Check patentability & draft patents in minutes with Patsnap Eureka AI!

A kind of industrial production method of bis(2,6-di-tert-butyl-4-methylphenyl)pentaerythritol phosphite

A technology for pentaerythritol phosphite and pentaerythritol dichlorodiphosphite, which is applied in the field of organic chemical preparation, can solve the problems of difficulty in catalyst separation and recovery, unsuitable for industrial production, easy to cause pollution to the environment, and the like, and achieves high production efficiency , the effect of shortening the reaction cycle and reducing energy consumption

Active Publication Date: 2020-11-27
安徽新秀化学股份有限公司
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disclosed in CN102206234: use pentaerythritol, phosphorus trichloride as raw material, pyridine as catalyst, carry out cyclization reaction to generate pentaerythritol dichlorodiphosphite, and then replace with hindered phenol under the catalysis of triethylamine or tributylamine The reaction generates pentaerythritol bisphosphite. In this reaction, pyridine, triethylamine, and tributylamine are used as catalysts, and triethylamine substances are used as acid-binding agents. The post-treatment process of the synthesis is cumbersome, and the separation and recovery of the catalyst after the reaction It is very difficult, and pyridine is a highly flammable liquid, which is harmful to aquatic organisms and is very dangerous. It is easy to pollute the environment and is not suitable for industrial production.

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 industrial production method of bis(2,6-di-tert-butyl-4-methylphenyl)pentaerythritol phosphite
  • A kind of industrial production method of bis(2,6-di-tert-butyl-4-methylphenyl)pentaerythritol phosphite
  • A kind of industrial production method of bis(2,6-di-tert-butyl-4-methylphenyl)pentaerythritol phosphite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] as per figure 1 The production process flow chart shown carries out the production preparation of bis(2,6-di-tert-butyl-4-methylphenyl) pentaerythritol phosphite (PEP-36), and the steps are as follows:

[0046] (1) Preparation of 2,6-di-tert-butyl-4-methylphenol sodium salt: add 2,6-di-tert-butyl-4-methylphenol and Sodium methoxide, while adding toluene in the primary reaction kettle 2 through the solvent pipeline 3, open the agitator 4, the reaction temperature is 60 ° C, and pass through the N 2 The booster pump 5 makes the pressure in the primary reactor 2 be 200kpa, and the reaction time is 2h, and the mol ratio of the 2,6-di-tert-butyl-4-methylphenol and sodium methylate is 1:1.2, after the reaction finishes , cooled to 20°C, suction filtered in filter 6, and washed twice with toluene to obtain 2,6-di-tert-butyl-4-methylphenol sodium salt;

[0047] (2) Preparation of dichlorodiphosphite pentaerythritol ester solution: add pentaerythritol in the secondary reactor ...

Embodiment 2

[0053] as per figure 1 The production process flow chart shown carries out the production preparation of bis(2,6-di-tert-butyl-4-methylphenyl) pentaerythritol phosphite (PEP-36), and the steps are as follows:

[0054] (1) Preparation of 2,6-di-tert-butyl-4-methylphenol sodium salt: add 2,6-di-tert-butyl-4-methylphenol and Sodium methylate, add xylene in the primary reactor 2 through solvent line 3 simultaneously, open agitator 4, reaction temperature is 80 ℃, pass N 2 The booster pump 5 controls the internal pressure of the primary reactor 2 to be 400kpa, and the reaction time is 1.5h. The mol ratio of the 2,6-di-tert-butyl-4-methylphenol and sodium methylate is 1:1.4, and the reaction ends Afterwards, the temperature was lowered to 50°C, suction filtration was performed in the filter 6, and rinsed twice with xylene to obtain 2,6-di-tert-butyl-4-methylphenol sodium salt;

[0055](2) Preparation of dichlorodiphosphite pentaerythritol ester solution: add pentaerythritol in sec...

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
melting pointaaaaaaaaaa
Login to View More

Abstract

The invention relates to an industrial production method of bis(2,6-ditertiary butyl-4-methyl phenyl) pentaerythritol phosphite. The method comprises the following steps: preparing 2,6-ditertiary butyl-4-methyl hydroxybenzene sodium salt from 2,6-ditertiary butyl-4-methyl hydroxybenzene, sodium methylate and an organic solvent in a primary reaction kettle; preparing a dichlorodiphosphite pentaerythritol ester solution from pentaerythritol, phosphorus trichloride and an organic solvent in a secondary reaction kettle; then adding the 2,6-ditertiary butyl-4-methyl hydroxybenzene sodium salt prepared in the primary reaction kettle into the secondary reaction kettle to prepare a bis(2,6-ditertiary butyl-4-methyl phenyl) pentaerythritol phosphite reaction solution; and then carrying out centrifugalization and impurity removal, freezing, crystallization and separation, centrifugalization and desolvation and drying to obtain the bis(2,6-ditertiary butyl-4-methyl phenyl) pentaerythritol phosphite product. The method is low in cost of raw materials, simple to operate, mild in reaction condition, short in production period of product, high in production efficiency, economical and environmentally friendly and quite suitable for industrial production.

Description

technical field [0001] The invention relates to an industrial production method of bis(2,6-di-tert-butyl-4-methylphenyl)pentaerythritol phosphite, which belongs to the field of organic chemical preparation. Background technique [0002] Antioxidants are important additives in the processing and application of polymer resins, and their applications involve almost all polymers and their material products. With the rapid increase in the output of synthetic materials worldwide, especially general-purpose plastics, the rapid growth of global antioxidant production capacity has been promoted and stimulated. The average annual growth rate of plastic antioxidant production has remained at about 8%, higher than other traditional The growth rate of plastic additives. [0003] Phosphite antioxidant is a kind of antioxidant, which generates stable inactive products by decomposing peroxides produced in the oxidation process, thereby delaying the oxidation process of polymer materials an...

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): C07F9/6574
CPCC07F9/65744C07F9/65746
Inventor 张秀秀唐赟吴春业
Owner 安徽新秀化学股份有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More