CN110075874A - 二硒化钼改性二氧化钛纳米光催化剂及其制备方法和应用 - Google Patents
二硒化钼改性二氧化钛纳米光催化剂及其制备方法和应用 Download PDFInfo
- Publication number
- CN110075874A CN110075874A CN201910274885.7A CN201910274885A CN110075874A CN 110075874 A CN110075874 A CN 110075874A CN 201910274885 A CN201910274885 A CN 201910274885A CN 110075874 A CN110075874 A CN 110075874A
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- China
- Prior art keywords
- mose
- agent
- tio
- powder
- titanium dioxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 29
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 16
- 239000011733 molybdenum Substances 0.000 title claims abstract description 16
- 238000000576 coating method Methods 0.000 claims abstract description 32
- 239000011248 coating agent Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000003112 inhibitor Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 11
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005282 brightening Methods 0.000 claims abstract description 10
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- 230000007613 environmental effect Effects 0.000 claims abstract description 10
- 235000019441 ethanol Nutrition 0.000 claims abstract description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003381 stabilizer Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 150000002751 molybdenum Chemical class 0.000 claims abstract description 7
- 150000003608 titanium Chemical class 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000011534 incubation Methods 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 239000002075 main ingredient Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 229910016001 MoSe Inorganic materials 0.000 claims description 25
- 239000011669 selenium Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000006210 lotion Substances 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 9
- 230000001699 photocatalysis Effects 0.000 claims description 9
- -1 polysiloxane Polymers 0.000 claims description 9
- 230000003197 catalytic effect Effects 0.000 claims description 8
- 239000000839 emulsion Substances 0.000 claims description 8
- 239000011684 sodium molybdate Substances 0.000 claims description 8
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000012279 sodium borohydride Substances 0.000 claims description 7
