CN104803364A - Preparation method of copper phosphide nanotube - Google Patents
Preparation method of copper phosphide nanotube Download PDFInfo
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- CN104803364A CN104803364A CN201510231148.0A CN201510231148A CN104803364A CN 104803364 A CN104803364 A CN 104803364A CN 201510231148 A CN201510231148 A CN 201510231148A CN 104803364 A CN104803364 A CN 104803364A
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- mantoquita
- erlenmeyer flask
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- 239000002071 nanotube Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000010949 copper Substances 0.000 title abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title abstract 4
- 229910052802 copper Inorganic materials 0.000 title abstract 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 5
- 239000010935 stainless steel Substances 0.000 claims abstract description 5
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 238000011002 quantification Methods 0.000 claims description 4
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 229960003280 cupric chloride Drugs 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 abstract 5
- -1 polytetrafluoroethylene Polymers 0.000 abstract 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 2
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 2
- 150000001879 copper Chemical class 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 125000002524 organometallic group Chemical group 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Inorganic Fibers (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a preparation method of a copper phosphide nanotube. The preparation method comprises the following steps that CTAB (cetyl trimethyl ammonium bromide) is added into an N,N-dimethylformamide (DMF) solution; stirring and ultrasound are carried out until the materials are completely dissolved; then, copper salt is added, and stirring and ultrasound treatment are carried out until the materials are completely dissolved; a transparent solution is obtained; the transparent solution is transferred into a polytetrafluoroethylene inner liner; next, yellow phosphorus is added; then, the polytetrafluoroethylene inner liner is sealed in a stainless steel mold; heating is carried out from the room temperature to carry out reaction under the sealed condition; after the reaction is completed, the materials are cooled to the room temperature along with a furnace; then, fast quantitative filter paper is used for filtering, and crude products are obtained; next, deionized water, benzene and absolute ethyl alcohol are sequentially and respectively used for washing the crude products; finally, the washed products are subjected to vacuum drying, and the copper phosphide nanotube is obtained. The preparation method has the advantages that the method is simple, and the prepared copper phosphide nanotube has the uniform appearance and size.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, be specifically related to a kind of preparation method of cuprous phosphide nanotube.
Background technology
The appearance of nano material of transition metal phosphide controls the focus having become research, because the pattern of material, size can its physical and chemical performances of extreme influence, as catalysis, electrochemistry, magnetic etc.Thus in recent years, investigators are devoted to the transition metal phosphide controlledly synthesis of specific morphology.In a series of phosphide, the especially Cu of special appearance
3p, as hexagon, dendritic, hollow ball etc. show excellent energy storage, photocatalytic degradation characteristic.Compared with traditional three-dimensional material, nanoparticle, the surface tissue at the inside of nano tube structure uniqueness, outside, edge makes it have more functionalization feature.But great majority are to Cu
3the preparation research of P is all confined to three-dimensional material, rarely has bibliographical information to synthesize the Cu of high quality, size uniformity
3the method of P nano tube structure.
The synthetic method of metal current phosphide nano-tube material mainly uses organometallic precursor decomposition method, chemical in-situ synthesis and solvent-thermal method.But the operation of organometallic precursor decomposition method is more complicated, cost is also higher, and organometallic precursor is difficult to synthesis, thus has significant limitation.And one-dimentional structure prepared by chemical in-situ synthesis, although product pattern is homogeneous, this method uses the organic phosphorus sources that toxicity is larger, and security is poor and cost is higher, is not suitable for scale operation.And solvent thermal system, although report can by extend the reaction times can obtain a small amount of Cu
3p nanotube, but its most product is still microballoon.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of preparation method of cuprous phosphide nanotube, method is simple, cuprous phosphide pattern, the size uniformity prepared.
In order to achieve the above object, the technical scheme that the present invention takes is:
A preparation method for cuprous phosphide nanotube, comprises the following steps:
1) in Erlenmeyer flask, add the DMF solution (DMF) of volume 30 ~ 45mL;
2) in Erlenmeyer flask, add 0.00 ~ 0.15g cetyl trimethylammonium bromide (CTAB), stir, ultrasonic to dissolving completely, CTAB concentration is 0g/L ~ 5.0g/L;
3) in Erlenmeyer flask, add mantoquita, stir, ultrasonic to dissolving completely, the concentration of mantoquita is 5.0g/L ~ 8.0g/L;
4) by step 3) clear solution that obtains proceeds in polytetrafluoroethyllining lining, the yellow phosphorus of 0.08 ~ 0.20g is added again in clear solution, its concentration is made to be 1.50 ~ 7.00g/L, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 140 ~ 200 DEG C of reacting by heating 12 ~ 20h;
5), after having reacted, furnace cooling, to room temperature, is then used fast quantification filter paper filtering, is obtained crude product;
6) with deionized water, benzene and dehydrated alcohol, crude product is washed respectively successively;
7) insert in vacuum drying oven by the product after washing, vacuum-drying 4h at 50 ~ 60 DEG C, obtains cuprous phosphide nanotube.
Described mantoquita is copper sulfate, cupric chloride or cupric nitrate.
Described polytetrafluoroethyllining lining is 50mL, and compactedness is 60% ~ 90%.
The present invention has following beneficial effect:
(1) have special nano tube structure, its diameter is about 100nm, and thickness of pipe is approximately 10nm.
(2) the nanotube pattern obtained easily is controlled, size uniformity, can effectively avoid using the organic phosphorus sources expensive, toxicity is larger simultaneously.
(3) cost of the present invention is low, and raw material is easy to get, and preparation technology is simple, reproducible, has a good application prospect.
Accompanying drawing explanation
Accompanying drawing is that embodiment 1 gained cuprous phosphide product TEM schemes.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
A preparation method for cuprous phosphide nanotube, comprises the following steps:
1) in Erlenmeyer flask, add the DMF solution (DMF) of volume 40mL;
2) in Erlenmeyer flask, add 0.10g cetyl trimethylammonium bromide (CTAB), stir, ultrasonic to dissolving completely, CTAB concentration is 2.5g/L;
3) in Erlenmeyer flask, add 0.25g Salzburg vitriol, stir, ultrasonic to dissolving completely, the concentration of mantoquita is 6.25g/L, and described mantoquita is Salzburg vitriol;
4) by step 3) clear solution that obtains proceeds in polytetrafluoroethyllining lining, the yellow phosphorus of 0.124g is added again in clear solution, its concentration is made to be 3.10g/L, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 160 DEG C of reacting by heating 16h;
5), after having reacted, furnace cooling, to room temperature, is then used fast quantification filter paper filtering, is obtained crude product;
6) with deionized water, benzene and dehydrated alcohol, crude product is washed respectively successively;
7) insert in vacuum drying oven by the product after washing, vacuum-drying 4h at 50 ~ 60 DEG C, obtains cuprous phosphide nanotube.
The nanotube-shaped cuprous phosphide material that the present embodiment 1 is prepared, its TEM picture as shown in Figure 1.
Embodiment 2
By step 2 in embodiment 1) CTAB consumption change 0.00g into, other conditions are constant, in product find do not have nanotube to be formed, the substitute is a hollow stores.
Embodiment 3
By step 2 in embodiment 1) CTAB consumption change 0.15g into, other conditions are constant, and obviously find in product that nanotube disappears, product is hollow ball structure.
Embodiment 4
By step 4 in embodiment 1) Heating temperature change 140 DEG C into, other conditions are constant, nanotube a small amount of in product, reunite serious, and its crystallinity is also very poor simultaneously.
Embodiment 5
By step 4 in embodiment 1) Heating temperature change 160 DEG C into, other conditions are constant, and in product, major part is nanotube, but dispersed poor.
Embodiment 6
By step 4 in embodiment 1) Heating temperature change 200 DEG C into, other conditions are constant, and product morphology is more assorted, bad dispersibility, and size is not too homogeneous, substantially do not have nanotube to occur.
Be described in detail description to specific embodiments of the invention above, and be described the product phenomenon of different embodiments, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (4)
1. a preparation method for cuprous phosphide nanotube, is characterized in that, comprises the following steps:
1) in Erlenmeyer flask, add the DMF solution (DMF) of volume 30 ~ 45mL;
2) in Erlenmeyer flask, add 0.00 ~ 0.15g cetyl trimethylammonium bromide (CTAB), stir, ultrasonic to dissolving completely, CTAB concentration is 0.00g/L ~ 5.0g/L;
3) in Erlenmeyer flask, add mantoquita, stir, ultrasonic to dissolving completely, the concentration of mantoquita is 5.00g/L ~ 8.00g/L;
4) by step 3) clear solution that obtains proceeds in polytetrafluoroethyllining lining, the yellow phosphorus of 0.08 ~ 0.20g is added again in clear solution, its concentration is made to be 1.50 ~ 7.00g/L, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 140 ~ 200 DEG C of reacting by heating 12 ~ 20h;
5), after having reacted, furnace cooling, to room temperature, is then used fast quantification filter paper filtering, is obtained crude product;
6) with deionized water, benzene and dehydrated alcohol, crude product is washed respectively successively;
7) insert in vacuum drying oven by the product after washing, vacuum-drying 4h at 50 ~ 60 DEG C, obtains cuprous phosphide nanotube.
