CN103990809A - HCO3-type ionic liquid disperse nano-iron particle preparation method - Google Patents
HCO3-type ionic liquid disperse nano-iron particle preparation method Download PDFInfo
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- CN103990809A CN103990809A CN201410222940.5A CN201410222940A CN103990809A CN 103990809 A CN103990809 A CN 103990809A CN 201410222940 A CN201410222940 A CN 201410222940A CN 103990809 A CN103990809 A CN 103990809A
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Abstract
The invention provides a HCO3-type ionic liquid disperse nano-iron particle preparation method and relates to a nano metal particle preparation method. The HCO3-type ionic liquid disperse nano-iron particle preparation method comprises the steps of dissolving soluble bivalent or tervalent molysite in distilled water (or a distilled water and alcohol mixed solution) by adding a certain dispersing agent and adopting a liquid phase chemical reduction method to form a molysite solution, then adopting a reducing agent having strong reducing property, such as hydroboron to reduce iron ions into zero-valent iron. A product is filtered, washed and then subjected to vacuum drying to obtain a nano iron powder material having a nano microstructure and good dispersing performance. The nano-iron particles prepared by adopting the method are spherical, small in diameter and small in particle size range, have certain oxidation resistance and are high purity, small in size, even in diameter, and a process is simple and easy to control and meets the actual production demands under the normal temperature and normal pressure.
Description
Technical field
The present invention relates to a kind of preparation method of nano-metal particle, particularly relate to a kind of HCO
3 -type ionic liquid dispersed iron nanoparticles preparation method.
Background technology
Nano material all has a wide range of applications in every field because of its unique character.Nanoscale Iron is because of its transitional region between macroscopical Commen powder and the elementide of microcosmic, therefore present some unique character, one of them important characteristic is exactly skin effect.Because particle diameter is little, specific area is large, and surface-active is strong, and Nanoscale Iron has the advantage unique than common iron powder in pollutant reparation.External many researchs show many pollutants that Nanoscale Iron can reduce in removal water, as dissolving, property organic chloride, PCBs and nitrobenzene compounds etc.
Because Nanoscale Iron particle diameter is little, activity strong, easily coalescent, oxidizable, be often therefore that existing use is now made, in preparation with all must starvation while using, use inconveniently, cost is high, therefore, be restricted in actual applications, conventional preparation method has Physical and chemical method at present.Certain methods is possible in theory, but practical operation conditional request is very high, is not easy to accomplish.
Summary of the invention
The object of the present invention is to provide a kind of HCO
3 -type ionic liquid dispersed iron nanoparticles preparation method, the present invention utilizes solvent directly in liquid reduction process, to add dispersant, effectively stops the reunion of nano iron particles, make the Nanoscale Iron particle diameter produced little, be uniformly dispersed, particle size range is narrow, has good practical application effect.And technique is simple, cost is low, is convenient to further expand the scale of production.
The object of the invention is to be achieved through the following technical solutions:
A kind of HCO
3 -type ionic liquid dispersed iron nanoparticles preparation method, described method comprises the process of being prepared as follows:
(1), taking solubility ferrous iron or trivalent iron salt as raw material, with distilled water or distilled water and alcohol mixed solution, volume ratio is 7:3 configuration solution, makes wherein iron concentration reach 0.2-2mol/L;
(2) in (1), add surfactant, make its concentration reach 0.2-0.4g/L, add complexing agent to make its concentration reach 0.002-0.005g/L;
(3) in (2), add dispersant, make its volume ratio reach (1-2): 100;
(4) the configuration boron hydride aqueous solution, making its concentration is 0.02-0.1mol/L;
(5) in (3), gained solution, under stirring, splashes into solution (4) wherein, and dripping speed is 1-10ml/s, and course of reaction temperature is room temperature, drips solution (4) to reacting completely;
(6) after (5) process finishes, gained product is carried out suction filtration, and repeatedly washs with distilled water and absolute ethyl alcohol;
(7) (6) products therefrom, through 60 DEG C of vacuum drying 10-24h, obtains black dispersed iron nanoparticles.
