Preparation method of hyperbranched polyamide modified organic silicon resin and paint prepared from resin

A technology of hyperbranched polyamide and organosilicon, applied in the field of polyamide resin, can solve problems such as unsatisfactory hardness of organosilicon resin, and achieve the effects of good hardness and high heat resistance

Inactive Publication Date: 2014-08-20
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 hyperbranched polyamide modified organic silicon resin and paint prepared from resin
  • Preparation method of hyperbranched polyamide modified organic silicon resin and paint prepared from resin
  • Preparation method of hyperbranched 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 silica

[0035] a) Formula

[0036] Ultrafine silica: 20g

[0037] γ-Aminopropyltriethoxysilane: 8g

[0038] Toluene: 300g

[0039] b) Preparation process

[0040] Add ultra-fine silica and toluene into a reactor equipped with a condenser tube, a thermometer and a stirrer, disperse evenly at a high speed, add γ-aminopropyltriethoxysilane, heat and reflux for 2 hours; filter under reduced pressure, and dry to obtain Aminated ultrafine silica 26.3g.

[0041] c) Performance

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

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

Embodiment 2

[0096] 1) Preparation of aminated ultrafine silica

[0097] a) Formula

[0098] Ultrafine silica: 40g

[0099] γ-(2,3-Glycidoxy)propylmethyldimethoxysilane: 32g

[0100] Toluene: 400g

[0101] b) Preparation process

[0102] Add superfine silicon dioxide and toluene into the reactor equipped with condenser tube, thermometer and stirrer, and add γ-(2,3-glycidoxy)propylmethyldimethoxysilane after high-speed dispersion, Heat to reflux for 5 hours; filter under reduced pressure, and dry to obtain 69.7 g of aminated ultrafine silicon dioxide.

[0103] c) Performance

[0104] The particle size of aminated ultrafine silica was detected by DSL, and the result was 150nm;

[0105] The ammonia value of the aminated ultrafine silicon dioxide is determined by acid-base titration method, and the ammonia value of the aminated ultrafine silicon dioxide prepared above is 2 mmol / g.

[0106] 2) Preparation of silicone oligomers

[0107] a) Composition

[0108] Monomethyltrimethoxysilane...

Embodiment 3

[0149] 1) Preparation of aminated ultrafine silica

[0150] a) Formula

[0151] Ultrafine silica: 30g

[0152] γ-Aminopropyltriethoxysilane: 15g

[0153] Toluene: 300g

[0154] b) Preparation process

[0155] Add ultra-fine silica and toluene into the reactor equipped with condenser tube, thermometer and stirrer, disperse evenly at high speed, add γ-aminopropyltriethoxysilane, heat and reflux for 3 hours; filter under reduced pressure, and dry to obtain Aminated ultrafine silica 43.6g.

[0156] c) Performance

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

[0158] The ammonia value of the aminated ultrafine silicon dioxide is measured by acid-base titration, and the ammonia value of the above-mentioned prepared aminated ultrafine silicon dioxide is 1.49 mmol / g.

[0159] 2) Preparation of silicone oligomers

[0160] a) Composition

[0161] Monomethyltrimethoxysilane: 42.0g (0.28mol)

[0162] Dimethyldimethoxysilan...

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Abstract

The invention relates to a preparation method of a hyperbranched polyamide modified organic silicon resin, which comprises the following steps: uniformly mixing diamine, tribasic acid which is 1-2.0 times of diamine by mole, aminated superfine silicon dioxide which is 1-2 times of diamine by weight, a crosslinking catalyst which is 1-5% of diamine by weight, and dipropylene glycol monobutyl ether acetate which is 3-8 times of diamine by weight, and heating at 180-220 DEG C for 1-4 hours; cooling to 90 DEG C, adding epoxy-terminated organic silicon low polymer which is 1.5-2.0 times of diamine by weight, and heating at 120-140 DEG C for 2-3 hours; and finally, cooling to 90 DEG C, and adding an organic solvent until the solid content is 40-50 wt%. The resin prepared by the method can be used for preparing a high-temperature-resistant low-surface-energy paint. The aminated superfine silicon dioxide, diamine and tribasic acid react together to prepare the modified hyperbranched polyamide, thereby enhancing the heat resistance and hardness of the polyamide; and the modified hyperbranched polyamide and the epoxy-containing organic silicon low polymer are subjected to crosslinking reaction, thereby enhancing the heat resistance and hardness of the polyamide.

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): C08G69/42C08G77/14C08K9/06C08K3/36C09D177/06
Inventor 刘瑞源严轶琛路新卫游文伟
Owner SOUTHERN MEDICAL UNIVERSITY
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