CN108275663A - A kind of method that molten mass hydrogen bubble template prepares the mesoporous boron nitride of uniform bore - Google Patents
A kind of method that molten mass hydrogen bubble template prepares the mesoporous boron nitride of uniform bore Download PDFInfo
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- 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
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Abstract
A kind of method that molten mass hydrogen bubble template prepares the mesoporous boron nitride of uniform bore is to mix nitrogen source, boron source and adjuvant, keeps the temperature 0.1 2 hours at 220 DEG C~500 DEG C, then keeps the temperature 1 20 minutes at 700 DEG C, pore-creating obtains presoma;It in nitrogen, nitrogen and hydrogen mixture or nitrogen ammonia gaseous mixture, is pyrolyzed at 900~1300 DEG C, obtains crude product, washed, filter in hydrochloric acid, deionized water and ethyl alcohol clean to obtain nitride porous boron powder.It is 150~600m that the present invention, which has product specific surface area,2/ g, aperture most probable size are 18 25 nm, and technology path is simple, are suitble to a large amount of the advantages of preparing.
Description
Technical field
The invention belongs to nano bubble templates in the technology of preparing of porous boron nitride more particularly to a kind of molten mass to prepare
Even pore-size distribution, the method for high specific surface area and mesoporous boron nitride.
Background technology
Porous boron nitride has excellent chemical stability, thermal stability and excellent antioxygenic property.Also have simultaneously
The characteristics of low-density, high porosity, bigger serface, in sewage disposal, gas absorption (purification), hydrogen storage, catalyst carrier
And it is nonmetal catalyzed etc. have huge application value, be one of the focus of recent domestic researcher.But
Staple commodities hexagonal boron nitride is mainly micron order product at present, and specific surface area is less than 20 ㎡/g, related bigger serface more
Porous boron nitride, which is not much, to be seen.
Recent years, the synthesis in relation to nitride porous boron material, which is reported on depth and range, huge progress.This
The main preparation method of a little nitride porous boron materials has following several.(1)It is pyrolyzed ammonia in the case where nitrogen, argon gas etc. protect gas atmosphere
The organo-boranes such as borine, such as Wang Xuebin have used " chemical blowing process ", have obtained porous boron nitride(Adv. Mater. 23
(2011) 4072-4076);(2)Micropore boron nitride is obtained as the two-stage method of representative then first synthesize boric acid using Tang at spring seminar
Melamine presoma is then pyrolyzed;(3)Sofia Marchesini et al. forging under an inert atmosphere by urea, boric acid
It is also a kind of typical white graphite alkene synthetic method to burn, and represents the preparation method of another kind of multi-stage porous boron nitride.(Microp
Mesopor Mater 243 (2017) 154-163).Although multilevel hole material has the advantage of mass transfer etc., it is unfavorable for
The specific applications such as the Selective Separation of gas/liquid.
Similar to series materials such as CMK, SBA of mesoporous carbon and mesoporous silicon, before the application of the mesoporous boron nitride of regular texture
Scape is wide, but can't be obtained at present by hydro-thermal reaction, liquid crystal soft template method, makes little progress.(4)Utilize other single apertures
Mould material carve that obtain corresponding porous boron nitride be then another kind of common preparation strategy again, such as using mesoporous carbon, titanium dioxide
Silicon hard template(CMK-3、SBA-15), the former can obtain the boron nitride of corresponding pore structure by carbon Hot swapping, and the latter is nitrogenizing
Boron carve again after by chemical attack means remove SiO2To obtain corresponding mesoporous boron nitride nanometer material (J. Mater.
Chem. 15 (2005) 1917-1923)。
In conclusion the relatively regular mesoporous boron nitride in hole also has many deficiencies in terms of preparation at present.Such as chemical blowing
Raw material used in method is expensive ammonia borine, and the specific surface area of the porous boron nitride of generation is less than 150m2/g;And template
Conventional template used in method needs that template is pre-machined, then removes removing template, complex process, also has template residual.These porous nitrogen
Change the preparation route of boron is influenced by organic boron nitrogen source, hard template, it is difficult to using staple commodities boron source, nitrogen source, in larger ruler
Degree obtains the mesoporous boron nitride material of rule(As more than 10 gram-grades)Aspect has difficulties, and constrains mesoporous boron nitride and is deposited in hydrogen energy source
Storage, the research in the environment such as carbon dioxide adsorption and oil spilling, waste water drop evil field and explorative research.
Invention content
The purpose of the present invention is overcome the deficiencies of the prior art and provide it is a kind of efficiently, can prepare with scale aperture it is opposite
The method of the mesoporous boron nitride of rule.
