A kind of method for preparing photoinitiator tpo while by-product benzyl chloride

A photo-initiator and by-product technology is applied in the field of preparing photo-initiator TPO and by-producing benzyl chloride, which can solve problems such as shortening the reaction time, achieve considerable economic benefits, reduce production costs, and realize the effects of large-scale production.

Active Publication Date: 2022-08-05
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method not only overcomes the generation of a large amount of organic gas ethyl chloride in the existing TPO preparation method, avoids the harm to the environment and the problem of ethyl chloride recovery, but also conveniently prepares the important industrial intermediate benzyl chloride, and adopts a one-pot method to save The solvent is used, the process is simplified, the reaction time is shortened, the energy consumption is reduced, the reaction process is safe and easy to control, and it is easy to realize large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Preparation of TPO and benzyl chloride

[0033] Dissolve 109.2 g of benzyl alcohol in 100 ml of toluene, add 108.1 g of sodium carbonate, cool to 15°C, add 221 g of diphenylphosphorus chloride dropwise, and control the temperature to 15±5°C. After the dropwise addition was completed, the temperature was slowly raised to 25°C for 2 hours, and the gas phase monitoring of diphenylphosphorus chloride was completed, and the residual benzyl alcohol was less than 0.5%. After the reaction was completed, the insoluble salt was filtered out.

[0034] The filtrate was heated to 100° C., 200.1 g of 2,4,6-trimethylbenzoyl chloride was slowly added dropwise, and the reaction was continued for 4 h after the drop was completed. After the reaction was completed, the temperature was cooled and crystallized, and the product TPO 300g was obtained by filtration, and the yield was 86.2%. The crystallization mother liquor was subjected to atmospheric distillation of the solvent, ...

Embodiment 2

[0035] Example 2: Preparation of TPO and benzyl chloride

[0036] 110.3 g of benzyl alcohol was dissolved in 100 ml of toluene, 115 g of sodium carbonate was added, the temperature was controlled at 25°C, 221 g of diphenylphosphorus chloride was added dropwise, and the temperature was controlled at 25±5°C. After the dropwise addition was completed, the temperature was slowly raised to 35°C for 3 hours, and the gas phase monitoring of diphenylphosphorus chloride was completed, and the residual benzyl alcohol was less than 0.5%. After the reaction was completed, the insoluble salt was filtered out.

[0037] The filtrate was heated to 110° C., 190 g of 2,4,6-trimethylbenzoyl chloride was slowly added dropwise, the dropping was completed, and the reaction was incubated for 4 h. After the reaction was completed, the temperature was cooled and crystallized, and the product TPO 295g was obtained by filtration, and the yield was 84.8%. The filtrate was evaporated under normal pressu...

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PUM

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Abstract

The method for preparing photoinitiator TPO and by-product benzyl chloride provided by the invention not only avoids the recovery problem of a large amount of organic waste gas such as ethyl chloride in the production of TPO, but also avoids the serious pollution of by-product polychlorine gas in the production of benzyl chloride. question. Benzyl chloride is an important chemical raw material for preparing photoinitiator 369, so the method of the invention greatly reduces the production cost. In addition, the whole process has the advantages of low preparation cost, simple operation process, safe and easy control of the reaction process, and easy realization of large-scale production.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing a photoinitiator TPO and by-producing benzyl chloride simultaneously, and at the same time producing the photoinitiator TPO, an important chemical intermediate benzyl chloride is also produced. Background technique [0002] The photoinitiator TPO (2,4,6-trimethylbenzoyl-diphenylphosphine oxide) is a light yellow powder with a melting point of 91-94°C and an absorption wavelength of 273-370nm. It can generate benzoyl and Phosphoryl radicals are radicals with high initiating activity and are widely used in UV-curable coatings, printing inks, UV-curable adhesives, optical fiber coatings, photoresists, photopolymerized printing plates, and stereolithographic resins. , composite materials, dental fillings, etc. [0003] BASF company discloses a preparation method of TPO in patents US4298738 and US4710523. Toluene, methanol and N,N-diethylaniline are mixed unifo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/53C07C17/361C07C22/04
CPCC07F9/5337C07C17/361C07C22/04
Inventor 赵国锋任凤霞武瑞毛桂红
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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