CN107697915A - A kind of nitrogen-doped porous carbon material and preparation method thereof - Google Patents
A kind of nitrogen-doped porous carbon material and preparation method thereof Download PDFInfo
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- CN107697915A CN107697915A CN201710963865.1A CN201710963865A CN107697915A CN 107697915 A CN107697915 A CN 107697915A CN 201710963865 A CN201710963865 A CN 201710963865A CN 107697915 A CN107697915 A CN 107697915A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The invention discloses a kind of nitrogen-doped porous carbon material and preparation method thereof, using deep-fried twisted dough sticks as carbon source, fibroin albumen and Hyperbranched Polymer with Terminal Amido（HBP‑NH2）As nitrogen source, activated by four-part form high-temperature calcination and saleratus, obtain the nitrogen-doped porous carbon material with high-specific surface area and abundant hole, preparation process is easy, cost is cheap, is easy to mass produce, and has important application value in lithium battery, ultracapacitor, electrode material, gas absorption separation, hydrogen storage and dusty gas removing etc..
Description
Technical field
The present invention relates to a kind of nitrogen-doped porous carbon material and preparation method thereof, belongs to field of compound material.
Background technology
Porous carbon is a kind of solid material containing abundant pore structure and high-specific surface area, also with corrosion-resistant, radiation hardness,
The characteristics of density is small, thermal deformation is small, it is widely used in the fields such as aviation, chemical industry, medicine, new energy.Micropore（Diameter is less than
2nm）Carbon material can effectively adsorbed gas small molecule or exchange ion, be usually used in gas separation and purification, ion exchange and water
Processing etc..It is mesoporous（Diameter is between 2-50nm）Carbon material is suitable for adsorbing the macromoleculars such as medicine, dyestuff, and adsorption effect is most
It is good, and caused pressure drop is small, can be used as medicine carrier, adsorbent, ion fast exchange electrode material etc..Macropore（Directly
Footpath is more than 50nm）The adsorption capacity of carbon material is weaker, but beneficial to quick transmission, a large amount of scattered load large biological molecules or micro- life
Thing etc., it is the good space for playing biological function, also acts as accumulation of heat, thermal insulation, acoustic material etc..Nature exists substantial amounts of more
The material or system of level pore structure, such as bone of the stalk of plant and animal etc., they have two or more chi
The duct of degree, pore structure are exquisite, duct UNICOMs at different levels, and collaboration plays the transmission advantage in various ducts, transport different material,
The activity etc. that sustains life plays an important role.These structures are also adapted to the courses of reaction such as the cracking for having macromolecular to participate in,
Thus exploitation new multistage pore structure material is always study hotspot both domestic and external（It is prepared by skeletal like polyurethane sponge template direction
Nitrogen-doped porous carbon material [J] chemical progress, 2014,26 (12):1924-1929；Chemical progress, 2012,24 (Z1):262-
274）.
It is the common method for preparing porous carbon using biological material as carbon source, wherein biological material has cotton, silk
（Electrochimica Acta, 2017, 227:7-16, RSC Advances, 2017,7 (22):13383-13389, in
State's patent of invention 201510399394.7, the preparation of Liu Fangfang biomass deriveds doping carbon-supported catalysts and its hydrogen reduction electricity are urged
Research [D] the South China Science ＆ Engineering University of change performance, 2015）, watermelon peel, starch, saccharomycete, oriental plane tree wadding, stalk, straw, tree
Branch, bagasse, lotus leaf（Multi-stage porous carbon sulphur composite positive pole and performance study [J] Journal of Inorganic Materials are prepared with lotus leaf,
2016,31(02):135-140）, alginic acid（Facile syntheesis and its absorption property [J] the North China of magnetic porous carbon composite
Polytechnics's journal (natural science edition), 2017,39 (03):25-31）, sugarcane, lichee, shrimp shell, ox bone, saccharomycete（Biomass
Sulfamethazine performance study [D] Jiangsu Universitys in the preparation of nitrogen-doped porous carbon material and its absorption water, 2016）, waterside
Tongue（Advanced Functional Materials, 2016,26(46): 8487-8495）, marine alga（Natural biological presoma
Prepare research [J] Fudan Journal (natural sciences of micropore/composite mesoporous nitrogen-doped porous carbon material and its chemical property
Version), 2012,51 (05):650-658）, wicker（The controllable preparation of porous carbon sill of sheet and its efficiently separate antibiotic behavior and
Study mechanism [D] Jiangsu Universitys, 2016）, lignin, sunflower disk, pomelo peel（Sunflower disk and pomelo peel base porous carbon prepare and
Application [D] Heilongjiang Universitys in ultracapacitor, 2016）, spirulina（Journal of Alloys and
Compounds,2017,704: 1-6）, silk cocoon（Electrochimica Acta, 2017, 227:7-16, RSC
Advances, 2017,7(22): 13383-13389）.
