Cation ultraviolet curing group-containing silicon oxide compound and preparation method thereof

A silicon-oxygen compound and light-curing technology, which is applied in the fields of compounds of group 4/14 elements of the periodic table, chemical instruments and methods, organic chemistry, etc., can solve difficult control of process conditions, unstable product quality, intense condensation reaction, etc. problem, to achieve the effect of easy control of process conditions, convenient industrial production, and low content of organic volatiles

Active Publication Date: 2010-12-08
ETERNAL SPECIALTY MATERIALS ZHUHAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the halogenated silanes used in this method have strong corrosiveness, and the condensation reaction is intense and complicated, acid removal treatment is required, and a large amount of organic solvents must be used, which brings difficult control of process conditions and poor product quality to large-scale industrial production. Stable and have to solve problems such as solvent recovery

Method used

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  • Cation ultraviolet curing group-containing silicon oxide compound and preparation method thereof
  • Cation ultraviolet curing group-containing silicon oxide compound and preparation method thereof
  • Cation ultraviolet curing group-containing silicon oxide compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 19.8g (0.1mol) phenyltrimethoxysilane, 100.8g (0.9mol) 3-cyclohexene-1-methanol and 0.28g (0.001mol) tetraisopropyl titanate were placed in a round bottom flask, React at 100°C under stirring until the methoxy peak in the H NMR spectrum disappears; after removing excess 3-cyclohexene-1-methanol under reduced pressure, add 80 mL of toluene to dilute the reaction solution, and then use 5% tartaric acid aqueous solution, Washing with 5% sodium bicarbonate aqueous solution and distilled water, and finally drying the organic phase with anhydrous sodium sulfate, and the transparent liquid obtained after vacuum distillation is silicon-containing olefin.

[0045] Add 62.1g (0.36mol) m-chloroperoxybenzoic acid and 200mL methylene dichloride in the flask equipped with mechanical stirring, thermometer and constant pressure dropping funnel, after mixing uniformly, add dropwise the silicon-containing olefin that above-mentioned reaction makes, in After reacting at 25°C for 24 hours,...

Embodiment 2

[0052] 13.6g (0.1mol) methyltrimethoxysilane, 37.3g (0.3mol) 5-norbornene-2-methanol and 0.28g (0.001mol) tetraisopropyl titanate were placed in a round bottom flask, React under stirring at 100°C until the methoxy peak in the H NMR spectrum disappears; then add 80 mL of toluene to dilute the reaction solution, then wash with 5% tartaric acid aqueous solution, 5% sodium bicarbonate aqueous solution and distilled water, and finally the organic phase Dry with anhydrous sodium sulfate and distill under reduced pressure to obtain a transparent liquid that is silicon-containing olefin.

[0053] In the flask equipped with mechanical stirring, thermometer and constant pressure dropping funnel, add 62.1g (0.36mol) m-chloroperoxybenzoic acid and 160mL dichloromethane and 40mLN, the mixed solvent of N-dimethylformamide composition, mix After uniformity, add the silicon-containing olefin prepared by the above reaction dropwise, and after reacting at 25°C for 24 hours, filter to remove th...

Embodiment 3

[0057] Put 15.2g (0.1mol) of methyl orthosilicate, 245g (2.4mol) of ethylene glycol monoallyl ether and 0.28g (0.001mol) of tetraisopropyl titanate in a round-bottomed flask, under stirring Vacuumize and react at 50°C until the methoxy peak in the H NMR spectrum disappears; then first add 80mL of toluene to dilute the reaction solution, then wash with 5% tartaric acid aqueous solution, 5% sodium bicarbonate aqueous solution and distilled water, and finally wash the organic phase with Dry over anhydrous sodium sulfate and distill under reduced pressure to obtain a transparent liquid that is silicon-containing olefin.

[0058] Add 82.8g (0.48mol) m-chloroperoxybenzoic acid and 250mL methylene dichloride in the flask that mechanical stirring, thermometer and constant pressure dropping funnel are housed, after mixing uniformly, add dropwise the silicon-containing olefin that above-mentioned reaction makes, in After reacting at 25°C for 24 hours, the white solid was removed by filt...

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Abstract

The invention discloses a cation ultraviolet curing group-containing silicon oxide compound and a preparation method thereof. The preparation method is characterized by comprising the following steps of: mixing and stirring monohydroxy vinyl ether compound or monohydroxy-3-oxetane compound and methoxysilane in the presence of a catalyst in a molar ratio of (1-6)*n:1 until methoxyl group peak disappears in nuclear magnetic resonance spectroscopy; or mixing and stirring monohydroxy olefin compound and the methoxysilane in the presence of the catalyst in a molar ratio of (1-6)*n:1 until the methoxyl group peak disappears in the nuclear magnetic resonance spectroscopy, and then adding the obtained silicon olefin-containing compound dropwise into organic solution of organic peracid for performing epoxidation, wherein the number n of siloxicon bonds in molecules is an integer of 2 to 4. The preparation method has the advantages of low cost and readily available raw materials, simple and convenient preparation operation and convenient industrial production; and the obtained cation ultraviolet curing group-containing silicon oxide compound can be cured rapidly by ultraviolet irradiation; and the obtained coating has the advantages of high smoothness, high flame retardant efficiency and wide industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of ultraviolet curing silicon-containing materials, and in particular relates to a silicon oxide compound containing cationic photocuring groups and a preparation method thereof. Background technique [0002] With the enhancement of people's awareness of environmental protection, UV-curable materials are gradually replacing traditional solvent-based coatings due to their advantages such as no solvent or low solvent, fast curing speed, low organic volatiles, and good coating performance. UV curing has two mechanisms: free radical curing and cationic curing. Among them, free radical curing is widely used, but due to the poor adhesion of the cured film to the substrate, it has a strong oxygen inhibition effect and unique mucosal stimulation. nature, so that its application is subject to certain restrictions. Compared with free radical curing, cationic curing can make up for the above defects, the volume shrink...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C09K21/06
Inventor 程喜娥施文芳王博世王小军陈荣
Owner ETERNAL SPECIALTY MATERIALS ZHUHAI CO LTD
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