CN109289883B - Preparation method of photocatalyst preparation - Google Patents
Preparation method of photocatalyst preparation Download PDFInfo
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- CN109289883B CN109289883B CN201811057613.3A CN201811057613A CN109289883B CN 109289883 B CN109289883 B CN 109289883B CN 201811057613 A CN201811057613 A CN 201811057613A CN 109289883 B CN109289883 B CN 109289883B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 229910017582 La2Ti2O7 Inorganic materials 0.000 claims abstract description 30
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 29
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 25
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 25
- 108010029541 Laccase Proteins 0.000 claims abstract description 20
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 15
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 15
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000015556 catabolic process Effects 0.000 claims abstract description 11
- 238000006731 degradation reaction Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- 239000004065 semiconductor Substances 0.000 claims description 26
- 239000010936 titanium Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000000354 decomposition reaction Methods 0.000 claims description 10
- 239000000839 emulsion Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims description 5
- INNSZZHSFSFSGS-UHFFFAOYSA-N acetic acid;titanium Chemical compound [Ti].CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O INNSZZHSFSFSGS-UHFFFAOYSA-N 0.000 claims description 5
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 229910052724 xenon Inorganic materials 0.000 claims description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 5
- 230000001678 irradiating effect Effects 0.000 claims 1
- 230000003287 optical effect Effects 0.000 claims 1
- 230000031700 light absorption Effects 0.000 abstract description 7
- 230000001276 controlling effect Effects 0.000 description 22
- 241000282414 Homo sapiens Species 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000003344 environmental pollutant Substances 0.000 description 6
- 231100000719 pollutant Toxicity 0.000 description 6
- 239000000463 material Substances 0.000 description 5
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- 230000007613 environmental effect Effects 0.000 description 4
- 229910052976 metal sulfide Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000001782 photodegradation Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
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- 150000004763 sulfides Chemical class 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000003915 air pollution 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
- 238000000889 atomisation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
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- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
The invention relates to a preparation method of a photocatalyst preparation, which is prepared by mixing perovskite type metal oxide La2Ti2O7With sulfide In2S3P-N heterostructure La constructed by assembling2Ti2O7/In2S3And then nano platinum and laccase are loaded to prepare the photocatalyst preparation capable of realizing solar hydrogen production and solar formaldehyde degradation. Compared with the prior art, the perovskite type metal oxide La of the invention2Ti2O7With sulfide In2S3Has an ultrathin two-dimensional structure, and the visible light absorption of the ultrathin two-dimensional structure is continuously adjustable between 550 nanometers and 600 nanometers. The photocatalyst preparation can realize the hydrogen production by fully decomposing water under sunlight and the indoor high-efficiency formaldehyde removal.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a preparation method of a photocatalyst preparation for preparing hydrogen by photolysis of water and removing formaldehyde pollutants in a room and other closed spaces.
Background
The human society develops rapidly, but the existing energy reserves are more and more difficult to meet the rapidly increasing energy requirements of human beings; in addition, the exploitation, use and discharge of fossil fuels induce serious environmental problems such as climate warming, ocean acidification, air pollution, etc., which seriously hinder the sustainable development of society. Therefore, developing or seeking a new sustainable way of energy utilization is the key to solving the above problems; meanwhile, with the progress of science and technology, the living standard of human beings is gradually improved, the health consciousness and the environmental protection consciousness of human beings are gradually enhanced, the formaldehyde pollutants are greatly damaged to human beings in the process of home decoration or the use process of automobiles, and the pollutants are difficult to be effectively removed by the traditional method, so that the technology for removing the formaldehyde toxic gas in the closed space (such as a new house or a new automobile) needs to be improved urgently.
