CN108479822A - 一种磷酸锑微球负载二氧化钛复合光催化剂的制备 - Google Patents
一种磷酸锑微球负载二氧化钛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 74
- WOJYMMRSNJJSRF-UHFFFAOYSA-N [Sb].P(O)(O)(O)=O Chemical compound [Sb].P(O)(O)(O)=O WOJYMMRSNJJSRF-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 33
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 32
- 239000011806 microball Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000007836 KH2PO4 Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 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
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 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 1
- 239000004005 microsphere Substances 0.000 claims 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 5
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 7
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical group [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 7
- 229940012189 methyl orange Drugs 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
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- 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
- 238000012545 processing Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 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
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- 150000002148 esters Chemical class 0.000 description 1
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- 238000010438 heat treatment Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 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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- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
本发明公开了一种磷酸锑微球负载二氧化钛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:具有三维的形貌特征,由三维结构的磷酸锑微球与二氧化钛纳米粒子复合而成。在制备光催化剂过程中,采用工艺简单的溶剂热法合成出磷酸锑微球负载二氧化钛复合光催化剂。在磷酸锑的作用下,磷酸锑微球负载二氧化钛复合光催化剂表现出良好的光催化性能,促进了TiO2光催化剂的研究。
Description
技术领域
本发明属于材料制备及光催化技术领域,具体涉及一种磷酸锑微球负载二氧化钛复合光催化剂的制备及光催化活性的研究。
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。本发明利用磷酸锑半导体材料与TiO2带进行复合,形成三维的微观结构,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:
利用磷酸锑半导体材料较低的禁带宽度,高的可见光吸收性,通过水热反应,制备出磷酸锑,然后在磷酸锑的表面进行二氧化钛纳米粒子的修饰,制备出磷酸锑微球负载二氧化钛复合光催化剂。在磷酸锑的作用下,提高二氧化钛的可见光催化活性。
一种磷酸锑微球负载二氧化钛复合光催化剂的制备,其特征步骤如下:
(1)称取一定量SbCl3溶解在去离子水中,搅拌均匀;
(2)称取一定量的KH2PO4于水溶液中,磁力搅拌均匀;
(3)向步骤(1)、(2)溶液混合,再加入25 mL油酸,搅拌均匀;
(4)将步骤(3)溶液放入高压反应釜中,进行水热反应。将反应完全的样品离心洗涤,干燥后研磨即得到磷酸锑;
(5)称取步骤(4)制得的磷酸锑0.05g,加入到乙醇溶液中,搅拌均匀;
(6)量取一定量钛酸四丁酯加到步骤(5)溶液中,搅拌24h。将反应完全的样品离心洗涤,干燥后研磨即得到磷酸锑微球负载二氧化钛复合光催化剂。
步骤(1)中SbCl3质量为1.1406 g。
