CN106744736B - A kind of synthetic method of the active porous boron nitride nanosheet for water process - Google Patents
A kind of synthetic method of the active porous boron nitride nanosheet for water process Download PDFInfo
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- CN106744736B CN106744736B CN201611217237.0A CN201611217237A CN106744736B CN 106744736 B CN106744736 B CN 106744736B CN 201611217237 A CN201611217237 A CN 201611217237A CN 106744736 B CN106744736 B CN 106744736B
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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Abstract
A kind of synthetic method of the active porous boron nitride nanosheet for water process; 0.1~10 gram of melamine or cdicynanmide are heated to 300~600 DEG C under protective atmosphere; heat preservation 0.5~4 hour, stop gas after heat preservation is passed through and cools the temperature to room temperature, obtains faint yellow product；By products therefrom and boric acid with molar ratio for 1:0.01~1:The 100 resulting mixtures of mixing are heated to 300~500 DEG C under protective atmosphere; then protective gas is passed through in the ammonium fluoroborate aqueous solution that concentration is 0.01~10mmol/L; it is passed through in reaction cavity again and continues to be heated to 600~1000 DEG C; heat preservation 0.5~4 hour; stop being passed through and cooling the temperature to room temperature for gas after heat preservation; acquired white product is active porous boron nitride nanosheet, and specific surface area is up to 817m2/ g, diameter be 50~300nm, 2~6nm of thickness, and to the organic and toxic heavy metal contamination in aqueous solution have excellent adsorption capacity, overcome common sewage treatment and scavenging material adsorption capacity it is low and reuse inefficient the defects of.
Description
Technical field
The invention belongs to inorganic porous material fields, and in particular to a kind of active porous boron nitride nanometer for water process
The synthetic method of piece.
Background technique
The structure of boron nitride nanosheet is similar to graphite, is nitrogen-atoms and the alternately arranged unlimited extension six of boron atom in layer
Hexagonal lattice, between layers by ABAB ... in a manner of be orderly alternately arranged, orderly alternate boron and nitrogen-atoms presence are very strong in layer
Polar bond.Therefore crystal structure has the interlamellar spacing along C axis direction is larger, intensity is lower, is easy to slide between layers
Soft lubrication property.Hexagonal boron nitride nanosheet has the anti-electricity vibration of preferable processability, heat resistanceheat resistant vibration, higher anti-electric field simultaneously
Breakdown strength, asepsis environment-protecting the excellent physicochemical characteristics such as do not infiltrate, are resistant to chemical etching with various metals, so that six side's nitrogen
Change boron nanometer sheet and be widely used in cosmetics, high temperature, high frequency, high-power, photoelectron and anti-radiation device, ultraviolet universe are empty
Between, the military projects space industry such as wave transparent, high performance turbine be antifriction, guided missile, carrier rocket, return formula satellite and macromolecule it is compound
Activeness and quietness improves the fields such as plastics thermal conductivity and environmental energy.
Common boron nitride nanometer piece preparation method has carbothermic method, ammonium chloride (urea)-borax method, template, water
There are low yields for (solvent) thermal method, chemical vapor deposition (CVD) method and thermal decomposition method etc., but these methods, and preparation temperature is high,
The disadvantages of at high cost or complex process is difficult to industrialization, the obtained small adsorption capacity of boron nitride nanosheet specific surface area is poor,
This seriously restricts boron nitride nanosheet in the extensive use in environmental energy field.The boron nitride nanosheet ruler of these methods synthesis
Degree is uneven, and bigger disadvantage is that synthesis process needs high temperature, and not only energy consumption is high, but also the safety for increasing production is hidden
Suffer from.Therefore, there is an urgent need to a kind of preparation cost is cheap, simple process, environmental pollution is small, and low energy consumption, and products obtained therefrom has
The method of excellent sewage disposal and purification ability.
Summary of the invention
It is an object of the invention to solve the problems of the prior art, provide that a kind of yield is high, preparation condition is mild, cost
The preparation side of low, simple process the active porous boron nitride nanosheet to pollutant in aqueous solution with good adsorbent ability
Method, and the preparation method is easy to amplify, and can achieve the purpose of batch production.