2. the preparation method of a kind of cuprous phosphide nanotube according to claim 1, is characterized in that:
Described mantoquita is copper sulfate, cupric chloride or cupric nitrate.
3. the preparation method of a kind of cuprous phosphide nanotube according to claim 1, is characterized in that:
Described polytetrafluoroethyllining lining is 50mL, and compactedness is 60% ~ 90%.
4. the preparation method of a kind of cuprous phosphide nanotube according to claim 1, is characterized in that: comprise the following steps:
1) in Erlenmeyer flask, add the DMF solution (DMF) of volume 40mL;
2) in Erlenmeyer flask, add 0.10g cetyl trimethylammonium bromide (CTAB), stir, ultrasonic to dissolving completely, CTAB concentration is 2.50g/L;
3) in Erlenmeyer flask, add mantoquita, stir, ultrasonic to dissolving completely, the concentration of mantoquita is 6.25g/L, and described mantoquita is Salzburg vitriol;
4) by step 3) clear solution that obtains proceeds in polytetrafluoroethyllining lining, the yellow phosphorus of 0.124g is added again in clear solution, its concentration is made to be 3.10g/L, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 160 DEG C of reacting by heating 16h;
5), after having reacted, furnace cooling, to room temperature, is then used fast quantification filter paper filtering, is obtained crude product;
6) with deionized water, benzene and dehydrated alcohol, crude product is washed respectively successively;
7) insert in vacuum drying oven by the product after washing, vacuum-drying 4h at 50 ~ 60 DEG C, obtains cuprous phosphide nanotube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510231148.0A CN104803364B (en) | 2015-05-07 | 2015-05-07 | A kind of preparation method of copper phosphide nanotube |
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| CN201510231148.0A CN104803364B (en) | 2015-05-07 | 2015-05-07 | A kind of preparation method of copper phosphide nanotube |
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| Publication Number | Publication Date |
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| CN104803364A true CN104803364A (en) | 2015-07-29 |
| CN104803364B CN104803364B (en) | 2016-08-24 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110085860A (en) * | 2019-04-26 | 2019-08-02 | 陕西科技大学 | A kind of preparation method of phosphorized copper nanotube |
| CN112194107A (en) * | 2020-09-28 | 2021-01-08 | 银隆新能源股份有限公司 | Transition metal phosphide nanowire bundle, and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103723694A (en) * | 2013-12-17 | 2014-04-16 | 陕西科技大学 | Method for preparing cathode material of hollow spherical copper phosphide lithium battery |
| CN104401949A (en) * | 2014-11-11 | 2015-03-11 | 华中科技大学 | Preparation method of nano cuprous phosphide/copper phosphide |
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2015
- 2015-05-07 CN CN201510231148.0A patent/CN104803364B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103723694A (en) * | 2013-12-17 | 2014-04-16 | 陕西科技大学 | Method for preparing cathode material of hollow spherical copper phosphide lithium battery |
| CN104401949A (en) * | 2014-11-11 | 2015-03-11 | 华中科技大学 | Preparation method of nano cuprous phosphide/copper phosphide |
Non-Patent Citations (2)
| Title |
|---|
| SHULING LIU ET AL.: "Surfactant-assisted synthesis and electrochemical performances of Cu3P dendrites", 《MATERIALS RESEARCH BULLETIN》 * |
| XINJUN WANG ET AL.: "Synthesis and characterization of Cu3P hollow spheres by a facile soft-template process", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110085860A (en) * | 2019-04-26 | 2019-08-02 | 陕西科技大学 | A kind of preparation method of phosphorized copper nanotube |
| CN110085860B (en) * | 2019-04-26 | 2020-09-22 | 陕西科技大学 | Preparation method of copper phosphide nanotube |
| CN112194107A (en) * | 2020-09-28 | 2021-01-08 | 银隆新能源股份有限公司 | Transition metal phosphide nanowire bundle, and preparation method and application thereof |
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| Publication number | Publication date |
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| CN104803364B (en) | 2016-08-24 |
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