CN106698374A - 菱形中空十二面体磷酸钾纳米晶体及其合成方法 - Google Patents
菱形中空十二面体磷酸钾纳米晶体及其合成方法 Download PDFInfo
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- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 title claims abstract description 74
- 229910000160 potassium phosphate Inorganic materials 0.000 title claims abstract description 37
- 235000011009 potassium phosphates Nutrition 0.000 title claims abstract description 37
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 title abstract 7
- 238000001308 synthesis method Methods 0.000 title abstract 3
- 239000002159 nanocrystal Substances 0.000 claims abstract description 40
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000001103 potassium chloride Substances 0.000 claims abstract description 12
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 3
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 17
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 9
- 229910052700 potassium Inorganic materials 0.000 claims description 9
- 239000011591 potassium Substances 0.000 claims description 9
- 238000010189 synthetic method Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000010432 diamond Substances 0.000 claims description 6
- 229910009112 xH2O Inorganic materials 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 230000001788 irregular Effects 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
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- 239000012190 activator Substances 0.000 description 8
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- 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 4
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- NNJVILVZKWQKPM-UHFFFAOYSA-N Lidocaine Chemical compound CCN(CC)CC(=O)NC1=C(C)C=CC=C1C NNJVILVZKWQKPM-UHFFFAOYSA-N 0.000 description 1
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- 229940019931 silver phosphate Drugs 0.000 description 1
- 229910000161 silver phosphate Inorganic materials 0.000 description 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M sodium bicarbonate Substances [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
