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Synthesis method of antioxidant 1076 using solid base catalyst

A solid base catalyst, antioxidant technology, applied in chemical recovery, organic chemistry, ester group and hydroxyl reaction preparation and other directions, can solve the problems of cumbersome post-processing operation, unsatisfactory catalytic effect, difficult recovery of catalyst, etc., to improve catalytic performance. Effect, stable product quality, reducing the effect of three wastes

Active Publication Date: 2013-09-25
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for synthesizing antioxidant 1076 by solid base catalysis, so as to overcome the disadvantages of unsatisfactory catalytic effect, cumbersome after-treatment operation, difficult recovery of catalyst and high cost in the prior art.

Method used

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  • Synthesis method of antioxidant 1076 using solid base catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Add 3g of porous hydroxyapatite to 0.05mol / L Sr(NO 3 ) 2 The solution was mechanically stirred at room temperature for 4 hours, filtered, and the obtained solid was dried at 100°C for 4 hours, and then burned at 400°C for 8 hours to obtain the self-made solid base catalyst of the present invention.

[0018] In a reactor equipped with heating, stirring, thermometer, water separator and reflux condensing device, 58.4 g of methyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate were added at room temperature g (0.2mol) and 54.1g (0.2mol) of stearyl alcohol, 3.0g of the solid base catalyst prepared above, gradually heated up to 100°C while stirring, reacted for 2.0 hours, cooled the reaction solution to room temperature, added 200mL of ethanol, and filtered Recover the solid base catalyst (recyclable after recovery), the filtrate was stirred and cooled at 15°C for 2h, and filtered to obtain 92.73g of white solid, which is the target product of the present invention, antiox...

Embodiment 2

[0020] Add 30g of porous hydroxyapatite to 0.05mol / L tetramethylammonium hydroxide solution, stir mechanically at room temperature for 8h, filter, dry the obtained solid at 100°C for 4h, and then burn at 400°C for 10h to obtain The self-made solid base catalyst of the present invention.

[0021] In a reactor equipped with heating, stirring, thermometer, water separator and reflux condensing device, 58.4 g of methyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate were added at room temperature g (0.2mol) and 59.51g (0.22mol) of stearyl alcohol, 5g of the solid base catalyst prepared above, gradually heated up to 130°C while stirring, reacted for 5.0 hours, cooled the reaction solution to room temperature, added 200mL of ethanol, and recovered by filtration Solid base catalyst (can be recycled after recovery), the filtrate was stirred and cooled at 15°C for 3h, and 100.56g of white solid was filtered, which was the target product of the present invention, antioxidant 1076, with...

Embodiment 3

[0023] Add 30 g of porous hydroxyapatite into 0.05 mol / L potassium hydroxide solution, stir mechanically at room temperature for 12 h, and filter. The obtained solid was dried at 100° C. for 4 hours, and then burned at 500° C. for 12 hours to obtain the self-made solid base catalyst of the present invention.

[0024] In a reactor equipped with heating, stirring, thermometer, water separator and reflux condensing device, 58.4 g of methyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate were added at room temperature g (0.2mol) and 64.92g (0.24mol) of octadecyl alcohol, 8g of the solid base catalyst prepared above, gradually heated up to 110°C while stirring, reacted for 3.0 hours, cooled the reaction solution to room temperature, added 200mL of ethanol, and recovered by filtration Solid base catalyst (recyclable after recovery), the filtrate was stirred and cooled at 15°C for 4h, filtered to obtain 95.65g of white solid, which is the target product of the present invention, ant...

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Abstract

The invention relates to a synthesis method of antioxidant 1076 using solid base catalyst. The 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate and the octadecanol are used as raw materials which are subjected to the interesterification reaction in the presence of a solid base catalyst to obtain the product of antioxidant 1076 with the purity more than or equal to 97.5% and the yield more than or equal to 85%. Compared with the prior art, the method provided by the invention utilizes the prepared solid base catalyst, thus the catalysis effect is improved, and the quality of obtained products is stable; in addition, the solid base catalyst is recyclable and environmental friendly, and the process operation is safe and convenient, therefore the method is suitable for the industrialized and mass production.

Description

technical field [0001] The present invention relates to a method for synthesizing antioxidant 1076, in particular to a method for synthesizing antioxidant 1076 by solid base catalysis. Background technique [0002] Antioxidant 1076, whose chemical name is 3-(3,5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate, is a phenolic antioxidant with excellent performance and compatibility Good, high anti-oxidation efficiency, no coloring, no pollution, washing resistance, extraction, heat resistance, low volatility and so on. The combination of antioxidant 1076 and ultraviolet absorber has a synergistic effect and is a high value-added product. It has been widely used in polyolefins, polyamides, polyesters, ABS resins, synthetic rubbers, greases, paints, lubricants, etc. Also suitable for some food packaging materials. The structural formula of antioxidant 1076 is as follows: [0003] [0004] At present, many patents and literatures have reported the preparation method of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/732C07C67/03
CPCY02P20/584
Inventor 顾慧娟袁振文洪海廖本仁
Owner SHANGHAI HUAYI GRP CO
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