CN109336127A - A kind of boron alkene and preparation method thereof - Google Patents
A kind of boron alkene and preparation method thereof Download PDFInfo
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- CN109336127A CN109336127A CN201811456915.8A CN201811456915A CN109336127A CN 109336127 A CN109336127 A CN 109336127A CN 201811456915 A CN201811456915 A CN 201811456915A CN 109336127 A CN109336127 A CN 109336127A
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Abstract
The invention discloses a kind of boron alkene and preparation method thereof.The present invention is by the way that boron source and oxidant to be added in polar organic solvent, under air-proof condition, through a long time stir process, reaction product is obtained, obtained reaction product is filtered, obtains boron nanometer sheet powder, again by boron nano powder dispersion in polar organic solvent, through ultrasonic wave liquid phase lift-off processing, dispersion liquid is obtained, then obtains boron alkene through centrifugal treating, compared with prior art, it is simple with chemical process, the advantages of lower production costs, matters large scale preparation boron alkene.
Description
Technical field
The present invention relates to two-dimension nano materials preparation technical fields more particularly to a kind of boron alkene and preparation method thereof.
Background technique
Since graphite has been removed to obtain since graphene is succeeded, scientific circles to the research interests of two-dimension nano materials very
Greatly, the core of research is had become in recent years.Various atom level ultra-thin two-dimension materials are all successively from layered solid material
It is derived, to these materials, from electronics (i.e. field effect transistor, photovoltaic, sensing), to membrane technology, (i.e. desalination is received for numerous researchs
Metre hole sensing) energy storage and the application progress for being catalyzed different fields such as (i.e. supercapacitor, photocatalysis, water decompositions) are arrived again
It explores.
Nevertheless, the discovery of New Two Dimensional material and synthesis are still most arduous one of the challenge of Material Field.Composition
The many factors such as element, growth substrate and preparation condition all play key effect to synthesis single layer two-dimensional material.Boron alkene has
Anisotropy and metallicity, therefore be described as most light two-dimensional metallic, at the same also show unique mechanical, optics and respectively to
Anisotropic metallicity, this is the supplement to conventional two-dimensional material.Boron-boron key multicenter characteristic causes it easy to form in structure
Void geometry, therefore in terms of electronic application, chemical functionalization, materials synthesis and labyrinth construction, it is two-dimensional material field
Provide unprecedented diversity.
Although boron alkene has caused extensive research interest, due to block boron powder itself and it is not belonging to stratiform knot
Structure, while complicated crystal structure is had both, the synthesis of boron alkene is not apparent also.In the exploration of early stage, the synthesis of boron alkene
In the significant challenge that faces be easily contaminated boron, material purity and matrix compatibility.In the recent period, there are two independent researchs
Using ultravacuum molecular beam epitaxy (UHV-MBE) technology, pure solid phase boron simultaneously as the silver of presoma and (111) face is matrix
Boron alkene is synthesized, but to test the performance of boron alkene itself, it is also necessary to it removes matrix and is grown in other substances on matrix
It influences.It is at high price that boron alkene device therefor is prepared at present, preparation condition requires harshness, and chemical process is complicated, and production cost is higher,
To large scale preparation boron alkene and being applied still in practice has very big difficulty.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of preparation methods of boron alkene, it is intended to solve
Certainly prior art processes are complicated, target product low output, to the demanding problem of production equipment.
The technical proposal for solving the technical problem of the invention is as follows:
A kind of preparation method of boron alkene, wherein comprising steps of
Boron source, oxidant are mixed with organic solvent, boron nanometer sheet powder is obtained after reaction；
The boron nanometer sheet powder is added in organic solvent again, under constant temperature conditions, with ultrasonic wave to contain boron nanometer sheet
The solution of powder carries out liquid phase lift-off processing, obtains dispersion liquid；
The dispersion liquid is centrifuged, retains bottom sediment, obtains boron alkene.
The preparation method, wherein the boron source is titanium diboride, aluminium diboride, magnesium diboride, silicon hexaboride and six
One of calcium boride is a variety of.
The preparation method, wherein the oxidant is one of nitric acid, bromine, iodine, potassium permanganate and hydrogen peroxide
Or it is a variety of.
