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分别采用含水体系和无水体系将γ-氨丙基三乙氧基硅烷(APTES)接枝到凹凸棒石(ATP)表面,制得改性粒子ATP-APTES。用Fourier红外光谱、Raman光谱、热重分析及透射电子显微镜对粒子进行了表征,结果表明:红外光谱的3 350 cm–1和Raman光谱的3321cm–1等处出现了伯氨基吸收峰,证实了APTES已成功接枝到ATP表面。用滴定法测定了改性粒子表面的APTES接枝率,研究了配方及工艺条件对APTES接枝率的影响。结果表明:在含水体系中,APTES用量大于5%、反应时间超过6 h均会造成接枝率的减小;无水体系制备的改性粒子接枝率明显高于含水体系,且接枝效率也较高;在乙二醇体系中,反应时间为6h时,改性粒子的接枝率高达725.8mmol/kg。
Γ-Aminopropyltriethoxysilane (APTES) was grafted to the surface of attapulgite (ATP) by aqueous system and anhydrous system, respectively, to obtain modified particle ATP-APTES. Fourier transform infrared spectroscopy, Raman spectroscopy, thermogravimetric analysis and transmission electron microscopy were used to characterize the particles. The results showed that the primary amino groups appeared at 3 350 cm-1 and 3321 cm-1 in the Raman spectrum. APTES has successfully grafted to the ATP surface. The grafting ratio of APTES on the surface of the modified particles was measured by titration. The effects of formulation and process conditions on the grafting yield of APTES were studied. The results showed that in the aqueous system, the APTES content of more than 5%, the reaction time of more than 6 h will result in a decrease in grafting rate; water-free system prepared modified particles grafted significantly higher than the aqueous system, and the graft efficiency In the ethylene glycol system, the grafting rate of the modified particles was as high as 725.8 mmol / kg when the reaction time was 6 h.