CN100427249C - Halocarbon triggered synthesized anthracene lanthanide series metal organic compounds and preparation of nano lanthanide series metal dust through vacuum decomposition of same - Google Patents
Halocarbon triggered synthesized anthracene lanthanide series metal organic compounds and preparation of nano lanthanide series metal dust through vacuum decomposition of same Download PDFInfo
- Publication number
- CN100427249C CN100427249C CNB2003101219855A CN200310121985A CN100427249C CN 100427249 C CN100427249 C CN 100427249C CN B2003101219855 A CNB2003101219855 A CN B2003101219855A CN 200310121985 A CN200310121985 A CN 200310121985A CN 100427249 C CN100427249 C CN 100427249C
- Authority
- CN
- China
- Prior art keywords
- anthracene
- lanthanide metal
- lanthanide series
- nanometer
- series metal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to the preparation of nanometer metal materials. The properties of nanometer lanthanide metal powder prepared by the present invention are more active than those of lanthanide metal commodities, and the applications of the nanometer lanthanide metal powder are also more extensive. The synthesis of anthracene lanthanide metal organic compounds and the preparation of the nanometer lanthanide metal powder by vacuum pyrolysis are initated by halogenated hydrocarbon, lanthanide metal and anthracene generate the anthracene lanthanide metal organic compounds under the action of initiators under the conditions of normal pressure and 0 to 60 DEG C of temperature, and the anthracene lanthanide metal organic compounds are pyrolyzed in a vacuum at 100 to 250 DEG C to obtain the corresponding nanometer lanthanide powder. Results measured by a transmission electron microscope indicate that the diameter of the obtained particles is from 10 to 40 nanometers. The method has the advantages of simple equipment, easy control of operating conditions, low production cost and high yield of products, and the obtained nanometer lanthanide metal powder has the advantages of high activity and good dispersion degree.
Description
Technical field
This invention relates to the preparation of nano metal material.Lanthanide series metal is the development and the application of indispensable raw material, especially some new materials in many high-technology fields, and by the nano lanthanide metal powder of this invention method preparation, than commodity group of the lanthanides metalline ripple more alive, its application is also more extensive.
This invention is that halogenated hydrocarbons causes elbs reaction lanthanide series metal organic compound and vacuum pyrolysis prepares the nano lanthanide metal powder.Under 0-60 ℃ and the condition of normal pressure, in the organic solvent, lanthanide series metal and anthracene generate anthracene lanthanide series metal organic compound under action of evocating, obtain corresponding nano lanthanide metal powder at 100-250 ℃ of following vacuum pyrolysis.
Background technology
Nano science has become one of scientific and technological forward position of greatest concern in this century.Nano science all is with a wide range of applications in fields such as catalysis, synthetic chemistry, material science, the energy and environmental protection.Nanometer technology is becoming and a kind ofly not only can bring new product, and the innovative production technology that can improve the quality of products.
Nano material is meant the material of its basic particle size in 1～100nm scope, and they have high decentralization, surface energy and great specific area, and chemism is also than high 2～4 orders of magnitude of its corresponding conventional substances.The research of its preparation is the emphasis and the basis of nano science, also is the important channel that nanometer technology is applied to produce, live.The preparation method can be divided into physics and chemical method usually.Chemical method is mainly by suitable chemical reaction (comprising liquid phase, gas phase and solid phase reaction), from molecule, atom preparation nano material.Have not yet to see the relevant halogenated hydrocarbons that uses and make initator elbs reaction lanthanide series metal organic compound, and it prepares the bibliographical information of nano lanthanide metal powder by vacuum pyrolysis.
Summary of the invention
The purpose of this invention provides under the condition of a kind of method of simple and feasible: 0-60 ℃ and normal pressure, in organic solvent, lanthanide series metal and anthracene generate metallo-organic compound under the halogenated hydrocarbons action of evocating, vacuum pyrolysis obtains corresponding nano lanthanide metal powder under the 100-250 ℃ of condition.
The halogenated hydrocarbons initator comprises C in the above-mentioned reaction
2H
5Br, CH
3Halogenated hydrocarbons such as I.
Organic solvent comprises oxolane, 1 in the above-mentioned reaction, 4-dioxane, pyridine, toluene, n-butyl ether, isoamyl ether etc.
Description of drawings
Fig. 1 is the reaction equation of this invention method
The specific embodiment
The halogenated hydrocarbons that this invention is provided below by example causes elbs reaction lanthanide series metal organic compound and vacuum pyrolysis thereof and prepares the nano lanthanide metal powder and be described further.
