CN108686617A - A kind of CO absorption2Carbon material preparation and method of modifying - Google Patents

A kind of CO absorption2Carbon material preparation and method of modifying Download PDF

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Publication number
CN108686617A
CN108686617A CN201810487386.1A CN201810487386A CN108686617A CN 108686617 A CN108686617 A CN 108686617A CN 201810487386 A CN201810487386 A CN 201810487386A CN 108686617 A CN108686617 A CN 108686617A
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carbon material
warming
absorption
preparation example
metal ion
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杨泛明
张龙
肖文杰
郑策
楚广
刘磊
陈思敏
王超林
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Hunan City University
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Hunan City University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The present invention provides a kind of CO absorption2Carbon material preparation and method of modifying, include the following steps:In water for a period of time by infusion of tea, tealeaf residue is obtained after removing water.Tealeaf residue is dried and is placed in small crucible, and small crucible is placed in Muffle furnace, after tealeaf residue is carbonized by heating, room temperature is cooled to, obtains carbon material.The present invention also provides prepared carbon material is carried out to metal ion-modified method.Carbon material prepared by the present invention is in low concentration CO2There is larger adsorbance, and preparation method is simple in environment, cost is relatively low, has preferable prospects for commercial application.

Description

A kind of CO absorption2Carbon material preparation and method of modifying
Technical field
The present invention relates to one kind in lower temperature, relatively low CO2There is efficient CO in concentration environment2The carbon material of absorption property Preparation and method of modifying.
Background technology
In recent years, global industry progress faster, CO2Discharge capacity increased dramatically, carbon dioxide (CO in air2) concentration is fast Speed increases, and greenhouse effects is caused to aggravate.Therefore CO2Capture has become various countries' focus.CO2In capture technique, CO2Absorption tool Have the advantages that adsorbance is larger, the rate of adsorption is very fast, corrosivity is smaller and receives significant attention.
Adsorbent preparation is CO2The core of adsorption technology.CO2In adsorbent, carbon material is because having larger CO2Adsorbance, The rate of adsorption is very fast, and suction-desorption temperature is relatively low, and energy consumption is smaller, it is cheap, not corrosive equipment the features such as and be concerned. After being modified to it using metal ion, the CO of material can be improved2Absorption property.Gas molecule is contacted with solid absorbent When, it can enter in carbon material duct, stronger electrostatic interaction can be also formed with material surface metal ion, to reach efficient suction Attached CO2Purpose.
The factors such as the absorption property of modified carbonaceous components and carbon material property, the type of modified material and the two quality are related. Different carbon materials has different pore structures, therefore has different CO2Absorption property.Carbon material is changed using metal ion After property, gas molecule not only can physics be piled up in carbon material surface, but also stronger electrostatic interaction can be formed with metal ion, make CO2 Molecule is easier to be adsorbed in material surface.It, can also be with CO if having Lewis acid position in metal ion2Molecule bonding improves CO2It inhales Attached performance.In addition to this, using after metal ion-modified, carbon material pore structure changes.When material aperture moves closer to CO2 When molecular dynamics diameter, CO2Adsorbance and selectivity increase.Therefore the carbon that different carbon source preparation structure can be utilized different Material, and preparation is modified to it with efficient CO using metal ion2The adsorbent of absorption property.
Invention content
The purpose of invention is to provide a kind of CO absorption2Carbon material preparation and method of modifying.
To achieve the above object, the present invention provides a kind of CO absorption2Carbon material preparation method, include the following steps:
Tealeaves is placed in immersion 0.5h~1h in 80 DEG C~100 DEG C water, tealeaf residue is obtained after removing water, tealeaf residue is dried It is placed in small crucible, and small crucible is placed in Muffle furnace, with 3~5 DEG C of min-1Rate heats up, and waits for that tealeaf residue is carbonized Afterwards, with 3~5 DEG C of min-1Rate is cooled to room temperature to get to CO absorption2Carbon material.