Described a kind of HCO
3 -type ionic liquid dispersed iron nanoparticles preparation method, described divalent iron salt is frerrous chloride, described trivalent iron salt is ferric sulfate or iron chloride.
Described a kind of HCO
3 -type ionic liquid dispersed iron nanoparticles preparation method, described surfactant is soluble starch.
Described a kind of HCO
3 -type ionic liquid dispersed iron nanoparticles preparation method, described complexing agent is citric acid.
Described a kind of HCO
3 -type ionic liquid dispersed iron nanoparticles preparation method, described dispersant is HCO
3 -, i.e. bicarbonate ion type ionic liquid.
Described a kind of HCO
3 -type ionic liquid dispersed iron nanoparticles preparation method, described reducing agent is sodium borohydride or potassium borohydride.
Advantage of the present invention and effect are:
1, synthetic nano iron particles dispersion of materials performance is good, effectively solves nano iron particles agglomeration traits; And product purity is high, particle diameter is little, and epigranular has certain non-oxidizability;
2, synthetic route is simple, and technical process control is easy;
3, under normal temperature and pressure, carry out manufacture process, meet production actual needs.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
Prepare dispersed iron nanoparticles, preparation process is:
(1) take iron chloride, be dissolved in distilled water, be made into the solution that iron concentration is 0.8 mol/L;
(2) in (1), in gained solution, add surfactant soluble starch, make its concentration reach 0.4 grams per liter, add complexing agent citric acid, make its concentration reach 0.004 grams per liter;
(3) by HCO
3 -(bicarbonate ion) type ionic liquid stoste adds in (2) gained solution after diluting 100 times, and making its content is 0.5:100(volume ratio).
(4) take sodium borohydride and be dissolved in distilled water, be made into the solution that sodium borohydride content is 0.02 mol/L;
(5) at (3) gained solution under stirring, solution (4) is splashed into and carries out reduction reaction, rate of addition is 5 milliliters/second, in course of reaction, temperature is controlled at 20 degrees Celsius, until react completely;
(6) after (5) reaction finishes, the solid product suction filtration that reaction is obtained, and with distilled water drip washing product three times, absolute ethyl alcohol drip washing product three times;
(7) by (6) products therefrom in 60 degrees Celsius of vacuum drying 10h, can obtain the finely dispersed nano iron particles of black.
Embodiment 2
Prepare dispersed iron nanoparticles, preparation process is:
(1) take ferric sulfate, be dissolved in distilled water and absolute ethyl alcohol mixed solution (volume ratio=7:3), be made into the solution that iron concentration is 0.2 mol/L;
(2) in (1), in gained solution, add surfactant soluble starch, make its concentration reach 0.2 grams per liter, add complexing agent citric acid, make its concentration reach 0.002 grams per liter;
(3) by HCO
3 -(bicarbonate ion) type ionic liquid stoste adds in (2) gained solution after diluting 100 times, and making its content is 1:20(volume ratio).
(4) take sodium borohydride and be dissolved in distilled water, be made into the solution that sodium borohydride content is 0.02 mol/L;
(5) at (3) gained solution under stirring, solution (4) is splashed into and carries out reduction reaction, rate of addition is 1 milliliters/second, in course of reaction, temperature is controlled at 20 degrees Celsius, until react completely;
(6) after (5) reaction finishes, the solid product suction filtration that reaction is obtained, and with distilled water drip washing product three times, absolute ethyl alcohol drip washing product three times;
(7) by (6) products therefrom in 60 degrees Celsius of vacuum drying 24h, can obtain the finely dispersed nano iron particles of black.
