CN108435168B - Visible light absorption and high-efficiency CO2Composite photocatalyst with adsorption and conversion performance and preparation method thereof - Google Patents
Visible light absorption and high-efficiency CO2Composite photocatalyst with adsorption and conversion performance and preparation method thereof Download PDFInfo
- Publication number
- CN108435168B CN108435168B CN201810367078.5A CN201810367078A CN108435168B CN 108435168 B CN108435168 B CN 108435168B CN 201810367078 A CN201810367078 A CN 201810367078A CN 108435168 B CN108435168 B CN 108435168B
- Authority
- CN
- China
- Prior art keywords
- adsorption
- visible light
- composite photocatalyst
- preparation
- stirring
- 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.)
- Expired - Fee Related
Links
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 61
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 230000031700 light absorption Effects 0.000 title claims abstract description 28
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000002131 composite material Substances 0.000 claims abstract description 56
- 238000003756 stirring Methods 0.000 claims abstract description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000001035 drying Methods 0.000 claims abstract description 35
- 239000002135 nanosheet Substances 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 31
- 238000005406 washing Methods 0.000 claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 29
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002028 Biomass Substances 0.000 claims abstract description 10
- 229910052724 xenon Inorganic materials 0.000 claims abstract description 10
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920002488 Hemicellulose Polymers 0.000 claims abstract description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract 2
- 239000000047 product Substances 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 22
- 230000004913 activation Effects 0.000 claims description 9
- 230000001699 photocatalysis Effects 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
- 238000007146 photocatalysis Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 description 37
- 229910021641 deionized water Inorganic materials 0.000 description 37
- 101710134784 Agnoprotein Proteins 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 230000001678 irradiating effect Effects 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8671—Removing components of defined structure not provided for in B01D53/8603 - B01D53/8668
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Electromagnetism (AREA)
- Optics & Photonics (AREA)
- Toxicology (AREA)
- Thermal Sciences (AREA)
- Plasma & Fusion (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The invention relates to visible light absorption and high-efficiency CO2A preparation method of a composite photocatalyst with adsorption and conversion performances, belonging to CO2The field of photocatalyst preparation. The method comprises the following steps: 1) dispersing the biomass residue after extracting the hemicellulose into water, and then placing the biomass residue in a high-pressure reaction kettle for reaction to obtain hydrothermal carbon; 2) activating the hydrothermal carbon in the step 1) in phosphoric acid; 3) placing the hydrothermal carbon activated by the phosphoric acid in the step 2) into a heating furnace for roasting; 4) placing the hydrothermal carbon roasted in the step 3) in concentrated hydrochloric acid for reaction to obtain AC; 5) adding TiO into the mixture2Dispersing the nanosheet and the AC in the step 4) into water respectively, then mixing the two solutions, performing ultrasonic treatment, washing and drying to obtain TiO2an/AC complex; 6) adding TiO into the mixture2Dispersing the/AC complex into an aqueous solution, adding AgNO3Stirring the solution for a period of time, and then illuminating the solution with a xenon lamp while stirring to obtain TiO2the/AC/Ag composite photocatalyst. The composite photocatalyst prepared by the invention has good visible light absorption and high-efficiency CO2Adsorption and light conversion ability.
Description
Technical Field
The invention belongs to CO2The field of photocatalyst preparation, in particular to a photocatalyst with visible light absorption and high-efficiency CO2A composite photocatalyst with adsorption and conversion performance and a preparation method thereof.
Background
In recent years, photocatalytic conversion of CO2Has attracted people's attention for organic matters with high added values. This study has potential application value: in solving CO2At the same time of the greenhouse effect of the gas, organic matters with high added value are generated to solve the increasingly severe energy problem. At present, it has been found that many photocatalysts have been found to have good CO2Light-converting properties, e.g. TiO2、ZnS、 ZnIn2S4、C3N4、BiVO4Etc.; especially TiO2The photocatalyst has good chemical stability, no toxicity, low price, chemical corrosion resistance and the like, and is regarded as the most promising and widely applied photocatalyst. However, due to TiO2The composite material is a wide band gap composite material, and can only absorb the ultraviolet light part (about 4 percent of the total sunlight) in the sunlight, thus the utilization rate of the sunlight is severely limited, and the CO is directly limited2Further improvement of light conversion performance; in addition, TiO2The separation efficiency of self photoproduction electrons and holes is too low and the reaction substance CO is generated2Too poor adsorption capacity of the gas also directly leads to low CO2Light conversion efficiency; thereby realizing TiO2Can absorb visible light even in full light and CO2The increase in adsorption capacity and efficient separation of photogenerated electrons and holes is TiO2Photocatalyst for light conversion of CO2Is an important challenge in the high value added organic industry.