Deep-fried twisted dough sticks are a kind of ancient Chinese style wheaten food, and elongated hollow form, it is sustained that mouthfeel is crisp, are the morning of Chinese tradition
One of point.Deep-fried twisted dough sticks add appropriate water, salt, additive using flour as primary raw material, through mix, smash, carry, proof, fried make
Into.Due to the reason of saccharomycetes to make fermentation, substantial amounts of carbon dioxide is produced, these gases are wrapped in not by the gluten in dough
It can escape, thus the hole of a large amount of honeycombs is formd inside deep-fried twisted dough sticks.This deep-fried twisted dough sticks with a large amount of honeycomb holes
After high temperature cabonization, the porous carbon materials with high-specific surface area can be formed, its effect will be better than most of natural biomass
Material.
The content of the invention
In view of the above problems, the present invention provides a kind of nitrogen-doped porous carbon material and preparation method thereof.
The technical scheme is that：
Deep-fried twisted dough sticks are cut into bulk, 80 DEG C of dry 24h, are subsequently placed in 150 DEG C of heat treatment 1-5h in the Muffle furnace under argon gas protection,
Wherein heating rate is 1 DEG C/min, after naturally cooling to room temperature, is immersed in mass fraction 1%-5% silk fibroin water solution
10-60min, after deionized water rinsing, it is placed in the lower Muffle furnace of argon gas protection 300 DEG C and is heat-treated 1-6h, wherein heating rate
For 2 DEG C/min, after naturally cooling to room temperature, 1-100g/L Hyperbranched Polymer with Terminal Amido is immersed in（HBP-NH2）The aqueous solution
Middle 1-6h, after deionized water rinsing, 500 DEG C of heat treatment 2-4h in the lower Muffle furnace of argon gas protection are placed in, wherein heating rate is 5
DEG C/min, after naturally cooling to room temperature, above-mentioned sample is immersed in 24h in 1-10g/L potassium bicarbonate solution, wherein the carbon
The mass ratio of potassium hydrogen phthalate and the sample is 10:1-4:1, after being rinsed repeatedly with deionized water after taking-up, naturally cooling to room temperature,
700-900 DEG C of heat treatment 1-6h in the Muffle furnace under argon gas protection is placed in, wherein heating rate is 10 DEG C/min, is naturally cooled to
After room temperature, 24h in 1mol/L hydrochloric acid solution is immersed in, is rinsed repeatedly with deionized water after taking-up, nitrogen is obtained after air drying
Doped porous carbon material.
Compared with prior art, the advantage of the invention is that：Using deep-fried twisted dough sticks as carbon source, fibroin albumen and amine-terminated hyperbrancedization
Polymer（HBP-NH2）As nitrogen source, activated by four-part form high-temperature calcination and saleratus, obtain with high-specific surface area and
The nitrogen-doped porous carbon material of abundant hole, preparation process is easy, cost is cheap, is easy to mass produce, in lithium battery, super
Capacitor, electrode material, gas absorption separation, hydrogen storage and dusty gas removing etc. have important application value.
