Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of preparation method of antioxidant 168

A technology of antioxidant and preparation process, which is 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 thorough separation, good test effect and simple operation

Active Publication Date: 2022-03-04
CHAMBROAD CHEM IND RES INST CO LTD
View PDF13 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of 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.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
acid valueaaaaaaaaaa
purityaaaaaaaaaa
Login to View More

Abstract

The invention belongs to the field of preparation of antioxidants, and in particular relates to a preparation method of antioxidant 168. The specific preparation method is as follows: (1) adding 2,4-di-tert-butylphenol, a solvent and a resin catalyst into a reactor, Stir and heat up; Add phosphorus trichloride dropwise to the reactor at a constant speed, after the reaction ends, add resin as a neutralizer to neutralize the reaction solution to neutrality; (2) filter the reaction solution obtained in step (1), Filter out the solid resin; the filtrate is processed to obtain the antioxidant 168 product; (3) the resin filtered out by step (2), a part is directly used as a catalyst for the synthesis reaction of the next batch; the rest are regenerated as intermediate Apply with the agent. The catalyst used in the present invention can be separated from the system simply, quickly and thoroughly after the reaction is completed, can be used continuously and without generating solid waste, can effectively improve the quality of the antioxidant 168 product, and reduce environmental pollution.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com