CN115672305A - CeVO 4 Preparation method and application of hollow cubic structure - Google Patents
CeVO 4 Preparation method and application of hollow cubic structure Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 9
- 239000013049 sediment Substances 0.000 claims abstract description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 7
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 7
- 238000006722 reduction reaction Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 5
- 239000010935 stainless steel Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005070 sampling Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims abstract 2
- 230000001699 photocatalysis Effects 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000003595 spectral effect Effects 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
- CKLJMWTZIZZHCS-UHFFFAOYSA-N D-OH-Asp Natural products OC(=O)C(N)CC(O)=O CKLJMWTZIZZHCS-UHFFFAOYSA-N 0.000 description 1
- CKLJMWTZIZZHCS-UWTATZPHSA-N L-Aspartic acid Natural products OC(=O)[C@H](N)CC(O)=O CKLJMWTZIZZHCS-UWTATZPHSA-N 0.000 description 1
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 1
- 229960005261 aspartic acid Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000012084 conversion product Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- ALTWGIIQPLQAAM-UHFFFAOYSA-N metavanadate Chemical compound [O-][V](=O)=O ALTWGIIQPLQAAM-UHFFFAOYSA-N 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
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Abstract
CeVO 4 Preparation method and application of hollow cubic structure, 1) CeCl is prepared 3 ·7H 2 O and NH 4 VO 3 Dispersing in saturated NaCl solution of over 4 times weight, and adding ethanol of over 8 times weight to obtain mixed solution; ceCl 3 ·7H 2 O and NH 4 VO 3 In a molar ratio of 1:0.75-1.5; 2) Stirring the mixed solution obtained in the step 1) for 0.3-1 hour, transferring the mixed solution into a stainless steel Teflon-lined high-pressure reaction kettle, and heating the mixed solution at the temperature of 150-180 ℃ for 24 +/-8 hours; 3) After the reaction is finished, naturally cooling the sample to room temperature, centrifuging the sediment at the bottom, washing the sediment for 2-5 times by using ethanol and deionized water respectively, and drying the sediment in a freeze dryer for 24 +/-8 hours to finally obtain the dark brown CeVO 4 And (3) sampling. CeVO is mixed with 4 Application of hollow cubic structure to lightCatalyzing the reduction reaction of carbon dioxide. The method has low cost, simple preparation and large-scale production.
Description
Technical Field
The invention relates to a CeVO 4 A preparation method and application of a hollow cubic structure belong to the technical field of new materials.
Background
The more ternary inorganic semiconductors and multicomponent compounds have been used in recent decadesAre increasingly used in the field of photocatalysis. Among them, ternary vanadate semiconductors have been preliminarily studied for their abundant atomic species and wide spectral absorption range, and are listed as one of the most promising catalysts for solar energy conversion. Vanadates are generally present in the ratio of three chemical components, namely orthovanadate, metavanadate and pyrovanadate. In order to synergistically improve the reactivity and the selectivity of a solar energy conversion product, the microstructure and the physicochemical properties of the ternary vanadate catalyst need to be further researched. The results of the preliminary studies based on this group of subjects showed that CeVO 4 The photocatalytic performance and the selectivity of the carbon dioxide reduction product are closely related to the morphology and the surface interface atoms. In addition, for CeVO 4 The development strategies of the photocatalytic material include widening a light absorption range, finely adjusting an energy band structure, improving carrier separation efficiency, increasing absorption and desorption of reactants and the like, and high efficiency of photocatalytic carbon dioxide reduction reaction and high selectivity of products can be realized.
Chinese patent 201810073654.5 discloses a CeVO 4 Method for preparing functional material by using CeO as fast-heating solid phase 2 And V 2 O 5 Grinding and mixing raw materials, preheating a reaction furnace to a set reaction temperature, directly putting the mixture into the heated reaction furnace, and quickly synthesizing CeVO 4 Functional materials, but V may be caused during temperature rise 2 O 5 The raw materials are volatilized to cause that the product contains a small amount of CeO 2 Impurities.
Document 1 (M.Wang, X.Hu, Z.Zhan, T.Sun, Y.Tang, facility failure of CeVO) 4 Materials Letters,2019, 253, 259-262 reported that L-aspartic acid was used as a structure directing agent, ce (NO) 3 )·6H 2 O and NH 4 VO 3 The reaction is carried out for 12 hours at the high temperature of 150 ℃, and CeVO with the average size of 5 mu m and the shell wall thickness of about 500nm is hydrothermally synthesized 4 Hollow microspheres.
Hitherto, theThe main problems of the photocatalytic material are non-uniform size, small specific surface area, low charge separation efficiency and poor photocatalytic performance. Although a plurality of micro-nano CeVO are successfully prepared by carrying out shape design and optimization on materials 4 Structures including rods, spheres, dendrites, flowers, etc., but there are still few reports on methods for preparing hollow structures.
