Method for preparing photoinitiator, namely TPO and simultaneously preparing byproduct, namely benzyl chloride

A photoinitiator and by-product technology, which is applied in the field of preparing photoinitiator TPO and by-product benzyl chloride, can solve the problems of shortening the reaction time, achieve the effects of reducing production costs, avoiding environmental hazards, and reducing recycling costs and losses

Active Publication Date: 2020-05-12
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

[0033] Embodiment 1: the preparation of TPO and benzyl chloride

[0034] Dissolve 109.2g of benzyl alcohol in 100ml of toluene, add 108.1g of sodium carbonate, cool to 15°C, add 221g of diphenylphosphorus chloride dropwise, and control the temperature at 15±5°C. After the dropwise addition, slowly raise the temperature to 25°C and keep it warm for 2 hours. The reaction of diphenylphosphorous chloride is complete by gas phase monitoring, and the residual benzyl alcohol is less than 0.5%. After the reaction was completed, the insoluble salt was filtered out.

[0035] The temperature of the filtrate was raised to 100°C, and 200.1 g of 2,4,6-trimethylbenzoyl chloride was slowly added dropwise, and the reaction was continued for 4 hours after the drop was completed. After the reaction was completed, the temperature was lowered to cool and crystallize, and the product TPO 300g was obtained by filtration, with a yield of 86.2%. The solvent was distilled from the crystallization mot...

Embodiment 2

[0036] Embodiment 2: the preparation of TPO and benzyl chloride

[0037] Dissolve 110.3g of benzyl alcohol in 100ml of toluene, add 115g of sodium carbonate, control the temperature at 25°C, add dropwise 221g of diphenylphosphorus chloride, and control the temperature at 25±5°C. After the dropwise addition, slowly raise the temperature to 35°C and keep it warm for 3 hours. The reaction of diphenylphosphorus chloride is complete by gas phase monitoring, and the residual benzyl alcohol is less than 0.5%. After the reaction was completed, the insoluble salt was filtered out.

[0038] The temperature of the filtrate was raised to 110°C, and 190 g of 2,4,6-trimethylbenzoyl chloride was slowly added dropwise, and the reaction was kept for 4 hours after dropping. After the reaction was completed, the temperature was lowered to cool and crystallize, and the product TPO 295g was obtained by filtration, with a yield of 84.8%. The filtrate was evaporated to remove the solvent under nor...

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PUM

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Abstract

The invention provides a method for preparing a photoinitiator, namely TPO and simultaneously preparing a byproduct, namely benzyl chloride. The method provided by the invention avoids the problem ofrecovery of a large amount of organic waste gas, namely chloroethane and the like in production of the TPO, and also avoids the problem of serious pollution caused by a large amount of the byproduct,namely chlorine in production of the benzyl chloride. The benzyl chloride is an important chemical raw material for preparing a photoinitiator 369, so the method disclosed by the invention greatly reduces the production cost. Meanwhile, the whole process is low in preparation cost, simple in operation process, safe and easily-controllable in reaction process and easy to realize 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 simultaneously producing benzyl chloride by-products. When the photoinitiator TPO is produced, benzyl chloride, an important chemical intermediate, 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 The two free radicals of the phosphoryl group are highly active free radicals, and are widely used in UV-curable coatings, printing inks, UV-curable adhesives, optical fiber coatings, photoresists, photopolymerization printing plates, and stereolithographic resins. , composite materials, dental fillings, etc. [0003] BASF company discloses a preparation method of TPO in patent US4298738 and US4710523, mix toluene, methanol and N,N-diethylanil...

Claims

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Application Information

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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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