CN101348925A - Preparation of nano Fe/carrier composite powder - Google Patents
Preparation of nano Fe/carrier composite powder Download PDFInfo
- Publication number
- CN101348925A CN101348925A CNA2008101959161A CN200810195916A CN101348925A CN 101348925 A CN101348925 A CN 101348925A CN A2008101959161 A CNA2008101959161 A CN A2008101959161A CN 200810195916 A CN200810195916 A CN 200810195916A CN 101348925 A CN101348925 A CN 101348925A
- Authority
- CN
- China
- Prior art keywords
- composite powder
- carrier
- nanometer
- carrier composite
- suspension
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 239000000843 powder Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000000725 suspension Substances 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
- 238000004070 electrodeposition Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 230000009471 action Effects 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 150000002505 iron Chemical class 0.000 claims abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 18
- 238000005868 electrolysis reaction Methods 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 5
- 239000008151 electrolyte solution Substances 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 229960001866 silicon dioxide Drugs 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- -1 deionized water compound Chemical class 0.000 claims description 2
- 235000019850 ferrous citrate Nutrition 0.000 claims description 2
- 239000011640 ferrous citrate Substances 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- APVZWAOKZPNDNR-UHFFFAOYSA-L iron(ii) citrate Chemical compound [Fe+2].OC(=O)CC(O)(C([O-])=O)CC([O-])=O APVZWAOKZPNDNR-UHFFFAOYSA-L 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical class [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 1
- 159000000014 iron salts Chemical class 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 239000000969 carrier Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 239000013528 metallic particle Substances 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000004913 activation Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 150000001728 carbonyl compounds Chemical class 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 235000003891 ferrous sulphate Nutrition 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Images
Landscapes
- Electrolytic Production Of Metals (AREA)
Abstract
A preparation method for nano Fe/carrier composite powder comprises the following steps that carriers are evenly dispersed in the prepared iron salt solution through ultrasonic wave; then an acid is used to adjust a suspension liquid to an appropriate pH value so as to obtain a suspension liquid suitable for ultrasonic electrodeposition; the prepared suspension liquid is fed into an electrolytic cell which is under the action of ultrasonic sound and takes an iron sheet as electrodes, thereby obtaining a uniform and carrier-carried nano Fe/carrier composite powder suspension liquid under the continuous action of direct current; and finally, the suspension liquid is separated, and the separated product undergoes vacuum drying at a temperature of 40 DEG C so as to obtain the nano Fe/carrier composite powder. Moreover, the carriers are formed through the combination of any one sort, two sorts or three sorts of materials such as silicon dioxide, aluminum oxide and active carbon.
Description
Technical field
The present invention relates to a kind of nanometer Fe/carrier composite powder extremely widely of using in fields such as chemical industry, oil, environment protection, solid lubrication, magnetic storages, the present invention can the galvanic deposit ultrasound parameter changes carrier and the carrier addition supports in the nanometer Fe/carrier composite powder of different carriers, different-grain diameter with acquisition by controlling.
Background technology
Because the widespread use of nanometer Fe/carrier composite powder, and, make the research for preparing the Fe/ carrier composite powder for the galvanic deposit ultrasonic method to have extremely important practical value in the existing intrinsic deficiency for preparing Fe/ carrier composite powder method.
At present the main method of preparation Fe/ carrier composite powder has two kinds: 1, sonochemistry method: promptly the carbonyl compound of iron is decomposed and deposit on the carrier with action of ultrasonic waves, thus the Fe/ carrier composite powder of system.2, electroless plating: the application reductive agent is reduced to simple substance with the salt of iron, deposits on the carrier then.
But all there is inherent defect in above-mentioned two kinds of methods: the carbonyl compound that the sonochemistry method is used has severe toxicity, is unfavorable for environment protection; Electroless plating then owing to use reductive agent, is introduced impurity easily, is not easy to prepare pure material.And these two kinds of methods all need carrier is activated, and technology is loaded down with trivial details.
In sum, be badly in need of a kind of fast and convenient effective means of development now and prepare nanometer Fe/carrier composite powder.
Summary of the invention
The objective of the invention is: the fast and convenient method for preparing nanometer Fe/carrier composite powder effectively of a kind of application galvanic deposit ultrasonic method is proposed, and the preparation the cost of material is low, the quality height.