The technical scheme is that：A kind of synthetic method of the active porous boron nitride nanosheet for water process,
It is characterized in that：(1) 0.1~10 gram of melamine or cdicynanmide are heated to 300~600 DEG C under protective atmosphere, heat preservation 0.5
~4 hours, stop gas after heat preservation was passed through and cools the temperature to room temperature, obtained faint yellow product；It (2) will be obtained by (1)
Product mixes resulting mixture with boric acid and is heated to 300~500 DEG C under nitrogen or argon, then leads to protective gas
Enter in ammonium fluoroborate aqueous solution, then be passed through in reaction cavity and continue to be heated to 600~1000 DEG C, keeps the temperature 0.5~4 hour, heat preservation
After stop gas be passed through and cool the temperature to room temperature, acquired white product is active porous boron nitride nanosheet,
Specific surface area is up to 817m2/ g, diameter is 50~300nm, 2~6nm of thickness, and is had to the pollutant in aqueous solution excellent
Adsorption capacity.
Protective atmosphere described in previous step (1) is neon, Krypton, argon gas or nitrogen.
When protective atmosphere in previous step (1) is neon, Krypton, argon gas or nitrogen, gas flow rate is 50-500 milliliters/
Per minute.
The molar ratio of faint yellow product described in previous step (2) and boric acid is 1:0.01~1:100.
The concentration of ammonium fluoroborate aqueous solution described in previous step (2) is 0.01~10mmol/L.
Protective atmosphere gas flow rate in previous step (2) is 100~300 milliliters/per minute.
The beneficial effects of the invention are as follows：
1. the obtained product of the method for the present invention is the active porous boron nitride nanosheet with hexagonal structure, such as Fig. 1 institute
Show, wide-angle part (2 θ=10~90 °) diffraction maximum is clear in x-ray diffractogram of powder spectrum, is staggered floor boron nitride；Fig. 2 and Fig. 3 are
The scanning electron microscope diagram and transmission electron microscope figure of active porous boron nitride nanosheet, respectively illustrate this method and obtain
Boron nitride nanosheet pattern it is uniform, thickness is only 2~6nm, and edge has fault of construction position abundant；Fig. 4 is that activity is more
The absorption of nitrogen and desorption isotherm in a low temperature of the boron nitride nanosheet of hole, it is shown that the active porous boron nitride nanosheet tool of gained
There is high specific surface area；It is excellent that Fig. 5 and Fig. 6 shows that active porous boron nitride nanosheet has the pollutant in aqueous solution
Adsorption capacity and regeneration recycling ability.
2. gained boron nitride nanosheet of the invention has the properties such as peculiar light, electricity, magnetic, heat and absorption, especially high
The characteristics such as specific surface area, fault of construction abundant and B-N bond polarity become excellent water purification material, this activity
Porous boron nitride nanometer sheet, which has, is up to every gram of 0.42 gram of absorption, weight to the adsorption capacity of toxic heavy metal contamination at normal temperature
It the use of adsorption capacity after 10 times is more than again 70%, the defect for overcoming common active carbon that cannot reuse, in water process and only
Change field is widely used.
3. the raw material that the present invention uses for boric acid, belongs to industrialization product, price is relatively inexpensive to be easy to get, and life can be greatly reduced
Produce cost.
4. synthesis needs used in the present invention are simple compared with low temperature, technical process, it is suitable for scale industrial production.
Detailed description of the invention
The present invention is further described with specific implementation with reference to the accompanying drawing.
Fig. 1 is active porous boron nitride nanosheet X-ray diffraction spectrogram in example 1.
Fig. 2 is active porous boron nitride nanosheet scanning electron microscope diagram in example 1.
Fig. 3 is active porous boron nitride nanosheet transmission electron microscope figure in example 1.
Fig. 4 is active porous boron nitride nanosheet low temperature nitrogen adsorption and desorption thermoisopleth in example 1.
Fig. 5 is the rate of adsorption of active porous boron nitride nanosheet room temperature inorganic pollution in example 1.
Fig. 6 is the power of regeneration test chart of active porous boron nitride nanosheet in example 1.
