现代化工

现代化工 ›› 2026, Vol. 46 ›› Issue (2) : 160-165. DOI: 10.16606/j.cnki.issn0253-4320.2026.02.026

科研与开发

介孔TiO₂-MoO₃复合催化剂的一锅法合成及其对噻吩类化合物的高效脱除

作者信息 +

One-pot synthesis of mesoporous TiO₂-MoO₃ composite catalyst and its high-efficiency desulfurization performance for thiophene compounds

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文章历史 +

Received		Published
2025-09-04		2026-02-20
Issue Date	Revised Date
2026-02-11	2025-09-04

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摘要

采用一锅水热法制备了二氧化钛-三氧化钼(TiO₂-MoO₃)复合材料,研究了这种材料在不同反应条件下对二苯并噻吩(DBT)等含硫化合物的脱除效果,探讨了相关反应机理。实验结果表明,在反应温度50℃、催化剂0.05 g和H₂O₂用量 25 μL的条件下,脱硫率可达100%。循环稳定性实验结果显示,在重复使用10次后,该催化剂的脱硫率仍保持在95%以上,展现出良好的催化稳定性。

Abstract

Titanium dioxide-molybdenum trioxide (TiO₂-MoO₃) composite materials were prepared using a one-pot hydrothermal method.The removal effect of this material on sulfur-containing compounds such as dibenzothiophene (DBT) under different reaction conditions was investigated,and the relevant reaction mechanisms were explored.Experimental results showed that at a reaction temperature of 50℃,with 0.05 g of catalyst and 25 μL of H₂O₂,the desulfurization efficiency could reach 100%.The results of the cyclic stability test indicated that after 10 consecutive reaction cycles,the desulfurization efficiency of the catalyst remained above 95%,demonstrating high catalytic stability.

Graphical abstract

关键词

TiO₂-MoO₃ / 噻吩 / 水热法 / 深度脱硫 / 过渡金属氧化物

Key words

TiO₂-MoO₃ / thiophene / hydrothermal method / deep desulfurization / transition metal oxides

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Chemical Engineering, Ningxia Normal University, Guyuan 756000, China), AuthorCompanyExt(id=1241417658869969685, tenantId=1226480274814496768, journalId=1226484258170171394, articleId=1240720284270949102, companyId=1241417658840609555, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=宁夏师范大学化学化工学院,宁夏绿色催化材料与技术重点实验室,宁夏固原 756000)])])] 周生学,欧少源,李瑾蓉,赵英孜. 介孔TiO₂-MoO₃复合催化剂的一锅法合成及其对噻吩类化合物的高效脱除[J]. 现代化工, 2026, 46(2): 160-165 DOI:10.16606/j.cnki.issn0253-4320.2026.02.026

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燃油中含有多种硫、氮化合物,大量燃烧时会产生硫氧化物和氮氧化物等有害气体,对大气环境具有严重危害^[1-3]。近年来,随着环境污染问题日益严峻,燃料油燃烧带来的污染问题逐渐凸显,各国推出更严格的燃料油质量标准,对柴油中的含硫化合物含量严格控制^[4-6],我国《重型柴油车污染物排放限值及测量方法》规定柴油中硫含量不高于10 mg/L^[7]。

传统的加氢脱硫(HDS)^[8-12]通常需要高温高压条件以及昂贵的催化剂,并且难以脱除二苯并噻吩(DBT)等噻吩类含硫化合物。氧化脱硫(ODS)^[13-17]利用氧化剂将燃油内的含硫化合物氧化后,形成易溶于水的化合物,萃取后与燃油分离,达到脱硫的效果,具有反应条件温和、效率高和成本低等优点。过渡金属氧化物(WO₃、MoO₃、TiO₂等)具有较高氧化态,在氧化脱硫反应过程中展现出高效的催化活性^[18-22],并且过渡金属氧化物易于回收,可以通过简单的物理或化学方法从反应体系中分离出来,经过适当的再生处理后,能够保持其原有的催化性能,进而实现资源的高效利用,减少废弃物的产生。

