CN109999835B - Carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material and preparation method and application thereof - Google Patents
Carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material and preparation method and application thereof Download PDFInfo
- Publication number
- CN109999835B CN109999835B CN201910239364.8A CN201910239364A CN109999835B CN 109999835 B CN109999835 B CN 109999835B CN 201910239364 A CN201910239364 A CN 201910239364A CN 109999835 B CN109999835 B CN 109999835B
- Authority
- CN
- China
- Prior art keywords
- bacterial cellulose
- cadmium sulfide
- sulfide composite
- preparation
- photocatalytic material
- 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.)
- Active
Links
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 31
- 230000001580 bacterial effect Effects 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920002749 Bacterial cellulose Polymers 0.000 claims abstract description 28
- 239000005016 bacterial cellulose Substances 0.000 claims abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001257 hydrogen Substances 0.000 claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 239000004964 aerogel Substances 0.000 claims abstract description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 6
- 239000012498 ultrapure water Substances 0.000 claims abstract description 6
- 239000001963 growth medium Substances 0.000 claims abstract description 4
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract 3
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000000047 product Substances 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 6
- AUIZLSZEDUYGDE-UHFFFAOYSA-L cadmium(2+);diacetate;dihydrate Chemical compound O.O.[Cd+2].CC([O-])=O.CC([O-])=O AUIZLSZEDUYGDE-UHFFFAOYSA-L 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 244000235858 Acetobacter xylinum Species 0.000 claims description 3
- 235000002837 Acetobacter xylinum Nutrition 0.000 claims description 3
- 239000007640 basal medium Substances 0.000 claims description 3
- 229940041514 candida albicans extract Drugs 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 239000012137 tryptone Substances 0.000 claims description 3
- 239000012138 yeast extract Substances 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 abstract description 12
- 241000032681 Gluconacetobacter Species 0.000 abstract 1
- 238000012258 culturing Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 6
- 239000003575 carbonaceous material Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000011941 photocatalyst Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000004310 lactic acid Substances 0.000 description 3
- 235000014655 lactic acid Nutrition 0.000 description 3
- 238000013032 photocatalytic reaction Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- LPEKGGXMPWTOCB-UHFFFAOYSA-N 8beta-(2,3-epoxy-2-methylbutyryloxy)-14-acetoxytithifolin Natural products COC(=O)C(C)O LPEKGGXMPWTOCB-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- ODQWQRRAPPTVAG-GZTJUZNOSA-N doxepin Chemical compound C1OC2=CC=CC=C2C(=C/CCN(C)C)/C2=CC=CC=C21 ODQWQRRAPPTVAG-GZTJUZNOSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229940057867 methyl lactate Drugs 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000002834 transmittance 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/39—
-
- 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
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention relates to a carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material and a preparation method and application thereof. The photocatalytic material is prepared by the following method: 1) gluconacetobacter xylinusGluconacetobacter xylinusInoculating the strain in a culture medium A, dynamically culturing for 96h, collecting a bacterial cellulose product, washing and drying the bacterial cellulose product, and then carrying out vacuum freeze drying to obtain a bacterial cellulose aerogel; 2) dissolving quantitative thiourea and cadmium sulfide in ultrapure water, adding a proper amount of bacterial cellulose aerogel, and carrying out hydrothermal reaction at high temperature and high pressure; 3) and (3) calcining the bacterial cellulose-cadmium sulfide composite product at high temperature in a tubular furnace to obtain the carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material. The preparation method has the advantages of simple operation, low cost and the like. The obtained carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material can be used as a catalyst in the photocatalytic water splitting hydrogen production.
Description
Technical Field
The invention relates to a carbon fiber-cadmium sulfide composite photocatalytic material and a preparation method and application thereof.
Background
Since the twenty-first century, with the rapid development of science and technology, the productivity is remarkably improved, and huge wealth is created for human beings. People create wealth by utilizing science and technology, and simultaneously bring a series of problems of excessive energy consumption, serious ecological environment damage and the like. In the face of this situation, heterogeneous photocatalytic technology using semiconductors and renewable solar energy is considered to be one of the most promising processes to mitigate and even address the world energy supply crisis and environmental pollution. The water splitting photocatalytic hydrogen production technology is favored by a large number of scientific researchers due to the advantages of environmental friendliness, reproducibility and reutilization and the like. Hydrogen energy is one of renewable energy sources, and shows a good development trend.
The core of the technology for producing hydrogen by photocatalytic cracking is a photocatalyst. The CdS is particularly concerned due to excellent visible light response, narrow band gap and controllable form, the band gap width of the CdS is 2.4 eV, and hydrogen can be produced by hydrolysis by effectively utilizing visible light. However, the development of cadmium sulfide in the field of hydrogen production by photocatalytic hydrolysis is limited by the photo-corrosion effect of cadmium sulfide in the process of photocatalytic reaction. In the research on the cadmium sulfide photocatalytic material, researchers have taken various measures to solve the above problems. For example, a sacrificial agent such as methyl lactate is added into a cadmium sulfide visible light catalytic reaction system to react with photogenerated holes to reduce the number of holes and inhibit the generation of hole oxidation reaction. The noble metal promoter is carried on the surface of the cadmium sulfide particles, so that the separation of photo-generated electrons and holes can be accelerated, and the hydrogen production reaction is promoted. Due to the combination of cadmium sulfide and graphene and derivatives thereof, the carbon material serving as a bridge for transmitting photoproduction electrons greatly reduces the combination of the photoproduction electrons and cavities because of good conductivity, thereby reducing the influence of the photo-corrosion effect on the photocatalyst. In addition, the cadmium sulfide can be compounded with other compounds to promote the hydrogen production reaction.
Carbon materials are often used as catalyst carriers in the field of photocatalysis due to their advantages of low cost, easy availability, high specific surface area, good electrical conductivity, excellent chemical stability, etc. The specific surface area, pore size distribution and pore structure of carbon materials are important factors affecting their photochemical properties. Common carbon materials mainly comprise activated carbon, carbon nanotubes, carbon quantum dots, graphene and the like. In the field of photocatalysis, the carbon material can not only improve the specific surface area of the traditional semiconductor catalyst, but also be used as a bridge for receiving and transmitting photoelectrons due to the conductivity of the semiconductor catalyst, and can obviously improve the catalytic performance of the photocatalyst.
Bacterial cellulose is a natural molecular material, and a unique three-dimensional network structure formed by nano-grade fibers can be used as a biological scaffold, a carbon scaffold and the like, and has the characteristics of high water absorption and water retention, high transmittance for liquid and gas, high wet strength, in-situ processing and forming particularly in a wet state and the like due to a nano effect. The high purity and excellent performance enable the bacterial cellulose fiber to be widely applied in special fields. At present, the research work of bacterial cellulose and derivative materials thereof at home and abroad is deeply carried out on the modification, modification and preparation of the composite materials of the bacterial cellulose, and bacterial cellulose derivatives and bacterial cellulose-based composite materials with different performances are prepared by combining the structural and performance characteristics of the bacterial cellulose, but the research of all aspects is still in the initial stage, and further research on the bacterial cellulose and the bacterial cellulose-based composite materials is needed.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a preparation method for simply and rapidly producing a carbon fiber-cadmium sulfide composite photocatalytic material, the prepared composite photocatalytic material and application thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a composite photocatalytic material by utilizing carbonized bacterial cellulose-cadmium sulfide. The method comprises the following specific steps:
1): obtaining of bacterial cellulose aerogel: gluconacetobacter xylinus to be preserved in freeze-drying tubeGluconacetobacter xylinusActivated in basal medium A, ready forGluconacetobacter xylinusAfter dynamic culture for 96h, the obtained product is collected, washed by distilled water and 0.5M solution of hydrogen hydroxide, washed by distilled water to be neutral, and finally freeze-dried to collect the product.
