CN109999835A - A kind of carbonization bacteria cellulose-cadmium sulfide composite photocatalyst material and its preparation method and application - Google Patents
A kind of carbonization bacteria cellulose-cadmium sulfide composite photocatalyst material and its preparation method and application Download PDFInfo
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- CN109999835A CN109999835A CN201910239364.8A CN201910239364A CN109999835A CN 109999835 A CN109999835 A CN 109999835A CN 201910239364 A CN201910239364 A CN 201910239364A CN 109999835 A CN109999835 A CN 109999835A
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- bacteria cellulose
- cadmium sulfide
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- composite photocatalyst
- sulfide composite
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- 241000894006 Bacteria Species 0.000 title claims abstract description 48
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 38
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000003763 carbonization Methods 0.000 title claims abstract description 18
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 15
- 229920002678 cellulose Polymers 0.000 claims abstract description 21
- 239000001913 cellulose Substances 0.000 claims abstract description 21
- 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
- 239000000047 product Substances 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000001699 photocatalysis Effects 0.000 claims abstract description 11
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 5
- 239000012498 ultrapure water Substances 0.000 claims abstract description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 4
- 238000003776 cleavage reaction Methods 0.000 claims abstract description 4
- 239000008103 glucose Substances 0.000 claims abstract description 4
- 239000001963 growth medium Substances 0.000 claims abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 230000007017 scission Effects 0.000 claims abstract description 4
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 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
- 238000010792 warming Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052793 cadmium Inorganic materials 0.000 claims description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 4
- 241000589220 Acetobacter Species 0.000 claims description 3
- 239000007640 basal medium Substances 0.000 claims description 3
- 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 3
- 229940041514 candida albicans extract Drugs 0.000 claims description 3
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 3
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 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
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims 1
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 239000013066 combination product Substances 0.000 abstract description 2
- 229940127555 combination product Drugs 0.000 abstract description 2
- 229920002749 Bacterial cellulose Polymers 0.000 abstract 1
- 239000005016 bacterial cellulose Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000003575 carbonaceous material Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000243 solution Substances 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
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 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
- 239000004065 semiconductor 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
- BIUXMENMIKBKFP-UHFFFAOYSA-N CO.CC(O)C(O)=O Chemical compound CO.CC(O)C(O)=O BIUXMENMIKBKFP-UHFFFAOYSA-N 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 238000013019 agitation 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
- 230000005540 biological transmission Effects 0.000 description 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000005539 carbonized material Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 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
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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 present invention relates to a kind of carbonization bacteria cellulose-cadmium sulfide composite photocatalyst materials and its preparation method and application.Catalysis material bottom right method preparation: 1) by the wooden glucose acetobacterGluconacetobacter xylinusIt is seeded in culture medium A, 96 h of dynamic cultivation collects bacterial cellulose product, washed drying, then obtains bacteria cellulose aeroge through vacuum freeze drying;2) quantitative thiocarbamide and cadmium sulfide are dissolved in ultrapure water, suitable bacteria cellulose aeroge is added, carries out hydro-thermal reaction under high temperature and pressure;3) by bacteria cellulose-cadmium sulfide combination product in tube furnace through high-temperature calcination, obtain carbonization bacteria cellulose-cadmium sulfide composite photocatalyst material.Preparation method of the present invention have many advantages, such as it is easy to operate, it is low in cost.Gained carbonization bacteria cellulose-cadmium sulfide composite photocatalyst material can be used as application of the catalyst in photocatalytic cleavage aquatic products hydrogen.
Description
Technical field
The present invention relates to a kind of carbon fiber-cadmium sulfide composite photocatalyst materials and its preparation method and application.
Background technique
Since 21st century, with the rapid development of science and technology, productivity significantly improve createed for the mankind it is huge
Big wealth.While using scientific and technological creation wealth, also the energy consumes excessively band people, ecological environment destruction is serious etc. one
Serial problem.In face of this case, the Heterogeneous photocatalysis technology using semiconductor and renewable solar energy is considered as mitigating
Even solve one of world energy supplies crisis and the most promising process of environmental pollution.Water-splitting photocatalysis hydrogen production technology,
The advantages that because of its environmental-friendly, renewable recycling, the favor of a large number of scientific researchers is obtained.Hydrogen Energy is as renewable energy
One kind, show good growth momentum.
