WO2022236914A1 - 一种以烟梗丝为模板制备TiO 2光催化材料的方法及用途 - Google Patents

一种以烟梗丝为模板制备TiO 2光催化材料的方法及用途 Download PDF

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WO2022236914A1
WO2022236914A1 PCT/CN2021/099788 CN2021099788W WO2022236914A1 WO 2022236914 A1 WO2022236914 A1 WO 2022236914A1 CN 2021099788 W CN2021099788 W CN 2021099788W WO 2022236914 A1 WO2022236914 A1 WO 2022236914A1
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template
tobacco stem
tio
photocatalytic material
shredded tobacco
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French (fr)
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李振杰
蒋昆明
陈永娟
刘春波
唐石云
张凤梅
杨继
王玉田
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云南中烟工业有限责任公司
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen

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  • the invention belongs to the technical field of nanocomposite material preparation, and in particular relates to a synthesis method and application of a TiO2 photocatalyst material prepared by using shredded tobacco stems as a template.
  • the heterogeneous photocatalytic process with semiconductor oxides as catalysts has become an ideal environment due to its unique properties such as reaction at room temperature, direct use of sunlight, mineralization of almost all organic pollutants, and no secondary pollution. pollution control technology.
  • the first-generation photocatalysts based on titanium dioxide can only absorb and utilize ultraviolet light or the ultraviolet part of sunlight due to their wide band gap. How to improve the spectral response range and catalytic efficiency of photocatalysts is a key issue that restricts the practicality of photocatalytic technology. , is currently the most concerned frontier and the most challenging subject in the field of photocatalysis, and has particularly important scientific value and practical prospects.
  • TiO 2 photocatalytic materials such as: sulfuric acid method, chlorination method, TiCl 4 hydrolysis method, sol-gel method, hydrothermal method, gas phase method, microemulsion method, etc. These methods are relatively traditional and have certain pollution to the environment.
  • Biological template synthesis is an environmentally friendly method to obtain materials with certain specific properties.
  • materials with special optical properties in nature or materials that can efficiently utilize light energy can be used.
  • These biological templates not only serve as structure-directing agents to make the synthesized products have the special morphology of the template, but also bring about the self-doping of the elements contained in the template, which improves the activity of the catalyst.
  • Chinese patent CN201911251202.2 discloses a method for preparing TiO2 using a biological template for immobilizing arsenic in plants.
  • the biological template used in this method is centipede grass, and the obtained composite material has an excellent arsenic fixation rate.
  • Chinese patent CN201810609991.1 discloses a method for preparing composite photocatalytic materials based on microbial templates. The biological templates used in this method are phages to improve photocatalytic efficiency.
  • Chinese patent CN201410839055.1 relates to a method for preparing a coating of titanium dioxide-diatom mud composite material loaded with photocatalyst, which is applied to degrade indoor formaldehyde, prepared by biological template, and the obtained composite material has high efficiency for the adsorbed formaldehyde photocatalytic degradation activity.
  • the present invention firstly uses tobacco waste, that is, shredded tobacco stems, as a template to prepare a TiO2 photocatalytic material, and the obtained TiO2 photocatalytic material shows high catalytic activity in degrading nicotine under sunlight.
  • the invention provides a TiO 2 photocatalytic material prepared from shredded tobacco stems as a template, a preparation method, and the use of the obtained TiO 2 photocatalytic material for degrading nicotine under sunlight.
  • the first aspect of the present invention discloses a method for preparing TiO photocatalyst material with cut tobacco stems as a template, comprising the following steps:
  • step (2) adding a certain amount of titanium compound into isopropanol, then adding a certain amount of hydrogen fluoride solution and mixing evenly, then adding the shredded tobacco stem template obtained in step (1), and dipping for a period of time;
  • step (3) The material obtained in step (2) is sealed and heated for a period of time, and then cooled to room temperature;
  • step (3) Separate the product obtained in step (3), and wash it several times with distilled water and absolute ethanol to obtain a solid, dry the solid and calcinate it in an air atmosphere at a certain temperature, and remove the shredded tobacco stem template to obtain the obtained
  • the TiO 2 photocatalytic material described above
  • the concentration of glutaraldehyde used in step (1) is 4-6wt%
  • the concentration of hydrochloric acid is 4-6wt%
  • the concentration of ethanol is respectively 30wt%, 50wt%, and 90wt%.
