CN106732503A - 负载纳米二氧化钛薄膜的活性炭纤维及其制备方法和用途 - Google Patents
负载纳米二氧化钛薄膜的活性炭纤维及其制备方法和用途 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 42
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- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 14
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Abstract
公开了一种活性炭纤维负载纳米二氧化钛薄膜的制备方法及其用途。该方法采用原位诱导反胶束法制备活性炭纤维负载均匀无裂纹、附着力强、薄膜厚度可控的致密纳米二氧化钛薄膜的复合光催化材料。具体制备方法包括：油包水型的反胶束体系的配制；二氧化钛前驱体活性位透明胶束的配制；原位诱导反胶束的配制；活性炭纤维毡浸泡负载氧化钛前驱体；干燥并高温焙烧活化活性炭纤维表面的“湿膜”，最终制得活性炭纤维负载纳米二氧化钛薄膜的复合光催化材料。本发明还提供依据本发明制备方法得到的复合材料在光催化氧化分解有机物方面的应用。本发明TiO2/ACF复合材料的制备方法简单，本发明方法可以在活性炭纤维表面制备附着力强、薄膜厚度可控的均匀致密纳米二氧化钛薄膜，制得的TiO2/ACF复合材料吸附能力强、光催化氧化活性高。
Description
技术领域
本发明涉及一种活性炭纤维负载均匀无裂纹、附着力强、薄膜厚度可控的致密纳米二氧化钛薄膜及其制备方法，以及该负载纳米二氧化钛薄膜的活性炭纤维用于光催化氧化水处理和空气处理的用途。
背景技术
活性炭纤维(ACF)是一种具有高效吸附活性的环保吸附材料，继粒状活性炭和粉状活性炭之后的第三代活性炭产品。活性炭纤维表面具有丰富的空介结构，扩散路径较短，其主要由2.0nm微孔组成，活性炭纤维直径范围为10～13μm，具有较大的吸附接触面积，吸附效率高。活性炭纤维的比表面大，吸附和脱附量大，可以有效吸附处理较宽浓度范围的气体和液体污染源。活性炭纤维被广泛应用在挥发性有机物(VOCs)和水处理净化等方面。但是，活性炭纤维在实际应用中吸附达到饱和状态后，需进行脱附处理活性炭纤维再生过程，常见的脱附过程有物理脱附过程和化学脱附过程。物理脱附过程效率低成本高，综合价值低；化学脱附过程是利用被吸附的污染物发生化学反应达到脱附的一种手段。高效率的脱附过程使得活性炭纤维活性位再生是扩大该吸附材料应用范围的有效手段。同时后段的脱附活化在一定程度上限制了活性炭纤维应用。
二氧化钛是一种宽禁带半导体，常见的晶型有锐钛矿、板钛矿和金红石三种。纳米二氧化钛半导体具有良好的稳定性和分散性，在光电子能照射下具有很强的氧化还原能力，成为促使各种有机物降解的光触媒催化剂，在光降解挥发性有机物(VOCs)和水处理方面发挥很大的作用。其紫外光响应光催化应用已扩展到新能源如太阳能敏化电池方面的应用，其具有更加广泛的实际应用前景。一维粉末纳米TiO2存在易团聚、难回收等缺点，甚至产生二次污染，限制了TiO2半导体材料的应用。目前TiO2半导体研究方向主要是降低TiO2半导体禁带宽度和改善TiO2结构形态。
