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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

Inactive Publication Date: 2007-11-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the short molecular chains of the above-mentioned coupling agents, the SiO 2 When the subsurface is effectively wrapped, it is often necessary to cover more coupling agent molecules
Modified SiO 2 The particles can be well dispersed in the organic solvent system, but there is still some agglomeration in the organic resin or polymer matrix

Method used

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  • Long-chain polyether type silane coupler of glycidol-ether-radical end-capping

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] With thermometer, condenser, stirrer, N 2 Add 40g of allyl polyether (n=2, m=5) (molecular weight: 436) into a 250mL dry four-neck flask with an inlet, and vacuum degas at 120°C for 30min. After the temperature drops to 70°C, add 0.24g Tin chloride (catalyst dosage 6‰), use a micro-injector to drop 13g of epichlorohydrin, the dropping time is controlled within 1 to 2 hours, and the temperature is controlled not to rise significantly. After the dropping, continue to react for 1.5 hours, reduce 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 chlorohydrin ether intermediate in 40mL toluene, add it into a 250mL dry four-necked flask equipped with a thermometer, condenser, stirrer, and constant pressure funnel, and dissolve 4.8g NaOH in deionized water to form a 30% The aqueous solution was added dropwise using a micro-injector, and the dropping ...

Embodiment 2

[0025] With thermometer, condenser, stirrer, N 2 Into a 250mL dry four-necked flask with an inlet, add 100g of allyl polyether (n=8, m=10) (molecular weight: 990), degass under vacuum at 120°C for 30min, and when the temperature drops to 60°C, add 0.40g of Boron fluoride diethyl ether (catalyst dosage 4‰), using a micro-sampler to drop 10g of epichlorohydrin, the dropping time is controlled within 1 to 2 hours, the control temperature does not rise significantly, and the reaction is continued for 2 hours after the dropping is completed. The unreacted epichlorohydrin was removed under 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 into a 500mL dry four-necked flask equipped with a thermometer, condenser, stirrer, and constant pressure funnel, dissolve 6.8g KOH in deionized water, and make 40% The aqueous solution was added d...

Embodiment 3

[0029] With thermometer, condenser, stirrer, N 2 Into a 250mL dry four-neck flask with an inlet, add 80g of allyl polyether (n=2, m=5) (molecular weight: 436), degass under vacuum at 120°C for 30min, and when the temperature drops to 50°C, add 0.72g of di Tin chloride (catalyst dosage 9‰), use a micro-sampler to drop 24g of epichlorohydrin, the dropping time is controlled within 2 to 3 hours, and the temperature is controlled not to rise significantly. After the dropping, continue to react for 3 hours, reduce the pressure 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 into a 500mL dry four-necked flask equipped with a thermometer, a condenser, a stirrer, and a constant pressure funnel, and add 9.6g NaOH to the flask five times, each interval 20-30min. Stir and control the temperature at 50°C...

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Abstract

The present invention discloses a glycidyl ether blocking long-chain polyether silane coupling agent, with the following general formula: (CH3)aSiX3-aCH2CH2CH2O(CH2CH2O)n(CH2CH(CH3)O)mCH2CH(O)CH2, in which n, m is 1-50 integer, X is Cl, -OCH3 or -OCH2CH3, and a is 0, 1, 2 or 3. The present invention provides the long-chain polyether silane coupling agent with glycidyl ether blocking. The glycidyl ether on its terminal which can react with the matrixes such as epoxy resin, polyurethane, etc., promotes the compatibility of nano-SiO2 with organic matrixes, and its polyether chain which can activate the encapsulation and surface of nano-SiO2, promotes the dispersion of nano-SiO2 in organic matrixes. Therefore, it largely increases the dispersion and stability of the nano-SiO2 in organic solvent, especially in organic polymer matrixes, such as epoxy resin and polyurethane.

Description

technical field [0001] The present invention relates to a method for synthesizing organosilicon compounds, in particular to a method for synthesizing a long-chain polyether-type silane coupling agent with a glycidyl ether group capping, which belongs to the intermediate of organosilicon functional compounds Synthesis and applied research fields. Background technique [0002] Silane coupling agent is a kind of silane compound with both inorganic and organophilic functional groups in the molecule. It is widely used in many industrial fields such as glass fiber, plastic, cable, rubber, organic resin and coating. There are many different brands and different types of silane coupling agents on the market. However, in order to make silane coupling agents better used in different products and different application environments, the research on synthesizing silane coupling agents with new molecular structures is also continuing to achieve the purpose of fully improving the performa...

Claims

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Application Information

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IPC IPC(8): C08G65/336C07F7/02
Inventor 范宏李伯耿冯金辉左春苗卜志扬刘万章
Owner ZHEJIANG UNIV
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