At present, the improvement of TiO2CO of2The method for improving the adsorption capacity mainly comprises the steps of preparing a hollow structure and an ultrathin layer to increase the specific surface area so as to improve the CO2Adsorption of (2), but the process is on CO2The improvement of the adsorption capacity is limited. Therefore, there is a need to develop a new method for CO enhancement2Thereby increasing the CO content of the photocatalyst2Light conversion capability.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide visible light absorption and high-efficiency CO2Adsorption capacity and high efficiency of CO2A composite photocatalyst with conversion performance and a preparation method thereof.The composite photocatalyst prepared by the invention has good visible light absorption capacity and high-efficiency CO2The adsorption and light conversion capability of the catalyst is greatly improved by using the Active Carbon (AC) prepared by the biomass2Adsorption performance while achieving TiO via good conductivity of AC2The effective space separation of the photoproduction electrons and the holes is carried out, and then the visible light absorption of the composite photocatalyst is realized by the surface plasma effect of Ag, so as to improve the TiO2CO of2The adsorption capacity and the carrier separation efficiency and the more effective sunlight utilization rate are simultaneously displayed, and a new way is provided.
One of the objectives of the present invention is to provide a visible light absorption and high efficiency CO2A preparation method of a composite photocatalyst with adsorption and conversion performances.
The second purpose of the invention is to provide a visible light absorption and high efficiency CO2A composite photocatalyst with adsorption and conversion performances.
It is another object of the present invention to provide visible light absorption and high efficiency CO2A composite photocatalyst with adsorption and conversion performance and an application of a preparation method thereof.
In order to achieve the above purpose, the invention specifically discloses the following technical scheme:
firstly, the invention discloses visible light absorption and high-efficiency CO2The preparation method of the composite photocatalyst with adsorption and conversion performance comprises the following steps:
(1) dispersing the biomass residue after extracting hemicellulose into water, then carrying out reaction, washing and drying a reaction product to obtain hydrothermal carbon;
(2) putting the hydrothermal carbon in the step (1) into phosphoric acid for activation, fully stirring and drying;
(3) placing the hydrothermal carbon activated by phosphoric acid in the step (2) in a heating furnace, and roasting in a protective atmosphere;
(4) placing the hydrothermal carbon roasted in the step (3) in concentrated hydrochloric acid, stirring, washing and drying to obtain AC;
(5) adding TiO into the mixture2Dispersing the nanosheets and the AC in step (4) into water respectivelyStirring at room temperature to obtain TiO2 nanosheet liquid and AC solution, slowly adding the TiO2 nanosheet liquid into the AC solution, performing ultrasonic treatment, washing and drying to obtain TiO2an/AC complex;
(6) adding TiO into the mixture2Dispersing the/AC complex into an aqueous solution, adding AgNO3Stirring the solution for a period of time, then illuminating the solution for a period of time by using a xenon lamp while stirring, washing and drying the product in vacuum to obtain TiO2the/AC/Ag composite photocatalyst.
Preferably, in the step (1), the biomass residue is corncob residue.
Preferably, in the step (1), the mass ratio of the biomass residue to the water is (1-3): (10-30).
Preferably, in the step (1), the reaction is carried out in a high-pressure reaction kettle, the reaction temperature is 250 ℃, and the reaction time is 4-8 h.
Preferably, in the step (2), the phosphoric acid is 40% by mass.
Preferably, in the step (2), the stirring time is 60 min.
Preferably, in the step (3), the roasting temperature is 300-.
Preferably, in the step (4), the stirring time is 1 h.
Preferably, in the step (5), the stirring time at room temperature is 20 min.
