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High-heat-resistant high-toughness low-dielectric-constant fluorenyl benzoxazine resin composition as well as preparation method and application thereof

A technology of benzoxazine resin and oxazine resin, applied in chemical instruments and methods, lamination, layered products, etc., can solve problems such as low bending strength, low product yield, and large steric hindrance

Active Publication Date: 2019-08-30
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But on the other hand, the structure of fluorenyl is too rigid, so that it will have the problems of high brittleness and low bending strength when it is applied.
In response to this problem, many patented technologies have synthesized a series of toughened and modified new fluorenyl benzoxazines through molecular design. For example, CN103936686A synthesized a tetrafunctional fluorenyl benzoxazine. By adjusting fatty amines and substituted or unsubstituted The rigid and flexible groups in the salicylaldehyde compound increase the crosslinking density of benzoxazine and improve the flexibility, but because there are four oxazine ring ring-forming positions in the molecule, the steric hindrance is relatively large, and there will be The problems of benzoxazine low cyclization rate and low product yield (45-80%), similar patents also include CN102702225A and CN103896867A
CN102634019A mentions that bisphenol compounds such as bisphenol A, bisphenol AF, bisphenol F, etc. and bisphenol fluorene are introduced into the fluorenyl benzo structure as a phenol source, and the ratio of bisphenol fluorene to bisphenol compounds is adjusted Heat resistance and flexibility, but it is difficult for this improved polymer to have both high heat resistance and high flexibility
CN102702128A and CN102702129A improve the flexibility of fluorenylbenzoxazine by introducing flexible ester groups and ether bonds, but there is also the problem of low product yield (50-85%)
Moreover, the above-mentioned patent documents only provide the molecular structure of the new fluorenylbenzo, heat resistance data (Tg: 180-390°C, Td5%: 330-420°C) and the theory of flexibility improvement, but fail to provide flexibility. Improvement effect and specific application method
And it has been verified that the dielectric properties of the fluorenylbenzoxazine castables with the above structure are poor (Dk: 3.78-4.42, Df: 0.0067-0.0098), and the high-frequency and high-speed characteristics of 5G communication require copper-clad laminates and laminates The substrate used has better dielectric properties (Dk≤3.5, Df≤0.007)
In addition, Wang Jun from Harbin Engineering University introduced a variety of alkyl segments from the amine source in the paper "Synthesis, Polymerization and Performance Research of Fluorenyl Benzoxazine", so that the synthesized alkyl fluorenyl benzoxazine The flexibility and dielectric properties are good, but because the alkyl group is connected to the amine source, the alkyl group does not remain on the main chain when the benzoxazine is cured, so the pendant alkyl group is easy to fall off, and the heat resistance of the product is poor. Poor (Tg: 180-230°C, Td5%: 310-350°C)

Method used

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  • High-heat-resistant high-toughness low-dielectric-constant fluorenyl benzoxazine resin composition as well as preparation method and application thereof
  • High-heat-resistant high-toughness low-dielectric-constant fluorenyl benzoxazine resin composition as well as preparation method and application thereof
  • High-heat-resistant high-toughness low-dielectric-constant fluorenyl benzoxazine resin composition as well as preparation method and application thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0095] Preparation of the prepreg: select a flat and smooth E-glass fiber cloth with a thickness of 0.2mm, soak it in the above composition (solution), take it out, and then bake it in an oven at 130-170°C for 4-7 minutes. The resin weight percentage content of the prepreg is 32%-68%.

[0096] Preparation of laminated boards: stack the prepreg pieces, cover the top and bottom with a release film, and then place them in a hot press, keeping the heating rate at 1-3°C / min. After reaching the temperature, press 0.2-3MPa and 150- It is formed by pressing at 250°C for 1 to 4 hours.

[0097] Preparation of copper-clad laminate: stack the above prepreg cut pieces, cover both sides or one side of the prepreg with copper foil, and press at 0.2-3MPa pressure and 130-250°C for 1-4 hours.

[0098] The comparison of some technical performances between the high heat-resistant, high-toughness and low-dielectric fluorenyl benzoxazine resin composition copper-clad laminate (halogen-free) prepa...