Specific embodiment
It is further described the present invention below by specific embodiment, but embodiment will not be constituted to limit of the invention
System.
Embodiment 1：
(1) it weighs and is heated to 0.1 gram of melamine in the case where throughput is 50 milliliters/nitrogen atmosphere protection per minute
300 DEG C, 0.5 hour is kept the temperature, stop gas after heat preservation is passed through and cools the temperature to room temperature, obtains faint yellow product；(2)
Products therefrom and boric acid are with molar ratio for 1:The 0.01 resulting mixture of mixing is heated to 300 DEG C under nitrogen protection, then will
Protective gas is passed through in the ammonium fluoroborate aqueous solution that concentration is 0.01mmol/L, then is passed through and is continued to be heated to 600 in reaction cavity
DEG C, 0.5 hour is kept the temperature, stop gas after heat preservation is passed through and cools the temperature to room temperature, and acquired white product is activity
Porous boron nitride nanometer sheet, specific surface area is up to 817m2/ g, diameter are 50~300nm, 2~6nm of thickness, and to aqueous solution
In organic and inorganic pollution there is excellent adsorption capacity.
It is tested through X-ray diffraction, the wide-angle diffraction peak in Fig. 1 shows that product is hexagonal boron nitride, and diffraction maximum is very clear
It is clear；Find out that product is laminated structure through scanning electron microscope diagram (Fig. 2)；Product is found out through transmission electron microscope figure (Fig. 3)
For laminated structure；Again through low temperature nitrogen adsorption and desorption thermoisopleth (Fig. 4), can calculate its specific surface area is 817 squares every gram
Rice, pore volume are 0.57 cubic metre every gram；The above map illustrates that obtain is to have a large amount of activated adoption positions, Gao Bibiao to the present invention
Area and macropore volume boron nitride ceramic material.Finally, we survey the water process and detergent power of active boron nitride
Examination.Fig. 5 shows that it reaches every gram in adsorption capacity of the room temperature to aqueous solution Poisoning heavy metal contaminants and adsorbs 0.42 gram；Fig. 6
Show that active boron nitride is reused 10 times, adsorption capacity keeps 70% or more adsorption capacity, this illustrates active nitride
Boron is convenient for recycling.This material is with a wide range of applications in field of environmental improvement.
Embodiment 2：
Be changed to cyanamid dimerization through step (1) melamine in embodiment 1, other operations with
Embodiment 1 is identical, obtains product with embodiment 1.
Embodiment 3,4：
The dosage of step (1) melamine or cyanamid dimerization in embodiment 1 is changed to 1g, 10g, other every behaviour respectively
Work is same as Example 1, obtains product with embodiment 1.
Embodiment 5,6,7：
Step (1) nitrogen in embodiment 1 is changed to neon, Krypton, argon gas respectively, other operations are and embodiment
1 is identical, obtains product with embodiment 1.
Embodiment, 8,9：
Per minute 100,500mL, other every behaviour are changed into the circulation of step (1) protection gas in embodiment 1 respectively
Work is same as Example 1, obtains product with embodiment 1.
Embodiment 10,11：
The heating temperature of step (1) in embodiment 1 is changed to 450,600 DEG C respectively, other operations with implementation
Example 1 is identical, obtains product with embodiment 1.
Embodiment 12,13：
The soaking time of step (1) in embodiment 1 is changed to 2,4 hours respectively, other operations with embodiment 1
It is identical, product is obtained with embodiment 1.
Embodiment 14,15：
The faint yellow crude product of step (2) in embodiment 1 and the molar ratio of boric acid are changed to 1 respectively:1,1:100, other
Operations it is same as Example 1, obtain product with embodiment 1.
Embodiment 16,17：
Heating temperature when step (2) gas does not pass through ammonium fluoroborate solution in embodiment 1 is changed to 400,500 DEG C respectively,
Other operations are same as Example 1, obtain product with embodiment 1.
Embodiment 18,19：
The concentration of step (2) ammonium fluoroborate solution in embodiment 1 is changed to 1mmol/L, 10mmol/L respectively, it is other each
Item operation is same as Example 1, obtains product with embodiment 1.
