CN105040069A - Method for preparing porous nanometer material Na6Mo7O24 14H2O through electrochemistry anodic oxidation method - Google Patents

Method for preparing porous nanometer material Na6Mo7O24 14H2O through electrochemistry anodic oxidation method Download PDF

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CN105040069A
CN105040069A CN201510527507.7A CN201510527507A CN105040069A CN 105040069 A CN105040069 A CN 105040069A CN 201510527507 A CN201510527507 A CN 201510527507A CN 105040069 A CN105040069 A CN 105040069A
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anodic oxidation
nanometer material
electrolytic solution
porous nanometer
cleaning
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CN105040069B (en
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杨敏
靳博文
徐慧芳
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention relates to a preparing method of a Na6Mo7O24 14H20 14H2O nanometer material, and in particular to a method for preparing the porous nanometer material Na6Mo7O24 14H2O through an electrochemistry anodic oxidation method to solve the problems that an existing Na6Mo7O24 14H2O nanometer material preparing technology is complex, and the preparing time is long. The method comprises the steps that firstly, an Mo piece is cleaned; secondly, Na2S is added in deionized water to be stirred and dissolved, then, NH4F is added in a mixture and stirred, glycerin is added in a bath solution to be mixed evenly, and the bath solution is obtained; thirdly, the cleaned Mo piece serves as an anode, a Pt piece serves as a cathode, the Mo piece and the Pt piece are added in the bath solution and completely immersed in the bath solution, voltage is added across the two ends of the cathode and the anode, and the anode is oxidized to obtain the oxidized Mo piece; and fourthly, cleaning and drying are carried out, and then the non-shaped Na6Mo7O24 14H2O is finally obtained. The preparing technology is simple, convenient to implement and low in cost. The method is used for preparing the Na6Mo7O24 14H2O material.