Preferably, in the step (5), the ultrasonic time interval is 10-30 min.
Preferably, in step (6), the AgNO is3The concentration of the solution is 1 percent by mass.
Preferably, in the step (6), the time for stirring is 10 min.
Preferably, in the step (6), the illumination time is 10-30 min.
Secondly, the invention discloses visible light absorption and high-efficiency CO2A composite photocatalyst with adsorption and conversion performances.
Finally, the invention discloses visible light absorption and efficient CO2Combination of adsorption and conversion propertiesThe application of the photocatalyst and the preparation method thereof in the field of photocatalysis.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention prepares TiO2The method of the/AC/Ag composite catalyst adopts green biomass residues as the raw material of the activated carbon, has low cost and is environment-friendly, and the synthesis method is simple.
2. The preparation method of the invention enhances CO of the catalyst by virtue of the characteristics of AC2Adsorption capacity and realizes effective space separation of photo-generated electron and hole pairs, and is TiO2To CO2The improvement of the adsorption capacity provides a new approach.
3. The preparation method of the invention utilizes the surface plasma effect of Ag to obtain high-efficiency CO2Adsorption capacity of TiO2the/AC complex also obtains the capability of absorbing visible light and is TiO2Synergistic CO2The increase of the adsorption capacity and the light absorption provides a new approach and an improved idea.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
FIG. 1 shows TiO prepared in example 1 of the present invention2X-ray diffraction pattern of/AC/Ag composite photocatalyst.
FIG. 2 shows TiO prepared in example 2 of the present invention2X-ray diffraction pattern of/AC complex.
FIG. 3 shows TiO prepared in example 1 of the present invention2SEM image of/AC/Ag composite photocatalyst.
FIG. 4 shows TiO prepared in example 2 of the present invention2SEM image of/AC/Ag composite photocatalyst.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As described in the background section, the prior art for improving TiO compounds2CO of2Method of adsorption Capacity on CO2The improvement of the adsorption capacity is limited, therefore, the invention provides visible light absorption and high-efficiency CO2The invention relates to a composite photocatalyst with adsorption and conversion performance and a preparation method thereof, and the invention is further described by combining the attached drawings and the specific embodiment.
Example 1
Visible light absorption and high-efficiency CO2The preparation method of the composite photocatalyst with adsorption and conversion performance comprises the following steps:
(1) dispersing 7g of corncob residues after hemicellulose is extracted into 70ml of deionized water, continuously stirring to uniformly disperse the corncob residues, then pouring the mixed solution into a high-pressure reaction kettle with the volume of 100ml, reacting for 4 hours at 250 ℃, cooling at room temperature, respectively washing the product with the deionized water and absolute ethyl alcohol for 3 times, and drying for 12 hours to obtain hydrothermal carbon;
(2) putting the hydrothermal carbon in the step (1) into concentrated phosphoric acid with the mass fraction of 40% for activation, stirring for 1h, and drying for 12 h;
(3) putting the hydrothermal carbon activated by phosphoric acid in the step (2) into a tube furnace, and adding N2Roasting at 400 ℃ for 4h under the protection of atmosphere;
(4) placing the hydrothermal carbon roasted in the step (3) in concentrated hydrochloric acid with the mass fraction of 38%, stirring for 60min, washing a product with deionized water, and drying to obtain AC;
(5) 5g of TiO are taken2Nanosheet and 2g in step (4)Respectively dispersing the AC into 100ml of deionized water, stirring for 20min at room temperature to obtain TiO2 nanosheet liquid and AC solution, slowly adding the TiO2 nanosheet liquid into the AC solution, performing ultrasonic treatment for 30min, washing the product with deionized water, and drying to obtain TiO2 nanosheet liquid2an/AC complex;
(6) 5g of TiO in step (5) are taken2Dispersing the/AC compound into 50ml of deionized water, and then adding AgNO with the mass fraction of 1%3Stirring the solution for 10min, irradiating with xenon lamp for 30min while stirring, washing the product, and vacuum drying to obtain TiO2the/AC/Ag composite photocatalyst.
