CN103551590A - Method for preparing dispersed iron nanoparticles from caprolactam type ionic liquid - Google Patents
Method for preparing dispersed iron nanoparticles from caprolactam type ionic liquid Download PDFInfo
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- CN103551590A CN103551590A CN201310542220.2A CN201310542220A CN103551590A CN 103551590 A CN103551590 A CN 103551590A CN 201310542220 A CN201310542220 A CN 201310542220A CN 103551590 A CN103551590 A CN 103551590A
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Abstract
The invention discloses a method for preparing dispersed iron nanoparticles from caprolactam type ionic liquid, and relates to dispersion and preparation methods for iron particles. The method comprises the following steps of adding a certain dispersing agent to dissolve a soluble ferrous or ferric salt into distilled water (or a mixed solution of distilled water and ethanol) to form an iron salt solution by adopting a liquid-phase chemical reduction method, directly reducing iron ions into zero-valent iron by adopting a reducing agent such as borohydride with high reducibility, and filtering, washing and vacuum-drying a product to obtain an iron nanopowder material with a nanoscale microstructure and higher dispersibility. The iron nanoparticles prepared by the method are spherical, narrow in particle size range and high in dispersibility and purity, and have small and uniform particle sizes and certain oxidation resistance, the problem of high agglomeration rate of the iron nanoparticles is effectively solved, a process is simple and easy to control, and is implemented under normal temperature and normal pressure, and actual production requirements are met.
Description
Technical field
The present invention relates to a kind of iron preparation method of granules,, particularly relate to a kind of caprolactam type ionic liquid dispersed iron nanoparticles preparation method.
Background technology
Conventionally particle size is called to nano material at powder or the material of 1～100 nanometer (nm) scope.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 therefore often that existing use is now made, all must starvation in preparation and while using, to 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 caprolactam type ionic liquid dispersed iron nanoparticles preparation method, utilize solvent directly in liquid reduction process, to add dispersant, effectively stop 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.
The object of the invention is to be achieved through the following technical solutions:
Caprolactam type ionic liquid dispersed iron nanoparticles preparation method, this Nanoscale Iron powder particle diameter, below 100nm, solves the agglomeration traits producing in Nanoscale Iron production process, and described method comprises:
(1) take 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, and 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 0.5-5%;
(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 ℃ of vacuum drying 10-24h, obtains black dispersed iron nanoparticles.
Described caprolactam type ionic liquid dispersed iron nanoparticles preparation method, described divalent iron salt is frerrous chloride, trivalent iron salt is ferric sulfate or iron chloride.
Described caprolactam type ionic liquid dispersed iron nanoparticles preparation method, described surfactant is soluble starch.
Described caprolactam type ionic liquid dispersed iron nanoparticles preparation method, described complexing agent is citric acid.
Described caprolactam type ionic liquid dispersed iron nanoparticles preparation method, described dispersant is caprolactam type ionic liquid.
Described caprolactam 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 is controlled easily;
3. under normal temperature and pressure, carry out manufacture process, meet production actual needs.
The specific embodiment
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 after 100 times of caprolactam type ionic liquid stoste dilutions, add in (2) gained solution, 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 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 10h, can obtain the finely dispersed nano iron particles of black.
Embodiment 2
Prepare dispersed iron nanoparticles, preparation process is:
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;
(8) 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;
(9) by after 100 times of caprolactam type ionic liquid stoste dilutions, add in (2) gained solution, making its content is 1:25(volume ratio);
(10) take sodium borohydride and be dissolved in distilled water, be made into the solution that sodium borohydride content is 0.02 mol/L;
(11) at (3) gained solution under stirring, solution (4) is splashed into and carries out reduction reaction, rate of addition is 10 milliliters/second, in course of reaction, temperature is controlled at 20 degrees Celsius, until react completely;
(12) 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;
(13) 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. caprolactam type ionic liquid dispersed iron nanoparticles preparation method, this Nanoscale Iron powder particle diameter, below 100nm, solves the agglomeration traits producing in Nanoscale Iron production process, it is characterized in that, and described method comprises:
Take solubility ferrous iron or trivalent iron salt as raw material, and with distilled water or distilled water and alcohol mixed solution, volume ratio is 7:3, and configuration solution, makes wherein iron concentration reach 0.2-2mol/L;
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;
In (2), add dispersant, make its volume ratio reach 0.5-5%;
The configuration boron hydride aqueous solution, making its concentration is 0.02-0.1mol/L;
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;
After (5) process finishes, gained product is carried out suction filtration, and repeatedly washs with distilled water and absolute ethyl alcohol;
(6) products therefrom, through 60 ℃ of vacuum drying 10-24h, obtains black dispersed iron nanoparticles.
