Method for preparing acyl and bisacyl phosphine oxide or acyl and bisacyl sulfur phosphines

A bisacylphosphine oxide and compound technology, which is applied in the field of preparation of acylphosphine and its derivatives, can solve the problems of many steps, low yield, high cost of raw materials, etc., and achieve the effects of low cost, fast finished product and easy operation

Inactive Publication Date: 2008-06-18
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

However, there are many steps, the cost of raw materials is high, and the yield is low

Method used

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  • Method for preparing acyl and bisacyl phosphine oxide or acyl and bisacyl sulfur phosphines
  • Method for preparing acyl and bisacyl phosphine oxide or acyl and bisacyl sulfur phosphines
  • Method for preparing acyl and bisacyl phosphine oxide or acyl and bisacyl sulfur phosphines

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Embodiment

[0033] 880kg chlorobenzene, 20kg water and 175kg2,4,6-trimethylbenzaldehyde (TPO-A: 2,4,6-trimethylbenzaldehyde alias: rice aldehyde Mesitoldehyde) were dropped into a 3000L reactor, stirred, and Condensed water was passed into the jacket to reduce the temperature of the reactor to below 5°C. Add 230kg phenyl phosphorus chloride, the temperature in the reactor remains on room temperature or below room temperature (reaction solution becomes turbid) all the time in the process of adding. After the addition was complete, the reactor was allowed to heat up naturally. After rising to room temperature, react for 1-2 hours. Then, feed condensed water into the reactor jacket, lower the temperature of the reactor to below 10° C., and adjust the pH value to 1-2 with 20% NaOH aqueous solution.

[0034] The temperature of reactor remains on below 10 ℃, adds 12kg catalyst (vanadium catalyst: V 2 o 5 ) and 190kg tert-butanol peroxide, the temperature during the reaction was no more than...

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Abstract

The invention relates to a preparation method of single acyl or two acyl phosphine oxide and single acyl or two acyl sulfur phosphine compound, in particular to a preparation method of the 2,4,6-trimethylbenzene formacyl-diphenyl phosphine oxide of the photoinitiator. The addition reaction is carried out between Trimethyl benzaldehyde and diphenyl phosphorus chloride and then the mixture is oxidized by tert-butyl alcohol peroxide. The invention adopts the addition reaction of aldehyde and halogenated phosphorus and replaces the original process of acyl chloride and halogenated phosphorus, and has the advantages of greatly shortening the preparation procedures, low cost, easy operation and quick production. The compound prepared by the invention has more than 98 percent of the 2,4,6-trimethylbenzene formacyl-diphenyl phosphine oxide and can be served as the photoinitiator for solid for producing the solidification product with the performance of paint, varnish, porcelain glaze, paint, pigment or ink, and can better satisfy the increasing market demand.

Description

technical field [0001] The present invention relates to a preparation method of acyl phosphine and its derivatives, which is a preparation method of mono- and bis-acyl phosphine oxide or mono- and bis-acyl phosphine sulfur compounds, in particular a photoinitiator 2,4,6-trimethyl Preparation method of benzoyl-diphenylphosphine oxide. Background technique [0002] Photoinitiators are mainly used in the initiation of monomers in radiation (UV) curable coatings. Because UV curable coatings have the advantages of fast curing speed, energy saving, low pollution, and good physical properties, the current application surface has been from wood coating to printed matter glazing. , ink curing, optical fiber manufacturing expanded to automotive metal parts coating and many other fields. Although the photoinitiator only accounts for 3%-5% in the UV coating system, its price is much higher than other components, accounting for about 1 / 3-1 / 4 of the total cost. Therefore, the research o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53C08F2/50C09D7/12
Inventor 陈波李晨曦解敏雨陈建新佐毅王弘蕾
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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