Preparation method of thiophenol compound antioxidant product

A compound and antioxidant technology, applied in the field of preparation of thiophenol compound antioxidant products, can solve problems such as low yield, non-universal problems, low product yield, etc., achieve high yield, reduce dissolution loss, good quality effect

Active Publication Date: 2013-09-25
宁波福天新材料科技有限公司
View PDF6 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] US4085132 discloses a technical method for preparing antioxidant 1035, which uses 2,6-di-tert-butylphenol, thiodiglycol, and methyl acrylate as raw materials to prepare 2,2'-sulfur Substitute diethyl bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate], its shortcoming is that the difficulty of refining and purifying the product is relatively large, and the product yield is low
[0015] US4228297 and US4694099 respectively disclose a technical method for preparing antioxidant 1035, which uses 2,6-di-tert-butylphenol and methyl acrylate as raw materials, and carries out transesterification under the action of a catalyst to prepare 2,2'-sulfur Diethyl bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate], its disadvantage is that the product is more difficult to refine and purify, and finally the product reaches the expected purity result low yield

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
  • Preparation method of thiophenol compound antioxidant product
  • Preparation method of thiophenol compound antioxidant product
  • Preparation method of thiophenol compound antioxidant product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 120g of 3,5-methyl ester, 29g of thiodiethylene glycol, 1.2g of dibutyltin oxide, 0.4g of 2-[1- (2-Hydroxy-3,5-di-t-pentylphenyl)-ethyl]-4,6-dit-pentyl phenyl acrylate; under nitrogen protection, heat up to 70-85°C and start stirring; heat up to 130-135°C, heat preservation reaction for 0.5h, intensify stirring to fully mix the reaction materials, depressurize until the pressure in the kettle is -0.04Mpa to -0.06Mpa, heat preservation reaction at 130-135°C for 2.5h; heat up to 160°C, the pressure in the kettle -0.05Mpa to -0.06Mpa, heat preservation reaction for 1.0h; heat up to 170°C, pressure inside the kettle is -0.085Mpa to -0.095Mpa, heat preservation reaction for 1.5h; cool down the temperature in the reaction kettle to 125-130°C, and use nitrogen Restore the pressure in the kettle to 0.0Mpa, press 1.0g of triethyl phosphite into the reaction kettle, keep the temperature at 140-145°C for 1.0h, cool down to 50-60°C, and obtain the antioxidant 1035 reaction pro...

Embodiment 2

[0040] Add 120g of 3,5-methyl ester, 25g of thiodiethylene glycol, 0.6g of dibutyltin oxide, 0.5g of 2-tert-butyl -6-(3-tert-butyl-2-hydroxy-5-methylphenyl)-4-methylphenol acrylate; under nitrogen protection, heat up to 70-85°C and start stirring; heat up to 130-135°C , heat preservation reaction for 0.5h, intensify stirring to fully mix the reaction materials, depressurize until the pressure in the kettle is -0.04Mpa to -0.06Mpa, heat preservation reaction at 130-135°C for 1.5h; heat up to 150°C, and the pressure in the kettle is -0.05Mpa to -0.06Mpa, keep warm for 2.0h; heat up to 170°C, the pressure inside the kettle is -0.085Mpa to -0.095Mpa, keep warm for 2.0h; Return to 0.0Mpa, press 1.2g of trimethyl phosphite into the reaction kettle, keep warm at 140-145°C for 1.0h, cool down to 50-60°C to obtain the reaction product containing antioxidant 1035 liquid. Add 300g (including: 245g ethanol, 18g ethylene glycol, 37g water) recrystallization solvent into the reaction kett...

Embodiment 3

[0042]Add 120g of 3,5-methyl ester, 28g of thiodiethylene glycol, 1.0g of dibutyltin oxide, 0.4g of 2-[1- (2-Hydroxy-3,5-di-tert-butylphenyl)-methyl]-4,6-di-tert-butylphenyl acrylate; under nitrogen protection, heat up to 70-85°C and start stirring; heat up to 130-135°C, heat preservation reaction for 2.0h, strengthen stirring to mix the reaction materials fully, reduce pressure until the pressure in the kettle is -0.04Mpa to -0.06Mpa, heat preservation reaction at 130-135°C for 2.0h; heat up to 155°C, the pressure in the kettle -0.05Mpa to -0.06Mpa, heat preservation reaction for 1.5h; heat up to 170°C, pressure inside the kettle is -0.085Mpa to -0.095Mpa, heat preservation reaction for 1.0h; cool down the temperature inside the reaction kettle to 125-130°C, while using nitrogen Restore the pressure in the kettle to 0.0Mpa, press 0.4g of triethyl phosphite into the reaction kettle, keep the temperature at 140-145°C for 0.5h, and cool down to 50-60°C to obtain the antioxidant ...

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

No PUM Login to view more

Abstract

The invention relates to a preparation method of a thiophenol compound antioxidant product, relating to the technical field of preparation of antioxidant products. A process technical method of the thiophenol compound antioxidant product comprises the following steps of: taking 3, 5-methyl ester and thiodiglycol as raw materials, performing ester exchange reaction under the actions of a catalyst and a color blocking agent, and generating a reaction product mixed solution containing 2, 2'-thiodiethyl bis(3-(3, 5-di-tert-butyl-4-hydroxyphenyl) propionate by continuously removing a byproduct, namely methanol during the reaction process; adding an appropriate amount of phosphite ester-like compound into the reaction product mixed solution, and generating a new phosphite ester-like compound by secondary ester exchange reaction; and selecting a recrystallization solvent, performing recrystallization and refining on the reaction product mixed solution, and performing solid-liquid separation to obtain a while granular crystal product.

Description

technical field [0001] The invention relates to a preparation method of a thiophenol compound antioxidant product, which relates to the technical field of antioxidant product preparation, and the thiophenol compound antioxidant product specifically refers to the following formula (I): [0002] [0003] Formula (I) chemical name: 2,2'-thiodiethylbis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]. Background technique [0004] 2,2'-thiodiethylbis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate] (abbreviated as Antioxidant 1035), is a thiophenol compound belonging to Intramolecular composite antioxidant, which is widely used in polymer materials such as polyethylene, polypropylene, polystyrene, ABS resin, and various synthetic rubbers. Antioxidant 1035 is used in combination with hindered phenolic main antioxidants, which has a good synergistic effect and can effectively improve the processing stability, heat resistance stability, color improvement and weather resistance ...

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
IPC IPC(8): C07C323/12C07C319/20C08K5/372
Inventor 杜飞韩斌赵文文张璐李新星
Owner 宁波福天新材料科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap