CN103332745A - Method for preparing alpha-MoO3 nanobelts by microwave-ultraviolet process - Google Patents

Method for preparing alpha-MoO3 nanobelts by microwave-ultraviolet process Download PDF

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CN103332745A
CN103332745A CN2013102452386A CN201310245238A CN103332745A CN 103332745 A CN103332745 A CN 103332745A CN 2013102452386 A CN2013102452386 A CN 2013102452386A CN 201310245238 A CN201310245238 A CN 201310245238A CN 103332745 A CN103332745 A CN 103332745A
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microwave
solution
ultraviolet
moo
moo3
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曹丽云
马凤兰
黄剑锋
吴建鹏
费杰
卢靖
李翠艳
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a method for preparing alpha-MoO3 nanobelts by a microwave-ultrasonic process, which comprises the following steps: adding ammonium molybdate into deionized water to obtain a solution A, and regulating the pH value of the solution A to less than 0.5 to obtain a solution B; pouring the solution B into a four-neck round-bottom flask, putting in a microwave-ultraviolet-ultrasonic integrated synthesis extraction reactor, carrying out microwave-ultraviolet synthesis, and after the reaction finishes, naturally cooling to room temperature; and taking out the product, washing, and drying in an electric heating vacuum drying oven to obtain the alpha-MoO3 nanobelts. The invention widens the synthesis technique range of the alpha-MoO3 nanobelts; the technique for preparing the alpha-MoO3 nanobelts has the advantages of simpleness, accessible raw materials, higher yield, short reaction period and low cost; the alpha-MoO3 nanobelts prepared by the method provided by the invention have the advantages of complete development, higher purity, favorable crystallinity and uniform distribution; and the method can implement large-scale synthesis of the alpha-MoO3 nanobelts.