The core of photocatalytic cleavage aquatic products hydrogen technology is photochemical catalyst.Wherein, CdS is since its is excellent visible light-responded,
Narrow band gap and controlled morphologies and it is especially concerned, band gap width be 2.4 eV, can effectively utilize visible light hydrolytic hydrogen production.But
Since in cadmium sulfide, during light-catalyzed reaction, photoetch effect limits it in the hair in photocatalysis hydrolytic hydrogen production field
Exhibition.In the research of cadmium sulfide catalysis material, researcher takes many kinds of measures to solve the above problems.For example, vulcanizing
Sacrifice agent such as lactic acid methanol etc. is added in cadmium visible light catalytic reaction system, is reacted it with photohole and is reduced number of cavities,
Inhibit the generation of Hole oxidation reaction.Precious metal catalytic agent is carried in cadmium sulfide particle surface, also can speed up light induced electron
With the separation in hole, promote the generation of hydrogen production reaction.The combination of cadmium sulfide and graphene and its derivative, carbon material are good because of it
Electric conductivity, the bridge as light induced electron transmission greatly reduces the combination in light induced electron and hole to reduce photoetch
Influence of the effect to photochemical catalyst.In addition, cadmium sulfide and the compound generation that can also promote hydrogen production reaction of other compounds.
Carbon material to be easy to get at a low price, high-specific surface area, good electric conductivity and the advantages that excellent chemical stability, often
Photocatalysis field is applied to as catalyst carrier.Specific surface area, pore-size distribution and the pore structure of carbon material are to influence
An important factor for its photochemical properties.The common carbon material seen mainly has: active carbon, carbon nanotube, carbon quantum dot and graphene
Deng.In photocatalysis field, carbon material can not only improve the specific surface area of conventional semiconductors catalyst, also make because of its electric conductivity
Receive that the catalytic performance of photochemical catalyst can be significantly improved with the bridge transmitted for photoelectron.
Bacteria cellulose is a kind of natural molecule material, the unique tridimensional network being made of Nano grade fiber
It can be used as biological support, carbon template etc., and there is high-hydroscopicity and high-moisture-retention, to liquids and gases because of " nano effect "
High transmittance, high wet strength, especially can the characteristics such as machine-shaping in situ under hygrometric state.High-purity and excellent performance make bacterium
Cellulose fibre can be widely applied in special dimension.At present both at home and abroad to the research work of bacteria cellulose and its derived material
It is deep into the modification to bacteria cellulose, modification and prepares its composite material, in conjunction with the structure and performance characteristics of bacteria cellulose,
Prepare the bacteria cellulose derivative and bacteria cellulose based composites of different properties, but the research of various aspects is also in rising
Step section also needs to carry out deeper research to it.
Summary of the invention
The technical problem to be solved by the present invention is to be directed to the deficiencies in the prior art, providing one kind can be simply fast
Production carbon fiber-cadmium sulfide composite photocatalyst material preparation method of speed and composite photocatalyst material obtained are answered with it
With.
In order to solve the above technical problems, present invention provide the technical scheme that
It is a kind of to utilize carbonization bacteria cellulose-cadmium sulfide composite photocatalyst material preparation method.Specific step is as follows:
1): the wooden glucose acetobacter of freeze-drying pipe the acquisition of bacteria cellulose aeroge: will be stored inGluconacetobacter xylinusIt is activated in basal medium A, toGluconacetobacter xylinusDynamically
It after cultivating 96h, products therefrom is collected, is successively washed with distilled water and 0.5M onium hydroxide solution, be then washed to distilling
Property, last freeze-dried rear collection product.
2): the preparation of bacteria cellulose-cadmium sulfide composite material: by step 1) product bacteria cellulose aeroge, thiocarbamide,
Cadmium diacetate dihydrate and ultrapure water are quantitatively adding in the reaction kettle with polytetrafluoro liner, and it is anti-that hydro-thermal is carried out under high temperature and pressure
It answers.
3): carbonization bacteria cellulose-cadmium sulfide composite material preparation: will react product 2), be put into tube furnace,
Final product is collected in the high-temperature calcination under argon atmosphere.
Main component and concentration in culture medium A described in step 1) are as follows: 25.0 g/L, 5.0 g/L of tryptone, yeast extract
5.0 g/L of object, citric acid 1g/L, Na2HPO42g/L, K2HPO41 g/L, pH=5.0.