In above-mentioned preparation method, the tealeaves is Anhua black tea tealeaves or Anhua black tea leaf.
In above-mentioned preparation method, the carbonization method is to keep 4h~6h after being warming up to 300 DEG C, then be warming up to 400 DEG C of guarantors 4h~6h is held, 500 DEG C of holding 4h~6h are finally warming up to.
The present invention also provides a kind of CO absorptions to above-mentioned preparation2Carbon material carries out metal ion-modified method, including Following step:
By the CO absorption of metal salt and preparation2Carbon material be placed in polytetrafluoroethyllining lining, be added deionized water in stir Dissolving is mixed, is subsequently placed in 100 DEG C~120 DEG C drying boxes and carries out hydro-thermal process 12h~for 24 hours, you can be made metal ion-modified Carbon material.
In above-mentioned method of modifying, the metal salt is ZrOCl2·8H2O or ZrO (NO3)2。
In above-mentioned method of modifying, the metal salt and CO absorption2Carbon material mass ratio be [0.3~0.7]:1.
According to experimental result, metal ion-modified carbon material provided by the present invention, in low concentration CO2In environment, have CO2The features such as adsorption capacity is larger, desorption temperature is relatively low, this method solve common low concentration CO2CO in environment2Adsorbance Small, the deficiencies of desorption temperature is higher, there is good prospects for commercial application.
Description of the drawings
Fig. 1 show carbon material CO made from the embodiment of the present invention 12Adsorbance changes over time curve graph.
The preparation of carbon material:
Preparation example I
A. the Anhua 5g black tea infusion of tea in 100 DEG C of water and is kept into 0.5h, tealeaf residue is obtained after removing water;
B. tealeaf residue is dried and is placed in small crucible, and small crucible is placed in Muffle furnace, with 3 DEG C of min-1Heating Rate keeps 4h after being warming up to 300 DEG C, then is warming up to 400 DEG C of holding 4h with identical heating rate, finally with identical heating Rate is warming up to 500 DEG C of holding 4h;
C. with 3 DEG C of min-1Rate of temperature fall be cooled to room temperature, obtain carbon material BT-C.
Preparation example 2
A. the Anhua 5g black tea infusion of tea in 90 DEG C of water and is kept into 0.75h, tealeaf residue is obtained after removing water;
B. tealeaf residue is dried and is placed in small crucible, and small crucible is placed in Muffle furnace, with 3 DEG C of min-1Heating Rate keeps 4h after being warming up to 300 DEG C, then is warming up to 400 DEG C of holding 4h with identical heating rate, finally with identical heating Rate is warming up to 500 DEG C of holding 4h;
C. with 3 DEG C of min-1Rate of temperature fall be cooled to room temperature, obtain carbon material BT-C.
Preparation example 3
A. the Anhua 5g black tea infusion of tea in 80 DEG C of water and is kept into 1h, tealeaf residue is obtained after removing water;
B. tealeaf residue is dried and is placed in small crucible, and small crucible is placed in Muffle furnace, with 3 DEG C of min-1Heating Rate keeps 4h after being warming up to 300 DEG C, then is warming up to 400 DEG C of holding 4h with identical heating rate, finally with identical heating Rate is warming up to 500 DEG C of holding 4h;
C. with 3 DEG C of min-1Rate of temperature fall be cooled to room temperature, obtain carbon material BT-C.
Preparation example 4
A. the Anhua 5g black tea infusion of tea in 100 DEG C of water and is kept into 0.5h, tealeaf residue is obtained after removing water;
B. tealeaf residue is dried and is placed in small crucible, and small crucible is placed in Muffle furnace, with 4 DEG C of min-1Heating Rate keeps 5h after being warming up to 300 DEG C, then is warming up to 400 DEG C of holding 5h with identical heating rate, finally with identical heating Rate is warming up to 500 DEG C of holding 5h;
