CN111330628A - 一种多元素共掺杂纳米二氧化钛光催化材料 - Google Patents
一种多元素共掺杂纳米二氧化钛光催化材料 Download PDFInfo
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 title claims abstract description 29
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 15
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical class O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052802 copper Inorganic materials 0.000 claims abstract description 10
- 239000010949 copper Substances 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 7
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 7
- 239000011701 zinc Substances 0.000 claims abstract description 7
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 4
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 4
- 239000011591 potassium Substances 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000002243 precursor Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000006255 coating slurry Substances 0.000 claims description 6
- 239000005543 nano-size silicon particle Substances 0.000 claims description 6
- 239000011941 photocatalyst Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
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- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 235000019738 Limestone Nutrition 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 239000004111 Potassium silicate Substances 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 2
- 239000010428 baryte Substances 0.000 claims description 2
- 229910052601 baryte Inorganic materials 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 239000001506 calcium phosphate Substances 0.000 claims description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 2
- 235000011010 calcium phosphates Nutrition 0.000 claims description 2
- 239000000378 calcium silicate Substances 0.000 claims description 2
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 2
- 230000003750 conditioning effect Effects 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 239000010440 gypsum Substances 0.000 claims description 2
- 229910052602 gypsum Inorganic materials 0.000 claims description 2
- 239000001023 inorganic pigment Substances 0.000 claims description 2
- 239000006028 limestone Substances 0.000 claims description 2
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052912 lithium silicate Inorganic materials 0.000 claims description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000391 magnesium silicate Substances 0.000 claims description 2
