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A kind of preparation method of 2-acrylamido alkylsulfonic acid

A technology of acrylamido alkyl sulfonic acid and acrylonitrile, which is applied in the field of polymer material monomer synthesis, can solve the problems of troublesome solvent recovery in the later stage of product purification, difficult preparation and operation, etc., and achieves stable and easy-to-control reaction process and simple post-processing. , the effect of easy industrial production

Active Publication Date: 2017-05-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to overcome the problems of the prior art that the preparation is not easy to operate, and need to use a dehydrating agent, product purification and solvent recovery in the later stage, and provide a preparation method of 2-acrylamido alkyl sulfonic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] According to n(α-olefin):n(H 2 SO 4 +SO 3 ):n(acrylonitrile)=1:0.95:5, n(H 2 SO 4 ):n(SO 3 )=1:2.28 ratio, 265.3 gram of acrylonitrile, 196.37 gram of tetradecene-1 are added in the reaction bottle with stirring, thermometer, dropping funnel, ventilation conduit and condenser, stir with ice-salt water bath after The temperature of the system dropped to -5°C, and 35.52 grams of 20% oleum was added to the system in 60 minutes, and the reaction temperature was kept below 10°C during the addition process; Feed 45.67 g of sulfur trioxide, keep the reaction temperature not exceeding 15°C during the addition process, add 5 mL of water after the amount of sulfur trioxide is reached, and stir the reaction at room temperature for 10 h; The acid crystals were filtered with a glass sand core funnel, and the obtained crystals were washed twice with acrylonitrile, and then dried in vacuum at 60°C to obtain 278.3 grams of product, calculated as tetradecene-1, with a yield of 80.2...

Embodiment 2

[0022] According to n(α-olefin):n(H 2 SO 4 +SO 3 ):n(acrylonitrile)=1:1.15:11, n(H 2 SO 4 ):n(SO 3 )=1:1.23 ratio, 583.66 gram of acrylonitrile, 168.32 gram of dodecene-1 are added in the reaction bottle with stirring, thermometer, dropping funnel, ventilation conduit and condenser, stir with ice-salt water bath after When the temperature of the system drops to -6°C, add 54.84 grams of 10% fuming sulfuric acid to the system in 30 minutes, and keep the reaction temperature not exceeding 10°C during the addition process; Feed 43.86 g of sulfur trioxide, keep the reaction temperature not exceeding 15°C during the addition process, add 2 mL of water after the amount of sulfur trioxide is reached, and stir the reaction at room temperature for 3 h; The acid crystals were filtered with a glass sand core funnel, and the obtained crystals were washed twice with acrylonitrile respectively, and then vacuum-dried at 60°C to obtain 269.6 g of the product, calculated as dodecene-1, wit...

Embodiment 3

[0024] According to n(α-olefin):n(H 2 SO 4 +SO 3 ):n(acrylonitrile)=1:1:9, n(H 2 SO 4 ):n(SO 3 )=1:1.84 ratio, 477.54 grams of acrylonitrile, 224.43 grams of hexadecene-1 are added in the reaction flask with stirring, thermometer, dropping funnel, vent tube and condenser, after stirring evenly, use ice-salt water bath to When the temperature of the system drops to -8°C, add 40.63 grams of 15% fuming sulfuric acid to the system in 45 minutes, and keep the reaction temperature not exceeding 10°C during the addition process; Add 45.71 g of sulfur trioxide, keep the reaction temperature not exceeding 15°C during the addition process, add 3.5 mL of water after the amount of sulfur trioxide is reached, and stir the reaction at room temperature for 6 hours; The sulfonic acid crystals were filtered with a glass sand core funnel, and the obtained crystals were washed twice with 350 g of acrylonitrile, and then vacuum-dried at 60 ° C to obtain 322.9 g of the product, calculated as ...

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Abstract

The invention relates to a preparing method of 2-acrylamide alkyl sulfonic acid and belongs to the technical field of high-polymer material monomer synthesis, wherein the 2-acrylamide alkyl sulfonic acid is a polymerizable surface active agent monomer. Raw materials of the 2-acrylamide alkyl sulfonic acid are alpha-olefin, industrial grade acrylonitrile, 10%-20% of fuming sulphuric acid and sulfur trioxide. A quantity relative ratio of the raw materials is n (the alpha-olefin): n (sulfuric acid (H2SO4) +sulfur trioxide (SO3)): n (the acrylonitrile) = 1: (0.95-1.15): (5-11), wherein n (H2SO4): n (SO3) =1: (1.23-2.28). 10%-20% of the fuming sulphuric acid and the sulfur trioxide serve as sulfonating agents. The industrial grade acrylonitrile which serves as the raw material and solvent can be directly applied without dehydration. In the process of preparation, no dehydration agent is needed. In addition, the yield of target products is larger than 80%, the purity is larger than 98%, the reaction process is stable and easy to control, the post processing of the products and the solvent is simple, and the industrial production is facilitated.

Description

[0001] Technical field: [0002] The invention relates to a preparation method of 2-acrylamido alkyl sulfonic acid. 2-acrylamido alkyl sulfonic acid is a polymerizable surfactant monomer and belongs to the technical field of polymer material monomer synthesis. [0003] technical background: [0004] Olefinic monomers and their polymers with sulfonic acid groups not only have the unique properties of strong acids, but also have specific stability to hydrolysis, temperature and divalent cations, and have become irreplaceable monolithic monomers in some applications. Solids and polymers, such as in emulsion polymerization, printing and dyeing, oil fields, and water treatment industries, are widely used. [0005] 2-Acrylamido-2-methylpropanesulfonic acid (AMPS) is an amidosulfonic acid monomer obtained earlier that can produce high molecular weight polymers. On this basis, acrylamide-based long-chain alkylsulfonic acids have been developed, such as 2-acrylamido hexadecanesulfonic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/15C07C303/06
Inventor 王中华
Owner CHINA PETROLEUM & CHEM CORP