CN113213496B - High-purity metastable phase Bi 2 O 2 SiO 3 Is prepared by the preparation method of (2) - Google Patents

High-purity metastable phase Bi 2 O 2 SiO 3 Is prepared by the preparation method of (2) Download PDF

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CN113213496B
CN113213496B CN202110551331.4A CN202110551331A CN113213496B CN 113213496 B CN113213496 B CN 113213496B CN 202110551331 A CN202110551331 A CN 202110551331A CN 113213496 B CN113213496 B CN 113213496B
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metastable phase
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CN113213496A (en
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伍媛婷
王笑颖
韩琳
胡靖悦
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The invention discloses a high-purity metastable phasing Bi 2 O 2 SiO 3 Is prepared by the preparation method of (1). Ethanol and deionized water are used as medium, and the raw materials, the dispersing agent and the like are fully mixedAfter the synthesis, preparing and obtaining a precursor solution, obtaining wet gel by water bath, and calcining for 4 to 6 hours at a certain temperature to obtain metastable phase Bi 2 O 2 SiO 3 The method has the advantages of simple process, easy operation of equipment, low cost, and the obtained metastable phase Bi 2 O 2 SiO 3 The powder has high purity which can reach more than 98 percent.

Description

High-purity metastable phase Bi 2 O 2 SiO 3 Is prepared by the preparation method of (2)
Technical Field
The invention belongs to the technical field of photocatalysis, and in particular relates to a high-purity metastable phase Bi 2 O 2 SiO 3 Is prepared by the preparation method of (1).
Background
Bi in three single crystals which can be grown in bismuth silicate melt 2 SiO 5 Is metastable phased crystal, belongs to orthorhombic system and has lattice constantZ=4, consisting of isolated [ SiO 3 ] 2- Of chains, and these [ SiO ] 3 ] 2- The chain is composed of [ Bi ] 2 O 2 ] 2+ Separated by a layer of [ Bi ] 2 O 2 ] 2+ The layer is composed of [ BiO ] 4 ]Two-dimensional network formed by square pyramid, [ SiO ] 3 ] 2- The chain is composed of [ SiO ] 4 ]One-dimensional chains of tetrahedral formation; bi (Bi) 12 SiO 20 Is a stable phase crystal belonging to cubic system, and has lattice constant +.>The structure is that the seven-coordinated Bi-O polyhedron is identical to other Bi-O polyhedrons and SiO 4 Tetrahedron corner sharing connection; it has also been found that a new metastable phased crystal, known as Bi, is present in the system 2 O 2 SiO 3 This phase is liable to be compatible with metastable phase Bi 2 SiO 5 Confusion, it is difficult to obtain a pure phase. Pure phase Bi 2 O 2 SiO 3 The obtained and photoelectric performance such as forbidden band width, valence band position and other parameters are determined and perfected, which is favorable for clearing the relation among the crystals in the bismuth silicate system so as to form different heterojunctions,provides theoretical support for the action mechanisms of different heterojunctions of bismuth silicate systems.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a high-purity metastable phase Bi 2 O 2 SiO 3 The preparation method of the high-purity metastable phasing Bi is prepared in a bismuth silicate melt system 2 O 2 SiO 3 And can be used for regulating the band gap of other photocatalysts.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
high-purity metastable phase Bi 2 O 2 SiO 3 The preparation method of (2) comprises the following steps:
step 1, weighing 2.5 g-3.5 g of complexing agent, 2 g-4 g of dispersing agent, 2 g-4 g of bismuth nitrate (bismuth source) and 5 g-7 g of tetraethoxysilane (silicon source) as raw materials, adding the raw materials into a mixed solution containing 10mL of absolute ethyl alcohol and 3 mL-9 mL of deionized water at one time, and stirring and dissolving to obtain a precursor solution;
step 2, the precursor liquid is subjected to water bath at the temperature of 80-85 ℃ until solid wet gel is formed;
step 3, heating the obtained wet gel to 600-650 ℃ at a heating rate of 5 ℃/min, and calcining for 4-6 h to obtain high-purity metastable phase Bi 2 O 2 SiO 3 And (3) powder.
The complexing agent is citric acid, and the dispersing agent is polyethylene glycol.
The volume ratio of the absolute ethyl alcohol to the deionized water is 5 (2-4).
High purity metastable phase Bi 2 O 2 SiO 3 Is definitely metastable in phase Bi 2 O 2 SiO 3 Valence band position and forbidden band width of (2) to obtain Bi 2 O 2 SiO 3 The conduction band position of the catalyst is used for regulating and controlling the band gap of other heterogeneous bismuth silicate system photocatalysts, and provides basis for researching heterogeneous photocatalysis mechanism.
Compared with the prior art, the invention discovers that the bismuth silicate melt system is prepared by sol-gel method, heat treatment and other processesAnother new metastable phase Bi of (2) 2 O 2 SiO 3 Can be stably prepared with high repeatability. In addition, the invention can obtain metastable phase Bi 2 O 2 SiO 3 Valence band position and forbidden band width of (2) to obtain Bi 2 O 2 SiO 3 Provides theoretical basis for researching photocatalytic action mechanism of heterogeneous bismuth silicate system, and can be used for judging Bi by utilizing the result 2 O 2 SiO 3 And whether heterojunction is formed with other BSO system materials or not, so that the photocatalytic performance is effectively improved. The method has simple process, easy operation of equipment, low cost, and the obtained metastable phase Bi 2 O 2 SiO 3 High purity and no impurity phase.
Drawings
FIG. 1 shows Bi obtained in example 1 of the present invention 2 O 2 SiO 3 Is an X-ray diffraction pattern of (2).
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings and examples.
As shown in figure 1 of the drawings,
example 1
High-purity metastable phase Bi 2 O 2 SiO 3 The preparation method comprises the following steps:
1. weighing 2.5 g-3.5 g of citric acid serving as a complexing agent and 2 g-4 g of polyethylene glycol serving as a dispersing agent; respectively weighing 2 g-4 g bismuth nitrate and 5 g-7 g tetraethoxysilane as bismuth source and silicon source; the raw materials are added into a mixed solution containing 10mL of absolute ethyl alcohol and 4mL of deionized water at one time, and the precursor solution is obtained by stirring and dissolving.
2. The precursor liquid is subjected to water bath at 80 ℃ for about 40min to form solid wet gel.
3. Heating the wet gel to 600 ℃ at a heating rate of 5 ℃/min, and calcining for 4 hours to obtain high-purity metastable phase Bi 2 O 2 SiO 3 And (3) powder.
As shown in FIG. 1, the product obtained in the embodiment has obvious diffraction peaks at 11.65 degrees, 29.31 degrees and 24.05 degrees, and the diffraction peaks of the obtained product are similar to those of a standard card PDF#75-1483The diffraction peak intensity and the position of the (B) are completely matched, which shows that the obtained product is Bi with high purity 2 O 2 SiO 3 And (3) powder.
Example 2
High-purity metastable phase Bi 2 O 2 SiO 3 The preparation method comprises the following steps:
1. weighing 2.5 g-3.5 g of citric acid serving as a complexing agent and 2 g-4 g of polyethylene glycol serving as a dispersing agent; respectively weighing 2 g-4 g bismuth nitrate and 5 g-7 g tetraethoxysilane as bismuth source and silicon source; adding the raw materials into a mixed solution containing 10mL of absolute ethyl alcohol and 6mL of deionized water, stirring and dissolving to obtain a precursor solution
2. The precursor liquid is subjected to water bath at 83 ℃ for about 50min to form solid wet gel.
3. Heating the wet gel to 630 ℃ at a heating rate of 5 ℃/min, and calcining for 5 hours to obtain high-purity metastable phase Bi 2 O 2 SiO 3 And (3) powder.
Example 3
High-purity metastable phase Bi 2 O 2 SiO 3 The preparation method comprises the following steps:
1. weighing 2.5 g-3.5 g of citric acid serving as a complexing agent and 2 g-4 g of polyethylene glycol serving as a dispersing agent; respectively weighing 2 g-4 g bismuth nitrate and 5 g-7 g tetraethoxysilane as bismuth source and silicon source; the raw materials are added into a mixed solution containing 10mL of absolute ethyl alcohol and 8mL of deionized water, and the precursor solution is obtained through stirring and dissolution.
2. The precursor liquid is subjected to water bath at 85 ℃ for about 60min to form solid wet gel.
3. Heating the wet gel to 650 ℃ at a heating rate of 5 ℃/min, and calcining for 6 hours to obtain high-purity metastable phase Bi 2 O 2 SiO 3 And (3) powder.

