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Benzoxazine monomer, benzoxazine precursor and low-dielectric benzoxazine resin

A benzoxazine and precursor technology, which is applied in the field of silicon-containing benzoxazine resins, can solve the problems of micro-phase separation of materials and damage to mechanical properties, unsuitable for industrial applications, uneven dispersion of components, etc., and achieves good toughness. , the effect of stable intermediate products and low dielectric constant

Inactive Publication Date: 2012-07-18
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has disadvantages such as uneven dispersion of components, microscopic phase separation of materials, and damage to mechanical properties; there are also nano-hybrid materials of polyhedral silsesquioxane and benzoxazine resin prepared by chemical structure design, but this method High raw material cost, not suitable for industrial applications

Method used

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  • Benzoxazine monomer, benzoxazine precursor and low-dielectric benzoxazine resin
  • Benzoxazine monomer, benzoxazine precursor and low-dielectric benzoxazine resin
  • Benzoxazine monomer, benzoxazine precursor and low-dielectric benzoxazine resin

Examples

Experimental program
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Effect test

Embodiment 1

[0051] A method for preparing a silicon-containing benzoxazine monomer, comprising the following steps:

[0052] In a reaction vessel with a stirrer and a thermometer, load 150ml of solvent chloroform, 24.03g (0.8mol) of paraformaldehyde and 44.2g (0.4mol), 3-aminopropyltriethoxysilane (KH550), and react at 40°C 1 hour. Then, 22.8 g (0.1 mol) of bisphenol A was added to the reaction mixture, and the temperature was raised to 85° C. and refluxed for 4 h under rapid stirring. After the reaction was completed, the insoluble matter was removed by filtration to obtain a yellow-green liquid. The solvent is distilled off under reduced pressure to obtain a bisphenol A benzoxazine monomer containing a silane coupling agent. 63 g of the monomer was obtained, and the yield was 80.7%. The silsesquioxane is a yellow-green viscous fluid (viscosity 2986 Nepal).

[0053] The H NMR spectra of the above products are as follows: figure 1 As shown, 4.81(a) and 3.92(b) in the figure are the c...

Embodiment 2

[0062] A method for preparing a silicon-containing benzoxazine monomer, comprising the following steps:

[0063] In a reaction vessel with a stirrer and a thermometer, load 150ml of solvent chloroform, 24.03g (0.8mol) of paraformaldehyde and 44.2g (0.4mol), 3-aminopropyltriethoxysilane (KH550), and react at 40°C 1 hour. Then, 35.5 g (0.1 mol) of bisphenol fluorene was added to the reaction mixture, and the temperature was raised to 85° C. and refluxed for 4 h under rapid stirring. After the reaction was completed, the insoluble matter was removed by filtration to obtain a yellow-green liquid. The solvent is distilled off under reduced pressure to obtain a product which is a bisphenol A benzoxazine monomer containing a silane coupling agent. 78 g of the monomer was obtained with a yield of 84.7%. The silsesquioxane is a yellow-green viscous fluid (viscosity 2986 Nepal).

[0064] The H NMR spectra of the above products, such as figure 2 As shown, 4.82(a) and 3.83(b) in the...

Embodiment 3

[0073] A method for preparing a silicon-containing benzoxazine monomer, comprising the following steps:

[0074] In a reaction vessel with a stirrer and a thermometer, load 150ml of solvent chloroform, 24.03g (0.8mol) of paraformaldehyde and 44.2g (0.4mol), 3-aminopropyltriethoxysilane (KH550), and react at 40°C 1 hour. Then, 18.8 g (0.2 mol) of phenol was added to the reaction mixture, and the temperature was raised to 85° C. and refluxed for 4 h under rapid stirring. After the reaction was completed, the insoluble matter was removed by filtration to obtain a yellow-green liquid. The solvent is distilled off under reduced pressure to obtain a product that is a phenolic benzoxazine monomer containing a silane coupling agent. 63 g of the monomer was obtained, and the yield was 80.7%. The silsesquioxane is a yellow-green viscous fluid (viscosity 2986 Nepal).

[0075] The infrared spectrum of the above product is as follows image 3 shown. From image 3 Medium, 1234cm - a...

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Abstract

The invention discloses a silicon-based benzoxazine monomer, a silicon-based benzoxazine precursor and low-dielectric silicon-based benzoxazine resin. An oily solvent, paraformaldehyde and an amino silane coupling agent are subjected to heating reflux reaction, so as to obtain the silicon-based benzoxazine monomer. The silicon-based benzoxazine monomer, an aqueous solvent and a catalytic agent are subjected to hydrolysis reaction, so as to obtain the silicon-based benzoxazine precursor. The silicon-based benzoxazine monomer or the silicon-based benzoxazine precursor is heated and cured gradually so as to prepare low-dielectric silicon-based benzoxazine resin. The low-dielectric silicon-based benzoxazine resin achieves low dielectric constant and high heat resistance; a great number of flexible cells are brought in molecular chains, so that the low-dielectric silicon-based benzoxazine resin achieves better toughness; and the low-dielectric silicon-based benzoxazine resin is a material with more excellent processing characteristics, mechanical properties, electric properties and heat resistance.

Description

technical field [0001] The invention relates to a silicon-containing benzoxazine resin, in particular to a silicon-containing benzoxazine monomer and a preparation method thereof, a silicon-containing benzoxazine precursor, and a low-dielectric silicon-containing Benzoxazine resins and their applications. Background technique [0002] With the development of electronic information technology, manufacturing high-speed, high-efficiency multi-functional integrated circuits has become the goal of the current development of the electronics industry. Electrically lossy electronic packaging materials. [0003] Benzoxazine is a kind of benzoxazine resin that has been proved to have a lower dielectric constant. The dielectric constant of ordinary benzoxazine is about 3.5, and this type of resin has good heat resistance and low water absorption. properties, which makes it have a wide range of potential applications in the field of electronic packaging materials. Materials with lowe...

Claims

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Application Information

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IPC IPC(8): C07F7/18C08G77/452C09D183/10C09J183/10C08G73/06C09D179/04C09J179/04
Inventor 许凯付子恩蔡华轮刘新郭莹陈鸣才
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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