Description

A kind of microwave-ultraviolet prepares α-MoO 3The method of nano belt
Technical field
The present invention relates to a kind of preparation MoO 3The method of nano belt, particularly a kind of microwave-ultraviolet prepares α-MoO 3The method of nano belt.
Background technology
MoO 3As a kind of important function inorganic materials, be the core material of devices such as electrochromism, photochromic, gas-discoloration, gas sensing, intelligence camouflage, have great application prospect in fields such as energy-conservation, the information demonstration of building and automobile and storage, environmental monitoring, foodstuffs industry, military affairs.MoO 3Three kinds of common crystalline structures are arranged: thermodynamically stable quadrature phase α-MoO 3, the monocline phase β-MoO of thermodynamics metastable structure 3With six sides h-MoO mutually 3In recent years, quadrature phase α-MoO 3Because it has thermodynamic stability and is studied widely.Nano level MoO 3Because specific surface area is less, its performance is than micron-sized MoO 3More superior.At present, the α-MoO that has reported 3Nanocrystalline have nano particle, nanometer rod, nanofiber, nanometer flower and a nano belt etc.Synthetic α-MoO 3Nanocrystalline method has hydrothermal method, microwave-hydrothermal method, flame method and solution combustion method etc., wherein the most frequently used is (1) hydrothermal method, [Jiwen Li such as Li Jiwen, Yanhua Ma, Fangfang Gong, et al, The Preparation Technique of nanometer Molybdenum Trioxide by Hydrothermal Synthesis[J] .Applied Mechanics and Materials, 2012,117-119:807-810] be raw material with ammonium dimolybdate and nitric acid, adopt hydrothermal method to obtain α-MoO 3Nano particle; [Minyan Yan such as Yan Minyan, Yi Shen, Li Zhao, Zhen Li, Synthesis and photochromic properties of EDTA-induced MoO3powder[J], Materials Research Bulletin, 2011,46:1648-1653] adopt hydrothermal method by control EDTA/Mo 6+Ratio, 120 ℃ down insulation 48h made α-MoO 3The nanometer flower; [Guicun Li such as Li Guicun, Li Jiang, Shuping Pang, et al, Molybdenum Trioxide Nanostructures:The Evolution from Helical Nanosheets to Crosslike Nanoflowers to Nanobelts[J], J.Phys.Chem., B2006,110:24472-24475] with metal M o powder and H 2O 2Be raw material, adopt hydrothermal method behind 180 ℃ of insulation 2-12h, to obtain spiral α-MoO 3Nanostructure.Emerging method has (2) microwave-hydrothermal method, [Anukorn Phuruangrat, Dong Jin Ham, Somchai Thongtem, et al, Electrochemical hydrogen evolution over MoO such as the Anukorn Phuruangrat in Taiwan 3Nanowires produced by microwave-assisted hydrothermal reaction[J], Electrochemistry Communications, 2009,11:1740-1743] be raw material with ammonium molybdate, CTAB and nitric acid, adopt microwave-hydrothermal method 150 ℃ down reaction 3h obtain α-MoO 3Nano wire; (3) flame method, [Lili Cai, Pratap M.Rao, and Xiaolin Zheng, Morphology-Controlled Flame Synthesis of Single, Branched, and Flower-like α-MoO such as the Lili Cai of Britain 3Nanobelt Arrays[J], Nano Letters, 2011,11:872-877] with a kind of catalysis freedom, the flame synthetic technology has obtained arranging different single, dendroids and flower-shaped α-MoO at different substrates fast 3Nano belt; (4) solution combustion method, [D.Parviz, M.Kazemeini, A.M.Rashidi, et al, Synthesis and characterization of MoO such as D.Parviz 3Nanostructures by solution combustion method employing morphology and size control[J], J Nanopart Res, 2010,12:1509-1521] be presoma with ammonium molybdate with different organic additives (PEG, EDTA and urea etc.), adopt solution combustion method to make the different α-MoO of pattern 3Nanocrystalline.Above several method has exists shortcomings such as temperature of reaction height, reaction times is long, and what have exists shortcoming such as complex process equipment, thus seek a kind of low temperature, easily control, simply, synthetic α-MoO fast 3Nanocrystalline method has great importance.
Summary of the invention
The object of the present invention is to provide a kind of microwave-ultraviolet to prepare α-MoO 3The method of nano belt, this method equipment is simple, control, and suitable scale operation easily; Raw materials used simple, can synthesize α-MoO cheaply 3Nano belt; α-the MoO that makes by preparation method of the present invention 3Nano belt purity height, the crystallization homogeneity is higher.
For achieving the above object, the technical solution used in the present invention is:
1) with analytically pure (NH 4) 6Mo 7O 244H 2It is the solution A of 0.005～0.5mol/L that O joins the concentration that makes ammonium molybdate in the deionized water;
2) the solution A stirring and dissolving is evenly got solution B in pH＜0.5 of back regulator solution A;
3) solution B is poured in the four neck round-bottomed flasks, the four neck round bottom flask that are equipped with are gone in the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave trinity, and fix, adopt the platinum resistor temperature measuring mode to carry out thermometric;
4) adopt microwave-ultraviolet synthesis model, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, select temperature-time service pattern, set 50～90 ℃ of temperature of reaction, time 30～150min, microwave heating time is made as 10min, the output rating of insulating process microwave is 24W, and reaction naturally cools to room temperature after finishing;
5) open the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave trinity, the taking-up product washs the electric vacunm drying case inner drying that is placed on 50～80 ℃ and namely obtains α-MoO 3Nano belt.
Described step 2) HNO of employing 6～9mol/L 3The pH of solution regulator solution A.
The synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave trinity of described step 3) adopts the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave trinity of UWave-1000 type.
The washing of described step 5) is adopted deionized water and dehydrated alcohol repeated washing 4～7 times successively.
The present invention has enlarged α-MoO 3The synthetic technology scope of nano belt; Prepared α-MoO 3Nano belt technology is simple, raw material is easy to get, and productive rate is higher, and reaction time is short, and cost is low; α-the MoO of gained 3That nano belt is grown is complete, purity is higher, crystallinity is better and be evenly distributed; α-the MoO that adopts present method to synthesize on a large scale 3Nano belt.
Description of drawings
Fig. 1 is the α-MoO of the inventive method preparation 3The XRD figure spectrum of nano belt;
Fig. 2 is the α-MoO of the inventive method preparation 3The SEM photo of nano belt.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1:
1) with analytical pure ammonium molybdate ((NH 4) 6Mo 7O 244H 2O) joining the concentration that deionized water for stirring makes ammonium molybdate is the solution A of 0.005mol/L;
