CN109160504A - A kind of porous spiral faceted material of 3D, preparation method and application - Google Patents
A kind of porous spiral faceted material of 3D, preparation method and application Download PDFInfo
- Publication number
- CN109160504A CN109160504A CN201810909748.1A CN201810909748A CN109160504A CN 109160504 A CN109160504 A CN 109160504A CN 201810909748 A CN201810909748 A CN 201810909748A CN 109160504 A CN109160504 A CN 109160504A
- Authority
- CN
- China
- Prior art keywords
- porous spiral
- porous
- preparation
- faceted material
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 239000002135 nanosheet Substances 0.000 claims abstract description 6
- 238000010521 absorption reaction Methods 0.000 claims abstract description 4
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 37
- 239000002904 solvent Substances 0.000 claims description 20
- 238000003763 carbonization Methods 0.000 claims description 18
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 16
- 239000011975 tartaric acid Substances 0.000 claims description 16
- 235000002906 tartaric acid Nutrition 0.000 claims description 16
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- 239000008247 solid mixture Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 235000019270 ammonium chloride Nutrition 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- -1 graphite Alkene Chemical class 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- 235000014653 Carica parviflora Nutrition 0.000 description 1
- 244000132059 Carica parviflora Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 235000011118 potassium hydroxide Nutrition 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 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
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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
- B01J20/28002—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 physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
-
- 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
- B01J20/28014—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 form
- B01J20/28042—Shaped bodies; Monolithic structures
-
- 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
- B01J20/28078—Pore diameter
- B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
-
- 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
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
-
- 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
- B01J20/28078—Pore diameter
- B01J20/28085—Pore diameter being more than 50 nm, i.e. macropores
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention provides a kind of porous spiral faceted material of 3D, there is micropore, mesoporous and/or macropore in the porous spiral faceted material of the 3D, the structural unit of the porous spiral faceted material of 3D is 2D carbon nanosheet.The present invention also provides the preparation methods of the porous spiral faceted material of above-mentioned 3D.Raw material and presoma of the invention is common to be easy to get, and the porous spiral faceted material of the 3D of synthesis has the carbon structure similar to spiral tetrahexahedron, and specific surface area is up to 2034.2m2/ g, preparation process is uncomplicated, and preparation condition is not harsh, utilize easy one-step synthesis, the porous spiral polyhedron of 3D can be burnt out by controlling pressure, though it is foreseeable that the porous spiral faceted material of 3D of the invention can be widely used in bulky molecular catalysis, absorption and separation field.
Description
Technical field
The invention belongs to porous material technical fields, and in particular to a kind of porous spiral faceted material of 3D, preparation method
And application.
Background technique
Graphene is considered as most firm material in two dimensional form, and researcher wants to always in three-dimensional material
The middle firm intensity using under its two dimensional form, graphene flakelet is pressed together, makes by applying heat and pressure by they
A kind of structure that complexity is stable is produced, and the structure is entitled " spiral tetrahexahedron ", the structure is similar to coral and diatom
The structure of class biology, surface area relative volume is very big, and density is only the 5% of iron, the firmness degree of the structure be 10 times of iron with
On, it is one of the material of most light firm so far.Researcher also uses 3D printer, simulates its structure and amplifies, produces expansion
Big thousands of times of similar structures, and it is tested, it was demonstrated that its excellent mechanical property.
The excellent properties of the structure are mostly derived from this unique construction rather than material itself, it means that if can be by it
Same geometry is also made by material in he, so that it may the light material of same intensity is obtained, however, with conventional method and graphite
Alkene is difficult to produce this kind of structure, and therefore, it is still necessary to develop a kind of new material and preparation method.
Summary of the invention
To solve the problem of that spiral tetrahexahedron, this hair can not be prepared with conventional method and graphene in the prior art
The bright first purpose is to provide a kind of porous spiral polyhedron of 3D.
The second object of the present invention is to provide the porous spiral of above-mentioned 3D polyhedral preparation method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of porous spiral faceted material of 3D, have in the porous spiral faceted material of 3D micropore, it is mesoporous and/or
Macropore, the structural unit of the porous spiral faceted material of 3D are 2D carbon nanosheet.
Preferably, the 2D carbon nanosheet with a thickness of 1~12nm.
Preferably, the specific surface area of the porous spiral faceted material of the 3D is 400~2500m2/g。
Preferably, the pore volume of the porous spiral faceted material of the 3D is 0.1~1.5cm3/g。
Preferably, the aperture of micropore is less than 1nm in the porous spiral faceted material of the 3D.
