Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of alpha-hydroxyketone photoinitiator

A technology of photoinitiator and hydroxyketone, which is applied in the field of preparation of α-hydroxyketone photoinitiator, can solve the problems that the catalyst cannot be recycled, the reaction steps are long, and the cost is high, and the pollution is small, the reaction steps are short, and the cost is low. Effect

Inactive Publication Date: 2019-06-18
孙建
View PDF2 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the extensive use of aluminum trichloride Lewis acid in the current process, a large amount of waste water is generated, the catalyst cannot be recycled, the reaction steps are long, dangerous processes such as chlorine gas also cause great hidden dangers in production, and the cost is high

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of alpha-hydroxyketone photoinitiator
  • Preparation method of alpha-hydroxyketone photoinitiator
  • Preparation method of alpha-hydroxyketone photoinitiator

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0022] A preparation method of α-hydroxyketone photoinitiator, comprises the following steps:

[0023] Step (1): ketone compounds and trihalomethyl substituted benzene and its derivatives are used as raw materials, and react in one step under the action of a polar solvent and a metal catalyst to generate a halogenated intermediate, wherein the feed ratio of the reaction raw materials is ketones Compound: trihalomethyl-substituted benzene and its derivatives: metal catalyst = 0.9-1.5: 1: 1-10, reaction temperature: -50-40°C, general reaction formula (I):

[0024]

[0025] where R 1 , R 2 C1-C6 alkane or R 1 and R 2 Combined into cyclohexyl; R3, R4, R5, R6, R7 are hydrogen, C1-C6 alkane, C1-C6 alkoxy or C1-C6 hydroxyalkyl; X is fluorine, chlorine or bromine;

[0026] Step (2): The halogenated intermediate obtained in step (1) is hydrolyzed under the action of an aqueous alkali metal hydroxide solution and a phase transfer catalyst to obtain an α-hydroxy ketone photoinitia...

Embodiment 1

[0041] Synthesis of 1-Hydroxycyclohexylphenyl Methanone

[0042] Dissolve and suspend 12g of 80-100mesh magnesium powder in 100ml of DMF (dimethylformamide) solvent, stir and cool down to -20°C under nitrogen protection, dissolve 9.8g of cyclohexanone and 23.46g of trichloromethylbenzene in 40ml of DMF solvent Slowly add it dropwise to the system in the first step, keep the system temperature below -20-10°C and react for 2 hours, naturally warm up to room temperature, filter, wash with water, extract with petroleum ether, add 20g of 30% NaOH The aqueous solution and 0.2 g of tetrabutylammonium bromide were reacted at a temperature of 50°C for two hours, washed with water, precipitated and recrystallized to obtain 16 g of a product with a purity of 99.6% and a yield of 86%.

Embodiment 2

[0044] Synthesis of 2-Hydroxy-2-methyl-1-phenylacetone

[0045] Dissolve and suspend 12g of 80-100mesh magnesium powder in 100ml of DMF solvent, stir and cool down to -20°C under nitrogen protection, dissolve 5.8g of acetone and 23.46g of trichloromethylbenzene in 40ml of DMF solvent, and slowly add it dropwise to the first In the first step system, keep the temperature of the system below -10-0°C and react for 2 hours, naturally warm up to room temperature, filter, wash with water, extract with petroleum ether, add 35% NaOH 17g aqueous solution and tetrabutylammonium bromide 0.15g , controlling the reaction temperature to 50° C. for two hours, washing with water, precipitation and rectification to obtain 13.3 g of the product with a purity of 99.2% and a yield of 82%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a preparation method of an alpha-hydroxyketone photoinitiator. The preparation method comprises the steps of taking a ketone compound and a trihalomethyl-substituted benzene anda derivative thereof as raw materials, enabling the raw materials to react under the action of a polar solvent and a metal catalyst to form a halogenated intermediate in one step, and hydrolyzing theobtained product under the action of an alkali metal hydroxide aqueous solution and a phase transfer catalyst to obtain the alpha-hydroxyketone photoinitiator. The operation is simple, the reaction step is short, no Lewis acid catalyst is used in the reaction, the pollution is small, the catalyst can be recycled, by-products are less, the cost is low, and a variety of products can be produced bythe same method.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of an alpha-hydroxy ketone photoinitiator. Background technique [0002] UV is also used as the abbreviation of radiation curing. UV is also UV ultraviolet light curing. It is cured by using medium and short waves (300-800 nanometers) in UV ultraviolet light. The stimulus becomes a free radical or a cation, thereby initiating the process of polymerizing the polymer material (resin) containing active functional groups into an insoluble / non-melting solid coating film. α-hydroxy ketone photoinitiators such as 1173 / 184 / 2959 / 180 are used It is widely used in UV-cured paper, ink for flooring, coatings and other industries, and the use volume in the entire market reaches 10,000 tons. [0003] At present, the current production process of α-hydroxyketone photoinitiator basically uses acid chloride and benzene or benzene derivatives to perform F...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C45/64C07C49/83C07C49/82
CPCY02P20/584
Inventor 孙建
Owner 孙建
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com