  • the titanium compound in step (2) is one of tetrabutyl titanate, titanium isopropoxide, and titanium tetrachloride, and the ratio of the titanium compound, isopropanol, hydrogen fluoride, and shredded tobacco stem template to The formula is (1-5)mL: 50mL: (0.20-1.00)mL: (1-5)g; the mass fraction of the hydrogen fluoride solution is 40%; the immersion time is 12-48h.
  • These kinds of titanium compounds are generally liquid, and it is easier to measure the volume; if the titanium compound used is solid, it can be weighed by multiplying the volume by the density and converting it into mass.
  • the reaction temperature in step (3) is 100-180°C, and the reaction time is 12-48h.
  • the calcination temperature in step (4) is 300-600°C; the calcination time is 5-20h.
  • the second aspect of the present invention discloses the TiO2 photocatalytic material prepared by the method.
  • the third aspect of the present invention discloses the use of the TiO 2 photocatalytic material for degrading nicotine.
  • the present invention uses shredded tobacco waste tobacco stems as a template, and adopts a simple solvothermal method to obtain TiO2 photocatalytic material under simultaneous etching with hydrofluoric acid.
  • the preparation method is simple, reliable, low in cost, strong in operability, and beneficial to large-scale industrial production.
  • the TiO 2 photocatalytic material prepared by the present invention degrades nicotine under sunlight, showing high catalytic activity.
  • the TiO2 photocatalytic material prepared by the invention also has broad application prospects in the fields of sewage treatment, environmental purification, solar energy conversion and utilization, and the like.
  • the present invention starts from tobacco waste shredded tobacco stems, combines the characteristics of biological templates to prepare photocatalytic materials, utilizes the special morphology characteristics of shredded tobacco stems, and replicates its appearance, and passes through hydrogen for the first time in the process of material synthesis.
  • the method of hydrofluoric acid etching is used to control its microstructure, and a highly efficient TiO 2 photocatalytic material is prepared.
  • the use of cut tobacco stem templates to prepare photocatalytic materials provides a corresponding theoretical basis and experimental evidence for further exploration and construction of materials with complex and special inorganic structures.
  • Fig. 1 is the XRD figure of the TiO photocatalyst material that embodiment 1 makes.
  • Fig. 2 is the scanning electron micrograph of the TiO photocatalyst material that embodiment 1 makes.
  • Fig. 3 is the transmission electron micrograph of the TiO2 photocatalyst material that embodiment 1 makes.
  • Fig. 4 is the TiO that embodiment 1 makes nitrogen adsorption/desorption curve and pore size distribution curve of photocatalytic material
  • Fig. 5 is the TiO 2 photocatalyst material HF-STiO 2 that embodiment 1 makes, the STiO 2 that comparative example 1 obtains (without hydrofluoric acid treatment), the TiO 2 that comparative example 2 obtains (without shredded tobacco stem template ), and a blank (no TiO 2 ) activity comparison curve for degrading nicotine.
  • Embodiment 1 take cut tobacco stem as the TiO2 photocatalytic material preparation of template, the steps are as follows:
  • Figures 1 to 4 show the characterization results of the obtained TiO 2 photocatalyst material using shredded tobacco stems as a template. It can be seen from Figure 1 that the obtained TiO2 photocatalytic material with cut tobacco stems as a template corresponds to the anatase TiO2 standard card (JCPDS 21-1272). It can be seen from the scanning electron microscope photos in Figure 2 and the transmission electron microscope photos in Figure 3 that the obtained TiO2 photocatalyst material with shredded tobacco stems as a template well replicates the overall morphology of shredded tobacco stems, consisting of polycrystalline particles and form a large number of nanopore structures.
  • the preparation method is the same as in Example 1, except that no hydrofluoric acid is added in step (2).
  • the TiO 2 photocatalytic material was obtained and named as STiO 2 .
  • Comparative Example 2 Preparation of TiO photocatalytic material without adding shredded tobacco stems as a template
  • the preparation method is the same as that in Example 1, except that no shredded tobacco stem template is added in step (2).
  • the TiO 2 photocatalytic material was obtained and named as TiO 2 .
  • the HF-STiO 2 obtained in Example 1, the STiO 2 obtained in Comparative Example 1, the TiO 2 obtained in Comparative Example 2, and the blank (without TiO 2 ) were subjected to photocatalytic degradation of nicotine, and the results are shown in FIG. 5 .
  • the blank sample cannot degrade nicotine under light; the TiO2 materials prepared in Example 1, Comparative Example 1 and Comparative Example 2 can degrade nicotine under light conditions, but the three The performance of degrading nicotine is different, and the HF-STiO obtained in Example 1 has the best performance in degrading nicotine; the performance of STiO obtained in Comparative Example 1 for degrading nicotine is better than the performance of TiO obtained in Comparative Example 2 for degrading nicotine.

