疏水性介孔TiO2/碳质复合材料的制备及其高效催化合成生物润滑油的研究

王婧莹, 毛辉麾, 陈斐轲, 华玉婷, 张青, 左士祥

现代化工 ›› 2023, Vol. 43 ›› Issue (6) : 122 -128.

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现代化工 ›› 2023, Vol. 43 ›› Issue (6) : 122-128. DOI: 10.16606/j.cnki.issn0253-4320.2023.06.023
科研与开发

疏水性介孔TiO2/碳质复合材料的制备及其高效催化合成生物润滑油的研究

    王婧莹, 毛辉麾, 陈斐轲, 华玉婷, 张青, 左士祥
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Preparation of hydrophobic mesoporous TiO2/carbonaceous composite and application in catalyzing synthesis of bio-lubricant oil

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摘要

以糠醛和羟乙基磺酸为碳源,通过水热法将含有磺酸基团的碳质与介孔二氧化钛复合制备TiO2/C-SO3H固体酸催化剂;利用3-氨基丙基三乙氧基硅烷对其进行表面改性,得到具有疏水性的TiO2/C-SO3H-NH2。利用SEM、TEM、BET、XRD、FT-IR等对TiO2/C-SO3H-NH2进行表征,结果表明,TiO2/C-SO3H-NH2保持了TiO2的介孔结构和富含磺酸基的碳质结构,3-氨基丙基三乙氧基硅烷的改性带来疏水性和弱碱性。氨基与表面磺酸基形成稳定的内盐结构,有效防止了磺酸基在反应过程中的流失,同时降低了酯化产品的酸值,增加了稳定性。通过正戊酸与三羟甲基丙烷酯化反应测试TiO2/C-SO3H-NH2的催化活性,当反应温度为180℃时,三羟甲基丙烷的转化率达到99.99%,三羟甲基丙烷三戊酸酯的选择性为93.56%。TiO2/C-SO3H-NH2具有良好的重复使用性能。

Abstract

Using furfural and hydroxyethyl sulfonic acid as carbon sources, TiO2/C-SO3H solid acid catalyst are prepared through hydrothermal synthesis method by compositing mesoporous titanium dioxide and carbon-containing sulfonic acid groups.Then, the surface of TiO2/C-SO3H solid acid catalyst is modified by 3-aminopropyltriethoxysilane to obtain hydrophobic TiO2/C-SO3H-NH2t, which is characterized by means of SEM, TEM, BET, XRD, and FT-IR.Results show that TiO2/C-SO3H-NH2 retains the mesoporous structure of TiO2 and the carbonaceous structure rich in sulfonic acid groups.The modification by 3-aminopropyltriethoxysilane results in hydrophobicity and weak alkalinity.A stable internal salt structure is formed between amino groups and surface sulfonic groups, effectively preventing sulfonic groups from losing during the reaction process, while reducing the acid value of the esterification product and increasing the stability.The catalytic activity of TiO2/C-SO3H-NH2 is tested through esterification between n-valeric acid and trimethylolpropane.The conversion of trimethylolpropane reaches 99.99% and the selectivity of trimethylolpropane tri-valerate reaches 93.56% over TiO2/C-SO3H-NH2 when the reaction temperature is 180℃.It is also found that TiO2/C-SO3H-NH2 has an excellent reusability.

关键词

介孔二氧化钛 / 酯化 / 生物润滑油 / 碳质

Key words

mesoporous titanium dioxide / esterification / bio-lubricant oil / carbonaceous

Author summay

王婧莹(1998-),女,硕士研究生,研究方向为纳米功能材料,2638649681@qq.com。

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疏水性介孔TiO2/碳质复合材料的制备及其高效催化合成生物润滑油的研究[J]. 现代化工, 2023, 43(6): 122-128 DOI:10.16606/j.cnki.issn0253-4320.2023.06.023

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