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A kind of synthetic technique of n-isopropylacrylamide

A technology for the synthesis of isopropylacrylamide, which is applied to the preparation of carboxylic acid amide, separation/purification of carboxylic acid amide, and the preparation of organic compounds, etc. It can solve the problems of many organic solvents, short process flow, and low product yield. , to achieve the effect of reducing residue, high reaction yield and good product purity

Inactive Publication Date: 2020-05-19
辽宁三洋新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product yield of this method is low, the process flow is long, the operation is cumbersome, the use of organic solvents is large, the environmental load is large, and the production cost is high. Low production cost, easy operation, safe and environmentally friendly purification method N -The industrial production of isopropylacrylamide is of great significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 10.6 kg of acrylonitrile, 12.6 kg of isopropanol, 0.1 kg of 1,4-benzenediol, 0.2 kg of tetra-n-butylammonium chloride to a 200-liter stainless steel kettle, and add 65.9 kg of 35% dropwise between 20-40 °C Sulfuric acid, after dropping, react at 40-50°C for 1 hour. Add 25% ammonia water dropwise to the reaction kettle to adjust the pH to about 7, let stand, separate the liquid, discard the water phase, add 120 kg of water to the reaction kettle, stir and extract at 90 ° C for 15 minutes, let stand, separate the liquid, and then The aqueous phase was transferred to another 200-liter stainless steel kettle, and the temperature was lowered to 5°C and stirred for 0.5 hours. Centrifuge, collect the solid, transfer it to a vacuum drying box, and dry it at -0.08MPa vacuum at 40-50°C for 4 hours to obtain 18.2 kg N -Isopropylacrylamide with a yield of 80.5% and a liquid phase purity of 99.3%.

[0039] Melting range: 61-63℃; 1 H NMR (DMSO-d6, 400 MHz) δ : 7.96 (s, 1H), 6...

Embodiment 2

[0041] Add 10.6 kg of acrylonitrile, 12.6 kg of isopropanol, 0.1 kg of 1,4-benzenediol, 0.15 kg of tetra-n-butylammonium chloride to a 200-liter stainless steel kettle, and add 51.5 kg of 45% dropwise between 20-40 °C Sulfuric acid, after dropping, react at 40-50°C for 1 hour. Add 25% ammonia water dropwise to the reaction kettle to adjust the pH to about 8, let stand, separate liquids, discard the water phase, add 130 kg of water to the reaction kettle, stir and extract at 85°C for 15 minutes, let stand, and separate liquids. The aqueous phase was transferred to another 200-liter stainless steel kettle, and the temperature was lowered to 5°C and stirred for 2 hours. Centrifuge, collect the solid, transfer it to a vacuum drying oven, and dry it at -0.08MPa vacuum at 40-50°C for 4 hours to obtain 18.6 kg N -Isopropylacrylamide with a yield of 82.3% and a liquid phase purity of 98.1%.

[0042] Melting range: 60-62℃; 1 H NMR (DMSO-d6, 400 MHz) δ : 7.95 (s, 1H), 6.21-6.01 (m, ...

Embodiment 3

[0044]Add 10.6 kg of acrylonitrile, 12.6 kg of isopropanol, 0.05 kg of 1,4-benzenediol, 0.2 kg of tetra-n-butylammonium chloride to a 200-liter stainless steel kettle, and add 92.3 kg of 25% dropwise between 20-40 °C Sulfuric acid, after dropping, react at 40-50°C for 1 hour. Add dropwise 25% ammonia water to the reaction kettle to adjust the pH to about 7, let it stand, separate the liquid, discard the water phase, add 90 kg of water to the reaction kettle, stir and extract at 90 ° C for 15 minutes, let it stand, and separate the liquid. The aqueous phase was transferred to another 200-liter stainless steel kettle, and the temperature was lowered to 5°C and stirred for 0.5 hours. Centrifuge, collect the solid, transfer it to a vacuum drying oven, and dry it at -0.08MPa vacuum at 40-50 °C for 4 hours to obtain 17.1 kg N -Isopropylacrylamide with a yield of 75.7% and a liquid phase purity of 99.0%.

[0045] Melting range: 61-62℃; 1 H NMR (DMSO-d6, 400 MHz) δ : 7.96 (s, 1H),...

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Abstract

The invention relates to a synthesis process of N-isopropylacrylamide, and belongs to the technical field of new materials. According to the process, acrylonitrile and isopropanol have an alkylation reaction under the catalyzing of tetra-n-butylammonium chloride and sulphuric acid to prepare the N-isopropylacrylamide, an organic layer is separated after the N-isopropylacrylamide is neutralized through ammonium hydroxide, then the N-isopropylacrylamide is extracted through water, an extraction liquid is directly cooled and crystalized after being concentrated to obtain an N-isopropylacrylamide crystal, and the N-isopropylacrylamide crystal is dried in vacuum to obtain a product. The used raw materials are cheap and easy to get, the cost is low, the product purity is high, the yield is high, and the process flow is short. The synthesis process has a broad application prospect in the large-scale production of the N-isopropylacrylamide in a workshop.

Description

technical field [0001] The present invention relates to a kind of polymer material monomer, specifically relate to a kind of N -The synthesis process of isopropylacrylamide belongs to the technical field of new materials. Background technique [0002] N -Isopropylacrylamide is an important temperature-sensitive material monomer, which is white or light yellow crystal. Its gel polymer has a critical temperature. When the temperature is lower than this value, the gel is swollen in water, and when the temperature reaches its critical temperature, the gel shrinks rapidly. Based on this feature, N -Isopropylacrylamide polymers are used to manufacture temperature-sensitive films, glass or display devices, and are also widely used in biology, medicine, environmental protection and other fields. [0003] currently synthesized N -The route of isopropyl acrylamide mainly has the following three kinds: [0004] One uses methyl acrylate and isopropylamine as raw materials, and is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/09C07C231/06C07C231/24
CPCC07C231/06C07C231/24C07C233/09
Inventor 于涛张泽群
Owner 辽宁三洋新材料科技有限公司
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