CN109663600B - One-step preparation method of multiphase uniform load - Google Patents
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- 238000002360 preparation method Methods 0.000 title abstract description 32
- 239000010453 quartz Substances 0.000 claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 25
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- QXYJCZRRLLQGCR-UHFFFAOYSA-N molybdenum(IV) oxide Inorganic materials O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims description 6
- 238000011068 loading method Methods 0.000 abstract description 20
- 239000007789 gas Substances 0.000 abstract description 19
- 239000002135 nanosheet Substances 0.000 abstract description 14
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 13
- 239000001257 hydrogen Substances 0.000 abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 13
- 150000001875 compounds Chemical class 0.000 abstract description 11
- 239000002105 nanoparticle Substances 0.000 abstract description 9
- 239000006227 byproduct Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000003039 volatile agent Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910015667 MoO4 Inorganic materials 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- B01J27/051—Molybdenum
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
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Abstract
The invention discloses a one-step preparation method of a multiphase uniform load, and relates to the technical field of preparation of multiphase loads. The one-step preparation method of the multiphase uniform load comprises the steps of respectively placing a plurality of volatile matters in different temperature areas of a quartz tube; an auxiliary gas is introduced into the quartz tube and calcined downstream in the flow direction of the auxiliary gas in the quartz tube to form a heterogeneous uniform load. And specifically will utilize CdS and MoO3The volatilization temperature is similar, and the CdS nanoparticles can be volatilized together with the air flow and react in a high-temperature region to obtain the CdS nanoparticles in the ultrathin hexagonal MoO2The nano-sheet is uniformly loaded with the compound, and has good photocatalytic hydrogen production performance. The method is used for multi-phase loading, has the characteristics of simple preparation method, low preparation cost, no generation of byproducts which are unfavorable to the environment, uniform loading, excellent performance and the like, and has good application prospect for the preparation of some two-phase materials in an energy environment.
Description
Technical Field
The invention relates to the technical field of preparation of multiphase loads, in particular to a one-step preparation method of a multiphase uniform load.
Background
Nowadays, the energy crisis is still a big problem of world progress and development, the development of clean and renewable hydrogen energy becomes a big hotspot of the development nowadays, and the hydrogen production technology by photocatalytic water decomposition becomes a hotspot of the energy technology nowadays because the traditional hydrogen production technology consumes a lot of non-renewable energy and can generate pollution. The basic requirements of the photocatalytic semiconductor are that firstly the position of a conduction band is more negative than zero, the position of a valence band is more than 1.23ev, namely the forbidden band width spans and is more than 1.23ev, so that the photocatalytic semiconductor can be used for decomposing water, secondly the commonly used semiconductor titanium dioxide can only absorb ultraviolet light, the ultraviolet light only accounts for 4 percent of sunlight, and in order to expand the utilization of the sunlight, the semiconductor with the proper forbidden band width is required, wherein the most typical semiconductor is CdS. However, CdS also has its disadvantages, firstly the problem of photo-corrosion, and secondly its easy recombination of photo-generated electron holes, which reduces the rate of photocatalysis. The common improvement method is to load a cocatalyst on the semiconductor to improve the separation of electron and hole, or to prepare a heterostructure of two semiconductors, and to improve the above problems by matching the energy levels of the two semiconductors. The two-phase composite method generally has the problems of more complex preparation or uneven load and the like, and can generate a plurality of byproducts which are not environment-friendly, so that a plurality of composite structures are difficult to construct.
Disclosure of Invention
The invention aims to provide a one-step preparation method of a multiphase uniform load, which can prepare the uniform multiphase load in one step, has the characteristics of simple preparation method, low preparation cost, no generation of byproducts which are unfavorable to the environment, uniform load, excellent performance and the like, and has good application prospect in energy environment for the preparation of some two-phase materials.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a one-step preparation method of a multiphase uniform load, which comprises the following steps:
placing a plurality of volatile matters in different temperature areas of a quartz tube respectively;
an auxiliary gas is introduced into the quartz tube and calcined downstream in the flow direction of the auxiliary gas in the quartz tube to form a heterogeneous uniform load.