The present invention is achieved in that the preparation method of nanometer Fe/carrier composite powder, be dispersed in carrier in the iron salt solutions for preparing in advance by ultrasonic wave, regulate suspension to suitable pH value with acid then, obtain being suitable for the ultransonic suspension of galvanic deposit; The prepared suspension liquid injection is applied the electrolyzer of ultransonic use iron plate as electrode, under the direct current continuous action, evenly supported the nanometer Fe/carrier composite powder suspension on carrier.At last this suspension is separated, separated product finally obtains nanometer Fe/carrier composite powder 40 ℃ of vacuum-dryings.Described carrier refers to that a kind of, any two kinds or three kinds in the materials such as silicon-dioxide, aluminum oxide, gac combine.
The present invention adopts deionized water compound concentration 〉=10
-8MolL
-1Molysite electrolytic solution; The addition of carrier can be regulated according to the concentration and the electrodeposition time difference of electrolytic solution, thereby obtains from the composite powder of different Fe content such as 0.1%~90% grade; The pH value scope of suspension: 0.1~7.0; Current density range during electrolysis: 1mA/cm
2~1000mA/cm
2(electrode area unit); Electrolysis time: 1~6000min.
Especially pH value scope: 1~3; Current density range during electrolysis: 20mA/cm
2~250mA/cm
2
Especially used iron plate as anode electrode, thereby realized directly changing block Fe into the nanometer Fe particle.
Regulate the size and the Fe metal loading of Fe metallic particles easily by regulating methods such as concentration of electrolyte, carrier add-on, current density, electrodeposition time, ultrasonic frequency, ultrasonic power, thereby obtain the different nanometer Fe/carrier composite powder of various performances.
The present invention uses the galvanic deposit ultrasonic method, by to the change of galvanic deposit and ultrasonic processing parameter and to the control of carrier addition, preparation nanometer Fe/carrier composite powder.Directly the nanometer Fe metallic particles is supported on carrier, avoided the high temperature reduction of additive method or used reductive agent to prepare the shortcoming of nanometer Fe, and do not need carrier is carried out independent activation or modification processing.Technology of the present invention is simple, metal and carrier granule size adjustable, non-environmental-pollution.The present invention directly supports the nanometer Fe metallic particles on carrier, has avoided the high temperature reduction of additive method or has used reductive agent to prepare the shortcoming of nanometer Fe, and do not needed carrier is carried out independent activation or modification processing.
Beneficial effect of the present invention: galvanic deposit ultrasonic method method is easy, quick, and product property is controlled, and is with low cost, and environmental protection, and can prepare nanometer Fe/carrier composite powder is a kind of easy, general, method of being easy to industrialized production.
Description of drawings
Fig. 1 prepares the device synoptic diagram of nanometer Fe/carrier composite powder for the present invention
Fig. 2 is the XRD spectrum of prepared nanometer Fe/carrier composite powder
Fig. 3 is the prepared TEM photo (a)-(b) of nanometer Fe/carrier composite powder under different multiplying
Fig. 4 is the EDX figure of prepared nanometer Fe/carrier composite powder
Fig. 5 is the magnetzation curve of prepared nanometer Fe/carrier composite powder
Specific implementation method
The invention will be further described below in conjunction with accompanying drawing and by example:
Nanometer Fe/carrier composite powder preparation method: the soft silica microballoon by in the ultrasonic ferrous sulfate electrolytic solution that is dispersed in prior preparation, is regulated suspension to suitable pH value with acid then, obtain being used for the suspension of galvanic deposit.The prepared suspension liquid injection is applied the electrolyzer (shown in Figure 1) of ultransonic use iron plate as electrode, and under the direct current continuous action, processing condition are pH value scopes: 1~3, and current density range during electrolysis: 200-250mA/cm
2Electrode area unit); Electrolysis time: 15min.Evenly supported the nanometer Fe/carrier composite powder suspension on carrier.Ultrasonic frequency does not have particular requirement, generally selects 20-100MHz.At last this suspension is separated, separated product finally obtains nanometer Fe/carrier composite powder 40 ℃ of vacuum-dryings.Adopt alumina nano powder (the main distribution is the 20-80 micron) can obtain same result.
Adopt absorbent charcoal material also can, but particle diameter is thicker.
Wherein big, the current density of concentration of electrolyte greatly, then the Fe metallic particles is big, and Fe metal loading is also big;
Electrodeposition time is long, and also Fe metal loading is big, and the high more Fe metallic particles of ultrasonic frequency is more little
Molysite can adopt water-soluble molysite such as ferrous sulfate, iron protochloride, ferrous citrate.