Embodiment 21

[0126] A high heat-resistant, high-toughness, low-dielectric fluorenyl-benzoxazine resin composition, the high-heat-resistant, high-toughness, low-dielectric fluorenyl-benzoxazine resin composition has a weight ratio of resin: inorganic filler: accelerator : Solvent=100:30:0.01:57 mixture of resin, inorganic filler, accelerator and solvent;

[0127] The resin is a mixture with a weight ratio of benzoxazine resin: DCPD epoxy resin: phosphorus-containing phenolic resin=100:40:10;

[0128] The benzoxazine resin is a fluorenyl benzoxazine resin with high heat resistance, high toughness and low dielectric.

Embodiment 22

[0130] A high heat-resistant, high-toughness, low-dielectric fluorenyl-benzoxazine resin composition, the high-heat-resistant, high-toughness, low-dielectric fluorenyl-benzoxazine resin composition has a weight ratio of resin: inorganic filler: accelerator : Solvent=100:70:1:80 mixture of resin, inorganic filler, accelerator and solvent;

[0131] The resin is a mixture with a weight ratio of benzoxazine resin: DCPD epoxy resin: phosphorus-containing phenolic resin=100:80:40;

[0132] The benzoxazine resin is a fluorenyl benzoxazine resin with high heat resistance, high toughness and low dielectric.

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Abstract

The invention discloses a high-heat-resistant high-toughness low-dielectric-constant fluorenyl benzoxazine resin composition and a preparation method thereof. The high-heat-resistant high-toughness low-dielectric-constant fluorenyl benzoxazine resin composition is characterized in that the resin is a mixture of resin, an inorganic filler, an accelerator and a solvent, wherein a weight ratio of theresin to the inorganic filler to the accelerator to the solvent is 100:(30-70):(0.01-1):(57-80); the resin is a mixture of benzoxazine resin, DCPD epoxy resin and phosphorus-containing phenolic resin, wherein a weight ratio of the benzoxazine resin to the DCPD epoxy resin to the phosphorus-containing phenolic resin is 100:(40-80):(10-40); and the benzoxazine resin is one or more selected from high-heat-resistant high-toughness low-dielectric-constant fluorenyl benzoxazine resin and other benzoxazine resin, wherein a weight ratio of the high-heat-resistant high-toughness low-dielectric-constant fluorenyl benzoxazine resin to the other benzoxazine resin is (60-100):(0-40). The composition provided by the invention is used in the fields of laminated boards, integrated circuit packages, high-frequency high-speed copper-clad boards and high-density internet, and has excellent heat resistance, a lower dielectric constant and dielectric loss factor, better flame retardancy and bending strength, a lower water absorption ratio and the like.

Description

technical field [0001] The invention belongs to a composition containing an organic polymer mixture and its preparation, and relates to a high heat-resistant, high-toughness, low-dielectric fluorenyl benzoxazine resin composition, its preparation method and application. The high heat-resistant, high-toughness and low-dielectric fluorenyl benzoxazine resin composition of the present invention can be used in laminated boards, integrated circuit packaging, high-frequency and high-speed copper-clad laminates, high-density Internet and other fields, and has broad application prospects. Background technique [0002] In recent years, 5G communication has become a research and development hotspot worldwide. Because of its higher reliability and faster speed, it will play a strategic leading role in China's manufacturing 2025. important basic conditions. Due to its data transmission rate and high reliability requirements, 5G communication puts forward very high requirements on the d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L61/34C08L63/00C08L61/06C08K13/02C08K3/36C08K3/22C08K5/3445C08G14/06B32B17/04B32B17/06B32B15/20B32B7/06B32B37/10B32B37/06
CPCC08L61/34C08G14/06B32B5/02B32B5/26B32B7/06B32B15/20B32B15/14B32B37/10B32B37/06C08L2201/08C08L2203/206C08L2203/20C08L2201/02C08L2205/025C08L2205/035C08K2003/2227B32B2260/021B32B2260/046B32B2262/101B32B2307/558B32B2307/546B32B2307/3065B32B2361/00C08L63/00C08L61/06C08K13/02C08K3/36C08K3/22C08K5/3445
Inventor 支肖琼黄杰李建学唐文东赵萧萧
Owner SICHUAN DONGFANG INSULATING MATERIAL
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