Disclosure of Invention
The invention aims to provide a CeVO 4 The preparation method and the application of the hollow cubic structure have the advantages of low production cost, simple operation and better repeatability. CeVO 4 The hollow cubic structure has higher catalytic activity, namely higher CO precipitation performance, and has certain commercial value.
The invention adopts the following technical scheme: ceVO 4 The preparation method of the hollow cubic structure comprises the following steps:
(1) Reacting CeCl 3 ·7H 2 O and NH 4 VO 3 Dispersing in saturated NaCl solution with weight more than 4 times, and adding ethanol with weight more than 8 times to obtain mixed solution; ceCl 3 ·7H 2 O and NH 4 VO 3 In a molar ratio of 1:0.75-1.5;
(2) Stirring the mixed solution obtained in the step (1) for 0.3-1 hour, transferring the mixed solution into a stainless steel Teflon-lined high-pressure reaction kettle, and heating the mixed solution at the temperature of 150-180 ℃ for 24 +/-8 hours;
(3) After the reaction is finished, the reaction kettle is naturally cooled to room temperature, sediment at the bottom is centrifuged and washed by ethanol and deionized water for 2-5 times respectively, and then the sediment is dried in a freeze dryer for 24 +/-8 hours to finally obtain dark brown CeVO 4 And (3) sampling.
Further, the volume ratio of the saturated NaCl solution to the ethanol in the step (1) is 4 (milliliters) to 10 (milliliters).
Further, 1 mmol of CeCl was immobilized in the step (1) 3 ·7H 2 O, post-addition of NH 4 VO 3 The amounts of (A) were 0.75,1 and 1.25 mmol, respectively. CeVO is regulated and controlled by adjusting the adding proportion of Ce and V precursors 4 And forming a hollow cubic structure.
CeVO prepared according to the above method 4 A hollow cubic structure.
CeVO obtained by the preparation method 4 The hollow cubic structure is used for photocatalytic carbon dioxide reduction.
The invention has the beneficial effects that: ceVO is obtained by the preparation procedure described in the present invention, i.e. the solvothermal method 4 The hollow cubic structure has higher catalytic activity. The reaction involved in the invention takes a mixed solution of saturated NaCl and ethanol as a solvent and is carried out at 160 ℃; in addition, ceVO is regulated and controlled by controlling the precursor proportion of Ce and V 4 Formation of hollow cubic structure and photocatalytic CO 2 Reducing the precipitation performance of CO products.
Drawings
Fig. 1 is an X-ray diffraction (XRD) pattern of the products of example CeV2 of the present invention and comparative examples CeV1, ceV 3.
In FIG. 2, a, b, c and d are images of CeV2 scanning electron microscopes of examples and comparative examples of the present invention.
FIG. 3 is a graph of the ultraviolet-visible absorption diffraction spectra (UV-Vis) of the products of example CeV2 according to the invention and of the comparative examples CeV1 and CeV 3.
FIG. 4 is a schematic diagram of the photocatalytic reduction of carbon dioxide using the example of the present invention, where a in FIG. 4 is the CO yield and b in FIG. 4 is the CO yield.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
Hollow cubic structure CeVO 4 The preparation method comprises the following steps:
(1) 1 mmol of CeCl respectively 3 ·7H 2 O with 0.75,1 and 1.25 mmoles of NH, respectively 4 VO 3 Dispersing in 4 ml of saturated NaCl solution, and then adding 10 ml of ethanol to obtain a mixed solution;
(2) Stirring the mixed solution obtained in the step (1) for 0.5 hour, transferring the mixed solution into a Teflon reaction kettle of a stainless steel high-pressure kettle with the volume of 30 ml, and heating the mixed solution in an oven for 24 hours at the temperature of 160 ℃;
(3) After the reaction is finished, the sample is naturally cooled to room temperature, and the bottom is precipitatedThe material was centrifuged and washed 3 times with ethanol and deionized water, respectively, and then dried in a lyophilizer for 24 hours to finally obtain dark brown CeVO 4 And (4) nano samples.
Example 1
(1) 1 mmol of CeCl 3 ·7H 2 O and 1 mmol NH 4 VO 3 Respectively added to a mixture of 4 ml of saturated NaCl solution and 10 ml of ethanol.
(2) The mixture was stirred for 0.5 hour, transferred to a stainless steel autoclave teflon liner with an internal volume of 30 ml, and placed in an oven at 160 degrees celsius for 24 hours.
(3) After the reaction was complete, the sample was allowed to cool to room temperature. Centrifuging the bottom precipitate and washing with anhydrous ethanol and deionized water 3 times, respectively, followed by drying in a freeze dryer for 24 hours to obtain dark brown CeVO 4 Nanosheet sample (CeV 2).
