CN108394882A - A kind of ultralight porous carbon materials and preparation method thereof - Google Patents
A kind of ultralight porous carbon materials and preparation method thereof Download PDFInfo
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
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Abstract
The present invention relates to a kind of ultralight porous carbon materials and preparation method thereof, it is 2000~2500m that the ultralight porous carbon materials, which have the microcellular structure that the macroporous structure that aperture is 50~300nm and the meso-hole structure that aperture is 2~50nm and aperture are less than 2nm, specific surface area,2/g；And the preparation method of the porous carbon materials is disclosed, ultralight porous carbon of the present invention has three-level pore passage structure, improves absorption, separation, column packing, catalytic performance；And can carried metal, metal component is evenly distributed, can effectively be regulated and controled to material property；Ultralight porous carbon materials preparation process of the present invention is easy to operate, low for equipment requirements, industrially applicable and height universality.
Description
Technical field
The invention belongs to ultralight carbon material fields, and in particular to a kind of ultralight porous carbon materials and preparation method thereof.
Background technology
Porous carbon materials refer to the carbon materials for having Different Pore Structures, and hole size is from being equivalent to molecular size
Nanometer ultrafine micropore has the mesoporous and macropore knot more than 50nm of the micropore, 2-50nm that are less than 2nm until micron order pore
Structure.Porous carbon materials have high-specific surface area, high porosity, good electric conductivity and thermal conductivity, regulatable aperture and superficiality
Can, it is widely used in fields such as catalyst carrier, ultracapacitor, catalyst, adsorbent and gas storages.Porous carbon materials
Synthetic method mainly have hard template method, soft template method etc., but these methods often exist of high cost, synthesis technology it is complicated or
The relatively low problem of purity, hinders the broader applications of porous carbon materials.
Numerous in Chinese population, rice husk, bark and discarded tealeaves etc. are common low value energy resources, are either existed
Field is burned or is abandoned, and pollutes the environment and destroys, and the method for efficiently using biomass production activated carbon will be to me
Economy, environment and the social concern of state generate significant impact；Currently, still without a kind of known method, general that can be simple and quick
Low value energy conversion is ultralight porous carbon materials, and loads a variety of different metals or metal oxide well, is obtained
Large specific surface area, the metal of separation and concentration excellent catalytic effect or metal oxide supported ultralight porous carbon materials.
Invention content
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of ultralight porous carbon materials and preparation method thereof.
In order to achieve the above objectives, the present invention is realized according to following technical solution：
It is 2~50nm that ultralight porous carbon materials of the present invention, which have the macroporous structure that aperture is 50~300nm and aperture,
Meso-hole structure and aperture be less than the microcellular structure of 2nm, the specific surface areas of the ultralight porous carbon materials is 2000~
2500m2/g。
Further, the ultralight porous carbon materials load has metal, the metal to account for the ultralight porous carbon materials
Mass ratio is 0.5%~3%, and the metallic particles grain size is 2~20nm.
Further, the metal is any one in Au, Ag, Pt, Pd.
The preparation method of ultralight porous carbon materials of the present invention, includes the following steps：
1) exodermis of pomelo peel is removed, is freeze-dried；
2) in parts by weight, by 100~2000 parts of pomelo peel, 70000 parts of water is added in hydrothermal reaction kettle, is heated to
160 DEG C~200 DEG C, react 20~30h；
3) by 2) gained reaction product filtering, dry, by the product after drying according to every gram of 15~20ml of addition 6~
The KOH solution of 8mol/L is impregnated, and soaking time is 15~25h, is then filtered, then be dried.
4) 3) product obtained is roasted under the conditions of non-oxidizing atmosphere, calcination temperature is 700 DEG C~900 DEG C, roasting
Time is 2~5h, and the product after roasting is impregnated 20~25h using acid solution, is then filtered and is cleaned with deionized water
It is in neutrality to filtrate, then is dried under the conditions of 60 DEG C~70 DEG C.