步骤(2)中KH2PO4质量0.68045 g。
步骤(4)中反应温度为160℃,反应时间为8h。
步骤(4)中二氧化钛带的质量为0.2g。
步骤(6)中钛酸四丁酯为0.05 mL。
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。
所述磷酸锑微球负载二氧化钛复合光催化剂用于水溶液中有机污染物的可见光催化降解。
目标污染物为甲基橙。
本发明具有如下优点:
1.本发明采用溶剂热法制备出磷酸锑微球,是首次报道该结果;
2.本发明制备的是磷酸锑微球负载二氧化钛复合光催化剂,属于新的复合体系;
3.本发明中的磷酸锑微球负载二氧化钛复合光催化剂具有良好的光催化活性,在90min可见光照射下降解甲基橙染料达90%,比已研究的二氧化钛催化剂的活性提高了20倍。
附图说明
图1为磷酸锑微球负载二氧化钛复合光催化剂的扫描电镜图。
图2为磷酸锑微球负载二氧化钛复合光催化剂的光催化降解图。
具体实施方式
一种磷酸锑微球负载二氧化钛复合光催化剂的制备,其特征步骤如下:
(1)称取一定量SbCl3溶解在去离子水中,搅拌均匀;
(2)称取一定量的KH2PO4于水溶液中,磁力搅拌均匀;
(3)向步骤(1)、(2)溶液混合,再加入25 mL油酸,搅拌均匀;
(4)将步骤(3)溶液放入高压反应釜中,进行水热反应。将反应完全的样品离心洗涤,干燥后研磨即得到磷酸锑;
(5)称取步骤(4)制得的磷酸锑0.05g,加入到乙醇溶液中,搅拌均匀;
(6)量取一定量钛酸四丁酯加到步骤(5)溶液中,搅拌24h。将反应完全的样品离心洗涤,干燥后研磨即得到磷酸锑微球负载二氧化钛复合光催化剂。
步骤(1)中SbCl3质量为1.1406 g。
步骤(2)中KH2PO4质量0.68045 g。
步骤(4)中反应温度为160℃,反应时间为8h。
步骤(6)中钛酸四丁酯为0.05 mL。
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。
所述磷酸锑微球负载二氧化钛复合光催化剂用于水溶液中有机污染物的可见光催化降解。
下面具体的实施例子制备磷酸锑微球负载二氧化钛复合光催化剂。
实施案例1
磷酸锑微球负载二氧化钛复合光催化剂的制备。
称取SbCl3 1.1406 g溶于25 mL水中;称取0.68045g KH2PO4溶于25 mL水中;将上述两溶液混合后加入25 mL油酸;然后将溶液倒入反应釜中,加热,加热温度为160℃,时间为8h。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,研磨即得到磷酸锑微球。
称取0.05 g磷酸锑,加入到10 mL乙醇溶液中,搅拌均匀;再加入0.05 mL钛酸四丁酯,搅拌24h。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,研磨即得到磷酸锑微球负载二氧化钛复合光催化剂。
实施案例2
磷酸锑微球负载二氧化钛复合光催化剂在可见光照射下降解甲基橙。
按实施案例1方法制得的磷酸锑微球负载二氧化钛复合光催化剂进行降解甲基橙实验。甲基橙溶液的浓度是1×10-6mol L-1;取复合材料粉体50mg,置于100mL上述罗丹明B溶液中,在暗室中搅拌60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甲基橙溶液,用紫外-可见分光光度计测出溶液中甲基橙的特征峰值。
按实施案例2得到磷酸锑微球负载二氧化钛复合光催化剂可见光降解甲基橙的降解曲线,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%。
Claims (6)
1.一种磷酸锑微球负载二氧化钛复合光催化剂的制备,其特征包括以下步骤:
(1)称取一定量SbCl3溶解在去离子水中,搅拌均匀;
(2)称取一定量的KH2PO4于水溶液中,磁力搅拌均匀;
(3)向步骤(1)、(2)溶液混合,再加入25 mL油酸,搅拌均匀;将步骤(3)溶液放入高压反应釜中,进行水热反应;
(4)将反应完全的样品离心洗涤,干燥后研磨即得到磷酸锑;
(5)称取步骤(4)制得的磷酸锑0.05g,加入到乙醇溶液中,搅拌均匀;
量取一定量钛酸四丁酯加到步骤(5)溶液中,搅拌24h;
(6)将反应完全的样品离心洗涤,干燥后研磨即得到磷酸锑微球负载二氧化钛复合光催化剂。
2.根据权利要求1一种磷酸锑微球负载二氧化钛复合光催化剂的制备,其特征在于SbCl3质量为1.1406 g。
3.根据权利要求1一种磷酸锑微球负载二氧化钛复合光催化剂的制备,其特征在于KH2PO4质量0.68045 g。
4.根据权利要求1一种磷酸锑微球负载二氧化钛复合光催化剂的制备,其特征在于溶剂热反应温度为160℃,反应时间为8h。
5.根据权利要求1一种磷酸锑微球负载二氧化钛复合光催化剂的制备,其特征在于钛酸四丁酯为0.05mL。
6.根据权利要求1一种磷酸锑微球负载二氧化钛复合光催化剂的制备,其特征在利用磷酸锑微球改性二氧化钛,制备复合光催化剂。
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CN116102916A (zh) * | 2021-09-16 | 2023-05-12 | 长沙民德消防工程涂料有限公司 | 氧化铟锡/二氧化钛复合材料及其制备方法、车用玻璃隔热涂料及其制备方法 |
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CN116102916A (zh) * | 2021-09-16 | 2023-05-12 | 长沙民德消防工程涂料有限公司 | 氧化铟锡/二氧化钛复合材料及其制备方法、车用玻璃隔热涂料及其制备方法 |
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