Synthesizing of example 1 anthracene lanthanum organic compound
Reguline metal lanthanum (purity＞99.9%) is sawn into the bits shape, takes by weighing 2.78g (20mmol), anthracene 4.28g (25mmol) places reaction bulb, adds 32.5mL THF, 0.01mL C
2H
5Br, constant temperature oil bath, electromagnetic agitation when solution becomes grey black, shows that anthracene lanthanum organic compound generates.
Example 2 anthracene neodymiums, anthracene samarium, anthracene dysprosium, anthracene ytterbium etc. are metal-organic synthetic
According to metallo-organic compounds such as the method elbs reaction neodymium of example 1, anthracene samarium, anthracene dysprosium, anthracene ytterbiums.
The preparation of example 3 nanometer lanthanum powder
Transfer in the special reaction bulb after will filtering by the anthracene lanthanum organic compound that example 1 method makes, it is carried out vacuum pyrolysis, 100-250 ℃ of temperature control, after anthracene all distilled, the bottom of reaction bulb had stayed the lanthanum powder of black.The result shows that its particle size is in the 10-40nm scope with Japan JEM-1200 EX of science transmissioning electric mirror determining.
The preparation of metal dusts such as example 4 nanometer neodymiums, samarium, dysprosium, ytterbium
Prepare metal dusts such as corresponding nanometer neodymium, samarium, dysprosium, ytterbium according to metallo-organic compounds such as the method thermal decomposition anthracene neodymium of example 3, anthracene samarium, anthracene dysprosium, anthracene ytterbiums.The transmissioning electric mirror determining result shows that particle size is all in the 10-40nm scope.
By above-mentioned example as seen, under the condition of 0-60 ℃ and normal pressure, in organic solvent, lanthanide series metal and anthracene generate anthracene lanthanide series metal organic compound under the halogenated hydrocarbons action of evocating, and vacuum pyrolysis obtains corresponding nano lanthanide metal powder under 100-250 ℃ of condition.This invention equipment is simple, operating condition is easy to control, low production cost, the nano lanthanide metal powder activity height and the good dispersion degree that obtain, can be applicable to multiple field.
Claims (3)
1. method for preparing the nano lanthanide metal powder, it is characterized by: under 0-60 ℃ and condition of normal pressure, in the organic solvent, lanthanide series metal is under the halogenated hydrocarbons action of evocating, generate anthracene lanthanide series metal organic compound with the anthracene reaction, it obtains corresponding nano lanthanide metal powder at 100-250 ℃ of vacuum pyrolysis.
2. in accordance with the method for claim 1, it is characterized in that: organic solvent is an oxolane, 1, any one in 4-dioxane, pyridine, toluene, n-butyl ether, the isoamyl ether.
3. it is characterized in that in accordance with the method for claim 1: the halogenated hydrocarbons initator is a kind of in iodomethane or the bromohexane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101219855A CN100427249C (en) | 2003-12-10 | 2003-12-10 | Halocarbon triggered synthesized anthracene lanthanide series metal organic compounds and preparation of nano lanthanide series metal dust through vacuum decomposition of same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101219855A CN100427249C (en) | 2003-12-10 | 2003-12-10 | Halocarbon triggered synthesized anthracene lanthanide series metal organic compounds and preparation of nano lanthanide series metal dust through vacuum decomposition of same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1546262A CN1546262A (en) | 2004-11-17 |
| CN100427249C true CN100427249C (en) | 2008-10-22 |
Family
ID=34338589
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2003101219855A Expired - Fee Related CN100427249C (en) | 2003-12-10 | 2003-12-10 | Halocarbon triggered synthesized anthracene lanthanide series metal organic compounds and preparation of nano lanthanide series metal dust through vacuum decomposition of same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100427249C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2626824C2 (en) * | 2015-09-22 | 2017-08-02 | Сиа Эволед | 9-antracenates of lanthanides, showing luminescent properties, and organic leds on its basis |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4659373A (en) * | 1983-11-09 | 1987-04-21 | Studiengesellschaft Kohle Mbh | Process for preparing finely divided highly reactive magnesium and use thereof |
| CN1240234A (en) * | 1998-06-16 | 2000-01-05 | 三菱麻铁里亚尔株式会社 | Hydrogen absorption alloy |
-
2003
- 2003-12-10 CN CNB2003101219855A patent/CN100427249C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4659373A (en) * | 1983-11-09 | 1987-04-21 | Studiengesellschaft Kohle Mbh | Process for preparing finely divided highly reactive magnesium and use thereof |