Further, in the step 1), freezing dry process includes：The pomelo peel of exodermis will first be removed in 20 DEG C of ﹣
Under the conditions of 30 DEG C of~﹣, 100MT, 90~150min is preserved；Then under the conditions of 20 DEG C of 10 DEG C~﹣ of ﹣, 100MT, preservation 300~
500min；Again under the conditions of 10 DEG C of 2 DEG C~﹣ of ﹣, 100MT, 300~500min is preserved；Finally in 20 DEG C~40 DEG C, 20MT conditions
Under, preserve 200~500min.
Further, in the step 4), the hydrochloric acid solution that acid solution is 2%~10%, and hydrochloric acid solution and roasting
The mass ratio of product afterwards is 50:1~80: 1.
The another preparation method of ultralight porous carbon materials of the present invention, includes the following steps：
1) exodermis of pomelo peel is removed, is freeze-dried；
2) in parts by weight, by 5~10 parts of loading metal-salt, 100~2000 parts of pomelo peel, 70000 parts of water is added to
In hydrothermal reaction kettle, 160 DEG C~200 DEG C are heated to, reacts 20~30h；
3) by 2) gained reaction product filtering, dry, by the product after drying according to every gram of 15~20ml of addition 6~
The KOH solution of 8mol/L is impregnated, and soaking time is 15~25h, is then filtered, then be dried.
4) 3) product obtained is roasted under the conditions of non-oxidizing atmosphere, calcination temperature is 700 DEG C~900 DEG C, roasting
Time is 2~5h, and the product after roasting is impregnated 20~25h using acid solution, is then filtered and is cleaned with deionized water
It is in neutrality to filtrate, then is dried under the conditions of 60 DEG C~70 DEG C.
Further, in the step 1), freezing dry process includes：The pomelo peel of exodermis will first be removed in 20 DEG C of ﹣
Under the conditions of 30 DEG C of~﹣, 100MT, 90~150min is preserved；Then under the conditions of 20 DEG C of 10 DEG C~﹣ of ﹣, 100MT, preservation 300~
500min；Again under the conditions of 10 DEG C of 2 DEG C~﹣ of ﹣, 100MT, 300~500min is preserved；Finally in 20 DEG C~40 DEG C, 20MT conditions
Under, preserve 200~500min.
Further, in the step 2), loading metal-salt is arbitrary in gold chloride, silver nitrate, chloroplatinic acid, palladium bichloride
It is a kind of.
Further, in the step 4), the hydrochloric acid solution that acid solution is 2%~10%, and hydrochloric acid solution and roasting
The mass ratio of product afterwards is 50:1~80: 1.
Beneficial effects of the present invention are：
1. ultralight porous carbon materials of the present invention have very big specific surface area, and have three-level pore passage structure,
Improve the performances such as absorption, separation, column packing, catalysis.
2. ultralight porous carbon materials of the present invention realize that the load of a variety of different metal components, metal component distribution are equal
It is even, material property can effectively be regulated and controled.
3. ultralight porous carbon materials preparation process of the present invention is easy to operate, low for equipment requirements, have industry practical
Property.
4. being participated in jointly instead by pomelo peel and metal precursor in ultralight porous carbon preparation method for material of the present invention
It answers, the material after being loaded, metal component is evenly distributed, and grain graininess is small.
5. ultralight porous carbon preparation method for material of the present invention has environmentally protective meaning, the universality with height.
Description of the drawings
Fig. 1 is the SEM figures for the ultralight porous carbon materials that embodiment 3 synthesizes.
Fig. 2 is the TEM figures for the ultralight porous carbon materials that embodiment 3 synthesizes.
Fig. 3 is the ultralight porous carbon materials isothermal adsorption-desorption curve figure that embodiment 3 synthesizes.
Fig. 4 is the Raman spectrogram for the ultralight porous carbon materials that embodiment 3 synthesizes.
Fig. 5 is saturated extent of adsorption result figure of the ultralight porous carbon materials to dyestuff and heavy metal of the synthesis of embodiment 3.
