Oxazine resin composition, method for producing same, prepreg, laminate, and cured product
A technology of resin composition and manufacturing method, applied in the direction of synthetic resin layered products, chemical instruments and methods, layered products, etc., can solve the problems of low elasticity, high curing temperature, long curing time, etc., and achieve flame retardancy Excellent, low thermal expansion effect
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[0174] Although an Example and a comparative example are given and this invention is demonstrated concretely, this invention is not limited to these examples unless the summary is exceeded. Unless otherwise specified, "part" means a mass part, and "%" means a mass %.
[0175] The analysis method or measurement method is shown below. In addition, the units of equivalent are all "g / eq."
[0176] Epoxy equivalent: measured according to Japanese Industrial Standard (JIS) K7236 standard.
[0177] Softening point: Measured in accordance with JIS K7234 and the ring and ball method. Specifically, an automatic softening point device (manufactured by Meitech Co., Ltd., ASP-MG4) was used.
[0178] Oxazine ring equivalent: The number of moles (equivalent) Z of the oxazine rings of the oxazine resin (A) is calculated from the value of the total amine value (Y) by the following formula. In addition, the measuring method of the total amine value is based on JISK7237 standard, but using c...
Synthetic example 1
[0187] Synthesis Example 1 (Synthesis of Phenol Novolak Resin)
[0188] 2500 parts of phenol and 7.5 parts of oxalic acid dihydrate were added to a separable glass flask equipped with a stirring device, a thermometer, a nitrogen gas introduction device, a condenser, and a dropping device, and stirred while injecting nitrogen gas, and heated to raise the temperature. Then, stirring at 80 degreeC, 474.1 parts of 37.4% formalin was dripped and made to react over 30 minutes. Furthermore, the reaction was carried out for 3 hours while maintaining the reaction temperature at 92°C. The temperature was raised to 110° C. while removing the reaction product water from the system. Residual phenol was recovered at 160°C under reduced pressure, and the temperature was raised to 250°C to recover a part of the k=0 body to obtain a phenol novolak resin (e-1). Regarding the obtained phenol novolac resin (e-1), hydroxyl equivalent: 105, k=0 body content: 10% (area %), k=1 body content: 46%, k...
Synthetic example 2
[0189] Synthesis example 2 (synthesis of phenol novolac)
[0190] Except having changed the recovery temperature of 250 degreeC into 240 degreeC, it carried out similarly to the synthesis example 1, and obtained the phenol novolac resin (e-2). About the obtained phenol novolak resin (e-2), hydroxyl equivalent: 105, k=0 body content rate: 19%, k=1 body content rate: 42%, k=2 body content rate: 20%, k= 3-body content rate: 10%, k=4-body or more content rate: 9%, Mn: 510, Mw: 567.
[0191] Abbreviations used in Examples and Comparative Examples are described below.
[0192] [Novolac phenol compound]
[0193] (e-1): Phenol novolac resin of Synthesis Example 1
[0194] (e-2): Phenol novolac resin of Synthesis Example 2
[0195] BRG-555: Phenol novolac resin (manufactured by Showa Denko Co., Ltd., Shonol BRG-555, hydroxyl equivalent: 105, k=0 body content: 25 area%, k=1 body content: 18 area %, k=2 body content rate: 14 area%, k=3 body content rate: 10 area%, k=4 body content rat...
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