CN108097279A - 一种贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸 - Google Patents
一种贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸 Download PDFInfo
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- CN108097279A CN108097279A CN201711423360.2A CN201711423360A CN108097279A CN 108097279 A CN108097279 A CN 108097279A CN 201711423360 A CN201711423360 A CN 201711423360A CN 108097279 A CN108097279 A CN 108097279A
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- 229910052588 hydroxylapatite Inorganic materials 0.000 title claims abstract description 105
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 title claims abstract description 105
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- 229910052737 gold Inorganic materials 0.000 claims abstract description 70
- 239000010931 gold Substances 0.000 claims abstract description 70
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- 238000006555 catalytic reaction Methods 0.000 claims abstract description 48
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 25
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 5
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- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
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- CQVDKGFMVXRRAI-UHFFFAOYSA-J Cl[Au](Cl)(Cl)Cl Chemical compound Cl[Au](Cl)(Cl)Cl CQVDKGFMVXRRAI-UHFFFAOYSA-J 0.000 description 1
- KVCWSJZUKMSPLM-UHFFFAOYSA-N O.O[PH2]=O Chemical compound O.O[PH2]=O KVCWSJZUKMSPLM-UHFFFAOYSA-N 0.000 description 1
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- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1806—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with alkaline or alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/864—Removing carbon monoxide or hydrocarbons
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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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
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1856—Phosphorus; Compounds thereof with iron group metals or platinum group metals with platinum group metals
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- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/30—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds
- C07C209/32—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups
- C07C209/36—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst
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Abstract
