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Preparation method of modified terminal-carboxyl-hyperbranched polyamide resin and paint containing resin

A polyamide resin and carboxyl-terminated technology, which is applied in the field of organic polymer compounds, can solve problems such as cracking and poor flexibility, and achieve high heat resistance, good flexibility, good acid resistance and water 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

However, the carboxyl-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 terminal-carboxyl-hyperbranched polyamide resin and paint containing resin
  • Preparation method of modified terminal-carboxyl-hyperbranched polyamide resin and paint containing resin
  • Preparation method of modified terminal-carboxyl-hyperbranched polyamide resin and paint containing 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: 0.1g

[0038] Concentrated sulfuric acid: 12g

[0039] Allyl glycidyl ether: 20g

[0040] Chloroplatinic acid: 0.1g

[0041] Toluene: 400g

[0042] b) Preparation process

[0043] After adding octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and concentrated sulfuric acid to the reactor equipped with condenser, thermometer, dropping funnel and stirrer according to the ratio, the reaction was protected by nitrogen for 9h; the temperature was raised to 180 ℃, vacuum distillation to remove low-boiling substances to obtain hydrogen-terminated silicone oil; add hydrogen-terminated silicone oil, allyl glycidyl ether, toluene and chloroplatinic acid into the reactor; heat up to 90 ℃, nitrogen protection reaction for 10 hours, vacuum distillation The solvent is removed to obtain epoxy-terminated silicone oil.

[0044] c) Performan...

Embodiment 2

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

[0075] a) Formula

[0076] Octamethylcyclotetrasiloxane: 200g

[0077] Tetramethylammonium hydroxide: 0.05g

[0078] Concentrated sulfuric acid: 6g

[0079] Allyl glycidyl ether: 11g

[0080] Chloroplatinic acid: 0.05g

[0081] Toluene: 320g

[0082] b) Preparation process

[0083] After adding octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and concentrated sulfuric acid to the reactor equipped with condenser, thermometer, dropping funnel and stirrer in sequence according to the ratio, the reaction was protected by nitrogen for 8h; the temperature was increased to 180 ℃, vacuum distillation to remove low-boiling substances to obtain hydrogen-terminated silicone oil; add hydrogen-terminated silicone oil, allyl glycidyl ether, toluene and chloroplatinic acid into the reactor; increase the temperature to 85°C, and react under nitrogen protection for 8.5 hours. The solvent is distilled off to obtain epoxy-terminated silicon...

Embodiment 3

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

[0113] a) Formula

[0114] Octamethylcyclotetrasiloxane: 200g

[0115] Tetramethylammonium hydroxide: 0.03g

[0116] Concentrated sulfuric acid: 3g

[0117] Allyl glycidyl ether: 3g

[0118] Chloroplatinic acid: 0.02g

[0119] Toluene: 240g

[0120] b) Preparation process

[0121] After adding octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and concentrated sulfuric acid to the reactor equipped with condenser, thermometer, dropping funnel and stirrer in sequence according to the ratio, the reaction was protected by nitrogen for 8h; the temperature was increased to 180 ℃, vacuum distillation to remove low-boiling substances to obtain hydrogen-terminated silicone oil; add hydrogen-terminated silicone oil, allyl glycidyl ether, toluene and chloroplatinic acid into the reactor; increase the temperature to 80 ℃, nitrogen protection reaction 10h, vacuum distillation The solvent is removed to obtain epoxy-terminated silicone oi...

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Abstract

The invention relates to a preparation method of modified terminal-carboxyl-hyperbranched polyamide resin. The method comprises the following steps of: uniformly mixing diamine and ternary acid with the mole number of 1-2.0 times that of the diamine, then heating to 70-90 DEG C, and adding terminal epoxy group silicone oil with the weight of 0.05-0.1 times that of the diamine and dimethylbenzene with the weight of 0.02-0.1 times that of the diamine; heating for 1-3 hours at the temperature of 180-210 DEG C, warming to 220-240 DEG C, and heating for 1-3 hours; cooling to 90 DEG C, adding an organic solvent with the weight of 1.0-1.5 times that of the diamine, an organic silicon low polymer with the weight of 1.5-2.0 times that of the diamine and a crosslinking catalyst with the weight of 1-5% that of the diamine; warming to 110-120 DEG C, and heating for 2-3 hours; and cooling to 90 DEG C, and finally adding the organic solvent to adjust solid content to 60-70%, so that the modified terminal-carboxyl-hyperbranched polyamide resin is obtained. The resin prepared by adopting the preparation method provided by the invention can be used for preparing high temperature resistant low-surface-energy paint. According to the preparation method provided by the invention, when the terminal-carboxyl-hyperbranched polyamide resin is synthesized, the terminal epoxy group silicon oil is added, so as to improve the heat-resisting performance and flexibility of polyamide; and crosslinking reaction is carried out on the organic silicon low polymer and the polyamide, so as to improve the heat-resisting performance of the polyamide.

Description

Technical field [0001] The invention relates to the field of organic polymer compounds, relates to polymer compounds obtained by amidation reaction, and specifically relates to polyamide resins. Background technique [0002] Polyamide resin has excellent heat resistance, abrasion 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 a large molecular weight, poor solubility, and high viscosity, making it difficult to chemically modify with other resins. In order to obtain polyamide resins with low viscosity and good solubility, dimer acid and diamine polymerization are commonly used. For example, Wu Jianliang et al. (Wu Jianliang, Development of Low Molecular Weight Polyamide Resin, Zhejiang Chemical Industry, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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