Using most conventional large chemical boron source, nitrogen source, core is to combine fuse salt technology and bubble mould the present invention
Pore-creating is obtained presoma and high-temperature calcination nitrogenizes two-phase seperation, has the characteristics that easy, efficient, low cost by plate technique.
It is realized particular by following technical scheme:
(1)First segment:Low temperature calcination pore-creating obtains presoma, and urea is in molten condition in calcination process, and boric acid and urea then can shapes
At (BO)x(BN)yPresoma, while boron source, nitrogen source are slowly decomposed, and in-situ preparation nano bubble acts as template, works as aerogenesis
Raw material exhausts, then obtains presoma porous structure, and the calcining of this stage is protected without specific gas.
Particularly by nitrogen source, boron source and adjuvant in mass ratio 3~8: 1:0.001~0.05 mixing, 220 DEG C~
500 DEG C keep the temperature 0.1-2 hours, then keep the temperature 1-20 minutes at 700 DEG C, pore-creating obtains presoma;
Nitrogen source is urea or urea and melamine or the mixture of ammonium carbonate, and wherein melamine or ammonium carbonate is in mixture
Content be less than 10wt.%.
Boron source is the mixture of boric acid or boric acid and boron oxide, and wherein the weight ratio of boric acid and boron oxide is 1:8 -10.
The purpose that a small amount of adjuvant is added is to regulate and control the viscosity of melt, influences the size of nano bubble, adjusts product table
Face chemical environment, crystallization degree and specific surface area, adjuvant are iron, cobalt, nickel, the nitrate of lanthanum element, chlorate and carbon
One kind in sour sodium, borax.
(2)Second section calcining presoma is pyrolyzed to obtain crude product:
In nitrogen, nitrogen and hydrogen mixture or nitrogen ammonia gaseous mixture, in 900~1300 DEG C of Means of Pyrolyzed Precursor, crude product is obtained, wherein
Nitrogen and hydrogen mixture is the nitrogen and hydrogen mixture that density of hydrogen is 2~5wt.%, and nitrogen ammonia gaseous mixture is the nitrogen ammonia of 2~20wt% of ammonia concentration
Gaseous mixture.
(3) crude product purifies:
After crude product washs in the hydrochloric acid of 0.1~3 mol/L, product is filtered, deionized water and ethyl alcohol is used in combination to clean to obtain
Nitride porous boron powder, pickling temperature is between 20 DEG C~60 DEG C.
The advantages of method of the synthesising mesoporous boron nitride of the present invention, is:
1. used reagent is cheap and easy to get, byproducts residual is few and easy purification;
2. technology path used in is simple, technical difficulty is small, is suitble to a large amount of prepare;
3. products therefrom specific surface area is 150~600m2/ g is adjustable;
4. the aperture most probable size of products therefrom is 18-25 nm.
Description of the drawings
Fig. 1 is the X-ray diffraction spectra that product is prepared using the embodiment of the present invention 1(XRD).
Fig. 2 is the transmission electron microscope that product is prepared using the embodiment of the present invention 1(TEM).
Fig. 3 is to prepare product using the embodiment of the present invention 1 to adsorb de-/attached equal curves.
Fig. 4 is to prepare product graph of pore diameter distribution using the embodiment of the present invention 1.
Fig. 5 is to use the large-scale transmission electron microscope photo of 3 products therefrom of the embodiment of the present invention.
Fig. 6 is the transmission electron microscope photo using 4 products therefrom of the embodiment of the present invention.
Fig. 7 is the transmission electron microscope photo using 5 products therefrom of the embodiment of the present invention.
Fig. 8 is the transmission electron microscope photo using 5 products therefrom of the embodiment of the present invention.
Specific implementation mode
Embodiment 1:
100 grams of boric acid, 400 grams of urea and the uniformly mixing of 1 gram of ferric nitrate are taken, is heated up with the heating rate of 10 DEG C/min in electric furnace
Presoma is obtained to 300 DEG C of heat preservations within 20 minutes, will then be cured 1 minute at 700 DEG C.Presoma is put into graphite boat nitrogen hydrogen to mix
Gas(5wt% H2/N2)Under atmosphere protection, 1000 DEG C are warming up to the heating rate of 10 DEG C/min, heat preservation obtains crude product in 2 hours.
Then crude product is placed in the hydrochloric acid of 0.5 mol/L of 500 ml, is stirred 2 hours at 60 DEG C.Product is filtered, and is spent
Ionized water and ethyl alcohol cleaning, it is 12 hours dry.Obtain 40 grams of products.