本发明涉及一种贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，所述贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸是由表面负载有贵金属纳米颗粒的羟基磷灰石超长纳米线抄造而成；所述羟基磷灰石超长纳米线的直径为5～100纳米，长度为20～2000微米；所述贵金属纳米颗粒为金、银、钯、铂中的至少一种，负载量为0.1～10 wt%。
Description
技术领域
本发明属于催化剂技术领域，具体涉及一种贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸。
背景技术
纳米金催化剂作为一种重要的高活性催化剂，在有机物加氢反应、一氧化碳氧化、甲醛降解、有机物选择性氧化和环氧化等反应中应用广泛。但因金纳米颗粒的尺寸小易团聚导致其活性急剧下降，在液相反应体系中难以分离并循环利用而限制其进一步应用。为了解决上述问题，研究人员对金纳米催化剂的固载化进行了大量的研究，采用不同的方式将金纳米粒子负载在各种有机或无机载体中以保持其高催化活性。但是金纳米催化剂在工业领域的应用仍然受到限制，如在液相反应体系中将金纳米催化剂分离出来的过程耗时繁琐。
连续流动纳米催化反应技术是将纳米催化剂负载在多孔膜或整体柱反应器中，反应物连续地流经与催化剂接触进行催化反应。该技术具有易实现连续化生产、产物与催化剂分离简便、改善催化剂失活等优势。整体柱反应器存在流化床孔内扩散严重、聚合物基质易膨胀和无机基质易坍塌等技术问题。相比之下，多孔膜反应器的微米或亚微米多孔结构内产物与催化剂间传质速率高、催化效率高。另外，多孔膜反应器存储、使用和更换简单方便，极大地提高了其在工业领域中的应用潜力。研究人员发展了多种有机纤维和无机纤维材质的多孔膜，相比于有机纤维，无机纤维材料具有高化学稳定性、耐高温性能和高催化剂固载量等优点。
羟基磷灰石是脊椎类动物牙齿和骨骼的主要无机矿物成分，是一种环境友好、生物相容性高的生物材料。羟基磷灰石纳米材料及其复合材料主要应用于生物成像、药物运输、骨缺损修复、吸附分离等领域。羟基磷灰石具有优异的离子交换、吸附等性质，在催化领域应用潜力大。多种贵金属包括钯、铷、铂和金纳米粒子等被负载在羟基磷灰石表面，用于有机合成反应、氧化反应和还原反应。传统羟基磷灰石材料为无规则形貌、颗粒、短棒、微球或片状，所制备的纳米催化剂多为粉末状，使用过程需要反复多次离心或过滤，限制了其在催化反应中的应用，且粉末状纳米催化剂容易发生团聚或板结，严重影响其催化效率。
发明内容
针对现有技术的不足，本发明的目的是提供一种贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，以克服传统催化剂载体热稳定性差、制备过程繁琐、使用不便、循环利用困难、催化效率低等缺点。
一方面，本发明提供了一种贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，所述贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸是由表面负载有贵金属纳米颗粒的羟基磷灰石超长纳米线抄造而成；
所述羟基磷灰石超长纳米线的直径为5～100纳米，长度为20～2000微米；
所述贵金属纳米颗粒为金、银、钯、铂中的至少一种，直径范围为2～100纳米，负载量为0.1～10wt％。
本发明中，贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸是由表面负载有贵金属纳米颗粒(例如，金、银、钯、铂等，负载量为0.1～10wt％)的羟基磷灰石超长纳米线(直径为5～100纳米，长度为20～2000微米)抄造而成，其具有纳米线自组装形成的纳米多孔结构的特征(如图1所示)，可以在催化反应过程中减少反应物的扩散，有利于增加反应物和催化剂接触机会，提高催化效率。本发明制备的贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸具有耐高温、不燃烧的性质，在高温条件下依然保持高效催化活性。
较佳地，贵金属纳米颗粒的负载量为1～6wt％。
较佳地，所述羟基磷灰石超长纳米线的直径20～80纳米，长度为50～1000微米。
较佳地，所述贵金属纳米颗粒的直径尺寸范围为2～100纳米，优选为5～40纳米。
较佳地，所述贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸的厚度为40～3000微米，优选为60～400微米。
另一方面，本发明提供了一种贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸的制备方法，包括：
将羟基磷灰石超长纳米线分散于贵金属前驱体的溶液中，在4～40℃下反应1～72小时，再经过滤、清洗后得到表面负载有贵金属纳米颗粒的羟基磷灰石超长纳米线；
将所得表面负载有贵金属纳米颗粒的羟基磷灰石超长纳米线分散于水中后，抄造成纸。
较佳地，所述贵金属前驱体为四氯金酸、四氯金酸钠、四氯金酸铵、氯化金钾、氯钯酸、氯钯酸钠、氯钯酸钾、氯钯酸铵、氯化钯、硝酸钯、硫酸钯、醋酸钯、碘化钯、二溴化钯、二氯二氨钯、二氯四氨钯、氯亚钯酸钠、氯亚钯酸钾、氯亚钯酸铵、硝酸银、氯铂酸、氯铂酸钠、氯铂酸钾、氯铂酸铵、氯亚铂酸钠、氯亚铂酸铵、氯亚铂酸钾、四氯化铂、二氯化铂、硝酸铂、四硝基铂酸钾、二亚硝基二氨铂、四氨合硝酸铂和四氨合氯化铂中的至少一种。
较佳地，所述贵金属前驱体和羟基磷灰石超长纳米线的质量比为(1～30)：100，优选为(4～16)：100。
