CN101348925B - Preparation of nano Fe/carrier composite powder - Google Patents
Preparation of nano Fe/carrier composite powder Download PDFInfo
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- CN101348925B CN101348925B CN2008101959161A CN200810195916A CN101348925B CN 101348925 B CN101348925 B CN 101348925B CN 2008101959161 A CN2008101959161 A CN 2008101959161A CN 200810195916 A CN200810195916 A CN 200810195916A CN 101348925 B CN101348925 B CN 101348925B
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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 (4)
1. the preparation method of nanometer Fe/carrier composite powder: it is characterized in that carrier is dispersed in by ultrasonic wave in ferrous sulfate, iron protochloride or the ferrous citrate water-soluble iron salts solution for preparing in advance, regulate the pH value scope of suspension then with acid: 0.1～7.0; 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, use iron plate, directly change block Fe into the nanometer Fe particle as anode; 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 silicon-dioxide, aluminum oxide or the absorbent charcoal material combine; The addition of carrier is regulated according to the concentration and the electrodeposition time difference of electrolytic solution, thereby obtains from the composite powder of 0.1%～90wt%Fe content; Current density range during electrolysis: 1mA/cm
2～1000mA/cm
2Electrolysis time: 1～6000min.
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 regulating nanometer Fe particulate size and Fe metal content by the method for regulating concentration of electrolyte, carrier add-on, current density, electrodeposition time, ultrasonic frequency or ultrasonic power.
4. by the described nanometer Fe of claim 1/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
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|---|---|---|---|
| CN2008101959161A CN101348925B (en) | 2008-09-11 | 2008-09-11 | Preparation of nano Fe/carrier composite powder |
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| CN2008101959161A CN101348925B (en) | 2008-09-11 | 2008-09-11 | Preparation of nano Fe/carrier composite powder |
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| CN101348925B true CN101348925B (en) | 2010-08-18 |
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| 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 |
| 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 |
| CN104928725B (en) * | 2015-07-07 | 2017-07-28 | 哈尔滨工业大学 | A kind of method for efficiently preparing dendritic α Fe absorbing materials |
| 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 |
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Granted publication date: 20100818 Termination date: 20130911 |