CN107117613A - A kind of preparation method of sulfur-bearing nitrogen activated carbon - Google Patents
A kind of preparation method of sulfur-bearing nitrogen activated carbon Download PDFInfo
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- CN107117613A CN107117613A CN201710468009.9A CN201710468009A CN107117613A CN 107117613 A CN107117613 A CN 107117613A CN 201710468009 A CN201710468009 A CN 201710468009A CN 107117613 A CN107117613 A CN 107117613A
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Abstract
A kind of preparation method of sulfur-bearing nitrogen activated carbon is by amine, aldehydes is added in reactor, pH value is adjusted between 89 with aqueous slkali, 50 DEG C 59 DEG C are warming up under stirring, the 30min of constant temperature 10, adds 1 3h that flowed back in above-mentioned solution by the phenols for being dissolved in absolute ethyl alcohol, is cooled to room temperature, vacuum drying removes remaining ethanol, then solidifies；In an inert atmosphere, carbonize, be 1 according to charing sample and alkali mass ratio:16, risen under inert atmosphere protection with 35 DEG C/min heating rate by room temperature and 1 3h is activated at 600 850 DEG C, naturally cooled to after room temperature, deionized water is washed till neutrality, sulfur-bearing nitrogen activated carbon is obtained after drying.The present invention has the advantages that in high-specific surface area, surface and body phase simultaneously containing nitrogen, sulphur.
Description
Technical field
The invention belongs to a kind of method for preparing sulfur and nitrogen co-doped activated carbon.
Background technology
Activated carbon is as a kind of carbonaceous porous material, because it has larger specific surface area, flourishing pore structure, surface
The multiple fields such as the advantages of chemical property is adjustable and being widely used in is adsorbed, be catalyzed, environmental protection.Hetero atom in activated carbon, such as oxygen,
Sulphur, nitrogen etc. can improve its absorption and chemical property to gas.Hetero atom in adjustment activated carbon is located after can using
The method of reason, Mangun et al. obtains the NACF that surface is rich in alkaline amido, the absorption to CO2 by using ammonia activation
Performance is improved（Carbon, 2001, 39, 1809-1820）.Another method is to use to contain heteroatomic presoma, and gold is small
It is beautiful etc.（Patent CN102360959A）Make raw material using the Lauxite rich in nitrogen, after raw material is carbonized under an inert atmosphere
Charing, activation prepare the activated carbon rich in nitrogen after being blended with potassium hydroxide.Liu Yongjun etc.（Patent CN105289686A）：Will
Powdered carbon, binding agent and hetero atom predecessor, which are put into kneader, to be mediated to uniform, extrusion forming, drying is sufficiently mixed, and high temperature is lived
The activated carbon of sulfur-bearing, nitrogen has been made after change.These above-mentioned methods can all influence the pore structure of activated carbon, or only in activated carbon surface
Increase hetero atom, and hetero atom used when post processing is not contained in activated carbon body phase, hetero atom are easy to run off.
Benzoxazine compares traditional phenolic resin or ammonia as a kind of new thermosetting, high performance resinamines
Base resin, has many advantages, such as.Nitrogenous activated carbon is prepared by presoma of benzoxazine colophony it has been reported that patent
CN102225996B, using phenol, aldehyde, amine as raw material, water is that solvent is prepared for being contained after benzoxazine colophony, then carbonization-activation
The activated carbon microballon of nitrogen.Patent CN105273188A provides a kind of self-catalysis preparation side of copolymerization benzoxazine colophony based carbon balls
Method, this method obtains corresponding charcoal ball after obtained copolymerization benzoxazine colophony high score bulbec is calcined.Patent
CN104925781B, CN104310396B are prepared for nitrogenous multistage mesoporous activated carbon for soft template with F127 etc. and are used for adsorbing
CO2Or it is used as electrode material.Nitrogen is comprised only in Carbon Materials prepared by the above method.And element sulphur can also be improved in activated carbon
The physicochemical properties of activated carbon（Carbon,2014,68,1-32）.Simultaneously containing nitrogen, sulphur activated carbon preparation method through retrieval
Have no report.
