CN112517069B - Photocatalytic active carbon aerogel material and preparation method thereof - Google Patents
Photocatalytic active carbon aerogel material and preparation method thereof Download PDFInfo
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- 239000004966 Carbon aerogel Substances 0.000 title claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 34
- 239000013081 microcrystal Substances 0.000 claims abstract description 21
- 239000004964 aerogel Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000003415 peat Substances 0.000 claims abstract description 10
- 239000002028 Biomass Substances 0.000 claims abstract description 8
- 238000004108 freeze drying Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 238000004132 cross linking Methods 0.000 claims abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 4
- 239000011941 photocatalyst Substances 0.000 claims abstract description 4
- 230000006641 stabilisation Effects 0.000 claims abstract description 4
- 238000011105 stabilization Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000003431 cross linking reagent Substances 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims description 6
- 229960002796 polystyrene sulfonate Drugs 0.000 claims description 6
- 239000011970 polystyrene sulfonate Substances 0.000 claims description 6
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical group [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001879 gelation Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 2
- 239000003054 catalyst Substances 0.000 claims 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- 239000002243 precursor Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 7
- 239000011148 porous material Substances 0.000 abstract description 6
- 239000003463 adsorbent Substances 0.000 abstract description 4
- 238000003763 carbonization Methods 0.000 abstract description 3
- 238000005087 graphitization Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000725 suspension Substances 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000013080 microcrystalline material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
-
- B01J35/39—
-
- B01J35/615—
-
- B01J35/647—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a photocatalytic active carbon aerogel material and a preparation method thereof, belonging to the field of inorganic non-metallic materials. The preparation method comprises the steps of respectively carrying out alkali washing, acidity and filtration on the biomass peat to remove inorganic mineral substances (ash), carrying out carbonization and graphitization calcination treatment in inert atmosphere, and then washing and drying to obtain the carbon microcrystal material. And (3) performing crosslinking stabilization treatment on the suspension of the carbon microcrystals, and performing freeze drying to obtain the three-dimensional carbon-based aerogel. Coating the surface of the carbon aerogel with the photocatalyst hydrosol to obtain the carbon aerogel with photocatalytic activity. Compared with the traditional carbon aerogel adsorbent, the carbon aerogel adsorbent can degrade organic pollutants adsorbed in an aerogel pore structure, thereby realizing the recycling of the composite material and greatly reducing the pollution treatment cost. The preparation process is simple, the raw materials are cheap and easy to obtain, and the prepared carbon aerogel material has good flexibility, photocatalytic activity and adsorption performance and has wide application prospect in the field of environment.
Description
Technical Field
The invention relates to a novel biomass-based photocatalytic active carbon aerogel material and a preparation method thereof, belonging to the field of inorganic non-metallic materials.
Background
As a novel carbon material, the carbon aerogel has a three-dimensional network structure, has the advantages of light weight, large specific surface area, porosity, visible light absorption, good conductivity, stable chemical performance and the like, and is widely applied to the fields of environment and energy. Functionalization of carbon aerogel is an effective way to improve performance and expand application of the carbon aerogel, and the development of a simple and convenient mass preparation method of functional carbon aerogel by using biomass raw materials with rich sources is still a major challenge in the field of carbon materials.
Disclosure of Invention
The invention aims to provide a novel biomass-based photocatalytic active carbon aerogel material; another object is to provide a process for the preparation thereof.
In order to realize the purpose of the invention, the technical scheme is as follows:
the biomass-based photocatalytic active carbon aerogel material is prepared by the following method:
(1) Biomass peat pretreatment: eluting with dilute alkali solution and dilute acid solution, respectively, and removing inorganic mineral substances from peat;
(2) Soaking the pretreated peat with potassium ferrate solution (to load potassium ferrate with catalytic activation), drying, placing in a tubular furnace, introducing nitrogen (or argon) as shielding gas, and calcining;
(3) Cooling to room temperature, adding hydrochloric acid solution, stirring, filtering, and washing with water to neutrality; drying overnight, and grinding to obtain graphitized carbon microcrystal powder;
(4) Adding the graphitized carbon microcrystal powder into a cross-linking agent solution under stirring, wherein the cross-linking agent adopts polyvinyl alcohol, polystyrene sulfonate or the combination of the polyvinyl alcohol and the polystyrene sulfonate, and performing cross-linking stabilization treatment to obtain hydrosol;
(5) Freeze-drying the hydrosol to obtain three-dimensional carbon microcrystal aerogel;
(6) Spin coating g-C 3 /N 4 /TiO 2 Uniformly spraying the photocatalyst hydrosol on the surface of the three-dimensional carbon microcrystal aerogel, and drying to obtain the functional carbon aerogel material with photocatalytic activity.
