CN107008334A - 一种光催化分解水制氢催化剂的改性方法 - Google Patents
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Abstract
一种光催化分解水制氢催化剂的改性方法，以低成本天然埃洛石纳米管（HNTs）为载体，以钛酸丁酯、硝酸镍、硝酸铁、硝酸铈为前驱物，在载体表面原位合成纳米二氧化钛（TiO2），然后经过浸渍、干燥、煅烧、氢还原等工序，在复合载体表面生成具有晶格缺陷的铁酸镍铈催化活性中心。本发明的优点是：该方法工艺简单，操作方便，成本低，光催化中心高度分散，催化剂活性高，光生电子复合率低，且催化剂具有抗烧结和坍塌特性。
Description
技术领域
本发明涉及一种光催化分解水制氢催化剂的改性方法。
背景技术
利用太阳光分解水制氢是未来解决能源危机的理想方法之一。与核能相比，太阳能更为安全；与水能、风能相比，太阳能利用的成本较低，而且不受地理条件的限制。日本学者Fujishima和Honda自上世纪六十年代末对光照n-型半导体TiO2电极导致水的分解从而产生氢气这一现象的发现，揭示了利用太阳能分解水制氢的可能性。TiO2由于其良好的化学稳定性，抗磨损性和无毒等特点，成为半导体光催化领域的主要研究对象之一。但是常规制备的TiO2存在着晶粒尺寸大，比表面积小以及低分散性等缺点，而且TiO2光催化剂中的大部分仅能吸收只占太阳光总能3 %～5 %的紫外线，研究和制备对太阳光高效吸收和转化的光解水催化剂成为太阳能半导体光解水制氢技术发展的关键因素。
发明内容
本发明的目的是针对上述存在问题，提供一种光催化分解水制氢催化剂的改性方法，该方法工艺简单，操作方便，成本低，光催化中心高度分散，催化剂活性高，光生电子复合率低，且催化剂具有抗烧结和坍塌特性。
本发明的技术方案：一种光催化分解水制氢催化剂的改性方法，以低成本天然埃洛石纳米管（HNTs）为载体，以钛酸丁酯、硝酸镍、硝酸铁、硝酸铈为前驱物，在载体表面原位合成纳米二氧化钛（TiO2），然后经过浸渍、干燥、煅烧、氢还原等工序，在复合载体表面生成具有晶格缺陷的铁酸镍铈催化活性中心，具体包括如下步骤：（1）将天然埃洛石纳米管除铁后，置于乙醇与水的混合溶液；（2）将一定量钛酸丁酯溶于乙醇溶液，磁力搅拌下加入（1）中溶液，继续搅拌，然后过滤、干燥，即在埃洛石表面生成锐钛矿型纳米二氧化钛；（3）将（2）中所得埃洛石/二氧化钛复合粉末置于硝酸镍、硝酸铁和硝酸铈混合溶液中浸渍，然后干燥、煅烧，最后氢气还原，即得CeO2-NiFe2O4/TiO2-HNTs。
所述煅烧温度500～800℃。
所述氢气还原温度200～500℃，氢气浓度5%～10%，稀释气为氮气。
所述催化活性中心成分为CeO2-NiFe2O4/TiO2。
所述催化组分为CeO2-NiFe2O4/TiO2-HNTs，其中单质Ni含量为0.1%～10%，NiFe2O4的含量为1%～15%，CeO2的含量为0.1%～5%，TiO2的含量为1%～25%。
本发明的优点是：埃洛石纳米管价格低廉，具有长径比高的尺寸优势，可高度分散催化中心，防止催化剂烧结和结构坍塌；锐钛型二氧化钛具有结构稳定和光催化活性，尖晶石型铁酸镍具有协同二氧化钛具有结构稳定和光催化活性；单质镍具有解离氢键的催化作用，促进水解制氢活性；氧化铈具有提高晶格氧传递效率作用，且破坏尖晶石铁酸镍的完美晶体结构，提高催化活性。
具体实施方式
下面结合实施例对本发明进一步说明，但是它们并不是对本发明作任何限制。这里仅指出，本发明中使用的试剂和测试设备除特别标明出处之外，均为市售的通用产品。
实施例1。
一种光催化分解水制氢催化剂的改性方法，包括如下步骤：（1）将3.0 g天然埃洛石纳米管酸洗，再水洗至中性，置于200 ml体积比为1：1的乙醇与水混合溶液，并用2%稀硝酸调pH为4左右；（2）将15 ml钛酸丁酯溶于20 ml乙醇溶液，磁力搅拌下加入（1）中溶液，连续搅拌3 h后，80℃干燥24 h，即在埃洛石表面生成锐钛矿型纳米二氧化钛；（3）然后将（2）中所得埃洛石/二氧化钛复合粉末置于浓度均为1.5%的硝酸镍、硝酸铁和1.0%硝酸铈混合溶液中浸渍6 h，然后80℃干燥6 h，再500℃煅烧6 h，最后2%氢气500℃还原3 h，即得CeO2-NiFe2O4/TiO2-HNTs，其中单质Ni含量为0.4%，NiFe2O4的含量为3.8%，CeO2的含量为0.9%，TiO2的含量为20.2%。
实施例2。
一种光催化分解水制氢催化剂的改性方法，包括如下步骤：（1）将3.0 g天然埃洛石纳米管酸洗，再水洗至中性，置于200 ml体积比为1：1的乙醇与水混合溶液，并用2%稀硝酸调pH为4左右；（2）将20 ml钛酸丁酯溶于20 ml乙醇溶液，磁力搅拌下加入（1）中溶液，连续搅拌3 h后，80℃干燥24 h，即在埃洛石表面生成锐钛矿型纳米二氧化钛；（3）然后将（2）中所得埃洛石/二氧化钛复合粉末置于浓度均为2.5%的硝酸镍、硝酸铁和1.5%硝酸铈混合溶液中浸渍6 h，然后80℃干燥6 h，再800℃煅烧6 h，最后5%氢气300℃还原3 h，即得CeO2-NiFe2O4/TiO2-HNTs，其中单质Ni含量为1.2%，NiFe2O4的含量为2.9%，CeO2的含量为1.3%，TiO2的含量为19.3%。
