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Synthesis method of tert-butyl acrylamide sulfonate

A technology of tert-butylacrylamide sulfonic acid and synthesis method, which is applied in the direction of sulfonic acid preparation and organic chemistry, etc., can solve problems such as harsh reaction conditions, achieve the effects of improving purity, saving raw material costs, and reducing production costs

Active Publication Date: 2013-03-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patent US3544597 first reported this method for preparing amidosulfonic acid compounds, and obtained monomers with higher purity, but the reaction conditions were harsher

Method used

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Examples

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preparation example Construction

[0016] The invention provides a kind of synthetic method of tert-butylacrylamide sulfonic acid, wherein, the method comprises the following steps:

[0017] (1) providing a first solution and a second solution,

[0018] The first solution is obtained by contacting acrylonitrile with the first sulfonating agent at -30°C to 15°C; the second solution is obtained by contacting acrylonitrile with the first sulfonating agent at -30°C to 15°C obtained by contacting the second sulfonating agent;

[0019] (2) At -20°C to 50°C, contacting the first solution with isobutene accounting for 10-100% of the isobutene feed and the second solution to obtain a third solution;

[0020] (3) at -20°C to 50°C, contacting the third solution with isobutene accounting for 0-90% of the isobutene feed to obtain a slurry product;

[0021] (4) separating and purifying the slurry product to obtain tert-butylacrylamide sulfonic acid;

[0022] Wherein, the first sulfonating agent is the same or different fr...

Embodiment 1

[0039] This example is used to illustrate the synthesis method of tert-butylacrylamide sulfonic acid provided by the present invention.

[0040] (1) In a four-neck flask provided with a temperature control device, a stirrer, a thermometer and a gas feed device, add 220 g of acrylonitrile, and after the acrylonitrile is cooled to -15° C., add 34 g of fuming sulfuric acid with a concentration of 103% by weight , the first solution was obtained, and the temperature was maintained at -15°C during and after the addition.

[0041] In another stirring vessel, add 110g of acrylonitrile, cool the acrylonitrile to -15°C and then add 27g of oleum with a concentration of 103% by weight to obtain the second solution, and maintain the temperature at -15°C during and after the addition And keep stirring.

[0042] (2) After continuing to stir the first solution for 1 hour, the temperature was raised to 40° C. and 12 g of isobutylene was introduced for reaction, and then the second solution w...

Embodiment 2

[0046] This example is used to illustrate the synthesis method of tert-butylacrylamide sulfonic acid provided by the present invention.

[0047] (1) In a four-necked flask provided with a temperature control device, a stirrer, a thermometer and a gas feed device, add 180 g of acrylonitrile, and after cooling the acrylonitrile to -15° C., add 25 g of fuming sulfuric acid with a concentration of 103% by weight , the first solution was obtained, and the temperature was maintained at -15°C during and after the addition.

[0048] In another stirring vessel, add 150g of acrylonitrile, cool the acrylonitrile to -15°C and then add 36g of oleum with a concentration of 101% by weight to obtain the second solution, and maintain the temperature at -15°C during and after the addition And keep stirring.

[0049] (2) After continuing to stir the first solution for 1 hour, the temperature was raised to 40° C., and then 8 g of isobutylene was introduced for reaction, and then the second solut...

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PUM

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Abstract

The invention discloses a synthesis method of tert-butyl acrylamide sulfonate, which comprises the following steps of: providing a first solution and a second solution, wherein the first solution is obtained through contact between acrylonitrile and a first sulfonating agent at -30 to 15 DEG C, and the second solution is obtained through contact between acrylonitrile and a second sulfonating agent at -30 to 15 DEG C; at -20 to 50 DEG C, enabling the first solution to contact with isobutene accounting for 10-100% of isobutene feed and the second solution to obtain a third solution; at -20 to 50 DEG C, enabling the third solution to contact with isobutene accounting for 0-90% of the isobutene feed to obtain a paste product; and separating and purifying the paste product to obtain tert-butyl acrylamide sulfonate. Through the method disclosed by the invention, other substances are not required in a reaction system, the production cost is greatly reduced, and the purity is improved.

Description

technical field [0001] The invention relates to a method for synthesizing tert-butylacrylamide sulfonic acid. Background technique [0002] Tertiary butylacrylamide sulfonic acid (acrylamido tertiary butyl sulfonic acid, hereinafter referred to as ATBS) is a multifunctional water-soluble anionic monomer with a molecular structure of Because the molecular structure of ATBS has a salt-insensitive sulfonic acid group and a well-protected amide group, its homopolymer and copolymer have many special properties and have broad application prospects. They can be widely used in oilfield chemistry and water treatment. Agents, chemical fibers, plastics, printing and dyeing, coatings, surfactants, antistatic agents, ceramics, photography, detergent additives, ion exchange resins, gas separation membranes, electronics and other fields. [0003] At present, the most typical process for producing ATBS is to prepare ATBS by reacting acrylonitrile, oleum and isobutylene under relatively mi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/15C07C303/06
Inventor 李斗星齐兰芝黄凤兴贾春革穆晓蕾赵冬
Owner CHINA PETROLEUM & CHEM CORP
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