Fig. 1 shows that products therefrom is pure boron nitride, and Fig. 2 is the transmission electron microscope photo of products therefrom, it is seen that the tool of product
There is porous character and aperture is relatively uniform, average-size is 18 nm or so, and Fig. 3 is nitrogen of the mesoporous boron nitride of gained in 77K
Isothermal adsorption desorption curve, P/P0=0.45 has the typical jumping of meso-hole structure, and the ratio table of sample is obtained using BET equation calculations
Area is 281m2/g.And it is as shown in Figure 4 through BJH methods to obtain pore-size distribution with desorption branch.Most may be used in conjunction with visible its of Fig. 2 and Fig. 4
Several apertures are in 18 nm, and pore size is mainly between 10~40 nm.
Embodiment 2:
The uniformly mixing of 2 grams of 100 grams of boric acid, 270 grams of urea, 30 grams of ammonium carbonate and cobalt nitrate is taken, with 10 DEG C/min's in electric furnace
Heating rate is warming up to 220 DEG C of heat preservations and obtains presoma in 2 hours, will then cure 10 minutes at 700 DEG C.Presoma is put into stone
Black boat nitrogen hydrogen mixes gas(2 wt. %H2/N2)Under atmosphere protection, 1000 DEG C are warming up to the heating rate of 10 DEG C/min, heat preservation 2 is small
When obtain crude product.Then crude product is placed in the hydrochloric acid of 3 mol/L of 500 ml and is stirred 4 hours at 40 DEG C.By product
Filtering is used in combination deionized water and ethyl alcohol to clean, dry, and the specific surface area for measuring sample is 220 m2/ g, most probable pore size 25
Nm, pore size is mainly between 8~50 nm.
Embodiment 3:
The uniformly mixing of 10 grams of boric acid, 90 grams of boron oxide powder, 800 grams of urea, 5 grams of ferric nitrate is taken, with 10 DEG C/min in electric furnace
Heating rate be warming up to 500 DEG C keep the temperature 6 minutes, will then cure 20 minutes at 700 DEG C.Presoma is put into graphite boat nitrogen hydrogen
Mixed gas(20wt.% NH3/N2)Under atmosphere protection, 900 DEG C are warming up to the heating rate of 10 DEG C/min, heat preservation obtains thick for 3 hours
Product.Then crude product is placed in the hydrochloric acid of 1 mol/L of 500 ml and is stirred 4 hours at 50 DEG C.Product is filtered, and
It is cleaned with deionized water and ethyl alcohol, 12 hours dry, products therefrom specific surface area is 150 m2/ g, transmission electron microscope picture are shown in Fig. 5.Most
Can 23 nm of several apertures, pore size is mainly between 8~50 nm.
Embodiment 4:
100 grams of boric acid, 400 grams of urea, 0.1 gram of sodium carbonate is taken uniformly to mix, with the heating rate liter of 10 DEG C/min in electric furnace
Temperature obtains presoma in 20 minutes to 300 DEG C of heat preservations, will then cure 1 minute at 700 DEG C.Presoma is put into graphite boat nitrogen gas
Under atmosphere protection, 900 DEG C are warming up to the heating rate of 10 DEG C/min, heat preservation obtains crude product in 30 minutes.Then crude product is used
It is stirred 10 minutes at 20 DEG C in the hydrochloric acid of 0.1 mol/L.Product is filtered, deionized water and ethyl alcohol is used in combination to clean, dry, institute
It is 600 m to obtain product specific surface area2/ g, most probable pore size are 23 nm, and pore size is mainly between 8~50nm transmission electron microscope pictures
See Fig. 6.
Embodiment 5:
The uniformly mixing of 0.5 gram of 100 grams of boric acid, 395 grams of urea, 5 grams of melamine and nickel nitrate is taken, with 10 DEG C/min in electric furnace
Heating rate be warming up to 300 DEG C of heat preservations and obtain presoma in 20 minutes, then cure at 700 DEG C.Presoma is put into graphite boat
10 wt. %NH3-N2Nitrogen hydrogen mixes under gas shielded, is warming up to 950 DEG C with the heating rate of 10 DEG C/min, heat preservation is slightly produced for 1 hour
Product.Then crude product is placed in the hydrochloric acid of 2 mol/L and is stirred 2 hours at 60 DEG C.Product is filtered, be used in combination deionized water and
Ethyl alcohol cleans, 12 hours dry, and the specific surface area for measuring sample is 300 m2/ g, most probable pore size are 23 nm, pore size master
To see Fig. 7 between 10~45nm, corresponding transmission electron microscope picture.
