CN108910859A - A kind of preparation method of Metal Supported N doping bulk porous carbon materials - Google Patents
A kind of preparation method of Metal Supported N doping bulk porous carbon materials Download PDFInfo
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Abstract
The invention discloses the preparation methods that a kind of Metal Supported nitrogen mixes blocky porous carbon materials, which is characterized in that natural polysaccharide Polymer Solution or suspension are mixed with inorganic ammonium salt, metal salt, it is then freeze-dried to prepare the high-molecular porous material of natural polysaccharide；Metal Supported N doping bulk porous carbon materials are made by high temperature carbonization in the high-molecular porous material of natural polysaccharide.Inorganic ammonium salt is vaporized pore-forming in substrate surface by thermal decomposition as pore-foaming agent and nitrogen source, ammonium salt in the present invention；On the other hand the ammonia generated is decomposed under the high temperature conditions with carbon-based precursor reactant, forms Metal Supported N doping bulk porous carbon materials.Metal Supported N doping bulk porous carbon materials produced by the present invention have many advantages, such as high-specific surface area, high porosity, low-density, the energy, catalyze and synthesize, gas absorption, water-oil separating etc. have wide practical use in fields.
Description
Technical field
The present invention relates to a kind of preparation methods of Metal Supported N doping bulk porous carbon materials, belong to Metal Supported material
Technical field.
Background technique
Porous carbon materials are a kind of important raw materials, in fields such as gas absorption, water-oil separating, the energy, catalyst carriers
In have a wide range of applications.Metal load type nitrogen-doped carbon sill, since the introducing of nitrogen-atoms can effectively adjust matrix
Acid-base property, distribution of charges and the charge transport capability of material, to improve the application performance of Metal Supported carbon material.It is conventional
The preparation of Metal Supported nitrogen-doped carbon material mainly includes two methods：1. being made using nitrogenous microorganism, macromolecule, organic molecule
For ligand stable metal ion (such as polyacrylonitrile, urea, melamine, thiocarbamide), prepared through Pintsch process under inert atmosphere；
2. post activation technique-first prepares Metal Supported carbon material, preparation is then reacted under ammonia atmosphere.In the present that the energy increasingly tightens
It, uses nitrogenous organic ligand not meet " low-carbon row " as nitrogen source and requires.In addition, conventional carbon size is mostly low-dimensional knot
Structure, the problems such as causing using rear difficult separation, difficult circulation.
Three-dimensional bulk porous carbon materials have the characteristics that specific surface area is high, three-dimensional appearance is stable, internally crosslinked cellular structure,
It has a wide range of applications in the energy, adsorbent material and integral catalyzer.Natural polymer sill, as cellulose,
Chitosan, sodium alginate etc. have many advantages, such as that from a wealth of sources, low in cost, biocompatibility is high, biodegradable, by
Function it is applied to the porous material or aeroge of preparation high added value.Therefore, seek a kind of novel to prepare Metal Supported N doping
The method of blocky porous carbon materials has far-reaching research significance.
Riccardo Sapienza et al. (ACS APPL.MATER.INTER.2017,9 (9), 7885-7890) uses poly-
Then phenylethylene micro ball prepares high-specific surface area fibrination Porous materials through toluene etching as template fiberfill fibers element filter paper.
Matyjaszewski et al. (JACS, 2017,139 (37)：It 12931-12934) reports and uses ZnCl2 as pore-foaming agent, it is high
ZnCl when temperature charing2Heated vaporization forms duct and prepares high-specific surface area carbon material.It is inspired by this, this patent uses Inorganic Ammonium
For salt as pore-foaming agent and nitrogen source, one-step method prepares metal in height ratio surface area load N doping bulk porous carbon materials.Metal Supported
N doping bulk porous carbon materials have the characteristics that high-specific surface area, high porosity, stable three-dimensional appearance, in the energy, catalysis
Have wide practical use in the fields such as synthesis, gas absorption, water-oil separating.
Summary of the invention
The technical problem to be solved by the present invention is to：A kind of simple method is provided and prepares metal in height ratio surface area load nitrogen
Mix blocky porous carbon materials.
