CN107311227B - 一种混合晶型的二氧化钛纳米片的制备方法及产物 - Google Patents
一种混合晶型的二氧化钛纳米片的制备方法及产物 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 78
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 24
- 239000013078 crystal Substances 0.000 title claims abstract description 21
- 238000002156 mixing Methods 0.000 title claims abstract description 20
- 239000002055 nanoplate Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 50
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 24
- OQRWAMBQGTYSRD-UHFFFAOYSA-N dipotassium;oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[K+].[K+].[Ti+4].[Ti+4].[Ti+4].[Ti+4] OQRWAMBQGTYSRD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 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 abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000005516 engineering process Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- 239000000428 dust Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 39
- 239000000047 product Substances 0.000 description 25
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 14
- 238000003756 stirring Methods 0.000 description 13
- 239000010936 titanium Substances 0.000 description 13
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- 229920001343 polytetrafluoroethylene Polymers 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 9
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
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- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
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- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
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- 231100000252 nontoxic Toxicity 0.000 description 2
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- 239000001301 oxygen Substances 0.000 description 2
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- 239000011591 potassium Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
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- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910003087 TiOx Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- GHQPBDDZGPAVJP-UHFFFAOYSA-N azanium;methanol;hydroxide Chemical compound N.O.OC GHQPBDDZGPAVJP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
