CN109399587A - Preparation method of mesoporous carbonitride and products thereof and application - Google Patents
Preparation method of mesoporous carbonitride and products thereof and application Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000006185 dispersion Substances 0.000 claims abstract description 27
- 239000012530 fluid Substances 0.000 claims abstract description 25
- 239000011787 zinc oxide Substances 0.000 claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 13
- 229920000877 Melamine resin Polymers 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 10
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 claims description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 claims description 4
- 230000001699 photocatalysis Effects 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 3
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 3
- -1 single Tryfac 5573 Chemical compound 0.000 claims description 3
- MJJJJEUEZVGFLW-UHFFFAOYSA-N 2-dodecyl-2-sulfobutanedioic acid Chemical compound CCCCCCCCCCCCC(S(O)(=O)=O)(C(O)=O)CC(O)=O MJJJJEUEZVGFLW-UHFFFAOYSA-N 0.000 claims description 2
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 2
- 244000060011 Cocos nucifera Species 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- GWTCIAGIKURVBJ-UHFFFAOYSA-L dipotassium;dodecyl phosphate Chemical compound [K+].[K+].CCCCCCCCCCCCOP([O-])([O-])=O GWTCIAGIKURVBJ-UHFFFAOYSA-L 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 239000008240 homogeneous mixture Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 2
- OOCCDEMITAIZTP-QPJJXVBHSA-N (E)-cinnamyl alcohol Chemical compound OC\C=C\C1=CC=CC=C1 OOCCDEMITAIZTP-QPJJXVBHSA-N 0.000 claims 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims 1
- OOCCDEMITAIZTP-UHFFFAOYSA-N allylic benzylic alcohol Natural products OCC=CC1=CC=CC=C1 OOCCDEMITAIZTP-UHFFFAOYSA-N 0.000 claims 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 8
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 238000001354 calcination Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002052 molecular layer Substances 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- TYTGWHZODQKWEF-UHFFFAOYSA-N 1-o-dodecyl 4-o-sulfo butanedioate Chemical compound CCCCCCCCCCCCOC(=O)CCC(=O)OS(O)(=O)=O TYTGWHZODQKWEF-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 244000147568 Laurus nobilis Species 0.000 description 1
- 235000017858 Laurus nobilis Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 235000005212 Terminalia tomentosa Nutrition 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 229940071180 lauryl sulfosuccinate Drugs 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The present invention relates to preparation methods of a kind of mesoporous carbonitride and products thereof and application, using nano zine oxide as presoma, nano zine oxide is first prepared into the nano dispersion fluid of monodispersity by the way of grinding distribution, then it is roasted after carbon nitride precursor being sufficiently mixed with zinc oxide fluid dispersion, then product of roasting is sufficiently stirred in hydrochloric acid, mesoporous carbonitride is finally prepared.Using the method for the present invention prepare mesoporous carbonitride, aperture is small and size is uniform, have it is easy to operate, difficulty is lower, and not will use the big hydrofluoric acid of risk, and be suitble to large-scale promotion.
Description
Technical field
The invention belongs to field of nano material preparation, and in particular to a kind of preparation method of mesoporous carbonitride and products thereof and
Using.
Background technique
Carbonitride is a kind of Huang by the way that carbon elements and nitrogen material abundant are carried out with certain roasting synthesis
Color nanocrystal.Its crystal structure is similar to graphite-structure.Because nitridation carbon-based group only exists in a molecular layer, only
Faint Van der Waals force can will connect between different molecular layer.It is widely known that light can produce in this material
Raw electron-hole pair.Therefore, carbonitride has excellent photocatalysis performance.It can convert height for the solar energy of low-density
The chemical energy of density or directly degradation and mineralising organic pollutant, have in terms of the problems such as solving energy shortage and environmental pollution
Important application prospect.
