CN105110320A - Preparation method of graphene porous material used for flue gas adsorption - Google Patents
Preparation method of graphene porous material used for flue gas adsorption Download PDFInfo
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- CN105110320A CN105110320A CN201510439103.2A CN201510439103A CN105110320A CN 105110320 A CN105110320 A CN 105110320A CN 201510439103 A CN201510439103 A CN 201510439103A CN 105110320 A CN105110320 A CN 105110320A
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Abstract
The invention relates to a preparation method of an adsorption material, and more specifically relates to a preparation method of a graphene porous material used for flue gas adsorption. According to the preparation method, ultrasonic treatment is adopted so as to obtain an oxidized graphene aqueous solution; the oxidized graphene aqueous solution is subjected to freeze drying and thermal reduction so as to obtain the graphene porous material. The preparation method is simple; operation is convenient; the resource of the raw materials is wide; no environmental pollution is caused in preparation processes; the preparation method is friendly to the environment; the surface structure and the internal structure of the graphene porous material are three-dimensional and porous; and the specific surface area and porosity are high.
Description
[technical field]
The present invention relates to a kind of sorbing material and preparation method thereof, specifically relate to a kind of preparation method of flue gas absorption Graphene porous material.
[background technology]
Nano-porous materials is as a kind of type material, it has the characteristics such as high porosity, high-specific surface area, unique mechanics, optics and electricity, and these characteristics make nano-porous materials play huge effect in various fields such as Materials science research and the developments of the national economy.
In numerous nano-porous materials, carbon-based material is a most widely used general and of paramount importance polyporous materials.Graphene, as novel nano-carbon material, has excellent mechanics, calorifics and electric property, has very wide application prospect.Common Graphene exists with the graphene powder form of micron order laminated structure.Simultaneously because graphene film interlayer is easily assembled, be difficult to manipulation in actual applications, cause the assembly based on Graphene to be difficult to obtain larger specific surface area, be more difficult to the theoretical specific surface area value 2630m reaching Graphene
2/ g, greatly hinders the application of Graphene as sorbing material.Therefore the Graphene of microcosmic is assembled into the graphene macroform with three-dimensional network shape vesicular structure, at the proper property macroscopically showing again porous material while making it have the essential characteristic of nano material on microcosmic, tool is of great significance.
At present about porous graphene acquisition pattern carries out chemical activation mainly through using sodium hydroxide under high temperature and inert atmosphere to Graphene, thus obtain porous graphene material, but the method complex process, wayward, obtained porous graphene material aperture narrow range, and foreign matter content is higher, specific surface area is low.
[summary of the invention]
The object of the present invention is to provide a kind of preparation method of flue gas absorption Graphene porous material, technique is simple, easy to operate, simultaneously by the adjustment experiment condition such as Heating temperature and time, carries out autotelic control to the porosity of Graphene porous material; It is large that the Graphene porous material adopting preparation method provided by the invention to obtain has specific surface area, porosity high.
The present invention is by the following technical solutions for achieving the above object:
The invention provides a kind of preparation method of flue gas absorption Graphene porous material, comprise the steps:
1) the supersound process graphene oxide of 20 ~ 25kHz is made into the aqueous solution 10 ~ 40min;
2) lyophilize step 1) treatment solution that obtains carries out, and obtains graphene oxide porous material;
3) thermal reduction step 2) graphene oxide porous material, obtain Graphene porous material.
Preparation method's step 1 provided by the invention) in, the concentration of graphene oxide is 5 ~ 20g/L.
Preparation method's step 1 provided by the invention) in, ultrasonic time is 15 ~ 30min.
Preparation process 1 provided by the invention) in, ultrasonic frequency is 25kHz.
Preparation method's step 2 provided by the invention) in, lyophilize is vacuum lyophilization, and temperature is-50 DEG C ~-15 DEG C, vacuum tightness < 10Pa.
Preparation method's step 2 provided by the invention) in, the cryodesiccated time is 2 ~ 5d.
Preparation method's step 3 provided by the invention) in, thermal reduction is atmosphere furnace thermal reduction, and temperature is 550 ~ 800 DEG C, and atmosphere is argon gas or nitrogen, and the treatment time is 2 ~ 4h.
The porosity of the Graphene porous material that preparation method provided by the invention obtains is 85 ~ 99%.
The specific surface area of the Graphene porous material that preparation method provided by the invention obtains is 500 ~ 900m
2/ g.
The Graphene porous material that preparation method provided by the invention obtains for adsorbing phenol, Resorcinol, citral, formic acid. acetic acid, butyric acid, positive valeric acid, isovaleric acid, palmitinic acid, linolenic acid, pyridine or pyrroles.
With immediate prior art ratio, technical scheme provided by the invention has following beneficial effect:
1, the invention provides preparation method and by the adjustment experiment condition such as Heating temperature and time, autotelic control can be carried out to the porosity of Graphene porous material;
2, preparation method's technique provided by the invention is simple, easily operates, and the raw material sources utilized is extensive, non-environmental-pollution in preparation process, technique environmental protection;
3, the macro-size size of the Graphene porous material of preparation method's acquisition provided by the invention is controlled, can be mass-produced;
4, the Graphene porous material that obtains of preparation method provided by the invention, surface and internal structure all present three-dimensional, vesicular, have high specific surface area.
[accompanying drawing explanation]
Fig. 1 is that Graphene porous material provided by the invention is to citral adsorption curve.
[embodiment]
With each embodiment, the present invention is described in further details below.
