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Phthalonitrile-terminated polyphenyl ether and preparation method and application thereof

A technology of phthalonitrile and double-terminated hydroxyl polyphenylene ether, which is applied in the field of polyphenylene ether modified materials and its preparation, can solve the problems of low curing crosslinking density, low activity of functional groups, limited dosing amount, etc.

Inactive Publication Date: 2021-03-26
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the functional group activity of double-terminated hydroxyl polyphenylene ether oligomers is still low, and the crosslinking density with other resins is not high, and the amount of incorporation is limited, which makes polyphenylene ether limited to a certain extent in the application of high-performance high-speed copper clad laminates. upper limit

Method used

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  • Phthalonitrile-terminated polyphenyl ether and preparation method and application thereof
  • Phthalonitrile-terminated polyphenyl ether and preparation method and application thereof
  • Phthalonitrile-terminated polyphenyl ether and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The synthesis route of the phthalonitrile-terminated polyphenylene ether prepared in this example is as follows:

[0043]

[0044] The preparation process of above-mentioned phthalonitrile-terminated polyphenylene ether comprises the following steps:

[0045] (1) Obtain a double-terminated hydroxyl polyphenylene ether solution under the action of a catalyst through oxidative copolymerization of phenolic monomers;

[0046] (11) Add 37.25g of 2,6-xylenol, 34.80g of bisphenol A and an organic solvent composed of 143.30g of toluene and 14.90g of methanol in sequence in the reaction kettle, and stir until the phenolic monomers are completely dissolved; then add 0.6g branched polyethyleneimine (Mn=600) and 0.80g cuprous bromide hydrobromic acid solution A (prepared with 0.10g cuprous oxide and 2.50g 48% hydrobromic acid in advance), after mixing uniformly 150sccm of oxygen was introduced, and the reaction was carried out at 20°C for 3 hours;

[0047] (12) After the react...

Embodiment 2

[0053] The synthesis route of the phthalonitrile-terminated polyphenylene ether prepared in this example is as follows:

[0054]

[0055] The preparation process of above-mentioned phthalonitrile-terminated polyphenylene ether comprises the following steps:

[0056] (1) Obtain a double-terminated hydroxyl polyphenylene ether solution under the action of a catalyst through oxidative copolymerization of phenolic monomers;

[0057] (11) Add 382.75g of 2,6-dimethylphenol, 29.70g of tetramethylbisphenol A and an organic solvent composed of 633.2g of toluene and 65.2g of methanol in sequence in the reaction kettle, and stir until the phenolic monomers are completely Dissolve, add 4.80g N,N-dimethylbutylamine, 1.60g branched polyethyleneimine (Mn=600) and 2.80g cuprous bromide hydrobromic acid solution (pre-prepared with 0.30g cuprous oxide and 2.50 g 48% hydrobromic acid), mix well and feed oxygen at 150 sccm, react at 60°C for 1 hour;

[0058] (12) After the reaction, add 40ml...

Embodiment 3

[0063] The synthesis route of the phthalonitrile-terminated polyphenylene ether prepared in this example is as follows:

[0064]

[0065] The preparation process of above-mentioned phthalonitrile-terminated polyphenylene ether comprises the following steps:

[0066] (1) Obtain a double-terminated hydroxyl polyphenylene ether solution under the action of a catalyst through oxidative copolymerization of phenolic monomers;

[0067] (11) Add 133.50g of 2,6-dimethylphenol, 24.50g of bisphenol F and an organic solvent composed of 430g of toluene and 43.2g of methanol to the reaction kettle in sequence, and stir until the phenolic monomers are completely dissolved; then add 4.50g N,N-dimethylbutylamine, 1.50g branched polyethyleneimine (Mn=600) and 2.80g cuprous bromide hydrobromic acid solution (pre-prepared with 0.30g cuprous oxide and 2.50g 48% Hydrobromic acid preparation), after mixing evenly, feed oxygen at 150 sccm, and react at 40°C for 2 hours;

[0068] (12) After the r...

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Abstract

The invention discloses phthalonitrile-terminated polyphenyl ether and a preparation method and application thereof. The phthalonitrile-terminated polyphenyl ether has a structural formula shown in the specification. The preparation method comprises the following steps: after washing a double-hydroxyl-terminated polyphenyl ether solution by adopting an alkaline aqueous solution, carrying out end-capping reaction on phthalonitrile and polyphenyl ether terminal hydroxyl, and separating and purifying to obtain the phthalonitrile-terminated polyphenyl ether. According to the preparation method, phthalonitrile reacts with terminal hydroxyl of polyphenyl ether, so that the molecular weight of polyphenyl ether can be reduced, the melt viscosity of polyphenyl ether is reduced, processing is facilitated, and meanwhile, the mechanical strength, solvent resistance, flame retardance and the like of polyphenyl ether are improved through a cyano cross-linking reaction; and the application of the resin in high-performance copper-clad plate matrix resin is further expanded.

Description

technical field [0001] The invention belongs to the technical field of polyphenylene ether modification, and relates to a polyphenylene ether modified material capped by phthalonitrile and its preparation method and application. Background technique [0002] Polyphenylene Oxide (PPO) is an engineering plastic with excellent performance. Its structure is an aromatic ring with high rigidity skeleton chain, and there are no hydrolyzable groups and polar groups; this structure makes it have excellent heat resistance Performance, hydrolysis resistance stability, low moisture absorption and good dimensional stability, flame retardancy and excellent adhesion to copper foil, especially in a wide temperature range with excellent dielectric properties, etc. Therefore, polyphenylene ether has great application prospects in high-performance and high-speed copper clad laminates. [0003] Generally commercialized polyphenylene ether has high molecular weight, high softening point and oth...

Claims

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Application Information

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IPC IPC(8): C08G65/48C08G65/44C08L71/12
CPCC08G65/44C08G65/485C08L71/126C08L2201/02C08L2203/20
Inventor 杨刚曾科梁博胡江淮
Owner SICHUAN UNIV
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