The content of the invention
It is an object of the invention to provide in a kind of high-specific surface area, surface and body phase simultaneously containing nitrogen, sulphur activated carbon
Preparation method.
The preparation method of the present invention comprises the following steps：
（1）By amine, aldehydes is added in reactor, is existed with 0.1M-0.9M potassium hydroxide or sodium hydroxide solution regulation pH value
Between 8-9,50 DEG C -59 DEG C are warming up under stirring, the phenols for being dissolved in ethanol is added in above-mentioned solution, stirred by constant temperature 10-30min
Lower backflow 1-3h is mixed, vacuum drying at room temperature, 30 DEG C -60 DEG C is cooled to and removes remaining ethanol, then at 110 DEG C -240 DEG C
Lower solidification 3-6h；
（2）In an inert atmosphere, by step（1）Sample rises to 600 DEG C -800 DEG C with 1-5 DEG C/min heating rate after solidification
Under, constant temperature charing 1-3h, Temperature fall is 1 according to charing sample and potassium hydroxide or sodium hydroxide mass ratio:1-6, will be carbonized
Sample is risen under inert atmosphere protection with potassium hydroxide or sodium hydrate solid with 3-5 DEG C/min heating rate by room temperature
1-3h is activated at 600-850 DEG C, is naturally cooled to after room temperature, deionized water is washed till neutrality, sulfur-bearing nitrogen activated carbon is obtained after drying.
Amine used is thiocarbamide, urea as described above；Aldehydes is formaldehyde, paraformaldehyde；Phenols is bisphenol S, thiobis benzene
Phenol, benzenethiol etc. are containing the one or more mixing in thiophenols.
Phenols as described above：Amine：Aldehydes：Absolute ethyl alcohol mol ratio is 1:1-2：1-6:10-20.
Advantages of the present invention is as follows：
1st, because this patent employs sulfur-bearing, the compound of nitrogen quantity is polymerize, therefore sulphur, nitrogen are also contained in gained polymers；Charing,
Sulphur nitrogen is all contained on the body phase of activity following activation charcoal and surface, and nitrogen content is between 12.7 wt%-25.9wt%, and sulfur content exists
Between 0.6wt%-1.1wt%.
2nd, the method that this patent employs chemical activation, the specific surface area of products obtained therefrom is in 1685-2439 m2Between/g,
Apparently higher than the performance of conventional physical activation products obtained therefrom.
Embodiment
Embodiment 1
According to mol ratio it is 1 by thiocarbamide and formaldehyde:4 add in reactor, are 8 with 0.1M potassium hydroxide solution regulation pH value,
Stirring is warming up to 50 DEG C, constant temperature 10min.By bisphenol S（It is 1 with thiocarbamide mol ratio：1）It is dissolved in the absolute ethyl alcohol of 10 times of moles
In, then add in above-mentioned reactor, the lower backflow 1h of stirring.It is down to after room temperature, is dried in vacuo at 30 DEG C, removes ethanol, so
Solidify 3h at 250 DEG C afterwards.In an inert atmosphere, sample after solidification is risen at 600 DEG C with 5 DEG C/min heating rate, it is permanent
Temperature charing 1h, Temperature fall.It is 1 according to charing sample and potassium hydroxide quality ratio:2, by charing sample and potassium hydroxide solid
Risen under inert atmosphere protection with 3 DEG C/min heating rate by room temperature at 700 DEG C and activate 1h, naturally cooled to after room temperature,
Deionized water is washed till neutrality, and sulfur-bearing nitrogen activated carbon is obtained after drying.Specific surface area 2038m2/ g, N content 18.7wt%, S content 0.9
wt%。
Embodiment 2
According to mol ratio it is 1 by thiocarbamide and formaldehyde:1 adds in reactor, with 0.9M potassium hydroxide solution regulation pH value be 9 it
Between, stirring is warming up to 59 DEG C, constant temperature 30min.By thio biphenol（It is 1 with thiocarbamide mol ratio：2）It is dissolved in the nothing of 20 times of moles
In water-ethanol, then add in above-mentioned reactor, the lower backflow 3h of stirring.It is down to after room temperature, is dried in vacuo at 60 DEG C, removes second
Alcohol, then solidifies 6h at 110 DEG C.In an inert atmosphere, sample after solidification is risen to 800 DEG C with 1 DEG C/min heating rate
Under, constant temperature charing 3h, Temperature fall.It is 1 according to charing sample and potassium hydroxide quality ratio:6, by charing sample and potassium hydroxide
Solid is risen at 850 DEG C by room temperature with 5 DEG C/min heating rate under inert atmosphere protection and activates 3h, naturally cools to room temperature
Afterwards, a large amount of deionized waters are washed till neutrality, and the activated carbon of sulfur-bearing nitrogen is obtained after drying.Specific surface area 2439m2/ g, N content 12.7wt%,
S contents 0.6wt%.