The preparation method of the above-mentioned porous spiral faceted material of 3D, comprising the following steps:
(1) tartaric acid and presoma are added in solvent, stirring and dissolving；
(2) step (1) acquired solution heating stirring to solvent is evaporated completely and is dried；
(3) grinding steps (2) obtained solid mixture, and the solid mixture after grinding is placed in inert gas shielding
Carbonization is heated in tube furnace.
Preferably, step (1) described presoma includes in ammonium chloride, zinc chloride, potassium hydroxide, sodium hydroxide and phosphoric acid
At least one, the solvent are deionized water.
It is further preferred that step (1) presoma is ammonium chloride.
Preferably, the mass ratio of step (1) tartaric acid, presoma and solvent is (1:1:15)~(1:1:50).
It is further preferred that the mass ratio of step (1) tartaric acid, presoma and deionized water is 1:1:15.
Preferably, the temperature of step (2) described heating is 70~80 DEG C, and the temperature of the drying is 70~80 DEG C, drying
Time be 10~15h.
It is further preferred that the temperature of step (2) described heating is 75 DEG C, the temperature of the drying is 75 DEG C, drying
Time is 12h.
Preferably, the inert gas is argon gas or nitrogen.
Preferably, the device of step (3) described grinding is agate mortar, and the time of grinding is greater than 10min.
Preferably, the method for the heating carbonization are as follows: under 0.2~0.5MPa pressure, heated up with the rate of 10 DEG C/min,
480~550 DEG C are warming up to, 0.5h is kept the temperature, is continuously heating to 800~1200 DEG C and keeps the temperature 3h.
It is further preferred that the method for the heating carbonization are as follows: under 0.4MPa pressure, with the rate liter of 10 DEG C/min
Temperature is warming up to 500 DEG C, keeps the temperature 0.5h, is continuously heating to 800~1200 DEG C and keeps the temperature 3h.
It is further preferred that the method for the heating carbonization are as follows: under 0.4MPa pressure, with the rate liter of 10 DEG C/min
Temperature is warming up to 500 DEG C, keeps the temperature 0.5h, is continuously heating to 800~1000 DEG C and keeps the temperature 3h.
Application of the above-mentioned porous spiral faceted material of 3D in bulky molecular catalysis, absorption and separation field.
Tartaric acid is a kind of organic monoacid for having both hydroxyl and carboxyl, is from the fermentation byproduct winestone of grape wine earliest
It extracts and obtains, the hydroxyls carboxylic acid such as structure and citric acid, malic acid is similar, under numerous conditions all with stronger reaction
Activity, due to its unique physicochemical properties, tartaric acid is widely used in industries such as food, pharmacy, light industry and chemical industry.
Tartaric acid can be condensed in the molecule, hydroxy esterification, have excellent ligand complex performance.
Beneficial effects of the present invention
1, raw material of the invention and presoma is common is easy to get, the porous spiral faceted material of the 3D of synthesis, which has, is similar to spiral shell
The carbon structure of tetrahexahedron is revolved, specific surface area is up to 2034.2m2/g；
2, preparation process of the invention is uncomplicated, and preparation condition is not harsh, using easy one-step synthesis, passes through control
Pressure can burn out the porous spiral polyhedron of 3D；
3, predictably, the porous spiral faceted material of 3D of the invention is in bulky molecular catalysis, absorption and separation neck
It can be widely used in domain.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the porous spiral faceted material of 3D of the present invention.
Fig. 2 is the structural schematic diagram of spiral tetrahexahedron.
Fig. 3 is the transmission electron microscope picture of the porous spiral faceted material of 3D of the present invention.
Fig. 4 is the scanning electron microscope (SEM) photograph for the porous spiral faceted material of 3D that heating carbonization is prepared at 800 DEG C.
Fig. 5 is the scanning electron microscope (SEM) photograph for the porous spiral faceted material of 3D that heating carbonization is prepared at 900 DEG C.
Fig. 6 is the scanning electron microscope (SEM) photograph for the porous spiral faceted material of 3D that heating carbonization is prepared at 950 DEG C.
Fig. 7 is the scanning electron microscope (SEM) photograph for the faceted material that heating carbonization is prepared at 1000 DEG C.
Fig. 8 is the graph of pore diameter distribution of 2~4 sample of embodiment.
Fig. 9 is the hydrogen reduction electrocatalysis characteristic test result figure of 2~4 sample of embodiment.
Specific embodiment
The following is specific embodiments of the present invention, and is described with reference to the drawings and further retouches to technical solution of the present invention work
It states, however, the present invention is not limited to these examples.