To solve the above-mentioned problems, the present invention provides the preparation sides that a kind of Metal Supported nitrogen mixes blocky porous carbon materials
Method, which is characterized in that natural polysaccharide Polymer Solution or suspension are mixed with inorganic ammonium salt, metal salt, it is then chilled dry
It is dry to prepare the high-molecular porous material of natural polysaccharide；Metal Supported nitrogen is made by high temperature carbonization in the high-molecular porous material of natural polysaccharide
Adulterate blocky porous carbon materials.The present invention is using inorganic ammonium salt as pore-foaming agent and nitrogen source, and one side ammonium salt is by thermal decomposition in substrate
Surface shape vaporizes pore-forming；On the other hand decompose generate ammonia under the high temperature conditions with carbon-based precursor reactant, formed high-specific surface area,
The nitrogen-doped porous carbon material of high porosity, low-density.
Preferably, the natural polysaccharide macromolecule is cellulose nano wire, cellulose micro wire, Cellulose nanocrystal, again
At least one of raw cellulose, carboxymethyl cellulose, starch, modified starch, sodium alginate, gelatin, lignin and chitosan.
Preferably, the inorganic ammonium salt is ammonium chloride, triammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium carbonate, bromine
Change in ammonium, ammonium hydrogen carbonate, ammonium oxalate, ammonium sulfate, ammonium dichromate, ammonium nitrate, ammonium acid fluoride, ammonium glycyrrhetate and ammonium acetate at least
It is a kind of.
Preferably, the metal salt be cobalt acetate, cobalt nitrate, cobalt chloride, acetylacetone cobalt, six water nickel chlorides, nickel nitrate,
At least one of nickel acetate, iron chloride, nine water ferric nitrates, acetic acid acetone iron, palladium chloride and gold chloride.
Preferably, the solid content of the natural polysaccharide macromolecule Polymer Solution or suspension is 0.5~5.0%.
Preferably, the natural polysaccharide macromolecule Polymer Solution or natural polysaccharide macromolecule and Inorganic Ammonium in suspension
The mass ratio of salt is 1: 0.1~1: 1.5.
Preferably, the natural polysaccharide macromolecule Polymer Solution or natural polysaccharide macromolecule and metal salt in suspension
Mass ratio be 1: 0.1~1: 1.
Preferably, the mixed temperature is 20~80 DEG C, and the time is 2~12h.
Preferably, the temperature of the freeze-drying is -60~-30 DEG C, and pressure is 8~50Pa, and the time is 12~48h.
Preferably, the technological parameter of the high temperature carbonization is：Under nitrogen atmosphere, it is warming up to the heating rate of 5 DEG C/min
500~900 DEG C, then keep the temperature 1~3h.
The present invention provides a kind of methods for inexpensively preparing metal in height ratio surface area load N doping bulk porous carbon materials.
Wherein inorganic ammonium salt is vaporized pore-forming in substrate surface by thermal decomposition as pore-foaming agent and nitrogen source, ammonium salt；On the other hand it decomposes and generates
Ammonia under the high temperature conditions with carbon-based precursor reactant, formed Metal Supported N doping bulk porous carbon materials.Metal Supported nitrogen is mixed
Miscellaneous bulk porous carbon materials have many advantages, such as high-specific surface area, high porosity, low-density, in the energy, catalyze and synthesize, gas suction
Have wide practical use in the fields such as attached, water-oil separating.
Detailed description of the invention
Fig. 1 is the flow chart of Metal Supported N doping bulk porous carbon preparation；
Fig. 2 is that cobalt prepared by embodiment 1 loads N doping porous carbon Co-N/C 0-800 transmission electron microscope photo；
Fig. 3 is that cobalt prepared by embodiment 2 loads N doping porous carbon Co-N/C 50-800 transmission electron microscope photo；
Fig. 4 is the cobalt load nitrogen-doped porous carbon material Co-N/C 50-800 cutting test photo for implementing 2 preparations；
Fig. 5 is that the cobalt prepared in embodiment 1,2 loads N doping porous carbon load-bearing experiment；
Fig. 6 is that the cobalt prepared in embodiment 1,2,6,7 loads N doping porous carbon nitrogen adsorption desorption curve；
Fig. 7 is that the cobalt prepared in embodiment 1,2,6,7 loads N doping porous carbon XRD diagram；
Fig. 8 is that the cobalt prepared in embodiment 1,2,6,7 loads N doping porous carbon XPS figure；
Fig. 9 is that the cobalt prepared in embodiment 1,2,6,7 loads N doping porous carbon Raman spectrogram.
