Continuous preparation method of trimethylbenzoyl-diphenylphosphine oxide compound

A technology of trimethylbenzoyl and diphenylphosphine oxide, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve problems such as high risk factors and large environmental pollution problems, to achieve the effect of high safety, environmental protection, and less waste

Pending Publication Date: 2019-09-27
维思普新材料(苏州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved in this application is the problems of large environmental pollution and high risk factor in the existing production method of synthesizing TPO and its derivatives from benzoin or its derivatives, thereby providing a kind of product that is beneficial to the environment and has high product conversion rate. Continuous preparation method of trimethylbenzoyl-diphenylphosphine oxide compound with excellent product quality

Method used

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  • Continuous preparation method of trimethylbenzoyl-diphenylphosphine oxide compound
  • Continuous preparation method of trimethylbenzoyl-diphenylphosphine oxide compound
  • Continuous preparation method of trimethylbenzoyl-diphenylphosphine oxide compound

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Experimental program
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Effect test

Embodiment 1

[0034] The molar flow ratio of 2,4,6-trimethylbenzaldehyde to diphenylphosphine chloride or its derivatives in the pipeline reactor is 1:1, and the reaction raw materials are all fed in the form of solution. According to 74g 2,4,6-trimethylbenzaldehyde, add 400g chlorobenzene to prepare the chlorobenzene solution of 2,4,6-trimethylbenzaldehyde, the concentration is 1.0mol / L; 110g diphenylphosphine chloride is added 400g Chlorobenzene Prepare a chlorobenzene solution of diphenylphosphine chloride with a concentration of 1.0mol / L. The volume flow rate of 2,4,6-trimethylbenzaldehyde solution is 50mL / min, and the volume flow rate of diphenylphosphine chloride is 45mL / min. The reaction was carried out at 2 bar pressure and 30° C. with a residence time of 10 s. Subsequently, the oxidation solution was fed with a volume flow rate of 47 mL / min. According to 0.8g V 2 o 5 , 400g chlorobenzene and 90g tert-butanol peroxide to configure the oxidation solution. The reaction was carrie...

Embodiment 2

[0036] The molar flow ratio of benzaldehyde to diphenylphosphine chloride or its derivatives in the pipeline reactor is 1:1, and the reaction raw materials are all fed in the form of solution. Add 400g chlorobenzene to prepare the chlorobenzene solution of 2 benzaldehyde according to 53g benzaldehyde, concentration is 1.0mol / L; mol / L. The volume flow of benzaldehyde solution is 36mL / min, and the volume flow of diphenylphosphine chloride is 45mL / min. The reaction was carried out at 2 bar pressure and 40° C. with a residence time of 15 s. Subsequently, the oxidation solution starts to feed. According to 0.8g V 2 o 5 , 400g chlorobenzene and 90g tert-butanol peroxide to configure the oxidation solution. The reaction was carried out at 2 bar pressure and 40° C. with a residence time of 10 s. The reaction solution was analyzed by HPLC, and the conversion rate of the product was 98.5%. The reaction solution is precipitated and recrystallized to obtain a finished product with ...

Embodiment 3

[0038]The molar flow ratio of 2,4,6-triethylbenzaldehyde to diphenylphosphine chloride or its derivatives in the pipeline reactor is 1:1, and the reaction raw materials are all fed in the form of solution. According to 95g 2,4,6-triethylbenzaldehyde, add 400g chlorobenzene to prepare the chlorobenzene solution of 2,4,6-triethylbenzaldehyde, the concentration is 1.0mol / L; 110g diphenylphosphine chloride is added 400g Chlorobenzene Prepare a chlorobenzene solution of diphenylphosphine chloride with a concentration of 1.0mol / L. The volume flow rate of 2,4,6-trimethylbenzaldehyde solution is 63mL / min, and the volume flow rate of diphenylphosphine chloride is 45mL / min. The reaction was carried out at 2 bar pressure and 30° C. with a residence time of 10 s. Subsequently, the oxidation solution was fed with a volume flow rate of 47 mL / min. According to 0.8g V 2 o 5 , 400g chlorobenzene and 90g tert-butanol peroxide to configure the oxidation solution. The reaction was carried ou...

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Abstract

The invention discloses a continuous preparation method of trimethylbenzoyl-diphenylphosphine oxide (TPO) and its derivatives. The preparation method comprises: in a tubular reactor, benzaldehyde or its derivative reacts with chlorodiphenyl phosphine or its derivative; and then a catalytic oxidation reaction is directly carried out without separation, and the reaction solution is desolvated and re-crystallized to obtain a TPO product. The conversion rate of the product TPO is 98% and above, and the finished product content reaches 99.5% and above.

Description

technical field [0001] The application relates to the field of organic synthesis, in particular to a continuous preparation method of trimethylbenzoyl-diphenylphosphine oxide compounds (TPO). Background technique [0002] In the field of UV curing, the phosphine-type aromatic ketone compound TPO is a radical photopolymerization initiator containing ethylenically unsaturated system with important industrial application value. 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 radical and diphenylphosphonyl radical) ), belongs to the photoinitiator with good comprehensive performance, and has been widely used in photoinitiated polymerization materials. [0003] The synthesis of TPO mainly has the following methods: [0004] One is prepared by reacting mesityl benzoic acid and corresponding acid chlorides as starting materials. This process releas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53
CPCC07F9/5337
Inventor 袁晓冬陈潇刘海丰陈华
Owner 维思普新材料(苏州)有限公司
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