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 5
- NMGYKLMMQCTUGI-UHFFFAOYSA-J diazanium;titanium(4+);hexafluoride Chemical compound [NH4+].[NH4+].[F-].[F-].[F-].[F-].[F-].[F-].[Ti+4] NMGYKLMMQCTUGI-UHFFFAOYSA-J 0.000 claims description 5
- KPHWPUGNDIVLNH-UHFFFAOYSA-M diclofenac sodium Chemical compound [Na+].[O-]C(=O)CC1=CC=CC=C1NC1=C(Cl)C=CC=C1Cl KPHWPUGNDIVLNH-UHFFFAOYSA-M 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 239000004611 light stabiliser Substances 0.000 claims description 5
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- 229910052711 selenium Inorganic materials 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical group Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000013530 defoamer Substances 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical group [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 229920002635 polyurethane Polymers 0.000 claims 1
- 239000004814 polyurethane Substances 0.000 claims 1
- 230000003449 preventive effect Effects 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000032683 aging Effects 0.000 abstract 1
- 235000010215 titanium dioxide Nutrition 0.000 description 18
- 239000000047 product Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000002086 nanomaterial Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013034 coating degradation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 229940035637 spectrum-4 Drugs 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
Classifications
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- B01D53/007—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by irradiation
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- B01D53/34—Chemical or biological purification of waste gases
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- B01D2259/802—Visible light
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/3045—Sulfates
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Abstract
本发明涉及二硒化钼改性二氧化钛纳米光催化剂及其制备方法和应用。该纳米光催化剂粒径是100～200nm，主要成份为MoSe2与TiO2，其中MoSe2的含量为5‑20wt％。该催化剂的制备方法是：将可溶性钼盐、硒粉、还原剂溶于乙醇水溶液中，恒温水热反应并过滤、洗涤和干燥，得到MoSe2粉末；将该粉末分散到可溶性钛盐的乙醇或水溶液中，恒温水热反应后洗涤和干燥，得到所述纳米光催化剂，将其加入到成膜剂、分散剂、消泡剂、增白剂的水溶液中，搅拌，加入稳定剂、流平剂和防霉剂，调节pH值到7.0‑8.0，陈化，即可制得具有甲醛降解能力的环保涂料。本发明的方法成本价廉，生产工艺简单易控，适合大规模工业生产。
Description
技术领域
本发明涉及纳米材料及环保材料领域，具体涉及一种二硒化钼改性二氧化钛纳米光催化剂及其制备方法和应用。
背景技术
