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Preparation method of anti-oxidizing agent

A technology of antioxidants and solvents, which is applied in the field of antioxidant preparation, can solve the problems of difficulty in industrialization implementation, high requirements for production equipment, and reduced quality of raw materials, and achieve the effects of saving raw material consumption, simple and easy process, and increased yield

Inactive Publication Date: 2008-07-23
RIANLON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But problem is because temperature is higher (material temperature is more than 200 ℃) in rectifying process, easily produces target product 3-(3,5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate and The de-tert-butyl reaction of the raw material 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate methyl ester leads to a decrease in product quality and a decrease in the quality of raw materials; moreover, the requirements for production equipment are high, energy consumption is large, and industrialization It is difficult to implement

Method used

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  • Preparation method of anti-oxidizing agent

Examples

Experimental program
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Effect test

Embodiment 1

[0014] Add 50ml of xylene to a 250ml four-necked flask equipped with a stirrer, a thermometer, a nitrogen conduit, a water separator and a condenser, start stirring, add 27.0g (0.10mol) of n-stearyl alcohol, 3-(3,5- 33.4g (0.12mol) of di-tert-butyl-4-hydroxyphenyl)propionic acid, 0.2g (0.001mol) of monobutylstannoic acid, feed nitrogen gas, heat up to reflux, keep the temperature of the reaction solution at about 160°C, and reflux for dehydration About 4.0 hours, the dehydration is close to the theoretical value. Cool down to 100°C, add 1.0g of activated carbon, keep stirring at 120-130°C for 30 minutes, cool down to 80-100°C, and filter. Recover xylene from the reaction solution at 180°C under normal pressure and reduced pressure (20-50mmHg), cool down to 60°C, add 150ml of isopropanol, crystallize at 25°C, filter through a Buchner funnel, rinse with isopropanol, and Dry to obtain 3-(3,5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate 46.0g, melting point 50-53°C, puri...

Embodiment 2

[0016] Repeat the technique and condition of embodiment 1, xylene is replaced by toluene, and the consumption of toluene is 35ml, and decolorizing agent changes gac into activated clay. Obtain 45.4g of 3-(3,5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propanoate, melting point 50-53°C, purity 98.8%, yield 85.85% (calculated by n-octadecanol ). 8.9 g of 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid was obtained. The final yield was 97.20% [based on 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid].

Embodiment 3

[0018] Repeat the process and conditions of Example 1, replacing isopropanol with ethanol, 0.4 g of monobutyl stannoic acid. Obtain 47.4 g of 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propanoic acid n-stearyl alcohol ester, melting point 50-53° C., purity 98.3%, yield 89.43% (calculated by n-stearyl alcohol ). 8.2 g of 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid was obtained. The final yield was 98.66% [based on 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid].

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Abstract

The invention relates to a preparation method for an antioxidant of 3-(3,5-Di-tertbutyl-4-hydroxyphenyl) propionic octadecyl alcohol ester, which comprises following steps: adding 3-(3,5-Di-tert-butyl-4-hydroxyphenyl) propionic acid, octadecyl alcohol and butylhydroxyoxo-stannane; dewatering through azeotropic esterification reaction; decolorizing using active carbon and active bentonite; filtrating to removing solvent, then melt solution with antioxidant is obtained; adding crystallizing solvent in the melt; crystallizing and filtering to obtain antioxidant; recovering crystallizing solvent in filtrate to obtain distillation residue; adding sodium hydroxide in the distillation residue for reaction; adding extractant to extract octadecyl alcohol; adding sulfate in aqueous phase for acidification reaction; recovering raw material of 3-(3,5-Di-tert-butyl-4-hydroxyphenyl) propionic acid through crystallization and filtration. The antioxidant of 3-(3,5-Di-tertbutyl-4-hydroxyphenyl) propionic octadecyl alcohol ester has the advantages of fully recovering and utilizing raw material of 3-(3,5-Di-tert-butyl-4-hydroxyphenyl) propionic acid and improving yield of product.

Description

technical field [0001] The present invention relates to a kind of preparation method of antioxidant, relate to a kind of preparation method of 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate n-stearyl alcohol ester to be precise, belong to antioxidant Oxidant preparation techniques. Background technique [0002] The preparation method of antioxidant 3-(3,5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate antioxidant, existing technology is to adopt 3-(3,5-di-tert-butyl -4-hydroxyphenyl) methyl propionate and n-stearyl alcohol are raw materials, carry out transesterification reaction and obtain target product in the presence of catalyzer, and reaction formula is as follows: [0003] [0004] R 1 , R 2 =C(CH 3 ) 3 [0005] In the prior art, one of methods is: adopt 3-(3,5-di-tert-butyl-4-hydroxyphenyl) methyl propionate and the molar ratio of n-stearyl alcohol to be greater than 1.0, the temperature of reaction is at 150-200°C, the catalysts...

Claims

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Application Information

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IPC IPC(8): C09K15/06C07C69/22C07C67/035C07C67/48
Inventor 李克国李海平孙春光汤翠祥曹学华
Owner RIANLON
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