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Phosphorus-containing epoxy resin, composition containing phosphorus-containing epoxy resin as essential component, and cured product

A technology of epoxy resin and composition, applied in the direction of synthetic resin layered products, layered products, chemical instruments and methods, etc. Toxic halide and other problems, to achieve the effect of good flame retardancy, good permeability and low viscosity

Active Publication Date: 2015-02-25
NIPPON STEEL CHEMICALL &MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when a halogenated epoxy resin is used, there is a problem that it is found that a highly toxic halide is produced due to a thermal decomposition reaction when the cured product is burned.
[0004] The phosphorus-containing epoxy resin obtained by the flame-retardant method of phosphorus compounds is difficult to achieve both high heat resistance and high adhesion. If multifunctionalization is performed in order to improve heat resistance, the adhesion will decrease; The heat resistance is lowered by the bifunctionalization of the phosphorus compound due to the adhesive force

Method used

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  • Phosphorus-containing epoxy resin, composition containing phosphorus-containing epoxy resin as essential component, and cured product
  • Phosphorus-containing epoxy resin, composition containing phosphorus-containing epoxy resin as essential component, and cured product

Examples

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Embodiment

[0066] Although an Example and a comparative example are given and this invention is concretely demonstrated, this invention is not limited to these. Unless otherwise specified, "part" means a mass part, and "%" means a mass %. Measuring method The measurement was performed by the following methods, respectively.

[0067] The measurement method is as follows.

[0068] Epoxy equivalent: According to JIS K7236.

[0069] Dinuclear body content rate, trinuclear body content rate, tetranuclear body content rate, pentanuclear body content rate, number average molecular weight (Mn), weight average molecular weight (Mw), and dispersion (Mw / Mn): Gel permeation chromatography was used to measure the molecular weight distribution. The dinuclear body content rate, trinuclear body content rate, tetranuclear body content rate, and pentanuclear body content rate were calculated from the peak area %, and the number average molecular weight, weight average molecular weight, and dispersion w...

Synthetic example 1

[0078] Synthesis Example 1 (Synthesis of Novolak Resin)

[0079] 2500 parts of phenol and 7.5 parts of oxalic acid dihydrate were charged into a 4-necked glass separable flask equipped with a stirring device, a thermometer, a condenser, and a nitrogen gas introduction device, stirred while introducing nitrogen gas, and heated to raise the temperature. Dropwise addition of 474.1 parts of 37.4% formalin was started at 80°C, and it took 30 minutes to complete the dropwise addition. Furthermore, the reaction temperature was kept at 92° C., and the reaction was performed for 3 hours. The temperature was raised, and the temperature was raised to 110° C. while removing the reaction-generated water to the outside of the system. The residual phenol was recovered at 160° C. under reduced pressure to obtain a novolak resin. Further, the temperature is raised to recover a part of dinuclear bodies. The dinuclear body content and trinuclear body content of the obtained novolac resin were...

Synthetic example 2

[0080] Synthesis example 2 (synthesis of novolac type epoxy resin)

[0081]Into the same apparatus as in Synthesis Example 1, 665.8 parts of novolac resin, 2110.8 parts of epichlorohydrin, and 17 parts of water of Synthesis Example 1 were added, and the temperature was raised to 50°C while stirring. 14.2 parts of 49% sodium hydroxide aqueous solution was added, and reaction was performed for 3 hours. The temperature was raised to 64° C., the pressure was reduced to such an extent that water reflux occurred, and 457.7 parts of a 49% sodium hydroxide aqueous solution was added dropwise over 3 hours to perform a reaction. The temperature was raised to 70° C. for dehydration, and the temperature was set to 135° C. to recover residual epichlorohydrin. Return to normal pressure, add 1232 parts of MIBK, and dissolve. 1200 parts of ion-exchanged water was added, stirred and left to stand, and the by-product common salt was dissolved in water and removed. Next, 37.4 parts of 49% aqu...

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Abstract

The present invention provides an epoxy resin that has further improved heat resistance, while maintaining conventional adhesion, specifically a phosphorus-containing epoxy resin (A) which is obtained by reacting, as essential components, a phosphorus compound represented by general formula (1), a quinone compound and an epoxy resin (a), and which is characterized in that the epoxy resin (a) is a novolac epoxy resin that has a molecular weight distribution having a dinuclear component content of 15% by area or less, a trinuclear component content of 15-60% by area, and a number average molecular weight of 350-700 as determined by gel permeation chromatography.

Description

technical field [0001] The present invention relates to a halogen-free flame-retardant epoxy resin containing phosphorus atoms in the molecular skeleton, and an epoxy resin composition using the epoxy resin as an essential component, and further relates to curing the epoxy resin composition to produce The formed epoxy resin cured product; the present invention provides an epoxy resin suitable for the following applications: prepregs used in circuit boards, film materials used in copper-clad laminates or electronic components, sealing materials, molding materials, casting Materials, adhesives, electrical insulating coatings, composite materials requiring flame retardancy, powder coatings, etc. Background technique [0002] Flame retardation of epoxy resins has conventionally been performed by halogenation, and brominated epoxy resins using tetrabromobisphenol A as a raw material are representative. However, when a halogenated epoxy resin is used, there is a problem that it ...

Claims

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Application Information

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IPC IPC(8): C08G59/14B32B27/38C08J5/24H05K1/03
CPCC08L63/04H05K2201/012H05K1/0366C08G59/3272C08G59/1488B32B27/38C08J5/24H05K1/0326C08J2363/04B32B15/14B32B15/20B32B2260/023B32B2260/046B32B2305/076C08J5/244
Inventor 三宅力石原一男村井秀征
Owner NIPPON STEEL CHEMICALL &MATERIAL CO LTD
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