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

Info

Publication number
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
Authority
CN
China
Prior art keywords
sio
purity
metastable phase
preparation
metastable
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110551331.4A
Other languages
Chinese (zh)
Other versions
CN113213496A (en
Inventor
伍媛婷
王笑颖
韩琳
胡靖悦
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN202110551331.4A priority Critical patent/CN113213496B/en
Publication of CN113213496A publication Critical patent/CN113213496A/en
Application granted granted Critical
Publication of CN113213496B publication Critical patent/CN113213496B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • 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)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110551331.4A CN113213496B (en) 2021-05-20 2021-05-20 High-purity metastable phase Bi 2 O 2 SiO 3 Is prepared by the preparation method of (2)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110551331.4A CN113213496B (en) 2021-05-20 2021-05-20 High-purity metastable phase Bi 2 O 2 SiO 3 Is prepared by the preparation method of (2)

Publications (2)

Publication Number Publication Date
CN113213496A CN113213496A (en) 2021-08-06
CN113213496B true CN113213496B (en) 2023-07-25

Family

ID=77093265

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110551331.4A Active CN113213496B (en) 2021-05-20 2021-05-20 High-purity metastable phase Bi 2 O 2 SiO 3 Is prepared by the preparation method of (2)

Country Status (1)

Country Link
CN (1) CN113213496B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115646479B (en) * 2022-10-21 2023-11-24 陕西科技大学 Preparation method of organic matter modified BSO heterogeneous photocatalytic material
CN116020494B (en) * 2022-10-21 2024-07-19 陕西科技大学 3D crosslinked porous bismuth silicate composite material and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112536050A (en) * 2020-12-15 2021-03-23 陕西科技大学 Bi2O2SiO3-Si2Bi24O40Preparation method of-BiOX double-heterojunction composite photocatalyst

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010037187A (en) * 2008-07-10 2010-02-18 Fujifilm Corp METHOD FOR PRODUCING Bi12XO20 POWDER, Bi12XO20 POWDER, RADIATION PHOTOCONDUCTOR, RADIATION DETECTOR, AND RADIATION IMAGING PANEL

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112536050A (en) * 2020-12-15 2021-03-23 陕西科技大学 Bi2O2SiO3-Si2Bi24O40Preparation method of-BiOX double-heterojunction composite photocatalyst

Also Published As

Publication number Publication date
CN113213496A (en) 2021-08-06

Similar Documents

Publication Publication Date Title
CN113213496B (en) High-purity metastable phase Bi 2 O 2 SiO 3 Is prepared by the preparation method of (2)
Saedy et al. Hydrothermal synthesis and physicochemical characterization of CuO/ZnO/Al2O3 nanopowder. Part I: Effect of crystallization time
CN101024503A (en) Method for preparing ordered mesoporous aluminium oxide
CN101549890B (en) Solvothermal synthesis method of nickel cobaltate nano particles
CN102757081B (en) Synthesis method of cerium oxide hydrosol dispersed by PVA (Polyvinyl Alcohol)
CN104477978B (en) A kind of method preparing perovskite nano-powder
Kakihana et al. The synthesis of photocatalysts using the polymerizable-complex method
CN113198518B (en) Epitaxial grain molecular sieve packaged sub-nano metal catalyst, and preparation method and application thereof
US20050130838A1 (en) Nano-scale magnetic solid base catalyst and its preparatiion method
CN112875755A (en) Preparation method of bismuth tungstate nano powder
KR20060009876A (en) Method for producing zirconium oxide and zirconium-based mixed oxide
CN106082298B (en) Preparation method of cerium-bismuth composite oxide nanorod material
CN106430289B (en) A kind of method of low temperature preparation high-specific area nano gallate spinel
CN108654663B (en) Boron-nitrogen co-doped single crystal mesoporous TiO prepared by mixed nitrate molten salt method2Method for catalyzing materials
CN106006743B (en) A kind of orthorhombic phase black WO3Preparation method
CN109225201B (en) Preparation method and application of micro-nano tungsten oxide
CN1076010C (en) Preparation of nanometer yttrium aluminium garnet powder without coacervate
CN109078636A (en) A kind of plasma photocatalysis agent, preparation method and its application in hydrogen manufacturing
CN115090281B (en) Three-dimensional flaky Na-alpha-MnO 2 Preparation method of (C) and application of (C) in catalytic combustion of VOCs
CN115092966B (en) Mixed phase MnO of three-dimensional lamellar structure for toluene catalytic combustion 2 Is prepared by the preparation method of (2)
CN110697773A (en) Preparation method of loose macroporous bismuth oxide nano material
CN113877585B (en) Apricot kernel-shaped hierarchical structure cerium-iron bimetallic composite oxide and preparation method and application thereof
CN114014349B (en) Preparation method of YAG nano powder
CN114604888B (en) Method for preparing rod-like, cube-like and polyhedral cerium oxide
CN116984007A (en) 0D/2DAg 3 PO 4 /Bi 3 TiNbO 9 Heterojunction photocatalyst, preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant