CN105664835B - A kind of method that organic carboxyl acid auxiliary batch prepares nitride porous carbon material - Google Patents
A kind of method that organic carboxyl acid auxiliary batch prepares nitride porous carbon material Download PDFInfo
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- 150000004767 nitrides Chemical class 0.000 title claims abstract description 56
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 42
- 239000002253 acid Substances 0.000 title claims abstract description 30
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 23
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 8
- 235000006408 oxalic acid Nutrition 0.000 claims description 7
- 239000005711 Benzoic acid Substances 0.000 claims description 6
- 235000010233 benzoic acid Nutrition 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 4
- 229960004889 salicylic acid Drugs 0.000 claims description 4
- 235000011054 acetic acid Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000000356 contaminant Substances 0.000 abstract 1
- 239000003814 drug Substances 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 238000011068 loading method Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 22
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 16
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 9
- 229940043267 rhodamine b Drugs 0.000 description 9
- 239000003125 aqueous solvent Substances 0.000 description 8
- 239000011261 inert gas Substances 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 4
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 241000894007 species Species 0.000 description 3
- -1 wherein Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000005829 trimerization reaction Methods 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- QTERRLQSXYDXAH-UHFFFAOYSA-N [C].N1=C(N)N=C(N)N=C1N Chemical compound [C].N1=C(N)N=C(N)N=C1N QTERRLQSXYDXAH-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
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Abstract
The present invention relates to the method that a kind of organic carboxyl acid auxiliary batch prepares nitride porous carbon material, it is using hydro-thermal calcining two-step method, organic carboxyl acid and melamine are uniformly mixed first, then reaction obtains nitride porous carbon hydro-thermal predecessor under hydrothermal conditions, above-mentioned hydro-thermal predecessor is calcined, obtains nitride porous carbon material.By changing organic carboxyl acid species and experiment condition, it is possible to achieve the controllable preparation of several different structure patterns and specific surface area nitride porous carbon material.This method raw material sources are abundant, cost is cheap, synthesis technique is simple, it is easy to operate, reproducible, can be prepared on a large scale.The nitride porous carbon material of preparation has efficient absorption degradation organic pollution ability, is with a wide range of applications in fields such as environmental contaminants improvement, Photocatalyzed Hydrogen Production, drug loadings.
Description
Technical field
The present invention relates to the method that a kind of organic carboxyl acid auxiliary batch prepares nitride porous carbon material, category material prepares neck
Domain.
Background technology
Graphite phase carbon nitride has caused people widely to pay close attention to as a kind of new metal-free semi-conducting material.Nitridation
Carbon has class graphite laminate structure, and interlayer is combined by Van der Waals force, and height is formed by hydridization by two kinds of elements of nitrogen and carbon in layer
The conjugated system of delocalization, stability are high.Carbonitride has suitable band gap width (about 2.7eV), energy as semi-conducting material
Most of visible ray is enough absorbed, there is stronger oxidation and reducing power again.Meanwhile carbonitride to environmental and biological materials without dirt
Dye, toxicity are low.Therefore, carbonitride is in photocatalytic degradation environmental organic pollutant, photocatalysis hydrogen production, fluorescent material, sterilization material
Etc. be with a wide range of applications.
By improving technology of preparing, pattern is controlled, and then the performance of Effective Regulation carbonitride is the target that people pursue.Mesh
The preparation method of preceding carbonitride is mainly melamine calcination method.This method mainly obtains block materials, can not effectively control shape
Looks, performance of control.Focus of the nitride porous carbon material due to turning into people's research with higher specific surface area.Mainly adopt at present
Prepared with hard template method.Such as CN103861630 A patent documents, to disclose the graphite phase carbon nitride that a kind of combined polymerization is modified hollow
Ball visible light catalyst, it is using cyanamide and organic molecule monomer as predecessor, mesoporous dioxy that it, which nitrogenizes the synthesis of carbon hollow ball,
SiClx ball is template, by thermal polymerization and goes what removing template obtained.Wang et al. (J.Mater.Chem.A, 2015,3,5126-
5131) by the use of calcium carbonate as template, it is prepared for nitride porous carbon material.But hard template method experimental procedure is complicated, removes removing template
Acid solution used easily causes pollution etc. and limits its extensive use.
The content of the invention
For overcome the deficiencies in the prior art, the invention provides a kind of organic carboxyl acid auxiliary batch to prepare nitride porous carbon
The method of material, it is in a kind of addition melamine by organic carboxyl acid, passes through hydro-thermal-calcining two-step method controllable preparation nitride porous
The method of carbon material.