发明专利申请号CN03100058.4和专利申请号CN02147089.8分别提出在光滑的玻璃表面制备纳米二氧化钛薄膜，其采用传统的反胶束法制备透明二氧化钛薄膜，存在钛离子浓度低、难以有效控制纳米二氧化钛晶核生长以及对基底选择应用存在一定限制，使得在微米级的ACF表面不易形成均匀致密结构稳定的纳米薄膜；专利申请号CN200710013501.3中采用溶胶-凝胶法制备纳米二氧化钛薄膜，一定程度上存在纳米二氧化钛颗粒的团聚和脱落，难以在ACF表面形成均匀、厚度可控的纳米氧化钛薄膜；发明专利申请号CN201510635983.0采用硅烷偶联剂对活性炭纤维表面进行改性，然后在二氧化钛前驱体溶胶中浸渍得到TiO2/ACF复合材料，其缺点是无法在ACF上制备得到纳米二氧化钛薄膜，ACF表面的二氧化钛颗粒发生团聚导致结构稳定性差。为改善TiO2薄膜在ACF表面的物理结构性质，本发明提出了一种原位诱导反胶束法制备得到活性炭纤维负载均匀无裂纹、附着力强、薄膜厚度可控的致密纳米二氧化钛薄膜的光催化复合材料。
发明内容
本发明的目的是提供一种活性炭纤维表面负载均匀无裂纹、附着力强、薄膜厚度可控的致密纳米二氧化钛薄膜复合光催化材料，在活性炭纤维表面负载均匀稳定的纳米二氧化钛薄膜的制备方法和该负载纳米二氧化钛薄膜的活性炭纤维在光催化氧化方面的应用，优选TiO2/ACF复合材料净化空气的应用。
本发明的活性碳纤维表面负载无裂纹的纳米二氧化钛薄膜复合光催化材料，解决了活性炭纤维吸附过饱和问题，结合纳米二氧化钛光催化氧化还原性质降解活性炭表面吸附的有机物从而实现化学脱附过程。获得可循环利用的TiO2/ACF纳米复合光催化材料，用于吸附降解挥发性有机物实现空气净化和水处理。
本发明的活性炭纤维负载均匀无裂纹、附着力强、薄膜厚度可控的致密纳米二氧化钛薄膜复合材料可通过原位诱导反胶束法制备，并负载到不同形貌和材质的活性炭纤维材料上。
本发明负载纳米二氧化钛薄膜的活性炭纤维复合材料的制备包括如下步骤：
(1)配制反胶束体系。在反胶束体系中按摩尔比水：表面活性剂为0.9～1.8加入环己烷中，搅拌90min后超声波中处理60min，制得热力学稳定的反胶束体系。
(2)配制活性位透明胶束。钛酸丁酯加入异戊醇中形成钛酸丁酯体积分数为30％的钛酸丁酯异戊醇溶液，依次添加二乙醇胺和水，制得活性位透明胶束；所述水用量按摩尔比为钛酸丁酯的2倍；二乙醇胺：水的摩尔比为0.6～1.7。
(3)将上述(2)的活性位透明胶束加入至上述(1)的反胶束体系中，制得具有活性位的反胶束微乳；补加钛酸丁酯，其用量为(1)中水的摩尔量的1/2；透明胶束溶液与反胶束的体积比为0.1033～0.4827；所得原位诱导反胶束微乳中钛离子浓度为0.15～0.31mol/L。
(4)活性炭纤维在去离子水中浸泡再经超声波震荡清洗，清洗完成后在温度为70～100℃完全烘干，浸入配制好的原位诱导反胶束微乳溶液中，浸渍5～20min后，得到负载二氧化钛前驱体的活性炭纤维。将浸渍好的活性炭纤维在100℃下保温30min，最后转移至氮气氛围的高温炉中升温至450～800℃进行焙烧活化，制得TiO2/ACF纳米复合光催化材料。
本发明所述的活性炭纤维是粘胶基纤维、沥青基纤维、酚醛基纤维、纤维素纤维、聚丙烯腈纤维等。
为了更好的实现本发明，步骤(2)二乙醇胺：钛酸丁酯的摩尔比为1.2～3.4，得到更加稳定的原位诱导反胶束微乳溶液。