Embodiment 3
According to mol ratio it is 1 by urea and formaldehyde:6 add in reactor, are 8 with 0.5M potassium hydroxide solution regulation pH value,
Stirring is warming up to 55 DEG C, constant temperature 15min.By benzenethiol（It is 1 with urea mol ratio：1）It is dissolved in the absolute ethyl alcohol of 15 times of moles
In, then add in above-mentioned reactor, the lower backflow 1h of stirring.It is down to after room temperature, is dried in vacuo at 50 DEG C, removes ethanol, so
Solidify 3h at 200 DEG C afterwards.In an inert atmosphere, sample after solidification is risen at 700 DEG C with 3 DEG C/min heating rate, it is permanent
Temperature charing 2h, Temperature fall.It is 1 according to charing sample and sodium hydroxide mass ratio:3, by charing sample and sodium hydrate solid
Risen under inert atmosphere protection with 5 DEG C/min heating rate by room temperature at 600 DEG C and activate 3h, naturally cooled to after room temperature,
A large amount of deionized waters are washed till neutrality, and the activated carbon of sulfur-bearing nitrogen is obtained after drying.Specific surface area 1685m2/ g, N content 20.9wt%, S contain
Measure 0.94wt%.
Embodiment 4
According to mol ratio it is 1 by sulphur urine and formaldehyde:4 add in reactor, are 9 with 0.5M sodium hydroxide solution regulation pH value,
Stirring is warming up to 55 DEG C, constant temperature 15min.By thio biphenol（It is 1 with thiocarbamide mol ratio：1）It is dissolved in the anhydrous of 20 times of moles
In ethanol, then add in above-mentioned reactor, the lower backflow 2h of stirring.It is down to after room temperature, is dried in vacuo at 40 DEG C, removes second
Alcohol, then solidifies 3h at 180 DEG C.In an inert atmosphere, sample after solidification is risen to 700 DEG C with 3 DEG C/min heating rate
Under, constant temperature charing 1h, Temperature fall.It is 1 according to charing sample and potassium hydroxide quality ratio:1, by charing sample and potassium hydroxide
Solid is risen at 700 DEG C by room temperature with 3 DEG C/min heating rate under inert atmosphere protection and activates 3h, naturally cools to room temperature
Afterwards, a large amount of deionized waters are washed till neutrality, and the activated carbon of sulfur-bearing nitrogen is obtained after drying.Specific surface area 1751m2/ g, N content 22.9wt%,
S contents 0.83wt%.
Embodiment 5
According to mol ratio it is 1 by sulphur urine and paraformaldehyde:3 are added in reactor, and pH value is adjusted with 0.5M potassium hydroxide solution
For 9, stirring is warming up to 59 DEG C, constant temperature 15min.By thio biphenol（It is 1 with thiocarbamide mol ratio：2）It is dissolved in 20 times of moles
In absolute ethyl alcohol, then add in above-mentioned reactor, the lower backflow 3h of stirring.It is down to after room temperature, is dried in vacuo at 50 DEG C, is removed
Ethanol, then solidifies 6h at 250 DEG C.In an inert atmosphere, sample after solidification is risen to 600 with 3 DEG C/min heating rate
At DEG C, constant temperature charing 1h, Temperature fall.It is 1 according to charing sample and potassium hydroxide quality ratio:2, by charing sample and hydroxide
Potassium solid is risen at 700 DEG C by room temperature with 3 DEG C/min heating rate under inert atmosphere protection and activates 1h, naturally cools to room
Wen Hou, a large amount of deionized waters are washed till neutrality, and the activated carbon of sulfur-bearing nitrogen is obtained after drying.Specific surface area 2372m2/ g, N content
25.9wt%, S content 1.1wt%.