Embodiment 6:
100 grams of boric acid, 400 grams of urea, 0.1 gram of iron chloride is taken uniformly to mix, with the heating rate liter of 10 DEG C/min in electric furnace
Temperature obtains presoma in 20 minutes to 300 DEG C of heat preservations, will then cure 1 minute at 700 DEG C.Presoma is put into graphite boat N2Atmosphere
Under protection, 1300 DEG C are warming up to the heating rate of 10 DEG C/min, 20 minutes is kept the temperature, obtains crude product.Then crude product is existed
With the HCl treatment of 2 mol/L 10 minutes at 40 DEG C.Product is filtered, deionized water and ethyl alcohol is used in combination to clean, dry, gained production
Object specific surface area is 230 m2/ g, most probable pore size are 22 nm, and pore size is mainly shown between the corresponding transmission electron microscope pictures of 8~45 nm
Fig. 8.
Claims (8)
1. a kind of method that molten mass hydrogen bubble template prepares the mesoporous boron nitride of uniform bore, it is characterised in that include the following steps:
(1) by nitrogen source, boron source and adjuvant in mass ratio 3~8: 1:0.001~0.05 mixing is kept the temperature at 220 DEG C~500 DEG C
0.1-2 hours, 1-20 minutes then are kept the temperature at 700 DEG C, pore-creating obtains presoma;
(2) in nitrogen, nitrogen and hydrogen mixture or nitrogen ammonia gaseous mixture, in 900~1300 DEG C of Means of Pyrolyzed Precursor, crude product is obtained;
(3) after crude product washs in the hydrochloric acid of 0.1~3 mol/L, product is filtered, deionized water and ethyl alcohol is used in combination to clean
Nitride porous boron powder is obtained, pickling temperature is between 20 DEG C~60 DEG C.
2. the method that a kind of molten mass hydrogen bubble template as described in claim 1 prepares the mesoporous boron nitride of uniform bore, feature
It is that nitrogen source is urea or urea and melamine or the mixture of ammonium carbonate.
3. the method that a kind of molten mass hydrogen bubble template as claimed in claim 2 prepares the mesoporous boron nitride of uniform bore, feature
It is that melamine or ammonium carbonate are less than 10wt% in the content of mixture.
4. the method that a kind of molten mass hydrogen bubble template as described in claim 1 prepares the mesoporous boron nitride of uniform bore, feature
It is that boron source is the mixture of boric acid or boric acid and boron oxide.
5. the method that a kind of molten mass hydrogen bubble template as claimed in claim 4 prepares the mesoporous boron nitride of uniform bore, feature
It is in boric acid and boron oxide mixture that the weight ratio of boric acid and boron oxide is 1:8 -10.
6. the method that a kind of molten mass hydrogen bubble template as described in claim 1 prepares the mesoporous boron nitride of uniform bore, feature
It is that adjuvant is the nitrate or chlorate of iron, cobalt, nickel, lanthanum element;Or one kind in sodium carbonate, borax.
7. the method that a kind of molten mass hydrogen bubble template as described in claim 1 prepares the mesoporous boron nitride of uniform bore, feature
It is that nitrogen and hydrogen mixture is the nitrogen and hydrogen mixture that density of hydrogen is 2~5wt.%.
8. the method that a kind of molten mass hydrogen bubble template as described in claim 1 prepares the mesoporous boron nitride of uniform bore, feature
It is that nitrogen ammonia gaseous mixture is the nitrogen ammonia gaseous mixture of 2~20wt% of ammonia concentration.
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Cited By (5)
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CN109174151A (en) * | 2018-08-30 | 2019-01-11 | 湖北第二师范学院 | One kind is for three-dimensional porous boron nitride composite of air cleaning and preparation method thereof |
CN112133888A (en) * | 2020-10-20 | 2020-12-25 | 天津市捷威动力工业有限公司 | Power battery composite positive electrode with excellent performance and preparation method of power battery |
CN112808294A (en) * | 2021-01-05 | 2021-05-18 | 中国石油大学(华东) | Boron nitride/nickel oxide composite material and preparation method and application thereof |
CN113860272A (en) * | 2021-11-25 | 2021-12-31 | 南京大学 | Preparation method of mesoporous-rich hexagonal boron nitride porous material |
JP7349921B2 (en) | 2020-01-24 | 2023-09-25 | デンカ株式会社 | Hexagonal boron nitride sintered body |
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CN106430126A (en) * | 2016-11-01 | 2017-02-22 | 河北正雍新材料科技有限公司 | Preparation method of high-crystallinity hexagonal boron nitride powder |
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CN109174151A (en) * | 2018-08-30 | 2019-01-11 | 湖北第二师范学院 | One kind is for three-dimensional porous boron nitride composite of air cleaning and preparation method thereof |
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CN112808294B (en) * | 2021-01-05 | 2023-02-17 | 中国石油大学(华东) | Boron nitride/nickel oxide composite material and preparation method and application thereof |
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