Specific embodiment
In order to make the present invention more obvious and understandable, hereby with preferred embodiment, and attached drawing is cooperated to be described in detail below.
Embodiment 1
A kind of Metal Supported nitrogen mixes the preparation method of blocky porous carbon materials：
(1) the nanowire suspended liquid of 10.0g solid content 3.0wt.% cellulose is taken, 3.0wt.% chitosan-acetic acid solution is added
(10.0g), Cobalt diacetate tetrahydrate (46.7mg), 60 DEG C of magnetic agitation 4h；
(2) suspension prepared by (1) is placed in liquid nitrogen and is rapidly frozen, cooling time, 10min, it is dry to be subsequently placed in freezing
It is freeze-dried in dry machine, cooling time 30h, obtains cobalt load natural polymer based porous materials；
(3) by (2) prepare porous material be placed in atmosphere furnace, under the conditions of nitrogen protection, heating rate be 5 DEG C/min extremely
800 DEG C, 3h is kept the temperature, obtains cobalt load N doping bulk porous carbon Co-N/C 0-800 (M-N/Cx y-z：M is the metal of load
Element, x are natural polysaccharide macromolecule, and raw material is cellulose nano wire when wherein x is default, and y is the matter that ammonium salt accounts for natural polymer
Percentage is measured, z is carbonization temperature).
Show that the 0-800 cobalt nanometer particle surface Co-N/C of preparation covers agraphitic carbon by Fig. 2.
Show that Co-N/C 0-800 carbon material does not have good mechanical performance, under external force easily broken change by Fig. 5
Shape.
Show that Co-N/C0-800 carbon material specific surface area is 102m by Fig. 62/g。
Show that Co-N/C 0-800 carbon material has apparent carbon, cobalt diffraction maximum, and cobalt diffraction maximum peak type and standard by Fig. 7
Cobalt simple substance is consistent.
Show that Co-N/C 0-800 carbon material surface has apparent cobalt, carbon, oxygen element characteristic peak by Fig. 8, nitrogen peak is not
Obviously.
Show that Co-N/C0-800 carbon material has apparent amorphous carbon and crystalline carbon peak, and amorphous carbon and knot by Fig. 9
Brilliant carbon peak area ratio (ID/IG) it is 1.51.
Embodiment 2
A kind of Metal Supported nitrogen mixes the preparation method of blocky porous carbon materials：
(1) the nanowire suspended liquid of 10.0g solid content 3.0wt.% cellulose is taken, 3.0wt.% chitosan-acetic acid solution is added
(10.0g), Cobalt diacetate tetrahydrate (46.7mg), ammonium chloride (0.3g), 60 DEG C of magnetic agitation 4h；
(2) suspension prepared by (1) is placed in liquid nitrogen and is rapidly frozen, cooling time, 10min, it is dry to be subsequently placed in freezing
It is freeze-dried in dry machine, cooling time is 30 hours, obtains cobalt load natural polymer based porous materials；
(3) by (2) prepare porous material be placed in atmosphere furnace, under the conditions of nitrogen protection, heating rate be 5 DEG C/min extremely
800 DEG C, 3h is kept the temperature, obtains cobalt load N doping bulk porous carbon Co-N/C 50-800.
Show that the Co-N/C 5-800 cobalt nanometer particle of preparation is embedded in porous carbon surface by Fig. 3, and carbon material surface is deposited
In a large amount of hole.
Show Co-N/C 50-800 carbon material to have under machinability and external force by Fig. 4,5 and keeps original shape
Shape.
Show Co-N/C 50-800 carbon material specific surface area up to 609m by Fig. 62/g。
Show that Co-N/C 50-800 carbon material has apparent carbon, cobalt diffraction maximum, and cobalt diffraction maximum peak type and standard by Fig. 7
Cobalt simple substance is consistent.