C. with 4 DEG C of min-1Rate of temperature fall be cooled to room temperature, obtain carbon material BT-C.
Preparation example 5
A. the Anhua 5g black tea infusion of tea in 90 DEG C of water and is kept into 0.75h, tealeaf residue is obtained after removing water;
B. tealeaf residue is dried and is placed in small crucible, and small crucible is placed in Muffle furnace, with 4 DEG C of min-1Heating Rate keeps 5h after being warming up to 300 DEG C, then is warming up to 400 DEG C of holding 5h with identical heating rate, finally with identical heating Rate is warming up to 500 DEG C of holding 5h;
C. with 4 DEG C of min-1Rate of temperature fall be cooled to room temperature, obtain carbon material BT-C.
Preparation example 6
A. the Anhua 5g black tea infusion of tea in 80 DEG C of water and is kept into 1h, tealeaf residue is obtained after removing water;
B. tealeaf residue is dried and is placed in small crucible, and small crucible is placed in Muffle furnace, with 4 DEG C of min-1Heating Rate keeps 5h after being warming up to 300 DEG C, then is warming up to 400 DEG C of holding 5h with identical heating rate, finally with identical heating Rate is warming up to 500 DEG C of holding 5h;
C. with 4 DEG C of min-1Rate of temperature fall be cooled to room temperature, obtain carbon material BT-C.
Preparation example 7
A. the Anhua 5g black tea leaf is soaked in 100 DEG C of water and is kept 0.5h, tealeaf residue is obtained after removing water;
B. tealeaf residue is dried and is placed in small crucible, and small crucible is placed in Muffle furnace, with 5 DEG C of min-1Heating Rate keeps 6h after being warming up to 300 DEG C, then is warming up to 400 DEG C of holding 6h with identical heating rate, finally with identical heating Rate is warming up to 500 DEG C of holding 6h;
C. with 5 DEG C of min-1Rate of temperature fall be cooled to room temperature, obtain carbon material RT-C.
Preparation example 8
A. the Anhua 5g black tea leaf is soaked in 90 DEG C of water and is kept 0.75h, tealeaf residue is obtained after removing water;
B. tealeaf residue is dried and is placed in small crucible, and small crucible is placed in Muffle furnace, with 5 DEG C of min-1Heating Rate keeps 6h after being warming up to 300 DEG C, then is warming up to 400 DEG C of holding 6h with identical heating rate, finally with identical heating Rate is warming up to 500 DEG C of holding 6h;
C. with 5 DEG C of min-1Rate of temperature fall be cooled to room temperature, obtain carbon material RT-C.
Preparation example 9
A. the Anhua 5g black tea leaf is soaked in 80 DEG C of water and is kept 60min, tealeaf residue is obtained after removing water;
B. tealeaf residue is dried and is placed in small crucible, and small crucible is placed in Muffle furnace, with 5 DEG C of min-1Heating Rate keeps 6h after being warming up to 300 DEG C, then is warming up to 400 DEG C of holding 6h with identical heating rate, finally with identical heating Rate is warming up to 500 DEG C of holding 6h;
C. with 5 DEG C of min-1Rate of temperature fall be cooled to room temperature, obtain carbon material RT-C.
The preparation of metal ion-modified carbon material:
Preparation example 10
A. BT-C and ZrOCl prepared in preparation example 1 are taken respectively2·8H2O is placed in polytetrafluoroethyllining lining, is added Deionized water, stirring and dissolving.Aforesaid operations are repeated, 5 parts of ZrOCl are obtained2·8H2The different turbid solution of the mass ratio of O and BT-C. Wherein, ZrOCl2·8H2The mass ratio of O and BT-C is respectively 0.3: 1,0.4: 1,0.5: 1,0.6: 1 and 0.7: 1;
B. gained turbid solution in a steps is placed in 100 DEG C of drying boxes, carries out hydro-thermal process for 24 hours, products therefrom is carried out Centrifugation, it is dry, obtain metal ion-modified carbon material BT-C (Zr).
