Process for in-situ polymerization preparation of nylon 6/epoxy resin/silicon dioxide nano composite materials

A technology of nano-composite materials and epoxy resin, which is applied in the field of in-situ polymerization of nano-composite materials, can solve the problems such as the decrease of tensile strength, and achieve the improvement of tensile strength, high monomer conversion rate, and extractable oligomers. low content effect

Inactive Publication Date: 2006-10-11
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Domestic patents CN90106778, CN97100554, CN97108021.6, CN99109924, CN00129200.5, CN03115279.1 and foreign patents EP0377511, EP0400964, EP0455507, US63036

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The first step: preparation of epoxy resin siloxane hydrolyzate

[0023] Heat the bisphenol A type epoxy resin (EP) to extract water and small molecules according to the formula, mix it with a certain amount of ethyl orthosilicate, add 0.5wt.% tetrabutyl titanate, under nitrogen protection, in React at 110°C to 130°C for 3 hours, then lower the temperature to 55°C, add a certain amount of THF, distilled water and catalyst 1M HCl (the molar ratio of TEOS, THF, water, and HCl is 1:15:4:0.002), and stir for about 6 hours , a clear and transparent solution was obtained.

[0024] The second step: before or during the caprolactam ring-opening reaction, add epoxy resin siloxane hydrolyzate, water and antioxidant

[0025] Add the epoxy resin silane hydrolyzate prepared in the previous step into 2.0Kg of molten caprolactam, mix well, raise the temperature to 120°C, and remove the solvent and ethanol produced by hydrolysis. Then add 50g distilled water, 1ml concentrated H 3 PO...

Embodiment 2

[0029] The first step: preparation of epoxy resin siloxane hydrolyzate

[0030] Heat the bisphenol A type epoxy resin (EP) to extract water and small molecules according to the formula, mix it with a certain amount of ethyl orthosilicate, add 0.5wt.% tetrabutyl titanate, under nitrogen protection, in React at 110°C to 130°C for 3 hours, then lower the temperature to 55°C, add a certain amount of THF, distilled water and catalyst 1M HCl (the molar ratio of TEOS, THF, water, and HCl is 1:75:4:0.002), and stir for about 6 hours , a clear and transparent solution was obtained.

[0031] The second step: before or during the caprolactam ring-opening reaction, add epoxy resin siloxane hydrolyzate, water and antioxidant

[0032] Add the epoxy resin silane hydrolyzate prepared in the previous step into 2.0Kg of molten caprolactam, mix well, raise the temperature to 120°C, and remove the solvent and ethanol produced by hydrolysis. Then add 50g distilled water, 1ml concentrated H 3 PO...

Embodiment 3

[0036] The first step: preparation of epoxy resin siloxane hydrolyzate

[0037] According to the formula, bisphenol A type epoxy resin (EP) was heated to extract water and small molecules, mixed with a certain amount of ethyl orthosilicate, added 1.5wt.% tetrabutyl titanate, under nitrogen protection, in React at 110°C to 130°C for 3 hours, then lower the temperature to 55°C, add a certain amount of THF, distilled water and catalyst 1M HCl (the molar ratio of TEOS, THF, water, and HCl is 1:5:4:0.002), and stir for about 6 hours , a clear and transparent solution was obtained.

[0038] The second step: before or during the caprolactam ring-opening reaction, add epoxy resin siloxane hydrolyzate, water and antioxidant

[0039] Add the epoxy resin silane hydrolyzate prepared in the previous step into 2.0Kg of molten caprolactam, mix well, raise the temperature to 120°C, and remove the solvent and ethanol produced by hydrolysis. Then add 50g distilled water, 1ml concentrated H 3...

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PUM

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Abstract

The invention discloses an in-situ polymerization method for preparation of nylon 6/epoxide resin/silica dioxide nanocomposite, which consists of the following steps:a)preparing epoxide resin siloxane solution by graft reaction and hydrolytic reaction; b) before or in the aminocaprolactam cycle-open reaction, introducing the epoxide resin siloxane solution into the mediator of the said aminocaprolactam cycle-open reaction, simultaneously adding the water and the anti-oxidant; c) making the aminocaprolactam open ring and polymerize to prepare high-strength and super ductility nylon-6/epoxide resin/silica dioxide nanocomposite. The invention makes the silicate react with the hydroxy group of the epoxide resin under the accelerating effect, then dissolvent, water and acid (or alkali) are added to hydrolyze. Because the silicasol surface graft and adsorb epoxide resin, the agglomeration of the earth silicon nanoparticles can be effectively avoided. On the other hand, because the epoxy radicals can react with the amidol and the carboxyl of the nylon-6 molecular chain to form partial interpenetration network architecture, accordingly the diphasic boundary action can be effectively improved. It has a good cooperating knife-bar with the nano earth silicon, so it can largely improve the bruise resistance of the materials as well as the hot strength of the composite, in which the hot strength has increased by 30 % compared with nylon-6 and the bruise resistance is 3-5 times of the nylon-6.

Description

technical field [0001] The invention belongs to the technical field of polymer nanocomposite materials, and relates to an in-situ polymerization preparation method of nanocomposite materials using caprolactam and epoxy resin siloxane hydrolyzate as raw materials. Background technique [0002] Due to the surface effect, volume effect, and quantum size effect of nanoparticles, coupled with the excellent properties of polymers such as low density, high strength, corrosion resistance, and easy processing, nanocomposites have attracted widespread attention at home and abroad in recent years, and have become a material Emphasis and hotspots of scientific research. [0003] At present, the preparation methods of nanocomposites mainly include sol-gel method, intercalation method, blending method, in-situ polymerization method, etc., and various methods exist to varying degrees. How to avoid phase separation in the preparation process of nanocomposites, increase nano The problem of ...

Claims

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Application Information

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IPC IPC(8): C08L77/02C08L63/00C08G69/16C08K3/36
CPCC08J5/005C08L77/02C08L63/00C08J2363/00C08J2377/02
Inventor 张平王霞瑜赵才贤陆绍荣易兰花姜勇
Owner XIANGTAN UNIV
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