Example 2
Visible light absorption and high-efficiency CO2The preparation method of the composite photocatalyst with adsorption and conversion performance comprises the following steps:
(1) dispersing 6g of corncob residues after hemicellulose is extracted into 60ml of deionized water, continuously stirring to uniformly disperse the corncob residues, then pouring the mixed solution into a high-pressure reaction kettle with the volume of 100ml, reacting for 5 hours at 250 ℃, cooling at room temperature, respectively washing the product with the deionized water and absolute ethyl alcohol for 3 times, and drying for 12 hours to obtain hydrothermal carbon;
(2) putting the hydrothermal carbon in the step (1) into concentrated phosphoric acid with the mass fraction of 40% for activation, stirring for 60min, and drying for 12 h;
(3) putting the hydrothermal carbon activated by phosphoric acid in the step (2) into a tube furnace, and adding N2Roasting at 500 ℃ for 5 hours under the protection of atmosphere;
(4) placing the hydrothermal carbon roasted in the step (3) in concentrated hydrochloric acid with the mass fraction of 38%, stirring for 60min, washing a product with deionized water, and drying to obtain AC;
(5) 5g of TiO are taken2Dispersing the nano sheet and 2g of the AC in the step (4) into 100ml of deionized water respectively, stirring at room temperature for 20min to obtain TiO2 nano sheet liquid and an AC solution, then slowly adding the TiO2 nano sheet liquid into the AC solution, performing ultrasonic treatment for 20min, cleaning a product with deionized water, and drying to obtain TiO2 nano sheet liquid2an/AC complex;
(6) 5g of TiO in step (5) are taken2/AC Complex DispersionAdding into 50ml deionized water, and adding AgNO with mass fraction of 1%3Stirring the solution for 10min, irradiating with xenon lamp for 20min while stirring, washing the product, and vacuum drying to obtain TiO2the/AC/Ag composite photocatalyst.
Example 3
Visible light absorption and high-efficiency CO2The preparation method of the composite photocatalyst with adsorption and conversion performance comprises the following steps:
(1) dispersing 5g of corncob residues after hemicellulose is extracted into 50ml of deionized water, continuously stirring to uniformly disperse the corncob residues, then pouring the mixed solution into a high-pressure reaction kettle with the volume of 100ml, reacting for 8 hours at 250 ℃, cooling at room temperature, respectively washing the product with the deionized water and absolute ethyl alcohol for 3 times, and drying for 12 hours to obtain hydrothermal carbon;
(2) putting the hydrothermal carbon in the step (1) into concentrated phosphoric acid with the mass fraction of 40% for activation, stirring for 60min, and drying for 12 h;
(3) putting the hydrothermal carbon activated by phosphoric acid in the step (2) into a tube furnace, and adding N2Roasting at 800 ℃ for 7h under the protection of atmosphere;
(4) placing the hydrothermal carbon roasted in the step (3) in concentrated hydrochloric acid with the mass fraction of 38%, stirring for 60min, washing a product with deionized water, and drying to obtain AC;
(5) take 4g of TiO2Dispersing the nano sheet and 1g of the AC in the step (4) into 100ml of deionized water respectively, stirring at room temperature for 20min to obtain TiO2 nano sheet liquid and an AC solution, then slowly adding the TiO2 nano sheet liquid into the AC solution, carrying out ultrasonic treatment for 10min, washing a product with deionized water, and drying to obtain TiO2 nano sheet liquid2an/AC complex;
(6) taking 4g of TiO in the step (5)2Dispersing the/AC compound into 50ml of deionized water, and then adding AgNO with the mass fraction of 1%3Stirring the solution for 10min, irradiating with xenon lamp for 10min while stirring, washing the product, and vacuum drying to obtain TiO2the/AC/Ag composite photocatalyst.