Description

A kind of electrochemistry anodic oxidation prepares porous nanometer material Na 6mo 7o 2414H 2the method of O
Technical field
The present invention relates to a kind of Na 6mo 7o 2414H 2the preparation method of O nano material.
Background technology
Research about nano material has had a lot of reports, because the reduction of particle can change the change of a lot of body phase performance in crystal.By controlling granular size, moiety and internal structure synthetizing inorganic nanocrystal body, and change geomery and obtain different performance material, have a lot of application in a lot of field.Molybdate receives publicity because of its application on inorganic inhibitor and metal deactivator.Sodium orthomolybdate is the staple product in molybdate, and its output and consumption are only second to ammonium molybdate, and it is substantially harmless to human body, therefore can make inhibiter and replace poisonous nitrite, chromic salt that even can be carcinogenic, become the first-selected material of environmental protection circle.But also do not have a kind of method effectively efficiently to prepare the nano material of porous so far, therefore exploitation is a kind of simple, preparation with low cost Na 6mo 7o 2414H 2the method of O is significant.
Summary of the invention
The present invention will solve existing Na 6mo 7o 2414H 2o nano material complicated process of preparation, the problem that preparation time is long, provides a kind of electrochemistry anodic oxidation to prepare porous nanometer material Na 6mo 7o 2414H 2the method of O.
Electrochemistry anodic oxidation of the present invention prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, carry out according to the following steps:
One, clean: adopt acetone, dehydrated alcohol and deionized water to be that clean-out system carries out ultrasonic cleaning to Mo sheet successively, removing Mo sheet surface and oil contaminant and impurity, be placed on air drying after cleaning, obtain cleaning rear Mo sheet;
Two, electrolytic solution is prepared: first by Na 2s joins in deionized water, utilizes magnetic stirring apparatus by its stirring and dissolving, adds NH afterwards 4f, continues to stir, then adds glycerol to electrolytic solution, continues stirring and glycerol is mixed with deionized water, obtain electrolytic solution;
Three, anodic oxidation treatment: using the Mo sheet after cleaning as anode, Pt sheet, as negative electrode, adds electrolytic solution, makes electrode be immersed in electrolytic solution, adds the volts DS of 10 ~ 40V at anode and cathode two ends, and anodic oxidation 1 hour obtains the Mo sheet after oxidation;
Four, cleaning-drying: the Mo sheet after oxidation to be dipped in dehydrated alcohol 30 minutes, is then placed in vacuum drying oven dry, takes out afterwards and obtains unformed Na 6mo 7o 2414H 2o.
Advantage of the present invention:
The inventive method significantly can reduce preparation Na 6mo 7o 2414H 2the complexity of O nano material technique, preparation technology is easy, just can obtain Na at normal temperatures 6mo 7o 2414H 2o nano material, and generated time obviously shortens, whole process only needs 2 hours.The inventive method operation steps obtains Na by electrochemistry anodic oxidation one step 6mo 7o 2414H 2o, the inventive method can obtain the Na of porous 6mo 7o 2414H 2o nano material is compared the Na prepared with other method 6mo 7o 2414H 2o, mild condition, synthetic method is simple, does not need to carry out at high temperature under high pressure.And reaction raw materials is the common raw material be easy to get, the product utilizing ammonium molybdate obtained with traditional method, obviously reduces the cost needed for synthesis.The product that present method obtains has larger surface-area compared with the product that additive method obtains, and the avtive spot of reaction increases, and is conducive to improving catalytic activity.
Accompanying drawing explanation
Fig. 1 is Na prepared by embodiment 1 6mo 7o 2414H 2o material amplifies the electron scanning micrograph of 10000 times; Fig. 2 is Na prepared by embodiment 1 6mo 7o 2414H 2o material amplifies the electron scanning micrograph of 35000 times; Fig. 3 is Na prepared by embodiment 1 6mo 7o 2414H 2the EDS test result of O material; Fig. 4 is Na prepared by embodiment 1 6mo 7o 2414H 2the XRD test result of O material; Fig. 5 is Na prepared by embodiment 1 6mo 7o 2414H 2o material Tafel curve test result.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment electrochemistry anodic oxidation prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, carry out according to the following steps:
One, clean: adopt acetone, dehydrated alcohol and deionized water to be that clean-out system carries out ultrasonic cleaning to Mo sheet successively, after cleaning, be placed on air drying, obtain cleaning rear Mo sheet;
Two, electrolytic solution is prepared: first by Na 2s joins in deionized water, utilizes magnetic stirring apparatus by its stirring and dissolving, adds NH afterwards 4f, continues to stir, then adds glycerol to electrolytic solution, continues stirring and glycerol is mixed with deionized water, obtain electrolytic solution;
Three, anodic oxidation treatment: using the Mo sheet after cleaning as anode, Pt sheet, as negative electrode, adds electrolytic solution, makes electrode be immersed in electrolytic solution, adds the volts DS of 10 ~ 40V at anode and cathode two ends, and anodic oxidation 1 hour obtains the Mo sheet after oxidation;
Four, cleaning-drying: the Mo sheet after oxidation to be dipped in dehydrated alcohol 30 minutes, is then placed in vacuum drying oven dry, takes out afterwards and obtains unformed Na 6mo 7o 2414H 2o.
