Supercharge Your Innovation With Domain-Expert AI Agents!

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

A technology of trimethylbenzoyl and phenyl phosphine oxide, which is applied in the field of preparation of bisphenyl phosphine oxide, can solve the problems of unfavorable safety, many activators, easy to catch fire, etc. The effect of reducing the amount and improving the safety

Pending Publication Date: 2020-12-18
SHANDONG JIURI CHEM TECH CO LTD
View PDF2 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN1328564A discloses a method for preparing mono- or bisacylphosphine, mono- and bisacylphosphine oxide and mono- and bisacylthiophosphine, comprising first using organic P-monohalophosphine or P, P-dihalophosphine or a mixture thereof and alkali Metal or magnesium in combination with lithium, reacted, if desired, in the presence of a catalyst, and then reacted with an acid halide, in the process for the preparation of oxides, the oxidation step is carried out, in the process for the preparation of sulphides, sulfur is used with the resulting The obtained phosphine reacts, but the aromatic hydrocarbon is used as a catalyst in the reaction process, and phenylphosphine hydrogen will be generated during the reaction process, which is easy to catch fire, which is not conducive to the safety of the reaction
[0005] CN100436461C discloses a method for preparing an acyl phosphine, the preparation method comprising: (1) reacting an organophosphorus halide with an alkali metal in the presence of an activator in a solvent, wherein the alkali metal is in the solvent with alkali metal particles having an average particle size of ≤500 μm (2) subsequently react with acid halides; in this reaction, chlorobenzene and / or n-butanol are used as activators, but phenylphosphine hydrogen will still be generated in the preparation process, which is not conducive to the safety of the reaction In addition, a large amount of activator is required, which cannot be recycled, and waste water containing a large amount of organic matter will be produced

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 bis(2, 4, 6-trimethylbenzoyl)phenylphosphine oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0091] This embodiment provides a preparation method of bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide, comprising:

[0092] (1) In a 500mL four-necked bottle, add 11g of sodium metal and 150g of toluene, protect the temperature with nitrogen and raise the temperature to 100°C, start stirring for 3 hours to beat the sodium into sodium sand, and obtain a mixture of sodium sand and toluene;

[0093] (2) Keep the reflux state, add 21g of phenylphosphine dichloride dropwise to the mixture of sodium sand and toluene, add it in about 2h, keep it warm and reflux for 4h, until the reaction solution becomes bright yellow, add 8.2g ( 0.5eq) of urotropine, drop it in about 0.5h, keep warm and reflux for 2h, lower the temperature to 70°C under the protection of nitrogen, add 43g of mesityl benzoyl chloride dropwise, control the reaction temperature at 75°C, add it in about 2h, 75 ℃ heat preservation reaction for 8h;

[0094] (3) After the reaction in step (2) ends, add 120g of water drop...

Embodiment 2

[0099] This embodiment provides a preparation method of bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide, comprising:

[0100] (1) In a 500mL four-necked bottle, add 11g of sodium metal and 150g of toluene, add 8.2g (0.5eq) of urotropine, and heat up to 100°C under nitrogen protection, and stir for 3 hours to beat the sodium metal into sodium sand, and obtain Sodium sand suspension;

[0101] (2) Keep the reflux state, add dropwise 21g phenylphosphine dichloride in the sodium sand suspension in step (1), add about 2h, insulate and reflux for 4h, until the reaction solution becomes bright yellow, nitrogen protection lowers the temperature to At 70°C, add 43g of mesitylene benzoyl chloride dropwise, control the reaction temperature at 75°C, finish adding in about 2 hours, and keep the reaction at 75°C for 8 hours;

[0102] (3) After the reaction in step (2) ends, add 120g of water dropwise to the reaction solution, stir at room temperature for 0.5h, let stand to separate liquids...

Embodiment 3

[0107] This embodiment provides a preparation method of bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide, comprising:

[0108] (1) In a 500mL four-necked bottle, add 20g of metallic sodium and 150g of toluene, protect the temperature with nitrogen and raise the temperature to 100°C, start stirring for 2 hours to beat the sodium into sodium sand, and obtain a mixture of sodium sand and toluene;

[0109] (2) Keep the reflux state, add 21g of phenylphosphine dichloride dropwise to the mixture of sodium sand and toluene, add it in about 2h, keep it warm and reflux for 6h, until the reaction solution becomes bright yellow, add 3.3g ( 0.2eq) of urotropine, drop it in about 0.5h, keep it warm and reflux for 4h, lower the temperature to 70°C under the protection of nitrogen, add 43g of mesityl benzoyl chloride dropwise, control the reaction temperature at 70°C, add it in about 2h, 70 ℃ heat preservation reaction for 10h;

[0110] (3) After the reaction finishes, 120g of water is adde...

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 bis(2, 4, 6-trimethylbenzoyl)phenylphosphine oxide, which comprises the following steps of (1) mixing sodium sand, phenylphosphine dichloride and urotropine in a non-polar solvent to react to obtain a reactant, and (2) adding mesitylene formyl chloride into the reactant obtained in the step (1), reacting, and oxidizing to obtain bis(2, 4, 6-trimethylbenzoyl)phenylphosphine oxide. According to the method, urotropine is used as an activating agent, sodium phenylphosphine can be effectively prevented from being agglomerated to form sodium phenylphosphine polyphosphide, generation of sodium phenylphosphine is promoted, the hydrogen phenylphosphine process is not needed, and the reaction safety is greatly improved; and the preparation process can be realized by only needing a small amount of activating agent, so that the economical efficiency of industrial production is facilitated, the content of organic matters in the wastewater can be reduced, certain environmental benefits are achieved, and the cost is saved.

Description

technical field [0001] The invention belongs to the field of photoinitiators and relates to a preparation method of bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide. Background technique [0002] Acylphosphine oxide compounds are used as high-efficiency photoinitiators, suitable for initiating radiation polymerization of some unsaturated resins under ultraviolet light, especially for white formulations and glass fiber reinforced polyester / styrene systems and with light stabilizers Compatible with varnish systems and paint systems for exterior use, such as for wood, paper, metal, plastics, optical fibers, printing inks and pre-impregnated systems, etc. [0003] Among them, bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide (initiator 819) and (2,4,6-trimethylbenzoyl)diphenylphosphine oxide (initiator TPO) These are two of them that are commonly and widely used. [0004] CN1328564A discloses a method for preparing mono- or bisacylphosphine, mono- and bisacylphosphine oxide and...

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): C07F9/53
CPCC07F9/5337
Inventor 赵国锋张齐毛桂红张建锋杨金明
Owner SHANDONG JIURI CHEM TECH CO LTD
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

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com