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Continuous preparation method of antioxidant 1076

A technology of antioxidant and catalyst, which is applied in the field of continuous preparation of antioxidant 1076, which can solve the problems of high equipment requirements, long reaction time, and high production cost, and achieve the effects of low equipment requirements, short reaction time, and less by-products

Pending Publication Date: 2022-07-26
陕西艾科莱特新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production process of antioxidant 1076 is mainly a batch method, using β-(3,5-di-tert-butyl-4-hydroxyphenyl) methyl propionate (3,5-methyl for short) and n-octadecyl Carbon alcohol is used as raw material, alkali metal compound is used as catalyst, and it is produced by transesterification reaction under vacuum conditions. The reaction process is to put the reaction raw materials and catalyst together into the reactor for reaction. Reaction, this kind of batch production process has long reaction time, discontinuous reaction, differences in quality between batches, and vacuum conditions have high requirements on equipment, resulting in high production costs

Method used

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  • Continuous preparation method of antioxidant 1076
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  • Continuous preparation method of antioxidant 1076

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The molar ratio of β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate to n-octadecyl alcohol is 1.1:1, the catalyst lithium amide and β-(3,5-di-tert-butyl) The mass ratio of methyl-4-hydroxyphenyl) propionate was 1:100, the temperature of the first tube reactor was 100°C, the pressure was 5bar, the residence time was 10min, the temperature of the second tube reactor was 150°C, and the pressure was 5bar, The residence time is 10min, the crude product of antioxidant 1076 is prepared by removing toluene, then adding methanol to fully dissolve, adding acetic acid to adjust the pH to neutrality, filtering and crystallizing at a constant temperature of 35 ° C to obtain the product of antioxidant 1076, the yield is 97.1%, through the gas phase Chromatographic analysis, the purity is 99.6%, and other test results are shown in Table 1.

Embodiment 2

[0031] The molar ratio of β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate to n-octadecyl alcohol is 1.1:1, the catalyst sodium methoxide and β-(3,5-di-tert-butyl) The mass ratio of methyl-4-hydroxyphenyl) propionate was 1:100, the temperature of the first tube reactor was 150°C, the pressure was 1bar, the residence time was 30min, the temperature of the second tube reactor was 200°C, and the pressure was 1bar, Residence time 30min. Toluene was removed from the prepared 1076 crude product, methanol was added to fully dissolve it, acetic acid was added to adjust the pH to neutrality, acetic acid was added to adjust the pH to neutrality, and after filtration, the product was obtained by crystallization at a constant temperature of 45° C. to obtain antioxidant 1076 product with a yield of 97.3%. Gas chromatographic analysis, the purity is 99.8%, other test results are shown in Table 1.

Embodiment 3

[0033] The molar ratio of β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate to n-octadecyl alcohol is 1.2:1, the catalyst lithium amide and β-(3,5-di-tert-butyl) The mass ratio of methyl-4-hydroxyphenyl) propionate was 1:100, the temperature of the first tube reactor was 150°C, the pressure was 1bar, the residence time was 30min, the temperature of the second tube reactor was 200°C, and the pressure was 1bar, Residence time 30min. Toluene was removed from the prepared 1076 crude product, methanol was added to fully dissolve it, formic acid was added to adjust the pH to neutrality, and after filtration, the product was crystallized at a constant temperature of 39 ° C to obtain antioxidant 1076 product, the yield was 96.8%, and the purity was 99.6% by gas chromatography analysis, Other test results are shown in Table 1.

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Abstract

The invention relates to a continuous preparation method of an antioxidant 1076, and belongs to the technical field of antioxidant production. The method comprises the following steps: respectively dissolving beta-(3, 5-di-tert-butyl-4-hydroxyphenyl) methyl propionate, octadecanol and a catalyst in a material preparation kettle, sequentially adding the dissolved materials into a material mixing kettle according to a ratio through a flow pump, mixing, reacting through two groups of tubular reactors, setting different temperatures for a first tubular reactor and a second tubular reactor, and carrying out high-temperature crystallization to obtain the beta-(3, 5-di-tert-butyl-4-hydroxyphenyl) methyl propionate. According to the present invention, the antioxidant 1076 can be continuously produced, the problems of unstable parameters and mass difference between batches of the traditional intermittent production process are avoided, the method has characteristics of short reaction time, less by-products, high yield and the like, the product yield is more than 96.5%, the production cost is low, and the method is suitable for industrial production. And the purity of the product reaches 99.8% or above.

Description

technical field [0001] The invention belongs to the technical field of antioxidant production, and in particular relates to a continuous preparation method of antioxidant 1076. Background technique [0002] Antioxidants have good antioxidant properties, stable oxidative stability and thermal stability, good compatibility with polymers, extremely low volatility, not easy to be lost due to volatilization at high temperatures, and can effectively prevent light and heat. , oxygen damage to the polymer, significantly improve the performance of the polymer, effectively prolong the life of the polymer, no pollution, no coloring, can be widely used in general plastics, engineering plastics, synthetic rubber, fibers, resins, inks, coatings and other industries middle. [0003] Antioxidant 1076, scientific name β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid n-octadecyl ester, is a hindered phenolic antioxidant with good heat resistance and water extraction resistance It is wide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/03C07C67/48C07C67/60C07C67/52C07C69/732
CPCC07C67/03C07C67/48C07C67/60C07C67/52C07C69/732
Inventor 齐涛许才宇
Owner 陕西艾科莱特新材料有限公司
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