Embodiment two: present embodiment and embodiment one unlike: the ultrasonic cleaning concrete operations described in step one are as follows: take first acetone as clean-out system, clean 5 ~ 10 minutes under ultrasonic frequency is 100kHz; Then take dehydrated alcohol as clean-out system, cleaning 5 ~ 10 minutes under ultrasonic frequency is 100kHz, take finally deionized water as clean-out system, cleans 5 ~ 10 minutes, namely complete ultrasonic cleaning under ultrasonic frequency is 100kHz.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one are unlike NH in the electrolytic solution that step 2 obtains 4the concentration of F is 0.2 ~ 0.5mol/L.Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one are unlike NH in the electrolytic solution that step 2 obtains 4the concentration of F is 0.3 ~ 0.4mol/L.Other is identical with embodiment one.
Embodiment five: present embodiment and embodiment one are unlike Na in the electrolytic solution that step 2 obtains 2the concentration of S is 0.005 ~ 0.5mol/L.Other is identical with embodiment one.
Embodiment six: present embodiment and embodiment one are unlike Na in the electrolytic solution that step 2 obtains 2the concentration of S is 0.05 ~ 0.4mol/L.Other is identical with embodiment one.
Embodiment seven: present embodiment and embodiment one are unlike Na in the electrolytic solution that step 2 obtains 2the concentration of S is 0.1 ~ 0.3mol/L.Other is identical with embodiment one.
Embodiment eight: present embodiment and embodiment one unlike: in step 2, the volume ratio of glycerol and deionized water is 4 ~ 19:1.Other is identical with embodiment one.
Embodiment nine: present embodiment and embodiment one unlike: in step 2, the volume ratio of glycerol and deionized water is 8 ~ 15:1.Other is identical with embodiment one.
Embodiment ten: present embodiment and embodiment one unlike: in step 2, the volume ratio of glycerol and deionized water is 9:1.Other is identical with embodiment one.
Embodiment 11: present embodiment and embodiment one unlike: in step 4, drying temperature is 60 DEG C.Other is identical with embodiment one.
For verifying beneficial effect of the present invention, carry out following test:
Embodiment 1:
The present embodiment electrochemistry anodic oxidation prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, carry out according to the following steps:
One, clean: the ultrasonic cleaning concrete operations described in step one are as follows: take first acetone as clean-out system, clean 5 ~ 10 minutes under ultrasonic frequency is 100kHz; Then take dehydrated alcohol as clean-out system, cleaning 5 ~ 10 minutes under ultrasonic frequency is 100kHz, is finally clean-out system with deionized water, clean 5 ~ 10 minutes under ultrasonic frequency is 100kHz, namely complete ultrasonic cleaning, after cleaning, be placed on air drying, obtain cleaning rear Mo sheet;
Two, electrolytic solution is prepared: get 10mL deionized water, add 1.2gNa 2s, stirs and makes it dissolve, then add 1.3gNH 4f, mixes, and finally adds 90mL glycerol, continues stirring 4 hours, obtained 100mL electrolytic solution;
Three, anodic oxidation treatment: using the Mo sheet after cleaning as anode, be of a size of: long 1.5cm, wide 1.5cm, thick 0.1mm.Pt sheet is as negative electrode, and electrode area is 1cm × 1cm.Two interelectrode distances are 1cm.Get 15mL electrolytic solution, pour in electrolyzer, make two electrodes be immersed in electrolytic solution, utilize constant voltage power supply to add the volts DS of 10V at anode and cathode two ends, anodic oxidation 1 hour, obtain the Mo sheet after oxidation;
Four, cleaning-drying: the Mo sheet after oxidation to be dipped in dehydrated alcohol 30 minutes, be then placed in vacuum drying oven dry, drying temperature is 60 DEG C, takes out afterwards and obtains unformed Na 6mo 7o 2414H 2o.Testing and characterization is carried out to it.
(1) SEM test result:
Fig. 1 is Na 6mo 7o 2414H 2o material amplifies the electron scanning micrograph of 10000 times.Drawn at the MoS forming porous after anodic oxidation on Mo surface by Fig. 1 2.Fig. 2 is Na 6mo 7o 2414H 2o material amplifies the electron scanning micrograph of 35000 times, can see the vesicular structure on its surface, and the internal diameter in hole is approximately 200-400nm.
(2) EDS test:
Na 6mo 7o 2414H 2eDS test result as shown in Figure 3, arranges and obtains the elementary composition of table 1 product by the EDS test result of O material.
Table 1
Element Weight percent Atomic percent
CK 22.18 39.01
OK 17.80 23.49
FK 14.66 16.29
NaK 7.19 6.60
SK 14.13 9.31
MoL 24.04 5.29
Total amount 100.00
Result in table 1 show sample by Mo, C, Na, F, O, S form, wherein a small amount of C, S, F from growth Na 6mo 7o 2414H 2the electrolytic solution of O nanoporous.S is that additive is adsorbed on Mo surface, and C is mainly due to the machine oil in the thoroughly not remaining partial glycerol of cleaning and scanning electronic microscope.
(3) XRD test:
Na 6mo 7o 2414H 2the XRD test result of O material as shown in Figure 4, in Fig. 4 ◆ represent Na 6mo 7o 2414H 2o, represent NaF.The X-ray diffraction pattern of product and PowerDiffractionFile (PDF) card [73-0278] the rhombic Na of JCPDS (JointCommitteeForPowderDiffractionStandards, JCPDS) 6mo 7o 2414H 2o, [36-1455] NaF is basically identical.Wherein NaF may be due to the Na in solution +with F +mo surface is attached in conjunction with the NaF formed.
(4) Tafel curve test;
Tafel curve test result as shown in Figure 5, in Fig. 5 ,-▲-represent pure iron+Na 6mo 7o 2414H 2o ,-■-represent pure iron.In the NaCl solution of 3.5%, working electrode selects area to be the Fe sheet of 1cm, adopts Pt electrode to electrode, and reference electrode adopts saturated calomel electrode.Result surface is found out and is added a small amount of (about 10mg) Na 6mo 7o 2414H 2after O, corrosion current is substantially constant, but corrosion potential becomes-0.552V from-0.641V, and corrosion potential improves 89mV, can reduce the corrosion of iron and steel to a certain extent.Na 6mo 7o 2414H 2o can reduce the corrosion of iron and steel as a kind of inhibiter.
The preparation method of the present embodiment is simple, and whole process only needs 2 hours.The Na of preparation 6mo 7o 2414H 2o material is porous nanometer material, has larger surface-area, and the avtive spot of reaction increases, and is conducive to improving catalytic activity.

