CN107161964A - A kind of method for preparing N doping phosphorus alkene - Google Patents
A kind of method for preparing N doping phosphorus alkene Download PDFInfo
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- CN107161964A CN107161964A CN201710495545.8A CN201710495545A CN107161964A CN 107161964 A CN107161964 A CN 107161964A CN 201710495545 A CN201710495545 A CN 201710495545A CN 107161964 A CN107161964 A CN 107161964A
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- phosphorus alkene
- doping
- doping phosphorus
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of method for preparing N doping phosphorus alkene, including：Phosphorus alkene and inorganic salt containing nitrogen are together placed in solution, the consumption of phosphorus alkene accounts for the 5%~95% of phosphorus alkene and inorganic salt containing nitrogen gross mass, then it is uniformly mixed with ultrasonic wave is scattered, is then evaporated solution, so as to obtain N doping phosphorus alkene presoma；The N doping phosphorus alkene presoma is placed in inert gas filled high temperature furnace and calcined, calcining heat is 300~1100 DEG C, and soaking time is 0.1~72h, is subsequently cooled to room temperature, so that N doping phosphorus alkene is made.The present invention can be by nitrogen-doping into phosphorus alkene, make phosphorus alkene that there is good antioxygenic property, not only the physical and chemical performance of phosphorus alkene will not be destroyed, and simple to operate, low for equipment requirements, good product quality, yield are high, and product can use the fields such as electronic communication, communications and transportation extensively.
Description
Technical field
The present invention relates to phosphorus alkene field of compound material, more particularly to a kind of method for preparing N doping phosphorus alkene.
Background technology
Phosphorus alkene material is new two-dimentional phosphorus nano material, and its special stable micro-structure makes it have excellent electrification
Performance and heat-conductive characteristic are learned, therefore phosphorus alkene material has broad prospect of application in fields such as electronic communication, communications and transportation.
The environmental stability of phosphorus alkene is poor, and the stronger chemism of phosphorus atoms makes it easily be corroded by materials such as oxygen gas and waters
And original performance is lost, and strict protection must be carried out by equipment or other method when in use, otherwise can be rapid because of erosion
Decompose, this makes it significantly be limited in actual use.In addition, the mechanical performance of phosphorus alkene is weaker, in practical application mistake
It is vulnerable to external force in journey and is destroyed.
In the prior art, the environment unstability (shortcoming for being oxidized easily erosion) to phosphorus alkene is not located well
Reason method, and there is not N doping phosphorus alkene and its synthetic method.
The content of the invention
, can the invention provides a kind of method for preparing N doping phosphorus alkene for above-mentioned weak point of the prior art
Into phosphorus alkene, to make phosphorus alkene have good antioxygenic property nitrogen-doping, not only the physical and chemical performance of phosphorus alkene will not
It is destroyed, and simple to operate, low for equipment requirements, good product quality, yield are high, and product can use electronic communication, friendship extensively
The fields such as logical transport.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method for preparing N doping phosphorus alkene, comprises the following steps：
Step A, phosphorus alkene and inorganic salt containing nitrogen is together placed in solution, the consumption of phosphorus alkene accounts for phosphorus alkene and inorganic salt containing nitrogen is total
The 5%~95% of quality, then it is uniformly mixed with ultrasonic wave is scattered, then solution is evaporated, so as to obtain N doping phosphorus alkene
Presoma；
Step B, the N doping phosphorus alkene presoma is placed in inert gas filled high temperature furnace and calcined, calcining temperature
Spend for 300~1100 DEG C, soaking time is 0.1~72h, is subsequently cooled to room temperature, so that N doping phosphorus alkene is made.
Preferably, in step, ultrasonic dispersing time is 0.01~48h.
Preferably, the inorganic salt containing nitrogen be ammonium chloride, ammonium sulfate, ammonium sulfite, ammonium phosphate, ammonium phosphite, ammonium nitrate,
At least one of ammonium nilrite.
Preferably, the solution described in step A is water, methanol, ethanol, propyl alcohol, acetone, tetrahydrofuran, carbon tetrachloride, second
Nitrile, ether, petroleum ether, pentane, hexane, carbon disulfide, dichloromethane, dichloroethanes, chloroform, trichloroethanes, acetic acid second
Ester, butanone, benzene,toluene,xylene, hexamethylene, N,N-dimethylformamide, formaldehyde, sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid,
At least one of ammoniacal liquor, hydrazine hydrate, 1-METHYLPYRROLIDONE.
