CN112774703A - 一种高效光催化分解水制氢的单质红磷负载的二氧化钛复合催化剂 - Google Patents
一种高效光催化分解水制氢的单质红磷负载的二氧化钛复合催化剂 Download PDFInfo
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Abstract
一种高效光催化分解水制氢的单质红磷负载的二氧化钛复合催化剂，属于催化化学与纳米科学领域。首先以异丙醇钛(TIP)为前驱体，以乙醇为溶剂，用溶胶‑凝胶法和水热法制备了介孔TiO2微球载体；然后利用化学气相沉积法将RP纳米棒沉积在TiO2表面，得到RP/TiO2复合催化剂。本发明材料新颖，制备工艺简单，产物粒子形貌规整可控，所得RP/TiO2催化剂表现出良好的优异的可见光光催化分解水制氢活性和稳定性。
Description
技术领域
本发明涉及一种高效光催化分解水制氢的单质红磷(RP)负载的二氧化钛(TiO2)复合催化剂(RP/TiO2)。本发明首先以溶胶-凝胶法和水热法制备了介孔TiO2微球载体，然后利用化学气相沉积法(CVD)将不同含量的纤维晶型的RP单质负载在TiO2载体表面，得到了一系列x wt％RP/TiO2(x＝20，25，35)复合催化剂。最终，在可见光照射下，25RP/TiO2表现出最好的光催化水分解制氢活性和稳定性。属于催化化学与纳米科学领域。
背景技术
氢能具有可循环再生以及对环境友好等优点，被认为是一种可取代传统矿石能源的理想新能源。如何无毒、高效、低成本的制备氢气已成为人们研究的热点问题。在众多制氢方案中，半导体光催化水分解技术被认为是经济、环保、解决能源和环境问题的最佳途径之一。
TiO2是众多光催化材料中最经典的半导体光催化剂，具有氧化能力强、化学惰性强、成本低、稳定性高的优点，被广泛应用于光分解水制氢、光降解污染物、大气净化、杀菌消毒等领域。然而TiO2具有较大的禁带宽度(约3.2eV)，只对紫外光有响应。同时，其较高的光生电子-空穴对复合率也极大制约了其光催化活性。因此，需要对TiO2进行改性研究，从而提高其可见光吸收性能和整体活性。
新型RP单质光催化剂具备可调节的禁带宽度以及较宽的可见光吸收范围等优点，是目前单质光催化剂中光催化水分解制氢活性最高的材料。同时，RP也被广泛的作为一种有效的助催化剂与其它半导体材料复合，从而提高材料整体的光吸收性能和光催化活性。本课题组在前期的工作中已成功采用CVD法合成了RP负载g-C3N4复合材料(Adv.Funct.Mater.2017,27,1703484)。该研究表明，RP的负载可以弥补g-C3N4的结构缺陷，抑制了g-C3N4中光生电荷的自我捕获，实现了电荷的有效分离和转移，显著延长了g-C3N4中活性电荷的寿命。同时，RP的负载显著提高了复合材料对可见光的吸收，使其在可见光照射下表现出优良的、稳定的光催化制氢活性。因此，将RP与宽禁带TiO2结合形成异质结，是一个能够有效改善TiO2光吸收范围，促进光生电荷的分离和转移，抑制电荷复合率，从而充分提高其光催化活性的可行策略。
因此，本发明首先以溶胶-凝胶法和水热法制备了介孔TiO2微球载体，然后利用CVD法成功制备了一系列不同纤维晶型RP负载量的x wt％RP/TiO2(x＝20，25，35)复合催化剂。据我们所知，目前尚无关于此类纤维晶型单质RP负载的TiO2微球复合催化剂的制备及其应用于光催化分解水制氢的报道。本发明公开了此类RP/TiO2复合催化剂的可控制备方法，研究发现25RP/TiO2复合催化剂具有最优良的可见光催化活性和稳定性能。
发明内容
本发明的目的在于，利用CVD法实现RP/TiO2复合催化剂的可控制备，并应用于高效的光催化分解水制氢。该光催化剂的特征在于，TiO2的形貌为粒径均匀的微球(直径约为1μm)，表面有介孔，且被纤维晶型的RP纳米棒均匀包裹。
所述RP/TiO2复合催化剂的制备方法包括以下步骤：
(1)采用溶胶-凝胶法制备非晶态TiO2微球。
(2)将制备的非晶态TiO2微球水热处理得锐钛矿TiO2微球。
(3)利用CVD法制备单质RP负载的锐钛矿TiO2复合催化剂RP/TiO2：
(i)对商业RP进行水热处理，去除表面含氧基团和杂质；
(ii)将TiO2、RP和碘加入到石英安瓿瓶中，抽真空并用乙炔火焰密封。其中，原料TiO2与碘的质量比为100:(0.5-1.5)，RP根据负载量调节；
(iii)在管式炉中对样品进行600℃高温煅烧4h；
(iv)以1℃/min的速率冷却到280℃，保温4h，接着以0.2℃/min的速率缓慢冷却至室温；
(v)将所制备的样品用CS2、蒸馏水和乙醇洗涤、干燥，最终得到x wt％RP/TiO2复合催化剂，x＝20-35。
本发明所得RP/TiO2复合催化剂的光催化分解水制氢性能评价的具体步骤如下：将20mg催化剂分散在50mL的水中其中10vol％甲醇作为空穴牺牲剂，以2wt％Pt为助催化剂；光催化水分解制氢的实验是在密闭的石英反应器中进行的；采用装有L40截止滤波片的300W氙灯作为可见光光源，用GC7920气相色谱仪测定了光催化反应产生的氢气含量。