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  • Toxicology (AREA)
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Abstract

本发明公开了一种以烟梗丝为模板制备TiO2光催化材料的方法，包括如下步骤：（1）将烟梗丝分别用戊二醛、盐酸及乙醇溶液浸泡处理；（2）将钛化合物、异丙醇、氟化氢溶液和烟梗丝模板混合浸渍；（3）升温反应一段时间；（4）将得到的固体煅烧除去烟梗丝模板后，即得到所述的TiO2光催化材料。本发明还公开了得到的TiO2光催化材料和其用于降解尼古丁的用途。

Description

一种以烟梗丝为模板制备TiO 2光催化材料的方法及用途 技术领域
本发明属于纳米复合材料制备技术领域，尤其涉及一种以烟梗丝为模板制备TiO 2光催化材料的合成方法和应用。
背景技术
半导体氧化物为催化剂的多相光催化过程，以其可在室温下反应、可直接利用太阳光、可将几乎全部有机污染物矿化、无二次污染等独特性能而成为一种理想的环境污染治理技术。以二氧化钛为主的第一代光催化剂由于禁带较宽，只能吸收利用紫外光或太阳光中的紫外线部分，如何提高光催化剂的光谱响应范围和催化效率是制约光催化技术实用的关键问题，也是光催化学界当前最受关注的前沿和最具挑战性的课题，具有特别重要的科学价值和实用前景。目前，制备TiO 2光催化材料的方法有很多如：硫酸法、氯化法、TiCl 4水解法、溶胶-凝胶法、水热法、气相法、微乳液法等。这些方法较为传统，对环境有一定的污染。生物模板合成法是一种环境友好的方法来获得具有某些特定性质材料的方法，对光催化材料的制备而言，可以利用自然界中具有特殊光学性质或对光能能够高效利用的材料。这些生物模板不仅作为结构导向剂使合成出的产物具有模板的特殊形貌，还带来了模板中所含元素的自掺杂，提高了催化剂的活性。
中国专利CN201911251202.2公开了一种用于固定植物中砷的生物模板制备TiO 2方法，该方法中使用的生物模板为蜈蚣草，得到的复合材料具有优良的固砷率。中国专利CN201810609991.1公开了一种基于微生物模板的复合光催化材料制备方法，该方法中使用的生物模板为噬菌体，提高光催化效率。中国专利CN201410839055.1涉及一种应用于降解室内甲醛的、由生物模板制备的、负载了光催化剂的二氧化钛-硅藻泥复合材料的涂料的制备方法，得到的复合材料对所吸附的甲醛具有高效的光催化降解活性。
本发明首次使用烟草废弃物即烟梗丝作为模板制备TiO2光催化材料，得到的TiO2光催化材料在太阳光下降解尼古丁显示了较高的催化活性。
发明内容
本发明提供一种烟梗丝作为模板制备的TiO 2光催化材料及制备方法、及得到的TiO 2光催化材料用于在太阳光下降解尼古丁的用途。
本发明的技术方案如下：
本发明第一方面公开了一种以烟梗丝为模板制备TiO 2光催化材料的方法，包括如下步骤：
(1)将烟梗丝分别用戊二醛、盐酸，以及用浓度逐渐增大的乙醇溶液浸泡处理后烘干得到烟梗丝模板；
(2)将一定量的钛化合物加入到异丙醇中，再加入一定量的氟化氢溶液混合均匀，然后加入步骤(1)得到的烟梗丝模板，浸渍一段时间；
(3)将步骤(2)得到的物质密封升温反应一段时间，然后冷却至室温；
(4)将步骤(3)得到的产物分离，并用蒸馏水和无水乙醇各洗涤几次得到固体，将固体干燥后在空气气氛中和一定温度下煅烧，除去烟梗丝模板后，即得到所述的TiO 2光催化材料。
优选地，步骤(1)所使用的戊二醛浓度为4-6wt％，盐酸浓度为4-6wt％，乙醇浓度分别为30wt％、50wt％、90wt％。
优选地，步骤(2)所述钛化合物为钛酸四丁酯、异丙醇钛、四氯化钛中的一种，所述钛化合物、异丙醇、氟化氢和烟梗丝模板加入量比为(1-5)mL∶50mL∶(0.20-1.00)mL∶(1-5)g；所述氟化氢溶液的质量分数为40％；浸渍时间为12-48h。这几种钛化合物一般情况是液体，量取体积比较容易；如果使用的钛化合物是固体，可以用体积乘以密度换算成质量进行称取。
优选地，步骤(3)的反应温度为100-180℃，反应时间为12-48h。
优选地，步骤(4)的煅烧温度为300-600℃；煅烧时间5-20h。
本发明第二方面公开了所述的方法制备得到的TiO 2光催化材料。
本发明第三方面公开了所述的TiO 2光催化材料用于降解尼古丁的用途。