Mesoporous carbonitride is since there are the apertures of a large amount of 2-50nm on carbonitride thin slice, so that it is with high ratio
The features such as surface area, regular cellular structure, narrow pore-size distribution；For purer carbonitride, have excellent
The absorption of macromolecular, separation characteristic, can play a greater role in catalysis reaction, higher photocatalysis efficiency is provided.And
And this orderly duct is alternatively arranged as " microreactor ", improves catalytic performance.The preparation method of current mesoporous carbonitride is universal
Template is used as using nano silicon oxide, mesoporous carbonitride is prepared by hard template method, Jie can be prepared in this way
Hole carbonitride.But this method has some disadvantages, the method first is first to mix silica with carbon nitride precursor, is then roasted
Burning obtains carbonitride, then mixes obtained powder with hydrofluoric acid, and dissolve silica can be obtained mesoporous nitrogen later
Change carbon.It is well known that hydrofluoric acid has extremely strong corrosive acid as a kind of, it can consumingly corrode metal, glass and siliceous
Object, such as sucking steam or contacting skin will cause burning of being difficult to cure, and be that a kind of height endangers poisonous substance；On the other hand,
It is known that agglomeration easily occurs for nano material, by mixing silica with carbonitride since its surface can be excessive
It is redissolved the mode fallen and prepares mesoporous carbonitride, since nano silicon oxide can reunite, this will result in final synthesising mesoporous
The pore size of carbonitride is different, it could even be possible to having the aperture of several hundred nanosizeds；Therefore, using conventional method preparation
Mesoporous carbonitride haves the shortcomings that aperture is different, and preparation process has the harm to people and environment, and preparation difficulty is higher,
It is only applicable to laboratory preparation.
Summary of the invention
To prepare mesoporous carbonitride pore size inhomogenous for existing, prepares the higher disadvantage of difficulty, the object of the invention exists
In providing a kind of preparation method of mesoporous carbonitride.
Another object of the present invention is: providing a kind of mesoporous nitridation carbon products of above method preparation.
Another object of the present invention is to: a kind of application of the said goods is provided.
The object of the invention is realized by following proposal: one kind is by nano zinc oxide fluid dispersion as presoma, using salt
Acid dissolution falls the mode of template to prepare the preparation method of mesoporous carbonitride, includes the following steps:
1) prepared by nano zinc oxide fluid dispersion: being in mass ratio 1:(0.05~0.6): (1~100) accurately weighs nano oxidized
Dispersing agent is added in deionized water first, after stirring to dissolve, adds nano oxygen by zinc, dispersing agent and deionized water
Change zinc, is uniformly mixed, then grinds, obtain the nano zinc oxide fluid dispersion that monodisperse is not reunited；
2) melamine, the matter of the nano zinc oxide fluid dispersion and melamine are added in above-mentioned nano zinc oxide fluid dispersion
Amount is than being 1:(0.01~0.5), 3h is then stirred at 60~100 DEG C, obtains melamine after the evaporation of above-mentioned solution is done
With nano zine oxide homogeneous mixture；It will be put into crucible after above-mentioned solid abrasive, with 2.5 DEG C/min of heating rate liter
Temperature is roasted to 400~600 DEG C, is kept the temperature 1~5 hour, is obtained brownish black powder；
3) the brownish black powder for obtaining above-mentioned roasting takes out 0.5~1g, and 1~3mol/L of 100~300ml is added after grinding
Hydrochloric acid in stir 2~6 hours, be then centrifuged for and cleaned using deionized water and ethyl alcohol, it is final it is dry after obtain
Mesoporous carbonitride.
Nano zine oxide, as presoma, is first prepared by the present invention using nano zine oxide by the way of grinding distribution
The nano dispersion fluid of monodispersity roasts, so after being then sufficiently mixed carbon nitride precursor with zinc oxide fluid dispersion
Product of roasting is sufficiently stirred in hydrochloric acid afterwards, mesoporous carbonitride is finally prepared.
In step 1), milling time is 0.5~10 hour.
The dispersing agent is lauryl sodium sulfate, cetyl trimethylammonium bromide, lauryl sulfosuccinate list
Ester disodium, fatty alcohol polyoxyethylene ether, sulfosuccinic acid monoesters disodium, Coconut Fatty Acid Monoethanolamide sulfosuccinic acid monoesters two
Sodium, single Tryfac 5573, Monododecylphosphate potassium, laurel alcohol ether phosphate potassium, nonylphenol polyoxyethylene ether, polyethylene
One of pyrrolidones or combinations thereof.
The present invention also provides a kind of mesoporous carbonitrides, are prepared according to any of the above-described the method.