Preferably, the inert gas is at least one of nitrogen, helium, argon gas or carbon dioxide.
Preferably, N doping phosphorus alkene is made in step B to preserve under inert gas or vacuum condition.
Preferably, the inert gas is at least one of nitrogen, helium, argon gas or carbon dioxide.
As seen from the above technical solution provided by the invention, the method provided by the present invention for preparing N doping phosphorus alkene
The N doping phosphorus alkene presoma of specified raw material proportioning has been made by nitrogen source of inorganic salt containing nitrogen, has then led under inert gas shielding
Cross and the N doping phosphorus alkene presoma is calcined, and control calcining heat and soaking time, so that by nitrogen-doping to phosphorus
In alkene, N doping phosphorus alkene is formd；Different from simple phosphorus alkene, the nitrogen-atoms in the N doping phosphorus alkene can be such that the material has very
Good antioxygenic property, and ensure that the excellent physical and chemical performance of phosphorus alkene is not destroyed, still with good electric conductivity, heat conduction
The performance such as property, stability, flexibility, therefore the method provided by the present invention for preparing N doping phosphorus alkene can not only make the physics of phosphorus alkene
Chemical property will not be destroyed, and simple to operate, low for equipment requirements, good product quality, yield are high, and product can be used extensively
The fields such as electronic communication, communications and transportation.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, being used required in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is the electron scanning micrograph of the N doping phosphorus alkene prepared by the embodiment of the present invention 1.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to protection scope of the present invention.
The method provided by the present invention for preparing N doping phosphorus alkene is described in detail below.
A kind of method for preparing N doping phosphorus alkene, may comprise steps of：
Step A, phosphorus alkene and inorganic salt containing nitrogen is together placed in solution, the consumption of phosphorus alkene accounts for phosphorus alkene and inorganic salt containing nitrogen is total
The 5%~95% of quality, then it is uniformly mixed with ultrasonic wave is scattered, ultrasonic dispersing time is 0.01~48h, then will be molten
Liquid is evaporated, so as to obtain N doping phosphorus alkene presoma.Wherein, described solution is water, methanol, ethanol, propyl alcohol, acetone, tetrahydrochysene
Furans, carbon tetrachloride, acetonitrile, ether, petroleum ether, pentane, hexane, carbon disulfide, dichloromethane, dichloroethanes, chloroform,
Trichloroethanes, ethyl acetate, butanone, benzene,toluene,xylene, hexamethylene, N,N-dimethylformamide, formaldehyde, sulfuric acid, hydrochloric acid,
At least one of nitric acid, acetic acid, propionic acid, ammoniacal liquor, hydrazine hydrate, 1-METHYLPYRROLIDONE.
Step B, the N doping phosphorus alkene presoma is placed in inert gas filled high temperature furnace and calcined, calcining temperature
Spend for 300~1100 DEG C, soaking time is 0.1~72h, is subsequently cooled to room temperature, so that N doping phosphorus alkene is made.Wherein, institute
It is at least one of nitrogen, helium, argon gas or carbon dioxide to state inert gas.
N doping phosphorus alkene is made in step C, step B to preserve under inert gas or vacuum condition.Wherein, the indifferent gas
Body is at least one of nitrogen, helium, argon gas or carbon dioxide.
Specifically, N doping is made by nitrogen source of inorganic salt containing nitrogen for the method provided by the present invention for preparing N doping phosphorus alkene
Phosphorus alkene presoma, then by being calcined to N doping phosphorus alkene presoma under inert gas shielding, and controls calcining heat
And soaking time, so as to by nitrogen-doping into phosphorus alkene, form N doping phosphorus alkene；Different from simple phosphorus alkene, the nitrogen is mixed
Nitrogen-atoms in miscellaneous phosphorus alkene can make it have good antioxygenic property, and ensure that the excellent physical and chemical performance of phosphorus alkene is not broken
It is bad, still with performances such as good electric conductivity, thermal conductivity, stability, flexibilities, therefore provided by the present invention prepare N doping
The method of phosphorus alkene can not only be such that the physical and chemical performance of phosphorus alkene is not destroyed, and simple to operate, low for equipment requirements, product
Quality is good, yield is high, and product can use the fields such as electronic communication, communications and transportation extensively.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, below with tool
The method that what body embodiment was provided the embodiment of the present invention prepare N doping phosphorus alkene is described in detail.