Example 4
Visible light absorption and high efficiencyCO2The preparation method of the composite photocatalyst with adsorption and conversion performance comprises the following steps:
(1) dispersing 8g of corncob residues after hemicellulose is extracted into 80ml of deionized water, continuously stirring to uniformly disperse the corncob residues, then pouring the mixed solution into a high-pressure reaction kettle with the volume of 100ml, reacting for 7 hours at 250 ℃, cooling at room temperature, respectively washing the product with the deionized water and absolute ethyl alcohol for 3 times, and drying for 12 hours to obtain hydrothermal carbon;
(2) putting the hydrothermal carbon in the step (1) into concentrated phosphoric acid with the mass fraction of 40% for activation, stirring for 60min, and drying for 12 h;
(3) putting the hydrothermal carbon activated by phosphoric acid in the step (2) into a tube furnace, and adding N2Roasting at 700 ℃ for 8h under the protection of atmosphere;
(4) placing the hydrothermal carbon roasted in the step (3) in concentrated hydrochloric acid with the mass fraction of 38%, stirring for 60min, washing a product with deionized water, and drying to obtain AC;
(5) 6g of TiO are taken2Dispersing the nano sheet and 2g of the AC in the step (4) into 100ml of deionized water respectively, stirring at room temperature for 20min to obtain TiO2 nano sheet liquid and an AC solution, then slowly adding the TiO2 nano sheet liquid into the AC solution, carrying out ultrasonic treatment for 15min, washing a product with deionized water, and drying to obtain TiO2 nano sheet liquid2an/AC complex;
(6) taking 6g of TiO in the step (5)2Dispersing the/AC compound into 50ml of deionized water, and then adding AgNO with the mass fraction of 1%3Stirring the solution for 10min, irradiating with xenon lamp for 15min while stirring, washing the product, and vacuum drying to obtain TiO2the/AC/Ag composite photocatalyst.
Example 5
Visible light absorption and high-efficiency CO2The preparation method of the composite photocatalyst with adsorption and conversion performance comprises the following steps:
(1) dispersing 5g of corncob residues after hemicellulose is extracted into 150ml of deionized water, continuously stirring to uniformly disperse the corncob residues, then pouring the mixed solution into a high-pressure reaction kettle with the volume of 100ml, reacting for 6 hours at 250 ℃, cooling at room temperature, respectively washing the product with the deionized water and absolute ethyl alcohol for 3 times, and drying for 12 hours to obtain hydrothermal carbon;
(2) putting the hydrothermal carbon in the step (1) into concentrated phosphoric acid with the mass fraction of 40% for activation, stirring for 60min, and drying for 12 h;
(3) putting the hydrothermal carbon activated by phosphoric acid in the step (2) into a tube furnace, and adding N2Roasting at 300 ℃ for 8h under the protection of atmosphere;
(4) placing the hydrothermal carbon roasted in the step (3) in concentrated hydrochloric acid with the mass fraction of 38%, stirring for 60min, washing a product with deionized water, and drying to obtain AC;
(5) take 4g of TiO2Dispersing the nano sheet and 1g of AC in the step (4) into 100ml of deionized water respectively, stirring at room temperature for 20min to obtain TiO2 nano sheet liquid and AC solution, then slowly adding the TiO2 nano sheet liquid into the AC solution, performing ultrasonic treatment for 25min, cleaning the product with deionized water, and drying to obtain TiO2 nano sheet liquid2an/AC complex;
(6) taking 6g of TiO in the step (5)2Dispersing the/AC compound into 50ml of deionized water, and then adding AgNO with the mass fraction of 1%3Stirring the solution for 10min, irradiating with xenon lamp for 25min while stirring, washing the product, and vacuum drying to obtain TiO2the/AC/Ag composite photocatalyst.