Solar energy has many advantages over fossil energy. Firstly, the solar energy reserves are huge, and according to estimation, the solar energy reaching the earth surface in one hour can meet the energy requirement of human in one year; in addition, solar radiation is widely distributed and easily obtained, and considerable solar radiation exists in human habitation except for the phenomenon of the south and north poles at the night. Secondly, the development and utilization of solar energy do not cause continuous harm to the environment. The existing solar energy utilization modes mainly comprise solar energy electric energy conversion, solar energy chemical energy conversion and solar heat energy conversion. Among them, chemical conversion of solar energy is an ideal energy development approach. For example, the intermittent solar radiation which is difficult to collect and store is converted into chemical energy (such as hydrogen energy and the like) which is easy to collect and store, so that the existing fossil energy utilization framework can be effectively matched, the fossil energy economy cannot be completely subverted, and the environmental problem caused by the development and utilization of the fossil energy can be effectively avoided; in addition, photodegradation of pollutants is also an ideal and effective environment-friendly pollution treatment mode, and the formaldehyde photodegradation of pollutants in a closed space can sequentially and effectively degrade the pollutants into pollution-free carbon dioxide and water molecules.
The conversion of solar chemical energy mainly comprises: 1. solar energy is utilized to decompose water into hydrogen and oxygen on the surface of the photocatalyst (namely, solar energy hydrogen production) 2. organic pollutants such as formaldehyde are decomposed by the solar energy and the photocatalyst (solar energy environment purification). Both of these solar energy utilization modes rely on highly efficient photocatalysts. A photocatalyst is a catalyst that is capable of absorbing and converting solar energy and catalyzing chemical reactions. Conventional photocatalysts such as TiO2(Energy&Environmental Science,5(2012), 6506-.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a photocatalyst with high catalytic activity and good stability.
The purpose of the invention can be realized by the following technical scheme:
preparation method of photocatalyst preparation, perovskite type metal oxide La2Ti2O7With sulfide In2S3P-N heterostructure La constructed through electrostatic assembly2Ti2O7/In2S3Then loading nano platinum and laccase to prepare the photocatalyst preparation capable of realizing solar hydrogen production and solar formaldehyde degradation, wherein the perovskite type metal oxygenCompound La2Ti2O7With sulfide In2S3The mass ratio of the nano platinum to the laccase is 2.5:1.0-12.5:1.0, the content of the loaded nano platinum is 1-3wt%, and the content of the laccase is 0-1 wt%. The visible light absorption of the prepared photocatalyst preparation is continuously adjustable within 500-600 nm.
The preparation method specifically comprises the following steps:
(1) controlling the temperature to be 263K-283K, mixing and dissolving titanium acetate and lanthanum nitrate in deionized water to obtain a transparent solution;
(2) controlling the temperature to be 273K-283K, and mixing sodium hydroxide and deionized water to prepare a transparent solution, wherein the concentration of the sodium hydroxide is 2 mol/L;
(3) controlling the temperature to be 273K-283K, and mixing the solution drop by drop and continuously and violently stirring to obtain a white milky mixed solution;
(4) controlling the temperature to 603K, sealing the mixed solution in a reaction kettle, keeping the temperature for 24 hours to obtain a white solid, and washing and drying the white solid;
(5) placing the white solid in DMF, and keeping for 48 hours under the ultrasonic condition to obtain the ultrathin N-type semiconductor La2Ti2O7The white emulsion of (4);
(6) controlling the temperature to be 263K-283K, weighing indium nitrate, hexadecyl trimethyl ammonium bromide and thioacetamide, mixing, dissolving in deionized water, and continuously stirring to obtain a transparent solution;
(7) refluxing the clear solution at 368K for 90 minutes to obtain a yellow precipitate;
(8) washing and drying the yellow precipitate S2 by using absolute ethyl alcohol and deionized water, and carrying out the same treatment In the step (5) to obtain the ultrathin P-type semiconductor In2S3The yellow emulsion of (1); (ii) a
(9) Mixing the ultrathin N-type semiconductor La with different mass ratios according to the proportion2Ti2O7And ultra-thin P-type semiconductor In2S3Mixing dropwise and performing ultrasonic treatment, during which the two subjected to ultrasonic stripping are detected to carry different kinds of charges on the surfaces by measuring the Zeta potential of the two, wherein La2Ti2O7Carrying a positive charge, In2S3Washing and drying the powder carrying negative charges, and treating the powder for two hours under the 453K condition;
(10) the treated powder was mixed with a chloroplatinic acid solution having a concentration of 2wt%, and irradiated under a 300 watt xenon lamp equipped with a 400 nm filter for 1 hour to obtain a photocatalyst for hydrogen production by water decomposition.