Preparation example 11
A. BT-C and ZrOCl prepared in preparation example 2 are taken respectively2·8H2O is placed in polytetrafluoroethyllining lining, is added Deionized water, stirring and dissolving.Aforesaid operations are repeated, 5 parts of ZrOCl are obtained2·8H2The different turbid solution of the mass ratio of O and BT-C. Wherein, ZrOCl2·8H2The mass ratio of O and BT-C is respectively 0.3: 1,0.4: 1,0.5: 1,0.6: 1 and 0.7: 1;
B. gained turbid solution in a steps is placed in 110 DEG C of drying boxes, carries out hydro-thermal process 18h, products therefrom is carried out Centrifugation, it is dry, obtain metal ion-modified carbon material BT-C (Zr).
Preparation example 12
A. BT-C and ZrOCl prepared in preparation example 3 are taken respectively2·8H2O is placed in polytetrafluoroethyllining lining, is added Deionized water, stirring and dissolving.Aforesaid operations are repeated, 5 parts of ZrOCl are obtained2·8H2The different turbid solution of the mass ratio of O and BT-C. Wherein, ZrOCl2·8H2The mass ratio of O and BT-C is respectively 0.3: 1,0.4: 1,0.5: 1,0.6: 1 and 0.7: 1;
B. gained turbid solution in a steps is placed in 120 DEG C of drying boxes, carries out hydro-thermal process 12h, products therefrom is carried out Centrifugation, it is dry, obtain metal ion-modified carbon material BT-C (Zr).
Preparation example 13
A. BT-C prepared in preparation example 4 and ZrO (NO is taken respectively3)2, be placed in polytetrafluoroethyllining lining, addition go from Sub- water, stirring and dissolving.Aforesaid operations are repeated, 5 parts of ZrO (NO are obtained3)2The turbid solution different with the mass ratio of BT-C.Wherein, ZrO (NO3)2Mass ratio with BT-C is respectively 0.3: 1,0.4: 1,0.5: 1,0.6: 1 and 0.7: 1;
B. gained turbid solution in a steps is placed in 100 DEG C of drying boxes, carries out hydro-thermal process for 24 hours, products therefrom is carried out Centrifugation, it is dry, obtain metal ion-modified carbon material BT-C (Zr).
Preparation example 14
A. BT-C prepared in preparation example 5 and ZrO (NO is taken respectively3)2, be placed in polytetrafluoroethyllining lining, addition go from Sub- water, stirring and dissolving.Aforesaid operations are repeated, 5 parts of ZrO (NO are obtained3)2The turbid solution different with the mass ratio of BT-C.Wherein, ZrO (NO3)2Mass ratio with BT-C is respectively 0.3: 1,0.4: 1,0.5: 1,0.6: 1 and 0.7: 1;
B. gained turbid solution in a steps is placed in 110 DEG C of drying boxes, carries out hydro-thermal process 18h, products therefrom is carried out Centrifugation, it is dry, obtain metal ion-modified carbon material BT-C (Zr).
Preparation example 15
A. BT-C prepared in preparation example 6 and ZrO (NO is taken respectively3)2, be placed in polytetrafluoroethyllining lining, addition go from Sub- water, stirring and dissolving.Aforesaid operations are repeated, 5 parts of ZrO (NO are obtained3)2The turbid solution different with the mass ratio of BT-C.Wherein, ZrO (NO3)2Mass ratio with BT-C is respectively 0.3: 1,0.4: 1,0.5: 1,0.6: 1 and 0.7: 1;
B. gained turbid solution in a steps is placed in 120 DEG C of drying boxes, carries out hydro-thermal process 12h, products therefrom is carried out Centrifugation, it is dry, obtain metal ion-modified carbon material BT-C (Zr).