Embodiment 1
A kind of porous spiral faceted material of 3D, as shown in Figure 1, the structural unit of the porous spiral faceted material of the 3D
For 2D carbon nanosheet.Fig. 2 is the structural schematic diagram of spiral tetrahexahedron, and Fig. 3 is the porous spiral faceted material of 3D of the present invention
Projection electron microscope, the light and shade difference in figure shows that nanometer sheet is distorted at high temperature under high pressure and is deformed into 3D structure.
Embodiment 2
The preparation method of the porous spiral faceted material of 3D, comprising the following steps:
(1) tartaric acid and presoma are added in solvent, stirring and dissolving；
(2) step (1) acquired solution heating stirring to solvent is evaporated completely and is dried；
(3) grinding steps (2) obtained solid mixture, and the solid mixture after grinding is placed in inert gas shielding
Carbonization is heated in tube furnace.
Step (1) presoma is ammonium chloride, and the mass ratio of tartaric acid, presoma and solvent is 1:1:15.
The temperature of step (2) described heating is 75 DEG C, and the temperature of the drying is 75 DEG C, and the time of drying is 12h, inertia
Gas is argon gas.
The method of step (3) the heating carbonization are as follows: under 0.4MPa pressure, heated up with the rate of 10 DEG C/min, heating
To 500 DEG C, 0.5h is kept the temperature, 800 DEG C is continuously heating to and keeps the temperature 3h.
Scanning electron microscope schematic diagram such as Fig. 4 of the porous spiral faceted material of the 3D being prepared.
Embodiment 3
The preparation method of the porous spiral faceted material of 3D, comprising the following steps:
(1) tartaric acid and presoma are added in solvent, stirring and dissolving；
(2) step (1) acquired solution heating stirring to solvent is evaporated completely and is dried；
(3) grinding steps (2) obtained solid mixture, and the solid mixture after grinding is placed in inert gas shielding
Carbonization is heated in tube furnace.
Step (1) presoma is ammonium chloride, and the mass ratio of tartaric acid, presoma and solvent is 1:1:15.
The temperature of step (2) described heating is 75 DEG C, and the temperature of the drying is 75 DEG C, and the time of drying is 12h, inertia
Gas is argon gas.
The method of step (3) the heating carbonization are as follows: under 0.4MPa pressure, heated up with the rate of 10 DEG C/min, heating
To 500 DEG C, 0.5h is kept the temperature, 900 DEG C is continuously heating to and keeps the temperature 3h.
Scanning electron microscope schematic diagram such as Fig. 5 of the porous spiral faceted material of the 3D being prepared.
Embodiment 4
The preparation method of the porous spiral faceted material of 3D, comprising the following steps:
(1) tartaric acid and presoma are added in solvent, stirring and dissolving；
(2) step (1) acquired solution heating stirring to solvent is evaporated completely and is dried；
(3) grinding steps (2) obtained solid mixture, and the solid mixture after grinding is placed in inert gas shielding
Carbonization is heated in tube furnace.
Step (1) presoma is ammonium chloride, and the mass ratio of tartaric acid, presoma and solvent is 1:1:15.
The temperature of step (2) described heating is 75 DEG C, and the temperature of the drying is 75 DEG C, and the time of drying is 12h, inertia
Gas is argon gas.
The method of step (3) the heating carbonization are as follows: under 0.4MPa pressure, heated up with the rate of 10 DEG C/min, heating
To 500 DEG C, 0.5h is kept the temperature, 950 DEG C is continuously heating to and keeps the temperature 3h.
The scanning electron microscope schematic diagram of the porous spiral faceted material of the 3D being prepared is as shown in Figure 6.
Comparative example 1
The preparation method of the porous spiral faceted material of 3D, comprising the following steps:
(1) tartaric acid and presoma are added in solvent, stirring and dissolving；
(2) step (1) acquired solution heating stirring to solvent is evaporated completely and is dried；
(3) grinding steps (2) obtained solid mixture, and the solid mixture after grinding is placed in inert gas shielding
Carbonization is heated in tube furnace.
Step (1) presoma is ammonium chloride, and the mass ratio of tartaric acid, presoma and solvent is 1:1:15.
The temperature of step (2) described heating is 75 DEG C, and the temperature of the drying is 75 DEG C, and the time of drying is 12h, inertia
Gas is argon gas.
The method of step (3) the heating carbonization are as follows: under 0.4MPa pressure, heated up with the rate of 10 DEG C/min, heating
To 500 DEG C, 0.5h is kept the temperature, 1000 DEG C is continuously heating to and keeps the temperature 3h.
The scanning electron microscope schematic diagram of the porous spiral faceted material of the 3D being prepared in figure as shown in fig. 7, can be seen that
The structure of faceted material is fallen apart.