2. caprolactam type ionic liquid dispersed iron nanoparticles preparation method according to claim 1, is characterized in that, described divalent iron salt is frerrous chloride, and trivalent iron salt is ferric sulfate or iron chloride.
3. caprolactam type ionic liquid dispersed iron nanoparticles preparation method according to claim 1, is characterized in that, described surfactant is soluble starch.
4. caprolactam type ionic liquid dispersed iron nanoparticles preparation method according to claim 1, is characterized in that, described complexing agent is citric acid.
5. caprolactam type ionic liquid dispersed iron nanoparticles preparation method according to claim 1, is characterized in that, described dispersant is caprolactam type ionic liquid.
6. caprolactam type ionic liquid dispersed iron nanoparticles preparation method according to claim 1, is characterized in that, described reducing agent is sodium borohydride or potassium borohydride.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104001935A (en) * | 2014-05-26 | 2014-08-27 | 沈阳化工大学 | [Hmim] HSO4- type ionic liquid disperse nano-iron particle preparation method |
| CN104001934A (en) * | 2014-05-26 | 2014-08-27 | 沈阳化工大学 | Preparing method for dispersing nanometer iron particles |
| CN104014806A (en) * | 2014-05-26 | 2014-09-03 | 沈阳化工大学 | Method for manufacturing nano-iron particles with TH-908 dispersed |
| CN105081340A (en) * | 2014-05-07 | 2015-11-25 | 沈阳农业大学 | Dispersed nano iron particle and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102133646A (en) * | 2011-03-23 | 2011-07-27 | 沈阳化工大学 | Preparation method of dispersed iron nanoparticles |
| CN103273077A (en) * | 2013-05-10 | 2013-09-04 | 沈阳化工大学 | Preparing method of [Bmim] BF4 dispersed nano-iron particle |
| CN103273075A (en) * | 2013-05-10 | 2013-09-04 | 沈阳化工大学 | HPAA nano-iron particle dispersing method |
| CN103273076A (en) * | 2013-05-10 | 2013-09-04 | 沈阳化工大学 | HDTMPA K6 nano-iron particle dispersing method |
-
2013
- 2013-11-06 CN CN201310542220.2A patent/CN103551590A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102133646A (en) * | 2011-03-23 | 2011-07-27 | 沈阳化工大学 | Preparation method of dispersed iron nanoparticles |
| CN103273077A (en) * | 2013-05-10 | 2013-09-04 | 沈阳化工大学 | Preparing method of [Bmim] BF4 dispersed nano-iron particle |
| CN103273075A (en) * | 2013-05-10 | 2013-09-04 | 沈阳化工大学 | HPAA nano-iron particle dispersing method |
| CN103273076A (en) * | 2013-05-10 | 2013-09-04 | 沈阳化工大学 | HDTMPA K6 nano-iron particle dispersing method |
Non-Patent Citations (1)
| Title |
|---|
| 冯婧微: "《中国博士学位论文全文数据库（电子期刊）》", 31 December 2012 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105081340A (en) * | 2014-05-07 | 2015-11-25 | 沈阳农业大学 | Dispersed nano iron particle and preparation method thereof |
| CN104001935A (en) * | 2014-05-26 | 2014-08-27 | 沈阳化工大学 | [Hmim] HSO4- type ionic liquid disperse nano-iron particle preparation method |
| CN104001934A (en) * | 2014-05-26 | 2014-08-27 | 沈阳化工大学 | Preparing method for dispersing nanometer iron particles |
| CN104014806A (en) * | 2014-05-26 | 2014-09-03 | 沈阳化工大学 | Method for manufacturing nano-iron particles with TH-908 dispersed |
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Application publication date: 20140205 |