Ultrathin N-type semiconductor La in step (9)2Ti2O7And ultra-thin P-type semiconductor In2S3The mass ratio of (b) is preferably 7.5: 1.0.
The water decomposition hydrogen preparation photocatalyst is further mixed with laccase and deionized water and dried to prepare the formaldehyde degradation photocatalyst.
Compared with the prior art, the invention has the following advantages:
(1) by controlling La2Ti2O7And In2S3The proportion of (2) can be used for preparing the surface-to-surface contact heterostructure with the optimal assembly proportion, and the ultrathin heterostructure has a larger specific surface and is beneficial to the catalytic reaction and the material transmission.
(2) Ultrasonic treatment of La by DMF solution2Ti2O7And In2S3To obtain ultrathin La with opposite charges on the surface2Ti2O7And In2S3And the spontaneous uniform distribution of the two components in the assembly process is facilitated.
(3) By regulating La2Ti2O7And In2S3The mass ratio of the photocatalyst can effectively regulate and control the sunlight absorption capacity of the photocatalyst, and the sunlight absorption photon range can be continuously regulated and controlled within 500-600 nanometers.
(4) By a photoreduction method, the surface of the photocatalyst is specifically loaded with noble metal nano platinum in situ, so that the electron capturing capability of the heterostructure for transferring electrons is enhanced; in addition, the killing effect of the characteristics on bacteria is more obvious.
(5) By loading laccase, the binding capacity of the photocatalyst and the wood material can be obviously enhanced, and the photocatalyst is favorably fixed on a wood appliance.
Drawings
FIG. 1 shows a heterostructure La constructed by perovskite type metal oxide and sulfide2Ti2O7/In2S3Scanning electron microscopy photographs of the tablets during self-assembly.
FIG. 2 shows a heterojunction La constructed by perovskite type metal oxides and sulfides with different mass ratios2Ti2O7/In2S3Absorbance versus ratio.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The method for loading laccase on metal nitrogen oxide comprises the following steps:
mixing and drying a composite material P5(7.5:1.0), laccase and deionized water to obtain a formaldehyde degradation type photocatalyst;
the application method of the photocatalytic water splitting hydrogen production photocatalyst comprises the following steps:
(1) selecting 1 clean FTO conductive glass (10 cm multiplied by 10 cm), decomposing water to prepare a hydrogen photocatalyst, and mixing ethylene glycol according to a weight ratio of 20: 1, mixing, grinding and blade coating the mixture on FTO conductive glass;
(2) FTO conductive glass and a platinum sheet (1 cm multiplied by 1 cm) which carry water decomposition hydrogen preparation photocatalyst are respectively used as a working electrode and a counter electrode, and sodium sulfate aqueous solution (0.1 mol/L concentration) is used as electrolyte to form a photoelectrolysis cell;
(3) the working electrode is used as an anode, the counter electrode is used as a cathode, 0.2 volt voltage is applied to two ends of the working electrode, water is decomposed under the condition that the working electrode is irradiated by sunlight, and the hydrogen can be collected by the cathode.
The application method of the photodegradation formaldehyde type photocatalyst comprises the following steps:
(1) mixing the formaldehyde degrading photocatalyst and deionized water according to the weight ratio of 1:20, and performing ultrasonic dispersion;
(2) cleaning the sprayed object, and covering the object to be prevented from being sprayed with a film;
(3) selecting a spray gun with a good atomization effect, and keeping a distance of 5-15 cm between the spray gun and an object to be sprayed;
(4) the object to be sprayed is naturally dry and is not wiped before drying.