Detect example
This example tests the specific surface area and pore volume for the porous spiral faceted material of 3D that embodiment 2~4 is prepared,
The results are shown in Table 1, and pore-size distribution is as shown in Figure 8.
Table 1
| Sample | Specific surface area (m2/g) | Pore volume (cm3/g) |
| Embodiment 2 | 404.9 | 0.21 |
| Embodiment 3 | 931.4 | 0.49 |
| Embodiment 4 | 2034.2 | 1.13 |
The hydrogen reduction electricity that this example further tests the porous spiral faceted material of 3D that embodiment 2~4 is prepared is urged
Change performance, as shown in figure 9, the wherein sample of 950 degree of firings, hydrogen reduction performance is close to platinum carbon, and wherein initial potential reaches 1v (Pt/C
=0.96v).
Claims (10)
1. a kind of porous spiral faceted material of 3D, which is characterized in that in the porous spiral faceted material of 3D have micropore,
Mesoporous and/or macropore, the structural unit of the porous spiral faceted material of 3D are 2D carbon nanosheet.
2. the porous spiral faceted material of 3D according to claim 1, which is characterized in that the 2D carbon nanosheet with a thickness of
1~12nm.
3. the porous spiral faceted material of 3D according to claim 1, which is characterized in that the porous spiral polyhedron material of 3D
The specific surface area of material is 400~2500m2/g。
4. the porous spiral faceted material of 3D according to claim 1, which is characterized in that the porous spiral polyhedron material of 3D
The pore volume of material is 0.1~1.5cm3/g。
5. a kind of preparation method of the porous spiral faceted material of the 3D as described in any one of Claims 1 to 4, which is characterized in that
The following steps are included:
(1) tartaric acid and presoma are added in solvent, stirring and dissolving；
(2) step (1) acquired solution heating stirring to solvent is evaporated completely and is dried；
(3) grinding steps (2) obtained solid mixture, and the solid mixture after grinding is placed in the tubular type of inert gas shielding
Carbonization is heated in furnace.
6. preparation method according to claim 5, which is characterized in that step (1) described presoma includes ammonium chloride, chlorination
At least one of zinc, potassium hydroxide, sodium hydroxide and phosphoric acid, the solvent are deionized water.
7. preparation method according to claim 5, which is characterized in that step (1) tartaric acid, presoma and solvent
Mass ratio is (1:1:15)~(1:1:50).
8. preparation method according to claim 5, which is characterized in that the temperature of step (2) described heating is 70~80 DEG C,
The temperature of the drying is 70~80 DEG C, and the time of drying is 10~15h.
9. preparation method according to claim 5, which is characterized in that the method for the heating carbonization are as follows: 0.2~
It under 0.5MPa pressure, is heated up with the rate of 10 DEG C/min, is warming up to 480~550 DEG C, keep the temperature 0.5h, it is continuously heating to 800~
1200 DEG C and keep the temperature 3h.
10. a kind of application of porous spiral faceted material of 3D in bulky molecular catalysis, absorption or separation field.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810909748.1A CN109160504B (en) | 2018-08-10 | 2018-08-10 | 3D porous spiral polyhedral material, preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810909748.1A CN109160504B (en) | 2018-08-10 | 2018-08-10 | 3D porous spiral polyhedral material, preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109160504A true CN109160504A (en) | 2019-01-08 |
| CN109160504B CN109160504B (en) | 2021-07-13 |
Family
ID=64895437
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810909748.1A Expired - Fee Related CN109160504B (en) | 2018-08-10 | 2018-08-10 | 3D porous spiral polyhedral material, preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109160504B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112264073A (en) * | 2020-10-29 | 2021-01-26 | 电子科技大学 | Helical structure C3N4Preparation method of nanofiber photocatalyst |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000342671A (en) * | 1999-06-02 | 2000-12-12 | Kunio Suzuki | Botanical deodorizing agent |
| CN104724693A (en) * | 2015-03-06 | 2015-06-24 | 苏州大学 | Organic-salt-based 3D porous carbon material, and preparation method and application thereof |
| WO2016002668A1 (en) * | 2014-07-03 | 2016-01-07 | 東レ株式会社 | Porous carbon material and method for manufacturing porous carbon material |
| WO2016032915A1 (en) * | 2014-08-23 | 2016-03-03 | Entegris, Inc. | Microporous carbon adsorbent from natural carbohydrates |
| CN105529472A (en) * | 2015-12-09 | 2016-04-27 | 武汉理工大学 | Co-N double-doped flaky porous two-dimensional carbon material and preparation method thereof |