Show that Co-N/C50-800 carbon material surface has apparent nitrogen, cobalt, carbon, oxygen element characteristic peak by Fig. 8.
Show that Co-N/C 50-800 carbon material has apparent amorphous carbon and crystalline carbon peak by Fig. 9, and amorphous carbon with
Crystalline carbon peak area ratio (ID/IG) it is 2.08.
Embodiment 3
A kind of Metal Supported nitrogen mixes the preparation method of blocky porous carbon materials：
(1) the nanowire suspended liquid of 10.0g solid content 3.0wt.% cellulose is taken, 3.0wt.% chitosan-acetic acid solution is added
(10.0g), six water nickel chlorides (217.0mg), ammonium chloride (0.3g), are stirred at room temperature 12h；
(2) suspension prepared by (1) is placed in liquid nitrogen and is rapidly frozen, cooling time, 10min, it is dry to be subsequently placed in freezing
It is freeze-dried in dry machine, cooling time is 30 hours, obtains nickel load natural polymer based porous materials；
(3) by (2) prepare porous material be placed in atmosphere furnace, under the conditions of nitrogen protection, heating rate be 5 DEG C/min extremely
800 DEG C, 3h is kept the temperature, nickel load N doping bulk porous carbon Ni-N/C 50-800 is obtained.
Embodiment 4
A kind of Metal Supported nitrogen mixes the preparation method of blocky porous carbon materials：
(1) the nanowire suspended liquid of 10.0g solid content 3.0wt.% cellulose is taken, 3.0wt.% chitosan-acetic acid solution is added
(10.0g), nine water ferric nitrates (370.0mg), ammonium chloride (0.3g), are stirred at room temperature 12h；
(2) suspension prepared by (1) is placed in liquid nitrogen and is rapidly frozen, cooling time, 10min, it is dry to be subsequently placed in freezing
It is freeze-dried in dry machine, cooling time is 30 hours, obtains iron load natural polymer based porous materials；
(3) by (2) prepare porous material be placed in atmosphere furnace, under the conditions of nitrogen protection, heating rate be 5 DEG C/min extremely
800 DEG C, 3h is kept the temperature, obtains iron load N doping bulk porous carbon Fe-N/C 50-800.
Embodiment 5
A kind of Metal Supported nitrogen mixes the preparation method of blocky porous carbon materials：
(1) 10.0g solid content 3.0wt.% gelatin solution is taken, 3.0wt.% chitosan-acetic acid solution (10.0g), chlorine is added
Change palladium (50.0mg), ammonium chloride (0.6g), 12h is stirred at room temperature；
(2) suspension prepared by (1) is placed in liquid nitrogen and is rapidly frozen, cooling time, 10min, it is dry to be subsequently placed in freezing
It is freeze-dried in dry machine, cooling time is 30 hours, obtains palladium load natural polymer based porous materials；
(3) by (2) prepare porous material be placed in atmosphere furnace, under the conditions of nitrogen protection, heating rate be 5 DEG C/min extremely
600 DEG C, 3h is kept the temperature, obtains palladium load N doping bulk porous carbon Pd-N/Cgelatin 100-600.
Embodiment 6
A kind of Metal Supported nitrogen mixes the preparation method of blocky porous carbon materials：
(1) the nanowire suspended liquid of 10.0g solid content 3.0wt.% cellulose is taken, 3.0wt.% chitosan-acetic acid solution is added
(10.0g), Cobalt diacetate tetrahydrate (46.7mg), ammonium chloride (0.3g), 60 DEG C of magnetic agitation 4h；
(2) suspension prepared by (1) is placed in liquid nitrogen and is rapidly frozen, cooling time, 10min, it is dry to be subsequently placed in freezing
It is freeze-dried in dry machine, cooling time is 30 hours, obtains cobalt load natural polymer based porous materials；
(3) by (2) prepare porous material be placed in atmosphere furnace, under the conditions of nitrogen protection, heating rate be 5 DEG C/min extremely
