CN108793107A - A method of preparing a nanometer black phosphorus - Google Patents
A method of preparing a nanometer black phosphorus Download PDFInfo
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- CN108793107A CN108793107A CN201810834309.9A CN201810834309A CN108793107A CN 108793107 A CN108793107 A CN 108793107A CN 201810834309 A CN201810834309 A CN 201810834309A CN 108793107 A CN108793107 A CN 108793107A
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- C—CHEMISTRY; METALLURGY
- 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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Abstract
The invention discloses a kind of methods preparing nanometer black phosphorus, and steps are as follows：Tin, the high tin of iodate and red phosphorus are encapsulated in quartz ampoule under an argon atmosphere, is placed in tube furnace, 2.5-3.5h is kept the temperature after 610-630 DEG C, be then cooled to 480-490 DEG C and keep the temperature 2.5-3.5h again, is down to room temperature, quartz ampoule is opened and can be obtained bulk black phosphorus；It will be add to deionized water after black phosphorus grinding uniformly, ultrasound, then finely dispersed black phosphorus dispersion liquid is added in high pressure homogenizer hopper, opens high pressure homogenizer, pressure 85-95MPa, the logical argon gas of whole process prevents nanometer black phosphorus from being aoxidized, it recycles homogeneous 65 times, after homogeneous is complete, obtained nanometer black phosphorus dispersion liquid is centrifuged, it collects supernatant liquor, is freeze-dried to obtain the final product.The preparation process is simple, and continuous operation is at low cost, and the size of obtained nanometer black phosphorus is small, and quality is high, and yield is high, has good industrial applications foreground.
Description
Technical field
The present invention relates to a kind of methods preparing nanometer black phosphorus.
Background technology
Nanometer black phosphorus has an excellent properties not available for many block black phosphorus, such as high specific surface area, adjustable straight
Tape splicing gap, good photoelectric properties and good anisotropy etc..Make it in energy storage based on these good performances, photoelectron, urge
The fields such as change have good application prospect.
The method of traditional preparation nanometer black phosphorus mainly has mechanical stripping method, liquid phase stripping method and chemical synthesis.Machinery
Stripping method is that the conventional method of two-dimensional material is prepared by blocky stratotype crystal, mainly by adhering to adhesive tape on block materials, so
Thinner flaky material can just be obtained by tearing repeatedly afterwards, and the size that such preparation method obtains is larger, and trivial operations, take
Effort, it is difficult to be mass produced.Liquid phase stripping method is that one kind is widely used prepares ultra-thin two-dimension material from block materials
Method, by block materials, directly ultrasonic stripping, electrochemical stripping, shearing such as remove at the mechanical treatments in a solvent.It is common molten
Agent mainly has organic solvent, water and ionic liquid, this maximum defect of method to be that ultrasonic wave added is needed to remove, and time-consuming,
And low yield, it is unfavorable for prepare with scale.Chemical synthesis is by the way that the presoma of reaction reacts in substrate, deposits
Made of ultra thin dimensions nanometer sheet.In conclusion the method for preparing nanometer black phosphorus now exists, time-consuming, low output etc. is asked
Topic need to develop a kind of method that simple, quick, efficient and energy serialization prepares high quality nanometer black phosphorus.
High pressure homogenizer be it is a kind of can with the equipment of continuous operation, when material is by homogeneous chamber, while by high speed
Mechanical forces and the corresponding fuel factors such as shearing, high frequency oscillation and convection current shock, can be by material nanosizing.
Invention content
The purpose of the present invention is to provide a kind of methods preparing nanometer black phosphorus.
The present invention is realized by following technical solution：
A method of a nanometer black phosphorus is prepared, is included the following steps：10-20 parts of tin, the high tin of 5-15 parts of iodate and 80-90 parts are red
Phosphorus encapsulates in quartz ampoule under an argon atmosphere, is placed in tube furnace, and 2.5-3.5h is kept the temperature after 610-630 DEG C, is then cooled to
480-490 DEG C keeps the temperature 2.5-3.5h again, and 150 DEG C are cooled in 10h, last to be down to room temperature naturally, and opening quartz ampoule can obtain
To bulk black phosphorus；It will be added in 90-100 parts of deionized waters after 20-30 parts of black phosphorus grindings uniformly, ultrasonic 1.5-2.5h, then
Finely dispersed black phosphorus dispersion liquid is added in high pressure homogenizer hopper, unlatching high pressure homogenizer, pressure 85-95MPa, entirely
Journey, which leads to argon gas, prevents nanometer black phosphorus from being aoxidized, and material can recycle homogeneous 65 times in high pressure homogenizer, to ensure to reach preferable
Effect, after homogeneous is complete, by obtained nanometer black phosphorus dispersion liquid centrifuge 15-20min, collect supernatant liquor, freeze-drying
71-73h to get；Each raw material is parts by weight.