| CN107394212A (en) * | 2017-07-07 | 2017-11-24 | 杨军 | A kind of three-dimensional porous electrode, its preparation method and application |
-
2018
- 2018-08-10 CN CN201810909748.1A patent/CN109160504B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000342671A (en) * | 1999-06-02 | 2000-12-12 | Kunio Suzuki | Botanical deodorizing agent |
| WO2016002668A1 (en) * | 2014-07-03 | 2016-01-07 | 東レ株式会社 | Porous carbon material and method for manufacturing porous carbon material |
| WO2016032915A1 (en) * | 2014-08-23 | 2016-03-03 | Entegris, Inc. | Microporous carbon adsorbent from natural carbohydrates |
| CN104724693A (en) * | 2015-03-06 | 2015-06-24 | 苏州大学 | Organic-salt-based 3D porous carbon material, and preparation method and application thereof |
| CN105529472A (en) * | 2015-12-09 | 2016-04-27 | 武汉理工大学 | Co-N double-doped flaky porous two-dimensional carbon material and preparation method thereof |
| CN107394212A (en) * | 2017-07-07 | 2017-11-24 | 杨军 | A kind of three-dimensional porous electrode, its preparation method and application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112264073A (en) * | 2020-10-29 | 2021-01-26 | 电子科技大学 | Helical structure C3N4Preparation method of nanofiber photocatalyst |
| CN112264073B (en) * | 2020-10-29 | 2021-12-03 | 电子科技大学 | Helical structure C3N4Preparation method of nanofiber photocatalyst |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109160504B (en) | 2021-07-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106563481B (en) | A kind of ultra-thin graphite phase carbon nitride photochemical catalyst of ammonification and preparation method thereof | |
| Laginhas et al. | Activated carbons with high nitrogen content by a combination of hydrothermal carbonization with activation | |
| Liu et al. | N-doped carbon spheres impregnated with highly monodispersed ruthenium nanoparticles as a hydrogenation catalyst | |
| Sevilla et al. | Superactivated carbide-derived carbons with high hydrogen storage capacity | |
| Sánchez-Sánchez et al. | Surface modification of nanocast ordered mesoporous carbons through a wet oxidation method | |
| WO2021121088A1 (en) | Mesoporous carbon material loaded cobalt-based catalyst and preparation method therefor | |
| CN105923623A (en) | Preparation method of graphene powder with three-dimensional hierarchical porous structure | |
| EP2203401B1 (en) | Method for preparing mesoporous carbonised materials from polysaccharides | |
| Morocco | Surface Characterization and Adsorption studies of Bambusa vulgaris-a low cost adsorbent | |
| CN110902680A (en) | Method for preparing mesoporous carbon material by organic potassium catalytic activation of sodium lignosulfonate | |
| Choi et al. | Preparation and characterization of sucrose-based microporous carbons for increasing hydrogen storage | |
| Sun et al. | Preparation, Optimization and Characterization of Carbon Fibers Adsorbent from Cotton by Microwave Induced ZnCl2 Activation | |
| CN109160504A (en) | A kind of porous spiral faceted material of 3D, preparation method and application | |
| Ma et al. | Aqueous route synthesis of mesoporous ZrO 2 by agarose templation | |
| CN108311130A (en) | A kind of step hole macroporous-mesoporous alumina carrier and preparation method thereof | |
| CN107601581A (en) | A kind of double pore dimension structure nano crystalline substance cobalt acetate powders and preparation method thereof | |
| Guy et al. | Synthesis and characterization of Cu doped activated carbon beads from chitosan | |
| JP5388051B2 (en) | Mesoporous carbon (MC-MCM-48) and method for producing the same | |
| Liang et al. | Borax-assisted hydrothermal carbonization to fabricate monodisperse carbon spheres with high thermostability | |
| Parayil et al. | Formation of titania-silica mixed oxides in solvent mixtures and their influences for the photocatalytic CO2 conversion to hydrocarbon | |
| Tang et al. | Efficient no‐glycerol biodiesel production using a novel biotemplated hierarchical porous‐structure CaO (O) | |
| CN110526228B (en) | Preparation method of petal-like carbon nanosheets | |
| CN107138127A (en) | A kind of bar-shaped Al of three-dimensional manometer2O3Shell-nuclear compounded material of@molecular sieves and preparation method thereof | |
| CN105905891A (en) | Method for preparing porous graphene by catalytic cracking and self-activation method | |
| CN108946707B (en) | Graphene aerogel and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Li Wenzhang Inventor after: Li Jie Inventor after: Yu Jiawen Inventor before: Li Jie Inventor before: Yu Jiawen Inventor before: Li Wenzhang |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210713 |