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    以二甲基-正丁基-磺化木质素基氯化铵为模板剂制备多孔钛材料

    Preparation for porous titanium material with dimethylbutylsulfonated lignin ammonium as a template

    • 摘要: 以碱木质素为原料合成二甲基-正丁基-磺化木质素基氯化铵两性表面活性剂,并以其为模板剂采用溶胶-凝胶法制备多孔钛材料。结果表明:二甲基-正丁基-磺化木质素基氯化铵含氮量为1.360%,含硫量1.860%;红外光谱和1H NMR证实产物中存在磺化和季胺的化学结构。溴酚蓝和亚甲基蓝实验表明二甲基-正丁基-磺化木质素基氯化铵具有两性化合物结构,溶于碱性、中性和稀酸溶液。随着模板剂与钛酸正丁酯的质量比增加,多孔钛材料的比表面积加大;继续增加模板剂的量,多孔钛材料的比表面积下降。多孔钛材料孔径分布范围较宽,为晶态,主要以锐钛矿形式存在。煅烧后的多孔材钛料中有TiO2特征吸收峰,也有少量残留的木质素。当二甲基-正丁基-磺化木质素基氯化铵与钛酸正丁酯的质量比为0.65∶1、煅烧温度为450 ℃时,可得到最大比表面积、锐钛矿晶态的多孔钛材料。

       

      Abstract: Dimethyl-butyl-sulfonated lignin ammonium chloride amphoterics was composed with alkali lignin as raw material. Then porous titanium material was prepared by sol-gel method with it as template. Analysis results were that nitrogen content of porous titanium material was 1.360%, sulphur content was 1.860%. Sulphonated structure and quaternary amine were identified in the product by FT-IR and 1H NMR. Bromophenol blue and methylene blue experiments showed that products had amphoteric compound and dissolved in alkaline, neutral and dilute acid solution. With the increasing mass ratio of template to Ti(OiPr)_4, specific surface area of porous titanium material increased. Continue to increase the amount of template and the specific surface area was down. N2 nadsorption-desorption isotherm and pore size distribution analysis showed that pore size distribution of this product was wider. XRD analysis showed that there was a peak at 2θ=25.1, showing that porous titanium material was crystal and it mainly existed in the form of anatase. Calcined porous material had TiO2 characteristic absorption peaks, but there were still a few traces of lignin in it. Therefore an eventual compromise was got, when the mass ratio between dimethyl-nbutyl-sulfonated lignin and Ti(OiPr)_4 was 0.65∶1 and calcining temperature was 450 ℃, porous titanium material of largest specific surface was made in the form of anatase.

       

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