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Method for preparing nitro-containing oxime ester photoinitiator by nitrification in micro-channel

A photoinitiator and microchannel technology, which is applied in chemical instruments and methods, formation/introduction of nitro/nitroso groups, oxime preparation, etc., can solve problems such as inability to use sulfuric acid and nitric acid, difficulty in obtaining target products, and safety issues, etc. problems, to achieve the effect of improving reaction efficiency and safety, enhancing mass transfer and heat transfer capabilities between phases, and ensuring safety

Pending Publication Date: 2020-06-05
泰兴先先化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Oxime ester photoinitiators generally adopt the well-known acylation reaction, oximation reaction, and esterification reaction. Two methods are generally used for nitration: 1. After the acylation reaction is completed, a mixed acid is used for nitration, but when two nitro groups are added, a large amount of Impurities, it is difficult to obtain qualified target products; 2. After esterification and nitration, the oxime ester structure will decompose in large quantities in contact with concentrated sulfuric acid, and sulfuric acid nitric acid mixed acid cannot be used for nitration, only acetic anhydride nitric acid system can be used; due to the presence of oxime ester photoinitiators High activity, easy to decompose, especially the instability of the ester structure under acidic conditions, the use of conventional reactors for reactions, there are risks of material accumulation, temperature rise, product decomposition, and even safety problems

Method used

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  • Method for preparing nitro-containing oxime ester photoinitiator by nitrification in micro-channel
  • Method for preparing nitro-containing oxime ester photoinitiator by nitrification in micro-channel
  • Method for preparing nitro-containing oxime ester photoinitiator by nitrification in micro-channel

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Experimental program
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Effect test

Embodiment 1

[0041]

[0042] The oxime ester initiator intermediate uses N-ethyl carbazole as a raw material, and is prepared through well-known acylation reactions, oximation reactions and esterification reactions.

[0043] Dissolving the oxime ester initiator intermediate in the inert solvent dichloromethane and acetic anhydride to form a solution with a mass fraction of 5% is used as a continuous phase, with nitric acid (mass concentration 60%) as a dispersed phase, the mass fraction of nitric acid and acetic anhydride The ratio is 0.1, the temperature of the nitrification reaction is controlled to be 0°C, and the pressure is 0.3 MPa. The dispersed phase is dispersed into the continuous phase in the membrane dispersed microchannel reactor. The molar ratio of the active ingredient in the nitric acid to the oxime ester initiator intermediate is 2.2, control the residence time of the mixed material (i.e. the nitration reaction time, the same below) to be 5min, after the reaction, the mat...

Embodiment 2

[0045] Using the oxime ester initiator intermediate in Example 1 as a raw material, the experiment was carried out according to this method, and the oxime ester initiator intermediate was dissolved in dimethylformamide and acetic anhydride to form a solution with a mass fraction of 20%. As the continuous phase, nitric acid (mass concentration 60%) is used as the dispersed phase, the mass ratio of nitric acid and acetic anhydride is 0.5, the controlled nitration reaction temperature is 20°C, and the pressure is 0.5MPa. Dispersed in the continuous phase, the molar ratio of active ingredient in nitric acid to oxime ester initiator intermediate is 2.8, and the residence time of the mixed material (i.e. nitration reaction time) is controlled to be 5min. After the reaction, the material enters the phase separation tank for phase separation. The obtained solution was analyzed, and the conversion rate of the oxime ester initiator intermediate was 98.3%, and the selectivity of the produ...

Embodiment 3

[0047]

[0048] Oxime ester initiator intermediate Ⅱ

[0049] The oxime ester initiator intermediate II is prepared from diphenyl sulfide through well-known acylation reaction, oximation reaction and esterification reaction.

[0050] Carry out experiment according to this method, dissolve initiator intermediate in ethylene dichloride and acetic anhydride and be made into the solution that mass fraction is 10% as continuous phase, take nitric acid (mass concentration 60%) as dispersed phase, nitric acid and acetic anhydride The mass ratio is 0.2, the control reaction temperature is 10°C, the pressure is 0.5MPa, the dispersed phase is dispersed into the continuous phase in the membrane dispersed microchannel reactor, and the molar ratio of nitric acid to oxime ester initiator intermediate II is 2.3 , the residence time of the mixed material is controlled to be 8min, and finally the material enters the phase separation tank for phase separation, and the obtained solution is an...

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Abstract

The invention belongs to the technical field of chemical reaction engineering, and relates to a method for preparing a nitro-containing oxime ester photoinitiator from an oxime ester initiator intermediate through a nitration reaction, and particularly provides a method for preparing the nitro-containing oxime ester photoinitiator through nitration in a micro-channel. According to the method, efficient mixing and excellent mass and heat transfer performance of a micro-channel are utilized, nitric acid serves as a dispersion phase in the micro-channel, an intermediate is dissolved in an inert solvent and acetic anhydride to serve as a continuous phase, the two phases are mixed to initiate a reaction, and the reaction is completed in the rear of the micro-channel. Compared with the reactionin the traditional reaction kettle, the conversion rate can be obviously improved, more importantly, the volume of the reactor can be obviously reduced, and the safety of the reaction process is improved.

Description

technical field [0001] The invention belongs to the technical field of chemical reaction engineering, and relates to a method for preparing a nitro-containing oxime ester photoinitiator from an oxime ester initiator intermediate through nitration reaction, and specifically provides a method for preparing a nitroxime by nitration in a microchannel Ester photoinitiator approach. Background technique [0002] Containing nitroxime ester photoinitiator, as disclosed in CN103819583A Chinese patent literature, containing nitrobisxime ester photoinitiator, CN107325206A Chinese patent literature, containing nitrocarbazole oxime ester photoinitiator, CN104076606A China Nitro-containing oxime ester photoinitiators as represented by NO.14 to NO.62 disclosed in the patent literature. Nitroxime-containing ester photoinitiators have excellent application performance in terms of storage stability, sensitivity, development and pattern integrity; they have good compatibility with single-wave...

Claims

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Application Information

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IPC IPC(8): C07D209/88C07C319/20C07C249/12C07C251/66C07C323/47C08F2/48G03F7/004C07B43/02B01J19/00
CPCC07D209/88C07C249/12C07C319/20C08F2/48G03F7/004C07B43/02C07C2601/14C07C2603/18B01J19/0093C07C251/66C07C323/47
Inventor 朱文斌王于峰常军
Owner 泰兴先先化工有限公司
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