2): preparing a bacterial cellulose-cadmium sulfide composite material: quantitatively adding the bacterial cellulose aerogel, thiourea, cadmium acetate dihydrate and ultrapure water which are obtained in the step 1) into a reaction kettle with a polytetrafluoroethylene inner container, and carrying out hydrothermal reaction at high temperature and high pressure.
3): preparing a carbonized bacterial cellulose-cadmium sulfide composite material: putting the product of the reaction 2) into a tubular furnace, calcining at high temperature in an argon atmosphere, and collecting the final product.
The culture medium A in the step 1) comprises the following main components in concentration: 25.0 g/L, tryptone 5.0 g/L, yeast extract 5.0 g/L, citric acid 1g/L, Na2HPO4 2g/L，K2HPO4 1 g/L，pH=5.0。
The amount of each component required by the hydrothermal reaction in the step 2) is as follows: 100mg of bacterial cellulose, 243mg of thiourea, 426mg of cadmium acetate dihydrate and 60 mL of ultrapure water. The reaction conditions are as follows: 100 mL of reaction kettle and 200 ℃ of high temperature.
Step 3) the calcination temperature programming is as follows: heating to 270 deg.C at 4 deg.C/min, heating to 360 deg.C at 0.33 deg.C/min, heating to 600 deg.C at 4 deg.C/min, calcining for 2 hr, and cooling to room temperature.
The invention also provides the bacterial cellulose carbide-cadmium sulfide composite photocatalytic material prepared by the preparation method.
The invention has the beneficial effects that: the invention provides a simple method for producing a carbonized bacterial cellulose and CdS composite photocatalyst. In the traditional hydrothermal synthesis process of CdS, bacterial cellulose aerogel is added, and then the composite product can be obtained through high-temperature calcination. The method has the advantages of simple operation, low cost, mild conditions, no toxicity, no harm and the like. The carbonized bacterial cellulose-cadmium sulfide composite material prepared by the invention has higher photocatalytic hydrogen production performance when being used as a catalyst in hydrogen production by photocatalytic water splitting.
Drawings
FIG. 1 is a graph of hydrogen production rates for four catalytic materials; wherein a is cadmium sulfide; b is calcined cadmium sulfide; c is bacterial cellulose-cadmium sulfide; d is carbonized bacterial cellulose-cadmium sulfide of the invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail with reference to the following examples.
The main components and concentrations in the culture medium A are as follows: 25.0 g/L, tryptone 5.0 g/L, yeast extract 5.0 g/L, citric acid 1g/L, Na2HPO4 2 g/L，K2HPO4 1 g/L，pH=5.0。
1): obtaining of bacterial cellulose aerogel: gluconacetobacter xylinus to be preserved in freeze-drying tubeGluconacetobacter xylinus ATCC 700178Activated in basal medium A, ready forGluconacetobacter xylinusAfter dynamic culture for 96h, the obtained product is collected, washed with distilled water and 0.5M solution of hydrogen hydroxide, washed with distilled water to neutrality, and finally subjected toAnd (4) performing vacuum freeze drying, and collecting the bacterial cellulose aerogel.
2): preparing a bacterial cellulose-cadmium sulfide composite material: respectively adding 0.1 g of bacterial cellulose aerogel, 0.36 g of thiourea, 0.638 g of cadmium acetate dihydrate and 60 mL of ultrapure water into a reaction kettle with a 100 mL polytetrafluoroethylene inner container, and reacting for 24h at 180 ℃.
3): preparing a carbonized bacterial cellulose-cadmium sulfide composite material: putting the product of the reaction 2) into a tubular furnace, heating to 270 ℃ at 4 ℃/min, heating to 360 ℃ at 0.33 ℃/min, heating to 600 ℃ at 4 ℃/min, calcining for 2h at the temperature, and finally cooling to room temperature. The obtained product is the carbonized bacterial cellulose-cadmium sulfide composite material.