Electrode 1,2 among Fig. 1, ultrasonic unit 3.
Figure 2 shows that concentration of electrolyte is 1.0 * 10
-5Mol/L, current density 20-30mA/cm
2, the silicon-dioxide add-on is 90% of Zong Quality amount, and ultrasonic electrodeposition time is 1h, the XRD spectrum of resultant catalyzer.
It is 1.0 * 10 that Fig. 3 (Fig. 3 a, Fig. 3 b are respectively the photo of different amplification) is depicted as concentration of electrolyte
-5Mol/L, current density 20-30mA/cm
2, the silicon-dioxide add-on is 90% of a gross weight, ultrasonic electrodeposition time is 1h, the TEM photo of resultant catalyzer under different enlargement ratios.
Claims (7)
1. the preparation method of nanometer Fe/carrier composite powder: it is characterized in that carrier is dispersed in by ultrasonic wave in the iron salt solutions for preparing in advance, regulate suspension to suitable pH value with acid then, obtain being suitable for the ultransonic suspension of galvanic deposit.The prepared suspension liquid injection is applied the electrolyzer of ultransonic use iron plate as electrode, under the direct current continuous action, evenly supported the nanometer Fe/carrier composite powder suspension on carrier; At last this suspension is separated, separated product finally obtains nanometer Fe/carrier composite powder 40 ℃ of vacuum-dryings; Carrier is that a kind of, any two kinds or three kinds in the materials such as silicon-dioxide, aluminum oxide, gac combine.
2. by the described nanometer Fe of claim 1/carrier composite powder preparation method, it is characterized in that with deionized water compound concentration 〉=10
-8MolL
-1Molysite electrolytic solution.
3. by the described nanometer Fe of claim 1/carrier composite powder preparation method, it is characterized in that the addition of carrier is regulated according to the concentration and the electrodeposition time difference of electrolytic solution, thereby obtain from the composite powder of 0.1%~90wt%Fe content; The pH value scope of suspension: 0.1~7.0; Current density range during electrolysis: 1mA/cm
2~1000mA/cm
2Electrolysis time: 1~6000min.
4. by the described nanometer Fe of claim 1/carrier composite powder preparation method, it is characterized in that using sulfated ferrous, iron protochloride or ferrous citrate water-soluble iron salts solution.
5. by the described nanometer Fe of claim 1/carrier composite powder preparation method, it is characterized in that using iron plate, directly change block Fe into the nanometer Fe particle as anode.
6. by the described nanometer Fe of claim 1/carrier composite powder preparation method, it is characterized in that regulating nanometer Fe particulate size and Fe metal content easily by regulating methods such as concentration of electrolyte, carrier add-on, current density, electrodeposition time, ultrasonic frequency, ultrasonic power.
7. by the described nanometer Fe of claim 3/carrier composite powder preparation method, it is characterized in that pH value scope 1~3; Current density range during electrolysis: 20mA/cm
2~250mA/cm
2
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2008101959161A CN101348925B (en) | 2008-09-11 | 2008-09-11 | Preparation of nano Fe/carrier composite powder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2008101959161A CN101348925B (en) | 2008-09-11 | 2008-09-11 | Preparation of nano Fe/carrier composite powder |
Publications (2)
Publication Number | Publication Date |
---|---|
CN101348925A true CN101348925A (en) | 2009-01-21 |
CN101348925B CN101348925B (en) | 2010-08-18 |
Family
ID=40267890
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN2008101959161A Expired - Fee Related CN101348925B (en) | 2008-09-11 | 2008-09-11 | Preparation of nano Fe/carrier composite powder |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN101348925B (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102839394A (en) * | 2012-09-17 | 2012-12-26 | 哈尔滨工业大学 | Method for rapidly preparing tree-like nano-iron with multi-level structure |
CN104928725A (en) * | 2015-07-07 | 2015-09-23 | 哈尔滨工业大学 | Method for efficiently preparing branch-shaped alpha-Fe wave absorbing material |
CN105236518A (en) * | 2015-07-02 | 2016-01-13 | 北京农业职业学院 | Magnetic-field-strengthening iron-carbon-microelectrolysis method for treating organic pollutants in landfill leachate |