本研究采用一锅水热法合成了二氧化钛-三氧化钼(TiO₂-MoO₃)复合材料,通过扫描电镜(SEM)、X射线衍射仪(XRD)、X射线光电子能谱仪(XPS)和N₂吸附-脱附自动吸附仪等多种仪器表征了其形貌和结构,并以所制备的TiO₂-MoO₃作为催化剂,探究了这类材料在模拟燃油催化氧化脱硫中的性能,并结合傅里叶变换红外光谱(FT-IR)、质谱(MS)等表征手段,分析了催化氧化脱硫的反应机理。

1 材料与方法

1.1 仪器与试剂

正辛烷(分析纯,上海泰坦科技股份有限公司);二苯并噻吩(分析纯,上海阿拉丁生化科技股份有限公司);苯并噻吩(分析纯,上海泰坦科技股份有限公司);4,6-二甲基二苯并噻吩(分析纯,上海泰坦科技股份有限公司);过氧化氢(分析纯,国药集团化学试剂有限公司);四氯化钛(分析纯,国药集团化学试剂有限公司);五氯化钼(分析纯,上海泰坦科技股份有限公司);乙腈(分析纯,上海泰坦科技股份有限公司);甲醇(色谱纯,上海泰坦科技股份有限公司)。

高效液相色谱仪(HPLC,Agilent 1200,安捷伦公司);紫外分光光度计(UV-Vis,Cary 3500,安捷伦公司);X射线衍射仪(D8 Advance,德国Bruker公司);红外光谱仪(NEXUS 870,美国Nicolet公司);XPS能谱仪(K-Alpha,美国Thermo Fisher Scientific公司);扫描电子显微镜(SEM,PhilipsXL 30,荷兰Philips公司);N₂吸附-脱附自动吸附仪(ASAP 2010,美国Micromeritics公司)。

1.2 催化剂制备

向聚四氟乙烯内衬高压反应釜中依次加入 2 mmol MoCl₅、18 mmol TiCl₄、58 mL蒸馏水,放入烘箱中于150℃下加热3 h,取出反应釜自然冷却至室温,离心收集沉淀,用去离子水洗涤,并在烘箱中于60℃下干燥12 h后,得到TiO₂-MoO₃复合材料。

1.3 氧化脱硫反应

使用H₂O₂作为氧化剂,TiO₂-MoO₃作为催化剂进行氧化脱硫。准确称量0.025 mg DBT,溶解到250 mL正辛烷中,配成硫含量为10 μg/g的模型油。取10 mL该模型油加入三角瓶中,再依次加入0.05 g TiO₂-MoO₃、25 μL H₂O₂和10 mL乙腈,于一定温度和搅拌转速下反应后,取少量上层油相,用高效液相色谱仪测定硫含量,并根据式(1)计算脱硫率:

(1)

D s = [(C 0 - C t) / C 0] × 100 %

式中,D_s为脱硫率,%;C₀为模拟燃油初始硫含量,mol/L;C_t为反应t时间后模拟燃油中硫含量,mol/L。

2 结果与讨论

2.1 TiO₂-MoO₃的形貌表征

TiO₂-MoO₃的SEM表征结果如图1(a)、(b)所示,可以看到,所合成的样品呈现疏松的无定形结构。TiO₂-MoO₃的EDS表征结果如图1(c)~(g)所示,其Ti、O、Mo元素在样品中分布均匀。

