CN106744736A - 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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- CN106744736A CN106744736A CN201611217237.0A CN201611217237A CN106744736A CN 106744736 A CN106744736 A CN 106744736A CN 201611217237 A CN201611217237 A CN 201611217237A CN 106744736 A CN106744736 A CN 106744736A
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- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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; insulation 0.5~4 hour, insulation stops being passed through and cooling the temperature to room temperature for gas after terminating, and obtains faint yellow product；By products therefrom and boric acid with mol ratio be 1:0.01~1:Mixture obtained by 100 mixing is 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 again in reaction cavity and continues to be heated to 600~1000 DEG C; insulation 0.5~4 hour; insulation stops being passed through and cooling the temperature to room temperature for gas after terminating; resulting white product is active porous boron nitride nanosheet, and its specific surface area is up to 817m2/ g, a diameter of 50~300nm, 2~6nm of thickness, and to the aqueous solution in organic and toxic heavy metal contamination there is excellent adsorption capacity, overcome conventional sewage disposal and scavenging material adsorption capacity low and reuse the defects such as inefficient.
Description
Technical field
The invention belongs to inorganic porous material field, and in particular to a kind of active porous boron nitride nanometer for water process
The synthetic method of piece.
Background technology
The structure of boron nitride nanosheet is unlimited extension six that nitrogen-atoms and boron atom are alternately arranged in layer similar to graphite
Hexagonal lattice, between layers with ABAB ..., mode is alternately arranged in order, and orderly alternate boron and nitrogen-atoms exist very strong in layer
Polar bond.Therefore crystal structure the interlamellar spacing along C direction of principal axis it is larger, intensity is relatively low, be easy between layers slide, have
Soft lubrication property.Simultaneously hexagonal boron nitride nanosheet have preferable processability, heat resistanceheat resistant shake anti-electricity shake, anti-electric field higher
Breakdown strength, asepsis environment-protecting and various metals do not infiltrate, the excellent physicochemical characteristics such as resistant to chemical etching so that six side's nitrogen
Change boron nanometer sheet and be widely used in cosmetics, high temperature, high frequency, high-power, photoelectron and radioresistance device, ultraviolet universe are empty
Between, the military project space industry such as wave transparent, antifriction high performance turbine, guided missile, carrier rocket, return formula satellite and macromolecule it is compound
The field such as activeness and quietness, raising plastics thermal conductivity and environmental energy.
Conventional boron nitride nanometer piece preparation method has carbothermic method, ammonium chloride (urea)-borax method, template, water
(solvent) hot method, chemical vapor deposition (CVD) method and thermal decomposition method etc., but there is low yield in these methods, and preparation temperature is high,
The shortcomings of high cost or complex process are difficult to industrialization, the resulting small adsorption capacity of boron nitride nanosheet specific surface area is poor,
This seriously governs extensive use of the boron nitride nanosheet in environmental energy field.The boron nitride nanosheet chi of these methods synthesis
Degree is uneven, and bigger shortcoming is that building-up process needs high temperature, not only high energy consumption, and it is hidden to increased the safety of production
Suffer from.Therefore, in the urgent need to a kind of preparation cost is cheap, process is simple, environmental pollution is small, and energy consumption is low, and products obtained therefrom has
The method of excellent sewage disposal and purification ability.
The content of the invention
It is an object of the invention to solve the problems of the prior art, there is provided a kind of yield is high, preparation condition gentle, cost
The preparation side of low, process is simple the active porous boron nitride nanosheet to pollutant in the aqueous solution with good adsorbent ability
Method, and the preparation method is easy to amplification, can reach 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, its
It is characterised by：(1) 0.1~10 gram of melamine or cdicynanmide are heated to 300~600 DEG C, insulation 0.5 under protective atmosphere
~4 hours, insulation stopped being passed through and cooling the temperature to room temperature for gas after terminating, and obtains faint yellow product；(2) by (1) gained
Product mix with boric acid obtained by mixture be heated to 300~500 DEG C under nitrogen or argon, then protective gas is led to
In entering the ammonium fluoroborate aqueous solution, then it is passed through in reaction cavity and continues to be heated to 600~1000 DEG C, is incubated 0.5~4 hour, insulation
Stop being passed through and cooling the temperature to room temperature for gas after end, resulting white product is active porous boron nitride nanosheet, its
Specific surface area is up to 817m2/ g, a diameter of 50~300nm, 2~6nm of thickness, and have to the pollutant in the 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/
It is per minute.
