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Method for synthesizing same carbon dicarbonyl photosensitive resin

A synthesis method and photosensitive resin technology, which is applied in the preparation of ketene/polyketene, coating, organic chemistry, etc., can solve the problems of loss of application value of photocurable resin, increase in viscosity, etc., and achieve improved storage stability and simple regeneration , the effect of reducing production costs

Inactive Publication Date: 2008-05-07
GUANGDONG BOSSIN NOVEL MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of these alkaline stronger catalysts also brings other disadvantages at the same time, because these catalysts are liquid or soluble in the reaction system, so the synthesis reaction is completed, and the alkaline catalysts permanently exist in the product oligomer system, which will play a further role. Catalytic action causes the viscosity of the product resin to continue to increase during storage. Depending on the storage environment temperature and product structure, it will generally turn into an immobile gel after a few days to a few weeks, losing its application value as a photocurable resin.

Method used

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  • Method for synthesizing same carbon dicarbonyl photosensitive resin
  • Method for synthesizing same carbon dicarbonyl photosensitive resin

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 4.0g KF 2H 2Dissolve O in 50ml of water, add 15.0g of 50-120mesh basic alumina, stir at 65-75°C for 1hr, depressurize the water pump, remove water slowly at 70°C, and activate in a muffle furnace at 140°C for 4hrs to obtain fluorine loaded on alumina Potassium chloride solid base catalyst.

[0026] 17.2g of trimethylolpropane triacrylate monomer and 3.6g of ethyl acetoacetate were mixed in a three-neck reaction flask, 0.01g of polymerization inhibitor p-methoxyphenol was added, and 8.0g of the above-mentioned obtained aluminum oxide supported potassium fluoride solid Base catalyst, stir rapidly, heat to 80°C, react for 6 hours, the viscosity of the system increases, stop the reaction, filter while hot, and obtain a light yellow viscous resin with a viscosity of 31000cps / 25°C.

Embodiment 2

[0028] 10.0g D290 type macroporous strongly basic anion-exchange resin (cross-linked polystyrene microspheres support quaternary ammonium salt, and the commercial product uses chloride ion as the exchange ion) is first soaked with deionized water to remove mechanical impurities and pulverized resin, Soak the resin with 100mL of 10% sodium hydroxide aqueous solution for a day and night, filter, rinse with deionized water until the filtrate becomes nearly neutral, rinse with absolute ethanol to remove water, and dry to obtain a strong basic anion exchange resin catalyst.

[0029] 17.2g trimethylolpropane triacrylate monomer and 3.6g ethyl acetoacetate are mixed in three-neck reaction flask, add polymerization inhibitor p-methoxyphenol 0.01g, 8.0g above-mentioned gained strongly basic anion exchange resin as Solid catalyst, stirred rapidly, heated to 80°C, reacted for 6 hours, the viscosity of the system increased, stopped the reaction, filtered while it was hot, and obtained a li...

Embodiment 3

[0031] The aluminum oxide-supported potassium fluoride obtained after filtering in Example 1 was washed with absolute ethanol, dried, and then activated in a muffle furnace at 140°C for 4 hours.

[0032] 17.2g of trimethylolpropane triacrylate monomer and 3.6g of ethyl acetoacetate were mixed in a three-necked reaction flask, and 0.01g of polymerization inhibitor p-methoxyphenol was added, and 8.0g of the above-mentioned activated alumina supported potassium fluoride Solid base catalyst, stirred rapidly, heated to 80°C, reacted for 6 hours, the viscosity of the system increased, stopped the reaction, filtered while it was hot, and obtained a slightly yellow viscous resin with a viscosity of 30600cps / 25°C.

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Abstract

The invention relates to a synthetic method of dicarbonyl sensitization resin with carbon, which comprises the steps that a polyol acrylic ester monomer and a Beta-dicarbonyl compound are mixed evenly, and then a reaction insoluble solid basic catalyst for mixing and heating is added to lead the multielement acrylic ester monomer and the Beta-dicarbonyl compound with agile methylene to act Michael reaction, and filtrating is held after finishing the reaction to lead the solid basic catalyst and the product resin to be separated. The catalysis system of the invention comprises an insolubility catalyst with alkali characteristic, such as alumina loaded with potassium fluoride and alkali negative ion exchange resin. The solid basic catalyst effectively promotes the Michael reaction and is convenient for filtrating after reaction, and the solid basic catalyst is removed from product oligomer, thereby avoiding the further influence to the product resin by an alkali catalyst to enable the storage stability of the product resin to be improved. The addition resin can realize rapid light curing under the condition of having no photo-initiator, and also can be used for photo-cured coating and printing ink blending.

Description

technical field [0001] The invention relates to a synthesis method of a class of oligomers which have photosensitivity and can initiate free radical photocuring. Specifically, polyacrylic acid ester monomers and ethyl acetoacetate or acetylacetone, etc. containing Beta-dicarbonyl The synthesis method of the gem-carbon dicarbonyl photosensitive resin obtained by catalyzing the Michael addition reaction of the compound of the structure. Background technique [0002] Photocurable resin is the main material for preparing various photocurable coatings and photocurable inks, including epoxy acrylate, polyurethane acrylate, polyester acrylate and other major categories. The general feature is that the structure contains acrylate groups. When the photoinitiator coexists, the active free radical can be generated by the photoinitiator after being irradiated with ultraviolet light, resulting in rapid polymerization, crosslinking and curing of the photocurable resin. That is to say, th...

Claims

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Application Information

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IPC IPC(8): C08F20/10C07C69/54C07C67/46C09D4/00
Inventor 庞来兴杨建文
Owner GUANGDONG BOSSIN NOVEL MATERIALS TECH CO LTD
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