再一方面，本发明还提供了一种上述贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸在催化领域和环境净化领域中的应用。本发明制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸具有良好的柔韧性，可作为连续流动催化纸，用于催化硝基苯化合物、甲醛和一氧化碳等，在工业生产、工业尾气净化、汽车尾气净化、环境保护等领域具有良好的应用前景。
本发明的有益效果在于：
本发明在羟基磷灰石超长纳米线表面负载贵金属纳米颗粒(例如，金纳米粒子等)，制备贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，负载过程在室温水溶液中完成，无需加热和添加剂，具有简便、环境友好等优点；
采用滤水成型、干燥步骤制备得到贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，制备工艺简单，易于批量制备，易于实现商品化应用；
本发明制备的贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸中贵金属纳米颗粒(例如，金纳米粒子等)直径尺寸小、分布均匀、负载量可调控，具有高效的催化活性功效。
附图说明
图1为实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线的扫描电子显微图，该图显示金纳米粒子分散固载在羟基磷灰石超长纳米线表面；
图2为实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线的透射电子显微图，该图示金纳米颗粒的平均直径为13纳米；
图3为实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸在乙醇火焰中不燃烧的数码照片，显示制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸具有良好的耐高温、不燃烧的特征；
图4为实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸在多种不同高温条件下处理1小时后的数码照片，显示制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸热处理后仍然保持完整性；
图5为实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸长时间使用对4-硝基苯酚的催化效率变化图，显示制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸的催化活性具有良好的稳定性；
图6为实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸在不同高温条件下处理1小时后对4-硝基苯酚的催化效率变化图，结果显示制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸在高温条件下仍然可以保持稳定的高效催化活性；
图7为实施例10制备的直径为20厘米的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸的数码照片，该图显示所制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸具有高柔韧性。
具体实施方式
以下通过下述实施方式进一步说明本发明，应理解，下述实施方式仅用于说明本发明，而非限制本发明。
本发明制备的贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸是由羟基磷灰石和贵金属纳米颗粒组成(例如，金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸由羟基磷灰石超长纳米线和金纳米颗粒组成)。其中，羟基磷灰石超长纳米线的直径可为5～100纳米，长度可为20～2000微米。所述羟基磷灰石超长纳米线的纸浆优选为20～80纳米，长度优选为50～1000微米。贵金属纳米颗粒(例如，金、银、钯、铂等)的直径尺寸范围可为2～100纳米，优选为5～40纳米。贵金属纳米颗粒的负载量可为0.1～10wt.％，若进一步提高贵金属纳米颗粒的负载量，贵金属纳米颗粒尺寸会增大，对催化性能提高的效果不显著；若是其负载量较少，其催化性能不明显，可进一步优选1～6wt.％。
本发明中，上述贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸的厚度范围可为40～3000微米，优选为60～400微米。
以下示例性地说明本发明提供的贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸的制备方法。
本发明中，羟基磷灰石超长纳米线可以采用溶剂热法或水热法制备，可参考文献和专利报道的方法制备，例如：朱英杰,路丙强,陈峰,高柔韧性耐高温不燃的羟基磷灰石纸及其制备方法,专利号ZL201310687363.2；Ceramics International,41,6098-6102(2015)；Materials Letters,144,135-137(2015)。也可采用其它合适的制备方法，所用方法只要能够制备出所述羟基磷灰石超长纳米线即可。
将羟基磷灰石超长纳米线分散于贵金属前驱体的溶液中，在4～40℃下反应1～72小时，再经过滤、清洗后得到表面负载有贵金属纳米颗粒的羟基磷灰石超长纳米线(贵金属纳米颗粒与羟基磷灰石超长纳米线结合良好)。其中所述贵金属前驱体为四氯金酸、四氯金酸钠、四氯金酸铵、氯化金钾、氯钯酸、氯钯酸钠、氯钯酸钾、氯钯酸铵、氯化钯、硝酸钯、硫酸钯、醋酸钯、碘化钯、二溴化钯、二氯二氨钯、二氯四氨钯、氯亚钯酸钠、氯亚钯酸钾、氯亚钯酸铵、硝酸银、氯铂酸、氯铂酸钠、氯铂酸钾、氯铂酸铵、氯亚铂酸钠、氯亚铂酸铵、氯亚铂酸钾、四氯化铂、二氯化铂、硝酸铂、四硝基铂酸钾、二亚硝基二氨铂、四氨合硝酸铂和四氨合氯化铂中的至少一种。所述贵金属前驱体和羟基磷灰石超长纳米线的质量比可为(1～30)：100，优选为(4～16)：100。作为一个示例，将羟基磷灰石超长纳米线和氯金酸水溶液混合，在室温(4～40℃)下搅拌1～72小时，经过滤分离、乙醇和水清洗，得到金纳米颗粒复合羟基磷灰石超长纳米线(表面负载有金纳米颗粒的羟基磷灰石超长纳米线)。
