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-but

Method used

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  • Preparation method of anti-oxidizing agent

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0013] Example 1

[0014] Add 50ml of xylene to a 250ml four-neck flask equipped with a stirrer, thermometer, nitrogen conduit, water separator and condenser, start stirring, add 27.0g (0.10mol) of n-octadecyl alcohol, 3-(3,5- 33.4g (0.12mol) of di-tert-butyl-4-hydroxyphenyl)propionic acid, 0.2g (0.001mol) of monobutylstannic acid, bubbling in nitrogen, heating to reflux, keeping the temperature of the reaction solution at about 160°C, refluxing for dehydration About 4.0 hours, the dehydration is close to the theoretical value. Cool down to 100°C, add 1.0g activated carbon, stir and keep at 120-130°C for 30 minutes, cool to 80-100°C, and filter. Recover xylene from the reaction solution at 180°C under normal pressure and reduced pressure (20-50mmHg), cool to 60°C, add 150ml isopropanol, crystallize at 25°C, filter through a cloth funnel, rinse with isopropanol, 40°C After drying, 46.0 g of n-stearyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate was obtained, with a melting poin...

Example Embodiment

[0015] Example 2

[0016] The process and conditions of Example 1 were repeated, xylene was replaced with toluene, the amount of toluene used was 35 ml, and the decolorizer was changed to activated carbon as activated clay. Obtained 45.4 g of n-stearyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate, melting point 50-53°C, purity 98.8%, yield 85.85% (calculated as n-octadecyl alcohol) ). 8.9 g of 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid was obtained. The final yield was 97.20% [calculated as 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid].

Example Embodiment

[0017] Example 3

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