Examples 1 to 4 and comparative examples 1 to 3
Examples 1-4 of photocatalyst for hydrogen production by water decomposition
The raw materials were prepared according to the proportions in table 1:
TABLE 1 raw material compounding ratio tables for examples 1 to 4 and comparative examples 1 to 3
| Name of reagent | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| La2Ti2O7 | 42.86 | 50.00mg | 52.94mg | 54.55mg | 52.94mg | 52.94mg | 52.94mg |
| In2S3 | 17.14mg | 10.00mg | 7.06mg | 5.45mg | 7.06mg | 7.06mg | 7.06mg |
| La2Ti2O7/In2S3 | 60.00mg | 60.00mg | 60.00mg | 60.00mg | 60.00mg | 60.00mg | 60.00mg |
| Chloroplatinic acid | 1.20mg | 1.20mg | 1.20mg | 1.20mg | 0.60mg | 1.20mg | 1.80mg |
| Laccase enzymes | 0.15mg | 0.15mg | 0.15mg | 0.15mg | 0.15mg | 0.00mg | 0.15mg |
Table 2 shows the photolytic properties under 400 nm cut-off filter conditions and the detection of the noraldehyde properties according to GB/T16129 for examples 1 to 4 and comparative examples 1 to 3.
TABLE 2
FIG. 1 shows a heterostructure La constructed by perovskite type metal oxide and sulfide2Ti2O7/In2S3Scanning electron microscopy photographs of the tablets during self-assembly. By controlling La2Ti2O7And In2S3The proportion of (2) can be used for preparing the surface-to-surface contact heterostructure with the optimal assembly proportion, and the ultrathin heterostructure has a larger specific surface and is beneficial to the catalytic reaction and the material transmission: in the figure a2S3The surface is smooth and presents an ultrathin two-dimensional structure, and the pictures b-f are La in sequence2Ti2O7/In2S32.5:1.0, 5.0:1.0, 7.5:1.0, 10.0:1.0, 12.5; 1.0, we can see that with La2Ti2O7The amount of the compound (A) is gradually increased, the smoothness of the surface of the heterojunction is gradually increased, the specific surface area is firstly reduced and increased, wherein the specific surface area with the ratio of 7.5:1.0 is the smallest, which indicates that the heterojunction is most fully assembled electrostatically under the condition of the ratio; graph g is original La2Ti2O7Scanning electron microscope images, from which it can be seen that the original La2Ti2O7The surface is smooth, and an ultrathin two-dimensional structure is presented; graph h shows the original DMF sample dispersions and differences during the synthesis of heterojunctionsProportional two-component mixture, the original La of ultrasonic stripping can be seen from the image2Ti2O7And original In2S3The composite material has good dispersibility in DMF liquid, which shows that the stripping effect is good, and the components of the two can be quickly precipitated in the dispersion liquid after the two are mixed, which shows that the electrostatic force action obviously plays a role of no substitution in the assembly process.
FIG. 2 shows a heterojunction La constructed by perovskite type metal oxides and sulfides with different mass ratios2Ti2O7/In2S3Absorbance versus ratio: it is evident from fig. 2 that the heterojunction compares to the original La2Ti2O7Has obvious visible light absorption with In2S3The amount of the hetero-junction is increased, and the visible light absorption capability of the hetero-junction is closer to the original In2S3And (3) sampling. This indicates In2S3Can be successfully assembled to La2Ti2O7The surface of the material can effectively improve the utilization and absorption of the heterojunction to visible light, thereby improving the photocatalytic activity of the product.
Example 5
Preparation method of photocatalyst preparation, perovskite type metal oxide La2Ti2O7With sulfide In2S3P-N heterostructure La constructed through electrostatic assembly2Ti2O7/In2S3Then loading nano platinum and laccase to prepare the photocatalyst preparation which can realize solar hydrogen production and solar formaldehyde degradation, wherein the perovskite type metal oxide La2Ti2O7With sulfide In2S3The mass ratio of the supported nano platinum to the photocatalyst is 2.5:1.0, the content of the supported nano platinum is 1wt%, and the visible light absorption of the prepared photocatalyst preparation is continuously adjustable from 500 nanometers to 600 nanometers.