The one-step preparation method of the multiphase uniform load provided by the embodiment of the invention can prepare the multiphase load by a quick and simple one-step method, and the multiphase load compound with controllable loading process is used for photocatalytic hydrogen production, so that the method has a great application prospect. Also, in the examples of the present invention, MoO is used3As a precursor, MoO3Under a certain reducing atmosphere, ultrathin hexagonal MoO can be prepared by controlling airflow2Nanosheets, utilizing CdS and MoO3Features similar volatilization temperature and blowing out with air flowPoint, the two are volatilized together and react in a high temperature region to obtain CdS nano-particles in ultrathin hexagonal MoO2The nano-sheet is uniformly loaded with the compound, and has good photocatalytic hydrogen production performance. The method for two-phase loading has the characteristics of simple preparation method, low preparation cost, no generation of byproducts which are unfavorable to the environment, uniform loading, excellent performance and the like, and has good application prospect for the preparation of some two-phase materials in an energy environment.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 shows CdS/MoO prepared in example 1 of the present invention2SEM picture of (1);
FIG. 2 shows CdS/MoO prepared in example 2 of the present invention2SEM picture of (1);
FIG. 3 shows CdS/MoO prepared in example 3 of the present invention2SEM picture of (1);
FIG. 4 shows CdS/MoO prepared by the embodiment of the invention2XRD pattern of (a);
FIG. 5 is a performance diagram of samples with different CdS loadings provided in embodiments 1-3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a specific description of the one-step preparation of heterogeneous homogeneous loads according to the examples of the present invention.
A one-step method of making a heterogeneous homogeneous load comprising:
placing a plurality of volatile matters in different temperature areas of a quartz tube respectively;
an auxiliary gas is introduced into the quartz tube and calcined downstream in the flow direction of the auxiliary gas in the quartz tube to form a heterogeneous uniform load.
In detail, the multiphase load can be prepared by a quick and simple one-step method, and the multiphase load compound with controllable load process is used for photocatalytic hydrogen production, so that the method has a great application prospect.
Further, in a preferred embodiment of the present invention, the placing of the plurality of volatiles in different temperature zones of the quartz tube respectively comprises: the two volatiles were placed in different temperature zones of a quartz tube, respectively. Of course, in other embodiments of the present invention, the number of the volatile matters may also be multiple, and is not limited to two, and may also be three, four or more, and the embodiments of the present invention are not limited.
Further, in a preferred embodiment of the invention, one of the two volatiles is CdS and the other is MoO3. Of course, in other embodiments of the present invention, the type of volatile can be selected according to the requirement, and is not limited to CdS and MoO3. Wherein, auxiliary gas is introduced into the quartz tube to lead CdS and MoO3Calcining in a quartz tube to form a multiphase uniform load of CdS/MoO2And (4) loading the substance. The obtained compound has good photocatalytic hydrogen production performance. CdS/MoO prepared by the method2The load is simple, convenient and feasible in process and environment-friendly, solves the problems of uncontrollable amount and poor two-phase composite uniformity under the traditional calcination condition, and has good photocatalytic hydrogen production performance.
Further, in the preferred embodiment of the invention, the temperature of the position of CdS is 780-795 ℃, and MoO is3The temperature of the position is 795-805 ℃. Preferably, the temperature of the position of CdS is 790 ℃, MoO3The temperature of the location of (2) is 800 ℃. Of course, in other embodiments of the invention, of CdSThe temperature of the location may also be about 790 ℃, MoO3The temperature of the location may also be around 800 c, and embodiments of the invention are not limited. Adding MoO3As a precursor, MoO3Under a certain reducing atmosphere, ultrathin hexagonal MoO can be prepared by controlling airflow2Nanosheets, utilizing CdS and MoO3The volatilization temperature is similar, and the CdS nanoparticles can be volatilized together with the air flow and react in a high-temperature region to obtain the CdS nanoparticles in the ultrathin hexagonal MoO2The nano-sheet is uniformly loaded with the compound, and has good photocatalytic hydrogen production performance. The method for two-phase loading has the characteristics of simple preparation method, low preparation cost, no generation of byproducts which are unfavorable to the environment, uniform loading, excellent performance and the like, and has good application prospect for the preparation of some two-phase materials in an energy environment.
