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Preparation method of hydrophobic monomer N-alkyl acrylamide

A technology of alkylacrylamide and hydrophobic monomer, which is applied in the field of preparation of hydrophobic monomer N-alkylacrylamide, can solve the problems of restricting industrial production, low product content, troublesome recycling and disposal, etc. Low cost, easy to obtain raw materials, easy to control the effect

Inactive Publication Date: 2014-09-17
JIANGSU ANDY CHEM PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sulfuric acid catalyzed synthetic conditions are mild. In the application of this method reported at present, Wu Guozhong et al. adopt alcohol solvents, preferably ethanol and methyl alcohol, and the resulting product yield is high (up to 92.5%); but a large amount of solvent-containing waste acid is produced. Recycling and disposal are cumbersome, limiting industrial production
He Yingchao et al. used solvent-free reaction, optimized the use of sulfuric acid with a concentration of 65-95%, and concentrated and recovered the post-treated aqueous solution to realize the recovery of sulfuric acid, with a yield of 90%. 93.8%, and then recrystallized with solvent, the best can only reach 98%

Method used

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  • Preparation method of hydrophobic monomer N-alkyl acrylamide

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Experimental program
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Effect test

Embodiment 1

[0031] Prepare a dry 1L four-neck flask equipped with a stirring paddle, feed port, thermometer and nitrogen tube, add 120 g of formic acid, 66 g (1.16 mol) of isobutylene, and 98 g (1.0 mol) of sulfuric acid into the reaction flask, and react with an ice-water bath. The mixture in the flask was cooled to 35±2°C, and 53g (1.0mol) of acrylonitrile was added dropwise; the reaction was continued to stir at 30-35°C for 4h. Add 1000g of deionized water into a 2L three-necked flask, start stirring, control the temperature at 15-20°C throughout the process, and add the above reaction solution dropwise; after the addition, continue to add about 550g of sodium hydroxide solution (15%) dropwise, and adjust the pH value to 5.0 , the white slurry was suction-filtered, and the obtained solid was washed with water until neutral. Dry in vacuum at 50°C for 4h. Obtained product 107g, the gas chromatographic examination content is 99.4%. Filtrate the mother liquor and distill to recover formi...

Embodiment 2

[0033] In the dry 1L four-necked flask that is equipped with stirring paddle, feeding port, thermometer and nitrogen tube, glacial acetic acid 160g, diisobutylene 135g (1.20mol), sulfuric acid 108g (1.1mol) are added in the reaction flask, and the reaction flask The mixture in the mixture was cooled to 30±2°C, and 53 g (1.0 mol) of acrylonitrile was added dropwise; the stirring reaction was continued at 25-30°C for 4 h. Add 1200g of deionized water into a 2L three-necked bottle, start stirring, control the temperature at 1-5°C throughout, and add the above reaction solution dropwise; after the addition, continue to add about 780g of sodium carbonate solution (15%) dropwise to adjust the pH value to 5.1, white The slurry was filtered with suction, and the obtained solid was washed with water until neutral. Dry in vacuum at 50°C for 4h. Obtain product 160g, gas chromatography inspection content is 99.1%. Filtrate the mother liquor and distill to recover acetic acid, then conce...

Embodiment 3

[0035] Prepare in the dry 1L four-neck flask that is equipped with stirring paddle, feeding port, thermometer and nitrogen tube, methanesulfonic acid 212g, hexadiene 82g (1.0mol), sulfuric acid 127.6g (1.3mol) join in the reaction flask, The mixture in the reaction flask was cooled to 5° C., and 53 g (1.0 mol) of acrylonitrile was added dropwise; the reaction was continued to stir at 15° C. for 8 h. Add 2120g of deionized water into a 2L three-necked bottle, start stirring, control the temperature at 0°C throughout the process, and add the above reaction solution dropwise; after the addition, continue to add potassium hydroxide solution dropwise to adjust the pH to 3, and filter the white slurry with suction The resulting solid was washed with water until neutral. Dry in vacuum at 50°C for 4h. Obtain product 116g, gas chromatography inspection content is 98.2%.

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Abstract

The invention discloses a preparation method of hydrophobic monomer N-alkyl acrylamide. The method comprises the following steps: by adopting a sulfuric acid catalysis method and taking low-molecular-weight organic acid as a catalyst promoter and a medium, reacting olefin and sulfuric acid with acrylonitrile to obtain active intermediate reaction liquid under the mild reaction conditions; dropwise adding the active intermediate reaction liquid into deionized water, then neutralizing by adopting alkali, to obtain the hydrophobic monomer N-alkyl acrylamide. According to the preparation method, the side product sulfate can be recovered, and environmental pollution can be reduced. According to gas chromatography the purity of the prepared hydrophobic monomer N-alkyl acrylamide can be up to more than 99.0%, and the yield can also achieve more than 90%. Compared with the existing method, the method is simple in technology, easy to control, easily available, and low in cost.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and relates to a preparation method of hydrophobic monomer N-alkylacrylamide. Background technique [0002] Poly(N-alkylacrylamide) and other multi-component copolymers are widely used in oil recovery, sewage treatment, cosmetics and paint industries. Their temperature-sensitive properties make them have great potential in the fields of bioseparation engineering, drug controlled release materials and sensor materials. Value. [0003] There are mainly four methods for the production and preparation of the hydrophobic monomer N-alkylacrylamide of poly N-alkylacrylamide: the synthesis of acryloyl chloride and alkylamine; the thermal decomposition of carboxylic acid or sulfonate amine compound; the olefin or Reaction of alcohols and nitriles; N-alkylation of acrylamides. [0004] (1) Synthesis of Acryloyl Chloride and Alkylamine [0005] The preparation of acryloyl chloride requir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/09C07C231/06
Inventor 杜娟康宏杰周旭东段红博万堂庆
Owner JIANGSU ANDY CHEM PHARMA CO LTD
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