通过改变步骤(4)中活性炭纤维在原位诱导反胶束微乳溶液中的浸渍时间和次数，可以在活性炭纤维表面负载不同厚度的纳米二氧化钛薄膜，从而实现控制纳米薄膜厚度以满足在不同材质和形貌的活性炭纤维吸附材料表面上镀膜。
在干燥和焙烧活化过程中，保持低的升温速率有利于形成表面均匀无裂纹的纳米二氧化钛薄膜，尤其是在焙烧活化升温过程中，要严格控制升温速率在4～6℃，并有氮气氛围保护。
本发明所述的活性炭纤维负载纳米二氧化钛薄膜复合光催化材料是由上述制备方法制备而成。
本发明所述的活性炭纤维负载纳米二氧化钛薄膜复合光催化材料具有光催化净化空气和水处理用途。
本发明与现有在活性炭纤维上负载纳米二氧化钛薄膜技术相比，具有如下优点：
1.本发明在反胶束微乳法的基础上提出添加活性位诱导工艺过程，得到了稳定性好的二氧化钛前驱体原位诱导反胶束溶液，解决了原来微乳法的钛离子浓度低的缺点，提高了二氧化钛前驱体在活性炭纤维表面上的负载率。
2.将纳米二氧化钛半导体的光催化氧化还原作用同活性炭纤维的高吸附能力相结合，提高了活性炭纤维活性吸附活性和使用寿命。
3.该方法工艺过程简单，设备要求较低，可满足在不同材质和形状的基底材料表面上浸渍镀膜。
附图说明
图1为本发明实施例1复合光催化材料的扫描电子显微镜SEM图。
图2为本发明实施例2复合光催化材料的扫描电子显微镜SEM图。
图3为本发明实施例2复合光催化材料的XRD图谱。
图4为本发明实施例3复合光催化材料的扫描电子显微镜SEM图。
图5为本发明实施例4复合光催化材料的扫描电子显微镜SEM图。
图6为本发明实施例4复合光催化材料的XRD图谱。
图7为实施例5复合材料光催化性能评价自制反应器装置示意图。
图8为本发明实施例1所得复合光催化材料对亚甲基蓝有机溶液的光催化降解曲线。
图9为本发明实施例2所得复合光催化材料对亚甲基蓝有机溶液的光催化降解曲线。
图10为本发明实施例3所得复合光催化材料对亚甲基蓝有机溶液的光催化降解曲线。
图11为本发明实施例4所得复合光催化材料对亚甲基蓝有机溶液的光催化降解曲线。
具体实施方式
下面结合具体实施例对本发明工艺过程做进一步详细说明，但本发明的实施方式不限于此。
实施例1
在磁力搅拌(25℃)条件下，将20.4ml Triton X-100添加到179ml环己烷中，20min后再缓慢的加入0.8ml的去离子水。超声波60min使其进一步分散，形成乳白色热力学稳定的反胶束体系，静置6h，得到三组分热力学稳定的油包水(W/O)型的反胶束体系。
在磁力搅拌下，将5ml钛酸丁酯(TBOT)滴加到11.7ml异戊醇，制得TBOT体积浓度30％的钛酸丁酯异戊醇溶液，继续搅拌并添加3.5ml二乙醇胺(DEA)，完全混合后，滴加0.5ml去离子水进行水解。将配置好的透明胶束在磁力搅拌条件下缓慢滴加到稳定的反胶束体系中，反胶束体系由原来的乳白色逐渐转变为淡黄色透明体系，添加7.8ml钛酸丁酯，形成微黄色的透明原位诱导反胶束。最终制备得到钛离子浓度为0.15mol/L的原位诱导反胶束。
在制备得到的原位诱导反胶束溶液中浸泡预处理好的活性炭纤维毡或活性炭纤维布5min，然后100℃干燥30min，转移至通有氮气保护的高温管式炉中升温至450℃并保温120min，制得活性炭纤维负载锐钛矿型和金红石型纳米二氧化钛薄膜的复合光催化材料，其电子显微镜照片见附图1。
实施例2