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- 239000002537 cosmetic Substances 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
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- 150000007524 organic acids Chemical class 0.000 description 1
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- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
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- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 231100001234 toxic pollutant Toxicity 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- 239000012463 white pigment Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- C01G23/04—Oxides; Hydroxides
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
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Abstract
本发明涉及一种混合晶型的二氧化钛纳米片的制备方法,包括如下步骤:1)将氢氧化钾溶液加入到钛酸四丁酯溶液中,混合后进行水热反应,产物过滤清洗后,得到钛酸钾纤维;2)将钛酸钾纤维分散在浓度为0.5~1M的硝酸溶液中,进行水热反应,产物过滤清洗后,得到二氧化钛纳米片。本发明还涉及该方法所制备的混合晶型的二氧化钛纳米片,同时具有锐钛矿型和金红石型,使得混合晶型的二氧化钛具有优异的催化性能。
Description
技术领域
本发明涉及二氧化钛制备领域,具体涉及一种混合晶型的二氧化钛纳米片的制备方法及产物。
背景技术
二氧化钛(TiO2)是一种无毒,不溶于水、无机弱酸和有机酸,微溶于碱的白色粉末或固体的两性氧化物。白度、光亮度和不透明性良好,在国内外被公认为是最具发展潜质的一种白色颜料,广泛应用于涂料、印刷油墨、塑料、橡胶、化纤、化妆品、造纸等工业。
同时TiO2具有很强的抗腐蚀性以及良好的光催化活性、紫外线屏蔽功能也很强、还可以发生很奇特的颜色效应等特性,在废水处理、空气净化、抗菌杀菌、防晒护肤、涂料和汽车工业、建筑、焊接、传感器、功能陶瓷、生物学、医学、光催化剂等诸多领域备受人们的关注。该材料被用作光催化剂,具有活性强、安全无毒、价格低、没有污染、性能稳定等优点,是很有发展前景的环保催化剂之一。二氧化钛光催化技术可以利用空气中的太阳光和氧,来降解有毒污染物,有望成为一种新的环保技术。
目前工业上应用较广的二氧化钛为锐钛矿型(Anatase)简称A型,和金红石型(Rutile)简称R型。国内外制备锐钛矿型二氧化钛采用溶胶凝胶法、四氯化钛气相氧化法、硫酸氧钛或硫酸钛溶液液相水解法等。通常锐钛矿型TiO2具有较好的光催化分解水的性能,这与其具有较大的禁带宽度(3.2eV)和较负的导带位置有关。而金红石型TiO2的相对密度和折射率比锐钛矿型TiO2大,分散光射线的能力较好,而其光催化性能比锐钛矿型的差,国内生产二氧化钛的方法主要有硫酸法和氯化法。
因此,亟待开发一种合成方法直接合成混合晶型的TiO2,并进一步提高其催化性能。
发明内容
本发明的目的在于针对现有技术的不足,提供一种混合晶型的二氧化钛纳米片的制备方法及产物,所得二氧化钛同时具有锐钛矿型和金红石型,使得混合晶型的二氧化钛具有优异的催化性能。
本发明所提供的技术方案为:
一种混合晶型的二氧化钛纳米片的制备方法,包括如下步骤:
1)将氢氧化钾溶液加入到钛酸四丁酯溶液中,混合后进行水热反应,产物过滤清洗后,得到钛酸钾纤维;
2)将钛酸钾纤维分散在浓度为0.5~1M的硝酸溶液中,进行水热反应,产物过滤清洗后,得到二氧化钛纳米片。
上述技术方案中采用两步水热法,先在高浓度OH-存在的情况下利用钛酸四丁酯的水解制备钛酸钾纤维(K2Ti8O17),然后以钛酸钾纤维为前驱体,在酸性条件下,利用H+对K+的取代,脱水。最终制备得到二氧化钛(TiO2)纳米片,产物是金红石型和锐钛矿型两种晶相混合,纳米片尺寸在20~50nm,具有大的比表面积,具有优异的催化性能。
优选的,所述步骤1)中氢氧化钾与钛酸四丁酯的投料比为16~18g:1~2ml。该比例是为了提供过量的OH-,使得钛酸四丁酯能够充分水解,获得单相钛酸钾纤维。
优选的,所述步骤1)中氢氧化钾溶液的浓度为0.8~0.9g/ml。