The potassium ferrate (K) 2 FeO 4 ) The concentration of the solution is preferably: 0.1mol/L;
the poly crosslinking agent is preferably a solution with a mass fraction of 5%.
In the step (1), the dilute alkali solution and the dilute acid solution are respectively 1mol/L sodium hydroxide and 1mol/L hydrochloric acid.
In the step (2), the roasting temperature is 800-900 ℃, the heating rate is 3-5 ℃/min, and the constant temperature time is 2h.
And (4) the concentration of the hydrochloric acid solution in the step (3) is 1mol/L.
And (5) carrying out quick-freezing treatment under liquid nitrogen before the freeze drying, and then carrying out freeze drying at-40 ℃.
The preferable preparation step of the hydrosol in the step (4): adding the graphitized carbon microcrystal powder into a mixed solution of glutaraldehyde, hydrochloric acid and polyvinyl alcohol, and carrying out gelation treatment for 24 hours.
The preferable preparation step of the hydrosol in the step (4): adding the graphitized carbon microcrystal powder into a cross-linking agent polystyrene sulfonate solution, and carrying out free radical polymerization reaction for 24 hours.
The preferable preparation step of the hydrosol in the step (4): adding the graphitized carbon microcrystal powder into a cross-linking agent solution consisting of polyvinyl alcohol and polystyrene sulfonate, and carrying out gelation treatment for 24 hours.
The invention constructs an adsorption-photocatalytic degradation synergistic action system based on carbon aerogel, the obtained carbon microcrystal material has both adsorption and photocatalytic properties, and compared with the traditional carbon aerogel adsorbent, the carbon aerogel adsorbent can degrade organic pollutants adsorbed in an aerogel pore structure, has long-term durability, can realize the recycling of composite materials, greatly reduces the pollution treatment cost, and is a promising approach for promoting solar water purification.
Compared with the prior art, the invention has the following advantages: the raw materials are low in price, the preparation process is simple, and the method is suitable for large-scale production. The obtained carbon microcrystalline material has good flexibility and large surface area (215 m) 2 More than g), good pore structure (more than 3.5nm on average), and verification shows excellent adsorption performance and remarkable photocatalytic activity, and has potential application prospects in the fields of adsorption, energy conversion and environment.
Drawings
FIG. 1 is a scanning electron micrograph of a sample of carbon crystallites prepared according to the present invention, wherein (a, b) -after carbonization, (c, d) -after graphitization;
FIG. 2 is an XRD analysis pattern of a sample of carbon crystallites prepared according to the present invention;
FIG. 3 is a Raman spectrum of a sample of carbon crystallites prepared according to the present invention;
fig. 4 is a sample object diagram of the carbon microcrystalline aerogel and the photocatalytic carbon microcrystalline aerogel prepared by the present invention, wherein: a-a carbon microcrystalline aerogel, b-a single-sided photocatalytic carbon microcrystalline aerogel;
fig. 5 shows the visible light performance and the reaction rate constant of the carbon microcrystal aerogel material prepared by the invention, wherein, a is a photocatalytic performance curve, and b is a first-order reaction kinetic rate constant.
Detailed Description
To better illustrate the invention, the following examples are given:
example 1
(1) Respectively adopting sodium hydroxide and hydrochloric acid solution with the concentration of 1mol/L to elute the peat and remove inorganic minerals, mechanically stirring for 1-2 hours, filtering and drying;
(2) Soaking the pretreated peat by 0.1mol/L potassium ferrate solution, drying, putting into a tubular furnace, introducing nitrogen (or argon) as a protective gas, heating at the speed of 3-5 ℃/min, and roasting at 800-900 ℃ for 1-2 hours;
(3) Cooling to room temperature, adding a 0.1mol/L hydrochloric acid solution, stirring, filtering, and washing with water to pH =7.0; drying at 80 ℃ overnight, and grinding to obtain a graphitized carbon microcrystal material;
(4) A polyvinyl alcohol (PVA) crosslinking agent is dissolved in water at 95 ℃ to prepare a solution with the mass fraction of 5%. Adding the prepared graphitized carbon microcrystal powder under stirring, and carrying out crosslinking stabilization treatment to obtain stable hydrosol;
(5) Freeze-drying the hydrosol at-40 ℃ to obtain the three-dimensional carbon microcrystal aerogel;
(6) Uniformly loading g-C on the surface of the carbon microcrystal aerogel by adopting a spin coating method 3 /N 4 /TiO 2 And (photocatalyst) hydrosol is dried at the temperature of 80 ℃ to prepare the carbon aerogel with visible light catalytic activity on one side.
