Siloxane-group light-initiated polyacrylic ester/silicon dioxide nanometer material and preparation method thereof

An acrylate and silica technology, applied in the direction of coating, can solve the problems of time-consuming and energy-consuming, unfavorable industrialization, unsolved or improved migration of small molecular photoinitiators, etc., and achieves environmental friendliness, easy industrial application, Effectiveness in solving toxicity and odor problems

Active Publication Date: 2010-11-03
ETERNAL SPECIALTY MATERIALS ZHUHAI CO LTD
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Problems solved by technology

The U.S. "Journal of Sol-Gel Science and Technology" (Journal of Sol-Gel Science and Technology 33, 9-13, 2005) reported a free radical polymerization of trimethoxyvinylsilane, which was first thermally initiated, and then The method of acid-catalyzed hydrolysis and condensation of trimethoxysilyl groups to finally obtain organic-inorganic hybrid film materials, however, this thermal curing system is time-consuming and energy-consuming, which is not conducive to industrialization, so the organic-inorganic hybrid film cured by ultraviolet light Materials have become a research hotspot
According to the U.S. "Progress in Organic Coatings" magazine (Progress in Organic Coatings 51, 312-320, 2004), by combining Tetraethyl orthosilicate (TEOS) with coupling agent 3-(methacryloyloxy ) Propyltrimethoxysilane co-hydrolyzed to obtain prepolymer, then mixed with acrylate monomer and acrylate oligomer, and finally obtained UV-curable acrylate / silica nano-hybrid material through UV curing. The coupling agent promotes the combination of organic phase and inorganic phase, which improves the mechanical and thermal properties of the final material, but the migration problem of small molecule photoinitiators is not solved or improved in this UV curing system

Method used

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  • Siloxane-group light-initiated polyacrylic ester/silicon dioxide nanometer material and preparation method thereof
  • Siloxane-group light-initiated polyacrylic ester/silicon dioxide nanometer material and preparation method thereof
  • Siloxane-group light-initiated polyacrylic ester/silicon dioxide nanometer material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 20.8g (0.1mol) of tetraethyl orthosilicate (TEOS), 5.4g (0.3mol) of water and 0.05g of hydrochloric acid were added to 23.75g of ethanol, and the mixture was subjected to hydrolysis and condensation at room temperature and a stirring speed of 300rpm After 4 hours, tetraethyl orthosilicate prepolymer was obtained;

[0031]Add 0.20mol 2-hydroxy-4'-(2-hydroxyethoxy)-2-methyl-1-phenylacetone-1 (manufactured by Ciba, product name Irgacure 2959), 0.22mol mercapto Acetic acid, 150mL toluene and 0.5% 4-dimethylaminopyridine p-toluenesulfonate by weight of Irgacure2959 were refluxed at 120°C for 12 hours to obtain 0.184mol of photoinitiator with mercapto groups; the above process can be represented by the reaction formula for:

[0032]

[0033] Take again 0.184mol of photoinitiator with mercapto, 0.184mol γ-glycidyl etheroxypropyl trimethoxysilane (Chinese Academy of Sciences, product name KH560), 60mL of dichloromethane and 0.5% triethylamine by weight of KH560 Add it into...

Embodiment 2

[0042] 10.4g (0.05mol) of tetraethyl orthosilicate (TEOS), 1.8g (0.1mol) of water, 0.075g of hydrochloric acid were added to 37.73g of ethanol, and the mixture was hydrolyzed at room temperature and at a stirring speed of 500rpm Condensate for 2 hours to obtain a prepolymer of tetraethyl orthosilicate;

[0043] In the 250mL there-necked flask, add 0.20mol1-hydroxyl-cyclohexyl benzophenone (produced by Ciba Company, product name Irgacure184), 0.21mol2-mercaptopropionic acid, 110mL toluene and 0.3% methanesulfonic acid by Irgacure 184 weight, at 125 Reflux at ℃ for 20 hours to obtain 0.182mol of photoinitiator with mercapto;

[0044] Take 0.182mol of photoinitiator with mercapto group, 0.182mol γ-glycidyl ether oxypropyl trimethoxysilane, 75mL dichloromethane and 0.3% of γ-glycidyl ether oxypropyl trimethoxysilane weight Sodium carbonate was added in a 150mL three-necked flask, and reacted for 24 hours under nitrogen protection and room temperature, and the solvent was removed ...

Embodiment 3

[0048] 15g (0.072mol) tetraethyl orthosilicate (TEOS), 1.29g (0.072mol) water, 0.04g hydrochloric acid were added to 33.67g ethanol, and the mixture was subjected to hydrolysis and condensation at room temperature and a stirring speed of 400rpm After 5 hours, tetraethyl orthosilicate prepolymer was obtained;

[0049] Add 0.20mol α-hydroxybenzoin methyl ether, 0.23mol 2-mercaptobutyric acid, 170mL p-xylene and 0.8% p-toluenesulfonic acid by α-hydroxybenzoin methyl ether weight in 250mL there-necked flask, at 130 Reflux for 24 hours at °C to obtain 0.18mol of photoinitiator with mercapto groups;

[0050] Then take 0.18mol of photoinitiator with mercapto, 0.18mol of γ-methacryloxypropyltrimethoxysilane, 55mL of dichloromethane and γ-methacryloxypropyltrimethoxy 0.8% potassium carbonate of silane weight was added in a 150mL three-necked flask, reacted for 24 hours under nitrogen protection and room temperature, and the solvent was removed to obtain 0.18mol of difunctional photoin...

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Abstract

The invention discloses a siloxane group contained bifunctional light initiator initiated polymerized ultraviolet light cured acrylic ester / silicon dioxide nanometer hybrid material and a preparation method thereof. The preparation method is characterized by comprising the following steps of: firstly, preparing a light initiator with a sulfhydryl group by adopting sulfhydryl carboxylic acid and a hydroxyl functional light initiator; then reacting the light initiator with a silane coupling agent to obtain a siloxane group contained bifunctional light initiator; and mixing the bifunctional light initiator with an acrylic ester monomer, an acrylic ester low polymer and a tetraethyl orthosilicate prepolymer to prepare an ultraviolet light curable acrylic ester / silicon dioxide nanometer hybrid coating of the invention. The ultraviolet light cured acrylic ester / silicon dioxide nanometer hybrid material obtained through the irradiation of a medium-pressure mercury lamp for the hybrid coating has good physical and mechanical performance and heat resisting property and wide industrial application prospect. The preparation method of the invention has simple and easy operation and can obtain an organic-inorganic nanometer hybrid coating with excellent dispersibility and better two-phase compatibility.

Description

technical field [0001] The invention belongs to the technical field of UV-curable acrylate / silicon dioxide nano-hybrid materials, in particular to UV-curable acrylate / silicon dioxide nano-hybrid materials that are polymerized by a bifunctional photoinitiator containing siloxane groups and its preparation method. Background technique [0002] In recent years, coating UV curing technology has been considered as an environmentally friendly green technology due to its fast curing speed, less pollution, low energy consumption, and excellent performance of cured products. As an important component of photocurable coatings, acrylate resins have been widely used in coatings, inks and adhesive formulations. The photoinitiator (PI) is the key to determine whether the acrylate oligomers and monomers of the formula system can quickly change from liquid to solid to form a cross-linked network structure during the light process. The basic characteristics of the photoinitiator are: the i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/12C08F2/48C09D4/02C09D4/06
Inventor 胡丽华施文芳王博世王小军陈荣
Owner ETERNAL SPECIALTY MATERIALS ZHUHAI CO LTD
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