
wavelengthaaaaaaaaaa
volumeaaaaaaaaaa
Login to View More

Abstract

The present invention provides a kind of production method that improves the yield of isophthalic acid-5-sulfonic acid for the synthesis of three monomers, it is characterized in that: described production method comprises feeding, charging into nitrogen, the first stage heating reaction, the second Stage temperature rise reaction, adding remaining fuming sulfuric acid, third stage temperature rise reaction, negative pressure reaction. The beneficial effects obtained by the present invention are shortening the reaction time and lowering the reaction temperature; compared with the existing production process, the maximum reaction temperature is reduced by 30°C, and the sulfonation reaction cycle is shortened by 2 hours; Overall product economic benefits; the amount of fuming sulfuric acid is reduced, which is 5% less than that of the existing process, which can reduce the amount of alkali used in the subsequent neutralization process by more than 5%, and at the same time shorten the reaction time of the neutralization process and reduce the amount of cooling water. The energy saving effect is remarkable. ; Improve the yield of isophthalic acid-5-sulfonic acid.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to the synthesis of isophthalic acid-5-sulfonic acid, an important intermediate when isophthalic acid is used as a starting material to synthesize a trimonomer. Background technique [0002] Using isophthalic acid as the starting material to synthesize the three monomers (chemical name: dimethyl isophthalate-5-sodium sulfonate, abbreviated as SIPM), the production methods are basically divided into There are the following types: (1) sulfonic acid crystallization method, sulfonate isophthalic acid with sulfur trioxide or oleum, and then dilute the sulfonated mother liquor with ice water to a sulfuric acid mass fraction of 50%-70%, The sulfonic acid is crystallized, and then the excess waste acid is removed, and excess methanol is used for esterification, and then neutralized and refined to obtain SIPM; (2) Esterification and sulfonation method, isophthalic acid ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/06C07C309/58
CPCC07C303/06C07C309/58
Inventor 杨荣华张秀玲杨明晖陈丙瑞王建亮倪文龙郭祥荣刘梅
Owner SHANDONG FIRST MEDICAL UNIV & SHANDONG ACADEMY OF MEDICAL SCI