本发明具有以下优点及效果：
1、本发明首次使用烟草废弃物烟梗丝作为模板，采用简单的溶剂热法，在氢氟酸同步刻蚀的情况下得到TiO 2光催化材料。制备方法简单、可靠，成本低，可操作性强，有利于大规模工业化生产。
2、本发明制备得到的TiO 2光催化材料在太阳光下降解尼古丁，显示了较高的催化活性。本发明制备得到的TiO 2光催化材料在污水处理、环境净化和太阳能转化利用等领域也具有广泛的应用前景。
3、本发明从烟草废弃物烟梗丝出发，结合生物模板制备光催化材料的特点，利用烟梗丝特殊的形貌特征，将其形貌复制出来，并且在材料合成的过程中首次通过氢氟酸刻蚀的方法，对其微结构进行调控，制备得到高效的TiO 2光催化材料。利用烟梗丝模板制备光催化材料，为进一步探索构建复杂特殊无机结构材料提供相应的理论基础与实验证据。
附图说明
图1为实施例1制得的TiO 2光催化材料的XRD图。
图2为实施例1制得的TiO 2光催化材料的扫描电镜图。
图3为实施例1制得的TiO 2光催化材料的透射电镜图。
图4为实施例1制得的TiO 2光催化材料的氮气吸附/脱附曲线和孔径分布曲线；
图5为实施例1制得的TiO 2光催化材料HF-STiO 2、对比实施例1得到的STiO 2(没有用氢氟酸处理)、对比实施例2得到的TiO 2(无烟梗丝模板)、和空白(无TiO 2)降解尼古丁的活性比较曲线图。
具体实施方式
下面结合部分具体实施方案对本发明进行详述。这些实施例仅用于说明本发明，而不用于限制本发明的范围。实施例中的实施方案仅为优选方案，但本发明并不局限于优选方案。
实施例1：以烟梗丝为模板的TiO 2光催化材料制备，步骤如下：
(1)分别用5wt％戊二醛和5wt％的HCl浸泡处理烟梗丝，然后再顺序用30wt％、50wt％、90wt％的乙醇溶液浸泡处理烟梗丝并烘干；
(2)将50mL异丙醇加入到100mL的聚四氟乙烯反应釜中，在室温磁力搅拌下加入1.2mL的钛酸四丁酯，快速搅拌1min后，加入0.5mL的质量分数 为40％的HF溶液，快速搅拌5min，取出搅拌子；加入2g步骤(1)处理好的烟梗丝模板，室温下恒温浸渍24h。
(3)将聚四氟乙烯反应釜放入不锈钢瓶中，密封后放入烘箱中于180℃溶剂热反应24h，然后冷却至室温。
(4)将产物用布氏漏斗过滤，并用蒸馏水和无水乙醇各洗涤3次，于60℃下干燥后，放入马弗炉中，2℃/min程序升温，在空气气氛中450℃下煅烧10h，除去烟梗丝模板，即得到以烟梗丝为模板的TiO 2光催化材料，命名为HF-STiO 2。
图1-图4为得到的以烟梗丝为模板的TiO 2光催化材料的表征结果。从图1可以看出得到的以烟梗丝为模板的TiO 2光催化材料与锐钛矿TiO2标准卡(JCPDS 21-1272)对应一致。从图2的扫描电镜照片和图3的透射电镜照片可以看出，得到的以烟梗丝为模板的TiO 2光催化材料很好地复制了烟梗丝的整体形貌，由多晶颗粒堆积而成，并形成大量纳米孔结构。从图4的氮气吸附/脱附曲线和孔径分布曲线(图4内)可以看出，得到的以烟梗丝为模板的TiO 2光催化材料具有由颗粒堆积造成的介孔结构。
对比实施例1：没有加入氢氟酸的TiO 2光催化材料制备
制备方法同实施例1，不同之处在步骤(2)中未加入氢氟酸。得到TiO 2光催化材料，命名为STiO 2。
对比实施例2：没有加入烟梗丝为模板的TiO 2光催化材料制备
制备方法同实施例1，不同之处在步骤(2)中未加入烟梗丝模板。得到TiO 2光催化材料，命名为TiO 2。
将实施例1得到的HF-STiO 2、对比实施例1得到的STiO 2、对比实施例2得到的TiO 2、和空白(无TiO 2)进行光催化降解尼古丁实验，结果如图5所示。由图5可以看出，空白样品在光照下不能使尼古丁降解；实施例1、对比实施例1和对比实施例2制备得到的TiO 2材料在光照条件下均能使尼古丁降解，但是三者的降解尼古丁性能不同，实施例1得到的HF-STiO 2降解尼古丁的性能最好；对比实施例1得到的STiO 2降解尼古丁的性能优于对比实施例2得到TiO 2降解 尼古丁的性能。
以上显示和描述了本发明的主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的较优实例，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入本发明要求保护的范围内。

