CN108706583A - A kind of preparation method of nanoporous carbon materials - Google Patents
A kind of preparation method of nanoporous carbon materials Download PDFInfo
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- CN108706583A CN108706583A CN201810622806.2A CN201810622806A CN108706583A CN 108706583 A CN108706583 A CN 108706583A CN 201810622806 A CN201810622806 A CN 201810622806A CN 108706583 A CN108706583 A CN 108706583A
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- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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- C01B32/336—Preparation characterised by gaseous activating agents
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Abstract
The present invention relates to a kind of preparation methods of nanoporous carbon materials, include the following steps：Template is dissolved in aqueous solution, template aqueous solution is uniformly mixing to obtain；Phloroglucin and melamine are added in template aqueous solution, formaldehyde is added after being completely dissolved, adds sodium bicarbonate solution, stirs evenly, forms colloidal sol；Colloidal sol sealing is put into baking oven and is heat-treated, gel is formed, is cooled to room temperature, obtains organic wet gel；Organic wet gel is cleaned repeatedly, later constant pressure and dry in the deionized water solution of sorbitan oleate, obtains organic xerogel block.Nanoporous carbon materials density prepared by this method is adjustable, and cheap, the characteristics such as specific surface area height play the role of key in electrochemical field.
Description
Technical field
The invention belongs to electrochemical fields, and in particular to a kind of preparation method of nanoporous carbon materials.
Background technology
The research of nanoporous carbon materials is used as always scientific research hot spot, in electricity, optics, calorifics, acoustics and electrochemistry etc.
Aspect shows excellent physical and chemical performance.The nanoporous carbon materials prepared by sol-gel process are in drying process
In usually by certain high-temperature high-pressure apparatus or cryogenic vacuum equipment, however the use of these equipment is for production application
In be unfavorable, it can be faced, and cost is higher, production takes and danger coefficient is big etc. difficult, it is difficult to realize large-scale production.Mesh
Before, the organic xerogel of nanoporous is usually prepared using constant pressure and dry technology in industrial processes, this method is to utilize
Chamber dryer freely volatilizees by the solvent in gel, and equipment is simple, and short preparation period is of low cost.
Chinese patent CN102874791A discloses a kind of preparation method of classifying porous nano-carbon material, and this method includes
Following steps：(1) organosol is prepared；(2) organosol aging prepared by step (1) is prepared into organic aerogel；(3) will
The organic aerogel vacuum constant temperature drying that step (2) obtains；(4) product that step (3) obtains once is carbonized；(5) will
The product ball milling that step (4) obtains；(6) product that step (5) obtains is impregnated in mixed acid liquid, it is 6 then to clean to pH value
~7, filtering, vacuum constant temperature drying；(7) KOH solids are added in the product that step (6) obtains and deionized water are mixed into paste,
Vacuum constant temperature is dried；(8) product for obtaining step (7) carries out secondary charing, but KOH activation processs are cumbersome, time-consuming, can deposit
In local corrosion phenomenon, makes the micropore on carbon particle microballoon and small mesoporous certain collapse occurs.
Invention content
The purpose of the present invention is exactly to solve the above-mentioned problems and provides a kind of preparation method of nanoporous carbon materials, receives
Porous carbon materials density is adjustable for rice, specific surface area is high, while reducing production cost, cheap in the industrial production, conveniently make
With.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of nanoporous carbon materials, includes the following steps：
(1) template is dissolved in aqueous solution, is uniformly mixing to obtain template aqueous solution；
(2) phloroglucin and melamine are added in template aqueous solution, formaldehyde is added after being completely dissolved, adds
Sodium bicarbonate solution stirs evenly, and forms colloidal sol；
(3) colloidal sol sealing is put into baking oven and is heat-treated, formed gel, be cooled to room temperature, obtain organic wet gel；
(4) organic wet gel is cleaned repeatedly in the deionized water solution of sorbitan oleate, later constant pressure and dry,
Obtain organic xerogel block；
(5) organic xerogel block is carbonized under nitrogen atmosphere, then the xerogel block being carbonized is subjected to CO2It is living
Change to get to nanoporous carbon materials.
Further, step (1) described template is selected from neopelex, lauryl sodium sulfate or hexadecane
One kind of base trimethylammonium bromide, a concentration of 0.006-0.028mol/L of template.
Further, the molar ratio of step (2) phloroglucin, melamine and formaldehyde is 0.25-4：1：10.
Further, a concentration of 0.04-0.06mol/L of step (2) described sodium bicarbonate solution, the phloroglucin and
It is 50-300 that melamine, which is mixed with the molar ratio of sodium bicarbonate,：1.