优选的,所述步骤1)中钛酸四丁酯溶液是将钛酸四丁酯溶解在乙二醇中,钛酸四丁酯溶液的浓度为0.05~0.1Vol%。
优选的,所述步骤1)中水热反应的温度为180~200℃,反应时间为24~30h。
优选的,所述步骤1)中清洗是指0.08~0.1M稀硝酸、去离子水和无水乙醇分别进行清洗。因为在制备钛酸钾纤维时,采用了高浓度的KOH溶液,容易吸收空气中的CO2形成K2CO3颗粒,并且在水热后混合在钛酸钾纤维产物中,可以通过稀硝酸洗涤后去除。进一步优选为0.1M稀硝酸。
优选的,所述步骤2)中钛酸钾纤维与硝酸溶液的投料比为0.8~1g:35~45ml。提供0.5~1M的硝酸是为了在反应体系中提供足量的H+,使得钛酸钾的K+被充分取代,并最终脱水获得TiO2。
优选的,所述步骤2)中水热反应的温度为180~200℃,反应时间为24~30h。进一步优选,温度为180~190℃。较高的反应温度和较长的反应时间,更加利于TiO2纳米片的形貌调控,使得产物的形貌更加规则,尺寸更加均一。
本发明还提供一种如上述的制备方法制备得到的混合晶型的二氧化钛纳米片。二氧化钛纳米片含有金红石型和锐钛矿型两种晶相,纳米片大小为20~50nm,产品形貌好,且纯度高,分散性好。
同现有技术相比,本发明的有益效果体现在:
(1)本发明工艺过程简单,易于控制,无环境污染,成本低,易于规模化生产。
(2)本发明制得的TiO2纳米片含有金红石型和锐钛矿型两种晶相,且纳米片尺寸为20~50nm,比表面积大,具有优异的光催化性能。
附图说明
图1为实施例1中制备的钛酸钾(K2Ti8O17)纤维的XRD图;
图2为实施例1中制备的钛酸钾(K2Ti8O17)纤维的SEM图;
图3为实施例1中制备的钛酸钾(K2Ti8O17)纤维的TEM图;
图4为实施例1中制备的TiO2纳米片的XRD图;
图5为实施例1中制备的TiO2纳米片的SEM图;
图6为实施例1中制备的TiO2纳米片的TEM图;
图7为对比例1中制备的产物的SEM图;
图8为对比例2中制备的产物的SEM图;
图9为对比例3中制备的产物的SEM图;
图10为TiO2纳米片和商用P25光催化制氢图。
具体实施方式
下面结合具体的实施例对本发明作进一步说明。
实施例1
1)取1ml钛酸四丁酯溶解在20ml乙二醇中,在室温下经过2h的搅拌,形成澄清溶液;
2)取16g氢氧化钾溶解在20ml水溶液中,搅拌10min后将KOH溶液倒入步骤1)中的钛酸四丁酯溶液中,在室温下搅拌2h,形成澄清前驱体溶液;
3)将前驱体溶液转移到50ml聚四氟乙烯反应釜中进行180℃,24h水热反应,将水热反应产物过滤,并用0.1M的稀硝酸、去离子水、无水乙醇分别清洗,干燥得到钛酸钾(K2Ti8O17)纤维;
4)将上述钛酸钾纤维溶解在40ml 0.5M的稀硝酸溶液中,在室温下搅拌1h后,将溶液转移至50ml聚四氟乙烯反应釜中进行180℃,24h水热反应,将水热反应产物过滤,并用去离子水、无水乙醇分别清洗,干燥得到TiO2纳米片。
对步骤3)中制备得到的钛酸钾(K2Ti8O17)纤维进行XRD表征,由图1可知水热获得的钛酸钾的峰和PDF卡片吻合,没有出现副产物K2CO3的峰。
分别对钛酸钾(K2Ti8O17)纤维进行SEM和TEM表征,由图2可知钛酸钾纤维分散性良好,没有出现纤维的团聚,通过图3透射照片还能看到获得的钛酸钾纤维是由单层钛酸钾卷曲重叠形成的,这样的形貌为下一步制备TiO2纳米片提供了良好的条件。
对步骤4)中制备得到的TiO2纳米片进行XRD表征,如图4所示,可知实施例1获得的TiO2结晶性良好,XRD衍射峰清晰,分析后可得产物TiO2是由锐钛矿和金红石两种晶相的TiO2混合而成。
同时图5可知获得的TiO2粉末是由极小的TiO2纳米片组成,通过图6看可知TiO2纳米片尺寸在20~50nm之间。纳米尺寸的TiO2可以带来极大的比表面积,为光催化水制氢提供良好条件。
实施例2
1)取1.5ml钛酸四丁酯溶解在20ml乙二醇中,在室温下经过2h的搅拌,形成澄清溶液;
2)取16g氢氧化钾溶解在20ml水溶液中,搅拌10min后将KOH溶液倒入步骤1)中的钛酸四丁酯溶液中,在室温下搅拌2h,形成澄清前驱体溶液;
3)将前驱体溶液转移到50ml聚四氟乙烯反应釜中进行180℃,24h水热反应,将水热反应产物过滤,并用0.1M的稀硝酸、去离子水、无水乙醇分别清洗,干燥得到钛酸钾(K2Ti8O17)纤维;
4)将上述钛酸钾纤维溶解在40ml 1M的稀硝酸溶液中,在室温下搅拌1h后,将溶液转移至50ml聚四氟乙烯反应釜中进行180℃,24h水热反应,将水热反应产物过滤,并用去离子水、无水乙醇分别清洗,干燥得到TiO2纳米片。
实施例3
1)取2ml钛酸四丁酯溶解在20ml乙二醇中,在室温下经过3h的搅拌,形成澄清溶液;
2)取18g氢氧化钾溶解在20ml水溶液中,搅拌10min后将KOH溶液倒入步骤1)中的钛酸四丁酯溶液中,在室温下搅拌2h,形成澄清前驱体溶液;
3)将前驱体溶液转移到50ml聚四氟乙烯反应釜中进行200℃,30h水热反应,将水热反应产物过滤,并用0.1M的稀硝酸、去离子水、无水乙醇分别清洗,干燥得到钛酸钾(K2Ti8O17)纤维;