The biomass carbon source peat is produced in Henan Hui county.
TABLE 1 analysis of specific surface area and pore size of carbon materials prepared according to the invention
| Sample (I) | Specific surface area (m) 2 /g) | Total pore volume of adsorption (cm) 3 /g) | Average pore diameter of adsorption (nm) |
| Carbonization (550 ℃ C.) | 215.605 | 0.195 | 3.579 |
| Graphitization (900 deg.C) | 405.675 | 0.119 | 2.392 |
Application example 1: application in the field of environmental photocatalysis
Performance evaluation experiment: the adopted sample is the photocatalytic carbon microcrystalline aerogel prepared by the invention. Using 500W xenon lamp and 420nm filter as visible light source, and using 1 × 10 -5 The Methylene Blue (MB) dye solution is used as degradation product. The performance evaluation experiment was performed on a photochemical reactor.
The method comprises the following specific operation steps: accurately weighing 25mg of the photocatalytic carbon microcrystalline aerogel disclosed by the invention, and dispersing the photocatalytic carbon microcrystalline aerogel into 50mL of MB solution to obtain suspension; and carrying out ultrasonic dispersion on the suspension for 10min, and stirring for 30min in a dark place. Then, a photoreaction was performed. The sampling interval is 20min, and the reaction time is 2h. After sampling, centrifugation was performed, and the supernatant was taken, and the absorbance was measured at an absorption wavelength λ =664 nm. The results of the reaction performance test are shown in FIG. 5. It shows strong adsorption property and obvious photocatalytic activity.
Claims (2)
1. A photocatalytically active carbon aerogel material, characterized by being produced by:
(1) Pretreatment of biomass peat: eluting with dilute alkali solution and dilute acid solution to remove inorganic minerals in peat;
(2) Soaking the pretreated peat by using a solution containing an iron catalyst, drying, putting into a tubular furnace, introducing nitrogen or argon as a protective gas, and controlling the heating rate to carry out roasting treatment;
(3) Cooling to room temperature, adding hydrochloric acid solution, stirring, filtering, and washing with water to neutrality; drying overnight, and grinding to obtain graphitized carbon microcrystal powder;
(4) Adding the graphitized carbon microcrystal powder into a cross-linking agent solution under stirring, and carrying out cross-linking stabilization treatment to obtain hydrosol;
(5) Freeze-drying the hydrosol to obtain the three-dimensional carbon microcrystal aerogel;
(6) Photocatalyst g-C was spin-coated 3 /N 4 /TiO 2 Uniformly spraying the hydrosol on the surface of the three-dimensional carbon microcrystal aerogel, and drying to obtain a photocatalytic carbon aerogel material;
the catalyst is selected from potassium ferrate;
the cross-linking agent is selected from polyvinyl alcohol, polystyrene sulfonate or a combination of the two;
the preparation step of the hydrosol in the step (4) comprises the following steps: adding the graphitized carbon microcrystal powder into a mixed solution containing glutaraldehyde, hydrochloric acid and polyvinyl alcohol, and performing gelation treatment; or adding the graphitized carbon microcrystal powder into the cross-linking agent C solution for gelation treatment; the cross-linking agent C is obtained by soaking polyvinyl alcohol in a polystyrene sulfonate precursor solution.
2. The photocatalytically active carbon aerogel material of claim 1, wherein the concentration of said potassium ferrate solution is selected from the group consisting of: 0.1mol/L; the cross-linking agent aqueous solution is a solution with the mass fraction of 5%.
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| CN107680833A (en) * | 2017-09-07 | 2018-02-09 | 中南大学 | The preparation method and carbon aerogels of a kind of carbon aerogels and its lithium-ion capacitor being prepared |
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| CN108479835A (en) * | 2018-03-20 | 2018-09-04 | 山东省科学院新材料研究所 | A kind of C (N)/g-C3N4/ PI aeroge composite photoelectric catalysis materials and preparation method thereof and its application |
| CN109158088A (en) * | 2018-09-06 | 2019-01-08 | 潘钕 | A kind of preparation method of cellulose aerogels adsorbent |
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| US20100190639A1 (en) * | 2009-01-28 | 2010-07-29 | Worsley Marcus A | High surface area, electrically conductive nanocarbon-supported metal oxide |
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| CN107680833A (en) * | 2017-09-07 | 2018-02-09 | 中南大学 | The preparation method and carbon aerogels of a kind of carbon aerogels and its lithium-ion capacitor being prepared |
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