A kind of method that organic carboxyl acid auxiliary batch prepares nitride porous carbon material, its preparation process are as follows：
By melamine and organic carboxyl acid according to mass ratio 1：1-1:Water dissolving, its reclaimed water and organic carboxylic are added after 20 mixings
The mass ratio of acid is 1：1；Or by melamine and organic carboxyl acid according to mass ratio 1：1-1:20 mix dissolving；Will be mixed after dissolving
Compound 80-180 DEG C of heating 1-16h in hydrothermal reaction kettle, obtains nitride porous carbon hydro-thermal predecessor；By nitride porous carbon hydro-thermal
Predecessor, in the lower 450-650 DEG C of calcining 1-6h of nitrogen protection, obtains nitride porous carbon material in tube furnace.
The species of the organic carboxyl acid is acetic acid, oxalic acid, benzoic acid or salicylic acid；
Preferably, the mass ratio of the melamine and organic carboxyl acid is 1:2-1:10；
Preferably, the 100-180 DEG C of heating 5-12h in hydrothermal reaction kettle of the mixture after the dissolving.
Preferably, nitride porous carbon hydro-thermal predecessor 500-600 DEG C of calcining 2- under nitrogen protection in tube furnace
4h。
The present invention using organic carboxyl acid auxiliary and hydro-thermal-calcining two-step mode technique, by change organic carboxyl acid species and
Addition, the controllable preparation nitride porous carbon material of a variety of different-shape structures and specific surface area.Decomposed using organic carboxyl acid
The characteristics of producing gas, form loose structure；Regulate and control the size of pore structure by changing organic carbochain or benzene ring structure.Increase
The specific surface area of carbon nitride material, the mass transfer diffusion process in multiphase photocatalysis reaction is improved, promotes photo-generated carrier
Quick separating, significantly improve the degradation capability to organic pollution.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) figure of ordered laminar nitride porous carbon material in the embodiment of the present invention 1；
From Fig. 1 it can be found that 13.7 ° and 27.6 ° place appearance two significantly belong to graphite phase carbon nitride (100) and
(002) the XRD diffraction maximums of crystal face, it was demonstrated that prepared material is graphite phase carbon nitride material.
Fig. 2 is the stereoscan photograph (SEM) of different-shape nitride porous carbon material in the embodiment of the present invention 1,2,6；
Wherein a figures are acetic acid and the melamine ordered laminar that in aqueous solvent prepared by hydro-thermal and then calcining in embodiment 1
Nitride porous carbon material；B figures are that in anhydrous conditions then hydro-thermal calcines the porous of preparation for acetic acid and melamine in embodiment 2
Carbon nitride material；C figures are benzoic acid and the melamine tubular porous that in aqueous solvent prepared by hydro-thermal and then calcining in embodiment 6
Carbon nitride material；
It is observed that obvious layered porous structure from Fig. 2 a；It is observed that uniform loose structure in Fig. 2 b；
It is observed that obvious tubular porous structure in Fig. 2 c.
Fig. 3 is the N of ordered laminar nitride porous carbon material in the embodiment of the present invention 12Adsorption/desorption curve and simple trimerization
The comparison diagram of carbon nitride material prepared by cyanamide；
Fig. 3 finds out that the adsorption/desorption performance of ordered laminar nitride porous carbon material is substantially better than the nitrogen of melamine preparation
Change carbon material, the specific surface area that BET methods calculate ordered laminar nitride porous carbon material is 138m2/ g, far above simple trimerization
The specific surface area 31m of carbon nitride material prepared by cyanamide2/g。
Fig. 4 is the carbonitride that in the embodiment of the present invention 1 prepared by ordered laminar nitride porous carbon material and simple melamine
Catalytic activity comparison diagram of the material to rhodamine B under sunshine；
Fig. 4 can see, and ordered laminar nitride porous carbon material is much better than pure three to the photocatalytic degradation effect of rhodamine B
Carbon nitride material prepared by poly cyanamid.
Embodiment：
The particular content of the present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
The species of heretofore described organic carboxyl acid can be acetic acid, oxalic acid, benzoic acid or salicylic acid, but it is several to be not limited to this
Kind organic carboxyl acid；Organic carboxyl acid used in the present embodiment is that analysis is pure.The present embodiment uses inert gas that nitrogen can be used.
Embodiment 1.