Embodiment
The invention will be further elucidated with reference to specific embodiments.
Embodiment 1：
Deep-fried twisted dough sticks are cut into bulk, 80 DEG C of dry 24h, are subsequently placed in 150 DEG C of heat treatment 1h in the Muffle furnace under argon gas protection, its
Middle heating rate is 1 DEG C/min, after naturally cooling to room temperature, is immersed in 10min in the silk fibroin water solution of mass fraction 1%,
After deionized water rinsing, 300 DEG C of heat treatment 1h in the Muffle furnace under argon gas protection are placed in, wherein heating rate is 2 DEG C/min, from
After being so cooled to room temperature, 10g/L Hyperbranched Polymer with Terminal Amido is immersed in（HBP-NH2）1h in the aqueous solution, deionized water punching
After washing, 500 DEG C of heat treatment 2h in the Muffle furnace under argon gas protection are placed in, wherein heating rate is 5 DEG C/min, naturally cools to room
Wen Hou, above-mentioned sample is immersed in 24h in 1g/L potassium bicarbonate solution, wherein the quality of the saleratus and the sample
Than for 5:1, after being rinsed repeatedly with deionized water after taking-up, naturally cooling to room temperature, it is placed in 700 in the Muffle furnace under argon gas protection
DEG C heat treatment 1h, wherein heating rate is 10 DEG C/min, after naturally cooling to room temperature, is immersed in 1mol/L hydrochloric acid solution
24h, rinsed repeatedly with deionized water after taking-up, nitrogen-doped porous carbon material is obtained after air drying.
Embodiment 2：
Deep-fried twisted dough sticks are cut into bulk, 80 DEG C of dry 24h, are subsequently placed in 150 DEG C of heat treatment 2h in the Muffle furnace under argon gas protection, its
Middle heating rate is 1 DEG C/min, after naturally cooling to room temperature, is immersed in 30min in the silk fibroin water solution of mass fraction 2%,
After deionized water rinsing, 300 DEG C of heat treatment 3h in the Muffle furnace under argon gas protection are placed in, wherein heating rate is 2 DEG C/min, from
After being so cooled to room temperature, 50g/L Hyperbranched Polymer with Terminal Amido is immersed in（HBP-NH2）3h in the aqueous solution, deionized water punching
After washing, 500 DEG C of heat treatment 3h in the Muffle furnace under argon gas protection are placed in, wherein heating rate is 5 DEG C/min, naturally cools to room
Wen Hou, above-mentioned sample is immersed in 24h in 5g/L potassium bicarbonate solution, wherein the quality of the saleratus and the sample
Than for 4:1, after being rinsed repeatedly with deionized water after taking-up, naturally cooling to room temperature, it is placed in 800 in the Muffle furnace under argon gas protection
DEG C heat treatment 4h, wherein heating rate is 10 DEG C/min, after naturally cooling to room temperature, is immersed in 1mol/L hydrochloric acid solution
24h, rinsed repeatedly with deionized water after taking-up, nitrogen-doped porous carbon material is obtained after air drying.