700 DEG C, 3h is kept the temperature, obtains cobalt load N doping bulk porous carbon Co-N/C 50-700.
Embodiment 7
A kind of Metal Supported nitrogen mixes the preparation method of blocky porous carbon materials：
(1) the nanowire suspended liquid of 10.0g solid content 3.0wt.% cellulose is taken, 3.0wt.% chitosan-acetic acid solution is added
(10.0g), Cobalt diacetate tetrahydrate (46.7mg), ammonium chloride (0.3g), 60 DEG C of magnetic agitation 4h；
(2) suspension prepared by (1) is placed in liquid nitrogen and is rapidly frozen, cooling time, 10min, it is dry to be subsequently placed in freezing
It is freeze-dried in dry machine, cooling time is 30 hours, obtains cobalt load natural polymer based porous materials；
(3) by (2) prepare porous material be placed in atmosphere furnace, under the conditions of nitrogen protection, heating rate be 5 DEG C/min extremely
600 DEG C, 3h is kept the temperature, obtains cobalt load N doping bulk porous carbon Co-N/C 50-600.
Claims (10)
1. the preparation method that a kind of Metal Supported nitrogen mixes blocky porous carbon materials, which is characterized in that natural polysaccharide macromolecule is molten
Liquid or suspension are mixed with inorganic ammonium salt, metal salt, then freeze-dried to prepare the high-molecular porous material of natural polysaccharide；Naturally
Metal Supported N doping bulk porous carbon materials are made by high temperature carbonization in polysaccharide polymer porous material.
2. the preparation method that Metal Supported nitrogen as described in claim 1 mixes blocky porous carbon materials, which is characterized in that the day
Right polysaccharide polymer be cellulose nano wire, cellulose micro wire, Cellulose nanocrystal, regenerated cellulose, carboxymethyl cellulose,
At least one of starch, modified starch, sodium alginate, gelatin, lignin and chitosan.
3. the preparation method that Metal Supported nitrogen as described in claim 1 mixes blocky porous carbon materials, which is characterized in that the nothing
Machine ammonium salt be ammonium chloride, triammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium carbonate, ammonium bromide, ammonium hydrogen carbonate, ammonium oxalate,
At least one of ammonium sulfate, ammonium dichromate, ammonium nitrate, ammonium acid fluoride, ammonium glycyrrhetate and ammonium acetate.
4. Metal Supported nitrogen as described in claim 1 mixes the preparation method of blocky porous carbon materials, which is characterized in that the gold
Category salt is cobalt acetate, cobalt nitrate, cobalt chloride, acetylacetone cobalt, six water nickel chlorides, nickel nitrate, nickel acetate, iron chloride, nine water nitre
At least one of sour iron, acetic acid acetone iron, palladium chloride and gold chloride.
5. the preparation method that Metal Supported nitrogen as described in claim 1 mixes blocky porous carbon materials, which is characterized in that the day
The solid content of right polysaccharide polymer Polymer Solution or suspension is 0.5~5.0%.
6. the preparation method that Metal Supported nitrogen as described in claim 1 mixes blocky porous carbon materials, which is characterized in that the day
The mass ratio of right polysaccharide polymer Polymer Solution or natural polysaccharide macromolecule and inorganic ammonium salt in suspension is 1: 0.1~1:
1.5。
7. the preparation method that Metal Supported nitrogen as described in claim 1 mixes blocky porous carbon materials, which is characterized in that the day
The mass ratio of right polysaccharide polymer Polymer Solution or natural polysaccharide macromolecule and metal salt in suspension is 1: 0.1~1: 1.
8. the preparation method that Metal Supported nitrogen as described in claim 1 mixes blocky porous carbon materials, which is characterized in that described mixed
The temperature of conjunction is 20~80 DEG C, and the time is 2~12h.
9. the preparation method that Metal Supported nitrogen as described in claim 1 mixes blocky porous carbon materials, which is characterized in that described cold
It is -60~-30 DEG C that dry temperature, which is lyophilized, and pressure is 8~50Pa, and the time is 12~48h.
10. the preparation method that Metal Supported nitrogen as described in claim 1 mixes blocky porous carbon materials, which is characterized in that described
The technological parameter of high temperature carbonization is：Under nitrogen atmosphere, 500~900 DEG C are warming up to the heating rate of 5 DEG C/min, then keep the temperature 1~
3h。
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