Claims (4)

1. High-purity metastable phase Bi 2 O 2 SiO 3 The preparation method of (2) is characterized by comprising the following steps:
step 1, weighing 2.5 g-3.5 g of complexing agent, 2 g-4 g of dispersing agent, 2 g-4 g of bismuth nitrate and 5 g-7 g of tetraethoxysilane as raw materials, adding the raw materials into a mixed solution containing 10mL of absolute ethyl alcohol and 3 mL-9 mL of deionized water at a time, and stirring and dissolving to obtain a precursor solution;
step 2, the precursor liquid is subjected to water bath at the temperature of 80-85 ℃ until solid wet gel is formed;
step 3, heating the obtained wet gel to 600-650 ℃ at a heating rate of 5 ℃/min, and calcining for 4-6 h to obtain high-purity metastable phase Bi 2 O 2 SiO 3 And (3) powder.
2. The high purity metastable phase Bi according to claim 1 2 O 2 SiO 3 The preparation method is characterized in that the complexing agent is citric acid and the dispersing agent is polyethylene glycol.
3. High purity metastable phase Bi according to claim 1 or 2 2 O 2 SiO 3 The preparation method is characterized in that the volume ratio of the absolute ethyl alcohol to the deionized water is 5 (2-4).
4. The high-purity metastable phase Bi prepared in claim 1 2 O 2 SiO 3 The method is used for regulating and controlling the band gap of the heterogeneous bismuth silicate system photocatalyst.
CN202110551331.4A 2021-05-20 2021-05-20 High-purity metastable phase Bi 2 O 2 SiO 3 Is prepared by the preparation method of (2) Active CN113213496B (en)

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