4): performance testing of composite materials
We evaluated the activity of the catalyst by measuring the amount of hydrogen generated during the photocatalytic process. At normal temperature and normal pressure, a 120mL borosilicate glass bottle is used as a reaction system. The rubber stopper of the opening of the bottle is sealed, a 500W xenon lamp is used as a light source, and ultraviolet light is cut off by an ultraviolet cut-off filter plate, so that light irradiated on a catalytic system is visible light with the wavelength being more than or equal to 420 nm. We measured the light intensity at the reactor surface with a Vision photometer (test range: for) of TES-132 of Taiwan Shishi, China to be about 150 mW/cm2。
The specific experimental process of photocatalytic water decomposition for hydrogen production is as follows: the prepared carbonized bacterial cellulose-cadmium sulfide photocatalyst sample is decomposed in 80 mL of lactic acid aqueous solution by stirring, wherein lactic acid is a sacrificial agent for photocatalytic hydrogen production reaction, and the volume concentration of the lactic acid is 10 v%. Then introducing nitrogen, generally for half an hour, and removing air and dissolved oxygen in water in the reactor to ensure an oxygen-free environment in the reaction system. After the reaction system is sealed, the photocatalytic reaction is carried out under the irradiation of a xenon lamp light source while stirring, so that the catalyst is suspended in the system, and the reaction is fully carried out. Turning on a light source to irradiate from the side, continuously stirring by magnetic force in the whole photocatalytic reaction process to ensure the suspension state of sample particles, reacting for 3 h, and sampling 10 mL of gas after the reaction is finishedPassing gas chromatograph test (GC 9790)PLUS). The measured data are shown in fig. 1: as can be seen from FIG. 1, the hydrogen production rate of the carbonized bacterial cellulose-cadmium sulfide sample is significantly higher than that of the uncalcined bacterial cellulose-cadmium sulfide sample, and both are much higher than that of the pure cadmium sulfide sample. The carbonized bacterial cellulose is proved to be capable of greatly improving the photocatalytic hydrogen production performance of the cadmium sulfide material.
Claims (8)
1. A preparation method of a carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material comprises the following specific steps:
1): obtaining of bacterial cellulose aerogel: acetobacter xylinum to be preserved in freeze-drying tubeGluconacetobacterxylinus ATCC 700718Activation in basal Medium A, to beGluconacetobacter xylinusAfter the dynamic culture is carried out for 96 hours, collecting the obtained product, washing the product with distilled water and 0.5M of hydrogen hydroxide solution in sequence, then washing the product with distilled water to be neutral, and finally, carrying out vacuum freeze drying and collecting the product to obtain the bacterial cellulose aerogel;
2): preparing a bacterial cellulose-cadmium sulfide composite material: adding the bacterial cellulose aerogel, thiourea, cadmium acetate dihydrate and ultrapure water which are obtained in the step 1) into a reaction kettle with a polytetrafluoroethylene inner container, and carrying out hydrothermal reaction in the reaction kettle to obtain a bacterial cellulose-cadmium sulfide composite material;
3): preparing a carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material: putting the product of the reaction 2), namely the bacterial cellulose-cadmium sulfide composite material, into a tubular furnace, calcining at high temperature in an argon atmosphere, and collecting the final product, namely the bacterial cellulose carbide-cadmium sulfide composite photocatalytic material.
2. The method according to claim 1, wherein the culture medium A of step 1) comprises the following main components in concentration: 25.0 g/L, tryptone 5.0 g/L, yeast extract 5.0 g/L, citric acid 1g/L, Na2HPO4 2g/L，K2HPO41 g/L，pH=5.0。
3. The preparation method according to claim 1, wherein the hydrothermal reaction in step 2) requires the following components: 100mg of bacterial cellulose aerogel, 360 mg of thiourea, 638mg of cadmium acetate dihydrate and 60 mL of ultrapure water; the reaction conditions are as follows: the polytetrafluoroethylene inner container of the reaction kettle is 100 mL, and the hydrothermal reaction temperature is 200 ℃.