将表面负载有贵金属纳米颗粒的羟基磷灰石超长纳米线分散于水中后，抄造成纸。作为一个示例，金纳米颗粒复合羟基磷灰石超长纳米线悬浮水溶液倒入纸张成型器，真空抽滤，60～100℃干燥5～30分钟，得到金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸。
本发明中，贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸可多次循环使用以及可长时间使用，在各种催化领域和环境净化领域中具有良好的应用前景。
下面进一步例举实施例以详细说明本发明。同样应理解，以下实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例，即本领域技术人员可以通过本文的说明做合适的范围内选择，而并非要限定于下文示例的具体数值。
羟基磷灰石超长纳米线的制备：
将12.000克乙醇和12.000克油酸搅拌均匀，加入20毫升含0.220克氯化钙的水溶液，搅拌均匀后，依次加入20毫升含1.000克氢氧化钠的水溶液和10毫升含0.280克二水合磷酸二氢钠的水溶液。所得混合物转入反应釜中，密封，加热至180℃，保温24小时。将所得产物分别用乙醇和水清洗多次，得到羟基磷灰石超长纳米线，其长度约为20～2000微米，直径约为5～100纳米。
实施例1：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入3.296毫升氯金酸(5毫克/毫升)溶液，室温搅拌12小时，过滤分离，乙醇和水清洗三次，量取一半悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度为121微米。采用电感耦合等离子体发射光谱仪测定金纳米粒子的负载量，采用透射电镜测定金纳米粒子的平均尺寸。实验表明，金纳米粒子的负载量为4.88wt.％，平均尺寸为13纳米。
实施例2：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入0.824毫升氯金酸(5毫克/毫升)溶液，室温搅拌12小时，过滤分离，乙醇和水清洗三次，量取一半悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度为118微米。测定金纳米粒子的负载量和平均尺寸的方法同实施例1。实验表明，金纳米粒子的负载量为0.96wt.％，平均尺寸为3纳米。
实施例3：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入1.648毫升氯金酸(5毫克/毫升)溶液，室温搅拌12小时，过滤分离，乙醇和水清洗三次，量取一半悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度为115微米。测定金纳米粒子的负载量和平均尺寸的方法同实施例1。实验表明，金纳米粒子的负载量为2.15wt.％，平均尺寸为6纳米。
实施例4：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入2.472毫升氯金酸(5毫克/毫升)溶液，室温搅拌12小时，过滤分离，乙醇和水清洗三次，量取一半悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度为125微米。测定金纳米粒子的负载量和平均尺寸的方法同实施例1。实验结果显示，金纳米粒子的负载量为3.6wt.％，平均尺寸为11纳米。
实施例5：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入4.120毫升氯金酸(5毫克/毫升)溶液，室温搅拌12小时，过滤分离，乙醇和水清洗三次，量取一半悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度为131微米。测定金纳米粒子的负载量和平均尺寸的方法同实施例1。实验结果显示，金纳米粒子的负载量为6.16wt.％，平均尺寸为16纳米。
实施例6：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入3.296毫升氯金酸(5毫克/毫升)溶液，室温搅拌4小时，过滤分离，乙醇和水清洗三次，量取一半悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度为112微米。测定金纳米粒子的负载量和平均尺寸的方法同实施例1。金纳米粒子的负载量为1.57wt.％，平均直径尺寸为9纳米。
实施例7：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入3.296毫升氯金酸(5毫克/毫升)溶液，室温搅拌8小时，过滤分离，乙醇和水清洗三次，量取一半悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度为122微米。测定金纳米粒子的负载量和平均尺寸的方法同实施例1。实验结果表明，金纳米粒子的负载量为3.44wt.％，平均尺寸为11纳米。
