A kind of polyeugenol-phenylsilsesquioxane and preparation method thereof

A technology of phenyl sesquioxane and phenyl trialkoxysilane, which is applied in the field of polyeugenol-phenyl silsesquioxane and its preparation, can solve the problem of affecting the impact strength of composite materials, polyphenyl silsesquioxane alkane precipitation, poor compatibility and other problems, to achieve the effect of improving dispersion, improving impact strength and precipitation resistance, and simple process

Active Publication Date: 2020-12-01
河源市山德科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ordinary polyphenylsilsesquioxane has the problem of affecting the impact strength of the composite material due to its poor compatibility with PC. In addition, because of the poor compatibility between the two, when the material is at a higher When the temperature is used, polyphenylsilsesquioxane is often precipitated and fogged

Method used

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  • A kind of polyeugenol-phenylsilsesquioxane and preparation method thereof
  • A kind of polyeugenol-phenylsilsesquioxane and preparation method thereof
  • A kind of polyeugenol-phenylsilsesquioxane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Preparation of polymercapto-phenylsilsesquioxane:

[0033] At room temperature, in a 250L three-necked flask, add 150L of water, 1kg of sodium lauryl sulfate, 1L of 25wt% aqueous solution of tetramethylammonium hydroxide, 4L of mercaptopropyl triethoxysilane and 16L of phenyl triethoxysilane After the ethoxysiloxane is mixed evenly, it is added dropwise to the three-necked flask under stirring, and the reaction is continued for 10 hours after the addition of 2 hours, centrifuged, the obtained precipitate is washed with water and then separated, and the powder is obtained after drying. The nuclear magnetic spectrum is as follows: figure 1 , with the structure:

[0034]

[0035] 2. Preparation of polyeugenol-phenylsilsesquioxane:

[0036] Add 10kg of polymercapto-phenylsilsesquioxane powder and 2.5kg of eugenol into a 100L three-necked flask, stir well under mechanical stirring, and then add 1-hydroxycyclohexyl phenyl ketone dissolved in 2L THF Wherein, under the ...

Embodiment 2

[0040] 1. Preparation of polymercapto-phenylsilsesquioxane:

[0041] At 40°C, add 120L of water, 1.2kg of sodium dodecylbenzenesulfonate, 1.4L of 30wt% aqueous solution of tetraethylammonium hydroxide, and 4kg of mercaptopropyl triethoxysilane in a 250L three-neck flask. After mixing evenly with 16kg of phenyltriethoxysiloxane, add it dropwise to a three-necked flask with stirring, continue to react for 15 hours after 2 hours of addition, and centrifuge to separate. The resulting precipitate is washed with water and then separated, and dried to obtain a powder.

[0042] 2. Preparation of polyeugenol-phenylsilsesquioxane:

[0043] Add 10kg of polymercapto-phenylsilsesquioxane powder and 3kg of eugenol to a 100L three-necked flask, stir well under mechanical stirring, then add benzophenone dissolved in 2L THF to it, at a wavelength of 300nm Under the irradiation of ultraviolet light, react at room temperature for 3 h. After the reaction, the solvent was evaporated to dryness a...

Embodiment 3

[0046] 1. Preparation of polymercapto-phenylsilsesquioxane:

[0047] At 30°C, add 140L of water, 1.5kg of potassium dodecylbenzenesulfonate, 1.2L of 25wt% aqueous solution of tetrabutylammonium hydroxide, 5kg of mercaptopropyltriethoxysilane and 50kg of After the phenyltrimethoxysiloxane is mixed evenly, it is added dropwise to the three-necked flask under stirring, and the reaction is continued for 8 hours after 2 hours of addition, and centrifuged, and the obtained precipitate is washed with water and then separated, and dried to obtain a powder.

[0048] 2. Preparation of polyeugenol-phenylsilsesquioxane:

[0049] Add 12kg of polymercapto-phenylsilsesquioxane powder and 4kg of eugenol to a 100L three-necked flask, stir well under mechanical stirring, and then dissolve 3,4-dimethylbenzophenone with 3L THF Add it, and react at room temperature for 4 hours under the irradiation of ultraviolet light with a wavelength of 365 nm. After the reaction, the solvent was evaporated t...

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Abstract

The invention belongs to the technical field of organic silicon high polymers and discloses polyeugenol-phenylsilsesquioxane. Polyeugenol-phenylsilsesquioxane has a structure as follows: the formula is shown in the description, wherein the sum of X, Y, Z and W is 10 to 40 and the sum of the Y, the Z and the W is greater than 1. The invention further discloses a preparation method of polyeugenol-phenylsilsesquioxane; the preparation method comprises the following steps: firstly, taking thiopropyl trialkoxy silane and phenyltrialkoxysilane to react, so as to obtain polythiol-phenylsilsesquioxane; then taking polythiol-phenylsilsesquioxane and eugenol to be subjected to thiol-alkene click chemical reaction to obtain polyeugenol-phenylsilsesquioxane; adding polyeugenol-phenylsilsesquioxane into polycarbonate, and melting and copolymerizing through an ester exchange method to obtain a polycarbonate-polysilsesquioxane copolymer; polyeugenol-phenylsilsesquioxane has good weather resistance and flame-retarding performance, and the impact strength and precipitation resistance of a material are improved.

Description

technical field [0001] The invention belongs to the technical field of organosilicon polymers, and in particular relates to a polyeugenol-phenylsilsesquioxane and a preparation method thereof. Background technique [0002] Polycarbonate (PC) has high heat distortion temperature and glass transition temperature, good toughness, transparency, flame retardancy, electrical insulation and heat resistance, so it is widely used in automobiles, optical devices, aerospace and other fields. Polycarbonate itself can reach the flame retardant grade of UL94-V2. In order to further improve the flame retardant effect of polycarbonate, brominated flame retardants, phosphate flame retardants, and sulfonate flame retardants are usually added to PC. etc., but each of these flame retardants has its limitations. Brominated flame retardants contain bromine, are resistant to discoloration, and have poor weather resistance; phosphate ester flame retardants seriously affect the heat distortion temp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/28C08G77/38C08L69/00C08L83/08
CPCC08G77/28C08G77/38C08G77/80C08L69/00C08L2201/02C08L83/08
Inventor 石磊乔晨光钟国辉
Owner 河源市山德科技有限公司
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