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Preparation method of hindered phenol antioxidant

A technology of hindered phenols and antioxidants, applied in the field of preparation of polymer antioxidants, to achieve the effects of solving the three wastes problem, improving yield and product quality, and easy operation

Inactive Publication Date: 2017-05-17
RIANLON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is easy to operate and solves the problem of traditional recovery of 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid methyl ester or 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid The loss of materials and the three wastes in the methyl ester process, improve the yield and product quality of the target antioxidant

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]Put 450.0kg of triethylene glycol and 2150.0kg of 3-methyl-5-tert-butyl-4-hydroxyphenylpropionate methyl ester into a 3000L reaction kettle, heat up and stir, raise the temperature to 120°C, depressurize, and control the absolute pressure in the kettle To 10mmHg, heat preservation and stirring for 1h to remove light components in the material, and then release the pressure with nitrogen, add 2.25kg of lithium acetate catalyst under the protection of nitrogen, then close the nitrogen, carry out decompression reaction to extract methanol, and gradually increase the reaction temperature to 190°C, reduce the pressure in the reactor to 10mmHg, and then keep it under this pressure for 10h. After the reaction, the 245 content (HPLC) of the reaction solution is 91.5%, and the 345 ester content (HPLC) is 4.8%. Cool to 140°C, nitrogen After the pressure is released, put the material into the scraper evaporator for flash evaporation to evaporate the unreacted 345 ester. The temperat...

Embodiment 2

[0032] Put 450.0kg of triethylene glycol and 2050.0kg of 3-methyl-5-tert-butyl-4-hydroxyphenylpropionate methyl ester into a 3000L reaction kettle, heat up and stir, raise the temperature to 120°C, depressurize, and control the absolute pressure in the kettle To 10mmHg, heat preservation and stirring for 1h to remove the light components in the material, and then release the pressure with nitrogen, add 4.50kg of aluminum isopropoxide catalyst under the protection of nitrogen, then close the nitrogen, carry out decompression reaction to extract methanol, and gradually increase the reaction time by 1~2h Temperature to 160°C, reduce the pressure in the reactor to 1mmHg, and then keep the temperature under this pressure for 6h. After the reaction, the 245 content (HPLC) of the reaction solution is 92.9%, the 345 ester content (HPLC) is 3.2%, and the temperature is lowered to 100°C , after the nitrogen pressure is released, put the material into the scraper evaporator for flash evap...

Embodiment 3

[0034] Put 450.0kg of triethylene glycol and 2050.0kg of 3-methyl-5-tert-butyl-4-hydroxyphenylpropionate methyl ester into a 3000L reaction kettle, heat up and stir, raise the temperature to 120°C, depressurize, and control the absolute pressure in the kettle To 10mmHg, heat preservation and stirring for 1h to remove light components in the material, and then release the pressure with nitrogen, add 2.25kg of lithium acetate catalyst under the protection of nitrogen, then close the nitrogen, carry out decompression reaction to extract methanol, and gradually increase the reaction temperature to 160°C, reduce the pressure in the reactor to 5mmHg, and then keep it under this pressure for 8 hours. After the reaction, the 245 content (HPLC) of the reaction solution is 92.9%, and the 345 ester content (HPLC) is 3.2%. Cool to 100°C, nitrogen After the pressure is released, put the material into the scraper evaporator for flash evaporation to evaporate the unreacted 345 ester. The temp...

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PUM

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Abstract

The invention discloses a preparation method of a hindered phenol antioxidant. The method comprises the steps of uniformly mixing 3-methyl-5-tertiary butyl-4-methyl hydroxyphenylpropionate or 3-(3,5-tert butyl-4-hydroxy phenyl) methyl propionate and corresponding alcohol or amine evenly under agitation, carrying out heating, decompression and light fraction removal, adding a catalyst and carrying out heating and decompression for transesterification; infiltrating reaction liquid into a scraper evaporator after reaction is completed or carrying out flash evaporation in short-range distillation equipment and evaporating unreacted 3-methyl-5-tertiary butyl-4-methyl hydroxyphenylpropionate or 3-(3,5-tert butyl-4-hydroxy phenyl) methyl propionate; and cooling and adding acid, carrying out heat preservation and neutralization, filtering out the catalyst through hot filtration, carrying out crystallization and drying to obtain a target product antioxidant. Compared with a traditional method, the preparation method has the advantages of being simple and convenient in operation, the material loss and energy consumption in recovery of 345 ester or 35 methyl ester are reduced, the problems of three wastes in a traditional recovery process is solved, and meanwhile, the yield and quality of the target antioxidant are improved.

Description

technical field [0001] The invention belongs to a preparation method of a polymer antioxidant, in particular to a preparation method of a high-efficiency hindered phenolic antioxidant. Background technique [0002] Hindered phenol antioxidant has the characteristics of high antioxidant efficiency, low volatility, and good oxidation resistance and coloring performance. It has a significant synergistic effect with auxiliary antioxidants (such as thioesters, phosphites, etc.), and can be used in combination with light stabilizers. Give the product excellent weather resistance. [0003] Hindered phenol antioxidants include tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate] pentaerythritol ester (Antioxidant 1010), β-(3,5-di-tert-butyl-4-hydroxy Phenyl) n-octadecyl propionate (antioxidant 1076), triethylene glycol bis[3-(3-tert-butyl-4-hydroxy-5-methylphenyl) propionate] (antioxidant Agent 245), 2.2-oxalamido-bis[ethyl-3-(3,5-di-tert-butyl-4-hydroxyphenyl)]propionate (an...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C67/48C07C67/52C07C69/732C07C231/02C07C231/24C07C235/34C07C231/12C07C233/56
CPCC07C67/03C07C67/48C07C67/52C07C231/02C07C231/12C07C231/24C07C69/732C07C235/34C07C233/56
Inventor 孙春光汤翠祥范小鹏常贻文
Owner RIANLON
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