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Preparation method of low molecular weight polyacrylic ester acrylic ester for photo-curing

A polyacrylate, low-molecular-weight technology, applied in the direction of coating, etc., can solve the problems that oligomers cannot be used alone, hinder application, and have high viscosity

Inactive Publication Date: 2011-02-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because it contains more polar atoms and its viscosity is too high, it cannot be used alone as an oligomer, but can only be used as an auxiliary or needs to add more toxic active diluents, which hinders its application.

Method used

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  • Preparation method of low molecular weight polyacrylic ester acrylic ester for photo-curing
  • Preparation method of low molecular weight polyacrylic ester acrylic ester for photo-curing
  • Preparation method of low molecular weight polyacrylic ester acrylic ester for photo-curing

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) in the reactor that condensing device is housed, stirring device, adding monomer molar ratio is 1.1: 1 methyl acrylate and hydroxyethyl acrylate, add azobisisobutyronitrile (monomer mole percent 1.5%), n-dodecyl mercaptan (monomer molar percentage 2%), solvent ethylene glycol monomethyl ether (monomer mass 120%), stir and heat up to 55°C, fully dissolve for half an hour, and then heat up to 74°C Carry out the reaction until the temperature automatically rises and stop heating, and the reaction ends when the temperature begins to fall back. When the temperature drops to normal temperature, add distilled water with a solvent mass ratio of 100%, and stratification occurs. After the stratification is stable, filter off the supernatant to obtain a white opaque resin. After washing with water three times, put the resin in a vacuum oven at 70°C Dry overnight to remove the remaining moisture to obtain the product poly-hydroxyethyl acrylate-methyl acrylate, the appearance is...

Embodiment 2

[0036] Methyl methacrylate and hydroxyethyl methacrylate are charged according to the monomer molar ratio of 1.1:1, and azobisisobutyronitrile (monomer molar percentage 0.5%), n-dodecanethiol (monomer molar percentage 2.0%) are added ), solvent ethyl acetate (monomer mass 100%), all the other heating and aftertreatment are with embodiment 1, and the product obtained is slightly yellow transparent resin, GPC test number average molecular weight Mn=7412, molecular weight polydispersity PDI=3.1.

[0037] Add 0.25wt% p-toluenesulfonic acid accounting for acrylic acid weight, 0.3wt% hydroquinone accounting for acrylic acid weight in the second step reaction, solvent adopts toluene, react at 124 ℃ for 2.2 hours, all the other conditions are the same as embodiment 1. The conversion rate was 90%.

[0038] Test the properties of the cured film on the tin plate, the gloss is 100Gs, the flexibility is grade 7, the adhesion is 84%, and the adhesion on PE is 75%.

Embodiment 3

[0040] (1) The ratio of ethyl acrylate to hydroxyethyl acrylate monomer is 1.2:1, add azobisisobutyronitrile (monomer molar percentage 5%), n-dodecanethiol (monomer molar percentage 2.0%), The solvent was ethyl acetate (monomer mass 400%), and the rest of the heating and post-treatment were the same as in Example 1. The product obtained was a light yellow transparent resin with a number-average molecular weight of Mn=2916 and a molecular weight polydispersity of PDI=3.2 by GPC.

[0041] In the second step reaction, add p-toluenesulfonic acid accounting for 5wt% of acrylic acid weight, hydroquinone accounting for 0.3wt% of acrylic acid weight, using toluene as a solvent, and reacting at 124° C. for 2.5 hours, and all the other conditions are the same as in Example 1. The conversion rate was 80%.

[0042] Test the properties of the cured film on the tin plate, the gloss is 100Gs, the flexibility is grade 7, the adhesion is 84%, and the adhesion on PE is 75%.

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Abstract

The invention discloses a preparation method of low molecular weight polyacrylic ester acrylic ester for photo-curing, belonging to the field of photo-curing low polymers. The lower polymer has the advantages of low molecular weight, low dispersibility, low viscosity, uniform structure and excellent property after being cured and can be used for photo-curing main body resin. The low polymer is synthesized by a two-step method and consists of a main chain and a branch chain, wherein the main chain is a pure carbon-carbon bond and is prepared by acrylic ester double-bond copolymerization. A polymerization monomer consists of (methyl) alkyl acrylate and functional monomers. The branch chain is prepared by a condensation reaction of functional groups; and a reaction product of a (methyl) acrylic ester copolymer in the first step carries the functional groups capable of further reaction, and functional monomers with light reactivity are grafted in the reaction product, wherein the functional monomers can be (methyl) acrylic acid, acryloyl chloride and the like. The invention realizes the preparation of the lower polymers with low molecular weight by using methods of adding a chain transfer agent and controlling the mixture ratio of the monomers and the dosage of initiators, is simple and convenient to operate and easy to industrialized production and has broad application prospect.

Description

technical field [0001] The invention relates to a preparation method of UV photocurable acrylate resin, belonging to the field of photocurable oligomers. Background technique [0002] Photocuring technology is a process in which light or electron beams are used as energy sources to trigger rapid transformation of chemically reactive liquid substances into solid states. Photocuring technology is an energy-saving and environmentally friendly new technology. It fully complies with the "5E principles": Efficient (high efficiency), Enabling (wide adaptability), Economical (economical), Energy Saving (energy saving), Environmental Friendly (environmental friendly). [0003] The photocuring system is mainly composed of oligomers, reactive diluents and photoinitiators, and the properties of oligomers have a decisive effect on the properties of the cured coating film. Polyacrylate Acrylate, as a new type of acrylate photocurable oligomer, has broad application prospects in the fiel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09D4/02C08F220/28C08F2/38C08F220/14C08F8/14C08F220/18C08F220/32
Inventor 何勇欧霄巍刘翠聂俊
Owner BEIJING UNIV OF CHEM TECH
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