2.2 TiO₂-MoO₃的结构表征

图2(a)是合成的TiO₂-MoO₃的XRD表征结果,在25.7°和39.6°出现的峰为MoO₃的特征衍射峰,在48.0、53.8、55.0°出现的衍射峰为TiO₂的(200)、(105)、(211)衍射面(PDF#99—0008),反应前后的催化剂谱图无明显差别,说明脱硫反应后催化剂性质未产生明显改变。图2(b)曲线为TiO₂-MoO₃的N₂吸附等温线,曲线中后段上升趋势加快,且末尾处出现吸附平台,呈现第二类吸附等温线的形状和特点,反映出介孔固体单一多层可逆吸附过程,并且吸附质发生毛细管凝聚^[23-24]。

TiO₂-MoO₃的比表面积和孔径参数如表1所示,其中,TiO₂-MoO₃的孔径为5.062 5 nm、孔容为0.318 020 cm³/g、比表面积为251.276 4 m²/g。TiO₂-MoO₃孔分布曲线如图2(c)所示,可以看出,在TiO₂-MoO₃中,孔径大小集中在10 nm左右,具有介孔结构^[25]。

图2(d)为TiO₂-MoO₃的全扫描XPS谱图,具有Ti、Mo、O、C的特征峰。图2(e)为TiO₂-MoO₃中Ti 2p的谱图,Ti 2p_1/2的峰位于464.13 eV,Ti 2p_3/2峰位于458.35 eV,对应TiO₂中的Ti⁴⁺,还可以发现位于471.49 eV处对应的Ti²⁺的卫星峰(Satellite)^[26]。图2(f)为TiO₂-MoO₃的Mo 3d的高分辨率窄光谱,可以看到Mo 3d_3/2的峰位于235.58 eV,Mo 3d_5/2峰位于232.38 eV,对应MoO₃中的Mo⁶⁺,表明TiO₂和MoO₃在TiO₂-MoO₃中以最高氧化态形式存在^[27]。

2.3 TiO₂-MoO₃对噻吩类化合物的脱硫性能分析

2.3.1 使用不同反应体系对脱硫性能的影响

图3(a)为TiO₂-MoO₃用量对脱硫率的影响。在本组实验中,H₂O₂的用量为10 μL。可以看到,TiO₂-MoO₃用量从0.01 g增长至0.06 g时,脱硫率提升27%。在TiO₂-MoO₃用量达到0.11 g时,脱硫率超过95%;随着用量继续加大,脱硫率可以达到100%。

图3(b)所示为不同TiO₂-MoO₃用量下,脱硫率随H₂O₂用量的变化规律。由图可知,当TiO₂-MoO₃用量为0.01 g时,脱硫率在不同H₂O₂用量时总体不高,维持在60%~75%范围;当TiO₂-MoO₃用量为0.02 g时,脱硫率在不同H₂O₂用量下普遍提升;当TiO₂-MoO₃用量为0.03 g时,脱硫率在不同H₂O₂用量下总体可达98%以上(除H₂O₂用量 50 μL样品外);当TiO₂-MoO₃用量为0.04 g时,脱硫率在不同H₂O₂用量下均可达到100%。因此,选用合适的H₂O₂用量,可在较低TiO₂-MoO₃用量下实现高脱硫率。本实验选取最佳的TiO₂-MoO₃用量为0.04 g,H₂O₂用量为25 μL。

图3(c)考察了不同温度下脱硫效果与反应时间的关系。随着反应时间增大,脱硫率逐渐增大。当反应温度为20℃时,脱硫率整体偏低,最高达65%,从反应时间5 min增长到60 min,脱硫率增长幅度为17%,增长幅度较小。当反应温度为30~40℃时,脱硫率最高可达97%,从反应时间5 min增长到60 min,脱硫率增长幅度约为35%,而30℃与40℃的温度对脱硫率影响差别不明显,曲线出现交叉;当反应温度为50℃时,脱硫率最高达100%,实现了硫的完全脱除,从反应时间5 min增长到 45 min,脱硫率增长幅度为31%。反应速率的阿伦尼乌斯拟合图如图3(d)所示,随着反应时间增加,脱硫率逐渐增大,增长幅度与时间呈线性关系,在反应温度为50℃时,脱硫率在反应时间40 min时达到100%。