2) with the solution A stirring and dissolving evenly after, adopt the HNO of 6mol/L 3PH＜0.5 of solution regulator solution A gets solution B;
3) solution B is poured in the four neck round-bottomed flasks, the four neck round-bottomed flasks that are equipped with are put into the synthetic extractive reaction instrument of the UWave-1000 type microwave ultraviolet excess sound wave trinity, and fix, adopt the platinum resistor temperature measuring mode to carry out thermometric;
4) adopt microwave-ultraviolet synthesis model, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, select temperature-time service pattern, set 50 ℃ of temperature of reaction, time 150min, microwave heating time is made as 10min, the output rating of insulating process microwave is 24W, and reaction naturally cools to room temperature after finishing;
5) open the synthetic extractive reaction instrument of the UWave-1000 type microwave ultraviolet excess sound wave trinity, take out product, the electric vacunm drying case inner drying that adopts deionized water and dehydrated alcohol repeated washing to be placed on 50 ℃ for 4～7 times successively namely obtains α-MoO 3Nano belt.
Embodiment 2:
1) with analytical pure ammonium molybdate ((NH 4) 6Mo 7O 244H 2O) joining the concentration that deionized water for stirring makes ammonium molybdate is the solution A of 0.03mol/L;
2) with the solution A stirring and dissolving evenly after, adopt the HNO of 7mol/L 3PH＜0.5 of solution regulator solution A gets solution B;
3) solution B is poured in the four neck round-bottomed flasks, the four neck round-bottomed flasks that are equipped with are put into the synthetic extractive reaction instrument of the UWave-1000 type microwave ultraviolet excess sound wave trinity, and fix, adopt the platinum resistor temperature measuring mode to carry out thermometric;
4) adopt microwave-ultraviolet synthesis model, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, select temperature-time service pattern, set 60 ℃ of temperature of reaction, time 120min, microwave heating time is made as 10min, the output rating of insulating process microwave is 24W, and reaction naturally cools to room temperature after finishing;
5) open the synthetic extractive reaction instrument of the UWave-1000 type microwave ultraviolet excess sound wave trinity, take out product, the electric vacunm drying case inner drying that adopts deionized water and dehydrated alcohol repeated washing to be placed on 60 ℃ for 4～7 times successively namely obtains α-MoO 3Nano belt.
Embodiment 3:
1) with analytical pure ammonium molybdate ((NH 4) 6Mo 7O 244H 2O) joining the concentration that deionized water for stirring makes ammonium molybdate is the solution A of 0.1mol/L;
2) with the solution A stirring and dissolving evenly after, adopt the HNO of 8mol/L 3PH＜0.5 of solution regulator solution A gets solution B;
3) solution B is poured in the four neck round-bottomed flasks, the four neck round-bottomed flasks that are equipped with are put into the synthetic extractive reaction instrument of the UWave-1000 type microwave ultraviolet excess sound wave trinity, and fix, adopt the platinum resistor temperature measuring mode to carry out thermometric;
4) adopt microwave-ultraviolet synthesis model, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, select temperature-time service pattern, set 70 ℃ of temperature of reaction, time 90min, microwave heating time is made as 10min, the output rating of insulating process microwave is 24W, and reaction naturally cools to room temperature after finishing;
5) open the synthetic extractive reaction instrument of the UWave-1000 type microwave ultraviolet excess sound wave trinity, take out product, the electric vacunm drying case inner drying that adopts deionized water and dehydrated alcohol repeated washing to be placed on 70 ℃ for 4～7 times successively namely obtains α-MoO 3Nano belt.
Embodiment 4:
1) with analytical pure ammonium molybdate ((NH 4) 6Mo 7O 244H 2O) joining the concentration that deionized water for stirring makes ammonium molybdate is the solution A of 0.3mol/L;
2) with the solution A stirring and dissolving evenly after, adopt the HNO of 9mol/L 3PH＜0.5 of solution regulator solution A gets solution B;
3) solution B is poured in the four neck round-bottomed flasks, the four neck round-bottomed flasks that are equipped with are put into the synthetic extractive reaction instrument of the UWave-1000 type microwave ultraviolet excess sound wave trinity, and fix, adopt the platinum resistor temperature measuring mode to carry out thermometric;
4) adopt microwave-ultraviolet synthesis model, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, select temperature-time service pattern, set 80 ℃ of temperature of reaction, time 60min, microwave heating time is made as 10min, the output rating of insulating process microwave is 24W, and reaction naturally cools to room temperature after finishing;
5) open the synthetic extractive reaction instrument of the UWave-1000 type microwave ultraviolet excess sound wave trinity, take out product, the electric vacunm drying case inner drying that adopts deionized water and dehydrated alcohol repeated washing to be placed on 80 ℃ for 4～7 times successively namely obtains α-MoO 3Nano belt.
Embodiment 5:
1) with analytical pure ammonium molybdate ((NH 4) 6Mo 7O 244H 2O) joining the concentration that deionized water for stirring makes ammonium molybdate is the solution A of 0.5mol/L;
2) with the solution A stirring and dissolving evenly after, adopt the HNO of 8mol/L 3PH＜0.5 of solution regulator solution A gets solution B;
3) solution B is poured in the four neck round-bottomed flasks, the four neck round-bottomed flasks that are equipped with are put into the synthetic extractive reaction instrument of the UWave-1000 type microwave ultraviolet excess sound wave trinity, and fix, adopt the platinum resistor temperature measuring mode to carry out thermometric;
4) adopt microwave-ultraviolet synthesis model, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, select temperature-time service pattern, set 90 ℃ of temperature of reaction, time 30min, microwave heating time is made as 10min, the output rating of insulating process microwave is 24W, and reaction naturally cools to room temperature after finishing;
5) open the synthetic extractive reaction instrument of the UWave-1000 type microwave ultraviolet excess sound wave trinity, take out product, the electric vacunm drying case inner drying that adopts deionized water and dehydrated alcohol repeated washing to be placed on 60 ℃ for 4～7 times successively namely obtains α-MoO 3Nano belt.
As can be seen from Figure 1, prepared α-MoO 3The nano belt crystallinity is better, and purity is higher.The as can be seen from Figure 2 prepared α-MoO of the present invention 3Nano belt physically well develops, and crystallization is even.