Claims (6)
1. a HCO
3 -type ionic liquid dispersed iron nanoparticles preparation method, is characterized in that, described method comprises the process of being prepared as follows:
(1), taking solubility ferrous iron or trivalent iron salt as raw material, with distilled water or distilled water and alcohol mixed solution, volume ratio is 7:3 configuration solution, makes wherein iron concentration reach 0.2-2mol/L;
(2) in (1), add surfactant, make its concentration reach 0.2-0.4g/L, add complexing agent to make its concentration reach 0.002-0.005g/L;
(3) in (2), add dispersant, make its volume ratio reach (1-2): 100;
(4) the configuration boron hydride aqueous solution, making its concentration is 0.02-0.1mol/L;
(5) in (3), gained solution, under stirring, splashes into solution (4) wherein, and dripping speed is 1-10ml/s, and course of reaction temperature is room temperature, drips solution (4) to reacting completely;
(6) after (5) process finishes, gained product is carried out suction filtration, and repeatedly washs with distilled water and absolute ethyl alcohol;
(7) (6) products therefrom, through 60 DEG C of vacuum drying 10-24h, obtains black dispersed iron nanoparticles.
2. a kind of HCO according to claim 1
3 -type ionic liquid dispersed iron nanoparticles preparation method, is characterized in that, described divalent iron salt is frerrous chloride, and described trivalent iron salt is ferric sulfate or iron chloride.
3. a kind of HCO according to claim 1
3 -type ionic liquid dispersed iron nanoparticles preparation method, is characterized in that, described surfactant is soluble starch.
4. a kind of HCO according to claim 1
3 -type ionic liquid dispersed iron nanoparticles preparation method, is characterized in that, described complexing agent is citric acid.
5. a kind of HCO according to claim 1
3 -type ionic liquid dispersed iron nanoparticles preparation method, is characterized in that, described dispersant is HCO
3 -be bicarbonate ion) type ionic liquid.
6. a kind of HCO according to claim 1
3 -type ionic liquid dispersed iron nanoparticles preparation method, is characterized in that, described reducing agent is sodium borohydride or potassium borohydride.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060088918A (en) * | 2005-02-02 | 2006-08-07 | (주)엔 파우다 | Method for manufacturing metal powder |
| KR20090055380A (en) * | 2007-11-28 | 2009-06-02 | 광주과학기술원 | Methods of controllable synthesis of nanoscale zerovalent iron |
| CN102133646A (en) * | 2011-03-23 | 2011-07-27 | 沈阳化工大学 | Preparation method of dispersed iron nanoparticles |
| CN103611944A (en) * | 2013-11-26 | 2014-03-05 | 沈阳化工大学 | Preparation method of ClO3- ionic liquid dispersed iron nanoparticles |
| CN103769599A (en) * | 2014-01-06 | 2014-05-07 | 沈阳化工大学 | Disperse nano-iron particle preparing method |
-
2014
- 2014-05-26 CN CN201410222940.5A patent/CN103990809A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060088918A (en) * | 2005-02-02 | 2006-08-07 | (주)엔 파우다 | Method for manufacturing metal powder |
| KR20090055380A (en) * | 2007-11-28 | 2009-06-02 | 광주과학기술원 | Methods of controllable synthesis of nanoscale zerovalent iron |
| CN102133646A (en) * | 2011-03-23 | 2011-07-27 | 沈阳化工大学 | Preparation method of dispersed iron nanoparticles |
| CN103611944A (en) * | 2013-11-26 | 2014-03-05 | 沈阳化工大学 | Preparation method of ClO3- ionic liquid dispersed iron nanoparticles |
| CN103769599A (en) * | 2014-01-06 | 2014-05-07 | 沈阳化工大学 | Disperse nano-iron particle preparing method |
Non-Patent Citations (1)
| Title |
|---|
| 冯婧微: "纳米零价铁及铁（氢）氧化物去除水中Cr（Ⅵ）和Cu2+的机制研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Application publication date: 20140820 |