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Chemical crosslinking curable fluorine-containing MDQ (mono-di-quarter) type silicone resin and preparation method thereof

A chemical cross-linking, silicone resin technology, applied in the field of organic polymer chemistry, can solve the problems of resin not curing, poor antifouling performance, etc., to avoid gaps or cracks, mild reaction conditions, uniform and stable structure.

Inactive Publication Date: 2020-01-17
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN 108610479A discloses a preparation method of fluorine-containing resin. After mixing perfluoropropylene dimer, perfluoropropylene trimer, fatty alcohol monomer, catalyst and organic solvent, react at 70~120℃ for 24~ After cooling for 38 hours, wash and then centrifuge and dehydrate to obtain hydroxyfluororesin. The resin has the properties of water resistance, solvent resistance, alkali resistance and surface antifouling, but the resin cannot be cured by hydrosilicon addition
Chinese invention patent CN102898648 discloses a method for preparing a chemically crosslinkable MDQ type phenylvinyl silicone resin, which uses hexamethyldisiloxane and 1,3-divinyl-1,1,3, 3-Tetramethyldisiloxane is used as a capping agent (i.e. the source of the M chain), methylphenyldiethoxysilane is used as the source of the D chain, ethyl orthosilicate is used as the source of the Q chain, and ethanol is used as the source of the Q chain. Solvent, under the catalysis of hydrochloric acid, carry out hydrolysis and condensation to obtain MDQ silicone resin with a refractive index of 1.46 to 1.50. Although this resin can be cured by hydrosilylation, because the molecule does not contain fluorine atoms, the antifouling performance is poor.

Method used

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  • Chemical crosslinking curable fluorine-containing MDQ (mono-di-quarter) type silicone resin and preparation method thereof
  • Chemical crosslinking curable fluorine-containing MDQ (mono-di-quarter) type silicone resin and preparation method thereof
  • Chemical crosslinking curable fluorine-containing MDQ (mono-di-quarter) type silicone resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In a 100mL three-necked flask equipped with a mechanical stirring device, a thermometer, a constant pressure dropping funnel and a condensing device, add 20.6925g (1.1496mol) of deionized water, 7.865g (0.1462mol) of absolute ethanol, 1.3348g (0.0082mol) mol) hexamethyldisiloxane, 1.276g (0.0069mol) 1,3-divinyl-1,1,3,3-tetramethyldisiloxane (referred to as vinyl double head, the same below) and 14.4291g (0.0714mol) of methyltrifluoropropyldimethoxysilane, after starting stirring to make it evenly mixed, 4.72g (0.0465mol) of concentrated hydrochloric acid with a concentration of 36wt% was added dropwise to the above mixture within 1min . After the concentrated hydrochloric acid was added dropwise, the temperature of the kettle liquid was raised from room temperature to 50° C. over 10 minutes, and then 21.3145 g (0.1506 mol) of tetraethoxysilane was added dropwise into the reaction kettle at a constant speed over 20 minutes. After the tetraethoxysilane was added dropwise...

Embodiment 2

[0046] In a 100mL three-necked flask equipped with a mechanical stirring device, a thermometer, a constant pressure dropping funnel and a condensing device, 18.0292g (1.0016mol) of deionized water, 8.1455g (0.1771mol) of absolute ethanol, 3.2298g (0.01994 mol) hexamethyldisiloxane, 1.641g (0.0888mol) 1,3-divinyl-1,1,3,3-tetramethyldisiloxane and 20.355g (0.1008mol) methyltrifluoro Propyldimethoxysilane, after starting stirring to make it evenly mixed, 4.18 g (0.0412 mol) of concentrated hydrochloric acid with a concentration of 36 wt % was added dropwise to the above mixture within 1 min. After the concentrated hydrochloric acid was added dropwise, the temperature of the kettle liquid was raised from room temperature to 50° C. over 5 minutes, and then 20.7757 g (0.0999 mol) of tetraethoxysilane was added dropwise into the reaction kettle at a constant speed over 25 minutes. After the tetraethoxysilane was added dropwise, the temperature of the material in the kettle was raised...

Embodiment 3

[0051] In a 100mL three-neck flask equipped with a mechanical stirring device, a thermometer, a constant pressure dropping funnel and a condensing device, add 23.7051g (1.317mol) of deionized water, 5.2678g (0.1145mol) of absolute ethanol, 3.9409g (0.0243 mol) hexamethyldisiloxane, 4.9687g (0.0267mol) 1,3-divinyl-1,1,3,3-tetramethyldisiloxane and 7.3439g (0.0364mol) methyltrifluoro Propyldimethoxysilane, after starting the stirring to make it evenly mixed, 4.2753g (0.0713mol) of acetic acid was added dropwise to the above mixture within 2min. After the acetic acid was added dropwise, the temperature of the kettle liquid was raised from room temperature to 40° C. over 3 minutes, and then 20.8098 g (0.0999 mol) of tetraethoxysilane was added dropwise into the reaction kettle at a constant speed over 5 minutes. After the tetraethoxysilane was added dropwise, the temperature of the material in the kettle was raised to 70°C and maintained at this temperature for 2 hours, then the t...

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PUM

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Abstract

The invention relates to the field of organic chemistry, aims to solve the problem of compatibility of organic silicone resin and organic fluorine resin in blending and crosslinking curing performanceand response performance of the organic fluorine silicone resin, and discloses a chemical crosslinking curable fluorine-containing MDQ (mono-di-quarter) type silicone resin and a preparation method thereof. The preparation method comprises the following step: by taking hexamethyl disiloxane and 1,3-divinyl-1,1,3,3-tetramethyl disiloxane as a source of M chains, methyltrifluoropropyl dimethoxysilane as a source of D chains, ethyl orthosilicate as a source of Q chains, an ethanol-aqueous solution as a reaction solvent, and toluene as an extraction agent, performing a co-hydrolysis condensationprocess under the action of an acid catalyst, so as to obtain the resin. The synthesis method provided by the invention is simple, the reaction condition is mild, the product is easy to separate and recycle, the equipment investment is low, the equipment utilization rate is high, and industrial production is easy. The MDQ silicone resin prepared by the invention has both excellent properties of silicone resin and fluorine resin, and is capable of improving the anti-fouling performance of display screens of mobile phones and the like.

Description

technical field [0001] The invention relates to the field of organic polymer chemistry, in particular to a chemically cross-linkable and curable fluorine-containing MDQ type silicone resin and a preparation method thereof. Background technique [0002] Silicone resin has Si-O bond as the main chain. Its unique structure combines the properties of inorganic materials and organic materials. It has basic properties such as low surface tension, small viscosity-temperature coefficient, high compressibility, and high gas permeability. High and low temperature, oxidation stability, flame retardant, corrosion resistance, non-toxic and tasteless, and physiological inertness, etc., are widely used in aerospace, electrical and electronic, construction, transportation, textile, food, light industry, medical and other industries. [0003] Compared with conventional plastics and organic polymers such as polyethylene and polypropylene, fluororesins have many unique and excellent properties...

Claims

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Application Information

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IPC IPC(8): C08G77/24C08G77/08
CPCC08G77/08C08G77/24C08G77/70
Inventor 伍川苏丽董红瞿志荣蒋攀荣瑞吕叶红邱化玉蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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