CN107840365A - A kind of preparation method of bismoclite nanometer bouquet - Google Patents
A kind of preparation method of bismoclite nanometer bouquet Download PDFInfo
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- CN107840365A CN107840365A CN201610835272.2A CN201610835272A CN107840365A CN 107840365 A CN107840365 A CN 107840365A CN 201610835272 A CN201610835272 A CN 201610835272A CN 107840365 A CN107840365 A CN 107840365A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a kind of preparation method of the nanometer flower ball-shaped bismoclite adjusted by different surfaces activating agent, and this method is completed by following steps：Using five water bismuth nitrates, potassium chloride, sodium oxalate as raw material, deionized water, glacial acetic acid are mixed solvent, and magnetic agitation makes it well mixed, puts the nanometer flower ball-shaped bismoclite that reactor hydro-thermal obtains into.Bismuth salt used in the present invention, potassium chloride, oxalic acid natrium surfactant etc. are cheap and easy to get, and cost is relatively low, and require low to consersion unit, easily operation.
Description
Technical field
The invention belongs to micro Nano material synthesis technical field, and in particular to a kind of Hydrothermal Synthesiss bismoclite nanometer bouquet
And preparation method thereof.
Background technology
Bismoclite due to higher chemical stability and preferable bio-compatibility, while have at room temperature compared with
Big conduction band width (Eg=3.44eV) and higher electron excitation combine can (60meV) and gain of light coefficient (300cm-1) and make
It has unique catalysis, electricity, photoelectricity, spectrochemical property, has been a great concern, and it is passed in optics, air-sensitive
Sensor, rubber additive, pigment, rheostat etc. have wide application (Wang Zhonglin et al Science
2001,291,1947).
With industrial development, especially environmental pollution, water pollution getting worse.In terms of water pollution processing, traditional controls
Reason method, such as precipitation, absorption and dialysis processing, simply complete separation of the pollutant with water quality, can not fundamentally solve
Problem, and it is costly needed for these conventional methods improvement sewage.Photocatalitic Technique of Semiconductor is administered sewage and just lacked without above-mentioned
Point, the principle of this technology are to convert solar energy into chemical energy with semi-conducting material, and it is simple small molecule to make organic matter degradation
Inorganic matter, so as to thoroughly solve water pollution problems.Photocatalitic Technique of Semiconductor can be used for degradable organic pollutant and sterilizing is killed
Poison.Bismoclite has extensive as a kind of semi-conducting material of excellent performance in terms of sewage is administered as photochemical catalyst
Using.
The content of the invention
It is an object of the invention to provide a kind of simple hydro-thermal method, with five water bismuth nitrates and potassium chloride, glacial acetic acid, sodium oxalate
For raw material, deionized water is solvent, and the bismoclite of different-shape is obtained by adding different surfactants.
A kind of bismoclite nanometer bouquet preparation method, it is characterised in that comprise the following steps：
(1) weigh appropriate bismuth salt, add in 2~5ml glacial acetic acid, 15~30min of electromagnetic agitation obtains A liquid.
(2) 1~5mmol potassium chloride is weighed, 1~5mmol sodium oxalates add 10~50ml distilled water and obtain B liquid.
(3) B liquid is added dropwise in A liquid, adds proper amount of surfactant and stir 30~60min, obtained white suspended
Liquid C.
(4) 10~20ml C liquid is measured to be put into 25~50ml reactors, maintain the temperature at 100~200 DEG C stand 1~
18h。
(5) by the solid product obtained in reactor distillation water washing 1~3 time, then with organic solvent washing 1~3 time,
Obtain product and kept for 20~60 DEG C, dry 12~24h, obtain bismoclite nanometer bouquet.
The present invention is raw material using five water bismuth nitrates, and the pattern of product is adjusted using second surfactant, has equipment letter
Singly, the features such as easy to operate, it is advantageously implemented large-scale industrial production.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of bismoclite bouquet in embodiment 1；
Fig. 2 is the electron scanning micrograph of bismoclite nanometer sheet in embodiment 4；
Fig. 3 is the XRD piece of bismoclite bouquet in embodiment 1；
Embodiment：
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment 1：
(1) the water bismuth nitrates of 1mmol five are weighed, are added in 2ml glacial acetic acid, 15~30min of electromagnetic agitation obtains A liquid.
(2) 2mmol potassium chloride is weighed, 2mmol sodium oxalates add 10ml distilled water and obtain B liquid.
(3) B liquid is added dropwise in A liquid, adds 0.1gCTAB, stirred 30~60min, obtain white suspension C.
(4) measure 15ml C liquid to be put into 25ml reactors, maintain the temperature at 160 DEG C of standing 16h.
(5) by the solid product obtained in reactor distillation water washing 3 times, then with organic solvent washing 3 times, produced
Thing is kept for 60 DEG C, is dried 12h, is obtained a nanometer bismoclite.
Embodiment 2：
(1) the water bismuth nitrates of 1mmol five are weighed, are added in 2ml glacial acetic acid, 15~30min of electromagnetic agitation obtains A liquid.