Fig. 6 is the SEM figures for the ultralight porous carbon materials that embodiment 4 synthesizes.
Fig. 7 is the TEM figures for the ultralight porous carbon materials that embodiment 4 synthesizes.
Fig. 8 is the XRD spectrum for the ultralight porous carbon materials that embodiment 4 synthesizes.
Fig. 9 is the catalytic effect collection of illustrative plates for the ultralight porous carbon materials that embodiment 4~7 is respectively synthesized.
Specific implementation mode
Following accompanying drawings and specific embodiment, are described in further detail technical solution of the present invention.
Embodiment 1：
It is 2~50nm that ultralight porous carbon materials of the present invention, which have the macroporous structure that aperture is 50~300nm and aperture,
Meso-hole structure and aperture be less than the microcellular structure of 2nm, the specific surface areas of the ultralight porous carbon materials is 2000~
2500m2/g。
Embodiment 2：
On the basis of embodiment 1, the ultralight porous carbon materials load has metal, the metal to account for described ultralight porous
The mass ratio of carbon material is 0.5%~3%, and the metallic particles grain size is 2~20nm.
Further, the metal is any one in Au, Ag, Pt, Pd.
Embodiment 3：
The preparation method of ultralight porous carbon materials, includes the following steps described in the embodiment of the present invention 1：
1) exodermis of pomelo peel is removed, is fitted into freeze drier, first in 25 DEG C of ﹣, under the conditions of 100MT, preserved
120min；Then in 15 DEG C of ﹣, under the conditions of 100MT, 400min is preserved；Again in 5 DEG C of ﹣, under the conditions of 100MT, 400min is preserved；Most
Afterwards at 30 DEG C, under the conditions of 20MT, 400min is preserved；
2) it takes the pomelo peel in 1.5g steps 1) to be added in the hydrothermal reaction kettle of 100ml with 70ml deionized waters, heats
To 180 DEG C, reaction for 24 hours, is cooled to room temperature；
3) by 2) filtering of gained reaction product, drying, the product after drying is carried out with the KOH solution of the 7mol/L of 25ml
It impregnates, then soaking time 20h is filtered, then is dried；
4) 3) product obtained is placed in tube furnace and 3h rises to 800 DEG C in a nitrogen atmosphere, kept 2h, be cooled to room
Temperature impregnates 5% hydrochloric acid solution of 40ml of the product after roasting for 24 hours, be then filtered and with deionized water clean to
Filtrate is in neutrality, then is dried under the conditions of 60 DEG C and obtains ultralight porous carbon materials.
Ultralight porous carbon materials made from 3 preparation method of the embodiment of the present invention measure average through nitrogen adsorption-detachment assays
Aperture is 3.0nm, specific surface area 2479m2/g；And by Fig. 1, Fig. 2, Fig. 3, Fig. 4 it is found that material prepared by the embodiment of the present invention 3
Material is ultralight porous carbon materials.
Ultralight porous carbon materials 50mg made from 3 preparation method of embodiment is chosen, 50mg is implemented into ultralight porous carbon materials
It is separately added into the rhodamine B of 100mL500mg/L, methyl orange, rhodamine 6G, plumbi nitras, cadmium nitrate, chromium nitrate solution, room temperature
For 24 hours, the content of dyestuff and heavy metal obtains the ultralight porous carbon materials and satisfies to dyestuff and heavy metal in test solution for stirring
And adsorbance, as shown in figure 5, simultaneously as shown in Figure 5, the ultralight porous carbon materials have superpower absorption to fuel and heavy metal
Ability.