The preparation method, wherein the organic solvent is water, acetonitrile, ethyl alcohol, n,N-Dimethylformamide, N- first
One of base pyrrolidones and dimethyl sub-maple are a variety of.
The preparation method, wherein in the boron source and the molal weight of the oxidant than the ratio for 1:1-10,
Boron source, oxidant are mixed with organic solvent, boron nanometer sheet powder is obtained after reaction.
The preparation method, wherein the step mixes boron source, oxidant with organic solvent, and boron is obtained after reaction
Nanometer sheet powder, specifically includes:
Boron source, oxidant and organic solvent are added in plastic containers, reacted 1-40 days under agitation, reaction is obtained and produces
Object；
The reaction product is filtered to obtain powder object；The powder object is dried under vacuum conditions again,
Obtain boron nanometer sheet powder.
The preparation method, wherein it is described under constant temperature conditions, with ultrasound carry out liquid phase lift-off processing, wherein constant temperature
Temperature is 5-25 DEG C, and ultrasonic time is 1-15 hours.
The preparation method, wherein the dispersion liquid is centrifuged the step, retains bottom sediment,
Boron alkene is obtained, is specifically included:
The dispersion liquid is subjected to first time centrifugal treating, the supernatant liquor after taking centrifugation carries out second and is centrifugated, retains
Bottom sediment obtains boron alkene；The condition of the first time centrifuge separation is centrifugal rotational speed 500-5000 r/min, is centrifuged duration
For 1-60min；The condition of second centrifuge separation is centrifugal rotational speed 1000-18000 r/min, when centrifugation a length of 1-
60min。
The preparation method, wherein the dispersion liquid is centrifuged the step, retains bottom sediment,
After obtaining boron alkene further include:
Obtained boron alkene is converted with organic solvent, is dried in vacuo 1-10 hours under the conditions of 40-80 DEG C of temperature after conversion,
Obtain boron alkene nanometer sheet.
A kind of boron alkene, wherein be prepared using preparation method described above
The utility model has the advantages that the invention has the following advantages over the prior art:
(1), equipment is simple and safe, easy to operate, and cost is relatively low.
(2), products obtained therefrom yield is high, and impurity is few.
It (3), is suitable for producing in enormous quantities, commercial value with higher.
Detailed description of the invention
Fig. 1 is a kind of flow chart of boron alkene preparation method preferred embodiment of the present invention.
Fig. 2 is the flow chart of step S10 in a kind of boron alkene preparation method preferred embodiment of the present invention.
Fig. 3 is the scanning electron microscope (SEM) photograph of boron alkene nanometer sheet in the embodiment of the present invention 1.
Fig. 4 is the scanning electron microscope (SEM) photograph of boron alkene nanometer sheet in the embodiment of the present invention 2.
Fig. 5 is the scanning electron microscope (SEM) photograph of boron alkene nanometer sheet in the embodiment of the present invention 3.
Fig. 6 is the scanning electron microscope (SEM) photograph of boron alkene nanometer sheet in the embodiment of the present invention 4.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer and more explicit, right as follows in conjunction with drawings and embodiments
The present invention is further described.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and do not have to
It is of the invention in limiting.
Referring to Fig. 1, its flow chart for the preparation method preferred embodiment of boron alkene of the present invention.The preparation method is specific
Include:
S10, boron source, oxidant are mixed with organic solvent, boron nanometer sheet powder is obtained after reaction；
S20, the boron nanometer sheet powder is added in organic solvent again, under constant temperature conditions, received with ultrasonic wave to containing boron
The solution of rice piece powder carries out liquid phase lift-off processing, obtains dispersion liquid；
S30, the dispersion liquid is centrifuged, retains bottom sediment, obtains boron alkene.
For the problem that the preparation method of boron alkene in the prior art is complicated, the high equipment of Price-dependent, low yield, this hair
It is bright by the way that boron source and oxidant are added in polar organic solvent, under air-proof condition, through a long time stir process is obtained anti-
Product is answered, obtained reaction product is filtered, obtains boron nanometer sheet powder, then boron nanometer powder is dissolved in polarity to have
In solvent, through ultrasonic wave liquid phase lift-off processing, dispersion liquid is obtained, then obtain boron alkene through centrifugal treating, compared with prior art,
It is simple with chemical process, the advantages of lower production costs, matters large scale preparation boron alkene.