Claims (4)

1. a microwave-ultraviolet prepares α-MoO 3The method of nano belt is characterized in that may further comprise the steps:
1) with analytically pure (NH 4) 6Mo 7O 244H 2It is the solution A of 0.005～0.5mol/L that O joins the concentration that makes ammonium molybdate in the deionized water;
2) the solution A stirring and dissolving is evenly got solution B in pH＜0.5 of back regulator solution A;
3) solution B is poured in the four neck round-bottomed flasks, the four neck round bottom flask that are equipped with are gone in the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave trinity, and fix, adopt the platinum resistor temperature measuring mode to carry out thermometric;
4) adopt microwave-ultraviolet synthesis model, the power of ultraviolet lamp is 300W, ultraviolet lamp centre wavelength is 365nm, select temperature-time service pattern, set 50～90 ℃ of temperature of reaction, time 30～150min, microwave heating time is made as 10min, the output rating of insulating process microwave is 24W, and reaction naturally cools to room temperature after finishing;
5) open the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave trinity, the taking-up product washs the electric vacunm drying case inner drying that is placed on 50～80 ℃ and namely obtains α-MoO 3Nano belt.
2. microwave-ultraviolet according to claim 1 prepares α-MoO 3The method of nano belt is characterized in that: the HNO that described step 2) adopts 6～9mol/L 3The pH of solution regulator solution A.
3. microwave-ultraviolet according to claim 1 prepares α-MoO 3The method of nano belt is characterized in that: the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave trinity of described step 3) adopts the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave trinity of UWave-1000 type.
4. microwave-ultraviolet according to claim 1 prepares α-MoO 3The method of nano belt is characterized in that: the washing of described step 5) is adopted deionized water and dehydrated alcohol repeated washing 4～7 times successively.
CN2013102452386A 2013-06-19 2013-06-19 Method for preparing alpha-MoO3 nanobelts by microwave-ultraviolet process Pending CN103332745A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103818960A (en) * 2014-03-03 2014-05-28 浙江理工大学 Method for preparing alpha-MoO3 nanobelt by adopting hot-wire chemical vapor deposition technology
CN104649323A (en) * 2015-01-21 2015-05-27 济南大学 Preparation method of strip-shaped molybdenum trioxide
CN107021523A (en) * 2017-01-19 2017-08-08 青岛科技大学 A kind of orthorhombic phase α MoO3The preparation method and its photocatalytic applications of nanobelt

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103086435A (en) * 2011-11-03 2013-05-08 中国科学院兰州化学物理研究所 Preparation method of molybdenum trioxide nanorod

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103086435A (en) * 2011-11-03 2013-05-08 中国科学院兰州化学物理研究所 Preparation method of molybdenum trioxide nanorod

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘志等: "室温离子液体对花球状α-氧化钼微波加热合成产物结构的影响", 《材料导报》 *
赵文彦等: "《辐射加工技术及其应用》", 31 March 2003, 兵器工业出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103818960A (en) * 2014-03-03 2014-05-28 浙江理工大学 Method for preparing alpha-MoO3 nanobelt by adopting hot-wire chemical vapor deposition technology
CN103818960B (en) * 2014-03-03 2015-06-17 浙江理工大学 Method for preparing alpha-MoO3 nanobelt by adopting hot-wire chemical vapor deposition technology
CN104649323A (en) * 2015-01-21 2015-05-27 济南大学 Preparation method of strip-shaped molybdenum trioxide
CN107021523A (en) * 2017-01-19 2017-08-08 青岛科技大学 A kind of orthorhombic phase α MoO3The preparation method and its photocatalytic applications of nanobelt

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Application publication date: 20131002