本发明具有制备工艺简单、原料价格便宜、产量较高且产物粒子形貌规整及晶体结构可控等特征。本发明制得到的一系列x wt％RP/TiO2(x＝20，25，35)复合催化剂在可见光照射下均表现出优异的光催化制氢性能。其中活性最好的催化剂为25wt％RP/TiO2，可见光照射下的产氢速率可以达到681μmol h-1g-1，是纯RP的32倍，是纯TiO2的681倍。连续进行20小时的光催化水分解制氢性能测试，该催化剂的活性没有明显下降，表现出了良好的稳定性。
附图说明
图1为所制得催化剂的XRD谱图。其中曲线(a)、(b)、(c)、(d)、(e)分别为经过CVD过程后，TiO2、20RP/TiO2、25RP/TiO2、35RP/TiO2、和RP催化剂的广角XRD谱图。
图2为所制得催化剂的TEM照片。图中依次为(a)TiO2、(b)20RP0.19/TiO2、(c)25RP0.25/TiO2、(d)35RP/TiO2的TEM照片。
图3为在可见光照射下所制备的催化剂水分解制氢活性图。
图4为在可见光照射下25RP/TiO2催化剂水分解制氢活性图(解释一下图4)。
具体实施方式
为了进一步阐述本发明，下面以实施例作详细说明，并给出附图描述本发明得到的各催化剂材料。
实施例1：非晶态TiO2微球的合成。称取0.662g十六胺(HDA)溶于100mL乙醇中，加入0.40mL KCl溶液(0.1M)；室温下，在剧烈搅拌下将2.2mL的异丙醇钛(TIP)缓慢加入上述溶液中，静置18h后得到白色TiO2悬浮液；然后过滤收集样品，用乙醇洗涤，干燥，得到非晶态TiO2微球。
实施例2：介孔锐钛矿TiO2微球的合成。具体过程为：将1.6g非晶态TiO2微球分散到20mL乙醇和10mL去离子水的混合溶液中；将混合物密封在聚四氟乙烯内衬的高压釜(50mL)中；在160℃下加热16h；过滤收集沉淀，用乙醇洗涤，室温下干燥得到介孔锐钛矿TiO2微球(图2中a)。
实施例3：采用CVD法制备了RP/TiO2复合材料。商业RP首先进行水热处理备用。将300mg TiO2、3mg碘和一定量纯化后的RP添加到石英安瓿瓶中，抽真空并用乙炔火焰密封；在管式炉中对样品进行600℃高温煅烧4h，加热速度为2℃/min；然后以1℃/min的速率冷却到280℃，保温4h，接着以0.2℃/min的速率缓慢冷却至室温；将所制备的样品用CS2、蒸馏水和乙醇洗涤，得到不同RP含量的样品x wt％RP/TiO2(x＝20，25，35)复合催化剂(图2中b-d)。
本发明具有制备工艺简单，原料价格便宜，产物粒子形貌规整可控等特点，本发明制得的25RP/TiO2，表现出了优异的可见光光催化分解水制氢活性。
Claims (6)
1.一种高效光催化分解水制氢的单质红磷负载的二氧化钛复合催化剂，其特征在于，单质红磷RP沉积在TiO2表面形成异质结，形成一系列x wt％RP/TiO2复合催化剂，x＝20-35。
2.按照权利要求1所述的一种高效光催化分解水制氢的单质红磷负载的二氧化钛复合催化剂，其特征在于，TiO2为锐钛矿，TiO2的形貌为粒径均匀的微球，表面有介孔，且被纤维晶型的RP纳米棒均匀包裹。
3.(按照权利要求1所述的一种高效光催化分解水制氢的单质红磷负载的二氧化钛复合催化剂，其特征在于，TiO2的直径为1μm。
4.权利要求1-3任一项所述的一种高效光催化分解水制氢的单质红磷负载的二氧化钛复合催化剂的制备方法，其特征在于，包括以下步骤：
(1)采用溶胶-凝胶法制备了非晶态TiO2微球；
(2)将制备的非晶态TiO2微球水热处理得锐钛矿TiO2微球；
(3)采用化学气相沉积法制备了单质RP负载的锐钛矿TiO2复合催化剂RP/TiO2；
(i)对RP进行水热处理，去除表面含氧基团和杂质；
(ii)将TiO2、RP和碘加入到石英安瓿瓶中，抽真空并用乙炔火焰密封。其中，原料TiO2与碘的质量比为100:(0.5-1.5)，RP根据负载量调节；
(iii)在管式炉中对样品进行600℃高温煅烧4h；
(iv)以1℃/min的速率冷却到280℃，保温4h，接着以0.2℃/min的速率缓慢冷却至室温；
(v)将所制备的样品用CS2、蒸馏水和乙醇洗涤、干燥，最终得到x wt％RP/TiO2复合催化剂，x＝20-35。
5.权利要求1-3任一项所述的一种高效光催化分解水制氢的单质红磷负载的二氧化钛复合催化剂的应用，用于光催化分解水制备氢气。
6.权利要求5所述的应用，具体步骤：将20mg催化剂分散在50mL的水中，其中含有10vol％甲醇作为空穴牺牲剂，以2wt％Pt为助催化剂；光催化水分解制氢的实验是在密闭的石英反应器中进行的；采用装有L40截止滤波片的300W氙灯作为可见光光源。
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