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Process for producing phosphorus-containing epoxy resin

A technology of epoxy resin and manufacturing method, applied in the field of cured product and epoxy resin composition, can solve the problems of poor impregnation of operable glass cloth, easy increase of viscosity, decrease of crosslinking density of cured product, etc., and achieves impregnation operation. Good properties, less crystal precipitation, and low molecular weight

Active Publication Date: 2019-03-01
NIPPON STEEL CHEM &MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the phosphorus-containing epoxy resin obtained by reacting such a phosphorus compound with an epoxy resin has an increased molecular weight as the phosphorus content increases, so the varnish of an epoxy resin with sufficient flame retardancy has a high viscosity, which is difficult to handle. The problem of poor impregnation with substrates such as glass cloth
In addition, because the molecular weight of phosphorus-containing epoxy resin increases, the crosslinking density of the cured product decreases, so it is difficult to obtain a high glass transition temperature.
[0004] In addition, Patent Document 4 discloses a method of increasing the phosphorus content by dissolving a phosphorus compound in a phosphorus-containing epoxy resin composition because sufficient flame retardancy cannot be obtained only by a phosphorus-containing epoxy resin, but the solvent must be Using high boiling point solvents such as N,N-dimethylformamide, there is a problem that phosphorus compounds are easy to precipitate
Patent Document 5 discloses a method of dispersing HCA-HQ in a resin varnish by finely pulverizing HCA-HQ to a size with an average particle diameter of 10 μm and a maximum particle diameter of 40 μm. Viscosity tends to increase more easily than varnish, and if the viscosity of varnish is lowered, there is a problem that sufficient flame retardancy cannot be obtained

Method used

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  • Process for producing phosphorus-containing epoxy resin
  • Process for producing phosphorus-containing epoxy resin
  • Process for producing phosphorus-containing epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Add 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide ( Sanko Co., Ltd. (trade name HCA, phosphorus content 14.2% by weight) 99 parts, 1,4-naphthoquinone (Kawasaki Chemical Industry Co., Ltd.) 71 parts, toluene 361 parts, stirred at 75°C for 30 minutes, and removed the system The water inside was reacted at 110°C for 90 minutes, and then the toluene was removed to obtain 10-(1,4-dihydroxynaphthalene)-10H-9-oxa-10-phosphaphenanthrene-10-oxide (HCA-NQ ). Add 531 parts of phenol novolac type epoxy resin (Nippon Steel Chemical Co., Ltd. product name YDPN-638, epoxy equivalent: 176g / eq.) and tris(2,6-dimethoxybenzene) as a catalyst Base) 0.01 part of phosphine (hereinafter referred to as DMPP), reacted at 165°C for 3 hours, then added 78 parts of propylene glycol monomethyl ether (hereinafter referred to as PGM), and reacted for 2 hours below the reflux temperature. Then, it was diluted with 43 parts of PGM and 179 parts of methyl ethyl ketone (hereinafter referred to as ...

Embodiment 2

[0079] Except that HCA is specified as 123 parts, 1,4-naphthoquinone is specified as 88 parts, YDPN-638 is specified as 488 parts, the catalyst is specified as 0.02 parts of DMPP, and the reaction is specified as 3.5 hours at 165°C, adding The same operation as in Example 1 was performed except that the reaction time after PGM was set to 3 hours. The resulting phosphorus-containing epoxy resin solution is dark brown and transparent, with a non-volatile content of 70%, a varnish viscosity of 3700mPa·s, an actual epoxy equivalent of 359g / eq., and a phenolic hydroxyl equivalent of 2100g / eq. The phosphorus content was 2.5%, and no turbidity was observed in the solvent solubility test. The weight average molecular weight was 6986, the number average molecular weight was 1017, and the dispersibility was 6.87. In addition, the functional group equivalent of the compound (b) having a reactive functional group relative to 1 equivalent of the epoxy group of the epoxy resin (a) is 0.40 ...

Embodiment 3

[0081] 99 parts of HCA and 71 parts of 1,4-naphthoquinone were charged, and it was made to react by the method similar to Example 1, and HCA-NQ was obtained. To this, 531 parts of triphenylmethane-type epoxy resin (trade name EPPN-501H manufactured by Nippon Kayaku Co., Ltd., epoxy equivalent 165.2 g / eq.), 37 parts of PGM, and 0.01 part of DMPP as a catalyst were added at 165° C. After reacting at lower temperature for 3 hours, add 41 parts of PGM, and react for 3 hours below the reflux temperature. Then, it was diluted with 43 parts of PGM and 179 parts of MEK, and cooled to normal temperature to complete the reaction. The resulting phosphorus-containing epoxy resin solution is dark brown and transparent, with a non-volatile content of 70%, a varnish viscosity of 1800mPa·s, an actual measured epoxy equivalent of 268g / eq., and a phenolic hydroxyl equivalent of 2200g / eq. The phosphorus content was 2.0%, and no turbidity was observed in the solvent solubility test. The weight ...

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Abstract

The invention provides a method for producing a stable phosphorus-containing epoxy resin capable of co-existing epoxy groups and phenolic hydroxyl groups, having lower viscosity and no crystal precipitation, the phosphorus-containing epoxy resin and its composition and cured product. The method for producing the phosphorus-containing epoxy resin uses a phosphine-based catalyst represented by the general formula (1) to react epoxy resins (a) with compounds (b) having reactive functional groups that react with epoxy groups, which It is characterized in that the compound (b) having a reactive functional group has a phosphorus-containing phenol compound represented by the general formula (2) as an essential component, and the epoxy equivalent of the obtained phosphorus-containing epoxy resin is obtained by mathematical formula 1 The range of 90% to 60% of the theoretical epoxy equivalent.

Description

technical field [0001] The present invention relates to a method for producing a phosphorus-containing epoxy resin having flame retardancy, low viscosity, and high heat resistance, a phosphorus-containing epoxy resin obtained by the production method, and an epoxy resin containing the epoxy resin as an essential component. Resin composition, cured product. Background technique [0002] Epoxy resins are widely used in laminates for electrical and electronic equipment, sealants, automotive parts, FRP, and sporting goods due to their excellent adhesiveness, heat resistance, and moldability. In particular, when used in laminated boards of electric and electronic equipment, it is strongly required to impart flame retardancy in order to prevent combustion and control smoke generation in the event of a fire. As methods for flame retarding resins for laminates, bromine-based flame retardants, nitrogen-based flame retardants, and phosphorus-based flame The flame retardant system of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/62C08G59/68C08L63/00
CPCC08G59/304C08G59/688C08K5/51C08L63/00C08L2201/02
Inventor 内田美幸佐藤洋石原一男森田阳子
Owner NIPPON STEEL CHEM &MATERIAL CO LTD
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