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A kind of synthetic method of β-mercaptopropionic acid

A synthesis method and technology of mercaptopropionic acid, applied in the preparation of mercaptans, organic chemistry, etc., can solve the problems of environmental protection problems, increase costs, and three wastes, etc., and achieve the effects of less three wastes, fewer by-products, and good purity.

Active Publication Date: 2018-05-01
荆州市诺亚化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Thereby increasing the cost, producing nitrogen-containing "three wastes", and environmental protection problems are not easy to solve
The cost of other methods is relatively high, and there are also "three wastes" produced

Method used

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  • A kind of synthetic method of β-mercaptopropionic acid
  • A kind of synthetic method of β-mercaptopropionic acid
  • A kind of synthetic method of β-mercaptopropionic acid

Examples

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Embodiment 1

[0042]A kind of synthetic method of β-mercaptopropionic acid, in the reaction bottle of 1000ml, add 206g (1.1mole) of newly-made 30% sodium hydrosulfide aqueous solution, under the protection of nitrogen, stir and cool down to 10 ℃, temperature control 10 ℃ ± 2 ℃, in 142 g (1 mole) of 50% acrylamide aqueous solution was added dropwise into the reaction flask within 2 hours, and then stirred for 2 hours. Raise the temperature to 40°C, react for 1 hour, and take a sample for analysis. Acrylamide is completely converted. Add 167g of 30% NaOH aqueous solution to the reaction liquid, turn on the tail gas absorption device, stir and raise the temperature and reflux for 3h for hydrolysis, and then distill 50ml of ammonia water under slight negative pressure. Cool down to 40°C, add 60% sulfuric acid dropwise to adjust PH=2 to 3, let stand for 1h, separate layers, add 50ml water to wash once on the upper layer, and collect fractions at 85°C (3mmHg) by fractional distillation to obtain ...

Embodiment 2

[0044] The present embodiment provides a kind of synthetic method of β-mercaptopropionic acid, with embodiment 1, difference only is that the consumption of sodium hydrosulfide drops to 187g (1mole), finally gets 92.2g of β-mercaptopropionic acid, content ≥ 99%, Yield 87%.

Embodiment 3

[0046] A method for synthesizing β-mercaptopropionic acid, replacing the air in a 1000ml autoclave with nitrogen for three times, adding 68g (2mole) of hydrogen sulfide, stirring to cool down to 0°C, adding 142g (1mole) of 50% acrylamide aqueous solution within 2h , then heat up to 40°C, react for 2 hours, release excess hydrogen sulfide gas and absorb it with alkali, cool down to 20°C, transfer the reacted mercaptopropionamide aqueous solution into a 1000ml reaction bottle, add 293g of 30% NaOH aqueous solution, stir and heat up to reflux reaction, The generated ammonia gas was absorbed into ammonia water, and then the temperature of the reaction liquid was lowered to 40° C., and the pH was adjusted to 2 with 60% sulfuric acid, and the layers were separated. The upper layer was washed once with 50ml of water, and the 85°C (3mmHg) fraction collected by fractional distillation was 98g of beta-mercaptopropionic acid, with a content of ≥99.0%, and a yield of 92.45%. The high boile...

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Abstract

The invention provides a beta-mercaptopropionic acid synthetic method. The method takes acrylamide and hydrogen sulfide or sodium sulfhydrate as raw materials to obtain the addition products through an addition reaction, caustic soda liquid is employed for hydrolyzing the addition products, and acidifying the addition products to obtain the beta-mercaptopropionic acid; the reaction activity of acrylamide is similar with acrylonitrile, when addition is carried out with hydrogen sulfide or sodium sulfhydrate, the yield is high, and the by-product is little. During hydrolysis and acidifying processes, three wastes can be ideally recovered, the three wastes are conversed to the industrial byproduct for sale, economic benefit is provided to the enterprise, and the synthesis route of the beta-mercaptopropionic acid has the advantages of high yield, good purity, less three wastes, easy processing of waste water, and is a better synthesis route.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis method of β-mercaptopropionic acid. Background technique [0002] β-mercaptopropionic acid is a basic chemical raw material, which is widely used in medicine, pesticide and other organic synthesis fields. In recent years, due to the increasing use of β-mercaptopropionic acid in the field of carboxylic acid water reducers, it is necessary to develop a cheap and environmentally friendly β-mercaptopropionic acid synthesis process. [0003] As early as 1950, American Thomas used 1,3-propionolactone and sodium hydrosulfide to synthesize β-mercaptopropionic acid with a yield of 87% (see US2449989), and 1,3-propionolactone can be synthesized from ketene Synthesized with formaldehyde (see US2356495). [0004] [0005] HSCH 2 CH 2 COONa+HCl→HSCH 2 CH 2 COOH+NaCl In 1960, Japan published the patent JP2913, using acrylonitrile and sodium hydrosulfi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/04C07C319/02C07C323/52
CPCC07C319/02C07C319/04C07C323/60C07C323/52
Inventor 张道远宋莉红周序辉
Owner 荆州市诺亚化工有限公司