Example 6
Visible light absorption and high-efficiency CO2The preparation method of the composite photocatalyst with adsorption and conversion performance comprises the following steps:
(1) dispersing 30g of corncob residues after hemicellulose is extracted into 100ml of deionized water, continuously stirring to uniformly disperse the corncob residues, then pouring the mixed solution into a high-pressure reaction kettle with the volume of 100ml, reacting for 6 hours at 250 ℃, cooling at room temperature, respectively washing the product with the deionized water and absolute ethyl alcohol for 3 times, and drying for 12 hours to obtain hydrothermal carbon;
(2) putting the hydrothermal carbon in the step (1) into concentrated phosphoric acid with the mass fraction of 40% for activation, stirring for 60min, and drying for 12 h;
(3) water after phosphoric acid activation in the step (2)The hot char is placed in a tube furnace at N2Roasting for 6 hours at 400 ℃ under the protection of atmosphere;
(4) placing the hydrothermal carbon roasted in the step (3) in concentrated hydrochloric acid with the mass fraction of 38%, stirring for 60min, washing a product with deionized water, and drying to obtain AC;
(5) take 4g of TiO2Dispersing the nano sheet and 1g of AC in the step (4) into 100ml of deionized water respectively, stirring for 15min at room temperature to obtain TiO2 nano sheet liquid and AC solution, then slowly adding the TiO2 nano sheet liquid into the AC solution, performing ultrasonic treatment for 20min, cleaning the product with deionized water, and drying to obtain TiO2 nano sheet liquid2an/AC complex;
(6) taking 6g of TiO in the step (5)2Dispersing the/AC compound into 50ml of deionized water, and then adding AgNO with the mass fraction of 1%3Stirring the solution for 10min, irradiating with xenon lamp for 20min while stirring, washing the product, and vacuum drying to obtain TiO2the/AC/Ag composite photocatalyst.
And (3) performance testing:
TiO prepared in example 1 and example 2 was analyzed by PCA-1100 gas adsorption Analyzer2CO of/AC/Ag composite photocatalyst2The adsorption performance was tested. The TiO prepared in example 1 and example 2 was treated with a photocatalytic system2CO of/AC/Ag composite photocatalyst sample2The light conversion performance was evaluated using a 300W xenon lamp as the light source. The test method comprises the following steps: weighing 0.1g of a composite photocatalyst sample, dispersing the sample in 100mL of deionized water, and introducing high-purity CO2Gas was turned on for 30min, then light was turned on and 1mL was sampled every 1h and the product species and content were analyzed by mass spectrometry and gas chromatography. The result shows that the composite photocatalyst prepared by the invention has good visible light absorption capacity and high-efficiency CO2Adsorption and light conversion ability.
For TiO prepared in example 12Composite photocatalyst of/AC/Ag and TiO prepared in example 22XRD testing of the/AC complex is carried out, and the results are shown in figures 1 and 3. As can be seen from the figure: TiO22Composite photocatalyst of/AC/Ag and TiO2Diffraction peaks of the/AC complex were in combination with anatase TiO2Standard card (JCPDS file)No.21-1272), which shows that TiO is successfully grown on the AC surface2。
The TiO prepared in example 1 and example 2 was examined under SEM2The results of the observation of the/AC/Ag composite photocatalyst are shown in figures 3 and 4. As can be seen from the figure: the surface of AC is uniformly loaded with a large amount of TiO2Nanosheets.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (13)
1. Visible light absorption and high-efficiency CO2The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: the method comprises the following steps:
(1) dispersing the biomass residue after extracting hemicellulose into water, then carrying out reaction, washing and drying a reaction product to obtain hydrothermal carbon;
(2) putting the hydrothermal carbon in the step (1) into phosphoric acid for activation, fully stirring and drying;
(3) placing the hydrothermal carbon activated by phosphoric acid in the step (2) in a heating furnace, and roasting in a protective atmosphere;
(4) placing the hydrothermal carbon roasted in the step (3) in concentrated hydrochloric acid, stirring, washing and drying to obtain active carbon, namely AC;
(5) adding TiO into the mixture2Dispersing the nanosheets and the AC in the step (4) into water respectively, and stirring at room temperature to obtain TiO2Nanosheet liquid and AC solution, followed by mixing the TiO2Slowly adding the nanosheet liquid into the AC solution, performing ultrasonic treatment, washing and drying to obtain TiO2an/AC complex;
(6) adding TiO into the mixture2Dispersing the/AC complex into an aqueous solution, adding AgNO3Stirring the solution for a period of time, then illuminating the solution for a period of time by using a xenon lamp while stirring, washing and drying the product in vacuum to obtain TiO2a/AC/Ag composite photocatalyst;
in the step (1), the biomass residue is corncob residue;
in the step (6), the illumination time is 10-30 min.
2. The visible light absorbing and CO-efficient of claim 12The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: the mass ratio of the biomass residues to the water is 1-3: 10-30.
3. The visible light absorbing and CO-efficient of claim 12The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: in the step (1), the reaction is carried out in a high-pressure reaction kettle, the reaction temperature is 250 ℃, and the reaction time is 4-8 h.
