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Polymer photoinitiator and preparation method thereof

A photoinitiator and polymer technology, applied in the field of polymer photoinitiator and its preparation, can solve the problems of uncontrollable chemical structure, low content of initiating group, uncontrollable molecular weight, etc., to overcome the problems of volatilization and migration, molecular weight The effect of narrow distribution and simple preparation process

Active Publication Date: 2021-06-11
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the uncontrollable chemical structure, uncontrollable molecular weight, low initiating group content or a large proportion of photolysis residues that exist in the prior art, the existing macromolecular initiators will volatilize and migrate, and small molecule photoinitiators and Macromolecular photoinitiators generally have the problem of low thermal stability. The present invention provides a macromolecular photoinitiator and a preparation method thereof;

Method used

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  • Polymer photoinitiator and preparation method thereof
  • Polymer photoinitiator and preparation method thereof
  • Polymer photoinitiator and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0050] A preparation method of macromolecular photoinitiator, specifically as follows:

[0051] Add 4,4'-dihydroxybenzophenone, dihalogenated hydrocarbon (1,10-dibromodecane) and inorganic base (potassium carbonate) into the solvent (acetone), and under nitrogen, the solvent is refluxed for polycondensation Reaction, the reaction temperature is 56°C, the reaction time is 4h, and the stirring speed is 300rpm; after the reaction, filter with suction, wash fully with water and methanol four times alternately, and vacuum dry at 80°C for 6h to obtain a polymer photoinitiator; Among them, the molar ratio of 4,4'-dihydroxybenzophenone to dihalogenated hydrocarbon is 1:1; the molar ratio of inorganic base to dihalogenated hydrocarbon is 2:1; 4,4'-dihydroxydiphenyl The ratio of the number of moles of ketone to the volume of solvent is 1mol:1L.

[0052] A kind of polymer photoinitiator prepared, its structural formula is:

[0053]

[0054] Among them, R 1 It is decylene; the numbe...

Embodiment 2

[0056] A preparation method of macromolecular photoinitiator, specifically as follows:

[0057] Add 4,4'-dihydroxybenzophenone, dihalogenated hydrocarbon (1,10-dibromodecane) and inorganic base (potassium carbonate) into the solvent (toluene), and under nitrogen, the solvent is refluxed for polycondensation Reaction, the reaction temperature is 110°C, the reaction time is 12h, and the stirring speed is 300rpm; after the reaction, filter with suction, wash fully with water and methanol four times alternately, and vacuum dry at 80°C for 6h to obtain a polymer photoinitiator; Among them, the molar ratio of 4,4'-dihydroxybenzophenone to dihalogenated hydrocarbon is 1:1; the molar ratio of inorganic base to dihalogenated hydrocarbon is 2:1; 4,4'-dihydroxydiphenyl The ratio of the number of moles of ketone to the volume of solvent is 2mol:1L.

[0058] A kind of polymer photoinitiator prepared, its structural formula is:

[0059]

[0060] Among them, R 1 It is decylene; the num...

Embodiment 3

[0062] A preparation method of macromolecular photoinitiator, specifically as follows:

[0063] Add 4,4'-dihydroxybenzophenone, dihalogenated hydrocarbon (1,4-dibromobenzene) and inorganic base (sodium carbonate) into the solvent (propanol), and under argon, the solvent is refluxed Polycondensation reaction, the reaction temperature is 87°C, the reaction time is 16h, and the stirring speed is 300rpm; after the reaction, filter with suction, wash fully with water and methanol four times alternately, and vacuum dry at 80°C for 6h to obtain a polymer photoinitiator ; Wherein, the molar ratio of 4,4'-dihydroxybenzophenone and dihalogenated hydrocarbon is 0.95:1; the molar ratio of inorganic base and dihalogenated hydrocarbon is 2:1; 4,4'-dihydroxydihydrocarbon The ratio of the number of moles of benzophenone to the volume of solvent is 3mol:1L.

[0064] A kind of polymer photoinitiator prepared, its structural formula is:

[0065]

[0066] Among them, R 1 It is 1,4-phenylene...

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Abstract

The invention relates to a polymer photoinitiator and a preparation method thereof, the method being a first method of carrying out condensation polymerization on 4,4'-dihydroxy benzophenone and dihalogenated hydrocarbon which are used as raw materials to prepare the polymer photoinitiator; a second method of firstly carrying out acetylation on 4,4'-dihydroxy benzophenone, and then carrying out melt polycondensation reaction with diacid to prepare the polymer photoinitiator; a third method of carrying out polymerization reaction on 4,4'-dihydroxy benzophenone and diisocyanate to prepare the polymer photoinitiator. The structural formula of the prepared high-molecular photoinitiator is shown in the specification, wherein n is an integer greater than or equal to 2; R1 is a cC1-C20 alkylene group, or R2 is a C1-C18 alkylene group; and R3 is a C4-C20 alkylene group. The preparation method disclosed by the invention is simple in process and has a wide application prospect in the field of engineering plastic processing; the prepared polymer photoinitiator is good in thermal stability and excellent in photo-initiation effect, and the problems of volatilization and migration of photo-initiation residues during photolysis of an existing photoinitiator can be solved as an initiation group is located in a main chain.

Description

technical field [0001] The invention belongs to the technical field of photoinitiators, and relates to a polymer photoinitiator and a preparation method thereof. Background technique [0002] UV curing technology refers to a photoprocessing process in which the liquid resin matrix is ​​rapidly cross-linked into a solid state by the decomposition of a photoinitiator by ultraviolet light of a certain wavelength. The photocuring reaction is essentially a photoinitiated polymerization and crosslinking reaction. The advantages of light curing technology are fast reaction rate, short processing cycle, high efficiency, energy saving and environmental protection, and cost saving. The current photocuring technology is mainly used in the preparation of photocurable coatings, photocurable inks, photocurable adhesives and 3D printing. [0003] Photoinitiator is the core factor of photocuring system. A photoinitiator refers to an active substance (free radical or ion) that can initiat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/40C08G63/193C08G18/32C08F2/48C08J7/12C08L67/02
CPCC08G65/40C08G63/193C08G18/3215C08F2/48C08J7/123C08J2367/02Y02P20/10
Inventor 何勇郭亚东董奎勇杨婷婷
Owner DONGHUA UNIV
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