The mol ratio of faint yellow product and boric acid described in previous step (2) is 1:0.01~1:100.
The concentration of the ammonium fluoroborate aqueous solution described in previous step (2) is 0.01~10mmol/L.
Protective atmosphere gas flow rate in previous step (2) for 100~300 milliliters/it is per minute.
The beneficial effects of the invention are as follows：
1. the product obtained by the inventive method is the active porous boron nitride nanosheet with hexagonal structure, such as Fig. 1 institutes
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 homogeneous, thickness is only 2~6nm, and its edge has abundant fault of construction position；Fig. 4 is more for activity
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 specific surface area high；It is excellent that Fig. 5 and Fig. 6 show that active porous boron nitride nanosheet has to the pollutant in the aqueous solution
Adsorption capacity and regeneration recycling ability.
2. present invention gained boron nitride nanosheet has the properties such as peculiar light, electricity, magnetic, heat and absorption, particularly high
The characteristics such as specific surface area, abundant fault of construction and B-N bond polarities, become excellent water purification material, this activity
There is porous boron nitride nanometer sheet the adsorption capacity at normal temperatures to toxic heavy metal contamination to be up to every gram of 0.42 gram of absorption, weight
Again using adsorption capacity after 10 times more than 70%, overcome conventional activated carbon can not reusable defect, in water process and net
Change field is widely used.
3. the raw material that the present invention is used is boric acid, belongs to industrialization product, and price is relatively inexpensive to be easy to get, and life can be greatly reduced
Produce cost.
4. synthesis used in the present invention needs compared with low temperature, technical process simply, to be suitable to scale industrial production.
Brief description of the drawings
The present invention is further described with specific implementation below in conjunction with the accompanying drawings.
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 normal 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
The present invention is further described below by specific embodiment, but embodiment will not be constituted to limit of the invention
System.
Embodiment 1：
(1) weigh and 0.1 gram of melamine is heated in the case where throughput is 50 milliliters/nitrogen atmosphere protection per minute
300 DEG C, 0.5 hour is incubated, insulation stops being passed through and cooling the temperature to room temperature for gas after terminating, and obtains faint yellow product；(2)
Products therefrom and boric acid with mol ratio be 1:Mixture obtained by 0.01 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 in reaction cavity and is continued to be heated to 600
DEG C, 0.5 hour is incubated, insulation stops being passed through and cooling the temperature to room temperature for gas after terminating, resulting white product is activity
Porous boron nitride nanometer sheet, its specific surface area is up to 817m2/ g, a diameter of 50~300nm, 2~6nm of thickness, and to the aqueous solution
In organic and inorganic pollution there is excellent adsorption capacity.
Tested through X-ray diffraction, the wide-angle diffraction peak in Fig. 1 shows product for hexagonal boron nitride, and diffraction maximum is very clear
It is clear；Scanned electron microscope picture (Fig. 2) finds out that product is laminated structure；Find out product through transmission electron microscope figure (Fig. 3)
It is laminated structure；Again through low temperature nitrogen adsorption and desorption thermoisopleth (Fig. 4), it is 817 squares every gram that can calculate its specific surface area
Rice, pore volume is 0.57 cubic metre every gram；What the above collection of illustrative plates explanation present invention was obtained is with a large amount of activated adoption position, Gao Bibiao
Area and macropore volume boron nitride ceramic material.Finally, we are surveyed the water process and detergent power to active boron nitride
Examination.Fig. 5 shows that it reaches every gram to the adsorption capacity of aqueous solution Poisoning heavy metal contaminants and adsorbs 0.42 gram in normal temperature；Fig. 6
Show that active boron nitride is reused 10 times, adsorption capacity keeps more than 70% adsorption capacity, and this illustrates active nitride
Boron is easy to recycle.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 consumption of step (1) melamine or cyanamid dimerization in embodiment 1 is changed to 1g, 10g, other every behaviour respectively
Make same as Example 1, obtain 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
Make same as Example 1, obtain product with embodiment 1.
