CN108380217A - 一种二氧化钛纳米片负载钛酸镍复合光催化剂的制备 - Google Patents
一种二氧化钛纳米片负载钛酸镍复合光催化剂的制备 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 36
- 239000002055 nanoplate Substances 0.000 title claims abstract description 33
- DGXKDBWJDQHNCI-UHFFFAOYSA-N dioxido(oxo)titanium nickel(2+) Chemical compound [Ni++].[O-][Ti]([O-])=O DGXKDBWJDQHNCI-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 title claims abstract description 12
- 239000011941 photocatalyst Substances 0.000 title abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 31
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 5
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229940078494 nickel acetate Drugs 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- XMOKRCSXICGIDD-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O XMOKRCSXICGIDD-UHFFFAOYSA-N 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 7
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- 238000011160 research Methods 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 239000002114 nanocomposite Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical group C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001045 blue dye Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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Abstract
本发明公开了一种二氧化钛纳米片负载钛酸镍复合光催化剂的制备方法及其在光催化降解污染物上的应用,属于材料制备及光催化的技术领域。该催化剂的特点有:具有二维的形貌特征,由二维结构的TiO2纳米片与钛酸镍纳米粒子复合而成。在制备光催化剂过程中,采用工艺简单的水热法和沉淀法,合成出二氧化钛纳米片负载钛酸镍复合光催化剂。在钛酸镍的作用下,二氧化钛纳米片负载钛酸镍复合光催化剂表现出良好的可见光吸收性能和光催化性能,促进了TiO2光催化剂的研究。
Description
技术领域
本发明属于材料的合成与光催化技术领域,主要涉及一种二氧化钛纳米片负载钛酸镍光催化剂的制备及其光电化学性质的研究。
背景技术
随着人们环境保护意识的增强,水污染的问题已受到越来越多的关注。传统的污水处理方法已经满足不了人们的要求。寻找出一种清洁,高效,节能环保的污水处理方法,成了人们研究的热点方向。
自1972年首次发现TiO2具有光催化活性以来,光催化技术的研究一直是材料领域的热点方向。光催化技术凭借其节能环保、无二次污染等优点为污水的处理提供了一个非常好的解决途径。半导体光催化材料可以利用取之不尽、用之不竭的太阳能处理空气中或者水中有毒有害物质,改善环境,达到资源利用生态化的目的。目前,各种不同的半导体光光催化剂材料被广泛研究,如ZnO,g-C3N4等,但是TiO2凭借其材料来源广泛,价格低廉,无生物毒性等优点成为光催化研究的主要材料,并且开发出多种产品应用于实际生活中。
但是, TiO2光催化剂也存在着一些缺陷,例如,其光响应范围较窄,只能被太阳光中的紫外光所激发;量子效率偏低,并且具有高的光生电子-空穴对复合速率,这些都阻碍了其进一步的发展与应用。在这种背景下,如何提高TiO2的光催化效率和拓宽其光相应范围,成了TiO2光催化剂的研究重点。近年来,利用其他材料与TiO2催化剂进行复合,制备复合光催化剂的研究取得了一定的进展,得到的TiO2基复合光催化剂在太阳光的照射下表现出良好的光催化活性。本发明利用钛酸镍半导体材料与TiO2纳米片进行复合,形成二维的微观结构,有效地提高了TiO2的可见光利用率和光催化活性。
发明内容
本发明的目的是制备出具有高的可见光利用率和高催化活性的TiO2基复合光催化剂,促进TiO2的实际应用。
为实现本发明目的采用如下技术方案:
利用钛酸镍高的光催化活性,与二氧化钛纳米片复合,制备出二氧化钛纳米片负载钛酸镍光催化剂。在钛酸镍和二氧化钛共同作用下,提高二氧化钛的可见光吸收性能和光催化活性。
一种二氧化钛纳米片负载钛酸镍光催化剂的制备,其特征步骤如下:
(1)称取一定量P25溶解在NaOH中,搅拌均匀;
(2)将上述溶液转移到反应釜中水热反应;