Embodiment 1
A kind of method for preparing N doping phosphorus alkene, comprises the following steps：
Step a1,1g phosphorus alkene and 9g ammonium chlorides is together placed in water, then it is uniformly mixed with ultrasonic wave is scattered, ultrasound
Ripple jitter time is 0.1h, is then evaporated solution, so as to obtain N doping phosphorus alkene presoma.
Step b1, the N doping phosphorus alkene presoma is placed in the high temperature furnace filled with nitrogen and calcined, calcining heat
For 1100 DEG C, soaking time is 0.2h, is then naturally cooling to room temperature, so that N doping phosphorus alkene as shown in Figure 1 is made.
Step c1, described N doping phosphorus alkene are preserved under vacuum.
Embodiment 2
A kind of method for preparing N doping phosphorus alkene, comprises the following steps：
Step a2,1g phosphorus alkene and 4g ammonium sulfate is together placed in the mixed solution of methanol and benzene, then it is scattered with ultrasonic wave
It is set uniformly to mix, ultrasonic dispersing time is 1h, is then evaporated solution, so as to obtain N doping phosphorus alkene presoma.
Step b2, the N doping phosphorus alkene presoma is placed in the high temperature furnace filled with argon gas and calcined, calcining heat
For 900 DEG C, soaking time is 5h, is then naturally cooling to room temperature, so that N doping phosphorus alkene is made.
Step c2, described N doping phosphorus alkene are preserved under argon gas protection.
Embodiment 3
A kind of method for preparing N doping phosphorus alkene, comprises the following steps：
Step a3,1g phosphorus alkene and 1g ammonium nilrites is together placed in the mixed solution of petroleum ether and ammoniacal liquor, then with ultrasound
Wavelength-division, which dissipates, makes it uniformly mix, and ultrasonic dispersing time is 5h, is then evaporated solution, and N doping phosphorus alkene presoma is made.
Step b3, the N doping phosphorus alkene presoma is placed in the high temperature furnace filled with helium and calcined, calcining heat
For 700 DEG C, soaking time is 10h, is then naturally cooling to room temperature, so that N doping phosphorus alkene is made.
Step c3, described N doping phosphorus alkene are preserved under nitrogen protection.
Embodiment 4
A kind of method for preparing N doping phosphorus alkene, comprises the following steps：
Step a4, the mixed solution that 1g phosphorus alkene and 0.3g ammonium phosphate are together placed in N,N-dimethylformamide and formaldehyde
In, then with ultrasonic wave is scattered it is uniformly mixed, ultrasonic dispersing time is 24h, is then evaporated solution, is mixed so that nitrogen is made
Miscellaneous phosphorus alkene presoma.
Step b4, the N doping phosphorus alkene presoma is placed in the high temperature furnace filled with helium and calcined, calcining heat
For 500 DEG C, soaking time is 48h, is then naturally cooling to room temperature, so that N doping phosphorus alkene is made.
Step c4, described N doping phosphorus alkene are preserved under carbon-dioxide protecting.
Embodiment 5
A kind of method for preparing N doping phosphorus alkene, comprises the following steps：
Step a5, the mixing that the mixture of 3g phosphorus alkene and 0.2g ammonium chlorides and ammonium phosphate is together placed in into acetonitrile and nitric acid are molten
In liquid, then with ultrasonic wave is scattered it is set uniformly to mix, ultrasonic dispersing time is 48h, is then evaporated solution, so that nitrogen is made
Adulterate phosphorus alkene presoma.
Step b5, the N doping phosphorus alkene presoma is placed in the high temperature furnace filled with carbon dioxide and calcined, calcined
Temperature is 300 DEG C, and soaking time is 72h, is then naturally cooling to room temperature, so that N doping phosphorus alkene is made.
Step c5, described N doping phosphorus alkene are preserved under nitrogen and carbon-dioxide protecting.
