Preparation method for photoinitiators containing phosphorus

A photoinitiator and solvent technology, applied in the field of preparation of phosphorous photoinitiators, can solve the problems of harsh reaction conditions, high equipment requirements, and many three wastes, and achieve the effects of less three wastes, high yield and simple process flow

Active Publication Date: 2015-03-11
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] Therefore, the cost of preparing 1 and 2 is higher, and the reaction conditions are harsh, the equipment requirements are higher, and the three wastes produced are more

Method used

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  • Preparation method for photoinitiators containing phosphorus
  • Preparation method for photoinitiators containing phosphorus
  • Preparation method for photoinitiators containing phosphorus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: the preparation of 2,4,6-trimethylbenzyl chloride

[0029] Get 400g mesitylene, 1.1L hydrochloric acid (36%), 0.5g phase transfer catalyst octadecyltrimethylammonium bromide (CTAB) after mixing evenly, stir at room temperature for 2h, add 110g paraformaldehyde under stirring, heat up 75 ℃, reacted for 4 hours, and monitored the reaction by GC. After the reaction was completed, cool down to room temperature, add a small amount of isopropanol to break the emulsion, and extract with dichloromethane. The organic phase obtained was first washed with 2mol / L sodium hydroxide solution, and then washed with water. It was dried with anhydrous sodium sulfate and fractionated to collect the fraction with a boiling point of 130-140°C, that is, 2,4,6-trimethylbenzyl chloride, with a yield of 85% and a melting point of 38°C.

Embodiment 2

[0030] Embodiment 2: the preparation of 2,4,6-trimethylbenzyl bromide

[0031] Take 400g mesitylene, 1.5L hydrogen bromide (40%), 0.7g phase transfer catalyst octadecyltrimethylammonium bromide (CTAB) and mix evenly, stir at room temperature for 2h, add 110g paraformaldehyde under stirring, Raise the temperature to 40-45°C, react for 3.5 hours, and monitor the reaction by GC. After the reaction, cool down to room temperature, add a small amount of isopropanol to break the emulsification, extract with 600ml of dichloromethane, stir evenly, put the separatory funnel to stand for stratification, and separate The organic layer was taken out, the aqueous layer was extracted twice with 300ml dichloroethane, the combined organic layers were washed with 5% N a HCO 3 Wash once with 400ml of aqueous solution, separate the water layer, wash twice with 400ml of water, dry over magnesium sulfate, remove the solvent, distill under reduced pressure, collect: 118°C / 2mmHg fraction 622g, yield...

Embodiment 3

[0032] Embodiment 3: the preparation of sodium phenyl phosphide

[0033]Under the protection of nitrogen, suspend sodium block (10.3g, 0.448mol) in 400g of anhydrous toluene at room temperature, stir and heat to reflux, when the temperature rises to 98°C, start stirring vigorously for 0.5-1h to form sodium sand, and reflux Dichlorophenylphosphine (20.1 g, 0.112 mol) was dissolved in 170 g of toluene under the conditions, and was added dropwise to sodium sand. The drop was completed in 1 hour, and the reaction was refluxed for 24 hours to obtain a bright yellow precipitate. Since sodium phenyl phosphide is unstable, the next step reaction was not carried out without separation.

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Abstract

The invention relates to a preparation method for a plurality of photoinitiators containing phosphorus. The preparation method comprises the steps of taking 2,4,6-trimethylphenyl halogen methane as a raw material, allowing 2,4,6-trimethylphenyl halogen methane to react with sodium phosphine to be oxidized, obtaining a phosphine oxide intermediate, finally, executing a key reaction step, namely the reaction that alpha-carbon is oxidized into ketone, and obtaining a high-yield target oxidation product through oxidation with an oxidizer under the action of a catalyst. The raw material required by the method is low in price and easy to obtain; process equipment is simple; and the method is easy to operate and low in cost.

Description

technical field [0001] The invention relates to the field of chemical product preparation, in particular to a method for preparing a phosphorescent initiator. Background technique [0002] Acylphosphine oxide photoinitiators are a class of excellent photoinitiators, the most important of which are TPO and 819 (also known as BAPO). TPO has sufficient solubility in the active diluent, and its absorption wavelength can reach 430nm. After photolysis, it produces two highly active free radicals (s-trimethylbenzoyl free radical and diphenylphosphonyl free radical) base). The maximum absorption wavelength of 819 can reach 450nm, and after photolysis, it produces three highly active free radicals (two mes-trimethylbenzoyl free radicals and one diphenylphosphonyl free radical). These two photoinitiators belong to photoinitiators with good comprehensive performance, and have been widely used in photoinitiated polymer materials. [0003] [0004] The preparation of the above two ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/53
Inventor 赵国锋张齐卢建华夏风振陈波武瑞毛桂红杨天艳
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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