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

Preparation method of 2, 4, 6-trimethylbenzoyldiphenylphosphine oxide

A technology of trimethylbenzoyl diphenyl and diphenyl phosphine oxide, which is applied in the field of preparation of 2,4,6-trimethylbenzoyl diphenyl phosphine oxide, can solve the problem of difficult disposal of solid waste residue, Problems such as large safety hazards and few sources of raw materials achieve the effects of low cost, high environmental protection pressure, and difficult preparation

Inactive Publication Date: 2019-02-01
CHANGSHANG NEWSUN CHEM IND
View PDF8 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are some defects in these preparation methods. In the patent CN99813713.8, metal lithium is used to react with diphenylphosphine chloride. This step reaction not only has low yield but also has the problems of high cost and potential safety hazard; Chinese patent CN10556342A, U.S. patent US5679863 has all used 2,4,6-trimethylbenzaldehyde, and this raw material source is few, and cost is high, and it still needs further oxidation to obtain product after it reacts with diphenylphosphine oxygen; Ph2P (OR ) as raw material, Ph2P(OR) itself is sensitive to water and oxygen, not easy to store and needs to be prepared and used now, post-treatment requires solid-liquid separation, and equipment investment is large; in addition, Ph2P(OR) is synthesized with diphenylphosphine chloride as raw material , and the production process of diphenylphosphine chloride has a large amount of solid waste which is not easy to handle, which has become the main factor restricting the production of TPO

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 2, 4, 6-trimethylbenzoyldiphenylphosphine oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Preparation of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide

[0026] (1) Under the protection of N2, take 120ml (1.35mol) of benzene, 40.0g (0.3mol) of aluminum trichloride, and 120ml (1.35mol) of phosphorus trichloride in a 500ml three-necked flask, stir well, and control the temperature at 70°C Left and right reflux reaction, after 4 hours of reaction, start to heat up and recover the solvent, raise the temperature to 200°C and continue the heat preservation reaction for 2 hours, after the heat preservation is completed, cool to room temperature, and slowly add the reaction solution dropwise to 300mL of 3% dilute hydrochloric acid in an ice bath to control the reaction The temperature does not exceed 20°C, react for 0.5h after dropping, add 100ml of benzene to extract, let it stand still, the water phase and the organic phase are clearly separated, both layers are transparent solutions, separate the organic phase, wash with water, remove the solvent to obt...

Embodiment 2

[0029] Embodiment 2: Preparation of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide

[0030] (1) Under the protection of N2, take 60ml (0.67mol) of benzene, 90.0g (0.67mol) of aluminum trichloride, and 175ml (2.0mol) of phosphorus trichloride in a 500ml three-necked flask, stir well, and control the temperature at 70°C Left and right reflux reaction, after 4 hours of reaction, start to heat up and recover the solvent, raise the temperature to 200°C and continue the heat preservation reaction for 2 hours, after the heat preservation is completed, cool to room temperature, and slowly add the reaction solution dropwise to 300mL of 3% dilute hydrochloric acid in an ice bath to control the reaction The temperature does not exceed 20°C, react for 0.5h after dropping, add 100ml of benzene to extract, let it stand still, the water phase and the organic phase are clearly separated, both layers are transparent solutions, separate the organic phase, wash with water, remove the solvent to o...

Embodiment 3

[0033] Embodiment 3: Preparation of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide

[0034] (1) The preparation process of diphenylphosphine oxide is the same as the (1) step in Example 1.

[0035] (2) Put 49.2g (0.3mol) of 2,4,6-trimethylbenzoic acid and 13.7g (0.1mol) of phosphorus trichloride in a 250ml three-necked flask, raise the temperature to 80°C and control the temperature for 5 hours, after the reaction is completed After standing for stratification, the phosphorous acid in the lower layer was separated, and the supernatant liquid was distilled under reduced pressure to obtain 47 g of refined 2,4,6-trimethylbenzoyl chloride, content: 99.0%, yield: 85.8%.

[0036] (3) The implementation steps are the same as those in Example 2 (3).

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 2, 4, 6-trimethylbenzoyldiphenylphosphine oxide and particularly relates to a method, which comprises that phosphorus trichloride, benzene and aluminumtrichloride as raw materials undergo a reaction, the reaction product undergoes a hydrolysis reaction to produce diphenylphosphine oxide, diphenylphosphine oxide and 2, 4, 6-trimethylbenzoyl chloridedirectly undergo a reaction to produce 2, 4, 6-trimethylbenzoyldiphenylphosphine oxide. The preparation method of TPO solves the problems that the raw materials are difficult to prepare, the cost ishigh, the reaction steps are many, and the yield is low. The preparation method is an eco-friendly preparation process.

Description

technical field [0001] The present invention relates to the preparation technology of 2,4,6-trimethylbenzoyl diphenyl phosphine oxide, especially relates to using phosphorus trichloride, benzene and aluminum trichloride as raw materials, after the reaction, one-step reaction of hydrolysis to synthesize diphenyl phosphine oxide, and then directly react with 2,4,6-trimethylbenzoyl chloride to prepare 2,4,6-trimethylbenzoyldiphenylphosphine oxide. Background technique [0002] 2,4,6-Trimethylbenzoyldiphenylphosphine oxide (TPO for short) is a highly efficient free radical (I) type photoinitiator, its effective absorption peak is 350-400nm, and it can generate Both benzoyl and phosphoryl free radicals can initiate polymerization, so the photocuring speed is fast, and it is suitable for deep curing of thick films. At the same time, TPO also has photobleaching effect, and the coating does not change yellow. It can be completely cured on white or high-titanium dioxide pigmented su...

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 Applications(China)
IPC IPC(8): C07F9/53
CPCC07F9/5337
Inventor 叶正培孙松林谢鹏
Owner CHANGSHANG NEWSUN CHEM IND
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