Embodiment 3：
Deep-fried twisted dough sticks are cut into bulk, 80 DEG C of dry 24h, are subsequently placed in 150 DEG C of heat treatment 5h in the Muffle furnace under argon gas protection, its
Middle heating rate is 1 DEG C/min, after naturally cooling to room temperature, is immersed in 60min in the silk fibroin water solution of mass fraction 5%,
After deionized water rinsing, 300 DEG C of heat treatment 6h in the Muffle furnace under argon gas protection are placed in, wherein heating rate is 2 DEG C/min, from
After being so cooled to room temperature, 100g/L Hyperbranched Polymer with Terminal Amido is immersed in（HBP-NH2）5h in the aqueous solution, deionized water punching
After washing, 500 DEG C of heat treatment 4h in the Muffle furnace under argon gas protection are placed in, wherein heating rate is 5 DEG C/min, naturally cools to room
Wen Hou, above-mentioned sample is immersed in 24h in 10g/L potassium bicarbonate solution, wherein the matter of the saleratus and the sample
Amount is than being 8:1, after being rinsed repeatedly with deionized water after taking-up, naturally cooling to room temperature, it is placed in the Muffle furnace under argon gas protection
900 DEG C of heat treatment 6h, wherein heating rate is 10 DEG C/min, after naturally cooling to room temperature, is immersed in 1mol/L hydrochloric acid solution
Middle 24h, rinsed repeatedly with deionized water after taking-up, nitrogen-doped porous carbon material is obtained after air drying.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.Here all embodiments can not be exhaustive.It is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is amplified out still in protection scope of the present invention.
Claims (3)
- A kind of 1. nitrogen-doped porous carbon material and preparation method thereof, it is characterised in that：Deep-fried twisted dough sticks are cut into bulk, 80 DEG C of dryings 24h, 150 DEG C of heat treatment 1-5h in the Muffle furnace under argon gas protection are subsequently placed in, wherein heating rate is 1 DEG C/min, naturally cold But to 10-60min in mass fraction 1%-5% silk fibroin water solution after room temperature, is immersed in, after deionized water rinsing, it is placed in 300 DEG C of heat treatment 1-6h in Muffle furnace under argon gas protection, wherein heating rate is 2 DEG C/min, after naturally cooling to room temperature, leaching Hyperbranched Polymer with Terminal Amido of the stain in 1-100g/L（HBP-NH2）1-6h in the aqueous solution, after deionized water rinsing, it is placed in argon gas 500 DEG C of heat treatment 2-4h in Muffle furnace under protection, wherein heating rate is 5 DEG C/min, will be above-mentioned after naturally cooling to room temperature Sample is immersed in 24h in 1-10g/L potassium bicarbonate solution, wherein the mass ratio of the saleratus and the sample is 10: 1-4:1, after being rinsed repeatedly with deionized water after taking-up, naturally cooling to room temperature, it is placed in 700- in the Muffle furnace under argon gas protection 900 DEG C of heat treatment 1-6h, wherein heating rate is 10 DEG C/min, and after naturally cooling to room temperature, the hydrochloric acid for being immersed in 1mol/L is molten 24h in liquid, rinsed repeatedly with deionized water after taking-up, nitrogen-doped porous carbon material is obtained after air drying.
- A kind of 2. nitrogen-doped porous carbon material according to claim 1 and preparation method thereof, it is characterised in that the fibroin Albumen is that silk is made after degumming, dissolving, dialysis, purification.
- A kind of 3. nitrogen-doped porous carbon material obtained by claim 1 preparation method.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112062128A (en) * | 2020-09-10 | 2020-12-11 | 中国矿业大学 | Preparation method and application of nitrogen-doped porous carbon material based on crop straws |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106207119A (en) * | 2016-07-23 | 2016-12-07 | 天津大学 | A kind of method preparing N doping porous spherical disordered carbon material |
| CN107188155A (en) * | 2017-06-05 | 2017-09-22 | 安徽大学 | Preparation method of nitrogen-doped nano porous carbon spheres |
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- 2017-10-16 CN CN201710963865.1A patent/CN107697915A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106207119A (en) * | 2016-07-23 | 2016-12-07 | 天津大学 | A kind of method preparing N doping porous spherical disordered carbon material |
| CN107188155A (en) * | 2017-06-05 | 2017-09-22 | 安徽大学 | Preparation method of nitrogen-doped nano porous carbon spheres |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112062128A (en) * | 2020-09-10 | 2020-12-11 | 中国矿业大学 | Preparation method and application of nitrogen-doped porous carbon material based on crop straws |
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