CN102430369A - Bamboo charcoal/carbon aerogel composite material and preparation method thereof - Google Patents
Bamboo charcoal/carbon aerogel composite material and preparation method thereof Download PDFInfo
- Publication number
- CN102430369A CN102430369A CN2011102741692A CN201110274169A CN102430369A CN 102430369 A CN102430369 A CN 102430369A CN 2011102741692 A CN2011102741692 A CN 2011102741692A CN 201110274169 A CN201110274169 A CN 201110274169A CN 102430369 A CN102430369 A CN 102430369A
- Authority
- CN
- China
- Prior art keywords
- bamboo charcoal
- composite material
- carbon aerogel
- aerogel composite
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention discloses a method for preparing bamboo charcoal/carbon aerogel composite material, comprising the following steps: 1) mixing m-dihydroxybenzene with formaldehyde, dissolving in water, and stirring to obtain mixed liquid A; 2) adding the bamboo charcoal to the mixed liquid A and sealing; firstly standing at room temperature, then standing at 70-80 DEG C, and filtering to obtain mixture B; 3) putting the mixture B in trifluoroacetic acid liquor of which the mass concentration is 0.4-0.6% to soak, then taking outside and putting in acetone to soak, wherein the acetone is changed every day; and 4) putting the mixture after being dried in a nitrogen atmosphere furnace, insulating at 800-1000 DEG C for 1-3 hours, and obtaining the bamboo charcoal/carbon aerogel composite material. The composite material can be widely applied to industries for purifying air, processing waste water, processing toxic waste water, chemical catalyst carrier, purifying tail gas of cars, preparing sugar and wine, and preparing food.
Description
Technical field
The present invention relates to a kind of high-specific surface area material and preparation method thereof, particularly a kind of preparation method of bamboo charcoal/carbon aerogel composite material.
Background technology
Forbid cutting down forest from country, environmentally friendly, resource-conserving bamboo industry has obtained great development.Relevant with it bamboo charcoal also just because of renewable, the excellent absorption property of resource that it had, discharge functions such as negative oxygen ion, radiation far infrared, electromagnetic shielding, received numerous researchers' favor.
Bamboo charcoal mainly concentrates on 2 points as the research of sorbing material: on the one hand, improve its specific area, like alkali activation, steam activation etc.; On the other hand, its load photocatalyst material is made it to have photodegradation, like load TiO
2And ZnO.
Charcoal-aero gel is a kind of amorphous, solid-state, lightweight, porous, novel nano raw material of wood-charcoal material, and its porosity is up to 80～99%, network colloidal solid size 3～20nm, specific area can reach 1000m
2/ g, electrical conductivity can reach 10～40S/cm.At application number is that the inventor utilizes specific area to be 3000m in 02130067.4 " a kind of preparation method of the high specific capacitance electrode material " literary composition
2Active carbon that/g is above and charcoal-aero gel mix, ball milling, add binding agent afterwards, in 5～10MPa compacted under, have prepared the electrode material for electric double layer capacitor with high specific capacitance.But its invention thinking is; The inventor mainly utilizes the high conductivity of charcoal-aero gel; Charcoal-aero gel as additive, is used to increase the electric conductivity between the activated carbon granule, reduces the internal driving of electrode; Simultaneously also utilize charcoal-aero gel to have certain specific area, being added in when increasing electric conductivity of it is less to the loss of composite specific area.
Summary of the invention
The technical problem that the present invention will solve provides a kind of bamboo charcoal/carbon aerogel composite material and preparation method thereof, and it has overcome the relatively low problem of existing bamboo charcoal specific area, thereby prepares a kind of bamboo charcoal composite that has high-specific surface area.
In order to solve the problems of the technologies described above, the present invention provides a kind of preparation method of bamboo charcoal/carbon aerogel composite material, may further comprise the steps successively:
1), with resorcinol and formaldehyde with 1: 2.5～3.5 mixed in molar ratio, soluble in water, stir, obtain mixed liquor A; The mol ratio of said resorcinol and water is 1: 4.5～5.5;
2), bamboo charcoal is added in the mixed liquor A sealing; Leave standstill 3～5d prior under the room temperature, under 70～80 ℃, leave standstill 3～5d then, filter, get mixture B; Said bamboo charcoal is 35～45% of a mixed liquor A gross weight;
3), mixture B is put into mass concentration earlier is that 0.4～0.6% trifluoroacetic acid solution is soaked 1～2d under room temperature, puts into acetone after the taking-up again and soaks 3～5d, in said acetone immersion process, changes acetone every day;
Air dry 1～3d under room temperature gets dry back mixture at last;
4), mixture after the drying is placed the nitrogen atmosphere stove, behind 800～1000 ℃ of insulation 1～3h, bamboo charcoal/carbon aerogel composite material.
