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Preparation method of pentaerythritol tetra(3-n-dodecylthiopropionate)

A technology of n-dodecyl thiopropionate and pentaerythritol tetra, which is applied in the field of preparation of sulfur-containing antioxidants, can solve the problems of great harm to the environment and operators, and difficult to achieve, so as to achieve reduced production costs, good quality, The effect of solving environmental pollution problems

Active Publication Date: 2014-04-16
RIANLON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is reported that the yield reaches 94.7%, but in fact it is difficult to achieve the said yield due to the production of a large number of by-products, and azobisbutyronitrile is heated to decompose to release nitrogen oxides and organic cyanide compounds, which is very harmful to the environment and operators

Method used

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  • Preparation method of pentaerythritol tetra(3-n-dodecylthiopropionate)
  • Preparation method of pentaerythritol tetra(3-n-dodecylthiopropionate)

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 161.9g (0.80mol) of 1-dodecylmercaptan (0.80mol) and 0.35g (0.0088mol) of sodium hydroxide to a 500ml reactor equipped with a stirrer, thermometer, condenser, nitrogen conduit and dropping funnel, and start to pass through Inject nitrogen, stir and heat up to 30°C, slowly add 70.4g (0.20mol) of pentaerythritol tetraacrylate dropwise to make the temperature between 30-45°C, then keep the reaction at 40°C for 4h, and recover excess 1-dodecyl by vacuum distillation Mercaptans. Adjust the pH to 6-7 with formic acid, recrystallize by adding methanol, filter and dry to obtain 217.4 g of white crystalline powder product, with a yield of 93.5% (based on pentaerythritol tetraacrylate). The obtained product has a liquid phase test purity of 99.1%, and the peak time is consistent with the standard sample, such as figure 1 As shown, the structure of the obtained product was characterized by infrared spectroscopy [2919cm-1 (methyl), 2851cm-1 (methylene), 1741cm-1 (ester carbony...

Embodiment 2

[0028] Add 166.0g (0.82mol) of 1-dodecylmercaptan and 0.35g (0.0065mol) of sodium methoxide into a 500ml reactor equipped with a stirrer, a thermometer, a condenser, a nitrogen conduit and a dropping funnel, and start feeding Nitrogen, stirred and heated to 30°C, slowly added 70.4g (0.20mol) of pentaerythritol tetraacrylate dropwise to make the temperature between 30-45°C, then kept at 40°C for 4 hours, and recovered excess 1-dodecylsulfur by distillation under reduced pressure alcohol. Adjust the pH to 6-7 with formic acid, add methanol for recrystallization, filter and dry to obtain 224.4 g of a white crystalline powder product with a yield of 96.6% and a purity of 99.2%.

Embodiment 3

[0030] Add 170.0g (0.84mol) of 1-dodecylmercaptan and 0.53g (0.0098mol) of sodium methoxide into a 500ml reactor equipped with a stirrer, thermometer, condenser, nitrogen conduit and dropping funnel, and start feeding Nitrogen, stirring and heating up to 40°C, slowly dropwise add 70.4g (0.20mol) of pentaerythritol tetraacrylate to make the temperature between 40-55°C, then keep the reaction at 50°C for 6h, and recover excess 1-dodecylsulfur by distillation under reduced pressure alcohol. Adjust the pH to 6-7 with glacial acetic acid, add absolute ethanol for recrystallization, filter and dry to obtain 226.2 g of a white crystalline powder product with a yield of 97.3% and a purity of 99.5%.

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Abstract

The invention provides a preparation method of pentaerythritol tetra(3-n-dodecylthiopropionate), which initially provides a one-step synthesis method of pentaerythritol tetra(3-n-dodecylthiopropionate) from pentaerythritol tetraacrylate and 1-dodecyl mercaptan. The method comprises the following steps: adding 1-dodecyl mercaptan and a catalyst into a reactor, dropwisely adding pentaerythritol tetraacrylate at 40-60 DEG C to react, distilling out excessive 1-dodecyl mercaptan under reduced pressure, adding formic acid or glacial acetic acid to regulate the pH value to 6-7, adding a crystallization solvent to recrystallize, filtering, and drying to obtain the white crystalline powder product. Compared with the prior art, the novel method provided by the invention has the advantages of simple technique, low equipment and operation cost, energy saving, environmental protection, high product quality and high yield.

Description

technical field [0001] The invention relates to a preparation method of sulfur-containing antioxidant, in particular to a preparation method of pentaerythritol tetrakis (3-n-dodecylthiopropionate). Background technique [0002] Pentaerythritol tetrakis(3-n-dodecylthiopropionate), which has the molecular formula C 65 h 124 o 8 S 4 , the pure product is white solid powder or crystal, due to its high molecular weight, low volatility, and good persistence, it exhibits excellent high temperature resistance and water extraction resistance, and the synergistic effect with phenolic antioxidants is greater than DSTDP and DLTDP et al. It is suitable for PP, PE, ABS, etc., especially suitable for polyolefin products that are susceptible to water damage or used under severe climate conditions, and has great application value in polymer fibers. In addition, as environmental protection issues become increasingly prominent, pentaerythritol tetrakis (3-n-dodecylthiopropionate) has biod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/14
Inventor 李萍孙春光汤翠祥李海平范小鹏彭啸张文轩
Owner RIANLON
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