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 2
- 235000019792 magnesium silicate Nutrition 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- -1 sericite Substances 0.000 claims description 2
- 150000004760 silicates Chemical class 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 238000007711 solidification Methods 0.000 claims description 2
- 230000008023 solidification Effects 0.000 claims description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 230000001954 sterilising effect Effects 0.000 abstract description 8
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
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- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 231100000956 nontoxicity Toxicity 0.000 description 1
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- 231100000719 pollutant Toxicity 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
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- 150000003568 thioethers Chemical class 0.000 description 1
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Abstract
本发明提供一种多元素共掺杂纳米二氧化钛光催化材料，其特征在于：包括以下步骤：以改性沸石为载体，以摩尔分数计，氮的掺杂量为1％，镧的掺杂量为1.5％，钾的掺杂量为1％，锌的掺杂量为1％，铋的掺杂量为1％，铜的掺杂量为2％，改性沸石载体占催化剂的质量含量为60％能够显著提高纳米二氧化钛的光催化效率，加快二氧化钛催化降污效果，同时银的加入使本材料具有杀菌的功能，使材料具有高效无污染的抗菌杀菌和降解空气中有机污染物的功能。
Description
技术领域
本发明是一种多元素共掺杂纳米二氧化钛光催化材料，属于光催化去污技术领域。
背景技术
光催化主要分为环境光催化与能源光催化两大类。环境光催化主要涉及杀菌、消毒、光降解、自洁净等方面，其中已有相当数量的技术实现了商品化。能源光催化主要研究光催化分解水制氢能，光催化分解可再生资源制氢能等。随着近代温室效应，化石燃料枯竭，能源危机等各种问题的日益突出，光解水制氢能逐渐成为本领域的研究热点。目前已知的光催化材料有氧化物、硫化物、氮化物、钛酸盐、钽酸盐、钨酸盐和铌酸盐等。其中，二氧化钛半导体因其廉价易得、无毒稳定等众多优势，被认为是最具有应用潜力的光催化材料。
用于净化的二氧化钛光催化材料制备方法，将纳米二氧化钛、纳米二氧化硅、纳米银、纳米氧化铁起来结合制得一种新型的光催化剂，能够显著提高纳米二氧化钛的光催化效率，现有的二氧化钛在光催化中存在没有杀菌和净化功能的缺点，现在急需一种多元素共掺杂纳米二氧化钛光催化材料来解决上述出现的问题。
发明内容
针对现有技术存在的不足，本发明目的是提供一种多元素共掺杂纳米二氧化钛光催化材料，以解决上述背景技术中提出的问题。
为了实现上述目的，本发明是通过如下的技术方案来实现：一种多元素共掺杂纳米二氧化钛光催化材料，包括以下步骤：
(1)以改性沸石为载体，以摩尔分数计，氮的掺杂量为1％，镧的掺杂量为1.5％，钾的掺杂量为1％，锌的掺杂量为1％，铋的掺杂量为1％，铜的掺杂量为2％，改性沸石载体占催化剂的质量含量为60％；(2)将氮掺杂前驱体、镧掺杂前驱体、钾掺杂前驱体、锌掺杂前驱体、铋的前驱体和铜掺杂前驱体的无水乙醇溶液加入反应器中，用硝酸调整pH为2，搅匀；然后搅拌下滴加钛酸四丁酯的无水乙醇溶液，室温搅拌12小时进行水解，得到掺杂的二氧化钛溶胶；将改性沸石载体浸于掺杂的二氧化钛溶胶中60min，然后在120℃烘干12小时得到干凝胶；将所得干凝胶在炉内焙烧，以8℃/min的升温速率从室温升至300℃，保持50min；然后以8℃/min的升温速率升温至600℃，保持2h；再以8℃/min的升温速率升温至900℃，保持3h；冷却至室温，得到氮、镧、铜、锌、铜共掺杂的纳米二氧化钛光催化剂；(3)将原料放入搅拌机中均匀搅拌30min，制得涂料浆体；(4)将步骤2中的光催化抗菌粉体加入到步骤(3)中的涂料浆体之中，于40°搅拌2h，制得光催化材料；(5)所述原料的质量份数比为纳米二氧化钛：纳米二氧化硅：纳米银：纳米氧化铁：硅酸盐：石膏粉：钛白粉：粉末抗结剂：固化调理剂：无机颜料：填料：水＝5:15：1:0.5:30:5:10:1:5：5:5:50。
