Long-chain polyether type silane coupler of glycidol-ether-radical end-capping
A glycidyl ether-based, silane coupling agent technology, applied in the direction of silicon organic compounds, can solve problems such as agglomeration and short molecular chains of coupling agents, and achieve the effect of promoting dispersion
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[0020] Example 1
[0021] With thermometer, condenser, stirrer, N 2 Add 40g (molecular weight 436) of allyl polyether (n=2, m=5) to a 250mL dry four-necked flask with an inlet, vacuum degas at 120℃ for 30min, wait until the temperature drops to 70℃, add 0.24g four-necked flask Tin chloride (catalyst amount 6‰), use a micro-injector to add 13g of epichlorohydrin dropwise, the dropping time is controlled within 1 to 2 hours, the temperature does not rise significantly, and the reaction is continued for 1.5 hours after the dropping is completed, and the pressure is reduced. The unreacted epichlorohydrin was removed to obtain 49.2 g of the product chlorohydrin ether intermediate with a conversion rate of 94.35%.
[0022] Dissolve the obtained 49.2g of chlorohydrin ether intermediate in 40mL of toluene, add it to a 250mL dry four-necked flask with a thermometer, condenser, stirrer, and constant pressure funnel. Dissolve 4.8g of NaOH in deionized water to make 30% The aqueous solution i...
Example Embodiment
[0024] Example 2
[0025] With thermometer, condenser, stirrer, N 2 Add 100g of allyl polyether (n=8, m=10) (molecular weight 990) to a 250mL dry four-necked flask with an inlet, vacuum degas at 120℃ for 30min, wait until the temperature drops to 60℃, add 0.40g three Boron fluoride ethyl ether (catalyst amount 4‰), use a micro-injector to add 10g epichlorohydrin dropwise, the dropping time is controlled within 1 to 2 hours, the temperature does not rise significantly, and the reaction is continued for 2 hours after the dropping is completed. The unreacted epichlorohydrin was removed by pressure to obtain 108.8 g of the product chlorohydrin ether intermediate with a conversion rate of 90.25%.
[0026] Dissolve the obtained 108.8g chlorohydrin ether intermediate in 80mL toluene, add it to a 500mL dry four-necked flask with thermometer, condenser, stirrer, and constant pressure funnel. Dissolve 6.8g KOH in deionized water to make 40% The aqueous solution is added dropwise using a mic...
Example Embodiment
[0028] Example 3
[0029] With thermometer, condenser, stirrer, N 2 Add 80g (molecular weight 436) of allyl polyether (n=2, m=5) to a 250mL dry four-necked flask with an inlet, vacuum degas at 120°C for 30min, wait until the temperature drops to 50°C, add 0.72g of two Tin chloride (catalyst amount 9‰), use a micro-injector to add 24g of epichlorohydrin dropwise, the dropping time is controlled within 2 to 3 hours, the temperature does not rise significantly, and the reaction is continued for 3 hours after the dropping is completed, and the pressure is reduced. The unreacted epichlorohydrin was removed to obtain 97.8 g of the product chlorohydrin ether intermediate with a conversion rate of 91.28%.
[0030] Dissolve the obtained 97.8g chlorohydrin ether intermediate in 80mL benzene, add it to a 500mL dry four-necked flask with a thermometer, condenser, stirrer, and constant pressure funnel. Add 9.6g of NaOH to the flask in five portions with intervals 20-30min. Stir and control the...
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