Preparation example 16
A. RT-C and ZrOCl prepared in preparation example 7 are taken respectively2·8H2O is placed in polytetrafluoroethyllining lining, is added Deionized water, stirring and dissolving.Aforesaid operations are repeated, 5 parts of ZrOCl are obtained2·8H2The different turbid solution of the mass ratio of O and BT-C. Wherein, ZrOCl2·8H2The mass ratio of O and RT-C is respectively 0.3: 1,0.4: 1,0.5: 1,0.6: 1 and 0.7: 1;
B. gained turbid solution in a steps is placed in 100 DEG C of drying boxes, carries out hydro-thermal process for 24 hours, products therefrom is carried out Centrifugation, it is dry, obtain metal ion-modified carbon material RT-C (Zr).
Preparation example 17
A. RT-C and ZrOCl prepared in preparation example 8 are taken respectively2·8H2O is placed in polytetrafluoroethyllining lining, is added Deionized water, stirring and dissolving.Aforesaid operations are repeated, 5 parts of ZrOCl are obtained2·8H2The different turbid solution of the mass ratio of O and BT-C. Wherein, ZrOCl2·8H2The mass ratio of O and RT-C is respectively 0.3: 1,0.4: 1,0.5: 1,0.6: 1 and 0.7: 1;
B. gained turbid solution in a steps is placed in 110 DEG C of drying boxes, carries out hydro-thermal process 18h, products therefrom is carried out Centrifugation, it is dry, obtain metal ion-modified carbon material RT-C (Zr).
Preparation example 18
A. RT-C and ZrOCl prepared in preparation example 9 are taken respectively2·8H2O is placed in polytetrafluoroethyllining lining, is added Deionized water, stirring and dissolving.Aforesaid operations are repeated, 5 parts of ZrOCl are obtained2·8H2The different turbid solution of the mass ratio of O and BT-C. Wherein, ZrOCl2·8H2The mass ratio of O and RT-C is respectively 0.3: 1,0.4: 1,0.5: 1,0.6: 1 and 0.7: 1;
B. gained turbid solution in a steps is placed in 120 DEG C of drying boxes, carries out hydro-thermal process 12h, products therefrom is carried out Centrifugation, it is dry, obtain metal ion-modified carbon material RT-C (Zr).
The CO of carbon material and its modified material2Determining adsorption
Embodiment 1
Suitable carbon material BT-C prepared by preparation example 1 is taken, is placed in the U-tube of AutoChem II 2920, is led to Enter high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 DEG C;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min, the CO of gained BT-C2Adsorbance changes over time song Line is as shown in Figure 1.
Embodiment 2
Suitable carbon material BT-C prepared by preparation example 2 is taken, is placed in the U-tube of AutoChem II 2920, is led to Enter high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 DEG C;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min, the CO of gained BT-C2Adsorbance changes over time song Line is similar to Fig. 1.
Embodiment 3
Suitable carbon material BT-C prepared by preparation example 3 is taken, is placed in the U-tube of AutoChem II 2920, is led to Enter high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 DEG C;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min, the CO of gained BT-C2Adsorbance changes over time song Line is similar to Fig. 1.
Embodiment 4
Suitable carbon material BT-C prepared by preparation example 4 is taken, is placed in the U-tube of AutoChem II 2920, is led to Enter high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 DEG C;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min, the CO of gained BT-C2Adsorbance changes over time song Line is similar to Fig. 1.
Embodiment 5
Suitable carbon material BT-C prepared by preparation example 5 is taken, is placed in the U-tube of AutoChem II 2920, is led to Enter high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 DEG C;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min, the CO of gained BT-C2Adsorbance changes over time song Line is similar to Fig. 1.
Embodiment 6
Suitable carbon material BT-C prepared by preparation example 6 is taken, is placed in the U-tube of AutoChem II 2920, is led to Enter high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 DEG C;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min, the CO of gained BT-C2Adsorbance changes over time song Line is similar to Fig. 1.
Embodiment 7
Suitable carbon material RT-C prepared by preparation example 7 is taken, is placed in the U-tube of AutoChem II 2920, is led to Enter high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 DEG C;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min, the CO of gained RT-C2Adsorbance changes over time song Line is similar to Fig. 1.
