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Preparation method and application of cured nano-structured epoxy resin

A technology of epoxy resin curing and nanostructure, which can be used in epoxy resin coatings, chemical instruments and methods, synthetic resin layered products, etc.

Active Publication Date: 2011-01-05
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] According to the analysis, whether it is self-assembly method or reaction-induced microphase separation method, the phase separation behavior of block copolymers in epoxy systems is greatly affected by solvent, curing agent type, curing temperature and pressure, especially before curing and Therefore, in the prior art, the reported block copolymer / epoxy resin composites obtained by self-assembly method and reaction-induced microphase separation method are generally realized under bulk conditions, and the polymerization method adopted The materials are all linear block copolymers, and there are no reports of the above two methods being mixed and re-solidified in solution.
However, since epoxy resins often need to use solvents or reactive diluents, or change the type of curing agent or temperature and pressure conditions in the actual application process, there are great limitations in the bulk preparation of self-assembly methods or reaction-induced microphase separation methods.

Method used

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  • Preparation method and application of cured nano-structured epoxy resin
  • Preparation method and application of cured nano-structured epoxy resin
  • Preparation method and application of cured nano-structured epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Example 1 Synthesis of Polyethylene Oxide Arm (PEO-arm), Crosslinked Divinylbenzene-Styrene Core [p(DVB-St)-core] Core Crosslinked Star Polymer

[0060] Add MPEO-Br (0.30g, 0.06mmol), cuprous chloride (0.0059g, 0.06mmol), N,N,N',N',N"-pentamethyldi Ethylenetriamine (0.024mL, 0.12mmol), divinylbenzene (0.16mL, 0.90mmol), styrene (0.10mL, 0.90mmol) and anisole (1.2mL), freezing-pumping-melting repeated three times , remove oxygen, then place the flask in a 110°C oil bath under the protection of nitrogen to stir the reaction, stop the reaction after 10h, add tetrahydrofuran to dissolve, pass through a neutral alumina column, remove the catalyst in the product, and add the filtrate dropwise to n-hexane after concentration Precipitate, filter with suction, collect the filter cake and put it in a vacuum oven at 40°C to dry to constant weight. The product is recorded as PEO / p(DVB-St)CCS polymer. Elemental analysis results: C: 66.28; H: 8.78.

Embodiment 2

[0061] Example 2 Core cross-linked star polymerization of poly(ethylene oxide-b-styrene) arm (PEO-b-PS arm), cross-linked divinylbenzene-styrene core [p(DVB-St)-core] synthesis

[0062] PEO-b-PS-Br (0.50g, 0.03mmol), cuprous chloride (0.0030g, 0.03mmol), N, N, N', N', N"- Pentamethyldiethylenetriamine (0.012mL, 0.06mmol), divinylbenzene (0.08mL, 0.45mmol), styrene (0.05mL, 0.45mmol), and anisole (1.2mL), freeze-pump -Melting was repeated three times to remove residual oxygen in the system, then placed the flask in an oil bath at 110°C under nitrogen protection and stirred for 15 hours, then added tetrahydrofuran to dissolve, passed the column to remove the catalyst, concentrated the filtrate, added dropwise to n-hexane to precipitate, and suction filtered , Collect the filter cake and put it in a 40°C vacuum oven to dry to constant weight. The product is recorded as PEO-b-PS / p(DVB-St)CCS polymer. Elemental analysis results: C: 85.26; H: 8.03.

[0063] The molecular weight, a...

Embodiment 3～9

[0071] Weigh the core crosslinked star polymer (CCS), epoxy resin NPEL-128 (Shenzhen Jiadida Chemical Industry Co., Ltd.) and curing agent 4,4'-diaminodiphenylmethane (DDM) according to the weight shown in Table 1, mix Dissolve in tetrahydrofuran to obtain a homogeneous transparent solution, then remove the solvent in vacuum at 40°C, then pour it into a mold while it is hot, and put it in an oven for curing under normal pressure. Take out the cured product at room temperature. The thermal properties of the obtained cured product were characterized by DSC and TGA; the size of the dispersed phase was characterized by AFM or SEM. The selection and proportioning of each component are listed in Table 2, and the performance and structural characterization of the obtained cured product are listed in Table 3. When Examples 3-6 in Table 3 adopt PEO / p(DVB-St)CCS, the nano phase obtained is not a core-shell structure, while Examples 7-9 adopt PEO-b-PS / p(DVB-St)CCS , the nanophase of co...

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Abstract

The invention discloses a method for preparing cured nano-structured epoxy resin. The method comprises the following steps of: mixing 1 to 20 weight percent of nano-sized nuclear cross-linked star polymer and 80 to 99 weight percent of mixture containing epoxy resin and curing agent or uniformly mixing solution of the nano-sized nuclear cross-linked star polymer and the solution of the mixture containing the epoxy resin and the curing agent in a solvent; and curing and molding under the condition that the temperature is between room temperature and 250 DEG C and pressure is between 0 and 10MPa. The cured epoxy resin prepared by the method has a disorder spherical dispersed phase and the average size of between 5 and 200nm, ensures excellent heat processability, has the mechanical properties higher than those of pure epoxy resin, and can be widely applied to paints, electric encapsulating materials and laminated boards. The preparation method is simple, and the phase separating process is not influenced by the curing agent, pressure, solvent and other conditions, so the mechanical properties of the epoxy resin can be improved under the condition that the processability of the epoxy resin is not lost.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a preparation method and application of a cured epoxy resin with a nanostructure. Background technique [0002] Cured epoxy resin has the advantages of good thermal stability, insulation, cohesiveness, good mechanical properties, excellent molding process performance and low cost. In addition, there are many types of epoxy resins and corresponding curing agents, The advantages of a wide range of formula adjustment make it widely used in coatings, bonding of electronic components, packaging and manufacturing of printed circuit boards. It is one of the most important thermosetting materials at present. However, the biggest disadvantage of cured epoxy resin is its high brittleness, such as coatings and profiles made of it are easy to crack or break. Therefore, the toughening of epoxy resin is a hot and difficult point in epoxy resin research, and there are many related ...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08L53/00C08F293/00C09K3/10C09D163/00C09D153/00B32B17/04B32B27/04B32B27/18B32B27/38
Inventor 张兴宏杜滨阳戚国荣
Owner ZHEJIANG UNIV
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