Also, the present invention also provides a kind of mesoporous carbonitride in formaldehyde photocatalysis as the application of catalyst.
The method of the present invention preparation mesoporous carbonitride, aperture is small and size is uniform, have it is easy to operate, difficulty is lower,
And it not will use the big hydrofluoric acid of risk, and be suitble to large-scale promotion.
Detailed description of the invention
The TEM photo of the mesoporous carbonitride of Fig. 1.
Specific embodiment
The present invention is further illustrated below by embodiment, is not intended to limit the scope of the invention.
Embodiment 1
A kind of preparation method of mesoporous carbonitride falls mould as presoma, using dissolving with hydrochloric acid using nano zinc oxide fluid dispersion
The mode of plate prepares the preparation method of mesoporous carbonitride, as follows:
1) prepared by nano zinc oxide fluid dispersion: for 1:0.3:50 precise nano zine oxide, dispersing agent and going in mass ratio
Ionized water, dispersing agent are lauryl sodium sulfate, and first dispersing agent is dissolved in deionized water, nano zine oxide is then added, is stirred
Sand mill is added after mixing uniformly, (wherein milling time is 2 hours) is ground after adjusting technological parameter and obtains monodispersed receive
Rice zinc oxide fluid dispersion.
It 2) is in mass ratio that 1:0.3 is mixed with appropriate melamine by nano zinc oxide fluid dispersion, then 80 DEG C of stirrings are steamed
It is dry, obtained solid matter is put into crucible and is roasted, wherein heating rate is 2.5 DEG C/min, final calcination temperature
For 500 DEG C and calcining time is 3 hours, obtains brownish black powder；
3) it finally, taking out 0.5g brownish black powder, is added in hydrochloric acid after grinding, wherein hydrochloric acid volume is 200ml, and concentration is
1mol/L is stirred 2 hours, be centrifuged and wash it is dry after finally obtain mesoporous carbonitride, as the TEM of the mesoporous carbonitride of Fig. 1 shines
Shown in piece.
Embodiment 2
A kind of preparation method of mesoporous carbonitride, it is approximate with embodiment 1, as follows:
1) nano zinc oxide fluid dispersion prepare: mass ratio be 1:0.5:70 precise nano zine oxide, dispersing agent and go from
Sub- water, dispersing agent are cetyl trimethylammonium bromide, and first dispersing agent is dissolved in deionized water, are then added nano oxidized
Sand mill is added after stirring evenly in zinc, adjusts after technological parameter grinding 3 hours, obtains mono-dispersed nano zinc oxide point
Dispersion liquid.
It 2) is in mass ratio that 1:0.2 is mixed with appropriate melamine by nano zinc oxide fluid dispersion, then 90 DEG C of high temperature stir
It mixes and is evaporated, obtained solid matter is put into crucible and is roasted, wherein heating rate is 2.5 DEG C/min, final to roast
Temperature is 550 DEG C, and calcining time is 4 hours, obtains brownish black powder；
3) 1g brownish black powder is taken out, it is 150ml that volume is added after grinding, and concentration is to stir 4 hours in 2mol/L hydrochloric acid, from
The heart and wash it is dry after finally obtain mesoporous carbonitride.
Embodiment 3
A kind of preparation method of mesoporous carbonitride, it is approximate with embodiment 1, as follows:
1) prepared by nano zinc oxide fluid dispersion: for 1:0.2:80 precise nano zine oxide, dispersing agent and going in mass ratio
Ionized water, dispersing agent are nonylphenol polyoxyethylene ether, and first dispersing agent is dissolved in deionized water, nano zine oxide is then added,
Sand mill is added after stirring evenly, adjusts after technological parameter grinding 1 hour, obtains the dispersion of mono-dispersed nano zinc oxide
Liquid.
It 2) is in mass ratio that 1:0.4 is mixed with appropriate melamine by nano zinc oxide fluid dispersion, then 85 DEG C of high temperature stir
It mixes and is evaporated, obtained solid matter is put into crucible and is roasted, wherein heating rate is 2.5 DEG C/min, final to roast
Temperature is 600 DEG C, and calcining time is 2 hours, obtains brownish black powder；
3) 0.5g brownish black powder is taken out, it is 300ml that volume is added after grinding, and concentration is that stirring 5 is small in the hydrochloric acid of 3mol/L
When, be centrifuged and wash it is dry after finally obtain mesoporous carbonitride.
