Method for preparing antioxidant
A technology of di-tert-butyl and hydroxyphenyl, which is applied in the field of preparation of antioxidant-N.N'-di[2-ethyl-3 propionate group] oxalamide, which can solve the problem of low yield and long reaction time and other problems to achieve the effect of increasing yield, improving product quality and shortening reaction time
Inactive Publication Date: 2010-06-23
天津市北方金恒新材料有限责任公司
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Problems solved by technology
This preparation method mostly adopts dibutyltin oxide, dioctyltin oxide, dibutyltin dilaurate and stannous oxalate etc. in the transesterification catalyst of preparation process, and the removal of low boiling point by-product has decompression method and solvent carrying method, Therefore, the yield of the product is low and the reaction time is long
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[0011] Put 150 grams of 3-(3.5 di-tert-butyl-4-hydroxyphenyl) methyl propionate, 42.4 grams of N.N'-dihydroxyethyl oxalamide, 50 ml of xylene, and 1.5 grams of alkyl stannic acid into 500 ml In the four-neck flask, under the protection of nitrogen, fully mix and stir, and heat the material to 160-190 ° C for 6 hours, after dissolution, decolorization, hot filtration, cooling, crystallization, and drying, N.N'-di[2 -Ethyl-3 (3.5 di-tert-butyl-4-hydroxyphenyl) propionate group] oxamide 140.5 grams, yield 84%, mother liquor recovery can obtain 1.5 grams, yield 9%, total yield is 93 %.
[0012] Reaction equation of the present invention is:
[0013]
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Abstract
A method for preparing N.N'-bis[2-ethyl-3(3.5-di tert butyl-4-hydroxyphenyl) propionic ester group] oxamide is characterized by throwing 3(3.5-di tert butyl-4-hydroxyphenyl) methyl propionate, N.N'-dihydroxyethyl oxamide, dimethylbenzene and alkyl stannate into a reactor in sequence, fully mixing and stirring the materials under the protection of nitrogen, and heating the materials to 160-190 DEG C and reacting for 6h, thus obtaining the N.N'-bis[2-ethyl-3(3.5-di tert butyl-4-hydroxyphenyl) propionic ester group] oxamide through dissolving, decoloring, thermal filtration, cooling, crystallizing and drying. The method has the following advantages and benefits: 1. the method improves the yield by over 10% compared with the traditional methods; 2. the quality of the product is obviously improved, the content is over 99.7% and the light transmittance is over 425nm99%; and 3. the reaction time is shortened.
Description
Technical field: [0001] The present invention relates to a kind of production method of chemical product, relate in particular to a kind of antioxidant-N.N'-bis[2-ethyl-3(3.5 di-tert-butyl-4-hydroxyphenyl) propionate group] oxalamide method of preparation. Background technique: [0002] N.N'-two [2-ethyl-3 (3.5 di-tert-butyl-4-hydroxyl phenyl) propionate group] oxamide, commercial name antioxidant 697, its traditional preparation method is: [0003] Methyl 3-(3.5-di-tert-butyl-4-hydroxyphenyl) propionate and N.N'-dihydroxyethyl oxalamide are reacted at 160-200°C for 6-20 hours under the action of a transesterification catalyst, The removal of low-boiling point by-products has two methods: decompression method and solvent-carrying method. The total yield of N.N'-bis[2-ethyl-3(3.5 di-tert-butyl-4-hydroxyphenyl)propionate]oxamide is about 80%. This preparation method mostly adopts dibutyltin oxide, dioctyltin oxide, dibutyltin dilaurate and stannous oxalate etc. in the trans...
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IPC IPC(8): C07C233/56C07C231/14
Inventor 索士满
Owner 天津市北方金恒新材料有限责任公司