Embodiment 6
According to mol ratio it is 1 by sulphur urine and formaldehyde:4 add in reactor, are with 0.8M potassium hydroxide solution regulation pH value
8.7, stirring is warming up to 59 DEG C, constant temperature 30min.By bisphenol S（It is 1 with thiocarbamide mol ratio：1）It is dissolved in the anhydrous second of 17 times of moles
In alcohol, then add in above-mentioned reactor, the lower backflow 2h of stirring.It is down to after room temperature, is dried in vacuo at 40 DEG C, removes ethanol,
Then 6h is solidified at 230 DEG C.In an inert atmosphere, sample after solidification is risen at 700 DEG C with 2 DEG C/min heating rate,
Constant temperature carbonizes 2h, Temperature fall.It is 1 according to charing sample and potassium hydroxide quality ratio:2, charing sample is consolidated with potassium hydroxide
Body is risen at 800 DEG C by room temperature with 3 DEG C/min heating rate under inert atmosphere protection and activates 1h, naturally cools to room temperature
Afterwards, a large amount of deionized waters are washed till neutrality, and the activated carbon of sulfur-bearing nitrogen is obtained after drying.Specific surface area 2006m2/ g, N content 20.7wt%,
S contents 0.76wt%.
Embodiment 7
According to mol ratio it is 1 by urea and paraformaldehyde:3 are added in reactor, and pH value is adjusted with 0.5M potassium hydroxide solution
For 8.3, stirring is warming up to 50 DEG C, constant temperature 10min.By bisphenol S（It is 1 with urea mol ratio：2）It is dissolved in the anhydrous of 13 times of moles
In ethanol, then add in above-mentioned reactor, the lower backflow 2h of stirring.It is down to after room temperature, is dried in vacuo at 40 DEG C, removes second
Alcohol, then solidifies 5h at 210 DEG C.In an inert atmosphere, sample after solidification is risen to 750 DEG C with 3 DEG C/min heating rate
Under, constant temperature charing 1h, Temperature fall.It is 1 according to charing sample and sodium hydroxide mass ratio:3, by charing sample and sodium hydroxide
Solid is risen at 700 DEG C by room temperature with 4 DEG C/min heating rate under inert atmosphere protection and activates 2h, naturally cools to room temperature
Afterwards, a large amount of deionized waters are washed till neutrality, and the activated carbon of sulfur-bearing nitrogen is obtained after drying.Specific surface area 1978m2/ g, N content 18.6wt%,
S contents 0.85wt%.
Embodiment 8
According to mol ratio it is 1 by sulphur urine and paraformaldehyde:5 are added in reactor, and pH value is adjusted with 0.5M potassium hydroxide solution
For 8.5, stirring is warming up to 40 DEG C, constant temperature 30min.By benzenethiol（It is 1 with thiocarbamide mol ratio：1）It is dissolved in the nothing of 17 times of moles
In water-ethanol, then add in above-mentioned reactor, the lower backflow 3h of stirring.It is down to after room temperature, is dried in vacuo at 58 DEG C, removes second
Alcohol, then solidifies 6h at 200 DEG C.In an inert atmosphere, sample after solidification is risen to 700 DEG C with 3 DEG C/min heating rate
Under, constant temperature charing 3h, Temperature fall.It is 1 according to charing sample and sodium hydroxide mass ratio:5, by charing sample and sodium hydroxide
Solid is risen at 750 DEG C by room temperature with 4 DEG C/min heating rate under inert atmosphere protection and activates 2h, naturally cools to room temperature
Afterwards, a large amount of deionized waters are washed till neutrality, and the activated carbon of sulfur-bearing nitrogen is obtained after drying.Specific surface area 2012m2/ g, N content 20.4wt%,
S contents 1.1wt%.