Preferably, in the method, 3h is kept the temperature after 620 DEG C.
Preferably, in the method, 485 DEG C is cooled to and keeps the temperature 3h again.
Preferably, in the method, ultrasonic 2h.
Preferably, in the method, pressure 90MPa.
Preferably, in the method, obtained nanometer black phosphorus dispersion liquid is centrifuged into 118min.
Preferably, in the method, it is freeze-dried 72h.
The technology of the present invention effect：
The preparation process is simple, and continuous operation is at low cost, and the size of obtained nanometer black phosphorus is small, and quality is high, and yield is high,
With good industrial applications foreground.
Specific implementation mode
The essentiality content of the present invention is specifically introduced with reference to embodiment.
Embodiment 1
A method of a nanometer black phosphorus is prepared, is included the following steps：By 15 parts of tin, the high tin of 10 parts of iodate and 85 parts of red phosphorus in argon gas
It is encapsulated in quartz ampoule under atmosphere, is placed in tube furnace, 3h is kept the temperature after 620 DEG C, be then cooled to 485 DEG C and keep the temperature 3h again, in 10h
150 DEG C are inside cooled to, it is last to be down to room temperature naturally, it opens quartz ampoule and can be obtained bulk black phosphorus；25 parts of black phosphorus grindings are uniform
After be added in 95 parts of deionized waters, finely dispersed black phosphorus dispersion liquid is then added to high pressure homogenizer hopper by ultrasonic 2h
In, high pressure homogenizer, pressure 90MPa are opened, the logical argon gas of whole process prevents nanometer black phosphorus from being aoxidized, and material can be high-pressure homogeneous
Homogeneous is recycled in machine 65 times, to ensure to reach preferable effect, after homogeneous is complete, obtained nanometer black phosphorus dispersion liquid is centrifuged
18min, collect supernatant liquor, freeze-drying 72h to get；Each raw material is parts by weight.
Embodiment 2
A method of a nanometer black phosphorus is prepared, is included the following steps：By 10 parts of tin, the high tin of 5 parts of iodate and 80 parts of red phosphorus in argon gas
It is encapsulated in quartz ampoule under atmosphere, is placed in tube furnace, 2.5h is kept the temperature after 610 DEG C, be then cooled to 480 DEG C and keep the temperature 2.5h again,
150 DEG C are cooled in 10h, it is last to be down to room temperature naturally, it opens quartz ampoule and can be obtained bulk black phosphorus；20 parts of black phosphorus are ground
It is added in 90 parts of deionized waters after uniformly, finely dispersed black phosphorus dispersion liquid is then added to high-pressure homogeneous by ultrasonic 1.5h
In machine hopper, high pressure homogenizer, pressure 85MPa are opened, the logical argon gas of whole process prevents nanometer black phosphorus from being aoxidized, and material can be in height
Press cycle homogeneous 65 times in homogenizer, to ensure to reach preferable effect, after homogeneous is complete, by obtained nanometer black phosphorus dispersion liquid from
The heart detach 15min, collect supernatant liquor, freeze-drying 71h to get；Each raw material is parts by weight.
Embodiment 3
A method of a nanometer black phosphorus is prepared, is included the following steps：By 20 parts of tin, the high tin of 15 parts of iodate and 90 parts of red phosphorus in argon gas
It is encapsulated in quartz ampoule under atmosphere, is placed in tube furnace, 3.5h is kept the temperature after 630 DEG C, be then cooled to 490 DEG C and keep the temperature 3.5h again,
150 DEG C are cooled in 10h, it is last to be down to room temperature naturally, it opens quartz ampoule and can be obtained bulk black phosphorus；30 parts of black phosphorus are ground
It is added in 100 parts of deionized waters after uniformly, finely dispersed black phosphorus dispersion liquid is then added to high-pressure homogeneous by ultrasonic 2.5h
In machine hopper, high pressure homogenizer, pressure 95MPa are opened, the logical argon gas of whole process prevents nanometer black phosphorus from being aoxidized, and material can be in height
Press cycle homogeneous 65 times in homogenizer, to ensure to reach preferable effect, after homogeneous is complete, by obtained nanometer black phosphorus dispersion liquid from
The heart detach 20min, collect supernatant liquor, freeze-drying 73h to get；Each raw material is parts by weight.
The preparation process is simple, and continuous operation is at low cost, and the size of obtained nanometer black phosphorus is small, and quality is high, yield
Height has good industrial applications foreground.