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- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 150000003732 xanthenes Chemical class 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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Abstract
菱形中空十二面体磷酸钾纳米晶体及其合成方法,属于可见光催化材料的制备技术领域。以去离子水为溶剂,将钾盐和磷钨酸混合进行水热反应,取沉淀以去离子水和无水乙醇清洗后干燥,即得菱形中空十二面体磷酸钾纳米晶体。本发明采用简便的方法在温和的条件下一步合成,得到形貌均一的中空菱形十二面体纳米晶体。该纳米晶体独特的中空菱形十二面体的特殊结构,通过纳米孔道显示出有效的降解染料污染物的能力,在90分钟可见光照射后,有效的降解染料污染物的能力,几乎可以将RhB完全分解,并且可以多次循环使用。
Description
技术领域
本发明属于可见光催化材料的制备技术领域。
背景技术
近年来,可控合成无机材料引起了广泛的关注,因为其独特的形状与大小决定了它们的性能。因此,化学合成被广泛应用于定向合成和自组装先进的微米纳米结构,如:仿生技术或者利用特定表面活性剂辅助可控合成微、纳米材料。尽管现有的合成方法已经合成了许多优秀的形貌,许多微、纳米材料的形成机制仍然缺乏深入的理解和讨论。
多金属氧酸盐(POMs)金属-氧阴离子簇和配合物。POMs结合适当的抗衡阳离子的通常会形成固态材料,这些固态材料在不同的领域如催化,磁性,医药材料,光电化学,电化学有一定的应用。微/纳米结构化的或者自自组装POMs具有杰出性能的引起了广泛研究和关注
利用光催化消除和降解污染物是当前最活跃的研究领域之一,人们研究开发了学过可见光催化剂。POMs近年来频被应用于光催化,如用于去除水中的重金属离子和污染物的光催化剂。可见光在太阳光中所占的比例为50%,因此利用可见光催化降解污染物可将太阳光的利用率达到最高。专利CN200910306562.8介绍了一中可见光催化剂磷酸银及其制备方法,但是这个材料制备方法比较复杂,且原料成本较高,在材料的实际应用阶段,产生了很大的不便利。
发明内容
本发明的目的是提供一种制备方法简单的菱形中空十二面体磷酸钾纳米晶体。
本发明菱形中空十二面体磷酸钾纳米晶体具有均匀的中空菱形十二面体。
并且,菱形十二面体磷钨酸钾纳米晶体的直径为450~500nm,在所述纳米晶体表面分布不规则的纳米孔洞。
经试验证实,本发明的菱形中空十二面体磷酸钾纳米晶体具有优秀的光催化性能和理想的光催化稳定性,在可见光照射下,活化剂活化后,可以迅速解降染料污染主要成分之一罗丹明B(RhB),光照90分钟后基本可以达到完全无色,可应用于可见光催化。
本发明另一目的是提出以上菱形中空十二面体磷酸钾纳米晶体的合成方法:以去离子水为溶剂,将钾盐和磷钨酸混合进行水热反应,取沉淀以去离子水和无水乙醇清洗后干燥,即得菱形中空十二面体磷酸钾纳米晶体。
与现有技术相比,本发明的显著优点是:
(1)采用简便的方法在温和的条件下一步合成,并没有其他模板试剂或者表面活性剂,即可得到形貌均一的中空菱形十二面体纳米结构。
(2)菱形十二面体磷钨酸钾纳米晶体因其独特的中空菱形十二面体的特殊结构,通过纳米孔道显示出有效的降解染料污染物的能力。
(3)菱形十二面体磷钨酸钾纳米晶体在90分钟可见光照射后,有效的降解染料污染物的能力,几乎可以将RhB完全分解。
(4)菱形十二面体磷钨酸钾纳米晶体可以多次循环使用。
进一步地,本发明所述钾盐为KNO3,K2SO4或KCl中的任意一种。这三种钾盐价格低廉,环保无毒,并且均为强酸强碱盐,在水溶液中可完全电离,与磷钨酸充分反应,提高产率。
所述磷钨酸为H3O40PW12·xH2O。H3O40PW12·xH2O具有酸性,而且具有氧化还原性,是一种多功能的新型催化剂,具有很高的催化活性,稳定性好,可作均相及非均相反应,甚至可作相转移催化剂,对环境无污染,是绿色催化剂。
所述水热反应的温度条件为120~180℃,反应时间5~20h。在水热反应中,溶液在密封体系中转化为汽态,使离子间均匀而充分的相互接触,避免局部过浓而导致的形貌不均的结果。在此温度与时间下,可得到均匀统一的中空菱形十二面体的磷钨酸钾,这种独特的纳米结构对其应用于可见光催化剂起了很大的帮助作用。
