Epoxy group-containing organosilicon compound and preparation method thereof, and epoxy resin composition and preparation method thereof
A technology of organosilicon compound and epoxy group, which is applied in the field of polyetheramine and organosilicon synergistically toughened fast-curing epoxy resin composition and its preparation, which can solve the problems of high curing temperature, singleness, and limited toughness improvement effect , to achieve the effect of good flexibility
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[0074] Preparation of cured product test samples: first raise the temperature of the polytetrafluoroethylene mold to 40°C and keep it warm for 10-20 minutes. According to the above curing process, mix A and B components, defoam, pour into the mold to level off naturally, and cure at 40°C for 5 hours. Wait for the mold to cool down naturally, and demould.
[0075] Process the above cured sample into 50×10×4mm 3 According to the national standard GB / T 2567 "Resin Casting Body Performance Test Method", the elongation at break was tested with a universal material testing machine (Germany, Zwick / Roell Z020).
[0076] 3. Gel content test of cured epoxy resin
[0077] The gel content of cured epoxy resin was determined by extraction method. Take 0.25g cured product test sample, cut into several 1.5×1.5×1mm 3 small piece, weighed as m 1 , with xylene as the extractant, extracted in a Soxhlet extractor for 24 hours, rinsed with xylene three times after the sample was taken out, th...
Embodiment 1
[0111] To prepare 1,1,3,3-tetramethyl-1-vinyl-3-epoxydisiloxane, the steps are:
[0112] 1) m-chloroperoxybenzoic acid was dissolved in dichloromethane to prepare solution A of 0.696mol / L;
[0113] 2) Dissolving tetramethyldivinyldisiloxane in dichloromethane to prepare 0.4mol / L solution B;
[0114] 3) Add solution A dropwise to solution B (the molar ratio of m-chloroperoxybenzoic acid to tetramethyldivinyldisiloxane is 2.5:1) under the condition of 0-4°C ice bath, dropwise The time was 1 hour. After the addition was completed, the temperature was raised to 50° C., and the reaction was refluxed for 47 hours; the progress of the reaction was monitored by thin-layer chromatography (using a mixed solvent with a mass ratio of hexane and ethyl acetate of 5:3). After the reaction finished, the crude product obtained was subjected to two times of pickling (using 5wt% 2,3-dihydroxysuccinic acid aqueous solution) and three times of alkali washing (using 5% NaHCO 3 aqueous solution), ...
Embodiment 2
[0117] To prepare 1,1,3,3-tetramethyl-1-vinyl-3-epoxydisiloxane, the steps are:
[0118] 1) Dissolving m-chloroperoxybenzoic acid in methylene chloride is prepared as solution A of 0.6mol / L;
[0119] 2) Dissolving tetramethyldivinyldisiloxane in dichloromethane to prepare 0.3mol / L solution B;
[0120] 3) Add solution A dropwise to solution B (the molar ratio of m-chloroperoxybenzoic acid to tetramethyldivinyldisiloxane is 2:1) under the condition of 0-4°C ice bath, dropwise The time was 1 hour. After the addition was completed, the temperature was raised to 55° C., and the reaction was refluxed for 46 hours; the progress of the reaction was monitored by thin-layer chromatography (using a mixed solvent with a mass ratio of hexane and ethyl acetate of 5:3). After the reaction finished, the crude product obtained was subjected to two times of pickling (using 5wt% 2,3-dihydroxysuccinic acid aqueous solution) and three times of alkali washing (using 5% NaHCO 3 aqueous solution), ...
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