By melamine and pure acetic acid is analyzed according to mass ratio 1:10 mix, and are scattered in aqueous solvent, wherein, water and acetic acid
Volume ratio be 1:1, above-mentioned solution is heated into 10h for 160 DEG C in hydrothermal reaction kettle, obtains nitride porous carbon hydro-thermal predecessor；
By above-mentioned hydro-thermal predecessor, 2h is calcined in lower 550 DEG C of nitrogen protection in tube furnace, obtains ordered laminar nitride porous carbon material, such as
Shown in Fig. 1, Fig. 2 a.The specific surface area of ordered laminar nitride porous carbon material is 138m2g-1, prepared far above simple melamine
Carbon nitride material specific surface area 31m2/ g, as shown in Figure 3.
Embodiment 2.
By melamine and acetic acid according to mass ratio 1:10 mix, under anhydrous condition, by above-mentioned solution in hydrothermal reaction kettle
In 180 DEG C heating 16h, obtain nitride porous carbon hydro-thermal predecessor；By above-mentioned hydro-thermal predecessor, inert gas is protected in tube furnace
Lower 500 DEG C of calcinings 6h is protected, obtains nitride porous carbon material, as shown in Figure 2 b.The specific surface area of even porous carbon nitride material is
76m2/g。
Embodiment 3.
By melamine and oxalic acid according to mass ratio 1:5 mix, and are scattered in aqueous solvent, wherein, the quality of water and oxalic acid
Than for 1:1, above-mentioned solution is heated into 5h for 180 DEG C in hydrothermal reaction kettle, obtains nitride porous carbon hydro-thermal predecessor；By above-mentioned water
The lower 600 DEG C of calcinings 2h of hot predecessor inert gas shielding in tube furnace, obtains nitride porous carbon material.Nitride porous carbon material
Specific surface area be 106m2/g。
Embodiment 4.
By melamine and oxalic acid according to mass ratio 1:20 mix, and are scattered in aqueous solvent, wherein, the quality of water and oxalic acid
Than for 1:1, above-mentioned solution is heated into 10h for 150 DEG C in hydrothermal reaction kettle, obtains nitride porous carbon hydro-thermal predecessor；Will be above-mentioned
The lower 500 DEG C of calcinings 4h of hydro-thermal predecessor inert gas shielding in tube furnace, obtains nitride porous carbon material.Nitride porous carbon materials
The specific surface area of material is 112m2/g。
Embodiment 5.
By melamine and butyric acid according to mass ratio 1:1 mixes, and is scattered in aqueous solvent, wherein, the quality of water and butyric acid
Than for 1:1, above-mentioned solution is heated into 16h for 80 DEG C in hydrothermal reaction kettle, obtains nitride porous carbon hydro-thermal predecessor；By above-mentioned water
The lower 450 DEG C of calcinings 6h of hot predecessor inert gas shielding in tube furnace, obtains nitride porous carbon material.Nitride porous carbon material
Specific surface area be 86m2/g。
Embodiment 6.
By melamine and benzoic acid according to mass ratio 1:1 mixes, and is scattered in aqueous solvent, wherein, water and benzoic acid
Mass ratio is 1:1, above-mentioned solution is heated into 16h for 180 DEG C in hydrothermal reaction kettle, obtains nitride porous carbon hydro-thermal predecessor；Will
The above-mentioned lower 550 DEG C of calcinings 6h of hydro-thermal predecessor inert gas shielding in tube furnace, obtains tubular porous carbon nitride material, such as schemes
Shown in 2c.The specific surface area of tubular porous carbon nitride material is 68m2/g。
Embodiment 7.
By melamine and salicylic acid according to mass ratio 1:5 mix, be scattered in aqueous solvent, wherein, water with it is salicylic
Mass ratio is 1:1, above-mentioned solution is heated into 16h for 180 DEG C in hydrothermal reaction kettle, obtains nitride porous carbon hydro-thermal predecessor；Will
The above-mentioned lower 550 DEG C of calcinings 6h of hydro-thermal predecessor inert gas shielding in tube furnace, obtains tubular porous carbon nitride material.Tubulose
The specific surface area of nitride porous carbon material is 66m2/g。
Verify example：
Ordered laminar nitride porous carbon material prepared in the embodiment of the present invention 1 is used for organic dyestuff rhodamine B
Photocatalytic degradation is tested, and detailed process and step are as follows：
50mg ordered laminar nitride porous carbon materials are scattered in 50mL 50mg/L rhodamine B solution, in dark bar
30min is stirred under part and reaches adsorption equilibrium, then solution is placed under sunshine, 1mL is drawn with liquid-transfering gun every 5min
Supernatant is collected by centrifugation into centrifuge tube in solution, absorbance is determined using ultraviolet-visible spectrophotometer, according to absorption maximum
The absorbance of rhodamine B solution is drawn out under different light application times to the light of 50mg/L rhodamine B solution under wavelength 553nm wavelength
Catalytic degradation curve map.