Improvement as the preparation method of bamboo charcoal/carbon aerogel composite material of the present invention: in step 1) and step 2) increases following steps between: bamboo charcoal is put into the sodium carbonate liquor that molar concentration is 6～7mol/L, soak 1～3d.That is, the bamboo charcoal after the above-mentioned immersion is added in the mixed liquor A, seal.
Further improvement as the preparation method of bamboo charcoal/carbon aerogel composite material of the present invention: between step 3) and step 4), increase following steps: the dry back mixture of step 3) gained is mixed the mass ratio 4.5～5.5: 1 of KOH and bamboo charcoal with KOH.That is, should place the nitrogen atmosphere stove with the mixed dry back of KOH mixture.
Further improvement as the preparation method of bamboo charcoal/carbon aerogel composite material of the present invention: bamboo charcoal is that grain diameter is 10～20 purpose bamboo charcoals.
The present invention also provides the bamboo charcoal/carbon aerogel composite material that utilizes method for preparing and get simultaneously.
In the present invention, sodium carbonate liquor plays the effect of catalyst, can guarantee that soak and is not soaked thing as long as soak.Room temperature is meant 5～30 ℃.In the step 1), the optimum mole ratio of resorcinol, formaldehyde and water is 1: 3: 5.Bamboo charcoal is that 40% of mixed liquor A gross weight is best proportion.In the present invention, do not inform in detail and all refer to temperature at room temperature to carry out.
The present invention be the inventor on the compound basis of study for a long period of time charcoal-aero gel and bamboo charcoal, obtain through exploring technical process repeatedly.Its advantage is: make catalyst pass through infusion process and in bamboo charcoal, introduce early stage; Thereby make organic aerogel original position in the micron order duct of bamboo charcoal generate; And pass through the organic aerogel charing and one step of the bamboo charcoal alkali activation high-temperature process in later stage, obtained the composite of high-specific surface area.
The present invention is on the basis of traditional preparation process organic aerogel; At first, reach the synthetic bamboo charcoal/organic aerogel of original position, and in carbonization process, add the alkali activation through the loaded on bamboo charcoal catalyst; Make organic aerogel in the process of charing, bamboo charcoal has also obtained activation.Charcoal-aero gel can well be attached in the bamboo charcoal large aperture, prepares bamboo charcoal/carbon aerogel composite material, has effectively improved the specific area of bamboo charcoal.
The composite that adopts the inventive method preparation and get, through detecting: its specific area reaches 2200～2700m
2/ g.Being superior to application number is that prepared its specific area is 640～1280m in 201010297043.2 " a kind of preparation methods of the bamboo charcoal based active carbon fiber " literary composition
2The material of/g; Also being superior to application number greatly is prepared bamboo charcoal composite in 201010190411.3 " a kind of adsorption decomposition agents and preparation method thereof " literary composition, and its specific area is 800～900m
2/ g.
Adopt the composite that the present invention produced, can be widely used in air cleaning, sewage disposal, poisonous wastewater treatment, chemical catalyst carrier, purifying vehicle exhaust, sugaring system wine, food and industry such as make with extra care.
In sum, improving on the bamboo charcoal specific area, proposed to novelty of the present invention the load carbon aeroge, reformed in the bamboo charcoal duct, the micron order macropore of bamboo charcoal is filled to mesopore and micropore with netted aeroge, it is higher to make it specific surface.
The specific embodiment
In following, do not inform in detail all to refer to temperature at room temperature to carry out.