Embodiment 10,11：
The heating-up 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 mol 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-up temperature is changed to 400,500 DEG C respectively when step (2) gas in embodiment 1 not passed through ammonium fluoroborate solution,
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-up temperature is changed to 800,1000 DEG C respectively when step (2) gas in embodiment 1 is passed through into ammonium fluoroborate solution, its
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 (9)
1. the synthetic method of a kind of active porous boron nitride nanosheet for water process, it is characterised in that comprise the following steps：
Step one：0.1~10 gram of melamine or cdicynanmide are heated to 300~600 DEG C, insulation 0.5 under protective atmosphere
~4 hours, insulation stopped being passed through and cooling the temperature to room temperature for gas after terminating, and obtains faint yellow product；
Step 2：By products therefrom mix with boric acid obtained by mixture be 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 again in reaction cavity continue to be heated to 600~
1000 DEG C, 0.5~4 hour is incubated, insulation stops being passed through and cooling the temperature to room temperature for gas, resulting white product after terminating
It is active porous boron nitride nanosheet, its specific surface area is up to 817m2/ g, a diameter of 50~300nm, 2~6nm of thickness, and it is right
Pollutant in the aqueous solution has excellent adsorption capacity.
2. the method for preparing active porous boron nitride nanosheet according to claim 1, it is characterised in that：Described protection
Atmosphere is neon, Krypton, argon gas or nitrogen.
3. the method for preparing active porous boron nitride nanosheet according to claim 1, it is characterised in that：Described protection
Atmosphere be neon, Krypton, argon gas or nitrogen when, gas flow rate be 50-500 milliliters/it is per minute.
4. the method for preparing active porous boron nitride nanosheet according to claim 1, it is characterised in that：Described mixing
The faint yellow product and the mol ratio of boric acid that thing is included are 1:0.01~1:100.
5. the method for preparing active porous boron nitride nanosheet according to claim 1, it is characterised in that：Described fluorine boron
The aqueous solution of sour ammonium is 0.01~10mmol/L.
6. the method for preparing active porous boron nitride nanosheet according to claim 1, it is characterised in that：Described is passed through
Ammonium fluoroborate aqueous solution protective atmosphere gas flow rate be 100~300 milliliters/it is per minute.
7. the boron nitride nanosheet being fabricated to according to claim 1 preparation method, it is characterised in that：Boron nitride nanosheet is six sides
It is structure, active porous.
8. the boron nitride nanosheet being fabricated to according to claim 7 preparation method, it is characterised in that：The boron nitride nanosheet tool
There are peculiar light, electricity, magnetic, heat and adsorption property.
9. the boron nitride nanosheet being fabricated to according to claim 7 preparation method, it is characterised in that：The boron nitride nanosheet tool
There are specific surface area high, abundant fault of construction and B-N bond polarity characteristics.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107265417A (en) * | 2017-07-24 | 2017-10-20 | 江苏大学 | A kind of boron defect boron nitride nanosheet and its production and use |
| CN107694595A (en) * | 2017-10-11 | 2018-02-16 | 中国地质大学（武汉） | A kind of preparation method of oxygen doping boron nitride catalyst carrier |
| CN107774292A (en) * | 2017-10-11 | 2018-03-09 | 中国地质大学（武汉） | A kind of preparation method of oxygen doping boron nitride catalyst carrier carried metal |
| 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 |
| CN112316567A (en) * | 2020-10-19 | 2021-02-05 | 江苏大学 | Nanofiber filter membrane and preparation method and device thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107265417A (en) * | 2017-07-24 | 2017-10-20 | 江苏大学 | A kind of boron defect boron nitride nanosheet and its production and use |
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| 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 |
| CN112316567A (en) * | 2020-10-19 | 2021-02-05 | 江苏大学 | Nanofiber filter membrane and preparation method and device thereof |
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| CN106744736B (en) | 2018-11-27 |
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