Embodiment 20,21：
Heating temperature when step (2) gas passes through ammonium fluoroborate solution in embodiment 1 is changed to 800,1000 DEG C respectively,
His operations are same as Example 1, obtain product with embodiment 1.
Embodiment 22,23：
The throughput of step (2) in embodiment 1 is changed to per minute 200,300mL respectively, other operations with
Embodiment 1 is identical, obtains product with embodiment 1.
Embodiment 23,24：
The soaking time of step (2) in embodiment 1 is changed to 2,4 hours respectively, other operations with embodiment 1
It is identical, product is obtained with embodiment 1.
Claims (6)
1. a kind of synthetic method of the active porous boron nitride nanosheet for water process, which is characterized in that include the following steps：
Step 1：0.1~10 gram of melamine or cdicynanmide are heated to 300~600 DEG C under protective atmosphere, heat preservation 0.5
~4 hours, stop gas after heat preservation was passed through and cools the temperature to room temperature, obtained faint yellow product；
Step 2：Products therefrom is mixed into resulting mixture with boric acid and is heated to 300~500 under nitrogen or argon
DEG C, then protective gas is passed through in the aqueous solution containing ammonium fluoroborate；Be passed through in reaction cavity again continue to be heated to 600~
1000 DEG C, 0.5~4 hour is kept the temperature, stop gas after heat preservation is passed through and cools the temperature to room temperature, acquired white product
For active porous boron nitride nanosheet, specific surface area reaches 817m2/ g, diameter are 50~300nm, 2~6nm of thickness, and to water
Pollutant in solution has adsorption capacity.
2. synthetic method according to claim 1, it is characterised in that：The protective atmosphere be neon, Krypton, argon gas or
Nitrogen.
3. synthetic method according to claim 1, it is characterised in that：The protective atmosphere be neon, Krypton, argon gas or
When nitrogen, gas flow rate is 50-500 milliliter/it is per minute.
4. synthetic method according to claim 1, it is characterised in that：The faint yellow product and boron that the mixture includes
The molar ratio of acid is 1:0.01~1:100.
5. synthetic method according to claim 1, it is characterised in that：The aqueous solution of ammonium fluoroborate is 0.01~10mmol/
L。
6. synthetic method according to claim 1, it is characterised in that：It is passed through containing ammonium fluoroborate aqueous solution protective gas stream
Speed for 100~300 milliliters/per minute.
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| CN107265417B (en) * | 2017-07-24 | 2019-10-01 | 江苏大学 | A kind of boron defect boron nitride nanosheet and its preparation method and application |
| CN107774292B (en) * | 2017-10-11 | 2019-11-15 | 中国地质大学（武汉） | A kind of preparation method of oxygen doping boron nitride catalyst carrier carried metal |
| CN107694595B (en) * | 2017-10-11 | 2019-11-15 | 中国地质大学（武汉） | A kind of preparation method of oxygen doping boron nitride catalyst carrier |
| CN109265178A (en) * | 2018-09-10 | 2019-01-25 | 湖北第二师范学院 | A kind of preparation method of the porous boron nitride foamed material for Water warfare |
| CN109894078A (en) * | 2019-03-13 | 2019-06-18 | 湖北第二师范学院 | A kind of cocoanut active charcoal adsorbent material and manufacture craft based on water process |
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| FR2597087B1 (en) * | 1986-04-15 | 1988-06-24 | Centre Nat Rech Scient | USE AS A FLOW IN THE PREPARATION OF CUBIC BORON NITRIDE OF A FLUORONITRIDE AND PROCESS FOR THE PREPARATION OF CUBIC BORON NITRIDE USING SUCH A FLOW |
| CN1329290C (en) * | 2004-09-01 | 2007-08-01 | 山东大学 | Phase selection in-situ synthesis method used for controlling boron nitride object phase |
| CN100590069C (en) * | 2008-03-28 | 2010-02-17 | 山东大学 | Method for preparing boron nitride coating carbon nano-tube/nano-wire and boron nitride nano-tube |
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| CN103539085A (en) * | 2013-11-05 | 2014-01-29 | 河北工业大学 | Synthesis method for hexagonal boron nitride nanosheet |
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