(3)步骤(2)中产物进行酸处理后,再经过500℃煅烧3h,得到二氧化钛纳米片;
(4)称取一定量的二氧化钛纳米片于30mL乙二醇溶液中,磁力搅拌均匀;
(5)向步骤(4)中加入一定量的乙酸镍,搅拌均匀;
(6)向步骤(5)溶液加入适量钛酸四丁酯,搅拌3h;
(7)向步骤(6)产物离心洗涤干燥,在600℃下煅烧2h,得到复合催化剂。
步骤(5)中乙酸镍的质量为0.0248 g。
步骤(6)中钛酸四丁酯为0.04mL。
步骤(6)中的离心清洗过程为先用乙醇清洗4次,再用去离子水清洗2次,离心速率8000rpm,时间7min。
所述二氧化钛纳米片负载钛酸镍光催化剂用于水溶液中有机污染物的可见光催化降解。
目标污染物为亚甲基蓝。
本发明具有如下优点:
1.本发明制备方法采用的是水热法和沉淀法,制备出二氧化钛纳米片负载钛酸镍光催化剂,具有新颖的显微结构。经透射电镜可发现该材料是由TiO2纳米片负载钛酸镍纳米粒子复合而成(图1);
2.本发明中的二氧化钛纳米片负载钛酸镍光催化剂具有良好的光催化活性,其催化活性在TiO2的基础上有了显著的提升。在90min人造可见光源的照射下降解亚甲基蓝染料,降解程度达到90%,是二氧化钛/钛酸镍催化活性的2倍 (图2)。
附图说明
图1为二氧化钛纳米片负载钛酸镍光催化剂的透射电镜图。
图2为二氧化钛纳米片负载钛酸镍光催化剂的光催化降解图。
具体实施方式
一种二氧化钛纳米片负载钛酸镍光催化剂的制备,其特征步骤如下:
(1)称取一定量P25溶解在NaOH中,搅拌均匀;
(2)将上述溶液转移到反应釜中水热反应;
(3)步骤(2)中产物进行酸处理后,再经过500℃煅烧3h,得到二氧化钛纳米片;
(4)称取一定量的二氧化钛纳米片于30mL乙二醇溶液中,磁力搅拌均匀;
(5)向步骤(4)中加入一定量的乙酸镍,搅拌均匀;
(6)向步骤(5)溶液加入适量钛酸四丁酯,搅拌3h;
(7)向步骤(6)产物离心洗涤干燥,在600℃下煅烧2h,得到复合催化剂。
步骤(5)中乙酸镍的质量为0.0248 g。
步骤(6)中钛酸四丁酯为0.04mL。
步骤(6)中的离心清洗过程为先用乙醇清洗4次,再用去离子水清洗2次,离心速率8000rpm,时间7min。
所述二氧化钛纳米片负载钛酸镍光催化剂用于水溶液中有机污染物的可见光催化降解。
下面例举实施例子制备二氧化钛纳米片负载钛酸镍光催化剂。
实施案例1
二氧化钛纳米片负载钛酸镍光催化剂的制备。
称取P25 1.0 g溶于20mol/L的NaOH溶液中;将溶液倒入反应釜中,加热,加热温度为130℃,时间为3h。反应完成后,将产物放入0.1mol/L的HCl溶液中浸泡24h,离心洗涤,干燥;再在管式炉中500℃ 煅烧3h,得到TiO2纳米片。
称取0.5 gTiO2纳米片,加入到30 mL乙二醇中,搅拌均匀;再加入0.0248g 乙酸镍,搅拌均匀;再加入0.04 mL钛酸四丁酯,搅拌3h。反应完成后,离心洗涤,先用乙醇清洗4次,在用水洗2次,离心速度为8000rpm,时间为7min。最后烘箱中60℃干燥。产物在600℃下煅烧2h,得到复合催化剂。
实施案例2
二氧化钛纳米片负载钛酸镍光催化剂在可见光照射下降解亚甲基蓝。
按实施案例1方法制得的二氧化钛纳米片负载钛酸镍光催化剂进行降解亚甲基蓝实验。亚甲基蓝溶液的浓度是2×10-6mol L-1;取复合材料粉体50mg,置于100mL上述亚甲基蓝溶液中,在暗室中搅拌50分钟,然后将溶液置于紫外光被过滤掉的可见光源中,每10分钟取5mL亚甲基蓝溶液,用紫外-可见分光光度计测出溶液中亚甲基蓝的特征峰值。
按实施案例2得到二氧化钛纳米片负载钛酸镍光催化剂可见光降解亚甲基蓝的降解曲线,见图2。从图2可以看出实施案例1制备的复合材料粉体在光照90min后催化降解达到90%以上,具有优异的光催化活性。
Claims (5)
1.一种二氧化钛纳米片负载钛酸镍光催化剂的制备,其特征包括以下步骤:
(1)称取一定量P25溶解在NaOH中,搅拌均匀;
(2)将上述溶液转移到反应釜中水热反应;
(3)步骤(2)中产物进行酸处理后,再经过500℃煅烧3h,得到二氧化钛纳米片;
(4)称取一定量的二氧化钛纳米片于30mL乙二醇溶液中,磁力搅拌均匀;
(5)向步骤(4)中加入一定量的乙酸镍,搅拌均匀;
(6)向步骤(5)溶液加入适量钛酸四丁酯,搅拌3h;
(7)向步骤(6)产物离心洗涤干燥,在600℃下煅烧2h,得到复合催化剂。
2.根据权利要求1一种二氧化钛纳米片负载钛酸镍光催化剂的制备,其特征在于NaOH浓度为20mol/L。
3.根据权利要求1一种二氧化钛纳米片负载钛酸镍光催化剂的制备,其特征在于乙酸镍质量0.0248g。
4.根据权利要求1一种二氧化钛纳米片负载钛酸镍光催化剂的制备,其特征在于钛酸四丁酯为0.04mL。
5.根据权利要求1一种二氧化钛纳米片负载钛酸镍光催化剂的制备,其特征在于复合催化剂的形貌结构为钛酸镍纳米粒子附着在二氧化钛纳米片表面。
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CN114684786A (zh) * | 2020-12-25 | 2022-07-01 | 江苏康润净化科技有限公司 | 一种基于钙钛矿二氧化钛异质结构高效制氢制氧的方法 |
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CN114684786A (zh) * | 2020-12-25 | 2022-07-01 | 江苏康润净化科技有限公司 | 一种基于钙钛矿二氧化钛异质结构高效制氢制氧的方法 |
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