CN1274588C - Method for synthesizing nano-size lanthanide metal hydride from lanthanide metal under nalohydrocarbon action - Google Patents
Method for synthesizing nano-size lanthanide metal hydride from lanthanide metal under nalohydrocarbon action Download PDFInfo
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- CN1274588C CN1274588C CNB021582181A CN02158218A CN1274588C CN 1274588 C CN1274588 C CN 1274588C CN B021582181 A CNB021582181 A CN B021582181A CN 02158218 A CN02158218 A CN 02158218A CN 1274588 C CN1274588 C CN 1274588C
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Abstract
Materials are the material basis of human civilization, and novel material industry is a novel growing point for the development of national economy. The research of nanometer materials becomes one of most important technological advanced technologies regarded all over the world. A novel method for synthesizing various lanthanide series metal hydrides with the size of nanometer in organic solvent and under the conditions of normal temperature and pressure under the action of halogenated hydrocarbon. The measuring result of transmission electron microscopes (TEM) indicates that the basic granule diameter range of the lanthanide series metal hydride is smaller than 40 nm. The method is characterized in that metal organic activating agents are not required to be added in the synthesis of lanthanide series metal hydrides with the size of nanometer, and thereby, the existence of trace metal impurities is avoided in products.
Description
Technical Field
The present invention relates to a method for synthesizing nano-size lanthanide metal hydride from lanthanide metal under the action of halohydrocarbon and in organic solvent under the condition of normal temp. and normal pressure.
Background
Nanomaterial science is an emerging discipline that is rapidly developing. The nano material has the size effect and the surface characteristic, not only shows extremely high reactivity, but also shows coalescence instability, so that the synthesis of the nano metal hydride material with small crystal grains, large specific surface area and high reactivity is difficult and challenging work. The nano lanthanide metal hydride has wide application value in the fields of catalytic chemistry, synthetic chemistry, material science, energy, environmental protection and the like, and can generate direct economic benefit.
The preparation method of the nanomaterial is generally classified into a physical method and a chemical method. Chemical processes produce nanomaterials primarily through appropriate chemical reactions, including liquid, gas and solid phase reactions. The method of the invention, namely the method for synthesizing nano-sized lanthanide metal hydride from lanthanide metal under the action of halogenated hydrocarbon, is not reported in the literature at present.
Disclosure of Invention
The invention aims to provide a novel method for synthesizing nano-sized lanthanide metal hydride from lanthanide metal under the action of halogenated hydrocarbon at 0-60 ℃.
The method can be represented by the following reaction formula:
adding metal powder into a reaction bottle, adding an organic solvent and halohydrocarbon, controlling the temperature by an oil bath, magnetically stirring, and carrying out hydrogenation reaction.
The organic solvent is any one of toluene, methyl ethyl ketone, pyridine, n-butyl ether, isoamyl ether, tetrahydrofuran and 1, 4-dioxane, and toluene is preferred.
The halogenated hydrocarbon is any one of aliphatic halogenated hydrocarbon and aromatic halogenated hydrocarbon (R-X, Ar-X), and preferably ethyl bromide.
Drawings
FIG. 1 is an electron Transmission Electron Microscope (TEM) of nano lanthanum hydride.
Detailed Description
The invention is further illustrated by the following examples.
EXAMPLE 1 Synthesis of nanosized lanthanum hydride
3.47g (25mmol) of scrap metal lanthanum (produced by Beijing institute of nonferrous metals, purity>99.5%), 15.0mL of toluene and 0.015mL of bromoethane were added to a reaction flask connected to a constant-pressure hydrogen burette, the temperature of the oil bath was controlled (45 ℃), the magnetic stirrer was opened, and hydrogen was introduced. After 58 hours, the hydrogenation reaction of lanthanum metal is stopped, and the hydrogen absorption amount of the reaction is directly read by a constant pressure burette. The organic phase in the reaction flask was separated, the solid phase was washed twice with toluene and dried in a vacuum oil bath (80 ℃) for 1 hour to give a black solid powder of lanthanum hydride.
