Continuous preparation method of photoinitiator

A photoinitiator and pipeline reactor technology, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of low production efficiency and quality differences between different batches, and achieve high production efficiency and high product quality. The effect of stability and short process flow

Inactive Publication Date: 2019-04-26
维思普新材料(苏州)有限公司
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Problems solved by technology

[0007] The purpose of the present invention is to provide a method for preparing tribromomethylphenyl sulfone photoinitiator using a pipeline reacto

Method used

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  • Continuous preparation method of photoinitiator
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  • Continuous preparation method of photoinitiator

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preparation example Construction

[0027] The invention provides a continuous preparation method of a photoinitiator, wherein, in a pipeline reaction system, preferably in a pipeline reactor, methyl phenyl sulfone and sodium hypobromite solution react according to the following reaction formula to obtain three Bromomethylphenylsulfone,

[0028]

[0029] The sodium hypobromite solution is prepared from bromine, liquid caustic soda and sodium hypochlorite solution.

[0030] In the prior art in the past, sodium hypobromite solution is prepared by bromine and liquid caustic soda, and reaction formula is as follows:

[0031]

[0032] However, with this preparation method, the utilization rate of bromine is only 50%, and bromine usually exists in the form of sodium bromide in the aqueous solution and has no reactivity. And the present invention is by continuing to add sodium hypochlorite solution in the sodium hypobromite solution (containing sodium bromide) after bromine and liquid alkali reaction, sodium bro...

Embodiment 1

[0048] Sodium hypobromite solution preparation:

[0049] Add 56.7g of bromine dropwise into 193g of 15%w liquid caustic soda at 0-5°C, stir for half an hour, then add 225g of sodium hypochlorite solution into the reaction solution, stir for half an hour to obtain sodium hypobromite solution for later use. In other embodiments, the sodium hypobromite solution is formulated and used according to this ratio.

[0050] Preparation of reaction solution:

[0051] In a 20L reactor at 20°C, add 674g of methyl phenyl sulfone, 1.5kg of 30%w liquid caustic soda, 3.4g of catalyst, and 9.5kg of sodium hypobromite solution in sequence, stir for half an hour until the feed liquid is uniform, and keep Stir and set aside. (Methyl phenyl sulfone to sodium hypobromite molar ratio=1:3)

[0052] The reaction raw materials are fed into the pipeline reactor in the form of slurry, and the mass concentration of methylphenyl sulfone is 6%w. The reaction slurry volume flow rate is 10L / h. Pipeline re...

Embodiment 2

[0054] In a 20L reactor at 20°C, sequentially add 674g of methyl phenyl sulfone, 1.5kg of 30%w liquid caustic soda, 3.4g of catalyst, and 9.5kg of sodium hypobromite solution, and stir for half an hour until the feed liquid is uniform, then keep stirring spare. (Methyl phenyl sulfone to sodium hypobromite molar ratio=1:3)

[0055] The reaction raw materials are fed into the pipeline reactor in the form of slurry, and the mass concentration of methylphenyl sulfone is 6%w. The reaction slurry volume flow rate is 15 L / h. Pipeline reactors 1 to 5 are reaction modules, the temperature is controlled at 100°C, the reaction is carried out under normal pressure, and the residence time is 2.4 minutes. Pipeline reactor 6 is a cooling module, and the temperature is controlled at 25°C. After post-processing and liquid chromatography analysis, the content of the finished product is 99.8% by mass.

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Abstract

The invention relates to a continuous preparation method of a photoinitiator. The method comprises the following steps: in a pipeline reaction system, methyl phenyl sulfone and a sodium hypobromite solution are subjected to a reaction in a pipeline reactor preferably according to the equation shown in the description, and phenyl tribromomethyl sulfone is prepared. The preparation method is simpleand high in production efficiency, and production cost is reduced; meanwhile, the product has stable quality and higher purity; the technical process is short, the safety is high, and the method is suitable for large-scale continuous industrial production. Part of sodium hypobromite is replaced with sodium hypochlorite, so that environmental protection is realized and production cost is reduced.

Description

technical field [0001] The invention relates to a photoinitiator, especially a continuous preparation method of a tribromomethylphenyl sulfone photoinitiator, belonging to the technical field of functional materials. Background technique [0002] Photoinitiator (PI for short) is a key component of photocurable materials, which plays a decisive role in the photocuring speed of photocurable materials. A photoinitiator is a substance that can absorb radiation energy, undergo photochemical changes after being excited, and produce active intermediates (free radicals or cations) with the ability to initiate polymerization. Photoinitiators can be divided into ultraviolet photoinitiators (absorbing ultraviolet light region 250-420nm) and visible light initiators (absorbing visible light region 400-700nm) due to different absorption of radiation energy. Photoinitiators can be divided into two categories: free radical photoinitiators and cationic photoinitiators due to the different ...

Claims

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Application Information

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IPC IPC(8): C07C315/04C07C317/14C08F2/48C01B11/20
CPCC01B11/20C07C315/04C08F2/48C07C317/14
Inventor 袁晓冬陈潇刘海丰陈华于利民
Owner 维思普新材料(苏州)有限公司
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