实施例8：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入3.296毫升氯金酸(5毫克/毫升)溶液，室温搅拌16小时，过滤分离，乙醇和水清洗三次，量取一半悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度为124微米。测定金纳米粒子的负载量和平均尺寸的方法同实施例1。实验结果表明，金纳米粒子的负载量为5.20wt.％，平均尺寸为16纳米。
实施例9：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入3.296毫升氯金酸(5毫克/毫升)溶液，室温搅拌24小时，过滤分离，乙醇和水清洗三次，量取一半悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度为119微米。测定金纳米粒子的负载量和平均尺寸的方法同实施例1。实验结果表明，金纳米粒子的负载量为5.65wt.％，平均尺寸为19纳米。
实施例10：
将1.5克羟基磷灰石超长纳米线分散于1.5升水中，加入3.296毫升氯金酸(5毫克/毫升)溶液，室温搅拌12小时，过滤分离，乙醇和水清洗三次，所得悬浮液倒入滤水成型器，真空抽滤，95℃干燥3分钟，分离即得金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度为147微米。测定金纳米粒子的负载量和平均尺寸的方法同实施例1。实验结果表明，金纳米粒子的负载量为4.92wt.％，平均尺寸为14纳米。
以实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸为例，测定其对4-硝基苯酚的催化效率。测试方法为：裁剪一定直径的圆片状催化耐火纸，装入过滤器内，连接蠕动泵，蠕动泵驱动4-硝基苯酚溶液流过催化耐火纸。采用紫外分光光度仪测定流动催化前后溶液的紫外吸收光谱。过滤效率计算方法为：流动催化后溶液光谱图中400纳米处对应吸光度/流动催化前溶液光谱图中400纳米处对应吸光度×100％。实验结果表明，4-硝基苯酚的过滤催化效率测定为100％。
以实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸为例，将其置于燃烧的乙醇火焰中，观察其耐高温、不燃烧的现象，如图3所示；
以实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸为例，将其分别用不同温度条件热处理1小时，观察其耐高温的稳定性，如图4所示；
以实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸为例，测定其长时间使用对4-硝基苯酚催化效率的变化，如图5所示。按照测定催化效率的方法，连续过滤催化约200小时(192小时)，每隔24小时测定4-硝基苯酚的催化效率，在约200小时催化效率仍然高于90％；
以实施例1制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸为例，将其分别用不同温度条件热处理1小时，冷却至室温后测定其对4-硝基苯酚的催化效率，如图6所示。
实施例11：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入5毫升氯钯酸钠(5毫克/毫升)溶液，室温搅拌12小时，过滤分离，乙醇和水清洗三次，所得悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得钯纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度约为120微米。
实施例12：
将100毫克羟基磷灰石超长纳米线分散于100毫升水中，加入5毫升氯铂酸(5毫克/毫升)溶液，室温搅拌12小时，过滤分离，乙醇和水清洗三次，所得悬浮液倒入砂芯漏斗，真空抽滤，95℃干燥3分钟，分离即得铂纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，厚度约为118微米。
产业应用性：本发明的制备工艺简单、无需使用复杂昂贵的设备，有望大规模制备及实现商品化生产。通过本发明制备的金纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，可作为连续流动催化纸用于催化硝基苯化合物、甲醛和一氧化碳等，在工业生产、工业尾气净化、汽车尾气净化、环境保护等领域具有良好的应用前景。
Claims (4)
1.一种贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，其特征在于，所述贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸是由表面负载有贵金属纳米颗粒的羟基磷灰石超长纳米线抄造而成；所述羟基磷灰石超长纳米线的直径为5～100纳米，长度为20～2000微米；所述贵金属纳米颗粒为金、银、钯、铂中的至少一种，负载量为0.1～10wt%。
2.根据权利要求1所述的贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，其特征在于，所述贵金属纳米颗粒的直径尺寸范围为2～100纳米，优选为5～40纳米。
3.根据权利要求1或2所述的贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸，其特征在于，所述贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸的厚度为40～3000微米，优选为60～400微米。
4.一种如权利要求1-3中任一项所述贵金属纳米颗粒复合羟基磷灰石超长纳米线催化耐火纸在催化领域和环境处理净化领域中的应用。
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