The preparation method specifically comprises the following steps:
(1) controlling the temperature to be 263K, mixing and dissolving titanium acetate and lanthanum nitrate in deionized water to obtain a transparent solution;
(2) controlling the temperature to be 273K, and mixing sodium hydroxide and deionized water to prepare a transparent solution, wherein the concentration of the sodium hydroxide is 2 mol/L;
(3) controlling the temperature to be 273K, mixing the solution drop by drop and stirring the solution continuously and violently to obtain a white milky mixed solution;
(4) controlling the temperature to 603K, sealing the mixed solution in a reaction kettle, keeping the temperature for 24 hours to obtain a white solid, and washing and drying the white solid;
(5) placing the white solid in DMF, and keeping for 48 hours under the ultrasonic condition to obtain the ultrathin N-type semiconductor La2Ti2O7The white emulsion of (4);
(6) controlling the temperature to be 263K, weighing indium nitrate, hexadecyl trimethyl ammonium bromide and thioacetamide, mixing, dissolving in deionized water, and continuously stirring to obtain a transparent solution;
(7) refluxing the clear solution at 368K for 90 minutes to obtain a yellow precipitate;
(8) washing and drying the yellow precipitate S2 by using absolute ethyl alcohol and deionized water, and carrying out the same treatment In the step (5) to obtain the ultrathin P-type semiconductor In2S3The yellow emulsion of (1); (ii) a
(9) The ultra-thin N-type semiconductor La is mixed according to the mass ratio of 2.5:1.02Ti2O7And ultra-thin P-type semiconductor In2S3Mixing dropwise and performing ultrasonic treatment, during which the two subjected to ultrasonic stripping are detected to carry different kinds of charges on the surfaces by measuring the Zeta potential of the two, wherein La2Ti2O7Carrying a positive charge, In2S3Washing and drying the powder carrying negative charges, and treating the powder for two hours under the 453K condition;
(10) the treated powder was mixed with a chloroplatinic acid solution having a concentration of 2wt%, and irradiated under a 300 watt xenon lamp equipped with a 400 nm filter for 1 hour to obtain a photocatalyst for hydrogen production by water decomposition.
Example 6
Preparation method of photocatalyst preparation, perovskite type metal oxide La2Ti2O7With sulfide In2S3Built by electrostatic assemblyP-N heterostructure La2Ti2O7/In2S3Then loading nano platinum and laccase to prepare a photocatalyst preparation capable of realizing solar hydrogen production and solar formaldehyde degradation, wherein the perovskite type metal oxide La2Ti2O7With sulfide In2S3The mass ratio of (1) to (7.5) is 7.5:1.0, the content of the loaded nano platinum is 2wt%, and the content of the laccase is 0.5 wt%. The visible light absorption of the prepared photocatalyst preparation is continuously adjustable within 500-600 nm.
