Preparation method of high-hardness polyamide modified organic silicon resin and coatings containing high-hardness polyamide modified organic silicon resin

A technology of polyamide and silicone, which is applied in the field of polyamide resin, can solve the problem of unsatisfactory hardness of silicone resin, and achieve the effect of good hardness and high heat resistance

Inactive Publication Date: 2014-08-27
SOUTHERN MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But the hardness of the silicone resin obtained by the above-mentioned prior art is still not ideal enough

Method used

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  • Preparation method of high-hardness polyamide modified organic silicon resin and coatings containing high-hardness polyamide modified organic silicon resin
  • Preparation method of high-hardness polyamide modified organic silicon resin and coatings containing high-hardness polyamide modified organic silicon resin
  • Preparation method of high-hardness polyamide modified organic silicon resin and coatings containing high-hardness polyamide modified organic silicon resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Preparation of aminated ultrafine alumina

[0035] a) Formula

[0036] Ultrafine alumina: 30g

[0037] γ-Aminopropyltriethoxysilane: 12g

[0038] Toluene: 500g

[0039] b) Preparation process

[0040] Add ultra-fine alumina and toluene into a reactor equipped with a condenser, thermometer and agitator, disperse evenly at high speed, add γ-aminopropyltriethoxysilane, heat and reflux for 3 hours; filter under reduced pressure, and dry to obtain amino 39g of superfine alumina.

[0041] c) Performance

[0042] The particle size of aminated ultrafine alumina was detected by DSL, and the result was 100nm;

[0043]The ammonia value of aminated superfine alumina is determined by acid-base titration, and the specific steps are as follows: First, accurately weigh about 1.5 g of aminated superfine alumina in a conical flask, add 20 mL of tetrahydrofuran and toluene, and stir to make it Disperse evenly; add 3 to 4 drops of methyl orange indicator, and titrate with hydroch...

Embodiment 2

[0095] 1) Preparation of aminated ultrafine alumina

[0096] a) Formula

[0097] Ultrafine alumina: 40g

[0098] γ-(2,3-Glycidoxy)propylmethyldimethoxysilane: 32g

[0099] Toluene: 600g

[0100] b) Preparation process

[0101] Add ultra-fine alumina and toluene into the reactor equipped with condenser tube, thermometer and stirrer, disperse evenly at high speed, add γ-(2,3-glycidoxy)propylmethyldimethoxysilane, heat Reflux for 5 hours; filter under reduced pressure, and dry to obtain 68 g of aminated superfine alumina.

[0102] c) Performance

[0103] The particle size of aminated ultrafine alumina was detected by DSL, and the result was 150nm;

[0104] The ammonia value of the aminated ultrafine alumina is determined by acid-base titration, and the ammonia value of the aminated ultrafine alumina prepared above is 2 mmol / g.

[0105] 2) Preparation of epoxy-terminated silicone oligomers

[0106] I) preparation of organosilicon oligomer

[0107] a) Composition

[0108]...

Embodiment 3

[0149] 1) Preparation of aminated ultrafine alumina

[0150] a) Formula

[0151] Ultrafine alumina: 40g

[0152] γ-Aminopropyltriethoxysilane: 20g

[0153] Toluene: 400g

[0154] b) Preparation process

[0155] Add ultra-fine alumina and toluene into a reactor equipped with a condenser, a thermometer and a stirrer, disperse evenly at a high speed, add γ-aminopropyltriethoxysilane, heat and reflux for 3 hours; filter under reduced pressure, and dry to obtain amino Ultrafine alumina 57g.

[0156] c) Performance

[0157] The particle size of aminated ultrafine alumina was detected by DSL, and the result was 30nm;

[0158] The ammonia value of the aminated ultrafine alumina was determined by acid-base titration, and the ammonia value of the above-prepared aminated ultrafine alumina was 1.48 mmol / g.

[0159] 2) Preparation of silicone oligomers

[0160] a) Composition

[0161] Monomethyltrimethoxysilane: 42.0g (0.28mol)

[0162] Dimethyldimethoxysilane: 22.7g (0.17mol)

...

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Abstract

The invention relates to a preparation method of high-hardness polyamide modified organic silicon resin. The method comprises the following steps that diamine, tribasic acid, aminated ultrafine alumina, a crosslinking catalyst and xylene are mixed evenly and heated at 180 DEG C-220 DEG C for 1 h-4 h, wherein the mole number of the tribasic acid is 1-2.0 times that of the diamine, the weight of the aminated ultrafine alumina is 1-2 times that of the diamine, the weight of the crosslinking catalyst is 1 percent-5 percent that of the diamine, and the weight of the xylene is 3-8 times that of the diamine; afterwards, the temperature is reduced to 90 DEG C, end-epoxy group organosilicone oligomer is added, and the mixture is heated at 120 DEG C-140 DEG C for 2 h-3 h, wherein the weight of the end-epoxy group organosilicone oligomer is 1.5-2.0 times that of the diamine; finally, the temperature is reduced to 90 DEG C, and an organic solvent is added, so that the solid content is 40 percent-50 percent by weight. The resin prepared through the method can be used for manufacturing high-temperature-resistant low-surface-energy coatings. According to the method, the aminated ultrafine alumina, the diamine and the tribasic acid react together to prepare modified hyperbranched polyamide, and the heat resistance and the hardness of polyamide are enhanced; as the modified hyperbranched polyamide and the epoxy-group-containing organosilicone oligomer are in a cross-linking reaction, the heat resistance and the hardness of the polyamide are further enhanced.

Description

technical field [0001] The invention relates to the field of organic macromolecular compounds, and relates to a macromolecular compound obtained by amidation reaction, in particular to a polyamide resin. Background technique [0002] Polyamide resin has excellent heat resistance, wear resistance, chemical resistance, good mechanical properties and processing properties, low friction coefficient, certain flame retardancy, easy processing, and is widely used as engineering plastics. Polyamide has good compatibility with various resins and is widely used in the coating industry. However, polyamide resin has large molecular weight, poor solubility, high viscosity, and is difficult to chemically modify with other resins. Hyperbranched polyamide resin has a highly branched structure and a large number of terminal active groups, with high solubility, low viscosity and high chemical reactivity, which make hyperbranched polyamide resin attractive in many aspects. Application prospe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/00C08G83/00C08G69/26C08G69/42C08K9/06C08K3/22C09D187/00
Inventor 刘瑞源严轶琛路新卫游文伟
Owner SOUTHERN MEDICAL UNIVERSITY
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