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Preparation method of modified amino-terminated hyper-branched polyamide resin and coating comprising resin

A polyamide resin and amino-terminated technology, which is applied in the field of polyamide resin, can solve problems such as cracking and poor flexibility, and achieve the effects of high heat resistance, good flexibility, and good heat resistance

Inactive Publication Date: 2013-03-20
SOUTHERN MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amino-terminated hyperbranched polyamide-modified silicone resin prepared above has poor flexibility and will crack under high and low temperature alternating conditions, which limits its application.

Method used

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  • Preparation method of modified amino-terminated hyper-branched polyamide resin and coating comprising resin
  • Preparation method of modified amino-terminated hyper-branched polyamide resin and coating comprising resin
  • Preparation method of modified amino-terminated hyper-branched polyamide resin and coating comprising resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Preparation of epoxy-terminated silicone oil

[0035] a) Formula

[0036] Octamethylcyclotetrasiloxane: 200g

[0037] Tetramethylammonium hydroxide: 0.02g

[0038] Concentrated sulfuric acid: 4g

[0039] Allyl glycidyl ether: 2g

[0040] Chloroplatinic acid: 0.02g

[0041] Toluene: 200g

[0042] b) Preparation process

[0043] After adding octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and concentrated sulfuric acid in the reactor equipped with a condenser tube, a thermometer, a dropping funnel and a stirrer in sequence, the nitrogen protection reaction was carried out for 7 hours; the temperature was raised to 180 ℃, remove low boilers by distillation under reduced pressure to obtain hydrogen-terminated silicone oil; add hydrogen-terminated silicone oil, allyl glycidyl ether, toluene and chloroplatinic acid into the reactor; heat up to 70 °C, react under nitrogen protection for 8 hours, and distill under reduced pressure The solvent was removed t...

Embodiment 2

[0074] 1) Preparation of epoxy-terminated silicone oil

[0075] a) Formula

[0076] Octamethylcyclotetrasiloxane: 200g

[0077] Tetramethylammonium hydroxide: 0.1g

[0078] Concentrated sulfuric acid: 12g

[0079] Allyl glycidyl ether: 20g

[0080] Chloroplatinic acid: 0.1g

[0081] Toluene: 400g

[0082] b) Preparation process

[0083] After adding octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and concentrated sulfuric acid in the reactor equipped with a condenser tube, a thermometer, a dropping funnel and a stirrer in sequence, the nitrogen protection reaction was carried out for 9 hours; the temperature was raised to 180 ℃, remove low boilers by distillation under reduced pressure to obtain hydrogen-terminated silicone oil; add hydrogen-terminated silicone oil, allyl glycidyl ether, toluene and chloroplatinic acid into the reactor; raise the temperature to 90℃, react under nitrogen protection for 10h, and distill under reduced pressure The solvent was r...

Embodiment 3

[0112] 1) Preparation of epoxy-terminated silicone oil

[0113] a) Formula

[0114] Octamethylcyclotetrasiloxane: 200g

[0115] Tetramethylammonium hydroxide: 0.06g

[0116] Concentrated sulfuric acid: 10g

[0117] Allyl glycidyl ether: 18g

[0118] Chloroplatinic acid: 0.07g

[0119] Toluene: 300g

[0120] b) Preparation process

[0121] After adding octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and concentrated sulfuric acid sequentially in the reactor equipped with a condenser tube, a thermometer, a dropping funnel and a stirrer, the nitrogen protection reaction was carried out for 8 hours; the temperature was raised to 180 ℃, remove low boilers by distillation under reduced pressure to obtain hydrogen-terminated silicone oil; add hydrogen-terminated silicone oil, allyl glycidyl ether, toluene and chloroplatinic acid into the reactor; raise the temperature to 80℃, react under nitrogen protection for 9 hours, and distill under reduced pressure The solven...

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Abstract

The invention relates to a preparation method of modified amino-terminated hyper-branched polyamide resin. The method comprises the following steps: uniformly mixing binary acid and melamine with the mol amount which is 1.2-1.8 times as much as that of the binary acid to 70-90 DEG C; adding epoxy-terminated silicone oil with the weight which is 0.05-0.1 time as much as that of the binary acid and dimethylbenzene with the weight which is 0.02-0.1 time as much as that of the binary acid; heating at 180-210 DEG C for 1-3 hours; raising the temperature to 220-240 DEG C and heating for 1-3 hours; then, reducing the temperature to 90 DEG C; adding an organic solvent with the weight which is 1.0-1.5 times as much as that of the binary acid, an organic oligomer with the weight which is 1.5-2.0 times as much as that of the binary acid and a cross-linking catalyst which is 1-5% of the weight of the binary acid; raising the temperature to 110-120 DEG C and heating for 2-3 hours; and finally, reducing the temperature to 90 DEG C and adding the organic agent to adjust the solid content to 60-70%. According to the method disclosed by the invention, the epoxy-terminated silicone oil is added when amino-terminated hyper-branched polyamide is synthesized, so that the thermal resistance and the flexibility of the polyamide are improved; and the organic oligomer and the polyamide are subjected to a cross-linking reaction so that the thermal resistance of the polyamide is improved. The polyamide resin prepared by the method can be used for preparing a coating which is high-temperature-resisting and has a good flexibility.

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. In order to obtain polyamide resins with low viscosity and good solubility, dimer acids and diamines are often used for polymerization. For example, Wu Jianliang et al. (Wu Jianliang, Development of low molecular weight polyamide resin, Zhejiang Chemical Indust...

Claims

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Application Information

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IPC IPC(8): C08G69/42C08G77/14C09D177/06
Inventor 刘瑞源游文玮路新卫席华松严轶琛
Owner SOUTHERN MEDICAL UNIVERSITY
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