4. The visible light absorbing and CO-efficient of claim 12The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: in the step (2), the mass fraction of the phosphoric acid is 40%.
5. The visible light absorbing and CO-efficient of claim 12The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: in the step (2), the stirring time is 60 min.
6. The visible light absorbing and CO-efficient of claim 12The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: in the step (3), the roasting temperature is 300-800 ℃, and the roasting time is 4-8 h.
7. The visible light absorbing and CO-efficient of claim 12The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: in the step (4), the stirring time is 1 h.
8. Such as rightThe visible light absorption and high efficiency CO according to claim 12The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: in the step (5), the stirring time at room temperature is 20 min.
9. The visible light absorbing and CO-efficient of claim 12The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: in the step (5), the ultrasonic time is 10-30 min.
10. The visible light absorbing and CO-efficient of claim 12The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: in the step (6), the AgNO3The concentration of the solution is 1 percent by mass.
11. The visible light absorbing and CO-efficient of claim 12The preparation method of the composite photocatalyst with adsorption and conversion performance is characterized in that: in the step (6), the stirring time is 10 min.
12. The visible light absorbing and CO-efficient composition of any of claims 1-112Visible light absorption and efficient CO prepared by preparation method of composite photocatalyst with adsorption and conversion performance2A composite photocatalyst with adsorption and conversion performances.
13. The visible light absorbing and high efficiency CO of any one of claims 1-112Visible light absorption and efficient CO obtained by preparation method of composite photocatalyst with adsorption and conversion performance2Composite photocatalyst with adsorption and conversion properties or visible light absorption and high efficiency CO according to claim 122The application of the composite photocatalyst with adsorption and conversion performance in the field of photocatalysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810367078.5A CN108435168B (en) | 2018-04-23 | 2018-04-23 | Visible light absorption and high-efficiency CO2Composite photocatalyst with adsorption and conversion performance and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810367078.5A CN108435168B (en) | 2018-04-23 | 2018-04-23 | Visible light absorption and high-efficiency CO2Composite photocatalyst with adsorption and conversion performance and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108435168A CN108435168A (en) | 2018-08-24 |
| CN108435168B true CN108435168B (en) | 2021-04-13 |
Family
ID=63200702
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810367078.5A Expired - Fee Related CN108435168B (en) | 2018-04-23 | 2018-04-23 | Visible light absorption and high-efficiency CO2Composite photocatalyst with adsorption and conversion performance and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108435168B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113769726B (en) * | 2021-08-16 | 2023-09-26 | 常州大学 | Preparation method and application of rare earth vanadate quantum dot/biochar nanosheet composite photocatalytic material |
| CN114160129A (en) * | 2021-11-19 | 2022-03-11 | 西安理工大学 | Preparation method of titanium dioxide/porous carbon supported composite photocatalyst |
| CN117205919B (en) * | 2023-11-09 | 2024-03-05 | 潍坊学院 | Photo-thermal CO with full spectrum 2 Catalyst with catalytic hydrogenation activity and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1490079A (en) * | 2003-09-01 | 2004-04-21 | 武汉理工大学 | High-adsorbability glass beads with photocatalysis function |
| CN1973736A (en) * | 2006-12-11 | 2007-06-06 | 张国栋 | Water purifying column of active carbon with supported Ag and photocatalytic TiO2 for household drinking water machine |
| CN101905154A (en) * | 2010-08-20 | 2010-12-08 | 中国林业科学研究院林产化学工业研究所 | Method for improving efficiency of visible light response doping-type M-TiO2/AC photocatalyst |
| CN106512941A (en) * | 2016-11-30 | 2017-03-22 | 安吉云界生物科技有限公司 | Composite nanometer titanium dioxide and active carbon adsorbent |
-
2018
- 2018-04-23 CN CN201810367078.5A patent/CN108435168B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1490079A (en) * | 2003-09-01 | 2004-04-21 | 武汉理工大学 | High-adsorbability glass beads with photocatalysis function |