以二氧化钛为代表的传统光催化材料因其优异的物理化学性能而被广泛应用于光催化净化环境，是解决当前日趋严重的环境污染问题的重要途径之一。然而二氧化钛仅能吸收太阳光谱中4％～5％的紫外光,因此拓展二氧化钛的吸收光谱，提高其光催化效率是当前光催化领域研究的重要方向。此外，传统的光催化材料也是当前环保涂料的重要的添加剂或助剂，国家发明专利201410104099.X、201110196966.3、201410781164.2公布了光催化材料在涂料领域的应用，因此发展高性能的二氧化钛光催化剂具有广阔的应用前景。
近来，研究人员将各种各样的半导体纳米材料应用于二氧化钛的改性，并取得了较好的成果。特别是近期热点的二维层状材料如石墨烯、g-C3N4及过度金属硫族化合物等，因其在光催化领域优异的性能，而被广泛用于光催化剂材料的复合，其中石墨烯与g-C3N4在光催化领域已得到了广泛的应用。而层状结构的MoSe2纳米材料成为当前纳米材料领域的热点，中国发明专利201510907556.3，201810457292X，201810241753X等报道了其应用于润滑摩擦、锂电及光催化领域的应用，然而有关其应用于环保涂料的报道较少。
发明内容
针对现有技术的不足，本发明的目的之一在于提供一种二硒化钼改性二氧化钛纳米光催化剂。
上述目的是通过如下技术方案实现的：
一种二硒化钼改性二氧化钛纳米光催化剂，所述催化剂是100～200nm粒径的粉末，其主要成份为MoSe2与TiO2，其中MoSe2的质量百分含量为5-20％，余量为TiO2。
本发明的目的之二在于提供一种所述二硒化钼改性二氧化钛纳米光催化剂的制备方法，具体技术方案如下：
一种二硒化钼改性二氧化钛纳米光催化剂的制备方法，包括如下步骤：
(1)MoSe2的水热合成：将可溶性钼盐、硒粉、还原剂溶于40-60wt％的乙醇水溶液中，磁力搅拌20-40分钟，然后在150-250℃恒温水热反应5-7h后，冷却至室温，得到反应产物；将上述反应产物加入热碱液中，磁力搅拌10-20分钟后置于70-90℃的烘箱中1-3h以去除多余的硒，自然冷却至室温，过滤、洗涤和干燥后，得到MoSe2粉末；
(2)MoSe2/TiO2的合成：将步骤(1)中制备的MoSe2粉末分散到浓度为8-12g/L的可溶性钛盐的乙醇或水溶液中，超声分散20-40min后在160-220℃恒温水热反应10-14h；自然冷却至室温后，经过洗涤和干燥，得到所述MoSe2/TiO2纳米光催化剂。
优选地，所述可溶性钼盐为钼酸铵、钼酸钠或五氯化钼；还原剂为盐酸羟胺或硼氢化钠；可溶性钛盐为钛酸四丁酯或氟钛酸铵；热碱液为60-80℃的氢氧化钠(NaOH)或氢氧化钾(KOH)溶液，浓度为1～3mol/L。
优选地，步骤(1)所述可溶性钼盐、硒粉、还原剂在所述乙醇水溶液中的浓度分别为30～35g/L、30～35g/L、5～6g/L，所述热碱液与乙醇水溶液的体积比为1:1～2；步骤(2)所述MoSe2粉末和可溶性钛盐的质量比为0.04～0.16:1。
本发明的目的之三是提供一种二硒化钼改性二氧化钛纳米光催化剂的应用，具体技术方案如下：
所述二硒化钼改性二氧化钛纳米光催化剂应用于一种光催化环保涂料，按照质量百分比，其组成如下：成膜物质26％-60％，分散剂2-5％，消泡剂0.1-0.5％，防霉剂0.5-1.5％，稳定剂2-5％，流平剂0.3-0.6％，增白剂10-15％，纳米光催化助剂MoSe2/TiO22-8％,去离子水或蒸馏水15-40％。
优选地，所述成膜物质为水溶性丙烯酸乳液与聚氨酯乳液的混合物，其中水溶性丙烯酸乳液占所述环保涂料的21-45wt％，聚氨酯乳液占所述环保涂料的5％-20wt％；所述分散剂为十二烷基苯磺酸钠；所述防霉剂为氯酚钠涂料专用防腐防霉剂；所述消泡剂为聚硅氧烷类消泡剂；所述稳定剂为受阻胺类光稳定剂，所述流平剂为聚醚改性聚硅氧烷；所述增白剂为钛白粉。
所述光催化环保涂料的制备方法如下：以所述光催化涂料的质量百分比计，将21-45％的水溶性丙烯酸乳液、5-20％的聚氨酯乳液、2-5％的分散剂、0.1-0.5％的消泡剂、10-15％的增白剂分散到20-45％的去离子水或蒸馏水中，以800～1000r/min的转速均匀搅拌10-20min后缓缓加入2-8％的MoSe2/TiO2光催化剂粉末，在1500～2500r/min的转速下搅拌分散30-60min，然后以2500～3000r/min的转速搅拌20-40min，再在800～1500r/min的转速搅拌下加入2-5％的稳定剂、0.3-0.6％的流平剂、4.0-6.0％的防霉剂，同时用NaOH或KOH调节pH值到7.0-8.0，以800～1000r/min的转速搅拌均匀后陈化2-5h，制得所述MoSe2/TiO2光催化涂料。
本发明的有益效果
本发明提供了一种二硒化钼改性二氧化钛纳米光催化剂，其制备方法成本价廉，生产工艺简单易控，产物差率高，适合大规模的工业生产。该催化剂可应用于自清洁环保光催化涂料，有效清除甲醛等有毒有害气体，方便有效地净化空气。
附图说明
图1为本发明制得的MoSe2/TiO2复合纳米材料的EDS谱图。
图2为本发明制得的MoSe2/TiO2复合纳米材料的微观形貌扫描电镜(SEM)图。
图3为本发明制得的MoSe2/TiO2复合纳米材料的微观形貌透射电镜图(TEM)。
具体实施方式
以下通过具体实施方式进一步描述本发明，由技术常识可知，本发明也可通过其它的不脱离本发明技术特征的方案来描述，因此所有在本发明范围内或等同本发明范围内的改变均被本发明包含。
实施例1