在磁力搅拌(25℃)条件下，将30.6ml Triton X-100添加到168ml环己烷中，20min后再缓慢的加入1.2ml的去离子水。超声波搅拌60min，形成乳白色热力学稳定的反胶束体系，静置6h，得到三组分热力学稳定的油包水(W/O)型的反胶束体系。
在磁力搅拌下，将10ml钛酸丁酯滴加到23.3ml异戊醇，制得TBOT体积分数30％的钛酸丁酯异戊醇溶液，继续搅拌并添加15.3ml二乙醇胺(DEA)，完全混合后，滴加1.022ml去离子水进行水解。将配置好的透明胶束在磁力搅拌条件下缓慢滴加到稳定的反胶束体系中，反胶束体系由原来的乳白色逐渐转变为淡黄色透明体系，添加7.8ml钛酸丁酯，形成微黄色的透明原位诱导反胶束。最终制备得到钛离子浓度为0.24mol/L的原位诱导反胶束。
在制备得到的原位诱导反胶束溶液中浸泡预处理好的活性炭纤维毡或活性炭纤维布5min，然后100℃干燥30min，转移至通有氮气保护的高温管式炉中升温至500℃并保温120min，制得活性炭纤维负载锐钛矿型和金红石型纳米二氧化钛薄膜的复合光催化材料，其电子显微镜照片见附图2，XRD图谱见附图3。
实施例3
在磁力搅拌(25℃)条件下，将30.6ml Triton X-100添加到178ml环己烷中，20min后再缓慢的加入1.2ml的去离子水。超声波搅拌60min，形成乳白色热力学稳定的反胶束体系，静置6h，得到三组分热力学稳定的油包水(W/O)型的反胶束体系。
在磁力搅拌下，将15ml钛酸丁酯(TBOT)滴加到35ml异戊醇制得TBOT体积浓度30％的钛酸丁酯异戊醇溶液，继续搅拌并添加8.2ml二乙醇胺(DEA)，完全混合后，滴加1.5ml去离子水进行水解。将配置好的透明胶束在磁力搅拌条件下缓慢滴加到稳定的反胶束体系中，反胶束体系由原来的乳白色逐渐转变为淡黄色透明体系，添加7.8ml钛酸丁酯，形成微黄色的透明原位诱导反胶束。最终制备得到钛离子浓度为0.28mol/L的原位诱导反胶束。
在制备得到的原位诱导反胶束溶液中浸泡预处理好的活性炭纤维毡或活性炭纤维布5min，然后100℃干燥30min，最后转移至通有氮气保护的高温管式炉中升温至600℃并保温120min，制得活性炭纤维负载锐钛矿型和金红石型纳米二氧化钛薄膜的复合光催化材料，其电子显微镜照片见附图4。
实施例4
在磁力搅拌(25℃)条件下，将30.6ml Triton X-100添加到118ml环己烷中，20min后再缓慢的加入1.2ml的去离子水。超声波搅拌60min，形成乳白色热力学稳定的反胶束体系，静置6h，得到三组分热力学稳定的油包水(W/O)型的反胶束体系。
在磁力搅拌下，将10ml钛酸丁酯(TBOT)滴加到23.3ml异戊醇制得TBOT体积浓度30％的钛酸丁酯异戊醇溶液，继续搅拌并添加2.7ml二乙醇胺(DEA)，完全混合后，最后滴加1.022ml去离子水进行水解。将配置好的透明胶束在磁力搅拌条件下缓慢滴加到稳定的反胶束体系中，反胶束体系由原来的乳白色逐渐转变为淡黄色透明体系，添加7.8ml钛酸丁酯，形成微黄色的透明原位诱导反胶束。最终制备得到钛离子浓度为0.31mol/L的原位诱导反胶束。
在制备得到的原位诱导反胶束溶液中浸泡预处理好的活性炭纤维毡或活性炭纤维布5min，然后100℃干燥30min，最后转移至通有氮气保护的高温管式炉中升温至800℃并保温120min，制得活性炭纤维负载金红石型纳米二氧化钛薄膜的复合光催化材料，其电子显微镜照片见附图5，XRD图谱见附图6。
