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Preparation method of nano-silicon dioxide composite organic silicon modified hyperbranched polyester resin and coating containing resin

A nano-silica, hyperbranched polyester technology, used in polyester coatings, dyed organosilicon compound treatment, coatings, etc., to achieve the effect of good hardness and high heat resistance

Active Publication Date: 2015-04-29
HANGZHOU JIHUA POLYMER MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the hyperbranched polyester modified silicone resin prepared by the invention still has room for improvement in terms of heat resistance and hardness

Method used

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  • Preparation method of nano-silicon dioxide composite organic silicon modified hyperbranched polyester resin and coating containing resin
  • Preparation method of nano-silicon dioxide composite organic silicon modified hyperbranched polyester resin and coating containing resin
  • Preparation method of nano-silicon dioxide composite organic silicon modified hyperbranched polyester resin and coating containing resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Preparation of organically modified nano-silica

[0027] a) Formula

[0028] Nano silica: 20g

[0029] 3-(2,3-Glycidoxy)propyltrimethoxysilane: 0.8g

[0030] Ethanol: 400g

[0031] Water: 100g

[0032] b) Preparation process

[0033] Add nano-silica, ethanol and water in the reactor equipped with condenser tube, thermometer and stirrer, add 3-(2,3-glycidoxy) propyltrimethoxysilane after high-speed dispersion, at 55 The reaction was carried out under reflux in a water bath at °C for 8 hours. After the reaction was stopped, the temperature was lowered to room temperature. The product was centrifuged and washed to obtain 18.7 g of organically modified nano-silica.

[0034] c) Performance

[0035] The particle size of organically modified nano-silica was detected by DSL, and the result was 20nm;

[0036] The epoxy value of the organically modified nano-silica was measured by the hydrochloric acid-acetone method, and the result was 12.6 mmol / g.

[0037] 2) Prepara...

Embodiment 2

[0073] 1) Preparation of organically modified nano-silica

[0074] a) Formula

[0075] Nano silica: 20g

[0076] 3-(2,3-Glycidoxy)propyltrimethoxysilane: 1.6g

[0077] Ethanol: 1200g

[0078] Water: 300g

[0079] b) Preparation process

[0080] Add nano-silica, ethanol and water in the reactor equipped with condenser tube, thermometer and stirrer, add 3-(2,3-glycidoxy) propyltrimethoxysilane after high-speed dispersion, at 55 °C water bath was refluxed for 16 hours. After the reaction was stopped, the temperature was lowered to room temperature. The product was centrifuged and washed to obtain 19.5 g of organically modified nano-silica.

[0081] c) Performance

[0082] The particle size of organically modified nano-silica was detected by DSL, and the result was 100nm;

[0083] The epoxy value of the organically modified nano silica was measured by the hydrochloric acid-acetone method, and the result was 11.5 mmol / g.

[0084] 2) Preparation of silicone oligomers

[008...

Embodiment 3

[0119] 1) Preparation of organically modified nano-silica

[0120] a) Formula

[0121] Nano silica: 30g

[0122] 3-(2,3-Glycidoxy)propyltrimethoxysilane: 1.5g

[0123] Ethanol: 600g

[0124] Water: 150g

[0125] b) Preparation process

[0126] Add nano-silica, ethanol and water in the reactor equipped with condenser tube, thermometer and stirrer, add 3-(2,3-glycidoxy) propyltrimethoxysilane after high-speed dispersion, at 55 ℃ water bath reflux reaction for 24 hours, after the reaction was stopped, the temperature was lowered to room temperature, and the product was centrifuged and washed to obtain 28.5 g of organically modified nano-silica.

[0127] c) Performance

[0128] The particle size of organically modified nano-silica was detected by DSL, and the result was 20nm;

[0129] The epoxy value of the organically modified nano silica was measured by the hydrochloric acid-acetone method, and the result was 16.5 mmol / g.

[0130] 2) Preparation of silicone oligomers

...

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Abstract

The invention discloses a preparation method of nano-silicon dioxide composite organic silicon modified hyperbranched polyester resin and a coating containing the resin. The method comprises the following steps: firstly preparing organic modified nano-silicon dioxide from nano-silicon dioxide, ethanol, water and 3-(2, 3-epoxypropoxy) propyltrimethoxysilane; uniformly mixing a binary acid, a trihydric alcohol, a crosslinking catalyst and dimethylbenzene, then heating to 170-210 DEG C, performing heat preservation for 1-3h, then heating to 225 DEG C, adding organic modified nano-silicon dioxide, performing heat preservation for 1h, then cooling to 85 DEG C, and adding an organic silicone oligomer; heating to 110-130 DEG C and then performing heat preservation for 1.5-2.5h; and cooling to 85 DEG C and adding an organic solvent to enable the solid content to be 51-60% by weight. According to the method, modified hyperbranched polyester is prepared by reaction of organic modified nano-silicon dioxide, the binary acid and the trihydric alcohol, so that the hardness of the polyester is improved; and crosslinking reaction is performed on the organic silicone oligomer and the polyester, so that the heat resistance of the polyester is improved. The polyester resin prepared by the method can be used for preparing high-temperature resistant low-surface energy coatings.

Description

technical field [0001] The invention relates to the field of preparation of organic polymer compounds, in particular to polymer compounds obtained by esterification, and in particular to hyperbranched polyester resins. Background technique [0002] Polyester resin is a general term for polymer compounds formed by polycondensation of diols or dibasic acids or polyols and polybasic acids. Pressurized and fast curing, its heat resistance, wear resistance, chemical resistance and mechanical properties are good. Mainly used for bonding glass fiber reinforced plastics, hard plastics, concrete, electrical pots, etc. Polyester resin is also widely used in the coating industry, but it also has obvious disadvantages, such as: polyester resin has a large molecular weight and poor solubility. High viscosity, difficult to chemically modify with other resins. [0003] The hyperbranched polyester resin after hyperbranching has a highly branched structure and a large number of terminal ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/91C08G81/00C08G63/127C08G63/78C09D167/00C09D7/12C09C1/28C09C3/12
Inventor 钱涛王晓莉刘海兵
Owner HANGZHOU JIHUA POLYMER MATERIAL CO LTD