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Preparation method of antioxidant 168

An antioxidant and preparation technology, applied in the field of antioxidant preparation, can solve the problems of excessive solid waste generation and difficult product refining, and achieve the effects of complete separation, excellent hydrolysis resistance and high catalyst activity

Active Publication Date: 2019-12-20
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the shortcomings of difficult product refining and high solid waste generation due to the use of liquid organic base in the current preparation process of antioxidant 168, the present invention proposes a preparation method of antioxidant 168, using a weak base type large Porous anion exchange resin is used as a catalyst to prepare antioxidant 168. The catalyst used can be easily, quickly and completely separated from the system at the end of the reaction. It can be used continuously and does not generate solid waste, which can effectively improve the antioxidant 168 product. quality, and reduce environmental pollution

Method used

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  • Preparation method of antioxidant 168

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 646g of 2,4-di-tert-butylphenol, 410g of benzene and 40g of weak base type macroporous anion exchange resin (model D301, Hunan Zhuzhou Xiangzhong Resin Co., Ltd.) Add 137g of phosphorus trichloride dropwise for 4 hours. After the addition, raise the constant temperature to 90°C and keep the temperature for 4 hours. The HCl gas generated during the reaction process is absorbed by the falling film absorption tower. After the reaction, add a weak base macroporous anion exchange 61g of resin (type D301, Hunan Zhuzhou Xiangzhong Resin Co., Ltd.) was used as a neutralizing agent to neutralize the reaction solution to neutrality. The obtained reaction liquid was filtered, and the solid resin was filtered out; the filtrate was precipitated, washed, crystallized, filtered, and dried to obtain 644.5 g of the antioxidant 168 product.

Embodiment 2

[0027] The solid resin part separated in Example 1 was used as the catalyst prepared in 168, and the rest was regenerated by alkali washing, distilled water washing, drying, etc. and used as a neutralizer.

[0028] 628.5g of 2,4-di-tert-butylphenol, 364.5g of toluene and 55.9g of weakly basic macroporous anion exchange resin were put into the reactor, and after the temperature was raised to 46°C, 137g of phosphorus trichloride was added dropwise to the reactor, and Add for 3 hours, after the addition, raise the constant temperature to 110°C, and keep the temperature for 3 hours; the HCl gas generated during the reaction process is absorbed by the falling film absorption tower; Neutral to neutral. The obtained reaction liquid was filtered, and the solid resin was filtered out; the filtrate was precipitated, washed, crystallized, filtered, and dried to obtain 643.6 g of the antioxidant 168 product.

Embodiment 3

[0030] The solid resin isolated in Example 1 was used mechanically in 20 batches, and the part of the solid resin isolated again was the catalyst prepared by 168, and the rest were regenerated by alkali washing, distilled water washing, drying, etc. and used mechanically as a neutralizer. 653g of 2,4-di-tert-butylphenol, 457g of xylene and 51.3g of weak base type macroporous anion exchange resin were put into the reactor, and after the temperature was raised to 50°C, 137g of phosphorus trichloride was added dropwise to the reactor, and the 4h, after the addition, raise the constant temperature to 120°C, and keep the temperature for 3h; the HCl gas generated during the reaction process is absorbed by the falling film absorption tower; Neutral to neutral. The obtained reaction solution was filtered to filter out the solid resin; the filtrate was precipitated, washed, crystallized, filtered, and dried to obtain 644.2 g of the antioxidant 168 product.

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Abstract

The invention belongs to the field of preparation of antioxidants, and particularly relates to a preparation method of an antioxidant 168. The specific preparation method comprises the following steps: (1) adding 2,4-di-tert-butylphenol, a solvent and a resin catalyst into a reaction kettle, and carrying out heating while stirring at a constant speed; dropwise adding phosphorus trichloride into the reaction kettle at a constant speed, and after the reaction is finished, adding resin as a neutralizer to neutralize the reaction solution to be neutral; (2) filtering the reaction solution obtainedin the step (1) to filtering out solid resin, and treating the filtrate to obtain an antioxidant 168 product; and (3) directly using one part of the resin filtered out in the step (2) as a catalyst for a next batch of synthetic reaction, and recycling the rest resin to be used as a neutralizer. The catalyst used in the method can be simply, conveniently, quickly and thoroughly separated from a system after the reaction is finished, can be continuously and mechanically used, and does not generate solid wastes; the product quality of the antioxidant 168 can effectively improved; and environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the field of antioxidant preparation, and in particular relates to a preparation method of antioxidant 168. Background technique [0002] Antioxidant 168 has excellent comprehensive properties, good hydrolysis resistance, high temperature resistance, low volatility, and strong extraction resistance. 1010, 1076, etc. are used together to play a synergistic effect. It is widely used in the processing of PP, HDPE, LDPE, ABS, polycarbonate and other polymers. It is currently the most widely used auxiliary antioxidant at home and abroad. In recent years, with the accelerated development of my country's polymer industry, the demand for antioxidant 168 is also increasing, and the market is expanding. The good market prospects have also intensified the competition among many domestic antioxidant manufacturers. Only high-quality products can win a broader market. [0003] According to literature reports, the preparation of antioxidant...

Claims

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Application Information

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IPC IPC(8): C07F9/145
CPCC07F9/145
Inventor 吕希林马韵升张新飞刘鹏裴立军郭龙龙
Owner CHAMBROAD CHEM IND RES INST CO LTD
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