| CN1973736A (en) * | 2006-12-11 | 2007-06-06 | 张国栋 | Water purifying column of active carbon with supported Ag and photocatalytic TiO2 for household drinking water machine |
| CN101905154A (en) * | 2010-08-20 | 2010-12-08 | 中国林业科学研究院林产化学工业研究所 | Method for improving efficiency of visible light response doping-type M-TiO2/AC photocatalyst |
| CN106512941A (en) * | 2016-11-30 | 2017-03-22 | 安吉云界生物科技有限公司 | Composite nanometer titanium dioxide and active carbon adsorbent |
Non-Patent Citations (2)
| Title |
|---|
| Preparation and CO2 adsorption properties of soft-templated mesoporous carbons derived from chestnut tannin precursors;Kimberly M. Nelson et al.;《Microporous and Mesoporous Materials》;20151009;第222卷;第12页第2.3节 * |
| Synthesis of Ag or Pt nanoparticle-deposited TiO2 nanorods for the highly efficient photoreduction of CO2 to CH4;Qingli Wang et al.;《Chemical Physics Letters》;20150903;第639卷;第95页第2.2节 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108435168A (en) | 2018-08-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110116988B (en) | Preparation method for producing hydrogen by photolyzing water | |
| CN108855076B (en) | Ag/ZnO composite photocatalyst and preparation method and application thereof | |
| Qiu et al. | Enhanced visible-light-driven photocatalytic degradation of tetracycline by 16% Er3+-Bi2WO6 photocatalyst | |
| CN109482152B (en) | Metal oxide composite nano material based on eggshell membrane template, and preparation method and application thereof | |
| CN108435168B (en) | Visible light absorption and high-efficiency CO2Composite photocatalyst with adsorption and conversion performance and preparation method thereof | |
| Khairol et al. | Excellent performance integrated both adsorption and photocatalytic reaction toward degradation of congo red by CuO/eggshell | |
| CN109569684B (en) | Plasma modified metal oxide and g-carbon nitride co-modified titanium dioxide nanorod composite photocatalyst as well as preparation method and application thereof | |
| CN106140242B (en) | A kind of visible-light response type boron nitride modification carbon nitride photocatalyst and its preparation method and application | |
| CN113262808B (en) | Water-soluble graphite-phase carbon nitride nanosheet catalyst for efficiently removing formaldehyde at room temperature and preparation method thereof | |
| CN107486152B (en) | A kind of preparation method and application of leaf based biomass carbon aerogels | |
| CN106881059A (en) | A kind of preparation method of iron/carbon composite | |
| CN110624566B (en) | CuInS2Preparation method and application of quantum dot/NiAl-LDH composite photocatalyst | |
| WO2017219382A1 (en) | Double-layer zno hollow sphere photocatalytic material and method for preparing same | |
| CN110152711A (en) | A kind of CeO2@MoS2/g-C3N4Three-element composite photocatalyst and preparation method thereof | |
| CN111437867A (en) | Composite photocatalyst containing tungsten oxide and preparation method and application thereof | |
| CN109126714B (en) | TiO 22/SiO2-banana peel biochar composite adsorption material and preparation method thereof | |
| CN114054019B (en) | Lithium, manganese and titanium composite oxide photocatalyst, preparation method and application thereof | |
| Ping et al. | Flexible TiO2 nanograss array film decorated with oxygen vacancies introduced by facile chemical reduction and their photocatalytic activity | |
| CN114570352A (en) | W18O49/ZnTiO3Nitrogen fixation photocatalyst and preparation method and application thereof | |
| CN109126700A (en) | A kind of preparation method and application of graphene/calcium and magnesium aluminum hydrotalcite composite material | |
| CN106902760B (en) | A kind of eggshell load zinc oxide material and its preparation method and application | |
| CN110935441B (en) | Titanium-based composite catalytic net for efficiently degrading formaldehyde and preparation method thereof | |
| CN105944745B (en) | A kind of titanium dioxide nanometer microballoons and its preparation method and application | |
| CN104475024B (en) | Heavy metal absorbent and its application prepared by a kind of utilization water hyacinth | |
| CN109289863A (en) | The preparation and its application in low concentration ozone decomposition of a kind of efficiently water-fast Copper-cladding Aluminum Bar manganese-based catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| 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: 20210413 |