Amount needed for each ingredient of hydro-thermal reaction described in step 2 are as follows: bacteria cellulose 100mg, thiocarbamide 243mg, two hydrations
Cadmium acetate 426mg, 60 mL of ultrapure water.Reaction condition are as follows: 100 mL of reaction kettle, 200 DEG C of high temperature.
The heating of calcination procedure described in step 3) are as follows: be warming up to 270 DEG C with 4 DEG C/min, then be warming up to 0.33 DEG C/min
360 DEG C, 600 DEG C then are warming up to 4 DEG C/min and calcines 2h at this temperature, is finally cooled to room temperature.
The present invention also provides the bacteria cellulose-cadmium sulfide composite photocatalyst materials that is carbonized as made from above-mentioned preparation method
Material.
The beneficial effects of the present invention are: the invention proposes a kind of simple production carbonization bacteria cellulose and CdS are multiple
The method of light combination catalyst.During conventional hydrothermal synthesizes CdS, bacteria cellulose aeroge is added, then through high-temperature calcination
Combination product can be obtained.This method has the advantages that easy to operate, low in cost, mild condition, nontoxic.System of the present invention
Carbonization bacteria cellulose-cadmium sulfide composite material as catalyst, the light with higher in photocatalytic cleavage aquatic products hydrogen is urged
Change H2-producing capacity.
Detailed description of the invention
Fig. 1 is the hydrogen-producing speed figure of four kinds of catalysis materials;Wherein a is cadmium sulfide;B is calcined cadmium sulfide;C is thin
Fungin-cadmium sulfide;D is present invention carbonization bacteria cellulose-cadmium sulfide.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention makees the present invention below with reference to embodiment
It is described in further detail.
Main component and concentration in culture medium A are as follows: 25.0 g/L, 5.0 g/L of tryptone, 5.0 g/L of yeast extract,
Citric acid 1 g/L, Na2HPO42 g/L, K2HPO41 g/L, pH=5.0.
1): the wooden glucose acetobacter of freeze-drying pipe the acquisition of bacteria cellulose aeroge: will be stored inGluconacetobacter xylinus ATCC 700178It is activated in basal medium A, toGluconacetobacter xylinusAfter dynamic cultivation 96h, products therefrom is collected, is successively washed with distilled water and 0.5M onium hydroxide solution, is then made again
It is washed to neutrality with distillation, most collects bacteria cellulose aeroge after vacuum freeze drying afterwards.
2): bacteria cellulose-cadmium sulfide composite material preparation: respectively by 0.1 g bacteria cellulose aeroge, 0.36 g
Thiocarbamide, 0.638 g Cadmium diacetate dihydrate and 60 mL ultrapure waters are added in the reaction kettle with 100 mL polytetrafluoro liners,
It is reacted for 24 hours under the conditions of 180 DEG C.
3): carbonization bacteria cellulose-cadmium sulfide composite material preparation: will react product 2), be put into tube furnace,
270 DEG C are warming up to 4 DEG C/min, then is warming up to 360 DEG C with 0.33 DEG C/min, is then warming up to 600 with 4 DEG C/min
DEG C and calcine 2 h at this temperature, be finally cooled to room temperature.Products therefrom is the bacteria cellulose-cadmium sulfide composite wood that is carbonized
Material.