实施例3。
一种光催化分解水制氢催化剂的改性方法，包括如下步骤：（1）将3.0 g天然埃洛石纳米管酸洗，再水洗至中性，置于200 mL体积比为1:1的乙醇与水混合溶液，并用2%稀硝酸调pH为4左右；（2）将5 ml钛酸丁酯溶于20 mL乙醇溶液，磁力搅拌下加入（1）中溶液，连续搅拌3 h后，80℃干燥24 h，即在埃洛石表面生成锐钛矿型纳米二氧化钛；（3）然后将（2）中所得埃洛石/二氧化钛复合粉末置于浓度均为1.5%的硝酸镍、硝酸铁和0.5%硝酸铈混合溶液中浸渍6 h，然后80℃干燥6 h，再700℃煅烧6 h，最后2%氢气400℃还原3 h，即得CeO2-NiFe2O4/TiO2-HNTs，其中单质Ni含量为0.8%，NiFe2O4的含量为5%，CeO2的含量为0.5%，TiO2的含量为12.5%。
本发明公开一种光催化分解水制氢催化剂的改性方法，本领域技术人员可通过借鉴本文内容，适当改变工艺路线等环节实现，尽管本发明的方法已通过较佳实施例子进行了描述，相关技术人员明显能在不脱离本发明内容与范围内对本文所述的方法进行改动或重新组合，来实现最终结果。特别需要指出的是，所有相类似的替换和改动对本领域技术人员来说是显而易见的，它们都被视为包括在本发明的内容和范围。
Claims (5)
1.一种光催化分解水制氢催化剂的改性方法，其特征在于：以低成本天然埃洛石纳米管（HNTs）为载体，以钛酸丁酯、硝酸镍、硝酸铁、硝酸铈为前驱物，在载体表面原位合成纳米二氧化钛（TiO2），然后经过浸渍、干燥、煅烧、氢还原等工序，在复合载体表面生成具有晶格缺陷的铁酸镍铈催化活性中心，具体包括如下步骤：（1）将天然埃洛石纳米管除铁后，置于乙醇与水的混合溶液；（2）将一定量钛酸丁酯溶于乙醇溶液，磁力搅拌下加入（1）中溶液，继续搅拌，然后过滤、干燥，即在埃洛石表面生成锐钛矿型纳米二氧化钛；（3）将（2）中所得埃洛石/二氧化钛复合粉末置于硝酸镍、硝酸铁和硝酸铈混合溶液中浸渍，然后干燥、煅烧，最后氢气还原，即得CeO2-NiFe2O4/TiO2-HNTs。
2.根据权利要求1所述一种光催化分解水制氢催化剂的改性方法，其特征在于：所述煅烧温度500～800℃。
3.根据权利要求1所述一种光催化分解水制氢催化剂的改性方法，其特征在于：所述氢气还原温度200～500℃，氢气浓度5～10%，稀释气为氮气。
4.根据权利要求1所述一种光催化分解水制氢催化剂的改性方法，其特征在于：所述催化活性中心成分为CeO2-NiFe2O4/TiO2。
5.根据权利要求1所述一种光催化分解水制氢催化剂的改性方法，其特征在于：所述催化组分为CeO2-NiFe2O4/TiO2-HNTs，其中单质Ni含量为0.1%～10%，NiFe2O4的含量为1%～15%，CeO2的含量为0.1%～5%，TiO2的含量为1%～25%。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107837802A (zh) * | 2017-11-03 | 2018-03-27 | 盛槿滺 | 一种复合光催化剂及其制备方法 |
| CN110479286A (zh) * | 2019-09-09 | 2019-11-22 | 井冈山大学 | 一种钛铁镍高析氢活性电催化剂的制备方法 |
| CN113786825A (zh) * | 2021-09-10 | 2021-12-14 | 蚌埠学院 | 一种纳米铁酸镍/钛酸锌改性微孔氧化硅、制备方法及其应用 |
| CN115151340A (zh) * | 2020-02-28 | 2022-10-04 | 杰富意矿物股份有限公司 | 复合体 |
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2016
- 2016-01-28 CN CN201610055835.6A patent/CN107008334A/zh active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107837802A (zh) * | 2017-11-03 | 2018-03-27 | 盛槿滺 | 一种复合光催化剂及其制备方法 |
| CN110479286A (zh) * | 2019-09-09 | 2019-11-22 | 井冈山大学 | 一种钛铁镍高析氢活性电催化剂的制备方法 |
| CN110479286B (zh) * | 2019-09-09 | 2022-03-08 | 井冈山大学 | 一种钛铁镍高析氢活性电催化剂的制备方法 |
| CN115151340A (zh) * | 2020-02-28 | 2022-10-04 | 杰富意矿物股份有限公司 | 复合体 |
| CN113786825A (zh) * | 2021-09-10 | 2021-12-14 | 蚌埠学院 | 一种纳米铁酸镍/钛酸锌改性微孔氧化硅、制备方法及其应用 |
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