The preparation method of embodiment 1, a kind of bamboo charcoal/carbon aerogel composite material may further comprise the steps successively:
1), resorcinol, formaldehyde and water are stirred after according to 1: 3: 5 mixed in molar ratio, obtains mixed liquor A;
2), bamboo charcoal is put into the sodium carbonate liquor that molar concentration is 6mol/L, immersion 1d; The grain diameter of bamboo charcoal is 10～20 orders, and bamboo charcoal is 40% of a mixed liquor A gross weight;
3), with step 2) bamboo charcoal that soaks gained adds in the mixed liquor A of step 1) gained sealing; Leave standstill 3d prior under the room temperature, under 70 ℃, leave standstill 3d then, filter, get mixture B;
4), mixture B is put into mass concentration earlier is that 0.5% trifluoroacetic acid solution is soaked 1d under room temperature, puts into acetone after the taking-up again and soaks 3d, in the acetone immersion process, changes acetone every day one time;
Air dry 1d under room temperature gets dry back mixture at last;
5), the dry back mixture with the step 4) gained mixes KOH and step 2 with KOH) in the mass ratio 5: 1 of bamboo charcoal;
6), the mixture of step 5) gained is placed the nitrogen atmosphere stove, behind 800 ℃ of insulation 1h, bamboo charcoal/carbon aerogel composite material.
Its specific area of this bamboo charcoal/carbon aerogel composite material reaches 2240m
2/ g.
The preparation method of embodiment 2, a kind of bamboo charcoal/carbon aerogel composite material may further comprise the steps successively:
1), resorcinol, formaldehyde and water are stirred after according to 1: 3: 5 mixed in molar ratio, obtains mixed liquor A;
2), bamboo charcoal is put into the sodium carbonate liquor that molar concentration is 7mol/L, immersion 3d; The bamboo charcoal particle particle diameter is 10～20 orders, and bamboo charcoal is 40% of a mixed liquor A gross weight;
3), with step 2) bamboo charcoal that soaks gained adds in the mixed liquor A of step 1) gained sealing; Leave standstill 5d prior under the room temperature, under 80 ℃, leave standstill 5d then, filter, get mixture B;
4), mixture B is put into mass concentration earlier is that 0.5% trifluoroacetic acid solution is soaked 2d under room temperature, puts into acetone after the taking-up again and soaks 5d, in the acetone immersion process, changes acetone every day one time;
Air dry 3d under room temperature gets dry back mixture at last;
5), the dry back mixture with the step 4) gained mixes KOH and step 2 with KOH) in the mass ratio 5: 1 of bamboo charcoal;
6), the mixture of step 5) gained is placed the nitrogen atmosphere stove, behind 900 ℃ of insulation 2h, bamboo charcoal/carbon aerogel composite material.
Its specific area of bamboo charcoal/carbon aerogel composite material reaches 2600m
2/ g.
The preparation method of embodiment 3, a kind of bamboo charcoal/carbon aerogel composite material may further comprise the steps successively:
1), resorcinol, formaldehyde and water are stirred after according to 1: 3: 5 mixed in molar ratio, obtains mixed liquor A;
2), bamboo charcoal is put into the sodium carbonate liquor that molar concentration is 6mol/L, immersion 2d; The bamboo charcoal particle particle diameter is 10～20 orders, and bamboo charcoal is 40% of a mixed liquor A gross weight;
3), with step 2) bamboo charcoal that soaks gained adds in the mixed liquor A of step 1) gained sealing; Leave standstill 4d prior under the room temperature, under 70 ℃, leave standstill 4d then, filter, get mixture B;
4), mixture B is put into mass concentration earlier is that 0.6% trifluoroacetic acid solution is soaked 2d under room temperature, puts into acetone after the taking-up again and soaks 4d, in the acetone immersion process, changes acetone every day one time;
Air dry 2d under room temperature gets dry back mixture at last;
5), the dry back mixture with the step 4) gained mixes KOH and step 2 with KOH) in the mass ratio 5: 1 of bamboo charcoal;
6), the mixture of step 5) gained is placed the nitrogen atmosphere stove, behind 1000 ℃ of insulation 3h, bamboo charcoal/carbon aerogel composite material.
Its specific area of bamboo charcoal/carbon aerogel composite material reaches 2700m
2/ g.
