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

Preparation method of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide

A technology of trimethylbenzoyl and trimethylbenzoyl chloride, applied in the field of preparation of phenyl bisphosphine oxide, can solve the problems of low yield and poor catalytic effect, and achieve high yield and high yield , high safety effect

Inactive Publication Date: 2019-08-30
王清才
View PDF8 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to solve the problems of poor catalytic effect and low yield in the prior art, and provide a preparation method of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide, which The method has better catalytic effect, higher yield and high safety

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 phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide
  • Preparation method of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide
  • Preparation method of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The present invention uses phenyl phosphorus dichloride as the starting material, replaces chlorine with powdery metal sodium in the presence of nitrogen, then reduces and condenses with 2,4,6-trimethylbenzoyl chloride under weakly alkaline conditions And oxidation reaction prepares phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide product; Specifically this embodiment comprises the following steps:

[0034] Step 1. Open the nitrogen valve, pass nitrogen gas into the synthesis reaction kettle respectively, and add 400kg of toluene into the synthesis reaction kettle after the bubbler bubbles. Heat up with water until no water drops drop, cool down, add 1.1mol of sodium metal and 0.03mol of catalyst (the catalyst is a mixture of potassium tert-butoxide and serine, and the mol ratio of potassium tert-butoxide and serine is 5:1), continue to heat up until the metal sodium is completely dissolved and keep the reaction for 3 hours, add 1.0mol of phenylphosphorous dichloride...

Embodiment 2

[0040] Step 1. Open the nitrogen valve, pass nitrogen gas into the synthesis reaction kettle respectively, and add 500kg of toluene into the synthesis reaction kettle after the bubbler bubbles. Heat up with water until no water droplets drop, cool down, add 1mol of sodium metal and 0.01mol of catalyst (the catalyst is a mixture of potassium tert-butoxide and serine, and the mol ratio of potassium tert-butoxide and serine is 4 : 1), continue to heat up until metal sodium is completely dissolved and keep warm for 3 hours, add 0.8 mol of phenylphosphorous dichloride dropwise, control the temperature at 90° C., keep warm for 4 hours.

[0041] Step 2. Preparation of 2,4,6-trimethylbenzoyl chloride: Add 2 mol of anhydrous aluminum chloride into 5.3 mol of mesitylene, stir, and feed 1 mol of CO at 26-30°C 2 After 8-10 hours, slowly drop the reacted feed liquid into the hydrolysis kettle equipped with dilute hydrochloric acid, the temperature should not exceed 80°C, after the hydroly...

Embodiment 3

[0046] Step 1. Open the nitrogen valve, pass nitrogen gas into the synthesis reaction kettle respectively, and add 600kg of toluene into the synthesis reaction kettle after the bubbler bubbles. Warming up with water until no water drops drop, cooling, adding 1.5mol of sodium metal and 0.05mol of catalyzer (the catalyzer is a mixture of potassium tert-butoxide and serine, and the mol ratio of potassium tert-butoxide and serine is 6:1), continue to heat up until the metal sodium is completely dissolved and keep the reaction for 3 hours, add 1.2mol of phenylphosphorous dichloride dropwise, control the temperature at 120°C, and keep the reaction for 4 hours.

[0047] Step 2. Preparation of 2,4,6-trimethylbenzoyl chloride: Add 2 mol of anhydrous aluminum chloride into 5.3 mol of mesitylene, stir, and feed 1 mol of CO at 26-30°C 2 After 8-10 hours, slowly drop the reacted feed liquid into the hydrolysis kettle equipped with dilute hydrochloric acid, the temperature should not excee...

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 provides a preparation method of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide. The preparation method comprises the following steps: using phenyl phosphorus dichloride as an initial raw material, under the protection of nitrogen, adopting a catalyst (the catalyst is a mixture of potassium tert-butoxide and serine) to replace chlorine with powdery metal sodium, carrying out reduction under a weak alkaline condition, and carrying out condensation and oxidation reaction with 2,4,6-trimethylbenzoyl chloride to prepare a phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide product. The preparation method of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide has better catalytic effect and higher yield; and the metal sodium is prepared into powder in a toluene solvent, and all reaction processes are carried out under the protection of nitrogen, so that the safety is high.

Description

technical field [0001] The invention relates to the technical field of substance synthesis, in particular to a preparation method of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide. Background technique [0002] Phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide is the bisbenzoyl phenyl phosphine oxide in the free radical polymerization photoinitiator. It is a highly efficient photoinitiator and is suitable for Radiation polymerization of some unsaturated resins is initiated by light irradiation. Particularly suitable for white formulations and glass fiber reinforced polyester / styrene systems as well as for exterior varnish systems in combination with light stabilizers, where it can also be cured in deep layers. It itself and its photocleavage products are non-toxic and tasteless; they have good stability and are convenient for long-term storage; the absorption spectrum matches the emission band of the radiation source, and has a high molar extinction coefficient; after a...

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 王清才
Owner 王清才
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