| CN1240234A (en) * | 1998-06-16 | 2000-01-05 | 三菱麻铁里亚尔株式会社 | Hydrogen absorption alloy |
Non-Patent Citations (2)
| Title |
|---|
| Preparation of Lanthanide Hydrides of Nanometric Size by the Catalytic Method. Fan Yin-Heng et al.Chinese Journal of chemistry,Vol.20 No.11. 2002 |
| Preparation of Lanthanide Hydrides of Nanometric Size by the Catalytic Method. Fan Yin-Heng et al.Chinese Journal of chemistry,Vol.20 No.11. 2002 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2626824C2 (en) * | 2015-09-22 | 2017-08-02 | Сиа Эволед | 9-antracenates of lanthanides, showing luminescent properties, and organic leds on its basis |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1546262A (en) | 2004-11-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Balwe et al. | Green synthesis and characterization of silver nanoparticles (Ag NPs) from extract of plant Radix Puerariae: An efficient and recyclable catalyst for the construction of pyrimido [1, 2-b] indazole derivatives under solvent-free conditions | |
| Keshipour et al. | Palladium nano-particles supported on ethylenediamine-functionalized cellulose as a novel and efficient catalyst for the Heck and Sonogashira couplings in water | |
| Firouzabadi et al. | Palladium nano-particles supported on agarose as efficient catalyst and bioorganic ligand for CC bond formation via solventless Mizoroki–Heck reaction and Sonogashira–Hagihara reaction in polyethylene glycol (PEG 400) | |
| Nasrollahzadeh et al. | Palladium nanoparticles supported on copper oxide as an efficient and recyclable catalyst for carbon (sp2)–carbon (sp2) cross-coupling reaction | |
| Huang et al. | Synthesis of bis (buckminsterfullerene) nickel cation, Ni (C60) 2+, in the gas phase | |
| CN105032424A (en) | Catalyst for selective hydrogenation reaction of aromatic nitrocompound and preparation method of catalyst | |
| CN107082408A (en) | A kind of method that utilization freeze-drying process prepares porous boron carbon nitrogen nanometer sheet | |
| CN104761488A (en) | Three-dimensional bipyridine functionalized covalent organic frame material synthesis method | |
| Firouzabadi et al. | Palladium nanoparticles supported on aminopropyl-functionalized clay as efficient catalysts for phosphine-free C–C bond formation via Mizoroki–Heck and Suzuki–Miyaura reactions | |
| Sarvestani et al. | Buchwald‐Hartwig amination reaction of aryl halides using heterogeneous catalyst based on Pd nanoparticles decorated on chitosan functionalized graphene oxide | |
| Patil et al. | Ash of pomegranate peels (APP): a bio-waste heterogeneous catalyst for sustainable synthesis of α, α′-bis (substituted benzylidine) cycloalkanones and 2-arylidene-1-tetralones | |
| CN106975489A (en) | A kind of preparation method of nickel oxide in-stiu coating graphene nanocomposite material | |
| Baran | Production and application of highly efficient and reusable palladium nanocatalyst decorated on the magnetically retrievable chitosan/activated carbon composite microcapsules | |
| Zhu et al. | Selective CC bonds formation, N-alkylation and benzo [d] imidazoles synthesis by a recyclable zinc composite | |
| US8236272B2 (en) | Combination catalysts based on iron for the substantial synthesis of multi-walled carbon nanotubes by chemical vapor deposition | |
| Ahmadzadi et al. | Structural and X-ray powder diffraction studies of nano-structured lead (II) coordination polymer with η2 Pb⋯ C interactions | |
| Dehbanipour et al. | Nano–silica supported palladium catalyst: Synthesis, characterization and application of its activity in Sonogashira cross–coupling reactions | |
| Khojasteh et al. | Palladium loaded on magnetic nanoparticles as efficient and recyclable catalyst for the Suzuki-Miyaura reaction | |
| CN100427249C (en) | Halocarbon triggered synthesized anthracene lanthanide series metal organic compounds and preparation of nano lanthanide series metal dust through vacuum decomposition of same | |
| Wang et al. | In situ growth of gold nanoparticles onto polyphosphazene microspheres with amino-groups for alcohol oxidation in aqueous solutions | |
| Moghaddam et al. | Nano CoCuFe2O4 catalyzed coupling reaction of acid chlorides with terminal alkynes: A powerful toolbox for palladium-free ynone synthesis | |
| Liu et al. | Direct methylation and carbonylation of in situ generated arynes via HDDA-Wittig coupling | |
| Xu et al. | In air liquid–solid phase synthesis of metal sulfide nanoparticles from metal acetates and thiourea | |
| Sharghi et al. | Rapid, Eco‐friendly, and One‐pot Synthesis of New Lariat Ethers Based on Anthraquinone by Using ZnO Nanoparticles via “Mannich” Reaction under Solvent‐free Condition | |
| Baghbanian et al. | Efficient synthesis of β-amino alcohols by regioselective ring opening of epoxides with amines catalyzed by CuFe 2 O 4 nanoparticles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20081022 Termination date: 20100111 |