Fluorine-containing low-dielectric cyanate ester modified resin and method for preparing same
An electrocyanate and modified resin technology, applied in the field of fluorine-containing low-dielectric cyanate-modified resin, and the preparation of fluorine-containing low-dielectric cyanate-modified resin, can solve the gap between high-performance radomes, etc. problem, to achieve the effect of improving the dielectric properties and mechanical properties
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[0015] The present invention also provides a method for preparing the above-mentioned fluorine-containing low dielectric cyanate ester modified resin, comprising the following steps:
[0016] (a) m-trifluoromethylphenol (mTFMP) and potassium carbonate (K 2 CO 3 ) into a three-neck flask equipped with a condenser and a stirrer, and react at 110-120° C. for 30 minutes under reflux of excess acetone. Then add excess epichlorohydrin (mass ratio, ECH:mTFMP=46.3-64.8:16.2) and continue to react at 110-120° C. for 4-5 hours. After the reaction, extract 10 times with water / dichloromethane (mass ratio, water:dichloromethane:mTFMP=500:150:16.2), then concentrate by rotary evaporation and perform chromatography on a silica gel column to obtain 2-((3 -(trifluoromethyl)phenoxy)methyl)oxirane (mTFMPMO), put it in a vacuum oven at 60°C for 12h;
[0017] (b) Get 80-95% by weight of bisphenol A type cyanate (BADCy) resin and place it in a beaker at 150° C. for 30 minutes with magnetic stirr...
Embodiment 1
[0019] Implementation example 1, the mTFMP of 16.2g and the K of 16.6g 2 CO 3 Add it into a three-necked flask equipped with a condenser and a stirrer, and react at 110° C. for 30 minutes under reflux of excess acetone. Then add 46.3g of ECH to continue the reaction for 5h. After the reaction, extract 10 times with water / dichloromethane (mass ratio, water:dichloromethane:mTFMP=500:150:16.2), then concentrate by rotary evaporation and perform chromatography on a silica gel column to obtain mTFMPMO, put into 60 ℃ vacuum oven for 12h, set aside. Put 76g of BADCy resin into a beaker, stir magnetically at 150°C for 30min to a clear liquid, then add 4g of mTFMPMO to the beaker, continue stirring for 30min to a light yellow transparent liquid, add 0.08g of dibutyltin dilaurate and stir for 2min to make Mix evenly; place in a vacuum drying oven at 150°C for defoaming treatment for 20 minutes, then pour into a preheated mold at 150°C, solidify according to the heating program of 180...
Embodiment 2
[0021] Implementation example 2, the mTFMP of 16.2g and the K of 16.6g 2 CO 3 Add it into a three-necked flask equipped with a condenser and a stirrer, and react at 120° C. for 30 minutes under reflux of excess acetone. Then add 55.6g of ECH to continue the reaction for 4h. After the reaction, extract 10 times with water / dichloromethane (mass ratio, water:dichloromethane:mTFMP=500:150:16.2), then concentrate by rotary evaporation and perform chromatography on a silica gel column to obtain mTFMPMO, put into 60 ℃ vacuum oven for 12h, set aside. Put 76g of BADCy resin into a beaker, stir magnetically at 150°C for 30min to a clear liquid, then add 4g of mTFMPMO to the beaker, continue stirring for 30min to a light yellow transparent liquid, add 0.08g of dibutyltin dilaurate and stir for 2min to make Mix evenly; place in a vacuum drying oven at 150°C for defoaming treatment for 20 minutes, then pour into a preheated mold at 150°C, solidify according to the heating program of 180...
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