Further, the mass fraction of solute is 10-40% in the colloidal sol that step (2) is formed.
Further, the temperature of step (3) baking oven is 80-90 DEG C, and processing time is 3-5 days.
Further, a concentration of 5-20g/L of step (4) described sorbitan oleate, cleaning 4-8 times repeatedly, daily 1
It is secondary.
Further, step (5) carbonization is to carry out 2.5- in tubular type retort with 900-1100 DEG C of temperature
3.5h, and nitrogen is continually fed into the rate of 200-400ml/min.
Further, step (5) CO2Activation carries out 2.5-3.5h at 900-1100 DEG C, and with 10-50ml/min
Rate be continually fed into CO2Gas.
The nanoporous carbon materials that the method for the present invention is prepared have nano-porous structure, density 200-800mg/
cm3, specific surface area 200-1200m2/g。
The present invention selects suitable catalyst (NaHCO3), recombination reaction object and suitable Solute mass fraction, use
Template synthesized gel rubber is used in combination deionized water to prepare organic wet gel as solvent, and deionization is selected before carrying out constant pressure and dry
Water replaces impurity extra in wet gel, then passes through high temperature cabonization and CO2Activation obtains the adjustable porous carbon materials of density.This
Invention selects recombination reaction object to prepare wet gel for presoma and template, while during constant pressure and dry, the mould of selection
Plate agent can extenuate the influence of water surface tension, change the hydrophily of gel skeleton, reduce collapsing for gel inner skeleton, to
Remain the nano-porous structure of gel.
To reduce the huge surface tension (72mNm of aqueous solvent-1), the present invention uses template (dodecyl benzene sulfonic acid
Sodium, lauryl sodium sulfate or cetyl trimethylammonium bromide) be added in deionized water solution prepared as solvent it is organic
Wet gel, the characteristics such as with good stability, surface-active of template, and also the hydrophobe group of template can be effectively improved
The hydrophilic and hydrophobic of material surface contains methyl in template, and due to the introducing of methyl, template makes the table of solution in aqueous solution
Face tension reduces, and has used template that can reduce caving in for gel inner skeleton during constant pressure and dry, keeps gel nanometer
Porous structure.
When the present invention carries out constant pressure and dry process to wet gel, solvent replacement is carried out to wet gel before dry, using containing
The surface tension of the aqueous solution of the surfactant feature smaller than aqueous solvent is replaced (clear using sorbitan oleate aqueous solution
Wash) organic wet gel, reduces shrinking percentage of wet gel during constant pressure and dry；Again by the xerogel of preparation by carbonization, CO2
Activation process obtains conductive nanometer porous carbon materials, and the nanoporous carbon materials being prepared can have that density is adjustable, price
The cheap, characteristics such as specific surface area is high, can apply on the fields such as electrochemistry, absorption.
Compared with prior art, the present invention includes at least following advantages and good effect：One kind of the present invention is cheap to be prepared
Density is adjustable, the method for the high nanoporous carbon materials of specific surface area, and deionized water solution is added to as molten using template
Agent prepares organic wet gel, plays the role of reaming, reduces the surface tension effects that aqueous solvent brings gel inner skeleton；
Simultaneously in carbonisation, template can be burnt up, nanoporous carbon will not be impacted, then pass through CO again2Activation
Technology manufactures micropore.
Description of the drawings
Fig. 1 is that the SEM of 1 nanoporous carbon of embodiment schemes；
Fig. 2 is nitrogen adsorption-desorption curve of 1 nanoporous carbon of embodiment.
Specific implementation mode
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of preparation method of nanoporous carbon materials, includes the following steps：
Step 1: aqueous solution of the configuration containing template (neopelex), uniform stirring, until template is complete
Portion is dissolved, and solution, which becomes, to be clarified, and a concentration of 25.00 × 10-3mol/L；
Step 2: a certain amount of drug phloroglucin, melamine are added in the aqueous solution containing template, completely
Formaldehyde is added after dissolving, adds catalyst sodium bicarbonate solution, stirs evenly, forms colloidal sol, wherein Solute mass fraction is
20%, the molar ratio of phloroglucin, melamine and formaldehyde is 4：1：10, a concentration of 0.05mol/L of sodium bicarbonate solution,
The molar ratio of benzenetriol and sodium bicarbonate is 100；
Step 3: colloidal sol sealing is put into 85 DEG C of baking oven, handle 5 days, gel postcooling to room temperature takes out sample, system
For organic wet gel；
Organic wet gel is replaced Step 4: being added in deionized water using the sorbitan oleate of 10g/L, is replaced daily
It 1 time, replaces 5 times, organic wet gel is then put in progress constant pressure and dry at aeration-drying；
Step 5: suitable organic xerogel block is put into tubular type retort, after vacuumizing, in the protection of nitrogen atmosphere
Under, using 1000 DEG C of carbonization 180min；The xerogel block being carbonized is subjected to CO again2Activation, in CO21000 are used under atmosphere
DEG C activation 180min, wherein active rate is within the scope of 10ml/min-50ml/min.
