Low-viscosity cyano resin monomer and polymer, and preparation method thereof

A nitrile-based resin and low-viscosity technology, which is applied in the field of low-viscosity nitrile-based resin monomers and polymers and their preparation, can solve the problems that heat resistance and flame retardancy cannot meet material performance requirements, low crosslinking density, and the like, Achieve the effect of good molecular structure design, low water absorption and excellent curing reactivity

Inactive Publication Date: 2013-11-27
725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because benzoxazine has a large number of intramolecular chelating hydrogen bonds during the polymerization process, resulting in low crosslinking density, its heat resistance and flame retardancy are difficult to meet the performance requirements of materials in extreme fields such as the aerospace industry.

Method used

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  • Low-viscosity cyano resin monomer and polymer, and preparation method thereof
  • Low-viscosity cyano resin monomer and polymer, and preparation method thereof
  • Low-viscosity cyano resin monomer and polymer, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Preparation of low-viscosity nitrile resin monomer:

[0041] Add 1g of p-nonylphenol-type phthalonitrile monomer into the reaction vessel, heat to 60°C, then add 9g of tetraphthalonitrile monomer containing benzoxazine ring and stir for 30 minutes; then cool to room temperature.

[0042] The low-viscosity nitrile-based resin monomer thus prepared has a viscosity of 20 Pa.s at room temperature and a curing peak temperature of 223°C.

[0043] (2) Preparation of low-viscosity nitrile-based resin polymer:

[0044] Heating the previously prepared low-viscosity nitrile-based resin monomer to 100-180°C for 1-5 hours to react, and then heat-treating at 240°C for 3-5 hours to obtain the nitrile-based resin polymer.

[0045] The Nitrile Polymer 1010 cm -1 (phthalocyanine ring); 1360 cm -1 and 1520 cm -1 (triazine ring); 1246, 1208 cm -1 (Ar-O-Ar); 832, 782, 729 cm -1The characteristic absorption peaks appeared at the (benzene ring). The low-viscosity nitrile-based resi...

Embodiment 2

[0047] (2) Preparation of low-viscosity nitrile-based resin monomer:

[0048] Add 3g of p-nonylphenol-type phthalonitrile monomer into the reaction vessel, heat to 60°C, then add 7g of tetraphthalonitrile monomer containing benzoxazine ring and stir for 30 minutes; then cool to room temperature.

[0049] The low-viscosity nitrile-based resin monomer thus prepared has a viscosity of 10 Pa.s at room temperature and a curing peak temperature of 228°C.

[0050] (2) Preparation of low-viscosity nitrile-based resin polymer:

[0051] Heating the previously prepared low-viscosity nitrile-based resin monomer to 100-180°C for 1-5 hours to react, and then heat-treating at 240°C for 3-5 hours to obtain a low-viscosity nitrile-based resin polymer.

[0052] The Low Viscosity Nitrile Polymer 1010 cm -1 (phthalocyanine ring); 1360 cm -1 and 1520 cm -1 (triazine ring); 1246, 1208 cm -1 (Ar-O-Ar); 832, 782, 729 cm -1 The characteristic absorption peaks appeared at the (benzene ring). Th...

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Abstract

The invention relates to a low-viscosity cyano resin and a preparation method thereof, belonging to the technical field of organic high polymer materials. The low-viscosity cyano resin is prepared by proportionally mixing benzoxazine-ring-containing tetra-ortho-phthalonitrile resin monomer and diluter with para-nonyl phenol-type phthalonitrile monomer. The benzoxazine-ring-containing tetra-ortho-phthalonitrile resin monomer and nonyl phenol-type phthalonitrile monomer can be blended within a wider proportion range; and the mixture has the advantages of lower and adjustable viscosity at low temperature, favorable flowability, low-temperature curing and other processing properties. Meanwhile, the addition of the para-nonyl phenol-type phthalonitrile monomer has small influence on the heat stability of the benzoxazine-ring-containing tetra-ortho-phthalonitrile resin. The mixed resin has favorable processability of the benzoxazine resin and excellent temperature tolerance of the cyano resin, has the advantages of low-temperature processing, medium-temperature molding and high-temperature application, and can be used in the fields of space navigation and ship structural materials, paints, adhesives, electronic packaging materials and the like. The preparation method is easy to control, has the advantages of low reaction temperature and energy saving, and is suitable for continuous industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic polymer materials, and in particular relates to a low-viscosity nitrile-based resin monomer and polymer and a preparation method thereof. Background technique [0002] Phthalonitrile resins were first synthesized by Keller at the US Naval Laboratory (NRL) in the 1980s. Although phthalonitrile polymers exhibit excellent thermal stability, mechanical properties, thermal oxygen stability and flame retardancy, the processing temperature window of this type of resin is narrow, the curing reaction is very slow, and the concentrated exotherm is obvious. Therefore, these disadvantages severely limit the processability and overall application of this resin. [0003] Benzoxazine resins were first discovered in the 1940s by Holly and Cope in the synthesis of Mannich reaction products. Although it overcomes the shortcomings of traditional phenolic resins that release small molecules during the forming and c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06
Inventor 郑劲东乔冬平马武伟
Owner 725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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