The halogenated hydrocarbon functions in that it enables the quantitative conversion of lanthanum into nanosized lanthanum hydride. Composition of nanosized rare earth metal hydrides to non-stoichiometric value, LnHmWherein m is between 2 and 3. TEM measurement results show that the lanthanum hydride synthesized by the novel method has basic particle size less than 40 nm. The XRD test result shows that the lanthanum hydride structure is cubic crystal.
EXAMPLE 2 Synthesis of nanosized Neodymium hydrides by the action of halogenated hydrocarbons
Nanometer-sized neodymium hydride was synthesized according to the method of example 1. The metallic neodymium hydrogenation reaction was stopped after 68 hours. The TEM measurement results show that the basic particle size is less than 40 nm.
EXAMPLE 3 Synthesis of nanosized samarium hydrides by the action of halogenated hydrocarbons
Nanosized samarium hydride was synthesized according to the method of example 1. After 120 hours, the hydrogenation reaction of the metal samarium is stopped. The TEM measurement results show that the basic particle size is less than 40 nm.
EXAMPLE 4 Synthesis of nanosized dysprosium hydride by halogenated hydrocarbons
Dysprosium hydride of nanometer size was synthesized according to the method of example 1. After 170 hours, the hydrogenation reaction of metallic dysprosium is stopped. The TEM measurement results show that the basic particle size is less than 40 nm.
EXAMPLE 5 Synthesis of nanosized ytterbium hydride by halogenated hydrocarbons
Nanometer-sized ytterbium hydride was synthesized according to the method of example 1. The ytterbium metal hydrogenation reaction was stopped after 260 hours. The TEM measurement results show that the basic particle size is less than 40 nm.
The experimental result shows that the synthesis reaction speed of the light rare earth lanthanum and neodymium nano hydride is higher; the synthesis reaction of the heavy rare earth nanometer ytterbium hydride is relatively slow. The amount of halogenated hydrocarbon used in the synthesis reaction (halogenated hydrocarbon: molar ratio of the reactants) can be as low as 0.1%. The experimental results show that when the dosage of the halogenated hydrocarbon is increased, the reaction speed is accelerated, and the reaction time is obviously shortened.
In this synthesis reaction, the halogenated hydrocarbon functions to quantitatively convert the lanthanide metal to the corresponding nanosized metal hydride.
The method is characterized in that the synthesized nano-sized lanthanide metal hydride does not contain a metal organic activator, thereby avoiding the possibility of introducing trace metal impurities into the product.
The present invention is an efficient method for synthesizing nanosized lanthanide metal hydrides.
Claims (3)
1. A process for synthesizing the nano-class hydride of lanthanide metal features that under the action of the halohydrocarbon chosen from aliphatic halohydrocarbon and aromatic halohydrocarbon, the different lanthanide metal powder and hydrogen are reacted for 58-260 hr in the organic solvent chosen from toluene, methyl ethyl ketone, pyridine, n-butyl ether, isopentyl ether, tetrahydrofuran and 1, 4-dioxane at 0-60 deg.C and ordinary pressure to obtain the hydride of lanthanide metal whose particle size is less than 40 nm.
2. The process of claim 1, wherein the organic solvent is toluene.
3. The process of claim 1 wherein the halogenated hydrocarbon is bromoethane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021582181A CN1274588C (en) | 2002-12-19 | 2002-12-19 | Method for synthesizing nano-size lanthanide metal hydride from lanthanide metal under nalohydrocarbon action |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021582181A CN1274588C (en) | 2002-12-19 | 2002-12-19 | Method for synthesizing nano-size lanthanide metal hydride from lanthanide metal under nalohydrocarbon action |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1508060A CN1508060A (en) | 2004-06-30 |
| CN1274588C true CN1274588C (en) | 2006-09-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021582181A Expired - Fee Related CN1274588C (en) | 2002-12-19 | 2002-12-19 | Method for synthesizing nano-size lanthanide metal hydride from lanthanide metal under nalohydrocarbon action |
Country Status (1)
| Country | Link |
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| CN (1) | CN1274588C (en) |
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- 2002-12-19 CN CNB021582181A patent/CN1274588C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1508060A (en) | 2004-06-30 |
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