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Preparation method for pentaerythritol tetra (3-R-alkyl thiopropionic acid)

A technology of alkylthiopropionic acid and pentaerythritol ester, which is applied in the preparation of thioether and organic chemistry, can solve the problems of toxicity and difficulty in obtaining alkylthiol, and achieve high activity, improved structural activity, and high yield Effect

Inactive Publication Date: 2015-04-22
北京极易控股集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the raw material of alkyl mercaptan has certain toxicity and unpleasant smell, and the mixed alkyl mercaptan is difficult to obtain

Method used

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  • Preparation method for pentaerythritol tetra (3-R-alkyl thiopropionic acid)
  • Preparation method for pentaerythritol tetra (3-R-alkyl thiopropionic acid)
  • Preparation method for pentaerythritol tetra (3-R-alkyl thiopropionic acid)

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Put 244g of pentaerythritol tetra-3-mercaptopropionate and 7.3g of potassium tert-butoxide into a 1000ml reactor, turn on the nitrogen replacement, turn on the agitator and raise the temperature to 35 degrees, slowly add 450.8g of n-tetradecene and keep the reaction The temperature is 35-40 degrees. After the addition, keep warm at 40 degrees for 5 hours, add 3.91g of acetic acid, after precision filtration, depressurize to -0.01MPa, temperature 290 degrees, recover excess n-tetradecene and trace unreacted pentaerythritol by distillation Tetra-3-mercaptopropionate obtained 596.4g white solid after cooling, the yield was 93.77%, and the product purity was 99.5%.

Embodiment 2

[0028] Put 244g of pentaerythritol tetra-3-mercaptopropionate and 4.88g of sodium methylate into a 1000ml reactor, turn on the nitrogen replacement, turn on the stirrer and heat up to 30 degrees, slowly add 378g of n-dodecene and keep the reaction temperature at 30°C ~35°C, keep warm at 35°C for 6 hours after the addition, add 5.43g of acetic acid, after precision filtration, depressurize to -0.01MPa, temperature 290°C, recover excess n-dodecene and trace unreacted pentaerythritol tetra-3 -Mercaptopropionate, after cooling, 573.1g white solid was obtained, the yield was 98.8%, and the product purity was 99.7%.

Embodiment 3

[0030] Put 244g of pentaerythritol tetra-3-mercaptopropionate and 2.8g of sodium hydroxide into a 1000ml reactor, after opening the nitrogen replacement, open the agitator and heat up to 30 degrees, slowly add 336g of n-decene and keep the reaction temperature at 30°C ~33°C, keep warm at 38°C for 5 hours after the addition, add 4.2g of acetic acid, after precision filtration, depressurize to -0.01MPa, temperature 290°C, recover excess n-decene and trace unreacted pentaerythritol tetra-3- Mercaptopropionate obtained 504.4g of white waxy solid after cooling, the yield was 96.2%, and the product purity was 99.3%.

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Abstract

The invention relate to a preparation method for pentaerythritol tetra (3-R-alkyl thiopropionic acid), and belongs to the technical field of antioxidant preparation. The preparation method includes the steps of firstly, adding pentraerythritol tetra (3-mercaptopropionate) and alkaline catalysts into a reactor, and then dropping or slowly injecting alkene R1, alkene R2, alkene R3 and alkene R4 to conduct the addition reaction; secondly, adding neutralizer after the addition reaction is completed, evaporating the redundant alkene R1, the redundant alkene R2, the redundant alkene R3, the redundant alkene R4 and the pentraerythritol tetra (3-mercaptopropionate) which does not participate in the reaction through a rectifying tower after the reaction mixture is precisely filtered, and conducting fractionation to obtain pentaerythritol tetra (3-R-alkyl thiopropionic acid). In the reaction process of the method, no solvent is used, the solvent recycle procedure is omitted, cost is reduced, and the method is more environmentally friendly. In addition, products are separated through rectifying in the postprocessing process, production is more environmentally friendly due to the fact that no solvent is used, the yield is higher than that of an ordinary crystallization centrifugal process, and quality is good.

Description

technical field [0001] The present invention relates to the technical field of antioxidant preparation, in particular to a preparation method of tetrakis (3-R alkylthiopropionate) pentaerythritol ester, which is a Sulfur-containing antioxidants. Background technique [0002] Tetrakis(3-R alkylthiopropionic acid) pentaerythritol ester is an excellent thioester antioxidant with high sulfur content per unit, and the structure containing pentaerythritol in the structure presents excellent high temperature resistance and anti-oxidation properties. Water extraction performance, so compared with the traditional sulfur-containing antioxidants DSTDP and DLTDP, it is especially suitable for polymer products that are susceptible to water damage or used under severe climate conditions, when the R alkyl C atoms are greater than 10 or more The high molecular weight structure also has great application value in polymer fibers. [0003] At present, the preparation method of four (3-R alky...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/18
Inventor 郭永武
Owner 北京极易控股集团有限公司
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