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Preparation method for 1,3,5-trimethyl-2,4,6-tri(3,5-di-tert-butyl-4-hydroxybenzyl)benzene as hindered phenol antioxidant

A technology of hindered phenols and di-tert-butyl, applied in the field of preparation of plastic additives, can solve the problems of easy loss, short single-pass catalytic life, easy deactivation, etc., to achieve non-corrosive equipment, easy separation and purification, simple operation Effect

Active Publication Date: 2013-12-11
CHIZHOU WANWEI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the 1,3,5-trihalomethyl-2,4,6-trimethylbenzene used in this method has no suitable source for large-scale production
And this solid superacid catalyst belongs to the solid superacid of one-component type, thus in the reaction main active component SO 4 2- It is easy to be lost in the reaction, especially easy to deactivate under higher temperature conditions. Although this type of single-component solid catalyst has good initial catalytic activity, the single-pass catalytic life is short, thus increasing the production cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1:Mix 10 moles of 1,3,5-trimethylbenzene, 70 moles of concentrated hydrochloric acid with a concentration of 36% and 50 moles of paraformaldehyde in the reactor, and then add 200 grams of rare earth composite solid superacid catalyst SO 4 2- / Fe 2 o 3 -La 2 o 3 , then heated and stirred under reflux for 48 hours, the reaction liquid was cooled and precipitated, and the separated solid obtained was dried, then petroleum ether was added to reflux for 1 hour, the rare earth composite solid superacid catalyst was recovered by suction filtration, the filtrate was cooled to precipitate solids, and dried to obtain 9.5 mole 1,3,5-Trichloromethyl-2,4,6-trimethylbenzene, melting point 170~172℃, 1 H NMR (400 MHz, CDCl 3 ): 4.69(s, 6H), 2.50(s, 9H). Mix the obtained 9.5 moles of 1,3,5-trichloromethyl-2,4,6-trimethylbenzene and 3.5 moles of 2,6-di-tert-butylphenol in a reaction kettle, add 500 grams of rare earth compound Solid Superacid Catalyst SO 4 2- / Fe 2 o ...

Embodiment 2

[0024] Mix 10 moles of 1,3,5-trimethylbenzene, 70 moles of concentrated hydrochloric acid with a concentration of 38% and 70 moles of paraformaldehyde in the reactor, and then add 300 grams of rare earth composite solid superacid catalyst SO 4 2- / TiO 2 -Dy 2 o 3 , then heated and stirred under reflux for 36 hours, and the separated solid obtained by cooling the reaction solution was dried, added petroleum ether and refluxed for 2 hours, and the rare earth composite solid superacid catalyst was recovered by suction filtration, and the filtrate was cooled to precipitate a solid, and dried to obtain 9.6 mole 1,3,5-Trichloromethyl-2,4,6-trimethylbenzene, with a melting point of 171-172°C. Mix the obtained 9.6 moles of 1,3,5-trichloromethyl-2,4,6-trimethylbenzene and 3.2 moles of 2,6-di-tert-butylphenol in the reaction kettle, add 25.5 grams of rare earth compound Solid Superacid Catalyst SO 4 2- / Fe 2 o 3 -La 2 o 3 , followed by adding 35 liters of carbon tetrachlor...

Embodiment 3

[0026] Mix 10 moles of 1,3,5-trimethylbenzene, 100 moles of concentrated hydrochloric acid with a concentration of 36% and 80 moles of paraformaldehyde in the reactor, then add 600 grams of rare earth composite solid superacid catalyst SO 4 2- / Al 2 o 3 -La 2 o 3 , then heated and stirred under reflux for 24 hours, the reaction solution was cooled and precipitated and the separated solid was dried, then petroleum ether was added to reflux for 1 hour, the rare earth composite solid superacid catalyst was recovered by suction filtration, the filtrate was cooled to precipitate solids, and dried to obtain 1, 3,5-Trichloromethyl-2,4,6-trimethylbenzene, with a melting point of 170-172°C. Mix the obtained 9.4 moles of 1,3,5-trichloromethyl-2,4,6-trimethylbenzene and 4 moles of 2,6-di-tert-butylphenol in the reaction kettle, add 499 grams of rare earth compound Solid Superacid Catalyst SO 4 2- / Al 2 o 3 -Gd 2 o 3 , followed by adding 39 liters of 1,2-dichloroethane for refl...

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Abstract

The invention discloses a preparation method for 1,3,5-trimethyl-2,4,6-tri(3,5-di-tert-butyl-4-hydroxybenzyl)benzene as hindered phenol antioxidant. The method includes the following steps: 1,3,5-trimethylbenzene and 2,6-di-tert-butylphenol which are cheap and easy to obtain are adopted as main materials, and under the function of SO42- / MxOy-R2O3 as rare earth composite solid super-acidic catalyst, two steps of alkylation reaction are carried out, so that the target product is prepared. The preparation method has the characteristics that: the preparation method is easy to operate, reaction conditions are mild, the product is easy to separate and purify, the single-pass catalysis life of the catalyst is long, the catalyst can be repetitively used and recycled, the production cost is low, and the preparation method is suitable for industrialized clean production.

Description

technical field [0001] The invention belongs to the preparation method of plastic additives, in particular to a hindered phenolic antioxidant 1,3,5-trimethyl-2,4,6-tri(3,5-di-tert-butyl-4-hydroxybenzyl Base) The preparation method of benzene. Background technique [0002] During the manufacture, storage, processing and use of polymer materials, the performance of polymer materials such as plastics and their products will be reduced or lost due to oxidation, resulting in the aging of polymer materials. Adding antioxidants can prevent the material from aging and make it have the necessary antioxidant properties [0003] force. Hindered phenolic antioxidants are the best non-polluting and non-discoloring properties among all antioxidants. [0004] 1,3,5-Trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, whose trade name is Antioxidant 330, is commonly used in plastic processing One of the additives, it is a high-tech, high value-added, and non-environmental pol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/15C07C37/18
CPCY02P20/584
Inventor 李伟军
Owner CHIZHOU WANWEI CHEM
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