4. The method according to claim 1, wherein the hydrothermal reaction temperature in step 2) is 200 ℃.
5. The preparation method of claim 1, wherein the capacity of the polytetrafluoroethylene inner container is 100 mL.
6. The preparation method according to claim 1, wherein the high-temperature calcination temperature programming of step 3) is: heating to 270 deg.C at 4 deg.C/min, heating to 360 deg.C at 0.33 deg.C/min, heating to 600 deg.C at 4 deg.C/min, calcining for 2 hr, and cooling to room temperature.
7. The carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material prepared by the preparation method of any one of claims 1 to 6.
8. The application of the carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material as described in claim 7 as a catalyst in hydrogen production by photocatalytic water splitting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910239364.8A CN109999835B (en) | 2019-03-27 | 2019-03-27 | Carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910239364.8A CN109999835B (en) | 2019-03-27 | 2019-03-27 | Carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109999835A CN109999835A (en) | 2019-07-12 |
| CN109999835B true CN109999835B (en) | 2022-05-10 |
Family
ID=67168385
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910239364.8A Active CN109999835B (en) | 2019-03-27 | 2019-03-27 | Carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109999835B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110844939B (en) * | 2019-11-12 | 2022-03-01 | 杭州电子科技大学 | Molybdenum sulfide carbon nanosphere carbon nanofiber composite electrode material and preparation method thereof |
| CN111569832B (en) * | 2020-05-19 | 2022-04-29 | 西南科技大学 | Method for preparing hypha/molybdenum sulfide adsorption-catalysis material by utilizing biological enrichment |
| CN111545169B (en) * | 2020-05-19 | 2022-05-17 | 西南科技大学 | Method for preparing hypha/molybdenum oxide adsorption-catalysis material by utilizing biological enrichment |
| CN111889073B (en) * | 2020-07-31 | 2022-05-17 | 西南科技大学 | Preparation method of defect-rich molybdenum disulfide-bacterial cellulose heterojunction material for treating radioactive wastewater |
| CN114177922B (en) * | 2021-12-14 | 2023-09-01 | 西南科技大学 | Composite catalyst for removing uranium in nuclear waste liquid and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288416A (en) * | 2013-05-27 | 2013-09-11 | 东华大学 | Modified three-dimensional fiber-based aerogel material and preparation method thereof |
| CN106268865A (en) * | 2016-07-19 | 2017-01-04 | 青岛富强新材料科技有限公司 | A kind of cadmium sulfide C-base composte material is as the preparation method of photoelectric |
| CN107369563A (en) * | 2016-05-12 | 2017-11-21 | 复旦大学 | A kind of preparation method of nickel sulphide particles/cellulose base composite carbon aerogel material |
| CN108557869A (en) * | 2018-05-11 | 2018-09-21 | 常州大学 | A kind of CdS nanometer piece preparation methods based on bacteria cellulose skeleton |
| CN108722366A (en) * | 2018-05-25 | 2018-11-02 | 海南大学 | A kind of preparation method of polysaccharide-based Thermo-sensitive metal ion trace carbon quantum dot material |
-
2019
- 2019-03-27 CN CN201910239364.8A patent/CN109999835B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288416A (en) * | 2013-05-27 | 2013-09-11 | 东华大学 | Modified three-dimensional fiber-based aerogel material and preparation method thereof |
| CN107369563A (en) * | 2016-05-12 | 2017-11-21 | 复旦大学 | A kind of preparation method of nickel sulphide particles/cellulose base composite carbon aerogel material |
| CN106268865A (en) * | 2016-07-19 | 2017-01-04 | 青岛富强新材料科技有限公司 | A kind of cadmium sulfide C-base composte material is as the preparation method of photoelectric |
| CN108557869A (en) * | 2018-05-11 | 2018-09-21 | 常州大学 | A kind of CdS nanometer piece preparation methods based on bacteria cellulose skeleton |
