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Method for producing tert-butyl acryloyl sulfonic acid

A technology of tert-butylacrylamide sulfonic acid and tert-butylacryloyl sulfonic acid is applied in the preparation of sulfonic acid, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of local reaction temperature increase, impurity difficulty and the like , to achieve the effect of reducing by-products, improving economic benefits and reducing by-products

Inactive Publication Date: 2018-05-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the existing AMPS synthesis process, the mixing of acrylonitrile and sulfuric acid and the addition of isobutylene are all exothermic processes, which can easily increase the local reaction temperature, making the control of impurities difficult.

Method used

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  • Method for producing tert-butyl acryloyl sulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The reaction is carried out in a small reactor with two external circulation devices, and both the first external circulation device and the second external circulation device have temperature control systems. The reactor has a stirring and temperature control system. There are circulation pumps in the first external circulation device and the second external circulation device so that the concentration in the entire external circulation device is in a relatively uniform state. In the first external circulation device, first add acrylonitrile to almost fill the circulation device, and adjust the temperature to -5°C. At the same time, in the second external circulation device, first add acrylonitrile to make it almost fill the circulation device, and adjust the temperature to 30°C. The temperature in the reaction kettle was adjusted to 40°C, and materials were started to be added to the external circulation device. The feed rate of the first part of acrylonitrile is 20...

Embodiment 2

[0032]The difference from Example 1 is that during the preparation of the crude AMPS, the temperature of the reactor was changed to 20°C. The yield of crude AMPS obtained was 90.2%. Randomly take out ten batches of crude AMPS from the continuously produced samples and use 10% acetic acid aqueous solution to recrystallize to obtain high-purity AMPS with a purity of 99.2-99.4%, and the mass content of tert-butylpropenesulfonic acid is 110-115ppm .

Embodiment 3

[0034] The difference from Example 1 is that the addition rate of the first part of acrylonitrile is 280g / h, the addition rate of the second part of acrylonitrile is 100g / h, the addition rate of sulfuric acid is 61g / h, and the addition rate of isobutylene is 35g / h. The yield of crude AMPS obtained was 91.3%. Randomly take out ten batches of crude AMPS from the continuous production samples and use 10% acetic acid aqueous solution to recrystallize to obtain high-purity AMPS with a purity of 99.5-99.6%, and the mass content of tert-butylpropenesulfonic acid is 88-94ppm .

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Abstract

The invention provides a method for producing tert-butyl acryloyl sulfonic acid. The method includes providing of a first external circulation device and a second external circulation device, adding of a first portion of acrylonitrile and a sulfonating agent into the first external circulation device to form a first mixture, and adding of a second portion of the acrylonitrile and isobutylene intothe second external circulation device to form a second mixture; mixing of the first mixture from the first external circulation device and the second mixture from the second external circulation device in a reaction kettle for reacting to produce tert-butylacryloyl sulfonic acid slurry; transferring of the tert-butylacryloyl sulfonic acid slurry to a maturation tank for maturation to produce maturated tert-butylacryloyl sulfonic acid slurry; solid-liquid separation of the maturated tert-butylacryloyl sulfonic acid slurry, and vacuum drying of a separated solid to obtain crude tert-butyl acryloyl sulfonic acid. The method can effectively reduce the formation of by-products and increase production efficiency.

Description

technical field [0001] The invention relates to a production method of an organic compound, in particular to a production method of tert-butylacrylamide sulfonic acid. Background technique [0002] Tert-butylacrylamide sulfonic acid (2-Acrylamide-2-methylpropane sulfonic acid, hereinafter referred to as AMPS) is one of the most widely used polymerized monomers. Its molecular structure has carbon-carbon double bonds, amido groups and sulfonic acid functional groups. Its homopolymers and copolymers have many special properties and have broad application prospects, and can be widely used in fields such as oilfield chemistry, water treatment agents, fiber synthesis, coatings, and pharmaceutical hydrogels. [0003] As disclosed in JP2904444, JP2904465 and JP81533062, the most common synthetic method of AMPS is to use excess acrylonitrile as a reaction solvent, and add fuming sulfuric acid at low temperature, then feed isobutylene under stirring to make it react, and the product A...

Claims

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Application Information

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IPC IPC(8): C07C303/02C07C303/44C07C309/15
CPCC07C303/02C07C303/44C07C309/15
Inventor 李斗星齐兰芝穆晓蕾贾春革
Owner CHINA PETROLEUM & CHEM CORP
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