Embodiment 4
A kind of preparation method of mesoporous carbonitride, it is approximate with embodiment 1, as follows:
1) prepared by nano zinc oxide fluid dispersion: for 1:0.3:40 precise nano zine oxide, dispersing agent and going in mass ratio
Ionized water, dispersing agent are the combination of lauryl sulfosuccinic acid monoester disodium and polyvinylpyrrolidone, are first dissolved in dispersing agent
In deionized water, nano zine oxide is then added, sand mill is added after stirring evenly, grinding 3 is small after adjusting technological parameter
When obtain mono-dispersed nano zinc oxide fluid dispersion.
It 2) is in mass ratio that 1:0.2 is mixed with appropriate melamine by nano zinc oxide fluid dispersion, then 100 DEG C of high temperature stir
It mixes and is evaporated, obtained solid matter is put into crucible and is roasted, wherein heating rate is 2.5 DEG C/min, final to roast
Temperature is 600 DEG C, and calcining time is 1 hour, obtains brownish black powder；
3) 1g brownish black powder is taken out, it is 150ml that volume is added after grinding, and concentration is to stir 2.5 hours in 3mol/L hydrochloric acid,
It is centrifuged and washs drying and finally obtain mesoporous carbonitride later.
Claims (5)
1. a kind of preparation method of mesoporous carbonitride, which is characterized in that using nano zinc oxide fluid dispersion as presoma, use
Dissolving with hydrochloric acid falls the mode of template to prepare the preparation method of mesoporous carbonitride, includes the following steps:
1) prepared by nano zinc oxide fluid dispersion: being in mass ratio 1:(0.05~0.6): (1~100) accurately weighs nano oxidized
Dispersing agent is added in deionized water first, after stirring to dissolve, adds nano oxygen by zinc, dispersing agent and deionized water
Change zinc, is uniformly mixed, then grinds, obtain the nano zinc oxide fluid dispersion that monodisperse is not reunited；
2) melamine, the matter of the nano zinc oxide fluid dispersion and melamine are added in above-mentioned nano zinc oxide fluid dispersion
Amount is than being 1:(0.01~0.5), 3h is then stirred at 60~100 DEG C, obtains melamine after the evaporation of above-mentioned solution is done
With nano zine oxide homogeneous mixture；It will be put into crucible after above-mentioned solid abrasive, with 2.5 DEG C/min of heating rate liter
Temperature is roasted to 400~600 DEG C, is kept the temperature 1~5 hour, is obtained brownish black powder；
3) the brownish black powder for obtaining above-mentioned roasting takes out 0.5~1g, and 1~3mol/L of 100~300ml is added after grinding
Hydrochloric acid in stir 2~6 hours, be then centrifuged for and cleaned using deionized water and ethyl alcohol, it is final it is dry after obtain
Mesoporous carbonitride.
2. the preparation method of mesoporous carbonitride according to claim 1, it is characterised in that in step 1), milling time 0.5
~10 hours.
3. the preparation method of mesoporous carbonitride according to claim 1, it is characterised in that dispersing agent be lauryl sodium sulfate,
Cetyl trimethylammonium bromide, lauryl sulfosuccinic acid monoester disodium, fatty alcohol polyoxyethylene ether, sulfosuccinic acid monoesters
Disodium, Coconut Fatty Acid Monoethanolamide sulfosuccinic acid monoesters disodium, single Tryfac 5573, Monododecylphosphate potassium, the moon
One of cinnamic alcohol ether phosphate potassium, nonylphenol polyoxyethylene ether, polyvinylpyrrolidone or combinations thereof.
4. a kind of mesoporous carbonitride, it is characterised in that -3 any the methods are prepared according to claim 1.
5. a kind of carbonitride mesoporous according to claim 4 is in formaldehyde photocatalysis as the application of catalyst.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109046428A (en) * | 2018-08-22 | 2018-12-21 | 广州大学 | A kind of mesoporous class graphite phase carbon nitride and its preparation method and application |
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