CN107955952A (en) * | 2017-11-02 | 2018-04-24 | 马鞍山市宝奕金属制品工贸有限公司 | A kind of method using scum production high-purity iron powder |
-
2008
- 2008-09-11 CN CN2008101959161A patent/CN101348925B/en not_active Expired - Fee Related
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102839394A (en) * | 2012-09-17 | 2012-12-26 | 哈尔滨工业大学 | Method for rapidly preparing tree-like nano-iron with multi-level structure |
CN102839394B (en) * | 2012-09-17 | 2014-10-15 | 哈尔滨工业大学 | Method for rapidly preparing tree-like nano-iron with multi-level structure |
CN105236518A (en) * | 2015-07-02 | 2016-01-13 | 北京农业职业学院 | Magnetic-field-strengthening iron-carbon-microelectrolysis method for treating organic pollutants in landfill leachate |
CN105236518B (en) * | 2015-07-02 | 2018-03-23 | 北京农业职业学院 | A kind of method of organic pollution in magnetic field-intensification iron-carbon micro-electrolysis processing percolate |
CN104928725A (en) * | 2015-07-07 | 2015-09-23 | 哈尔滨工业大学 | Method for efficiently preparing branch-shaped alpha-Fe wave absorbing material |
CN107955952A (en) * | 2017-11-02 | 2018-04-24 | 马鞍山市宝奕金属制品工贸有限公司 | A kind of method using scum production high-purity iron powder |
Also Published As
Publication number | Publication date |
---|---|
CN101348925B (en) | 2010-08-18 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Zhang et al. | Recent advances and challenges of metal–organic framework/graphene-based composites | |
CN111097414B (en) | Simple method for loading superfine nano zero-valent iron on porous material | |
Fugare et al. | Study on structural, morphological, electrochemical and corrosion properties of mesoporous RuO2 thin films prepared by ultrasonic spray pyrolysis for supercapacitor electrode application | |
CN101348925B (en) | Preparation of nano Fe/carrier composite powder | |
Zhao et al. | A Bi‐Co Corridor Construction Effectively Improving the Selectivity of Electrocatalytic Nitrate Reduction toward Ammonia by Nearly 100% | |
CN110942924A (en) | Yeast cell-based Ni-Co-S-loaded porous carbon material and preparation method and application thereof | |
CN115233253A (en) | Electro-catalytic nitrate radical reduction ammonia production catalyst, and preparation method and application thereof | |
Gao et al. | Self-sustained recovery of silver with stainless-steel based Cobalt/Molybdenum/Manganese polycrystalline catalytic electrode in bio-electroreduction microbial fuel cell (BEMFC) | |
Feng et al. | Oxygenates from the electrochemical reduction of carbon dioxide | |
Zaabar et al. | Influence of nettle extract on zinc electrodeposition in an acidic bath: Electrochemical effect and coating morphology | |
CN113061931B (en) | CO (carbon monoxide)2Preparation method of electrode catalyst for electrochemical reduction | |
JP2000077070A (en) | Nickel hydroxide powder and its manufacture | |
CN114250482B (en) | High-load copper monatomic catalyst and preparation method and application thereof | |
CN105728039A (en) | Fullerene derivative/palladium nanoparticle film and preparation method and application thereof | |
CN106337275B (en) | A kind of spherical Cu on activated carbon fibre surface2O crystal films and preparation method thereof | |
CN110306199A (en) | A kind of carbon dioxide electro-catalysis reduction film and the preparation method and application thereof | |
CN114540840B (en) | FeCo/N-C nano composite material and preparation method and application thereof | |
Zhang et al. | Preparation of stainless steel mesh-supported ZnO and graphene/ZnO nanorod arrays with high photocatalytic performance | |
Bommireddy et al. | Surfactant mediated electrodeposition of copper nanostructures for environmental electrochemistry: influence of morphology on electrochemical nitrate reduction reaction | |
He et al. | Fabrication and nucleation study of β-PbO 2–Co 3 O 4 OER energy-saving electrode | |
Saini et al. | Rod-shaped copper (Cu, Cu2O) nano catalyst for the facile oxidation of methanol | |
CN114836786B (en) | Nickel-cobalt Prussian blue analogue nano-film material and preparation method thereof | |
CN114192749B (en) | Method for preparing nano material by electrodeposition based on corrosion amorphous alloy anode material | |
Budi et al. | TIME-DEPENDENT COMPOSITION OF THE ELECTRODEPOSITED NANOCRYSTALLINE Fe-Co-Ni FILMS. | |
Swaminathan et al. | An improved method of water electrolysis–effect of complexing agent |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100818 Termination date: 20130911 |