Further, in the preferred embodiment of the present invention, MoO3The dosage of the CdS is 5g, and the dosage of the CdS is 0.6-2 g. By adjusting the CdS and MoO added in the early stage3In different proportions, to meet various production requirements.
Further, in the preferred embodiment of the present invention, the amount of CdS may be specifically any one of 0.6g, 1g, and 2 g. Of course, in other embodiments of the present invention, the amount of CdS may also be adjusted according to requirements, and the embodiments of the present invention are not limited.
Further, in a preferred embodiment of the present invention, the auxiliary gas is a reducing gas. The reducing gas is used in the examples of the invention mainly for reducing MoO3To MoO2. Of course, in other embodiments of the present invention, the auxiliary gas may be selected to be other kinds of gases, such as an inert gas, an oxidizing gas, etc., according to the nature of different kinds of volatile matters, and the embodiments of the present invention are not limited.
Further, in a preferred embodiment of the present invention, the reducing gas may be 10% Ar/H2. In other embodiments of the invention, of course, the specific type of reducing gas may also be selected as desired,the embodiments of the present invention are not limited.
Further, in the preferred embodiment of the present invention, the flow rate of the reducing gas is 180 to 220 sccm. Through the setting of the flow rate and the selection of the amount of each volatile matter, high-quality multiphase uniform load can be effectively synthesized.
Further, in the preferred embodiment of the present invention, CdS/MoO2The thickness of the support is 1 to 1.5 nm. This scheme utilizes MoO3The MoO prepared by the co-volatilization of the compound and CdS2The nano sheet is very thin, the thickness of the nano sheet is only a few nanometers, the thickness of the nano sheet is about 1.1nm, when CdS particles are loaded on the nano sheet, the particles are very small and uniform, two phases are in good contact to form an interface structure, and the interface structure is in full contact with water molecules. By adjusting the CdS and MoO added in the early stage3The amount of the two compounds is regulated and controlled. The formed two-phase compound fully combines the advantages of the two substances, and has good light absorption performance and photocatalytic hydrogen production performance. Compared with the traditional two-phase photocatalyst compounding method, the method has the advantages of simple preparation process, low cost, environmental friendliness and excellent performance.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
This example provides a one-step preparation method of a heterogeneous homogeneous load, comprising the following steps:
s1: 5g of MoO were added separately3And 0.6g of CdS are placed in different temperature zones in a quartz tube, the temperature of the CdS is 780-795 ℃, and MoO is performed3The temperature of the position is 795-805 ℃;
s2: introducing an auxiliary gas into the quartz tube to make CdS and MoO3Calcining in quartz tube to form CdS/MoO2And (4) loading the substance.
Example 2
This example provides a one-step preparation method of a heterogeneous homogeneous load, comprising the following steps:
s1: 5g of MoO were added separately3And 1.0g of CdS are placed in different temperature zones in a quartz tube, the temperature of the CdS is 790 ℃, and MoO is adopted3In the position ofThe temperature is 800 ℃;
s2: introducing an auxiliary gas into the quartz tube to make CdS and MoO3Calcining in quartz tube to form CdS/MoO2And (4) loading the substance.
Example 3
This example provides a one-step preparation method of a heterogeneous homogeneous load, comprising the following steps:
s1: 5g of MoO were added separately3And 2g of CdS are placed in different temperature zones in a quartz tube, the temperature of the CdS is 795 ℃, and MoO is3At a temperature of 805 ℃ of the location;
s2: introducing an auxiliary gas into the quartz tube to make CdS and MoO3Calcining in quartz tube to form CdS/MoO2And (4) loading the substance.