Fig. 1 is that the SEM of nanoporous carbon schemes, and Fig. 2 is nitrogen adsorption-desorption curve of nanoporous carbon, the nanometer of preparation
Porous carbon materials have nano-porous structure, density 0.68g/cm3, specific surface area 673m2/g。
Embodiment 2
A kind of preparation method of nanoporous carbon materials, includes the following steps：
Step 1: at 35 DEG C, aqueous solution of the configuration containing template (cetyl trimethylammonium bromide) uniformly stirs
It mixes, until template all dissolves, solution, which becomes, to be clarified, and a concentration of 25.00 × 10-3mol/L。
Step 2: a certain amount of drug phloroglucin, melamine are added in the aqueous solution containing template, completely
Formaldehyde is added after dissolving, adds catalyst sodium bicarbonate solution, stirs evenly, forms colloidal sol, wherein Solute mass fraction is
20%, the molar ratio of phloroglucin, melamine and formaldehyde is 3：2：10, a concentration of 0.05mol/L of sodium bicarbonate solution,
The molar ratio of benzenetriol and sodium bicarbonate is 50；
Step 3: colloidal sol sealing is put into 85 DEG C of baking oven, handle 5 days, gel postcooling to room temperature takes out sample, system
For organic wet gel；
Organic wet gel is replaced Step 4: being added in deionized water using the sorbitan oleate of 10g/L, is replaced daily
It 1 time, replaces 5 times, organic wet gel is then put in progress constant pressure and dry at aeration-drying；
Step 5: suitable organic xerogel block is put into tubular type retort, after vacuumizing, in the protection of nitrogen atmosphere
Under, using 1000 DEG C of carbonization 180min；The xerogel block being carbonized is subjected to CO again2Activation, in CO21000 are used under atmosphere
DEG C activation 180min, wherein active rate is within the scope of 10ml/min-50ml/min.
The nanoporous carbon materials inexpensively prepared have nano-porous structure, density 0.49g/cm3, specific surface area is
1031m2/g。
Embodiment 3
A kind of preparation method of nanoporous carbon materials, includes the following steps：
Step 1: at 35 DEG C, aqueous solution of the configuration containing template (neopelex), uniform stirring, directly
It all being dissolved to template, solution, which becomes, to be clarified, and a concentration of 15.00 × 10-3mol/L。
Step 2: a certain amount of drug phloroglucin, melamine are added in the aqueous solution containing template, completely
Formaldehyde is added after dissolving, adds catalyst sodium bicarbonate solution, stirs evenly, forms colloidal sol, wherein Solute mass fraction is
10%, the molar ratio of phloroglucin, melamine and formaldehyde is 3：2：10, a concentration of 0.05mol/L of sodium bicarbonate solution,
The molar ratio of benzenetriol and sodium bicarbonate is 50；
Step 3: colloidal sol sealing is put into 85 DEG C of baking oven, handle 5 days, gel postcooling to room temperature takes out sample, system
For organic wet gel；
Organic wet gel is replaced Step 4: being added in deionized water using the sorbitan oleate of 15g/L, is replaced daily
It 1 time, replaces 5 times, organic wet gel is then put in progress constant pressure and dry at aeration-drying；
Step 5: suitable organic xerogel block is put into tubular type retort, after vacuumizing, in the protection of nitrogen atmosphere
Under, using 1000 DEG C of carbonization 180min；The xerogel block being carbonized is subjected to CO again2Activation, in CO21000 are used under atmosphere
DEG C activation 180min, wherein active rate is within the scope of 10ml/min-50ml/min.