4)将上述钛酸钾纤维溶解在40ml 1M的稀硝酸溶液中,在室温下搅拌1h后,将溶液转移至50ml聚四氟乙烯反应釜中进行200℃,30h水热反应,将水热反应产物过滤,并用去离子水、无水乙醇分别清洗,干燥得到TiO2纳米片。
对比例1
1)取2ml钛酸四丁酯溶解在20ml乙二醇中,在室温下经过3h的搅拌,形成澄清溶液;
2)取6g氢氧化钾溶解在20ml水溶液中,搅拌10min后将KOH溶液倒入步骤1)中的钛酸四丁酯溶液中,在室温下搅拌2h,形成澄清前驱体溶液;
3)将前驱体溶液转移到50ml聚四氟乙烯反应釜中进行200℃,30h水热反应,将水热反应产物过滤,并用0.1M的稀硝酸、去离子水、无水乙醇分别清洗,干燥。
通过图7可知,因为反应体系中OH-含量不足,因此钛酸四丁酯不能完全转化为钛酸钾,产物中有大量未反应完的前驱体,不能获得钛酸钾纤维。
对比例2
1)取2ml钛酸四丁酯溶解在20ml乙二醇中,在室温下经过3h的搅拌,形成澄清溶液;
2)取6g氢氧化钾溶解在20ml水溶液中,搅拌10min后将KOH溶液倒入步骤1)中的钛酸四丁酯溶液中,在室温下搅拌2h,形成澄清前驱体溶液;
3)将前驱体溶液转移到50ml聚四氟乙烯反应釜中进行200℃,30h水热反应,将水热反应产物过滤,并用去离子水、无水乙醇分别清洗,干燥;
由图8可知,由于产物未经过稀硝酸的清洗,产物中有大的K2CO3颗粒,获得的钛酸钾不纯。
对比例3
1)取2ml钛酸四丁酯溶解在20ml乙二醇中,在室温下经过3h的搅拌,形成澄清溶液;
2)取18g氢氧化钾溶解在20ml水溶液中,搅拌10min后将KOH溶液倒入步骤1)中的钛酸四丁酯溶液中,在室温下搅拌2h,形成澄清前驱体溶液;
3)将前驱体溶液转移到50ml聚四氟乙烯反应釜中进行200℃,30h水热反应,将水热反应产物过滤,并用0.1M的稀硝酸、去离子水、无水乙醇分别清洗,干燥得到钛酸钾(K2Ti8O17)纤维;
4)将上述钛酸钾纤维溶解在40ml 0.05M的稀硝酸溶液中,在室温下搅拌1h后,将溶液转移至50ml聚四氟乙烯反应釜中进行200℃,30h水热反应,将水热反应产物过滤,并用去离子水、无水乙醇分别清洗,干燥。
由图9可知,因为在第二次水热过程中所提供的H+浓度不够,在水热后钛酸钾不能顺利转变为TiO2,在扫描电镜下看到产物依然是钛酸钾纤维。
性能试验
催化剂在紫外光下的光解水产氧反应在一管状密闭石英反应器内进行,采用500W的高压氙灯(上海比朗仪器有限公司)作为紫外光源,光源被放在接有低温冷却循环的U形冷阱中减少光照过程中产生的热量。
反应器同样在两端设有开关截止阀,反应器体积约为150ml,光照时光源从顶部照射反应器。反应前依旧打开两端截止阀通入高纯氩气除去反应器内空气,反应器内空气去除干净后关闭所有截止阀将反应器放到具体光源约5cm处在室温条件下开始搅拌。称取0.05g的样品加入到盛有100ml甲醇铵和水(比例为95:5)混合溶液的石英反应器中,超声使之分散均匀。然后在紫外光下照射4h,产生的气体产物用气相色谱仪在线分析,用热导池检测,然后根据标准曲线计算产生氢气量。
图10为实施例1制备的TiO2纳米片和商用P25两种催化剂的制氢性能比较,由图可知TiO2纳米片光催化制氢在4h时产氢量为18.78mmol/g,而商用P25产氢量为16.53mmol/g,TiO2纳米片光催化制氢性能比P25更加优越。
TiO2纳米片光催化性能优异原因在于,由于实施例1制备的TiO2纳米片是由锐钛矿和金红石两种晶相的TiO2混合而成,根据对TiO2光催化原理的分析,通常锐钛矿型TiO2具有较好的光催化分解水的性能,这与其具有较大的禁带宽度(3.2eV)和较负的导带位置有关,而金红石型TiO2光催化性能比锐钛矿型差,但是实际在应用过程中,因为混晶效应的存在,并非纯锐钛矿型的效果最好,而是锐钛矿和金红石定比例混合时,才能表现出最佳催化效果。
Claims (4)
1.一种混合晶型的二氧化钛纳米片的制备方法,其特征在于,包括如下步骤:
1)将氢氧化钾溶液加入到钛酸四丁酯溶液中,混合后进行水热反应,产物过滤清洗后,得到钛酸钾纤维;所述步骤1)中氢氧化钾与钛酸四丁酯的投料比为16~18g:1~2mL ;所述步骤1)中氢氧化钾溶液的浓度为0.8~0.9g/ mL ;所述步骤1)中钛酸四丁酯溶液是将钛酸四丁酯溶解在乙二醇中;所述步骤1)中水热反应的温度为180~200℃,反应时间为24~30h;
2)将钛酸钾纤维分散在浓度为0.5~1M的硝酸溶液中,进行水热反应,产物过滤清洗后,得到二氧化钛纳米片;所述步骤2)中水热反应的温度为180~200℃,反应时间为24~30h。
2.根据权利要求1所述的混合晶型的二氧化钛纳米片的制备方法,其特征在于,所述步骤1)中钛酸四丁酯溶液的浓度为0.05~0.1Vol%。
3.根据权利要求1所述的混合晶型的二氧化钛纳米片的制备方法,其特征在于,所述步骤1)中清洗是指0.08~0.1M稀硝酸、去离子水和无水乙醇分别进行清洗。
4.根据权利要求1所述的混合晶型的二氧化钛纳米片的制备方法,其特征在于,所述步骤2)中钛酸钾纤维与硝酸溶液的投料比为0.8~1g:35~45mL 。
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