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Production method for photoinitiator GR-FMT

A technology of GR-FMT and photoinitiator, which is applied in chemical instruments and methods, organic chemistry, metallocene, etc., can solve the problems of insufficient yield, large discharge of waste water and liquid, and complicated production process, so as to simplify the process , production cost reduction, high product yield effect

Inactive Publication Date: 2012-07-18
HUBEI GURUN TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The disadvantage of this method is that the whole process of Swiss Ciba Refining requires two steps of synthesis reaction, two times of refining and purification, and at least two sets of reaction devices are required.
[0009] The production process is relatively complicated, the yield is not high enough (75-80%), and the discharge of waste water and liquid is relatively large

Method used

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Examples

Experimental program
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Embodiment Construction

[0028] Introduce inert gas argon into the reaction kettle to replace oxygen; add 100kg of xylene and 11kg of 2,5-dimethoxytetrahydrofuran into the replaced reaction kettle, and after cooling down to -4--5°C, slowly add 2 , 20-80kg of 4-difluoroaniline, preferably 10kg, the time of dropping is 4-6 hours, preferably 5 hours, to generate 2,4-difluorophenylpyrrole; --10 hours, preferably 8 hours; then add 200-800kg of xylene, preferably 100kg; then put it into a still with an inert atmosphere, heat up to 140-145°C for distillation; after the distillation is completed, lower the temperature to 25-50°C , preferably 30°C; then put it into a reaction kettle with an inert atmosphere, and put in 8-20kg of titanocene dichloride, preferably 10kg; cool down to 10--40°C, preferably -20°C, and start adding dropwise lithium amide salt ( Such as: sodium diethylpropylamide, lithium diethylpropylamide, sodium diethylamide or lithium diethylamide, the solvent is xylene) 6-10kg, preferably 6.5kg, ...

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Abstract

Provided is a production method for a photoinitiator GR-FMT. The production method includes the following steps: adding dimethylbenzene and 2,5- dimethoxy tetrahydrofuran to a reaction kettle with inert atmosphere, cooling to -4 - 5 DEG C, then slowly dropwise adding 2,4-two fluoroaniline, heating to 50-60 DEG C, and maintaining the temperature for 5-10 hours; adding dimethylbenzene, heating to 140-145 DEG C for distillation; adding titanocene dichloride; cooling to -10- 40 DEG C, dropwise adding a catalyst of organic alkali amino lithium salt, reacting and synthesizing to obtain reaction liquid of the photoinitiator GR-FMT at -10 - 40 DEG C; heating to 15-30 DEG C, and chromatographing; maintaining the temperature and crystallizing; chromatographing, washing with dimethylbenzene, and draining to obtain wet product; and vacuum drying and obtaining the photoinitiator GR-FMT. The production method has the advantages of being fast in curing speed and not requiring heating.

Description

technical field [0001] The invention relates to the field of production methods of chemical products. In particular, it relates to the production method of photoinitiator FMT. Background technique [0002] Photoinitiator is one of the indispensable components in UV curing materials, and it plays a decisive role in the sensitivity of the photocuring system. Photoinitiator GR-FMT (chemical name double 2,6-difluoro-3-pyrrole phenyl titanocene, molecular formula: C 30 h 22 f 4 N 2 Ti, molecular weight 534) is a relatively high-end photoinitiator product, which is only produced by Swiss Ciba Specialty Chemicals in the world. [0003] The production method of Swiss Ciba Specialty Chemicals is a four-step process. [0004] (1) Condensation of 2,5-dimethoxyfuran and 2,4-difluoroaniline at room temperature to obtain crude 2,4-difluorophenylpyrrole. [0005] (2) After steam distillation and recrystallization, refined 2,4-difluorophenylpyrrole is obtained. [0006] (3) React re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/00
Inventor 何长云
Owner HUBEI GURUN TECH CO LTD
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