Claims (7)
1. a kind of method preparing nanometer black phosphorus, it is characterised in that include the following steps：10-20 parts of tin, 5-15 parts of iodate are high
Tin and 80-90 parts of red phosphorus encapsulate in quartz ampoule under an argon atmosphere, are placed in tube furnace, 2.5- is kept the temperature after 610-630 DEG C
3.5h, is then cooled to 480-490 DEG C and keeps the temperature 2.5-3.5h again, and 150 DEG C are cooled in 10h, is finally down to room temperature naturally, beats
It opens quartz ampoule and can be obtained bulk black phosphorus；It will be added in 90-100 parts of deionized waters after 20-30 parts of black phosphorus grindings uniformly, ultrasound
Finely dispersed black phosphorus dispersion liquid is then added in high pressure homogenizer hopper by 1.5-2.5h, opens high pressure homogenizer, pressure
For 85-95MPa, the logical argon gas of whole process prevents nanometer black phosphorus from being aoxidized, and material can recycle homogeneous 65 times in high pressure homogenizer, with
Guarantee reaches preferable effect, after homogeneous is complete, obtained nanometer black phosphorus dispersion liquid is centrifuged 15-20min, it is clear to collect upper layer
Liquid, freeze-drying 71-73h to get；Each raw material is parts by weight.
2. according to the method described in claim 1, it is characterized in that：3h is kept the temperature after 620 DEG C.
3. according to the method described in claim 1, it is characterized in that：It is cooled to 485 DEG C and keeps the temperature 3h again.
4. according to the method described in claim 1, it is characterized in that：Ultrasonic 2h.
5. according to the method described in claim 1, it is characterized in that：Pressure is 90MPa.
6. according to the method described in claim 1, it is characterized in that：Obtained nanometer black phosphorus dispersion liquid is centrifuged
118min。
7. according to the method described in claim 1, it is characterized in that：It is freeze-dried 72h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810834309.9A CN108793107A (en) | 2018-07-26 | 2018-07-26 | A method of preparing a nanometer black phosphorus |
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| CN201810834309.9A CN108793107A (en) | 2018-07-26 | 2018-07-26 | A method of preparing a nanometer black phosphorus |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650359A (en) * | 2018-12-29 | 2019-04-19 | 广西越洋科技股份有限公司 | A kind of the industrialization continuous producing apparatus and method of black phosphorus |
| CN110627028A (en) * | 2019-09-17 | 2019-12-31 | 江苏大学 | High-stability two-dimensional black phosphorus alkene, and preparation method and application thereof |
| CN110963474A (en) * | 2019-12-03 | 2020-04-07 | 昆明理工大学 | Preparation method of black phosphorus-based nano material |
| CN111892027A (en) * | 2020-08-24 | 2020-11-06 | 昆明理工大学 | Method for preparing nano black phosphorus by one-step method |
| CN112315977A (en) * | 2020-11-30 | 2021-02-05 | 南京大学 | Black phosphorus oxide nano material for osteoporosis |
| CN113174634A (en) * | 2021-04-27 | 2021-07-27 | 陕西科技大学 | Crystal red phosphorus nanowire and preparation method thereof |
| CN113666348A (en) * | 2021-09-25 | 2021-11-19 | 湖北兴发化工集团股份有限公司 | Device and method for preparing black phosphorus nanosheet by electrochemical method |
| CN115818596A (en) * | 2022-11-26 | 2023-03-21 | 昆明理工大学 | Efficient preparation method of nano black phosphorus |
-
2018
- 2018-07-26 CN CN201810834309.9A patent/CN108793107A/en not_active Withdrawn
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650359A (en) * | 2018-12-29 | 2019-04-19 | 广西越洋科技股份有限公司 | A kind of the industrialization continuous producing apparatus and method of black phosphorus |
| CN109650359B (en) * | 2018-12-29 | 2020-07-03 | 广西越洋科技股份有限公司 | Industrial continuous production equipment and method for black phosphorus |
| CN110627028A (en) * | 2019-09-17 | 2019-12-31 | 江苏大学 | High-stability two-dimensional black phosphorus alkene, and preparation method and application thereof |
| CN110963474A (en) * | 2019-12-03 | 2020-04-07 | 昆明理工大学 | Preparation method of black phosphorus-based nano material |
| CN111892027A (en) * | 2020-08-24 | 2020-11-06 | 昆明理工大学 | Method for preparing nano black phosphorus by one-step method |
| CN112315977A (en) * | 2020-11-30 | 2021-02-05 | 南京大学 | Black phosphorus oxide nano material for osteoporosis |
| CN113174634A (en) * | 2021-04-27 | 2021-07-27 | 陕西科技大学 | Crystal red phosphorus nanowire and preparation method thereof |
| CN113174634B (en) * | 2021-04-27 | 2022-05-31 | 陕西科技大学 | Crystal red phosphorus nanowire and preparation method thereof |
| CN113666348A (en) * | 2021-09-25 | 2021-11-19 | 湖北兴发化工集团股份有限公司 | Device and method for preparing black phosphorus nanosheet by electrochemical method |
| CN115818596A (en) * | 2022-11-26 | 2023-03-21 | 昆明理工大学 | Efficient preparation method of nano black phosphorus |
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Application publication date: 20181113 |