As fully visible, the embodiment of the present invention can have phosphorus alkene anti-oxidant well by nitrogen-doping into phosphorus alkene
Performance, not only the physical and chemical performance of phosphorus alkene will not be destroyed, and simple to operate, low for equipment requirements, good product quality, production
Rate is high, and product can use the fields such as electronic communication, communications and transportation extensively.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (7)
1. a kind of method for preparing N doping phosphorus alkene, it is characterised in that comprise the following steps：
Step A, phosphorus alkene and inorganic salt containing nitrogen is together placed in solution, the consumption of phosphorus alkene accounts for phosphorus alkene and inorganic salt containing nitrogen gross mass
5%~95%, then it is uniformly mixed with ultrasonic wave is scattered, be then evaporated solution, so as to obtain N doping phosphorus alkene forerunner
Body；
Step B, the N doping phosphorus alkene presoma is placed in inert gas filled high temperature furnace and calcined, calcining heat is
300~1100 DEG C, soaking time is 0.1~72h, is subsequently cooled to room temperature, so that N doping phosphorus alkene is made.
2. the method according to claim 1 for preparing N doping phosphorus alkene, it is characterised in that in step, ultrasonic wave disperses
Time is 0.01~48h.
3. the method according to claim 1 or 2 for preparing N doping phosphorus alkene, it is characterised in that the inorganic salt containing nitrogen is
At least one of ammonium chloride, ammonium sulfate, ammonium sulfite, ammonium phosphate, ammonium phosphite, ammonium nitrate, ammonium nilrite.
4. the method according to claim 1 or 2 for preparing N doping phosphorus alkene, it is characterised in that the solution described in step A
For water, methanol, ethanol, propyl alcohol, acetone, tetrahydrofuran, carbon tetrachloride, acetonitrile, ether, petroleum ether, pentane, hexane, curing
Carbon, dichloromethane, dichloroethanes, chloroform, trichloroethanes, ethyl acetate, butanone, benzene,toluene,xylene, hexamethylene, N,
In dinethylformamide, formaldehyde, sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid, ammoniacal liquor, hydrazine hydrate, 1-METHYLPYRROLIDONE extremely
Few one kind.
5. the method according to claim 1 or 2 for preparing N doping phosphorus alkene, it is characterised in that the inert gas is nitrogen
At least one of gas, helium, argon gas or carbon dioxide.
6. the method according to claim 1 or 2 for preparing N doping phosphorus alkene, it is characterised in that N doping is made in step B
Phosphorus alkene is preserved under inert gas or vacuum condition.
7. the method according to claim 6 for preparing N doping phosphorus alkene, it is characterised in that the inert gas be nitrogen,
At least one of helium, argon gas or carbon dioxide.
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| CN201710495545.8A CN107161964A (en) | 2017-06-26 | 2017-06-26 | A kind of method for preparing N doping phosphorus alkene |
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| CN201710495545.8A CN107161964A (en) | 2017-06-26 | 2017-06-26 | A kind of method for preparing N doping phosphorus alkene |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109422255A (en) * | 2017-08-25 | 2019-03-05 | 段兴宇 | Halogen doping phosphorus nanoparticle and its manufacturing method |
| CN113122253A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Nitrogen-doped phospholene quantum dot and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449411A (en) * | 2012-05-30 | 2013-12-18 | 海洋王照明科技股份有限公司 | Preparation method for nitrogen-doped graphene |
-
2017
- 2017-06-26 CN CN201710495545.8A patent/CN107161964A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449411A (en) * | 2012-05-30 | 2013-12-18 | 海洋王照明科技股份有限公司 | Preparation method for nitrogen-doped graphene |
Non-Patent Citations (1)
| Title |
|---|
| DANIL W. BOUKHVALOV: "The atomic and electronic structure of nitrogen- and boron-doped phosphorene", 《PHYS. CHEM. CHEM. PHYS.》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109422255A (en) * | 2017-08-25 | 2019-03-05 | 段兴宇 | Halogen doping phosphorus nanoparticle and its manufacturing method |
| CN113122253A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Nitrogen-doped phospholene quantum dot and preparation method thereof |
| CN113122253B (en) * | 2019-12-30 | 2022-03-01 | Tcl科技集团股份有限公司 | Nitrogen-doped phospholene quantum dot and preparation method thereof |
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Application publication date: 20170915 |