Fig. 4 is the carbonitride that in the embodiment of the present invention 1 prepared by ordered laminar nitride porous carbon material and simple melamine
Catalytic activity comparison diagram of the material to rhodamine B under sunshine, it can be seen that ordered laminar nitride porous carbon material is in the sun
100% is basically reached after light irradiation 20min to rhodamine B degradation rate, and carbon nitride material prepared by simple melamine is too
It is only 4.1% to the degradation rate of rhodamine B after sunlight 20min, shows prepared ordered laminar nitride porous carbon material
Excellent photocatalysis performance.
The explanation of above case study on implementation can be used to help the principle and method for understanding the present invention.But above case study on implementation is simultaneously
It is not unique, it should not be construed as limiting the invention.With various process programs of the present inventive concept without substantial differences at this
Within the protection domain of invention.
Claims (4)
1. a kind of method that organic carboxyl acid auxiliary batch prepares nitride porous carbon material, it is characterised in that its preparation process is as follows：
By melamine and organic carboxyl acid according to mass ratio 1：1-1:Addition water dissolving after 20 mixings, its reclaimed water and organic carboxyl acid
Mass ratio is 1：1；Or by melamine and organic carboxyl acid according to mass ratio 1：1-1:20 mix dissolving；By the mixture after dissolving
80-180 DEG C of heating 1-16h, obtains nitride porous carbon hydro-thermal predecessor in hydrothermal reaction kettle；By nitride porous carbon hydro-thermal forerunner
Thing, in the lower 450-650 DEG C of calcining 1-6h of nitrogen protection, obtains nitride porous carbon material in tube furnace；
The organic carboxyl acid is acetic acid, oxalic acid, benzoic acid or salicylic acid.
2. the method that a kind of organic carboxyl acid auxiliary batch as claimed in claim 1 prepares nitride porous carbon material, its feature exist
In the mass ratio of the melamine and organic carboxyl acid be 1:2-1:10.
3. the method that a kind of organic carboxyl acid auxiliary batch as claimed in claim 1 prepares nitride porous carbon material, its feature exist
Mixture after the dissolving heats 5-12h for 100-180 DEG C in hydrothermal reaction kettle.
4. the method that a kind of organic carboxyl acid auxiliary batch as claimed in claim 1 prepares nitride porous carbon material, its feature exist
In the nitride porous carbon hydro-thermal predecessor lower 500-600 DEG C of calcining 2-4h is protected in tube furnace in nitrogen.
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| CN109012734A (en) * | 2018-09-14 | 2018-12-18 | 江南大学 | A kind of perforated tubular C3N4Photochemical catalyst and preparation method thereof |
| CN109351363A (en) * | 2018-10-16 | 2019-02-19 | 安徽理工大学 | A kind of evolving hydrogen reaction catalyst of layered mesoporous structure and preparation method thereof |
| CN110152706B (en) * | 2019-05-09 | 2021-06-01 | 北京师范大学 | Method for preparing carbon-rich carbon nitride visible-light-induced photocatalyst from eutectic precursor |
| CN110548534A (en) * | 2019-09-18 | 2019-12-10 | 常州大学 | preparation method of amino-modified flaky carbon nitride photocatalytic material |
| CN110560140A (en) * | 2019-09-29 | 2019-12-13 | 辽宁大学 | Weak luminescence g-C3N4Photocatalyst and preparation method and application thereof |
| CN110639590A (en) * | 2019-10-11 | 2020-01-03 | 江苏理工学院 | Preparation method and application of carbon nitride/carbon nano composite photocatalytic material |
| CN111250135B (en) * | 2020-02-17 | 2021-01-15 | 燕山大学 | Graphite-phase carbon nitride nanosheet material and preparation method and application thereof |
| CN111939961B (en) * | 2020-08-24 | 2023-04-11 | 南昌航空大学 | Controllable synthesis method of low-cost and high-load monatomic catalyst |
| CN113735074B (en) * | 2021-08-31 | 2024-05-10 | 大韩道恩高分子材料(上海)有限公司 | Preparation method of inorganic nucleating agent for biodegradable material |
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| CN105195190A (en) * | 2015-07-06 | 2015-12-30 | 阜阳师范学院 | Heterojunction photocatalyst SnS2/g-C3N4 as well as preparation method and application thereof |
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