所述钾盐和磷钨酸的混合质量比为1∶2~5∶4。在制备反应中,钾盐与磷钨酸进行简单的置换反应:
K++H3O40PW12·xH2O→K3O40PW12·xH2O+H+
在该离子浓度范围进行的反应,在保证样品形貌与性能的基础上,最多限度的提高了反应产率,几乎没有反应原料的浪费。
附图说明
图1为制备的菱形中空十二面体磷酸钾纳米晶体的X射线粉末衍射图。
图2为制备的菱形中空十二面体磷酸钾纳米晶体的扫描电子显微镜图。
图3为制备的菱形中空十二面体磷酸钾纳米晶体的透射电子显微镜图。
图4为制备的菱形中空十二面体磷酸钾纳米晶体的可见光催化分解RhB图谱。
图5为制备的菱形中空十二面体磷酸钾纳米晶体的回收重复催化分解RhB图谱。
具体实施方式
1、菱形中空十二面体磷酸钾纳米晶体的制备。
(1)称取150mg的KNO3,K2SO4或KCl与120~300mg的H3O40PW12·xH2O,加入去离子水置于聚四氟乙烯反应釜中,搅拌均匀。
(2)将上述反应釜密封,并加上不锈钢反应釜外壳,置于120~180℃烘箱中反应5~20h。
(3)将所得沉淀物使用去离子水和无水乙醇清洗数次,然后在室温下自然干燥,取得约300mg菱形中空十二面体磷酸钾纳米晶体。
图1显示了得到的菱形中空十二面体磷酸钾纳米晶体的X射线粉末衍射图谱。从图1可见:图谱中的特征峰几乎完全与标准磷钨酸钾晶体特征峰相拟合,证明所合成样品即为磷钨酸钾。
图2为制备的菱形中空磷酸钾纳米晶体的扫描电子显微镜图。从图2可见:所制备样品为规则均一的菱形十二面体材料,并且其表面分布着大小不一的不规则孔洞。
图3为制备的菱形中空十二面体磷酸钾纳米晶体在不同放大倍数下的透射电子显微镜图。从图3可见:制成的菱形中空十二面体磷酸钾纳米晶体均匀的中空菱形十二面体,直径约为450~500nm,并且表面分布着不规则的纳米孔洞。
2、菱形中空十二面体磷酸钾纳米晶体光催化降解罗丹明B(RhB)的测试。
(1)以200~800 W 碘钨灯作为光源。
(2)在碘钨灯外包一个柱形玻璃冷凝管,再外套一个截至滤波器,以保证只有可见光的照射。
(3)将所制备的菱形中空十二面体磷酸钾纳米晶体、活化剂和RhB的水溶液混合均匀,在无光条件下搅拌均匀,取得混合溶液。
上述菱形中空十二面体磷酸钾纳米晶体、活化剂和罗丹明B的混合质量比为1∶10∶150。
上述罗丹明B:9-(2-羧基苯基)-3,6-双(二乙氨基)占吨翁氯化物,是一种具有鲜桃红色的人工合成的染料,在废水中会造成严重的水体污染。
上述活化剂为质量百分数为30%的过氧化氢溶液。
(4)将上步取得的混合溶液在可见光源下照射。
(5)用浓度为0.5~1.5mol/L的Na2CO3-NaHCO3缓冲液将光照后的混合溶液的pH值调至8.0。
6)图4显示了三种平行试验实验方案下测试结果:
为了证明所制备磷钨酸钾与活化剂在光照下降解RhB过程中分别所起作用,分别配制三种体系:
1、体系1:纯RhB水溶液。
2、体系2:活化剂和RhB混合溶液。
3、体系3:制备的菱形中空十二面体磷酸钾纳米晶体(S)和活化剂、RhB混合。
然后分别在可见光照射下分别记录三种体系对RhB的降解百分比。
图4可见:在可见光的照射下,菱形中空十二面体磷酸钾纳米晶体在活化剂的作用下可以迅速降解RhB,在90 min时,RhB几乎完全分解。
图5中,1至7分别是经历1至7次循环的催化分解RhB图谱。从图5可见:菱形中空十二面体磷酸钾纳米晶体作为催化剂的稳定性和循环寿命,经历了7次循环后,菱形中空十二面体磷酸钾纳米晶体催化能力也没有发生明显的降低。
Claims (7)
1.菱形中空十二面体磷酸钾纳米晶体,其结构为均匀的中空菱形十二面体。
2.根据权利要求1所述菱形中空十二面体磷酸钾纳米晶体,其特征在于,所述菱形十二面体磷钨酸钾纳米晶体的直径为450~500nm,所述纳米晶体表面分布不规则的纳米孔洞。
3.如权利要求1或2所述菱形中空十二面体磷酸钾纳米晶体的合成方法,其特征在于以去离子水为溶剂,将钾盐和磷钨酸混合进行水热反应,取沉淀以去离子水和无水乙醇清洗后干燥,即得菱形中空十二面体磷酸钾纳米晶体。
4.根据权利要求3所述菱形中空十二面体磷酸钾纳米晶体的合成方法,其特征在于所述钾盐为KNO3,K2SO4或KCl中的任意一种。
5.根据权利要求3所述菱形中空十二面体磷酸钾纳米晶体的合成方法,其特征在于所述磷钨酸为H3O40PW12·xH2O。
6.根据权利要求3所述菱形中空十二面体磷酸钾纳米晶体的合成方法,其特征在于所述水热反应的温度条件为120~180℃,反应时间5~20h。
7.根据权利要求3所述菱形中空十二面体磷酸钾纳米晶体的合成方法,其特征在于所述钾盐和磷钨酸的混合质量比为1∶2~5∶4。
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