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Preparation method of ultraviolet-curable organic-inorganic hybrid material

A hybrid material and ultraviolet light technology, applied in the direction of coating, etc., can solve the problems of limited addition, low grafting rate, limited compatibility improvement, etc., to achieve improved solubility, simple synthesis process, and good transparency Effect

Inactive Publication Date: 2013-06-26
山西省应用化学研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the modified product still exists in solid form after washing with water, suction filtration, etc., and the compatibility improvement in the organic system is very limited, and the grafting rate is relatively low, resulting in limited addition.

Method used

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  • Preparation method of ultraviolet-curable organic-inorganic hybrid material
  • Preparation method of ultraviolet-curable organic-inorganic hybrid material
  • Preparation method of ultraviolet-curable organic-inorganic hybrid material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 73g of tripropylene glycol diacrylate into a 250mL four-necked flask equipped with a thermometer, a stirrer, and a dropper, stir rapidly, and add the coupling agent γ-aminopropyltriethoxysilane dropwise under ice-water bath conditions. (KH550) 27g, the dropwise addition was completed in 90 minutes, and the temperature was raised to 25°C for 12 hours.

[0024] After measuring the amine value of the reaction solution to 30 mgKOH / g, add 4 g of nano-silica, 30 mL of ethanol, and 4 mL of distilled water, adjust the pH of the system to 6.5 with 0.1 mol / L formic acid, and raise the temperature to 50 ° C for 8 hours. The reactant was washed with acetone, suction filtered and dried to obtain the product.

[0025] Take a small amount of the product and grind it with KBr, and put it into a tablet machine for tableting after the grinding is uniform. KBr pellets of nano-silica before modification were also prepared. The infrared spectra of the two samples were measured separat...

Embodiment 2

[0036] In a 250mL four-necked flask equipped with a thermometer, a stirrer, and a dropper, add 62g of trimethylolpropane triacrylate, stir rapidly, and add the coupling agent γ-aminopropyl triethoxy dropwise under ice-water bath conditions. 38g of silane was added dropwise in 90 minutes, and the reaction was carried out at a constant temperature of 25°C for 15 hours.

[0037] After the measured amine value reaches 35mgKOH / g, add 3.6g nano-silica, 20mL ethanol, 4.3mL distilled water, add 0.1mol / L acetic acid to adjust the pH to 6.5, and react at 55°C for 9h. After washing with acetone, suction filtration and drying, the product was obtained.

[0038] Through scanning electron microscopy and thermogravimetric (TG) curve analysis, the average particle size of the hybrid material was measured to be 150nm, and the grafting rate was 35.72%.

Embodiment 3

[0040] In a 250mL four-neck flask equipped with a thermometer, a stirrer, and a dropper, add 67g of hexanediol diacrylate, stir rapidly, and add the coupling agent γ-aminopropyltriethoxysilane dropwise under ice-water bath conditions. 33g, the dropwise addition was completed in 90 minutes, and the reaction was carried out at a constant temperature of 25°C for 20 hours.

[0041] After the measured amine value reaches 40mgKOH / g, add 4.5g nano-silica, 20mL ethanol, 8mL distilled water, add 0.1mol / L formic acid to adjust the pH to 6.5, and react at 60°C for 10h. After washing with acetone, suction filtration and drying, the product was obtained.

[0042] Through scanning electron microscopy and thermogravimetric (TG) curve analysis, the average particle size of the hybrid material was measured to be 230nm, and the grafting rate was 52.18%.

[0043] Table 1 shows the effect of adding different amounts of the organic-inorganic hybrid material of Example 3 on the hardness and wear r...

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Abstract

The invention relates to a preparation method of an ultraviolet-curable organic-inorganic hybrid material. The preparation method comprises the following steps of: performing Michael addition reaction on gamma-aminopropyltriethoxysilane and polyfunctional acrylate to get an intermediate product taking -Si(OC2H5)3 and one or more -CH=CH2 as a terminal group, performing hydrolysis on the product under weak acidic conditions, and grafting with dry nano-silicon dioxide to get the organic-inorganic hybrid material which takes SiO2 as a core, takes a tertiary amine structure as an intermediate layer and takes -CH=CH2 as a shell layer. The organic-inorganic hybrid material can be applied to preparation of an ultraviolet curing coating. The organic-inorganic hybrid material prepared based on the method disclosed by the invention has a core-shell structure, a terminal C=C double bond and the tertiary amine structure, when the organic-inorganic hybrid material is applied to the ultraviolet curing coating, the wear resistance, the heat resistance, the hardness and other performances of the coating can be improved, the problems of dissolubility and participation in polymerization of inorganicnano-particles in the ultraviolet curing coating can be particularly solved, and the organic-inorganic hybrid material can be widely applied to the ultraviolet curing coatings on the surfaces of metals, woodware and plastics.

Description

technical field [0001] The invention relates to an organic-inorganic hybrid material, in particular to a preparation method of an organic-inorganic hybrid material with a core-shell structure. Background technique [0002] UV-curable coatings are widely used in the surface coating of paper, metal, wood, plastic, etc. due to their low VOC content, fast curing speed, and good comprehensive performance of the coating film. The introduction of inorganic nanoparticles will improve the wear resistance, hardness, adhesion and other properties of UV-curable coatings. The performance of organic-inorganic hybrid materials largely depends on the chemical structure, surface modification of inorganic nanomaterials and their dispersion in organic polymer materials. [0003] As a commonly used inorganic nanoparticle, nano-silica can improve the overall performance of the cured film in UV-curable coatings. However, due to the existence of a large number of hydroxyl groups on its surface, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08G77/20C09D183/07
Inventor 吴建兵李萍刘伟马小龙梁庆丰侯彩英马国章
Owner 山西省应用化学研究所
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