Embodiment 8
Suitable carbon material RT-C prepared by preparation example 8 is taken, is placed in the U-tube of AutoChem II 2920, is led to Enter high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 DEG C;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min, the CO of gained RT-C2Adsorbance changes over time song Line is similar to Fig. 1.
Embodiment 9
Suitable carbon material RT-C prepared by preparation example 9 is taken, is placed in the U-tube of AutoChem II 2920, is led to Enter high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 DEG C;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min, the CO of gained RT-C2Adsorbance changes over time song Line is similar to Fig. 1.
Embodiment 10
Suitable metal ion-modified carbon material BT-C (Zr) prepared by preparation example 10 is taken, AutoChem II are placed in In 2920 U-tube, it is passed through high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 ℃;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min;
Compared with carbon material BT-C in preparation example 1, the CO of metal ion-modified carbon material BT-C (Zr)2Adsorbance obviously increases Greatly, between 3~5mmolg-1Between.
Embodiment 11
Suitable metal ion-modified carbon material BT-C (Zr) prepared by preparation example 11 is taken, AutoChem II are placed in In 2920 U-tube, it is passed through high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 ℃;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min;
Compared with carbon material BT-C in preparation example 2, the CO of metal ion-modified carbon material BT-C (Zr)2Adsorbance obviously increases Greatly, between 3~5mmolg-1Between.
Embodiment 12
Suitable metal ion-modified carbon material BT-C (Zr) prepared by preparation example 12 is taken, AutoChem II are placed in In 2920 U-tube, it is passed through high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 ℃;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min;
Compared with carbon material BT-C in preparation example 3, the CO of metal ion-modified carbon material BT-C (Zr)2Adsorbance obviously increases Greatly, between 3~5mmolg-1Between.
Embodiment 13
Suitable metal ion-modified carbon material BT-C (Zr) prepared by preparation example 13 is taken, AutoChem II are placed in In 2920 U-tube, it is passed through high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 ℃;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min;
Compared with carbon material BT-C in preparation example 4, the CO of metal ion-modified carbon material BT-C (Zr)2Adsorbance obviously increases Greatly, between 3~5mmolg-1Between.
Embodiment 14
Suitable metal ion-modified carbon material BT-C (Zr) prepared by preparation example 14 is taken, AutoChem II are placed in In 2920 U-tube, it is passed through high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 ℃;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min;
Compared with carbon material BT-C in preparation example 5, the CO of metal ion-modified carbon material BT-C (Zr)2Adsorbance obviously increases Greatly, between 3~5mmolg-1Between.
Embodiment 15
Suitable metal ion-modified carbon material BT-C (Zr) prepared by preparation example 15 is taken, AutoChem II are placed in In 2920 U-tube, it is passed through high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 ℃;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min;
Compared with carbon material BT-C in preparation example 6, the CO of metal ion-modified carbon material BT-C (Zr)2Adsorbance obviously increases Greatly, between 3~5mmolg-1Between.
Embodiment 16
Suitable metal ion-modified carbon material RT-C (Zr) prepared by preparation example 16 is taken, AutoChem is placed in In the U-tube of II2920, it is passed through high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 ℃;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min;
Compared with carbon material RT-C in preparation example 7, the CO of metal ion-modified carbon material BT-C (Zr)2Adsorbance obviously increases Greatly, between 3~5mmolg-1Between.
Embodiment 17
Suitable metal ion-modified carbon material RT-C (Zr) prepared by preparation example 17 is taken, AutoChemII is placed in In 2920 U-tube, it is passed through high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 ℃;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min;
Compared with carbon material RT-C in preparation example 8, the CO of metal ion-modified carbon material BT-C (Zr)2Adsorbance obviously increases Greatly, between 3~5mmolg-1Between.