Embodiment 4, a kind of bamboo charcoal/carbon aerogel composite material and preparation method thereof may further comprise the steps successively:
1), resorcinol, formaldehyde and water are stirred after according to 1: 3: 5 mixed in molar ratio, obtains mixed liquor A;
2), bamboo charcoal is put into the sodium carbonate liquor that molar concentration is 6.5mol/L, immersion 3d; The bamboo charcoal particle particle diameter is 10～20 orders, and bamboo charcoal is 40% of a mixed liquor A gross weight;
3), with step 2) bamboo charcoal that soaks gained adds in the mixed liquor A of step 1) gained sealing; Leave standstill 5d prior under the room temperature, under 80 ℃, leave standstill 3d then, filter, get mixture B;
4), mixture B is put into mass concentration earlier is that 0.6% trifluoroacetic acid solution is soaked 1d under room temperature, puts into acetone after the taking-up again and soaks 3d, in the acetone immersion process, changes acetone every day one time;
Air dry 3d under room temperature gets dry back mixture at last;
5), the dry back mixture with the step 4) gained mixes KOH and step 2 with KOH) in the mass ratio 5: 1 of bamboo charcoal;
6), the mixture of step 5) gained is placed the nitrogen atmosphere stove, behind 900 ℃ of insulation 1h, bamboo charcoal/carbon aerogel composite material.
Its specific area of bamboo charcoal/carbon aerogel composite material reaches 2560m
2/ g.
Comparative Examples 1, cancellation step 2) the sodium carbonate liquor impregnation steps, that is, bamboo charcoal is directly added in the mixed liquor A of step 1) gained and seals; All the other are with embodiment 1.
The specific area of the bamboo charcoal/carbon aerogel composite material of final gained reaches 1500m
2/ g.
Comparative Examples 2, cancellation step 5) mix with KOH, that is, directly place the nitrogen atmosphere stove to be incubated in the dry back mixture of step 4) gained; All the other are with embodiment 1.
The specific area of the bamboo charcoal/carbon aerogel composite material of final gained reaches 1850m
2/ g.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (5)
1. the preparation method of bamboo charcoal/carbon aerogel composite material is characterized in that may further comprise the steps successively:
1), with resorcinol and formaldehyde with 1: 2.5～3.5 mixed in molar ratio, soluble in water, stir, obtain mixed liquor A; The mol ratio of said resorcinol and water is 1: 4.5～5.5;
2), bamboo charcoal is added in the mixed liquor A sealing; Leave standstill 3～5d prior under the room temperature, under 70～80 ℃, leave standstill 3～5d then, filter, get mixture B; Said bamboo charcoal is 35～45% of a mixed liquor A gross weight;
3), mixture B is put into mass concentration earlier is that 0.4～0.6% trifluoroacetic acid solution is soaked 1～2d under room temperature, puts into acetone after the taking-up again and soaks 3～5d, in said acetone immersion process, changes acetone every day;
Air dry 1～3d under room temperature gets dry back mixture at last;
4), mixture after the drying is placed the nitrogen atmosphere stove, behind 800～1000 ℃ of insulation 1～3h, bamboo charcoal/carbon aerogel composite material.
2. the preparation method of bamboo charcoal/carbon aerogel composite material according to claim 1 is characterized in that: in said step 1) and step 2) between increase following steps:
Bamboo charcoal is put into the sodium carbonate liquor that molar concentration is 6～7mol/L, soak 1～3d.
3. the preparation method of bamboo charcoal/carbon aerogel composite material according to claim 2 is characterized in that: between said step 3) and step 4), increase following steps:
The dry back mixture of step 3) gained is mixed the mass ratio 4.5～5.5: 1 of said KOH and bamboo charcoal with KOH.
4. according to the preparation method of claim 1,2 or 3 described bamboo charcoal/carbon aerogel composite materials, it is characterized in that: said bamboo charcoal is that grain diameter is 10～20 purpose bamboo charcoals.