实施例5：TiO2/ACF复合材料的光催化氧化活性的测试
采用亚甲基蓝模拟液体有机污染物测定复合材料的光催化性能。
采用相同实验条件测试不同实施例下得到的复合材料光催化性能，分别分为四组测试其亚甲基蓝降解率。在紫外灯照射下，对亚甲基蓝有机溶液的降解表征实施例1～4所制备的负载纳米二氧化钛薄膜的活性炭纤维复合材料的光催化氧化活性。具体步骤如下：采用自制的简单反应器(紫外灯管套入石英玻璃管中，TiO2/ACF复合光催化材料固定在石英管壁，催化剂同石英管插入反应液面中)，详见附图7，图中1、2、3和4分别为波长为320nm紫外灯、烧杯、磁力搅拌机和防护外壳。
在400ml烧杯浓度为8mg/L亚甲基蓝有机溶液中加入实施例1～4制备的1g TiO2/ACF催化剂，无光照条件下磁力搅拌30min，初次取样；然后紫外灯照射180min，每10min取样进行分析。每次取样经离心分离后取上层清夜，使用可见分光光度计测定波长664nm处的吸光度，计算得到光催化降解曲线，结果见图8～11。
Claims (7)
1.一种活性炭纤维负载均匀无裂纹、附着力强、薄膜厚度可控的致密纳米二氧化钛薄膜复合光催化材料的制备方法，其特征在于包括如下步骤：
(1)水∶表面活性剂摩尔比为0.9～1.8，分别加入连续油相环己烷中，环己烷的体积分数为0.58～0.68，磁力搅拌90min后在超声波中震荡60min，制得高度分散的热力学稳定反胶束体系；
(2)钛酸丁酯加入异戊醇中形成钛酸丁酯体积分数为30％的钛酸丁酯异戊醇溶液，依次添加二乙醇胺和水，制得活性位透明胶束；所述水用量按摩尔比为钛酸丁酯的2倍；二乙醇胺∶水的摩尔比为0.6～1.7；
(3)将上述(2)的活性位透明胶束加入至上述(1)的反胶束体系中，制得具有活性位的反胶束微乳；补加钛酸丁酯，其用量为(1)中水的摩尔量的1/2；透明胶束溶液与反胶束的体积比为0.1033～0.4827；所得原位诱导反胶束微乳中钛离子浓度为0.15～0.31mol/L；
(4)活性炭纤维在去离子水中浸泡再经超声波震荡清洗，清洗完成后在温度为70～100℃完全烘干，浸入配制好的原位诱导反胶束微乳溶液中，浸渍5～20min后，得到负载二氧化钛前驱体的活性炭纤维。将浸渍好的活性炭纤维在100℃下保温30min，最后转移至氮气氛围的高温炉中升温至450～800℃进行焙烧活化，制得TiO2/ACF纳米复合光催化材料。
2.根据权利要求1所述的活性炭纤维负载纳米二氧化钛薄膜复合光催化材料的制备方法，其特征在于表面活性剂为曲拉通X-100。
3.根据权利要求1的方法，其特征在于步骤(2)中先加入二乙醇胺后加入去离子水的滴加顺序。
4.根据权利要求1～3任一项的方法，其特征在于步骤(3)中二乙醇胺∶钛酸丁酯的摩尔比为1.2～3.4。
5.根据权利要求1～4任一项的方法，其特征在于活性炭纤维为不同厚度的活性炭纤维毡或活性炭纤维布，在所述制得的原位诱导反胶束溶液中浸泡5～20min和1～5次得到不同厚度的纳米二氧化钛薄膜。
6.根据权利要求5的方法，其特征在于在氮气氛围下升温速率为每分钟4～6℃至450～800℃并保温120min。
7.根据权利要求1～6任一项所述的活性炭纤维负载纳米二氧化钛薄膜的制备方法制备的TiO2/ACF复合光催化材料。
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