Embodiment 4：
The preparation method of ultralight porous carbon materials, includes the following steps described in the embodiment of the present invention 2：
1) exodermis of pomelo peel is removed, is fitted into freeze drier, first in 30 DEG C of ﹣, under the conditions of 100MT, preserved
140min；Then in 15 DEG C of ﹣, under the conditions of 100MT, 500min is preserved；Again in 5 DEG C of ﹣, under the conditions of 100MT, 500min is preserved；Most
Afterwards at 30 DEG C, under the conditions of 20MT, 500min is preserved；
2) pomelo peel in 1.5g steps 1), the aqueous solution of chloraurate and 69ml deionized waters of the 10g/L of 1mL is taken to be added to
In the hydrothermal reaction kettle of 100ml, 180 DEG C are heated to, 22h is reacted, is cooled to room temperature；
3) by 2) filtering of gained reaction product, drying, the product after drying is carried out with the KOH solution of the 7mol/L of 20ml
It impregnates, then soaking time 20h is filtered, then is dried；
4) 3) product obtained is placed in tube furnace and 3h rises to 800 DEG C in a nitrogen atmosphere, kept 2h, be cooled to room
Product after roasting 5% hydrochloric acid solution of 40ml is impregnated 20h by temperature, be then filtered and with deionized water clean to
Filtrate is in neutrality, then the ultralight porous carbon materials for obtaining load Au are dried under the conditions of 60 DEG C.
EDS tests are carried out to the ultralight porous carbon materials made from the embodiment of the present invention 4, test result is as shown in table 1：
Table 1
| Element | Atomic percent |
| C K | 96.10 |
| O K | 3.64 |
| Au M | 0.26 |
| Total amount | 100 |
The ultralight porous carbon materials prepared by the embodiment of the present invention 4 measure average pore size through nitrogen adsorption-detachment assays
For 2.9nm, specific surface area 2036m2/g；And by Fig. 6, Fig. 7, Fig. 8 it is found that material prepared by the embodiment of the present invention 4 is ultralight
Porous carbon materials.
Embodiment 5：
The present embodiment method is substantially the same manner as Example 4, the difference is that only in step 2) gold chloride being substituted for nitre
Sour silver.
Embodiment 6：
The present embodiment method is substantially the same manner as Example 4, the difference is that only in step 2) gold chloride being substituted for chlorine
Platinic acid.
Embodiment 7：
The present embodiment method is substantially the same manner as Example 4, the difference is that only in step 2) gold chloride being substituted for chlorine
Change palladium.
The porous carbon materials 1mg, the 4-NP of 2.9mL0.2mM, 0.1ml that the embodiment of the present invention 4~7 is prepared respectively
The NaHB solution of 0.3M, which is placed in cuvette, carries out catalytic performance test, is tested the concentration of 4-NP in solution per 2min,
Test results are shown in figure 9, and as shown in Figure 9, the porous carbon materials that the embodiment of the present invention 4~7 is prepared respectively have very
Good catalytic effect.
Present invention is not limited to the embodiments described above, without departing substantially from substantive content of the present invention, art technology
Any deformation, improvement, the replacement that personnel are contemplated that each fall within protection scope of the present invention.
Claims (10)
1. a kind of ultralight porous carbon materials, which is characterized in that it is the big of 50~300nm that the ultralight porous carbon materials, which have aperture,
Pore structure and the microcellular structure of meso-hole structure and aperture less than 2nm that aperture is 2~50nm, the ultralight porous carbon materials
Specific surface area is 2000~2500m2/g。
2. ultralight porous carbon materials according to claim 1, which is characterized in that the ultralight porous carbon materials load has gold
Belong to, the mass ratio that the metal accounts for the ultralight porous carbon materials is 0.5%~3%.
3. ultralight porous carbon materials according to claim 3, which is characterized in that the metal is in Au, Ag, Pt, Pd
Any one.
4. the preparation method of ultralight porous carbon materials as described in claim 1, which is characterized in that include the following steps：
1) exodermis of pomelo peel is removed, is freeze-dried；
2) in parts by weight, by 100~2000 parts of pomelo peel, 70000 parts of water is added in hydrothermal reaction kettle, is heated to 160
DEG C~200 DEG C, react 20~30h；
3) by 2) gained reaction product filtering, dry, 6~8mol/L that 15~20ml is added according to every gram in the product after drying
KOH solution impregnated, soaking time be 15~25h, then filter, then be dried.