| CN108722366A (en) * | 2018-05-25 | 2018-11-02 | 海南大学 | A kind of preparation method of polysaccharide-based Thermo-sensitive metal ion trace carbon quantum dot material |
Non-Patent Citations (2)
| Title |
|---|
| Organic-free synthesis of porous CdS sheets with controlled windows size on bacterial cellulose for photocatalytic degradation and H2 production;Man Zhou等;《Applied Surface Science》;20181126;第470卷;文章第909页第2.2节,文章第909页右栏第2.5节 * |
| 大豆渣制备细菌纤维素的研究;高媛等;《纤维素科学与技术》;20180630;第26卷(第2期);文章第19页第1.6.4节 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109999835A (en) | 2019-07-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109999835B (en) | Carbonized bacterial cellulose-cadmium sulfide composite photocatalytic material and preparation method and application thereof | |
| Liu et al. | Template-free preparation of non-metal (B, P, S) doped g-C3N4 tubes with enhanced photocatalytic H2O2 generation | |
| CN103316714B (en) | Catalyst for photo-catalytically decomposing water to produce hydrogen and preparation method of catalyst | |
| CN108816234B (en) | Preparation method and application of derivative catalyst based on LDH (layered double hydroxide) immobilized transition metal MOF (Metal organic framework) | |
| CN108607593B (en) | Cadmium sulfide nanoparticle modified niobium pentoxide nanorod/nitrogen-doped graphene composite photocatalyst and application thereof | |
| CN110773213A (en) | One-dimensional cadmium sulfide/two-dimensional titanium carbide composite photocatalyst and preparation method and application thereof | |
| CN112076791A (en) | Ni-MOF film photocatalyst growing on surface of foamed nickel in situ, and preparation method and application thereof | |
| CN105771948A (en) | Double-shell titanium dioxide catalyst with high photocatalytic hydrogen generation performance and preparation method thereof | |
| CN113401876B (en) | Method for producing hydrogen peroxide through photocatalysis without sacrificial agent | |
| CN109225276B (en) | Flower-like molybdenum diselenide/carbon nanotube composite material and synthesis method and application thereof | |
| CN106732671A (en) | Defect induces photocatalysis H high2Production two dimension MoS2The preparation method of nanometer layer | |
| CN110102349B (en) | alpha-Fe2O3Preparation of TpPa-2 composite material and hydrogen production by photolysis of water | |
| CN112316969A (en) | N-doped TiO2Hollow microsphere-BiOBr photocatalytic degradation material and preparation method thereof | |
| Mohamed et al. | Hollow N-TiO2/MnO2 nanocomposite based yeast biomass for gaseous formaldehyde degradation under visible light | |
| CN113880073B (en) | Lignin-based carbon nanotube and preparation method thereof | |
| CN107233901A (en) | A kind of MoS2Nanometer sheet composite Ti O2The preparation method of the photochemical catalyst of nanometer sheet | |
| CN110743535B (en) | Tungsten oxide homojunction composite photocatalyst and preparation method and application thereof | |
| CN113117721A (en) | Cyano-functionalized g-C3N4Colloidal catalyst, preparation method and application thereof | |
| CN104028309A (en) | Composite type visible-light-induced photocatalyst and preparation method thereof | |
| CN111468138A (en) | One-dimensional rod-shaped CuBi2O4@CuBi2S4Visible light catalyst and preparation method and application thereof | |
| CN110787784A (en) | Silk screen type TiO2Device and method for photocatalytic degradation of VOCs (volatile organic compounds) by nanotube array | |
| CN113713798B (en) | Preparation method of graphene quantum dot modified zinc oxide and application of degradation dye | |
| CN110743534A (en) | Tungsten oxide core-shell structure composite photocatalyst and preparation method and application thereof | |
| CN116371452A (en) | Efficient CO adsorption and reduction 2 Cs of (2) 2 CuBr 4 Photocatalyst | |
| CN111747410A (en) | Method for preparing hemp stalk core-based carbon material by hydrothermal method |
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 |