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Production method of 2-acrylamide-2-methylpropanesulfonic acid

A technology based on methylpropanesulfonic acid and acrylamide, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low purity and yield of AMPS products, affecting product preparation, and low work efficiency , to achieve the effect of reducing the length of the synthesis process, improving the synthesis efficiency, and improving the purity and yield

Active Publication Date: 2014-03-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since acrylonitrile is greatly added in excess relative to the sulfonating agent, in order to minimize the content of acrylonitrile in the filter cake containing 2-acrylamido-2-methylpropanesulfonic acid, it is necessary to vacuum the filter cake obtained after filtration. Drying to prevent the acrylonitrile entrained in the filter cake from being brought into the subsequent AMPS refining process for polymerization, thus affecting the product preparation of AMPS
In this method, in order to realize the effective removal of acrylonitrile entrained in the filter cake, the time of vacuum drying is often as long as 3-5 hours, the operation period is long, the work efficiency is low, and the purity and yield of the obtained AMPS product are on the low side

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach

[0019] According to the present invention, although the present invention has no special requirements on the mode and times of washing the filter cake containing 2-acrylamido-2-methylpropanesulfonic acid in the step (4), the glacial acetic acid can be continuously Wash the filter cake containing 2-acrylamido-2-methylpropanesulfonic acid, or wash the filter cake containing 2-acrylamido-2-methylpropanesulfonic acid several times with glacial acetic acid. In one embodiment, the method of washing the filter cake containing 2-acrylamido-2-methylpropanesulfonic acid obtained in step (3) with glacial acetic acid in step (4) is intermittent washing. The intermittent flushing is that the glacial acetic acid used to wash the filter cake containing 2-acrylamido-2-methylpropanesulfonic acid is not a continuous flushing. After flushing with part of the glacial acetic acid, it needs to be filtered, and then use part of the glacial acetic acid to rinse. Wash with glacial acetic acid. Rinse ...

Embodiment 1

[0031] This example is used to illustrate the production method of 2-acrylamido-2-methylpropanesulfonic acid provided by the present invention.

[0032] (1) Add 330g of acrylonitrile to a four-necked flask equipped with a temperature control device, a stirrer, a thermometer and a gas feeding device, cool the acrylonitrile to -10°C, add 61g of 102% by weight fuming sulfuric acid, and add During the process and after the addition, the temperature was maintained at -10 ° C and continued to stir for 1 hour to form an acrylonitrile solution of the sulfonating agent;

[0033] (2) After the temperature is raised to 38°C, 35g of isobutene is introduced for reaction. After the introduction of isobutene is completed, the reaction is completed after 1 hour of heat preservation, and a slurry product is obtained;

[0034](3) Vacuum filter the slurry product obtained in step (2) to obtain 180 g of filter cake containing 2-acrylamido-2-methylpropanesulfonic acid;

[0035] (4) Use 360g of gl...

Embodiment 2

[0041] Synthesize 2-acrylamido-2-methylpropanesulfonic acid according to the method of Example 1, the difference is that in step (4), 440g of glacial acetic acid is used to continuously wash the filter cake and then filter, and glacial acetic acid is mixed with 2 -The mass ratio of the filter cake of acrylamido-2-methylpropanesulfonic acid is 2:1, and the time of washing and filtering is 15 minutes. The other steps are the same. In the high-purity AMPS obtained, the purity is 99.3% by weight, the total The yield is 85%.

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Abstract

The invention discloses a production method of 2-acrylamide-2-methylpropanesulfonic acid. The method comprises the steps of (1) mixing acrylonitrile with a sulfonating agent to form an acrylonitrile solution of the sulfonating agent; (2) enabling the acrylonitrile solution of the sulfonating agent, obtained in the step (1), to be in contact with isobutylene to form a pasty product; (3) filtering the pasty product to obtain a filter cake containing 2-acrylamide-2-methylpropanesulfonic acid; (4) washing the filter cake containing the 2-acrylamide-2-methylpropanesulfonic acid, obtained in the step (3), by using glacial acetic acid, thereby obtaining an AMPS crude product. By adopting the method, the synthesis time of the 2-acrylamide-2-methylpropanesulfonic acid can be effectively reduced, the synthesis efficiency is improved, and the cost is reduced. Moreover, the obtained product is high in yield and purity.

Description

technical field [0001] The invention relates to a production method of 2-acrylamido-2-methylpropanesulfonic acid. Background technique [0002] 2-acrylamide-2-methylpropanesulfonic acid (2-acrylamide-2-methylpropanesulfonic acid, hereinafter referred to as AMPS) is a multifunctional water-soluble anionic monomer, due to its molecular structure has carbon-carbon double bonds and is insensitive to salt The sulfonic acid group is easy to polymerize, and its homopolymer and copolymer have many special properties, which have broad application prospects and can be widely used in oilfield chemistry, water treatment agents, chemical fibers, plastics, printing and dyeing, coatings, and surfactants , antistatic agent, ceramics, photography, detergent additives, ion exchange resin, gas separation membrane, electronics industry and other fields. [0003] At present, the most typical process for producing AMPS is to prepare AMPS by reacting acrylonitrile, oleum and isobutylene under rel...

Claims

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Application Information

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IPC IPC(8): C07C309/15C07C303/44
Inventor 李斗星黄凤兴齐兰芝贾春革穆晓蕾
Owner CHINA PETROLEUM & CHEM CORP
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