Embodiment 1
Be after the graphene oxide solution 25kHz supersound process 30min of 10g/L by concentration, at-15 DEG C, carry out lyophilize 5 days, be heated to 800 DEG C in a nitrogen atmosphere subsequently, constant temperature 5 days.Obtain Graphene porous material, porosity is 95%, and specific surface area is 856m
2/ g.
At room temperature measure this Graphene porous material to the equilibrium adsorption capacity of the saturated vapo(u)r of citral solution over time.Find through test, this Graphene porous material is 24.08g/g to the adsorptive capacity of citral.
Embodiment 2
Be after the graphene oxide solution 20kHz supersound process 15min of 6g/L by concentration, at-50 DEG C, carry out lyophilize 3 days, be heated to 650 DEG C under an argon atmosphere subsequently, constant temperature 3 days.Obtain Graphene porous material, porosity is 90%, and specific surface area is 768m
2/ g.
At room temperature measure this Graphene porous material to the equilibrium adsorption capacity of the saturated vapo(u)r of formic acid solution over time.Find through test, this Graphene porous material is 20.56g/g to the adsorptive capacity of formic acid.
Embodiment 3
Be after the graphene oxide solution supersound process 20min of 12g/L by concentration, at-45 DEG C, carry out lyophilize 4 days, be heated to 700 DEG C in a nitrogen atmosphere subsequently, constant temperature 2 days.Obtain Graphene porous material, porosity is 87%, and specific surface area is 645m
2/ g.
At room temperature measure this Graphene porous material to the equilibrium adsorption capacity of the saturated vapo(u)r of acetic acid solution over time.Find through test, this Graphene porous material is 15.52g/g to the adsorptive capacity of acetic acid.
Embodiment 4
Be after the graphene oxide solution supersound process 30min of 10g/L by concentration, at-25 DEG C, carry out lyophilize 3 days, be heated to 750 DEG C in a nitrogen atmosphere subsequently, constant temperature 4 days.Obtain Graphene porous material, porosity is 94%, and specific surface area is 733m
2/ g.
At room temperature measure this Graphene porous material to the equilibrium adsorption capacity of the saturated vapo(u)r of pyridine solution over time.Find through test, this Graphene porous material is 16.85g/g to the adsorptive capacity of pyridine.
Embodiment 5
Be after the graphene oxide solution supersound process 20min of 5g/L by concentration, at-35 DEG C, carry out lyophilize 5 days, be heated to 650 DEG C in a nitrogen atmosphere subsequently, constant temperature 4 days.Obtain Graphene porous material, porosity is 86%, and specific surface area is 611m
2/ g.
At room temperature measure this Graphene porous material to the equilibrium adsorption capacity of the saturated vapo(u)r of citral solution over time.Find through test, this Graphene porous material is 18.34g/g to the adsorptive capacity of citral.
Embodiment 6
Be after the graphene oxide solution supersound process 20min of 8g/L by concentration, at-30 DEG C, carry out lyophilize 2 days, be heated to 550 DEG C in a nitrogen atmosphere subsequently, constant temperature 2 days.Obtain Graphene porous material, porosity is 91%, and specific surface area is 789m
2/ g.
At room temperature measure this Graphene porous material and align the equilibrium adsorption capacity of the saturated vapo(u)r of valeric acid solution over time.Find through test, the adsorptive capacity that this Graphene porous material aligns valeric acid is 12.90g/g.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; those of ordinary skill in the field are to be understood that; can modify to the specific embodiment of the present invention with reference to above-described embodiment or equivalent replacement; these do not depart from any amendment of spirit and scope of the invention or equivalent replacement, and it all should be encompassed within claims of the present invention.
Claims (10)
1. a flue gas absorption preparation method for Graphene porous material, described preparation method comprises the steps:
1) the supersound process graphene oxide of 20 ~ 25kHz is made into the aqueous solution 10 ~ 40min;
2) lyophilize step 1) treatment solution that obtains carries out, and obtains graphene oxide porous material;
3) thermal reduction step 2) graphene oxide porous material, obtain described Graphene porous material.
2. preparation method according to claim 1, is characterized in that step 1) described in the concentration of graphene oxide be 5 ~ 20g/L.
3. preparation method according to claim 1, is characterized in that step 1) described in ultrasonic time be 15 ~ 30min.
4. preparation method according to claim 1, is characterized in that step 1) described in ultrasonic frequency be 25kHz.
5. preparation method according to claim 1, is characterized in that step 2) described in lyophilize be vacuum lyophilization, temperature is-50 DEG C ~-15 DEG C, vacuum tightness < 10Pa.
6. preparation method according to claim 1, is characterized in that step 2) described in the cryodesiccated time be 2 ~ 5d.
7. preparation method according to claim 1, is characterized in that step 3) described in thermal reduction be atmosphere furnace thermal reduction, temperature is 550 ~ 800 DEG C, and atmosphere is argon gas or nitrogen, and the treatment time is 2 ~ 4h.
8. preparation method according to claim 1, is characterized in that the porosity of the Graphene porous material that described preparation method obtains is 85 ~ 99%.
9. preparation method according to claim 1, is characterized in that the specific surface area of the Graphene porous material that described preparation method obtains is 500 ~ 900m
2/ g.
10. preparation method according to claim 1, is characterized in that Graphene porous material that described preparation method obtains is for adsorbing phenol, Resorcinol, citral, formic acid, acetic acid, butyric acid, positive valeric acid, isovaleric acid, palmitinic acid, linolenic acid, pyridine or pyrroles.
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Cited By (1)
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| CN105967181A (en) * | 2016-07-21 | 2016-09-28 | 苏州协鑫集成科技工业应用研究院有限公司 | Graphene and preparation method thereof |
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