MoSe2/TiO2纳米光催化剂的合成(MoSe2含量为5wt％)
(1)将1.6452g钼酸钠(Na2MoO4·2H2O)、1.5492g硒(Se)粉、0.2595g硼氢化钠(NaBH4)溶于50mL的乙醇水溶液(50wt％)中，磁力搅拌30min后转移至100mL不锈钢反应釜中，置于真空干燥箱，200℃下保温6h后，冷却至室温；将制备的黑色产物转入60℃的NaOH溶液(50mL，2mol/L)，磁力搅拌10min后转移至烘箱中80℃保温2h以除去多余的Se，再自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2粉末。
(2)根据MoSe2在MoSe2/TiO2中5wt％的理论值，将步骤(1)中制备的MoSe2粉末0.02g分散到50mL的氟钛酸铵[(NH4)2TiF6]的乙醇溶液(10g/L)中,超声分散30min后将该混合液移至100mL内衬聚四氟乙烯的高温水热反应釜中密封，将反应釜放入真空干燥箱，180℃下保温12h。自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2/TiO2纳米光催化剂。
MoSe2/TiO2光催化涂料的制备
以所述光催化涂料的质量百分比计，将成膜物质(25％的水溶性丙烯酸乳液、20％的聚氨酯乳液)、2％的分散剂(十二烷基苯磺酸钠)，0.1％的消泡剂(聚硅氧烷类消泡剂)，10％的增白剂(钛白粉)分散到34.6％的蒸馏水中，以800r/min的转速均匀搅拌10min后缓缓加入2％的MoSe2/TiO2光催化剂粉末作为纳米光催化助剂，在2000r/min的转速下搅拌分散45min左右，得到水性胶体。然后以2500r/min的转速搅拌30min使之充分分散，再800r/min的转速搅拌下加入2％的稳定剂(受阻胺类光稳定剂)、0.3％的流平剂(聚醚改性聚硅氧烷)、4.0％的防霉剂(氯酚钠涂料专用防腐防霉剂)，同时用2M的NaOH调节pH值到8.0，最后以800r/min的转速搅拌均匀后陈化2h，制得MoSe2/TiO2光催化涂料。
实施例2
MoSe2/TiO2纳米光催化剂的合成(MoSe2含量为10wt％)
(1)将1.6452g钼酸钠(Na2MoO4·2H2O)、1.5492g硒(Se)粉、0.2595g硼氢化钠(NaBH4)溶于50mL的乙醇水溶液(50wt％)中，磁力搅拌30min后转移至100mL不锈钢反应釜中，置于真空干燥箱，200℃下保温6h后，冷却至室温；将制备的黑色产物转入80℃的NaOH溶液(50mL，3mol/)，磁力搅拌10min后转移至烘箱中80℃保温2h以除去多余的Se，再自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2粉末。
(2)根据MoSe2在MoSe2/TiO2中10wt％的理论值，将步骤(1)中制备的MoSe2粉末0.04g分散到50mL的氟钛酸铵[(NH4)2TiF6]的乙醇溶液(10g/L)中,超声分散30min后将该混合液移至100mL内衬聚四氟乙烯的高温水热反应釜中密封，将反应釜放入真空干燥箱，180℃下保温12h。自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2/TiO2纳米光催化剂。
MoSe2/TiO2光催化涂料的制备:
以所述光催化涂料的质量百分比计，将成膜物质(21％的水溶性丙烯酸乳液、5％的聚氨酯乳液)、4％的分散剂(十二烷基苯磺酸钠)，0.3％的消泡剂(聚硅氧烷类消泡剂)，15％的增白剂(钛白粉)分散到41.3％的蒸馏水中，以1000r/min的转速均匀搅拌10min后缓缓加入4％的MoSe2/TiO2光催化剂粉末作为纳米光催化助剂，在2000r/min的转速下搅拌分散45min左右，得到水性胶体。然后以3000r/min的转速搅拌30min使之充分分散，再以1000r/min的转速搅拌下加入3％的稳定剂(受阻胺类光稳定剂)、0.4％的流平剂(聚醚改性聚硅氧烷)、6.0％的防霉剂(氯酚钠涂料专用防腐防霉剂)，同时用2M的NaOH调节pH值到8.0，最后以1000r/min的转速搅拌均匀后陈化2h，制得MoSe2/TiO2光催化涂料。
实施例3
MoSe2/TiO2纳米光催化剂的合成(MoSe2含量为20wt％)
(1)将1.6452g钼酸钠(Na2MoO4·2H2O)、1.5492g硒(Se)粉、0.2595g硼氢化钠(NaBH4)溶于50mL的乙醇水溶液(50wt％)中，磁力搅拌30min后转移至100mL不锈钢反应釜中，置于真空干燥箱，200℃下保温6h后，冷却至室温；将制备的黑色产物转入的70℃的NaOH溶液(50mL，2mol/L)，磁力搅拌10min后转移至烘箱中80℃保温2h以除去多余的Se，再自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2粉末。
(2)根据MoSe2在MoSe2/TiO2中20wt％的理论值，将步骤(1)中制备的MoSe2粉末0.08g分散到50mL的氟钛酸铵[(NH4)2TiF6]的水溶液(10g/L)中,超声分散30min后将该混合液移至100mL内衬聚四氟乙烯的高温水热反应釜中密封，将反应釜放入真空干燥箱，180℃下保温12h。自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2/TiO2纳米光催化剂。
MoSe2/TiO2光催化涂料的制备:
以所述光催化涂料的质量百分比计，将成膜物质(25％的水溶性丙烯酸乳液、20％的聚氨酯乳液)、5％的分散剂(十二烷基苯磺酸钠)，0.5％的消泡剂(聚硅氧烷类消泡剂)，10％的增白剂(钛白粉)分散到21.9％的蒸馏水中，以900r/min的转速均匀搅拌10min后缓缓加入8％的MoSe2/TiO2光催化剂粉末作为纳米光催化助剂，在2000r/min的转速下搅拌分散45min左右，得到水性胶体。然后以2800r/min的转速搅拌30min使之充分分散，再以900r/min的转速搅拌下加入5％的稳定剂(受阻胺类光稳定剂)、0.6％的流平剂(聚醚改性聚硅氧烷)、4.0％的防霉剂(氯酚钠涂料专用防腐防霉剂)，同时用2M的KOH调节pH值到8.0，最后以900r/min的转速搅拌均匀后陈化2h，制得MoSe2/TiO2光催化涂料。
图1为EDS图谱，表明产物由Mo、Se、Ti、O元合成产物MoSe2/TiO2的素组成，无其它杂质，其Mo：Se为1:1.98，Ti：O为1：2.05，与化学式相一致，证明了MoSe2/TiO2的成功制备。图2和图3分别为合成产物MoSe2/TiO2的SEM和TEM图，由图可知四方结构TiO2纳米颗粒生长在花状MoSe2之上，其平均颗粒尺度约为200nm。
为了考察光催化涂料降解甲醛的实际效果，本发明利用欧盟普遍采用的HJC-1型环境测试舱模拟可见光源下室内环境。采用乙酰丙酮分光光度法(GB/T 15516-1995)，选择每隔2h采样5L舱内的气体，检测环境测试舱中甲醛气体的浓度变化,从而可以计算出MoSe2/TiO2光催化涂料光催化降解甲醛气体的效率，具体见表1。从表1中可以看出本发明的光催化剂8小时的甲醛降解率最高可达34.5％。
表1.对比实施例光催化涂料光催化降解甲醛气体的效率(％)
Claims (7)
1.一种二硒化钼改性二氧化钛纳米光催化剂，其特征在于，所述催化剂是100～200nm粒径的粉末，其主要成份为MoSe2与TiO2，其中MoSe2的质量百分含量为5-20％，余量为TiO2。
2.一种如权利要求1所述的二硒化钼改性二氧化钛纳米光催化剂的制备方法，其特征在于，包括如下步骤：
(1)MoSe2的水热合成：将可溶性钼盐、硒粉、还原剂溶于40-60wt％的乙醇水溶液中，磁力搅拌20-40分钟，然后在150-250℃恒温水热反应5-7h后，冷却至室温，得到反应产物；将上述反应产物加入热碱液中，磁力搅拌10-20分钟后置于70-90℃的烘箱中1-3h以去除多余的硒，自然冷却至室温，过滤、洗涤和干燥后，得到MoSe2粉末；
(2)MoSe2/TiO2的合成：将步骤(1)中制备的MoSe2粉末分散到浓度为8-12g/L的可溶性钛盐的乙醇或水溶液中，超声分散20-40min后在160-220℃恒温水热反应10-14h；自然冷却至室温后，经过洗涤和干燥，得到所述MoSe2/TiO2纳米光催化剂。
3.根据权利要求2所述的二硒化钼改性二氧化钛纳米光催化剂的制备方法，其特征在于，所述可溶性钼盐为钼酸铵、钼酸钠或五氯化钼；还原剂为盐酸羟胺或硼氢化钠；可溶性钛盐为钛酸四丁酯或氟钛酸铵；热碱液为60-80℃的氢氧化钠或氢氧化钾溶液，浓度为1-3mol/L。
4.根据权利要求3所述的二硒化钼改性二氧化钛纳米光催化剂的制备方法，其特征在于，步骤(1)所述可溶性钼盐、硒粉、还原剂在所述乙醇水溶液中的浓度分别为30～35g/L、30～35g/L、5～6g/L，所述热碱液与乙醇水溶液的体积比为1:1～2；步骤(2)所述MoSe2粉末和可溶性钛盐的质量比为0.04～0.16:1。
5.根据权利要求1所述的二硒化钼改性二氧化钛纳米光催化剂应用于一种光催化环保涂料，其特征在于，按照质量百分比，其组成如下：成膜物质为26％-60％，分散剂为2-5％，消泡剂为0.1-0.5％，防霉剂为0.5-1.5％，稳定剂为2-5％，流平剂为0.3-0.6％，增白剂为10-15％，纳米光催化助剂MoSe2/TiO2为2-8％,去离子水或蒸馏水为15-40％。
6.根据权利要求5所述的应用，其特征在于，所述成膜物质为水溶性丙烯酸乳液与聚氨酯乳液的混合物，其中水溶性丙烯酸乳液占所述环保涂料的21-45wt％,聚氨酯乳液占所述环保涂料的5％-20wt％；所述分散剂为十二烷基苯磺酸钠；所述防霉剂为氯酚钠涂料专用防腐防霉剂；所述消泡剂为聚硅氧烷类消泡剂；所述稳定剂为受阻胺类光稳定剂，所述流平剂为聚醚改性聚硅氧烷；所述增白剂为钛白粉。
7.根据权利要求6所述应用的方法，其特征在于，所述光催化环保涂料的制备方法如下：以所述光催化涂料的质量百分比计，将21-45％的水溶性丙烯酸乳液、5-20％的聚氨酯乳液、2-5％的分散剂、0.1-0.5％的消泡剂、10-15％的增白剂分散到20-45％的去离子水或蒸馏水中，以800～1000r/min的转速均匀搅拌10-20min后缓缓加入2-8％的MoSe2/TiO2光催化剂粉末，在1500～2500r/min的转速下搅拌分散30-60min，然后以2500～3000r/min的转速搅拌20-40min，再在800～1500r/min的转速搅拌下加入2-5％的稳定剂、0.3-0.6％的流平剂、4.0-6.0％的防霉剂，同时用NaOH或KOH调节pH值到7.0-8.0，以800～1000r/min的转速搅拌均匀后陈化2-5h，制得所述MoSe2/TiO2光催化涂料。
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