4): the performance test of composite material
We evaluate the activity of catalyst by the amount of the hydrogen generated in test photocatalytic process.At normal temperatures and pressures, it adopts
The 120mL high borosilicate material glass bottle used is as reaction system.Bottle opening rubber stopper is sealed, and light source uses 500 W
Xenon lamp clips ultraviolet light with one piece of ultraviolet cut-on filter plate, so that the light being radiated in catalyst system is that wavelength is more than or equal to 420
The visible light of nm.We learn reactor surface with the visible photometer of TaiWan, China Thailand bodyguard TES-132 (test scope is) measurement
The light intensity at place is about 150 mW/cm2。
The specific experiment process of photocatalysis Decomposition aquatic products hydrogen is as follows: by obtained carbonization bacteria cellulose-cadmium sulfide light
Catalyst sample is decomposed in 80 mL lactic acid aqueous solutions by stirring, wherein and lactic acid is the sacrifice agent of Photocatalyzed Hydrogen Production reaction,
Its volumetric concentration is 10 v%.It is passed through nitrogen later, generally continues half an hour, removes the dissolution in the air and water in reactor
Oxygen, to guarantee the oxygen-free environment in reaction system.After reaction system is sealed, light is carried out under xenon source irradiation when whisking
Catalysis reaction, is suspended in catalyst in system, and reaction is sufficiently carried out.It opens light source to irradiate from side, be urged in entire light
Change and need lasting magnetic agitation in reaction process to guarantee the suspended state of sample particle, the reaction time is 3 h, and reaction terminates
The gas for sampling 10 mL afterwards tests (GC9790 by gas chromatographPLUS).The data measured such as Fig. 1: as shown in Figure 1, carbonization
Bacteria cellulose-cadmium sulfide sample hydrogen-producing speed, which is apparently higher than, does not calcine bacteria cellulose-cadmium sulfide sample, and both remote
Greater than the hydrogen-producing speed of bright sulfur cadmium sample.Prove that the Photocatalyzed Hydrogen Production of vulcanization cadmium material can be substantially improved in carbonization bacteria cellulose
Performance.
Claims (8)
1. a kind of carbonization bacteria cellulose-cadmium sulfide composite photocatalyst material preparation method, the specific steps are as follows:
1): the wooden glucose acetobacter of freeze-drying pipe the acquisition of bacteria cellulose aeroge: will be stored inGluconacetobacter xylinus ATCC 700718It is activated in basal medium A, toGluconacetobacter xylinusAfter dynamic cultivation 96h, products therefrom is collected, is successively washed with distilled water and 0.5 M onium hydroxide solution, is then used
Distillation is washed to neutrality, most collects product after vacuum freeze drying afterwards and obtains bacteria cellulose aeroge;
2): bacteria cellulose-cadmium sulfide composite material preparation: by step 1) product bacteria cellulose aeroge, thiocarbamide, two water
It closes cadmium acetate and ultrapure water is added in the reaction kettle with polytetrafluoro liner, carry out hydro-thermal reaction in a kettle and bacterium is made
Cellulose-cadmium sulfide composite material;
3): product bacteria cellulose-sulphur 2) carbonization bacteria cellulose-cadmium sulfide composite photocatalyst material preparation: will be reacted
Cadmium composite material is put into tube furnace, the high-temperature calcination under argon atmosphere, collects final product carbonization bacteria cellulose-sulphur
Cadmium composite photocatalyst material.
2. preparation method according to claim 1, which is characterized in that main component and dense in culture medium A described in step 1)
Degree are as follows: 25.0 g/L, 5.0 g/L of tryptone, 5.0 g/L of yeast extract, citric acid 1g/L, Na2HPO42g/L, K2HPO4
1 g/L, pH=5.0.
3. preparation method according to claim 1, which is characterized in that amount needed for each ingredient of hydro-thermal reaction described in step 2
Are as follows: 100 mg of bacteria cellulose aeroge, thiocarbamide 360 mg, Cadmium diacetate dihydrate 638mg, 60 mL of ultrapure water;Reaction condition
Are as follows: reaction kettle polytetrafluoro liner 100 mL, 200 DEG C of hydrothermal temperature.
4. preparation method according to claim 1, which is characterized in that 200 DEG C of hydrothermal temperature in step 2.
5. preparation method according to claim 1, which is characterized in that polytetrafluoro liner capacity is 100 mL.
6. preparation method according to claim 1, which is characterized in that high-temperature calcination temperature programming described in step 3) are as follows: with 4
DEG C/min is warming up to 270 DEG C, then is warming up to 360 DEG C with 0.33 DEG C/min, then 600 DEG C are warming up to simultaneously with 4 DEG C/min
2 h are calcined at this temperature, are finally cooled to room temperature.
7. be carbonized bacteria cellulose-cadmium sulfide composite photocatalyst as made from preparation method described in any one of claims 1-6
Material.
8. carbonization bacteria cellulose-cadmium sulfide composite photocatalyst material is as catalyst in photocatalytic cleavage described in claim 7
Application in aquatic products hydrogen.
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CN114177922A (en) * | 2021-12-14 | 2022-03-15 | 西南科技大学 | Composite catalyst for removing uranium in nuclear waste liquid and preparation method and application thereof |
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