In one embodiment, the boron source can be titanium diboride (TiB2), aluminium diboride (AlB2), magnesium diboride
(MgB2), silicon hexaboride (SiB6) and six calcium boride (CaB6) etc. one of or it is a variety of, but not limited to this.
In one embodiment, the oxidant can be in nitric acid, bromine, iodine, potassium permanganate and hydrogen peroxide etc.
It is one or more, but not limited to this.
In one embodiment, the organic solvent is polar organic solvent, and polar organic solvent can be acetonitrile, second
One of alcohol, N,N-dimethylformamide (DMF), N-Methyl pyrrolidone (NMP), dimethyl sub-maple (DMSO) and water etc. or
It is a variety of, but not limited to this.
In one embodiment, it is 1 by the molal weight ratio of the boron source and the oxidant in the step S10:
The ratio of 1-10 is mixed.Preferably, the molal weight ratio of boron source and the oxidant is 1:1.5.
In one embodiment, as shown in Fig. 2, the step S10 is specifically included:
S101, boron source, oxidant and organic solvent are added in plastic containers, react 1-40 days, obtains under agitation
Reaction product；
S102, the reaction product is filtered to obtain powder object；The powder object is dried under vacuum conditions again
Processing, obtains boron nanometer sheet powder.
Specifically, after boron source and oxidant being added in organic solvent, since it is desired that long agitation, organic solvent
It is volatile therefore be sealed.Further, mixing speed is 100-800 r/min(such as 400 r/min), when stirring
Between be 30 days, with guarantee reaction can thoroughly carry out.
Further, after stirring, the product in step S101 is filtered, the powder filtered has with polarity
Solvent is repeated rinse, ultrasonic disperse processing, filter and etc. 1-6 times, to remove byproduct of reaction.
In a preferred embodiment, will in step S102 filter after resulting powder under vacuum conditions, 40-80
After DEG C (such as 60 DEG C) dry 1-10 hour, pure boron nanometer sheet powder is obtained.
In one embodiment, in the step S20, it is described under constant temperature conditions, with ultrasound carry out at liquid phase removing
Reason is specifically by the way of water bath with thermostatic control heating, by temperature control at 5-25 DEG C, ultrasonic machine is carried out at liquid phase removing
Reason, ultrasonic machine power 50-800W, sonication treatment time are 1-15 hours.It should be noted that the heating method in this step
But it is other heated at constant temperature, such as can be electromagnetism, oil bath, be not limited in cited water bath with thermostatic control.
In one embodiment, the step S30 is specifically included: the dispersion liquid is subjected to first time centrifugal treating,
Supernatant liquor after taking centrifugation；Obtained supernatant liquor is carried out second to be centrifugated, reservation bottom sediment, in removing
Layer clear liquid, obtains boron alkene；Wherein, the condition of the first time centrifuge separation is centrifugal rotational speed 500-5000 r/min(such as 3000
R/min), a length of 1-60min(such as 15min when centrifugation)；The condition of second of centrifuge separation is centrifugal rotational speed 1000-
18000 r/min(such as 14000 r/min), when centrifugation a length of 1-60min(such as 30min).
In a kind of better embodiment, after the step S30 further include: turned obtained boron alkene with ethyl alcohol
It changes, is dried in vacuo 1-10 hours (such as 5 hours) after conversion under the conditions of 40-80 DEG C of temperature (such as 60 DEG C), obtains boron alkene nanometer sheet.
Boron alkene obtained in step S30 is converted to remove polar organic solvent remaining in boron alkene with ethyl alcohol, such as N- methyl pyrrole
Then pyrrolidone is under vacuum conditions dried the boron alkene after conversion, obtain boron alkene nanometer sheet.
It the present invention also provides a kind of boron alkene, is obtained by above-mentioned preparation method.