Examples of the experiments
The different CdS/MoO prepared in examples 1-3 were recorded2SEM and XRD patterns of (a), three samples of different loading were prepared by varying the amount of CdS, as shown above, fig. 1-3 are different CdS/MoO, respectively2SEM image of proportion, FIG. 1 shows that when CdS is loaded in a small amount, a small amount of nanoparticles are loaded on the ultrathin nanosheets, and MoO is generated with the increase of CdS2The nano-particles loaded on the nano-sheets gradually increase until the particles are uniformly loaded on the ultra-thin nano-sheets at the maximum loading as shown in fig. 3. XRD of FIG. 4 shows that sample No. 1 with a small CdS loading has the main crystalline phase of MoO2And Cd (MoO)4) Sample No. 2 and sample No. 3 are mainly CdS and MoO2And Cd (MoO)4) And the crystallinity of No. 3 is better. Can prove that MoO2And CdS formation and formation of Cd (MoO)4) Interface, therefore most likely MoO2/CdS/Cd(MoO4) The performance of the three-phase system is improved. FIG. 5 shows the performance diagram of samples with different CdS loading, as shown in the figure, the sample No. 3 with large CdS loading has the best performance, which reaches 39.08 umol/(mg.h).
In summary, the one-step preparation method of the heterogeneous uniform load provided by the embodiment of the invention can prepare the heterogeneous load through a rapid and simple one-step method, and the heterogeneous loaded compound with controllable loading process is used for photocatalytic hydrogen production, includingHas wide application prospect. Also, in the examples of the present invention, MoO is used3As a precursor, MoO3Under a certain reducing atmosphere, ultrathin hexagonal MoO can be prepared by controlling airflow2Nanosheets, utilizing CdS and MoO3The volatilization temperature is similar, and the CdS nanoparticles can be volatilized together with the air flow and react in a high-temperature region to obtain the CdS nanoparticles in the ultrathin hexagonal MoO2The nano-sheet is uniformly loaded with the compound, and has good photocatalytic hydrogen production performance. The method for two-phase loading has the characteristics of simple preparation method, low preparation cost, no generation of byproducts which are unfavorable to the environment, uniform loading, excellent performance and the like, and has good application prospect for the preparation of some two-phase materials in an energy environment.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (6)
1. A one-step method for preparing a heterogeneous homogeneous load, comprising:
placing the two volatile matters in different temperature areas of a quartz tube respectively; one of the two volatile matters is CdS, and the other volatile matter is MoO3；
Introducing auxiliary gas into the quartz tube, and calcining the quartz tube at the downstream of the flow direction of the auxiliary gas to form a multi-phase uniform load, wherein the multi-phase uniform load is CdS/MoO2A load;
wherein the temperature of the CdS position is 780-795 ℃, and the MoO is3The temperature of the position is 795-805 ℃; the auxiliary gas is a reducing gas.
2. The one-step method of making a multiphase homogeneous load according to claim 1, wherein:
the MoO3The dosage of the CdS is 5g, and the dosage of the CdS is 0.6-2 g.
3. The one-step method of making a multiphase homogeneous load according to claim 2, wherein:
the consumption of the CdS is specifically any one of 0.6g, 1g and 2 g.
4. The one-step method of making a multiphase homogeneous load according to claim 1, wherein:
the reducing gas is 10% Ar/H2。
5. The one-step method of making a multiphase homogeneous load according to claim 1, wherein:
the flow rate of the reducing gas is 180-220 sccm.
6. The one-step method of making a multiphase homogeneous load according to claim 1, wherein:
the CdS/MoO2The thickness of the support is 1 to 1.5 nm.
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| CN105688945B (en) * | 2016-03-22 | 2018-06-15 | 福州大学 | MoS2Nanometer sheet/CdS nanowire core shell structure composite photo-catalysts |
| CN107162058A (en) * | 2017-06-30 | 2017-09-15 | 华南理工大学 | A kind of molybdenum dioxide hexagonal nano-flake and preparation method thereof |
| CN108448091B (en) * | 2018-03-20 | 2020-11-06 | 济南大学 | MoO (MoO)2/SnS2Nanocomposite and method for preparing same |
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