CN1517297A - Method of synthesizing nanometer size lanthanum-series metal hydride by activating lanthanum metal and using solvent effect - Google Patents
Method of synthesizing nanometer size lanthanum-series metal hydride by activating lanthanum metal and using solvent effect Download PDFInfo
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- CN1517297A CN1517297A CNA031012779A CN03101277A CN1517297A CN 1517297 A CN1517297 A CN 1517297A CN A031012779 A CNA031012779 A CN A031012779A CN 03101277 A CN03101277 A CN 03101277A CN 1517297 A CN1517297 A CN 1517297A
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Abstract
A process for synthesizing the nano-class hydrid of La-series metal includes such steps as activating the La-series metal, and using solvent effect. Its advantages are small particle diameter less than 40 nm and high purity.
Description
Technical Field
The new method of the invention is that lanthanide metal is activated and lanthanide metal hydride with nanometer size is synthesized by solvent effect under normal temperature and 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 sources 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 methods produce nanomaterials primarily through appropriate chemical reactions. The invention, namely a method for synthesizing nano-sized lanthanide metal hydride by activating lanthanide metal and utilizing solvent effect, has not been reported in documents.
Disclosure of Invention
The invention aims to provide a novel method for synthesizing nano-size lanthanide metal hydride by activating lanthanide metal and utilizing solvent effect.
The method can be represented by the following reaction formula:
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
Lanthanum metal filings (purity>99.5%), weighing 3.47g (25mmol), adding into a reaction bottle, heating to 200 deg.C, cooling to room temperature, adding 15.0mL tetrahydrofuran, controlling the temperature of oil bath (45 deg.C), opening the magnetic stirrer, introducing hydrogen into the reaction bottle, and reading the hydrogen absorption amount of the reaction by a constant pressure gas pipe. After 64 hours the lanthanum metal hydrogenation reaction was stopped.
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 1h to give black solid lanthanum hydride powder.
The effect of the solvent effect is that it enables the quantitative conversion of lanthanum into nanosized lanthanum hydride. Its composition is LnH2.85. TEM measurement results show that the lanthanum hydride synthesized by the novel method has basic particle size less than 40 nm. The specific surface area is 9.0m2·g-1XRD test results show that the lanthanum hydride structure is cubic crystal.
EXAMPLE 2 Synthesis of nanosized Neodymium hydride by solvent Effect method
Nanometer-sized neodymium hydride was synthesized according to the method of example 1. The neodymium hydrogenation reaction was stopped after 74 hours. The TEM measurement results show that the basic particle size is less than 40 nm.
EXAMPLE 3 Synthesis of nanosized samarium hydride by solvent Effect method
Nanosized samarium hydride was synthesized according to the method of example 1. After 128 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 solvent Effect method
Dysprosium hydride of nanometer size was synthesized according to the method of example 1.
After 178 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 solvent Effect method
Nanometer-sized ytterbium hydride was synthesized according to the method of example 1. The ytterbium metal hydrogenation reaction was stopped after 266 hours. The TEM measurement results show that the basic particle size is less than 40 nm.
Experimental results show that the effect of the solvent effect is to quantitatively convert lanthanide metals to the corresponding nanosized metal hydrides. Composition of nanosized rare earth metal hydrides to non-stoichiometric value, LnHmWherein m is between 2 and 3.
In the synthesis reaction, 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. Compared with the two patents of 'method for catalytically synthesizing nano lanthanide metal hydride (application number: 02141735.0)' and 'method for synthesizing nano lanthanide metal hydride from lanthanide metal under the action of halohydrocarbon (application number: 02158218.1)', the reaction time is slightly increased. However, the method has the advantage that the synthesized nano-sized lanthanide metal hydride does not need to be added with a metal or organic activator, so that the possibility of introducing trace metal or organic impurity residues into the product is avoided.
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 series metal by activating lanthanide series metal and using the solvent effect of organic solvent features that after activating the lanthanide series metal powder, the solvent effect is used to prepare it at ordinary temp and pressure.
2. A method of synthesizing nanosized lanthanide metal hydrides according to claim 1 wherein said lanthanide metal powders are first activated. The activation is carried out by heating or the like.
3. The method of synthesizing nanosized lanthanide metal hydrides claimed in claim 1 wherein said second step is carried out by utilizing the solvent effect of an organic solvent. The organic solvent includes toluene, methyl ethyl ketone, pyridine, n-butyl ether, isoamyl ether, tetrahydrofuran, 1, 4-dioxane, etc.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031012779A CN1317181C (en) | 2003-01-19 | 2003-01-19 | Method of synthesizing nanometer size lanthanum-series metal hydride by activating lanthanum metal and using solvent effect |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB031012779A CN1317181C (en) | 2003-01-19 | 2003-01-19 | Method of synthesizing nanometer size lanthanum-series metal hydride by activating lanthanum metal and using solvent effect |
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| CN1517297A true CN1517297A (en) | 2004-08-04 |
| CN1317181C CN1317181C (en) | 2007-05-23 |
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| CNB031012779A Expired - Fee Related CN1317181C (en) | 2003-01-19 | 2003-01-19 | Method of synthesizing nanometer size lanthanum-series metal hydride by activating lanthanum metal and using solvent effect |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100386337C (en) * | 2006-01-24 | 2008-05-07 | 北京工业大学 | Method for in-situ synthesizing preparation of high-purity GdH2 block material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP0969110A3 (en) * | 1998-06-16 | 2000-01-19 | Mitsubishi Materials Corporation | Hydrogen occluding alloy |
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- 2003-01-19 CN CNB031012779A patent/CN1317181C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100386337C (en) * | 2006-01-24 | 2008-05-07 | 北京工业大学 | Method for in-situ synthesizing preparation of high-purity GdH2 block material |
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| CN1317181C (en) | 2007-05-23 |
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