4) 3) product obtained is roasted under the conditions of non-oxidizing atmosphere, calcination temperature is 700 DEG C~900 DEG C, roasting time
For 2~5h, the product after roasting is impregnated into 20~25h using acid solution, is then filtered and is cleaned to filter with deionized water
Liquid is in neutrality, then is dried under the conditions of 60 DEG C~70 DEG C.
5. preparation method according to claim 4, which is characterized in that in the step 1), freezing dry process includes：First
By the pomelo peel for removing exodermis under the conditions of 30 DEG C of 20 DEG C~﹣ of ﹣, 100MT, 90~150min is handled；Then in 10 DEG C~﹣ of ﹣
20 DEG C, under the conditions of 100MT, handle 300~500min；Again under the conditions of 10 DEG C of 2 DEG C~﹣ of ﹣, 100MT, 300~500min is handled；
Finally under the conditions of 20 DEG C~40 DEG C, 20MT, 200~500min is handled.
6. preparation method according to claim 4, which is characterized in that in the step 4), acid solution is 2%~10%
Hydrochloric acid solution, and the mass ratio of hydrochloric acid solution and the product after roasting is 50：1~80: 1.
7. the preparation method of ultralight porous carbon materials as claimed in claim 2 or claim 3, which is characterized in that include the following steps：
1) exodermis of pomelo peel is removed, is freeze-dried；
2) in parts by weight, by 5~10 parts of loading metal-salt, 100~2000 parts of pomelo peel, 70000 parts of water is added to hydro-thermal
In reaction kettle, 160 DEG C~200 DEG C are heated to, reacts 20~30h；
3) by 2) gained reaction product filtering, dry, 6~8mol/L that 15~20ml is added according to every gram in the product after drying
KOH solution impregnated, soaking time be 15~25h, then filter, then be dried.
4) 3) product obtained is roasted under the conditions of non-oxidizing atmosphere, calcination temperature is 700 DEG C~900 DEG C, roasting time
For 2~5h, the product after roasting is impregnated into 20~25h using acid solution, is then filtered and is cleaned to filter with deionized water
Liquid is in neutrality, then is dried under the conditions of 60 DEG C~70 DEG C.
8. preparation method according to claim 7, which is characterized in that in the step 1), freezing dry process includes：First
By the pomelo peel for removing exodermis under the conditions of 30 DEG C of 20 DEG C~﹣ of ﹣, 100MT, 90~150min is handled；Then in 10 DEG C~﹣ of ﹣
20 DEG C, under the conditions of 100MT, handle 300~500min；Again under the conditions of 10 DEG C of 2 DEG C~﹣ of ﹣, 100MT, 300~500min is handled；
Finally under the conditions of 20 DEG C~40 DEG C, 20MT, 200~500min is handled.
9. preparation method according to claim 7, which is characterized in that in the step 2), loading metal-salt be gold chloride,
Any one in silver nitrate, chloroplatinic acid, palladium bichloride.
10. preparation method according to claim 7, which is characterized in that in the step 4), acid solution is 2%~10%
Hydrochloric acid solution, and hydrochloric acid solution with roasting after product mass ratio be 50：1~80: 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110203931A (en) * | 2019-07-01 | 2019-09-06 | 湖南城市学院 | A method of high pressure water system electrode material for super capacitor is prepared using pomelo peel |
| CN111268666A (en) * | 2020-01-20 | 2020-06-12 | 上海应用技术大学 | Hemicellulose-based carbon material and preparation method thereof |
| CN113045072A (en) * | 2021-02-10 | 2021-06-29 | 深圳市彤石科技有限公司 | Multistage filtration adsorption unit and waste water recovery water purification system |
| CN113213478A (en) * | 2021-02-10 | 2021-08-06 | 杨磊 | Porous carbon-based nano material and preparation method and application thereof |
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