5. utilize the bamboo charcoal/carbon aerogel composite material that gets like any one method preparation in the claim 1～4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110274169 CN102430369B (en) | 2011-09-16 | 2011-09-16 | Bamboo charcoal/carbon aerogel composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110274169 CN102430369B (en) | 2011-09-16 | 2011-09-16 | Bamboo charcoal/carbon aerogel composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102430369A true CN102430369A (en) | 2012-05-02 |
| CN102430369B CN102430369B (en) | 2013-08-14 |
Family
ID=45978934
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110274169 Expired - Fee Related CN102430369B (en) | 2011-09-16 | 2011-09-16 | Bamboo charcoal/carbon aerogel composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102430369B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824154A (en) * | 2015-12-07 | 2017-06-13 | 车春玲 | A kind of bamboo carbon powder photocatalysis air-cleaning composite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333100A (en) * | 2008-08-05 | 2008-12-31 | 浙江大学 | Bamboo charcoal-based far infrared composite material and method for preparing same |
| CN101844072A (en) * | 2010-06-03 | 2010-09-29 | 浙江碧岩环保材料有限公司 | Adsorption decomposition agent and preparation method thereof |
| CN101974846A (en) * | 2010-09-28 | 2011-02-16 | 朱君铭 | Method for preparing bamboo charcoal-based activated carbon fibers |
-
2011
- 2011-09-16 CN CN 201110274169 patent/CN102430369B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333100A (en) * | 2008-08-05 | 2008-12-31 | 浙江大学 | Bamboo charcoal-based far infrared composite material and method for preparing same |
| CN101844072A (en) * | 2010-06-03 | 2010-09-29 | 浙江碧岩环保材料有限公司 | Adsorption decomposition agent and preparation method thereof |
| CN101974846A (en) * | 2010-09-28 | 2011-02-16 | 朱君铭 | Method for preparing bamboo charcoal-based activated carbon fibers |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824154A (en) * | 2015-12-07 | 2017-06-13 | 车春玲 | A kind of bamboo carbon powder photocatalysis air-cleaning composite |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102430369B (en) | 2013-08-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103771407B (en) | Take biomass power plant ash as the method that super-activated carbon prepared by raw material | |
| CN102247802A (en) | Method for preparing activated carbon | |
| CN110935280B (en) | Nitrogen-doped mesoporous bamboo-based biochar and application thereof | |
| CN113209937B (en) | Method for preparing nano metal oxide loaded active carbon and application thereof | |
| CN102728339B (en) | Porous inorganic ceramic membrane-graphene-TiO2 photocatalyst composite material and its preparation method | |
| CN104084126B (en) | The preparation method of biomass-based iron aluminium complex spherical charcoal | |
| CN105080540A (en) | Wet oxidation catalyst and preparation method thereof | |
| CN112194127A (en) | Method for preparing nitrogen-doped carbon material from biomass | |
| CN115475604B (en) | Manufacturing method of composite multifunctional adsorbent based on cork activated carbon and amino carbon quantum dots | |
| CN110683540A (en) | Nitrogen-rich hierarchical pore biomass charcoal and application thereof | |
| CN112938969A (en) | Method for preparing nitrogen-sulfur co-doped activated carbon by pore-forming/doping integrated activating agent and application of method | |
| CN109225187B (en) | Preparation method and application of sludge-based ceramic-based catalyst | |
| CN104001371A (en) | Method for recycling waste dust removal filter material | |
| CN106000310A (en) | Preparation method of halloysite-carbon composite adsorbent for removing NO | |
| CN103736457A (en) | Preparation method and magnetic activated carbon prepared by same | |
| CN102744051B (en) | Porous inorganic ceramic membrane-carbon nanotube-TiO2 photocatalyst composite material and preparation method thereof | |
| CN104437394B (en) | Dual-layer high-amino density plant fiber-based adsorption material and preparation method and application thereof | |
| CN102430369B (en) | Bamboo charcoal/carbon aerogel composite material and preparation method thereof | |
| CN102728365B (en) | Porous inorganic ceramic membrane-Fe modified TiO2-carbon nanotube photocatalyst material and its preparation method | |
| CN102580690B (en) | Nano-aperture granular adsorbent and preparation and application thereof | |
| CN110590227A (en) | Diatom ooze capable of efficiently and durably removing formaldehyde and preparation method thereof | |
| CN102989522A (en) | Porous cement-based photocatalytic material and preparation process thereof | |
| CN105692583A (en) | Method for preparing beta-cyclodextrin-based boron-doped mesoporous carbon material through soft template method | |
| CN102744091B (en) | Porous inorganic ceramic membrane-graphene-N modified TiO2 photocatalyst material and preparation method thereof | |
| CN106345487B (en) | A kind of porous catalytic composite material of air cleaning and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130814 Termination date: 20200916 |