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Continuous synthesis method of carboxyethyl thiosuccinic acid

A carboxyethyl thiosuccinic acid, chemical synthesis technology, applied in chemical instruments and methods, preparation of carboxylic acid anhydride, preparation of organic compounds, etc., can solve the problem of phosphorus in the product, achieve good market application prospects, and stable quality The effect of high resistance and high product content

Pending Publication Date: 2021-03-12
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction is green and efficient; at the same time, it solves the problem of phosphorus in the current product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 1000g of solvent water into a 2000ml beaker, weigh 417g of maleic anhydride, add it into the beaker, stir mechanically until the solids are completely dissolved, then add 430g of β-mercaptopropionic acid and 40.98g of triethylamine, and stir until uniform; open the tube in advance Reactor device, the external temperature is set at 95°C, and the flow rate is 2.2ml / min. The reaction solution is pumped into the tubular reactor by the liquid feed pump, and the residence time is 90min. , Obtain 675.12g of white powdery solid, product crystallization yield 75%, carboxyethyl thiosuccinic acid content is 97.84%.

[0021] Add water to the obtained mother liquor after the above-mentioned filtration to replenish to 1000g, weigh 417g maleic anhydride, add in the beaker, mechanically stir until the solid is completely dissolved, then add 430g β-mercaptopropionic acid, and then add triethylamine to 40.98g (according to the detection , part of the catalyst will be lost during the ...

Embodiment 2

[0023] Add 1000g of solvent water into a 2000ml beaker, weigh 437g of maleic anhydride, add it into the beaker, stir mechanically until the solids are completely dissolved, then add 430g of β-mercaptopropionic acid and 3.2g of sodium hydroxide, and stir until uniform; open the tube in advance Reactor device, the external temperature is set at 105°C, and the flow rate is 2.0ml / min. The reaction solution is pumped into the tubular reactor by the liquid feed pump, and the residence time is 100min. The reaction effluent is cooled and crystallized, filtered and dried. Obtain 719.66 g of white powdery solids, the product crystallization yield is 80%, and the content of carboxyethylthiosuccinic acid is 97.50%.

[0024] Add water to the mother liquor obtained after the above filtration to make up to 1000g, weigh 437g of maleic anhydride, add it into a beaker, stir until the solids are completely dissolved, then add 430g of β-mercaptopropionic acid, add sodium hydroxide to 3.2g, and sti...

Embodiment 3

[0026] Add 1000g of solvent water into a 2000ml beaker, weigh 437g of maleic anhydride, add it into the beaker, stir mechanically until the solids are completely dissolved, then add 430g of β-mercaptopropionic acid and 30.21g of triethanolamine, and stir until uniform; start the tube reaction in advance The reactor device, the external temperature is set at 115°C, and the flow rate is 2.85ml / min. The reaction solution is pumped into the tubular reactor by the liquid feed pump, and the residence time is 70min. White powdery solid 805.71g, product crystallization yield 88%, carboxyethyl thiosuccinic acid content is 98.20%.

[0027] Add water to the mother liquor obtained after the above filtration to make up to 1000g, weigh 409g of maleic anhydride, add it into a beaker, stir until the solids are completely dissolved, then add 430g of β-mercaptopropionic acid, add triethanolamine to 30.21g, and stir until uniform; Open the tubular reactor device in advance, set the external temp...

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PUM

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Abstract

The invention belongs to the field of application of fine chemicals, and particularly relates to a continuous synthesis method of carboxyethyl thiosuccinic acid. Beta-mercaptopropionic acid and maleicanhydride are used as reaction raw materials, green solvent water is used as a reaction medium, a tubular reactor is used for continuous production, on the basis that reaction requirements are met, the price is low, obtaining is easy, and meanwhile due to the water solubility of CETSA, recycled mother liquor can be used indiscriminately. The reaction is green and efficient; and meanwhile, the problem that the product contains phosphorus at present is solved. The technological process is simple, the obtained product is high in quality stability, the technology is environmentally friendly, andthe product content is high. The defects of complex traditional process flow, serious three-waste pollution and low product content are avoided.

Description

technical field [0001] The invention belongs to the application field of fine chemicals, and in particular relates to a continuous synthesis method of carboxyethylthiosuccinic acid. Background technique [0002] Carboxyethylthiosuccinic acid (CETSA), white solid, slight odor, melting point 150.5-152.5, soluble in water, ethanol, ether and acetone. Carboxyethylthiosuccinic acid (CETSA) contains 3 carboxyl groups in each molecule and is extremely acidic (1% aqueous solution pH = 1). CETSA also has a strong ability to disperse and prevent secondary deposition. It has good salt resistance under high temperature conditions, so its various properties are very suitable for neutralization-free use. [0003] At present, the annual production capacity of carboxyethyl thiosuccinic acid in the world is about 7,000 tons. The main manufacturers are Mexico Xihe Petroleum Company, Nippon Oils and Fats and French Alpha-Ato Chemical Company. Among them, Xihe Petroleum Company, the main impo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/18C07C319/28C07C323/52C07C51/087C07C57/145
CPCC07C319/18C07C319/28C07C51/087C07C57/145C07C323/52
Inventor 陈志敏易先君吴玉强高艳丽高云龙袁新洁侯小敏张建林张超
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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