A kind of boron alkene of the present invention and preparation method thereof is explained below by specific embodiment:
Embodiment 1:
Weigh the MgB of certain mass respectively by the molar ratio of 1:12With elemental iodine, it is added to the plastic bottle equipped with 200 ml acetonitriles
In, then with the revolving speed stir process of 100 r/min 1 day under air-proof condition；After stirring, product in bottle is taken out
Rinse is repeated with acetonitrile in filtered powder by filter processing, and ultrasonic disperse processing filters five times, removes by-product；Cleaning
40 DEG C of powder 1 hour of vacuum drying afterwards；Powder is added in the nmp solvent of 250ml, water bath with thermostatic control ultrasonic machine carries out liquid
Phase lift-off processing: power is 500 W, 5 DEG C of bath temperature, is ultrasonically treated 1 hour；Obtained dispersion liquid after being ultrasonically treated
It carries out centrifugal treating: behind revolving speed centrifugal treating 1 minute of 3000 r/min, taking supernatant liquor；Then turned with 14000 r/min
Fast centrifugal treating 20 minutes, takes bottom sediment.With nmp solvent remaining in ethanol conversion sediment, 40 DEG C of vacuum drying 1 are small
When, obtain boron alkene nanometer sheet.Boron alkene nanometer sheet pattern is referring to Fig. 3.
Embodiment 2:
Weigh the TiB of certain mass respectively by the molar ratio of 1:52With bromine simple substance, it is added in the bottle equipped with 200 ml acetonitriles,
Then with the revolving speed stir process of 300 r/min 35 days under air-proof condition；After stirring, product in bottle is filtered
Rinse, ultrasonic disperse processing is repeated with acetonitrile in filtered powder by processing, and suction filtration etc. five times removes by-product；Cleaning
60 DEG C of powder 4 hours of vacuum drying afterwards；Powder is added in the DMF solvent of 250ml, water bath with thermostatic control ultrasonic machine carries out
Liquid phase lift-off processing: power is 600 W, 10 DEG C of bath temperature, is ultrasonically treated 5 hours；Obtained point after being ultrasonically treated
Dispersion liquid carries out centrifugal treating: behind revolving speed centrifugal treating 15 minutes of 3000 r/min, taking supernatant liquor；Then with 15000 r/
The revolving speed centrifugal treating of min 20 minutes, takes bottom sediment.With DMF solvent remaining in ethanol conversion sediment, 60 DEG C of vacuum
It is 4 hours dry, obtain boron alkene nanometer sheet.Boron alkene nanometer sheet pattern is referring to fig. 4.
Embodiment 3:
Weigh the AlB of certain mass respectively by the molar ratio of 1:1.52With HNO3, it is added to the bottle equipped with 300 ml deionized waters
In, then with the revolving speed stir process of 350 r/min 40 days under air-proof condition；After stirring, product in bottle is taken out
Rinse, ultrasonic disperse processing is repeated with ethyl alcohol in filtered powder by filter processing, and suction filtration etc. five times removes by-product；Clearly
80 DEG C of powder 10 hours of vacuum drying after washing；Powder is added in the DMSO solvent of 250 ml, water bath with thermostatic control ultrasonic machine
Carry out liquid phase lift-off processing: power is 500 W, 25 DEG C of bath temperature, is ultrasonically treated 15 hours；Obtained by after being ultrasonically treated
Dispersion liquid carry out centrifugal treating: the revolving speed centrifugal treating of 3000 r/min after sixty minutes, takes supernatant liquor；Then with 18000
The revolving speed centrifugal treating of r/min 60 minutes, takes bottom sediment.With DMSO solvent remaining in ethanol conversion sediment, 80 DEG C
Vacuum drying 10 hours, obtains boron alkene nanometer sheet.Boron alkene nanometer sheet pattern is referring to Fig. 5.
Embodiment 4:
Weigh the CaB of certain mass respectively by the molar ratio of 1:106With H2O2, it is added in the bottle equipped with 300 ml ethyl alcohol, so
Afterwards with the revolving speed stir process of 800 r/min 25 days under air-proof condition；After stirring, product in bottle is carried out at suction filtration
Rinse, ultrasonic disperse processing is repeated with ethyl alcohol in filtered powder by reason, and suction filtration etc. five times removes by-product；After cleaning
Powder 60oC is dried in vacuo 4 hours；Powder is added in the water of 250ml, water bath with thermostatic control ultrasonic machine carries out liquid phase removing
Processing: power is 600 W, 10 DEG C of bath temperature, is ultrasonically treated 5 hours；Obtained dispersion liquid carries out after being ultrasonically treated
Centrifugal treating: behind revolving speed centrifugal treating 15 minutes of 3000 r/min, supernatant liquor is taken；Then with the revolving speed of 15000 r/min
Centrifugal treating 20 minutes, take bottom sediment.60 DEG C are dried in vacuo 4 hours, obtain boron alkene nanometer sheet.Boron alkene nanometer sheet pattern ginseng
See Fig. 6.