Comparative example
The procedure is essentially the same as in the examples, except that NH is added 4 VO 3 The amounts of (A) and (B) were varied and were 0.75 mmol (CeV 1) and 1.25 mmol (CeV 3), respectively.
The product was analyzed by X-ray diffraction (XRD), scanning Electron Microscope (SEM), ultraviolet-visible diffraction spectroscopy (UV-Vis).
Fig. 1 is an XRD pattern of the products of comparative example and example, and purity and crystallinity of the prepared samples were characterized by XRD. FIG. 1 shows that all prepared samples are CeVO 4 Pure tetragonal phase of (A), (B), (C)
I41/amd), all diffraction peaks correspond to JCPDS No.12-0757, with no impurity peaks. CeVO 4 The (200), (112) and (312) crystal planes of (a) have three strong diffraction peaks at diffraction angles 2 θ of 24.03 °,32.40 ° and 47.86 °, respectively, indicating that the prepared samples have high crystallinity.
FIGS. 2a and 2c are comparative examples CeV1 and CeV3, respectivelySEM can see that CeV1 hollow lattices are formed preliminarily, the edges are not obvious, ceV3 has a small amount of single rod-shaped structures, and the appearance is not uniform. FIGS. 2b and 2d are enlarged SEM pictures of the example CeV2 product in a large scale, and it can be seen that CeVO 4 The hollow cubic structure accounts for more than 80 percent, and has clear cubic edges and the wall thickness of about 600 nanometers.
FIG. 3 is a UV-Vis diagram of the products of comparative and examples, from which it can be seen that CeVO was synthesized 4 The absorption band edge of the product is about 760 nanometers, and the product has wider spectral absorption.
Application example
The carbon dioxide photocatalytic reduction reaction is carried out at normal temperature and normal pressure. First, a 10 mg sample of the powder prepared by the method of the present invention was uniformly distributed on a sample stage having an area of 4.91 cm square, and placed in a quartz photocatalytic reaction system having a volume of 440 ml. Second, high purity CO injected in the reactor 2 Gas (99.99%), excess CO 2 NaHCO for gas 3 The solution was collected and 1 ml of ultrapure water was injected into the reactor and magnetic stirring was turned on. Finally, the xenon lamp (Microsolr 300W) was turned on and samples were taken periodically. Starting the work timing from the xenon lamp, extracting 1 ml of gas from the reaction cell every other hour, injecting the gas into a gas chromatograph, analyzing products, turning off the lamp until 5 hours later, recording and analyzing data.
As shown in FIG. 4, the average yield of CO of CeV2 was 78.12. Mu. Mol g -1 h -1 5.47 and 6.96 times of CeV1 and CeV 3. The result shows that the CeVO prepared based on the NaCl hard template method 4 Hollow cubic structure, when the ratio of cerium to vanadium is 1:1, i.e., ceV2, has higher catalytic activity and CO product selectivity.
Claims (4)
1. CeVO 4 The preparation method of the hollow cubic structure is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
(1) Reacting CeCl 3 ·7H 2 O and NH 4 VO 3 Dispersing in saturated NaCl solution of over 4 times weight, and adding ethanol of over 8 times weight to obtain mixed solution; ceCl 3 ·7H 2 O and NH 4 VO 3 In a molar ratio of 1:0.75-1.5;
(2) Stirring the mixed solution obtained in the step (1) for 0.3-1 hour, transferring the mixed solution into a stainless steel Teflon-lined high-pressure reaction kettle, and heating the mixed solution at the temperature of 150-180 ℃ for 24 +/-8 hours;
(3) After the reaction is finished, naturally cooling the sample to room temperature, centrifuging the sediment at the bottom, washing the sediment for 2-5 times by using ethanol and deionized water respectively, and drying the sediment in a freeze dryer for 24 +/-8 hours to finally obtain the dark brown CeVO 4 And (4) sampling.
2. CeVO according to claim 1 4 The preparation method of the hollow cubic structure is characterized by comprising the following steps: in the step (1), naCl is used as a hard template, a mixed solution of saturated NaCl solution and ethanol is used as a solvent, and the volume ratio of the saturated NaCl solution to the ethanol is 4: 10.
3. CeVO of hollow cubic structure according to claim 1 4 The preparation method is characterized by comprising the following steps: immobilization of 1 millimolar CeVO 4 The formation of the hollow structure is regulated by adjusting the proportion of Ce and V precursors, i.e. NH is added 4 VO 3 The amounts are 0.75,1,1.25 mmoles each.
4. CeVO prepared by the method of any one of claims 1 to 4 4 The hollow cubic structure material is applied to photocatalytic carbon dioxide reduction reaction.
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