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Reduced preparation method for metal nanometer particle using hydroxy ion liquid

A technology of metal nanoparticles and ionic liquids, which is applied in the field of nano powder preparation, can solve the problems of a large amount of waste liquid, waste gas, complex methods, environmental pollution, etc., and achieve the advantages of avoiding the introduction of impurities, simple preparation process and high product purity Effect

Inactive Publication Date: 2007-04-25
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There have been a lot of reports on the preparation of nanoparticles. The preparation of metal nanoparticles by ordinary liquid phase reduction method has the advantages of being economical and easy to produce in large quantities, but the reaction steps are complicated, a large amount of modifiers must be added, and a large amount of waste liquid and gas are generated, which is harmful to the environment. Serious pollution, such as Chinese Patent Publication No. 1483539, 1672836, 1680060, US Patent No. 2005002829, No. 2004131937, etc.
In addition, metal nanomaterials are prepared in ordinary room temperature ionic liquids, such as Chinese Patent Publication No. 1559663A, which requires the addition of reducing agents, so that a large amount of other compounds remain in the ionic liquids, which will not only have a certain impact on the product, but also significantly Affect the catalytic properties of ionic liquid doped nanoparticles, affect the tribological properties of ionic liquid doped metal nanoparticles, some aspects greatly limit the application of ionic liquid doped metal nanoparticles, and these methods are more complicated, not conducive to Mass production

Method used

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  • Reduced preparation method for metal nanometer particle using hydroxy ion liquid
  • Reduced preparation method for metal nanometer particle using hydroxy ion liquid
  • Reduced preparation method for metal nanometer particle using hydroxy ion liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Example 1 Preparation of Ag nanoparticles

[0034] (1) Preparation of ionic liquid: Take 0.48mol chloroethanol and 0.32mol methylimidazole and reflux in 80°C oil bath for 24h. After the reaction, a viscous colorless transparent liquid is obtained. When the temperature drops to normal temperature, the amount of heat released becomes The solid was washed four times with ether to obtain a colorless crystal 1-hydroxyethyl-3-methylimidazolium chloride ionic liquid, which was dried in a vacuum oven at 80°C for 48 hours, and the dried 1-hydroxyethyl-3-methylimidazole Add 25g (0.15mol) of chloride ionic liquid into 150mL acetone, then add 19g (0.17mol) sodium fluoroborate, stir at room temperature for 24 hours, and filter with suction. The filter residue is a waxy solid, which is washed twice with acetone. Anhydrous MgSO 4 After drying overnight, the acetone was evaporated by rotary evaporation at 40°C, and then the water was evaporated by rotary evaporation in an oil bath at ...

Embodiment 2

[0036] Example 2 Preparation of Ag nanorods

[0037] (1) Weigh 0.85g AgNO 3 Dissolve in 50mL of distilled water, add 0.5g of thioglycolic acid dropwise after dissolving, a large amount of light yellow precipitates will gradually appear in the solution after mixing, after the addition of thioglycolic acid is completed, react for another hour, filter under normal pressure, and wash the product three times with distilled water , vacuum-dried at normal pressure, and finely ground after drying to obtain silver thioglycolate powder;

[0038] (2) Preparation of ionic liquid: 1-(4'-hydroxyl) butyl-3-methylimidazolium tetrafluoroborate ([C 4 OHmim] BF 4 ) The preparation steps of ionic liquid are the same as in Example 1;

[0039] (3) Add 10 mg of silver thioglycolate to 5 mL of 1-(4'-hydroxy)butyl-3-methylimidazolium tetrafluoroborate ([C 4 OHmim] BF 4 ) in the ionic liquid, ultrasonically dispersed, heated on an oil bath at 160°C for 4 hours, cooled to room temperature, centrifu...

Embodiment 3

[0040] Example 3 Preparation of Ag nanowires

[0041] (1) Preparation of ionic liquid: 1-(6'-hydroxyl) hexyl-3-methylimidazolium tetrafluoroborate ([C 6 OHmim] BF 4 ) The preparation steps of the ionic liquid are the same as in Example 1;

[0042](2) preparation of silver thioglycolate: with embodiment 2;

[0043] (3) Add 10 mg of silver thioglycolate to 5 mL of 1-(6'-hydroxyl) hexyl-3-methylimidazolium tetrafluoroborate ([C 6 OHmim] BF 4 ) in the ionic liquid, ultrasonically disperse it, keep the temperature in an oil bath at 160°C for 6 hours, cool to room temperature, and centrifuge the product, wash it four times with distilled water, and finally dry it under vacuum at room temperature. That is, Ag nanowires are obtained. The diameter distribution of the prepared Ag nanowires is wide, distributed between 40-100nm, and the length exceeds 5μm.

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Abstract

The invention relates to a method for using hydroxyl ion liquid to reduce and prepare metal nanometer particles. Wherein, it comprises that: (1), using the cation of hydroxyl group, as N-hydroxyalkyl pyridine ion, N- hydroxyalkyl-N-imidazolidinyl ion, etc, and one acid anion to prepare the ion liquid; (2), using ultrasonic wave to disperse or dissolve metal oxide, metal hydroxide or metal salt into ion liquid; (3), heating the liquid in oil bath; (40, separating the product, washing and vacuum drying. In said invention, the ion liquid can be used as solvent as well as reducer, to avoid inactive foreigner when using catalyst. And the ion liquid is non volatile with better thermal stability. The invention can avoid pollution.

Description

technical field [0001] The invention relates to a method for preparing metal nanoparticles by reduction of hydroxyl ionic liquid, which belongs to the field of nano powder preparation. Background technique [0002] Room temperature ionic liquid (ionic liquid) is a salt composed of anions and cations that is liquid near room temperature. As a novel medium, it has many characteristics different from common organic solvents: its liquid state Large temperature range, up to 300°C or more; can selectively dissolve inorganic salts that cannot be dissolved in many organic solvents; no significant vapor pressure; stable, non-flammable, and an environmentally friendly green solvent; therefore, ionic liquids are widely used In electrochemistry, catalysis, organic synthesis. [0003] There have been a lot of reports on the preparation of nanoparticles. The preparation of metal nanoparticles by ordinary liquid phase reduction method has the advantages of being economical and easy to pro...

Claims

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Application Information

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IPC IPC(8): B22F9/24
Inventor 张晟卯李健吴志申张治军
Owner HENAN UNIVERSITY
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