The nanoporous carbon materials inexpensively prepared have nano-porous structure, density 0.32g/cm3, specific surface area is
872m2/g。
Embodiment 4
A kind of preparation method of nanoporous carbon materials, includes the following steps：
Step 1: at 35 DEG C, aqueous solution of the configuration containing template (lauryl sodium sulfate), uniform stirring, until
Template all dissolves, and solution, which becomes, to be clarified, and a concentration of 25.00 × 10-3mol/L。
Step 2: a certain amount of drug phloroglucin, melamine are added in the aqueous solution containing template, completely
Formaldehyde is added after dissolving, adds catalyst sodium bicarbonate solution, stirs evenly, forms colloidal sol, wherein Solute mass fraction is
30%, the molar ratio of phloroglucin, melamine and formaldehyde is 1：4：10, a concentration of 0.05mol/L of sodium bicarbonate solution,
The molar ratio of benzenetriol and sodium bicarbonate is 100；
Step 3: colloidal sol sealing is put into 85 DEG C of baking oven, handle 5 days, gel postcooling to room temperature takes out sample, system
For organic wet gel；
Organic wet gel is replaced Step 4: being added in deionized water using the sorbitan oleate of 15g/L, is replaced daily
It 1 time, replaces 3 times, organic wet gel is then put in progress constant pressure and dry at aeration-drying；
Step 5: suitable organic xerogel block is put into tubular type retort, after vacuumizing, in the protection of nitrogen atmosphere
Under, using 1000 DEG C of carbonization 180min；The xerogel block being carbonized is subjected to CO again2Activation, in CO21000 are used under atmosphere
DEG C activation 180min, wherein active rate is within the scope of 10ml/min-50ml/min.
The nanoporous carbon materials inexpensively prepared have nano-porous structure, density 0.66g/cm3, specific surface area is
248m2/g。
Claims (10)
1. a kind of preparation method of nanoporous carbon materials, which is characterized in that include the following steps：
(1) template is dissolved in aqueous solution, is uniformly mixing to obtain template aqueous solution；
(2) phloroglucin and melamine are added in template aqueous solution, formaldehyde is added after being completely dissolved, adds carbonic acid
Hydrogen sodium solution, stirs evenly, and forms colloidal sol；
(3) colloidal sol sealing is put into baking oven and is heat-treated, formed gel, be cooled to room temperature, obtain organic wet gel；
(4) organic wet gel is cleaned repeatedly in the deionized water solution of sorbitan oleate, constant pressure and dry, obtains later
Organic xerogel block；
(5) organic xerogel block is carbonized under nitrogen atmosphere, then the xerogel block being carbonized is subjected to CO2Activation, i.e.,
Obtain nanoporous carbon materials.
2. a kind of preparation method of nanoporous carbon materials according to claim 1, which is characterized in that step (1) is described
The one kind of template selected from neopelex, lauryl sodium sulfate or cetyl trimethylammonium bromide, template
A concentration of 0.006-0.028mol/L.
3. a kind of preparation method of nanoporous carbon materials according to claim 1, which is characterized in that step (2) is described
The molar ratio of phloroglucin, melamine and formaldehyde is 0.25-4：1：10.
4. a kind of preparation method of nanoporous carbon materials according to claim 1, which is characterized in that step (2) is described
A concentration of 0.04-0.06mol/L of sodium bicarbonate solution, mole of the phloroglucin and melamine mixing and sodium bicarbonate
Than for 50-300：1.
5. a kind of preparation method of nanoporous carbon materials according to claim 1, which is characterized in that step (2) formation
Colloidal sol in solute mass fraction be 10-40%.
6. a kind of preparation method of nanoporous carbon materials according to claim 1, which is characterized in that step (3) baking oven
Temperature be 80-90 DEG C, processing time be 3-5 days.
7. a kind of preparation method of nanoporous carbon materials according to claim 1, which is characterized in that step (4) is described
A concentration of 5-20g/L of sorbitan oleate, cleaning 4-8 times repeatedly, 1 time a day.
8. a kind of preparation method of nanoporous carbon materials according to claim 1, which is characterized in that step (5) is described
Carbonization is to carry out 2.5-3.5h in tubular type retort with 900-1100 DEG C of temperature, and hold with the rate of 200-400ml/min
It is continuous to be passed through nitrogen.
9. a kind of preparation method of nanoporous carbon materials according to claim 1, which is characterized in that step (5) is described
CO2Activation carries out 2.5-3.5h at 900-1100 DEG C, and is continually fed into CO with the rate of 10-50ml/min2Gas.
10. a kind of preparation method of nanoporous carbon materials according to claim 1, which is characterized in that be prepared
Nanoporous carbon materials have nano-porous structure, density 200-800mg/cm3, specific surface area 200-1200m2/g。
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Cited By (2)
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| CN114477171A (en) * | 2022-03-25 | 2022-05-13 | 愉悦家纺有限公司 | Porous electrode carbon, preparation method and application thereof |
| CN115261890A (en) * | 2022-09-26 | 2022-11-01 | 苏州仕净科技股份有限公司 | Method for preparing porous carbon material by electrochemically reducing carbon dioxide |
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