2.3.2 催化剂循环稳定性

图4(a)为催化剂脱硫性能的循环稳定性测试结果。在一次脱硫实验结束后,取出TiO₂-MoO₃催化剂,用乙醇浸泡1 h后进行离心处理,收集沉淀物,在50℃下烘干,再将其用于后续的脱硫反应。由图可以看出,TiO₂-MoO₃重复使用10次后,脱硫率保持在95%以上,表明该催化剂具有良好的循环稳定性。

2.3.3 TiO₂-MoO₃对其他含硫物质的脱除性能

考察了TiO₂-MoO₃对其他噻吩类含硫物质,如4,6-二甲基二苯并噻吩(4,6-DMDBT)和苯并噻吩(BT)的脱除性能。如图4(b)所示,分别用4,6-DMDBT和BT配制模拟柴油,测得其脱硫效率分别为98%和60%,考虑到前述对DBT的脱硫率可以达到100%,可以看出,TiO₂-MoO₃对4,6-DMDBT和DBT均能实现深度脱硫,而对BT的脱除效果一般。这3种含硫物质脱除性能的顺序为:DBT>4,6-DMDBT>BT。虽然4,6-DMDBT和DBT的空间位阻较大,但它们具有较强的离域π电子,在电子离域π键和金属离子活性位点之间发生的配位作用比BT更强,这使得TiO₂-MoO₃更容易与DBT和4,6-DMDBT结合形成配合物,因此,TiO₂-MoO₃对4,6-DMDBT和DBT的脱除性能比BT更好。

2.4 TiO₂-MoO₃的脱硫反应机理

图5(a)为脱硫反应前后模拟燃油的FT-IR图。从谱图可知,脱硫反应后,在1 100 cm^-1处有吸收峰,对应S—O键的吸收峰;在1 700 cm^-1处有吸收峰,对应S=O键的吸收峰,表明在脱硫反应后有DBTO₂生成。对反应后的模拟燃油取上清液油相进行MS表征,图5(b)为表征得到的MS图,其最高峰对应的质荷比(m/z)为216,与DBTO₂的相对分子量一致,表明脱硫反应后DBT主要被转化为 DBTO₂,与图5(a)脱硫反应前后模拟燃油的FT-IR实验结果一致。

在以上实验结果的基础上,探究了TiO₂-MoO₃催化剂在本研究体系中的催化氧化脱硫机理,如图6所示。TiO₂-MoO₃具有疏松多孔结构,使反应物可以充分扩散到催化剂内部,使活性位点和反应物之间能够完全接触。TiO₂-MoO₃首先与H₂O₂结合,形成过氧金属物质,再与DBT上的S结合,形成亚砜结构,进一步氧化转变为砜^[28]。

3 结论

(1)采用水热法合成了介孔TiO₂-MoO₃复合催化剂,并对其进行了结构表征,以TiO₂-MoO₃作为催化剂进行催化氧化脱硫,在反应温度50℃、催化剂0.05 g、H₂O₂用量25 μL、搅拌速率1 000 r/min时,可以稳定实现DBT的完全脱除,催化性能和循环使用稳定性具有应用价值。

(2)对比考察了TiO₂-MoO₃对DBT、4,6-DMDBT和BT的脱除效果,TiO₂-MoO₃对4,6-DMDBT也能实现深度脱硫(98%),对这3种含硫物质脱除性能的顺序为:DBT>4,6-DMDBT>BT。

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基金资助

宁夏重点研发项目(引才专项)(2021BEB04052)

宁夏自然科学基金项目(2023AAC03329)

宁夏回国留学人员创新创业项目([2023]5号)

宁夏高校一流学科建设项目(HGZD23-01)

宁夏高校一流学科建设项目(HGZD22-23)

宁夏师范大学大学生科技创新基金项目资助

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