The preparation method specifically comprises the following steps:
(1) controlling the temperature to be 273K, mixing and dissolving titanium acetate and lanthanum nitrate in deionized water to obtain a transparent solution;
(2) controlling the temperature to be 280K, and mixing sodium hydroxide and deionized water to prepare a transparent solution, wherein the concentration of the sodium hydroxide is 2 mol/L;
(3) controlling the temperature to be 280K, mixing the solution drop by drop and stirring the solution continuously and violently to obtain a white milky mixed solution;
(4) controlling the temperature to 603K, sealing the mixed solution in a reaction kettle, keeping the temperature for 24 hours to obtain a white solid, and washing and drying the white solid;
(5) placing the white solid in DMF, and keeping for 48 hours under the ultrasonic condition to obtain the ultrathin N-type semiconductor La2Ti2O7The white emulsion of (4);
(6) controlling the temperature to be 273K, weighing indium nitrate, hexadecyl trimethyl ammonium bromide and thioacetamide, mixing, dissolving in deionized water, and continuously stirring to obtain a transparent solution;
(7) refluxing the clear solution at 368K for 90 minutes to obtain a yellow precipitate;
(8) washing and drying the yellow precipitate S2 by using absolute ethyl alcohol and deionized water, and carrying out the same treatment In the step (5) to obtain the ultrathin P-type semiconductor In2S3The yellow emulsion of (1); (ii) a
(9) The ultra-thin N-type semiconductor La is mixed according to the mass ratio of 7.5:1.02Ti2O7And ultra-thin P-type semiconductor In2S3Mixing drop by drop and sonicatingIn the process, the two ultrasonically stripped surfaces are found to carry different types of charges by measuring the Zeta potential of the two surfaces, wherein La2Ti2O7Carrying a positive charge, In2S3Washing and drying the powder carrying negative charges, and treating the powder for two hours under the 453K condition;
(10) the treated powder was mixed with a chloroplatinic acid solution having a concentration of 2wt%, and irradiated under a 300 watt xenon lamp equipped with a 400 nm filter for 1 hour to obtain a photocatalyst for hydrogen production by water decomposition.
(11) The water decomposition hydrogen preparation photocatalyst is also mixed with laccase and deionized water and dried to prepare the formaldehyde degradation photocatalyst.
Example 7
Preparation method of photocatalyst preparation, perovskite type metal oxide La2Ti2O7With sulfide In2S3P-N heterostructure La constructed through electrostatic assembly2Ti2O7/In2S3Then loading nano platinum and laccase to prepare a photocatalyst preparation capable of realizing solar hydrogen production and solar formaldehyde degradation, wherein the perovskite type metal oxide La2Ti2O7With sulfide In2S3The mass ratio of (1) to (2) is 12.5:1.0, the content of the loaded nano platinum is 3wt%, and the content of the laccase is 1 wt%. The visible light absorption of the prepared photocatalyst preparation is continuously adjustable within 500-600 nm.
The preparation method specifically comprises the following steps:
(1) controlling the temperature to be 283K, mixing titanium acetate and lanthanum nitrate, and dissolving the mixture in deionized water to obtain a transparent solution;
(2) controlling the temperature to be 283K, and mixing sodium hydroxide and deionized water to prepare a transparent solution, wherein the concentration of the sodium hydroxide is 2 mol/L;
(3) controlling the temperature to be 283K, mixing the solution drop by drop and stirring the solution continuously and violently to obtain a white milky mixed solution;
(4) controlling the temperature to 603K, sealing the mixed solution in a reaction kettle, keeping the temperature for 24 hours to obtain a white solid, and washing and drying the white solid;
(5) placing the white solid in DMF, and keeping for 48 hours under the ultrasonic condition to obtain the ultrathin N-type semiconductor La2Ti2O7The white emulsion of (4);
(6) controlling the temperature to be 283K, weighing indium nitrate, hexadecyl trimethyl ammonium bromide and thioacetamide, mixing, dissolving in deionized water, and continuously stirring to obtain a transparent solution;
(7) refluxing the clear solution at 368K for 90 minutes to obtain a yellow precipitate;
(8) washing and drying the yellow precipitate S2 by using absolute ethyl alcohol and deionized water, and carrying out the same treatment In the step (5) to obtain the ultrathin P-type semiconductor In2S3The yellow emulsion of (1); (ii) a
(9) The ultra-thin N-type semiconductor La is mixed according to the mass ratio of 12.5:1.02Ti2O7And ultra-thin P-type semiconductor In2S3Mixing dropwise and performing ultrasonic treatment, during which the two subjected to ultrasonic stripping are detected to carry different kinds of charges on the surfaces by measuring the Zeta potential of the two, wherein La2Ti2O7Carrying a positive charge, In2S3Washing and drying the powder carrying negative charges, and treating the powder for two hours under the 453K condition;
(10) the treated powder was mixed with a chloroplatinic acid solution having a concentration of 2wt%, and irradiated under a 300 watt xenon lamp equipped with a 400 nm filter for 1 hour to obtain a photocatalyst for hydrogen production by water decomposition.