Embodiment 18
Suitable metal ion-modified carbon material RT-C (Zr) prepared by preparation example 18 is taken, AutoChem II are placed in In 2920 U-tube, it is passed through high-purity Ar purging carbon material surface, while being warming up to 100 DEG C, after keeping 60min, is cooled to 75 ℃;
It is passed through 5%CO2- He gases, gas pressure 0.2MPa, gas flow 10mlmin-1, keep 10min, 5% CO2CO in-He gases2Percentage by volume is that 5%, He percentage by volumes are 95%;
It is passed through high-purity Ar, while being warming up to 100 DEG C, keeps 60min;
Compared with carbon material RT-C in preparation example 9, the CO of metal ion-modified carbon material BT-C (Zr)2Adsorbance obviously increases Greatly, between 3~5mmolg-1Between.
The superiority of metal ion-modified carbon material in order to further illustrate the present invention selects following adsorbent conduct pair Ratio.
2g graphite and 17.5g Fluorine monohydroxide sodium are dissolved in 40ml fuming nitric aicds, stirred for 24 hours, by washing, 60 DEG C of dryings Afterwards, graphite oxide (GO) is obtained, it is spare;
After 200mg GO are scattered in 200ml deionized waters, 3- aminopropyls-tetraethoxysilane (2ml) is added thereto, After reflux for 24 hours, products therefrom obtains the graphite oxide GA-W of organic amine modification by centrifugation, washing, 60 DEG C of dryings, spare;
When temperature is 303K, the CO of GO and GA-W2Adsorbance is respectively 0.074mmolg-1And 1.64mmolg-1。

Claims (6)

1. a kind of CO absorption2Carbon material preparation method, include the following steps:
Tealeaves is placed in immersion 0.5h~1h in 80 DEG C~100 DEG C water, tealeaf residue is obtained after removing water, tealeaf residue is dried into postposition It is placed in Muffle furnace in small crucible, and by small crucible, with 3~5 DEG C of min-1Rate heats up, after tealeaf residue carbonization, With 3~5 DEG C of min-1Rate is cooled to room temperature to get to CO absorption2Carbon material.
2. CO absorption according to claim 12Carbon material preparation method, which is characterized in that the tealeaves be Anhua it is black Tea tealeaves or Anhua black tea leaf.
3. CO absorption according to claim 12Carbon material preparation method, which is characterized in that the carbonization method be rise Temperature is to holding 4h~6h after 300 DEG C, then is warming up to 400 DEG C of holding 4h~6h, is finally warming up to 500 DEG C of holding 4h~6h.
4. a kind of CO to described in claim 1-4 any one2Absorption carbon material carries out metal ion-modified method, including Following step:
By the CO absorption of metal salt and preparation2Carbon material be placed in polytetrafluoroethyllining lining, be added deionized water in stir it is molten Solution is subsequently placed in 100 DEG C~120 DEG C drying boxes and carries out hydro-thermal process 12h~for 24 hours, you can metal ion-modified carbon is made Material.
5. method of modifying according to claim 4, which is characterized in that the metal salt is ZrOCl2·8H2O or ZrO (NO3)2。
6. method of modifying according to claim 4, which is characterized in that the metal salt and CO absorption2Carbon material quality Than than [0.3~0.7]:1.
CN201810487386.1A 2018-05-07 2018-05-07 A kind of CO absorption2Carbon material preparation and method of modifying Pending CN108686617A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106943983A (en) * 2017-05-02 2017-07-14 湖南大学 A kind of CO absorption2Oxide ZrO2Preparation and method of modifying
CN106967858A (en) * 2017-05-10 2017-07-21 中冶华天工程技术有限公司 A kind of converter slag ladle movement system and technique

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106943983A (en) * 2017-05-02 2017-07-14 湖南大学 A kind of CO absorption2Oxide ZrO2Preparation and method of modifying
CN106967858A (en) * 2017-05-10 2017-07-21 中冶华天工程技术有限公司 A kind of converter slag ladle movement system and technique

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