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Method for preparing polyamide modified organic silicon resin and paint prepared from resin

A silicone and polyamide technology, 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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  • Method for preparing polyamide modified organic silicon resin and paint prepared from resin
  • Method for preparing polyamide modified organic silicon resin and paint prepared from resin
  • Method for preparing polyamide modified organic silicon resin and paint prepared from resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Preparation of aminated ultrafine zinc oxide

[0035] a) Formula

[0036] Superfine zinc oxide: 30g

[0037] γ-Aminopropyltriethoxysilane: 22.5g

[0038] Toluene: 420g

[0039] b) Preparation process

[0040] Add ultra-fine zinc oxide 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 4.5 hours; filter under reduced pressure, and dry to obtain Aminated Superfine Zinc Oxide 48.8g.

[0041] c) Performance

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

[0043] The ammonia value of aminated superfine zinc oxide is determined by acid-base titration, and the specific steps are as follows: first accurately weigh about 1.5 g of aminated superfine zinc oxide 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...

Embodiment 2

[0096] 1) Preparation of aminated ultrafine zinc oxide

[0097] a) Formula

[0098] Superfine zinc oxide: 40g

[0099] γ-Aminopropyltriethoxysilane: 26g

[0100] Toluene: 350g

[0101] b) Preparation process

[0102] Add ultra-fine zinc oxide and toluene into a reactor equipped with a condenser, thermometer and agitator, disperse evenly at high speed, add γ-aminopropyltriethoxysilane, heat and reflux for 5 hours; filter under reduced pressure, and dry to obtain amino Ultrafine zinc oxide 62g.

[0103] c) Performance

[0104] The particle size of the aminated ultrafine zinc oxide was detected by DSL, and the result was 65nm;

[0105] The ammonia value of the aminated superfine zinc oxide is determined by acid-base titration, and the ammonia value of the above-prepared aminated superfine zinc oxide is 1.75 mmol / g.

[0106] 2) Preparation of silicone oligomers

[0107] a) Composition

[0108] Monomethyltrimethoxysilane: 42.0g (0.28mol)

[0109] Dimethyldimethoxysilane: ...

Embodiment 3

[0148] 1) Preparation of aminated ultrafine zinc oxide

[0149] a) Formula

[0150] Superfine zinc oxide: 40g

[0151] γ-Aminopropyltriethoxysilane: 20g

[0152] Toluene: 400g

[0153] b) Preparation process

[0154] Add ultra-fine zinc oxide 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 Ultrafine zinc oxide 57g.

[0155] c) Performance

[0156] The particle size of the aminated ultrafine zinc oxide was detected by DSL, and the result was 30nm;

[0157] The ammonia value of the aminated ultrafine zinc oxide is determined by acid-base titration, and the ammonia value of the aminated ultrafine zinc oxide prepared above is 1.5 mmol / g.

[0158] 2) Preparation of silicone oligomers

[0159] a) Composition

[0160] Monomethyltrimethoxysilane: 42.0g (0.28mol)

[0161] Dimethyldimethoxysilane: 2...

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Abstract

The invention relates to a method for preparing polyamide modified organic silicon resin. The method includes the following steps that diamine, tribasic acid with the mole number 1 to 2.0 times that of the diamine, aminated superfine zinc oxide with the weight 1 to 2 times that of the diamine, cross-linking catalyst with the weight 1 percent to 5 percent that of the diamine and 2-(2-butoxyethoxy)ethyl acetate with the weight 3 to 8 times that of the diamine are evenly mixed and then heated at 180 DEG C to 220 DEG C for 1 h to 4 h; then, the mixture is cooled to 90 DEG C, organosilicone oligomer with end epoxy groups with the weight 1.5 to 2.0 times that of the diamine is added, and the mixture is heated at 120 DEG C to 140 DEGC for 2 h to 3 h; finally, the mixture is cooled to 90 DEG C, and organic solvent is added to make the solid content range from 40wt% to 50wt%. The resin prepared with the method can be used for preparing high-temperature-resistant paint with low surface energy. According to the method, the aminated superfine zinc oxide, the diamine and the tribasic acid react together to prepare modified hyperbranched polyamide, and thus the heat resistance and the hardness of the polyamide are improved; the modified hyperbranched polyamide and the organosilicone oligomer with end epoxy groups undergo cross-linking reaction, and thus the heat resistance and the hardness of the polyamide are improved.

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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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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