Claims (7)

  1. 一种以烟梗丝为模板制备TiO 2光催化材料的方法，其特征在于，包括如下步骤：
    (1)将烟梗丝分别用戊二醛、盐酸，以及用浓度逐渐增大的乙醇溶液浸泡处理后烘干得到烟梗丝模板；
    (2)将一定量的钛化合物加入到异丙醇中，再加入一定量的氟化氢溶液混合均匀，然后加入步骤(1)得到的烟梗丝模板，浸渍一段时间；
    (3)将步骤(2)得到的物质密封升温反应一段时间，然后冷却至室温；
    (4)将步骤(3)得到的产物分离，并用蒸馏水和无水乙醇各洗涤几次得到固体，将固体干燥后在空气气氛中和一定温度下煅烧，除去烟梗丝模板后，即得到所述的TiO 2光催化材料。
  2. 根据权利要求1所述的方法，其特征在于，步骤(1)所使用的戊二醛浓度为4-6wt％，盐酸浓度为4-6wt％，乙醇浓度分别为30wt％、50wt％、90wt％。
  3. 根据权利要求1所述的方法，其特征在于，步骤(2)所述钛化合物为钛酸四丁酯、异丙醇钛、四氯化钛中的一种，所述钛化合物、异丙醇、氟化氢和烟梗丝模板加入量比为(1-5)mL∶50mL∶(0.20-1.00)mL∶(1-5)g；所述氟化氢溶液的质量分数为40％；浸渍时间为12-48h。
  4. 根据权利要求1所述的方法，其特征在于，步骤(3)的反应温度为100-180℃，反应时间为12-48h。
  5. 根据权利要求1所述的方法，其特征在于，步骤(4)的煅烧温度为300-600℃；煅烧时间5-20h。
  6. 根据权利要求1-5任一所述的方法制备得到的TiO 2光催化材料。
  7. 根据权利要求6所述的TiO 2光催化材料用于降解尼古丁的用途。
PCT/CN2021/099788 2021-05-12 2021-06-11 一种以烟梗丝为模板制备TiO 2光催化材料的方法及用途 WO2022236914A1 (zh)

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