Embodiment described above is only the preferred embodiments of the present invention, and the simultaneously exhaustion of the feasible implementation of non-invention.It is right
For persons skilled in the art, any aobvious to made by it on the premise of without departing substantially from the principle of the invention and spirit and
Within the change being clear to, the claims that should be all contemplated as falling with the present invention.
Claims (5)
1. a kind of preparation method of sulfur-bearing nitrogen activated carbon, it is characterised in that comprise the following steps：
（1）By amine, aldehydes is added in reactor, is existed with 0.1M-0.9M potassium hydroxide or sodium hydroxide solution regulation pH value
Between 8-9,50 DEG C -59 DEG C are warming up under stirring, the phenols for being dissolved in absolute ethyl alcohol is added above-mentioned solution by constant temperature 10-30min
In, the lower backflow 1-3h of stirring is cooled to vacuum drying at room temperature, 30 DEG C -60 DEG C and removes remaining ethanol, then 110 DEG C -
Solidify 3-6h at 240 DEG C；
（2）In an inert atmosphere, by step（1）Sample rises to 600 DEG C -800 DEG C with 1-5 DEG C/min heating rate after solidification
Under, constant temperature charing 1-3h, Temperature fall is 1 according to charing sample and potassium hydroxide or sodium hydroxide mass ratio:1-6, will be carbonized
Sample rises to 600- with 3-5 DEG C/min heating rate under inert atmosphere protection with potassium hydroxide or sodium hydroxide by room temperature
1-3h is activated at 850 DEG C, is naturally cooled to after room temperature, deionized water is washed till neutrality, sulfur-bearing nitrogen activated carbon is obtained after drying.
2. a kind of preparation method of sulfur-bearing nitrogen activated carbon as claimed in claim 1, it is characterised in that the amine be thiocarbamide or
Urea.
3. a kind of preparation method of sulfur-bearing nitrogen activated carbon as claimed in claim 1, it is characterised in that the aldehydes be formaldehyde or
Paraformaldehyde.
4. a kind of preparation method of sulfur-bearing nitrogen activated carbon as claimed in claim 1, it is characterised in that the phenols be bisphenol S or
One or several kinds in thio biphenol, benzenethiol.
5. a kind of preparation method of sulfur-bearing nitrogen activated carbon as claimed in claim 1, it is characterised in that the phenols：Amine
Class：Aldehydes：Absolute ethyl alcohol mol ratio is 1:1-2：1-6:10-20.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109748279A (en) * | 2019-02-21 | 2019-05-14 | 南京大学 | One kind is based on poromeric micro-pore carbon material of benzoxazine and its preparation method and application |
| CN111554519A (en) * | 2020-05-13 | 2020-08-18 | 陈志林 | α -Bi2O3Carbon material-loaded supercapacitor electrode material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925781A (en) * | 2015-06-09 | 2015-09-23 | 中国科学院山西煤炭化学研究所 | Preparation method of level hole charcoal rich in nitrogen with high CO2 yield and specific capacitance |
| CN105948045A (en) * | 2016-07-18 | 2016-09-21 | 湘潭大学 | Preparation method and application of nitrogen-doped starch-based activated carbon microsphere material |
-
2017
- 2017-06-20 CN CN201710468009.9A patent/CN107117613B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925781A (en) * | 2015-06-09 | 2015-09-23 | 中国科学院山西煤炭化学研究所 | Preparation method of level hole charcoal rich in nitrogen with high CO2 yield and specific capacitance |
| CN105948045A (en) * | 2016-07-18 | 2016-09-21 | 湘潭大学 | Preparation method and application of nitrogen-doped starch-based activated carbon microsphere material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109748279A (en) * | 2019-02-21 | 2019-05-14 | 南京大学 | One kind is based on poromeric micro-pore carbon material of benzoxazine and its preparation method and application |
| CN111554519A (en) * | 2020-05-13 | 2020-08-18 | 陈志林 | α -Bi2O3Carbon material-loaded supercapacitor electrode material and preparation method thereof |
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| CN107117613B (en) | 2019-06-25 |
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