In conclusion the present invention is provided, the present invention provides a kind of boron alkene and preparation method thereof.The present invention is by by boron source
It is added in polar organic solvent with oxidant, under air-proof condition, through a long time stir process obtains reaction product, to institute
Obtained reaction product is filtered, and obtains boron nanometer sheet powder, then boron nanometer powder is dissolved in polar organic solvent, warp
Ultrasonic wave liquid phase lift-off processing obtains dispersion liquid, then obtains boron alkene through centrifugal treating, compared with prior art, has chemical mistake
The advantages of journey is simple, lower production costs, matters large scale preparation boron alkene.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of preparation method of boron alkene, which is characterized in that comprising steps of
Boron source, oxidant are mixed with organic solvent, boron nanometer sheet powder is obtained after reaction；
The boron nanometer sheet powder is added in organic solvent again, under constant temperature conditions, with ultrasonic wave to contain boron nanometer sheet
The solution of powder carries out liquid phase lift-off processing, obtains dispersion liquid；
The dispersion liquid is centrifuged, retains bottom sediment, obtains boron alkene.
2. preparation method according to claim 1, which is characterized in that the boron source is titanium diboride, aluminium diboride, two boron
Change one of magnesium, silicon hexaboride and six calcium borides or a variety of.
3. preparation method according to claim 1, which is characterized in that the oxidant is nitric acid, bromine, iodine, potassium permanganate
With one of hydrogen peroxide or a variety of.
4. preparation method according to claim 1, which is characterized in that the organic solvent is acetonitrile, ethyl alcohol, water, N, N-
One of dimethylformamide, N-Methyl pyrrolidone and dimethyl sub-maple are a variety of.
5. preparation method according to claim 1, which is characterized in that by the molal weight of the boron source and the oxidant
Than the ratio for 1:1-10, boron source, oxidant are mixed with organic solvent, boron nanometer sheet powder is obtained after reaction.
6. preparation method according to claim 1, which is characterized in that the step is by boron source, oxidant and organic solvent
Mixing, obtains boron nanometer sheet powder, specifically includes after reaction:
Boron source, oxidant and organic solvent are added in plastic containers, reacted 1-40 days under agitation, reaction is obtained and produces
Object；
The reaction product is filtered to obtain powder object；The powder object is dried under vacuum conditions again,
Obtain boron nanometer sheet powder.
7. preparation method according to claim 1, which is characterized in that it is described under constant temperature conditions, carry out liquid with ultrasonic wave
Phase lift-off processing, wherein thermostat temperature is 5-25 DEG C, and ultrasonic time is 1-15 hours.
8. preparation method according to claim 1, which is characterized in that the dispersion liquid is carried out centrifugation point by the step
From reservation bottom sediment obtains boron alkene, specifically includes:
The dispersion liquid is subjected to first time centrifugal treating, the supernatant liquor after taking centrifugation carries out second and is centrifugated, retains
Bottom sediment obtains boron alkene；The condition of the first time centrifuge separation is centrifugal rotational speed 500-5000 r/min, is centrifuged duration
For 1-60min；The condition of second centrifuge separation is centrifugal rotational speed 1000-18000 r/min, when centrifugation a length of 1-
60min。
9. the preparation method according to claim 4, which is characterized in that the dispersion liquid is carried out centrifugation point by the step
From retaining bottom sediment, after obtaining boron alkene further include:
Obtained boron alkene is converted with ethyl alcohol, is dried in vacuo 1-10 hours, obtains under the conditions of 40-80 DEG C of temperature after conversion
Boron alkene nanometer sheet.
10. a kind of boron alkene, which is characterized in that be prepared using the described in any item preparation methods of the claims 1-9.
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| CN109884838A (en) * | 2019-03-20 | 2019-06-14 | 深圳大学 | Full photo threshold device and the preparation method of application, boron alkene quantum dot solution |
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