Claims (10)

1. an electrochemistry anodic oxidation prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, is characterized in that the method is carried out according to the following steps:
One, clean: adopt acetone, dehydrated alcohol and deionized water to be that clean-out system carries out ultrasonic cleaning to Mo sheet successively, after cleaning, be placed on air drying, obtain cleaning rear Mo sheet;
Two, electrolytic solution is prepared: first by Na 2s joins in deionized water, utilizes magnetic stirring apparatus by its stirring and dissolving, adds NH afterwards 4f, continues to stir, then adds glycerol to electrolytic solution, continues stirring and glycerol is mixed with deionized water, obtain electrolytic solution;
Three, anodic oxidation treatment: using the Mo sheet after cleaning as anode, Pt sheet, as negative electrode, adds electrolytic solution, makes electrode be immersed in electrolytic solution, adds the volts DS of 10 ~ 40V at anode and cathode two ends, and anodic oxidation 1 hour obtains the Mo sheet after oxidation;
Four, cleaning-drying: the Mo sheet after oxidation to be dipped in dehydrated alcohol 30 minutes, is then placed in vacuum drying oven dry, takes out afterwards and obtains unformed Na 6mo 7o 2414H 2o.
2. a kind of electrochemistry anodic oxidation according to claim 1 prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, is characterized in that the ultrasonic cleaning concrete operations described in step one are as follows: take first acetone as clean-out system, cleans 5 ~ 10 minutes under ultrasonic frequency is 100kHz; Then take dehydrated alcohol as clean-out system, cleaning 5 ~ 10 minutes under ultrasonic frequency is 100kHz, take finally deionized water as clean-out system, cleans 5 ~ 10 minutes, namely complete ultrasonic cleaning under ultrasonic frequency is 100kHz.
3. a kind of electrochemistry anodic oxidation according to claim 1 prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, is characterized in that NH in the electrolytic solution that step 2 obtains 4the concentration of F is 0.2 ~ 0.5mol/L.
4. a kind of electrochemistry anodic oxidation according to claim 1 prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, is characterized in that NH in the electrolytic solution that step 2 obtains 4the concentration of F is 0.3 ~ 0.4mol/L.
5. a kind of electrochemistry anodic oxidation according to claim 1 prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, is characterized in that Na in the electrolytic solution that step 2 obtains 2the concentration of S is 0.005 ~ 0.5mol/L.
6. a kind of electrochemistry anodic oxidation according to claim 1 prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, is characterized in that Na in the electrolytic solution that step 2 obtains 2the concentration of S is 0.05 ~ 0.4mol/L.
7. a kind of electrochemistry anodic oxidation according to claim 1 prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, is characterized in that Na in the electrolytic solution that step 2 obtains 2the concentration of S is 0.1 ~ 0.3mol/L.
8. a kind of electrochemistry anodic oxidation according to claim 1 prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, is characterized in that the volume ratio of glycerol and deionized water in step 2 is 4 ~ 19:1.
9. a kind of electrochemistry anodic oxidation according to claim 1 prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, is characterized in that the volume ratio of glycerol and deionized water in step 2 is 9:1.
10. a kind of electrochemistry anodic oxidation according to claim 1 prepares porous nanometer material Na 6mo 7o 2414H 2the method of O, is characterized in that in step 4, drying temperature is 60 DEG C.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107059038A (en) * 2017-04-27 2017-08-18 北京航空航天大学 Metal sulfide electrode, preparation method and applications with hydrogen reduction activity
CN110684990A (en) * 2018-07-04 2020-01-14 国家纳米科学中心 Molybdenum phosphide nano material and preparation method and application thereof
CN113061954A (en) * 2021-03-15 2021-07-02 深圳大学 Method for preparing metal molybdate by anodic oxidation method, metal molybdate and application thereof
CN113355716A (en) * 2021-06-15 2021-09-07 北京化工大学 Preparation of mesoporous MoO by electrochemical anodic oxidation method2Method (2)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107059038A (en) * 2017-04-27 2017-08-18 北京航空航天大学 Metal sulfide electrode, preparation method and applications with hydrogen reduction activity
CN110684990A (en) * 2018-07-04 2020-01-14 国家纳米科学中心 Molybdenum phosphide nano material and preparation method and application thereof
CN113061954A (en) * 2021-03-15 2021-07-02 深圳大学 Method for preparing metal molybdate by anodic oxidation method, metal molybdate and application thereof
CN113355716A (en) * 2021-06-15 2021-09-07 北京化工大学 Preparation of mesoporous MoO by electrochemical anodic oxidation method2Method (2)
CN113355716B (en) * 2021-06-15 2022-10-04 北京化工大学 Preparation of mesoporous MoO by electrochemical anodic oxidation method 2 Method (2)

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