(11) The water decomposition hydrogen preparation photocatalyst is also mixed with laccase and deionized water and dried to prepare the formaldehyde degradation photocatalyst.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (6)
1. A preparation method of a photocatalyst preparation is characterized in that perovskite type metal oxide La is used2Ti2O7With sulfide In2S3P-N heterostructure La is assembled and constructed2Ti2O7/ In2S3Then loading nano platinum and laccase to prepare the photocatalyst preparation for realizing solar hydrogen production and solar formaldehyde degradation, wherein the method specifically comprises the following steps:
(1) controlling the temperature to be 263K-283K, mixing and dissolving titanium acetate and lanthanum nitrate in deionized water to obtain a transparent solution;
(2) controlling the temperature to be 273K-283K, and mixing sodium hydroxide and deionized water to prepare a transparent solution;
(3) controlling the temperature to be 273K-283K, and mixing the solution drop by drop and continuously and violently stirring to obtain a white milky mixed solution;
(4) controlling the temperature to 603K, sealing the mixed solution in a reaction kettle, keeping the temperature for 24 hours to obtain a white solid, and washing and drying the white solid;
(5) placing the white solid in DMF, and keeping for 48 hours under the ultrasonic condition to obtain the ultrathin N-type semiconductor La2Ti2O7The white emulsion of (4);
(6) controlling the temperature to be 263K-283K, weighing indium nitrate, hexadecyl trimethyl ammonium bromide and thioacetamide, mixing, dissolving in deionized water, and continuously stirring to obtain a transparent solution;
(7) refluxing the clear solution at 368K for 90 minutes to obtain a yellow precipitate;
(8) washing and drying the yellow precipitate by using absolute ethyl alcohol and deionized water, and carrying out the same treatment In the step (5) to obtain the ultrathin P-type semiconductor In2S3The yellow emulsion of (1); n-type semiconductor La subjected to ultrasonic stripping2Ti2O7And P-type semiconductor In2S3The Zeta potential of the two is measured to find that the surfaces of the two carry different kinds of charges, wherein La2Ti2O7Carrying a positive charge, In2S3Carry a negative charge;
(9) mixing the ultrathin N-type semiconductor La with different mass ratios according to the proportion2Ti2O7And ultra-thin P-type semiconductor In2S3Mixing dropwise and performing ultrasonic treatment, washing and drying the obtained powder, and treating for two hours under the 453K condition;
(10) mixing the treated powder with a chloroplatinic acid solution, and irradiating for 1 hour under the condition of a 300-watt xenon lamp provided with a 400-nanometer optical filter to obtain a water-decomposed hydrogen preparation photocatalyst;
(11) the water decomposition hydrogen preparation photocatalyst is also mixed with laccase and deionized water and dried to prepare the formaldehyde degradation photocatalyst.
2. The method according to claim 1, wherein the perovskite-type metal oxide La is2Ti2O7With sulfide In2S3The mass ratio of (A) to (B) is 2.5:1.0-12.5: 1.0.
3. The method of claim 1, wherein the supported nano-platinum is present in an amount of 1-3wt%, the laccase is present in an amount of 0-1wt%, and the laccase is not present in an amount of 0.
4. The method of claim 1, wherein the concentration of NaOH in step (2) is 2 mol/L.
5. The method for preparing photocatalyst preparation as claimed in claim 1, wherein in step (9) the ultra-thin N-type semiconductor La is used2Ti2O7And ultra-thin P-type semiconductor In2S3The mass ratio of (A) to (B) is 7.5: 1.0.
6. The method of claim 1, wherein the concentration of the chloroplatinic acid solution in step (10) is 2 wt%.
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