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

Method used

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  • Preparation method of antioxidant 168

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0024] Example 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.) into the reactor. After heating to 45℃, put it into the reactor Add 137g phosphorus trichloride dropwise for 4h, after the addition, increase the constant temperature to 90℃, keep the reaction for 4h; the HCl gas produced during the reaction is absorbed by the falling film absorption tower; after the reaction, add the weak base macroporous anion exchange 61 g of resin (model D301, Hunan Zhuzhou Xiangzhong Resin Co., Ltd.) was used as a neutralizer to neutralize the reaction liquid to neutrality. The obtained reaction liquid is filtered to filter out the solid resin; the filtrate is desolventized, washed, crystallized, filtered, and dried to obtain 644.5 g of antioxidant 168 product.

Example Embodiment

[0026] Example 2

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

[0028] Put 628.5g of 2,4-di-tert-butylphenol, 364.5g of toluene and 55.9g of weakly basic macroporous anion exchange resin into the reactor. After the temperature is raised to 46°C, 137g of phosphorus trichloride is added dropwise to the reactor. Add 3h, after the addition, increase the temperature to 110℃, keep the reaction temperature for 3h; the HCl gas produced during the reaction is absorbed by the falling film absorption tower; after the reaction is over, add 45g of weakly basic macroporous anion exchange resin as a neutralizer to the reaction liquid Neutral to neutral. The obtained reaction liquid is filtered to filter out the solid resin; the filtrate is desolventized, washed, crystallized, filtered, and dried to obtain 643.6 g of antioxidant 1...

Example Embodiment

[0029] Example 3

[0030] The solid resin separated in Example 1 is used as a catalyst prepared by 168 after 20 batches of the solid resin separated again, and the rest is used as a neutralizer after being regenerated by alkaline washing, distilled water washing, and drying. Put 653g of 2,4-di-tert-butylphenol, 457g of xylene and 51.3g of weak base type macroporous anion exchange resin into the reactor. After the temperature is raised to 50℃, 137g of phosphorus trichloride is added dropwise to the reactor. 4h, after the addition, increase the constant temperature to 120℃, and keep the reaction temperature for 3h; the HCl gas produced during the reaction is absorbed by the falling film absorption tower; after the reaction, 40.8g of weakly basic macroporous anion exchange resin is added as a neutralizing agent to make the reaction liquid Neutral to neutral. The obtained reaction liquid is filtered to filter out the solid resin; the filtrate is desolventized, washed, crystallized, ...

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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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