进一步地，所述硅酸盐取自硅酸钠、硅酸钾、硅酸锂、硅酸钙、硅酸镁或硅酸铝中的任意一种或几种的混合物。
进一步地，所述粉末抗结剂取自氧化镁、滑石粉、超细二氧化硅或轻质碳酸钙中的任意一种或几种的混合物。
进一步地，所述固化调理剂为缩合磷酸盐或铵盐的任意一种或混合物。
进一步地，所述填料取自石灰石、重晶石、氧化锌、绢云母、石英或磷酸钙中的任意一种或几种的混合物。
本发明的有益效果：本发明用于净化的二氧化钛光催化材料制备方法，将纳米二氧化钛、纳米二氧化硅、纳米银、纳米氧化铁起来结合制得一种新型的光催化剂，能够显著提高纳米二氧化钛的光催化效率，加快二氧化钛催化降污效果，同时银的加入使本材料具有杀菌的功能，使材料具有高效无污染的抗菌杀菌和降解空气中有机污染物的功能；同时掺杂稀土元素、多种金属元素以及氮，所得纳米二氧化钛光催化材料具有良好的光催化性能，同时所制备材料为均匀的细颗粒，在液相中容易分离，容易回收利用，对污染物呈现出较好的光降解效果，具有良好的应用潜力。
具体实施方式
为使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施方式，进一步阐述本发明。
本发明提供一种技术方案：一种多元素共掺杂纳米二氧化钛光催化材料，其特征在于：包括以下步骤：
(1)以改性沸石为载体，以摩尔分数计，氮的掺杂量为1％，镧的掺杂量为1.5％，钾的掺杂量为1％，锌的掺杂量为1％，铋的掺杂量为1％，铜的掺杂量为2％，改性沸石载体占催化剂的质量含量为60％；
(2)将氮掺杂前驱体、镧掺杂前驱体、钾掺杂前驱体、锌掺杂前驱体、铋的前驱体和铜掺杂前驱体的无水乙醇溶液加入反应器中，用硝酸调整pH为2，搅匀；然后搅拌下滴加钛酸四丁酯的无水乙醇溶液，室温搅拌12小时进行水解，得到掺杂的二氧化钛溶胶；将改性沸石载体浸于掺杂的二氧化钛溶胶中60min，然后在120℃烘干12小时得到干凝胶；将所得干凝胶在炉内焙烧，以8℃/min的升温速率从室温升至300℃，保持50min；然后以8℃/min的升温速率升温至600℃，保持2h；再以8℃/min的升温速率升温至900℃，保持3h；冷却至室温，得到氮、镧、铜、锌、铜共掺杂的纳米二氧化钛光催化剂；
(3)将原料放入搅拌机中均匀搅拌30min，制得涂料浆体；
(4)将步骤2中的光催化抗菌粉体加入到步骤(3)中的涂料浆体之中，于40°搅拌2h，制得光催化材料；
(5)原料的质量份数比为纳米二氧化钛：纳米二氧化硅：纳米银：纳料：填料：水＝5:15：1:0.5:30:5:10:1:5：5:5:50。
作为本发明的实施例：将纳米二氧化钛、纳米二氧化硅、纳米银、纳米氧化铁起来结合制得一种新型的光催化剂，能够显著提高纳米二氧化钛的光催化效率，加快二氧化钛催化降污效果，同时银的加入使本材料具有杀菌的功能，使材料具有高效无污染的抗菌杀菌和降解空气中有机污染物的功能，所用原料均为无机固体粉末，涂料易于储存与运输，施工过程对人体无害，制得的光催化材料，性能稳定，可直接取代腻子粉和乳胶漆，和水泥砂浆墙面直接结合，牢固，不起皮，不脱落，不裂纹。可做成各种造型墙面，成本低。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点,对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。
Claims (5)
1.一种多元素共掺杂纳米二氧化钛光催化材料，其特征在于：包括以下步骤：
(1)以改性沸石为载体，以摩尔分数计，氮的掺杂量为1％，镧的掺杂量为1.5％，钾的掺杂量为1％，锌的掺杂量为1％，铋的掺杂量为1％，铜的掺杂量为2％，改性沸石载体占催化剂的质量含量为60％；
(2)将氮掺杂前驱体、镧掺杂前驱体、钾掺杂前驱体、锌掺杂前驱体、铋的前驱体和铜掺杂前驱体的无水乙醇溶液加入反应器中，用硝酸调整pH为2，搅匀；然后搅拌下滴加钛酸四丁酯的无水乙醇溶液，室温搅拌12小时进行水解，得到掺杂的二氧化钛溶胶；将改性沸石载体浸于掺杂的二氧化钛溶胶中60min，然后在120℃烘干12小时得到干凝胶；将所得干凝胶在炉内焙烧，以8℃/min的升温速率从室温升至300℃，保持50min；然后以8℃/min的升温速率升温至600℃，保持2h；再以8℃/min的升温速率升温至900℃，保持3h；冷却至室温，得到氮、镧、铜、锌、铜共掺杂的纳米二氧化钛光催化剂；
(3)将原料放入搅拌机中均匀搅拌30min，制得涂料浆体；
(4)将步骤2中的光催化抗菌粉体加入到步骤(3)中的涂料浆体之中，于40°搅拌2h，制得光催化材料；
(5)所述原料的质量份数比为纳米二氧化钛：纳米二氧化硅：纳米银：纳米氧化铁：硅酸盐：石膏粉：钛白粉：粉末抗结剂：固化调理剂：无机颜料：填料：水＝5:15：1:0.5:30:5:10:1:5：5:5:50。
2.根据权利要求1所述的一种多元素共掺杂纳米二氧化钛光催化材料，其特征在于：所述硅酸盐取自硅酸钠、硅酸钾、硅酸锂、硅酸钙、硅酸镁或硅酸铝中的任意一种或几种的混合物。
3.根据权利要求1所述的一种多元素共掺杂纳米二氧化钛光催化材料，其特征在于：所述粉末抗结剂取自氧化镁、滑石粉、超细二氧化硅或轻质碳酸钙中的任意一种或几种的混合物。
4.根据权利要求1所述的一种多元素共掺杂纳米二氧化钛光催化材料，其特征在于：所述固化调理剂为缩合磷酸盐或铵盐的任意一种或混合物。
5.根据权利要求1所述的一种多元素共掺杂纳米二氧化钛光催化材料，其特征在于：所述填料取自石灰石、重晶石、氧化锌、绢云母、石英或磷酸钙中的任意一种或几种的混合物。
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