(2) 2mmol potassium chloride is weighed, 2mmol sodium oxalates add 10ml distilled water and obtain B liquid.
(3) B liquid is added dropwise in A liquid, adds 0.1gPEG, stirred 30~60min, obtain white suspension C.
(4) measure 15ml C liquid to be put into 25ml reactors, maintain the temperature at 160 DEG C of standing 16h.
(5) by the solid product obtained in reactor distillation water washing 3 times, then with organic solvent washing 3 times, produced
Thing is kept for 60 DEG C, is dried 12h, is obtained a nanometer bismoclite.
Embodiment 3：
(1) the water bismuth nitrates of 1mmol five are weighed, are added in 2ml glacial acetic acid, 15~30min of electromagnetic agitation obtains A liquid.
(2) 2mmol potassium chloride is weighed, 2mmol sodium oxalates add 10ml distilled water and obtain B liquid.
(3) B liquid is added dropwise in A liquid, adds 0.1gSDS, stirred 30~60min, obtain white suspension C.
(4) measure 15ml C liquid to be put into 25ml reactors, maintain the temperature at 160 DEG C of standing 16h.
(5) by the solid product obtained in reactor distillation water washing 3 times, then with organic solvent washing 3 times, produced
Thing is kept for 60 DEG C, is dried 12h, is obtained a nanometer bismoclite.
Embodiment 4：
(1) the water bismuth nitrates of 1mmol five are weighed, are added in 2ml glacial acetic acid, 15~30min of electromagnetic agitation obtains A liquid.
(2) 2mmol potassium chloride is weighed, 2mmol sodium oxalates add 10ml distilled water and obtain B liquid.
(3) B liquid is added dropwise in A liquid, adds 0.1gPVP, stirred 30~60min, obtain white suspension C.
(4) measure 15ml C liquid to be put into 25ml reactors, maintain the temperature at 160 DEG C of standing 16h.
(5) by the solid product obtained in reactor distillation water washing 3 times, then with organic solvent washing 3 times, produced
Thing is kept for 60 DEG C, is dried 12h, is obtained a nanometer bismoclite.
Claims (4)
- A kind of 1. preparation method of bismoclite nanometer bouquet, it is characterized in that comprising the following steps：(1) weigh appropriate bismuth salt, add in 2~5ml glacial acetic acid, 15~30min of electromagnetic agitation obtains A liquid.(2) 1~5mmol potassium chloride is weighed, 1~5mmol sodium oxalates add 10~50ml distilled water and obtain B liquid.(3) B liquid is added dropwise in A liquid, adds proper amount of surfactant and stir 30~60min, obtain white suspension C.(4) measure 10~20ml C liquid to be put into 25~50ml reactors, maintain the temperature at 100~200 DEG C of 1~18h of standing.(5) by the solid product obtained in reactor distillation water washing 1~3 time, then with organic solvent washing 1~3 time, obtain Product is kept for 20~60 DEG C, is dried 12~24h, is obtained bismoclite nanometer bouquet.
- 2. the preparation method of bismoclite nanometer bouquet as described in claim 1, it is characterized in that：Described in the step (1) Water-soluble bismuth salt can be five water bismuth nitrates, alkali formula bismuth sulfate, sodium bismuthate.
- 3. the preparation method of bismoclite nanometer bouquet as described in claim 1, it is characterized in that：Described in the step (1) 100~200 DEG C of reaction temperature.
- 4. the preparation method of bismoclite nanometer bouquet as described in claim 1, it is characterised in that described surfactant Species.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108383158A (en) * | 2018-04-04 | 2018-08-10 | 湘潭大学 | A kind of metallic element doping Bi2O3The preparation method and applications of material |
| CN108383159A (en) * | 2018-04-11 | 2018-08-10 | 湘潭大学 | A kind of Bi2O3The preparation method and applications of nanometer sheet material |
| CN108502924A (en) * | 2018-04-04 | 2018-09-07 | 湘潭大学 | A kind of preparation method and applications of metallic element doping BiOF materials |
| CN110776007A (en) * | 2019-11-05 | 2020-02-11 | 北华航天工业学院 | Preparation method of ping-pong chrysanthemum-shaped lithium vanadate material |
| CN111359658A (en) * | 2018-12-26 | 2020-07-03 | 广西大学 | Flower-shaped BiOBr loaded with organically-modified magnetic bentonite and preparation method and application thereof |
| CN113274499A (en) * | 2021-06-25 | 2021-08-20 | 中国药科大学 | Bionic bismuth nanoflower and preparation method and application thereof |
-
2016
- 2016-09-20 CN CN201610835272.2A patent/CN107840365A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 高竹青: "《功能配位化合物及其应用探析》", 30 June 2015 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108383158A (en) * | 2018-04-04 | 2018-08-10 | 湘潭大学 | A kind of metallic element doping Bi2O3The preparation method and applications of material |
| CN108502924A (en) * | 2018-04-04 | 2018-09-07 | 湘潭大学 | A kind of preparation method and applications of metallic element doping BiOF materials |
| CN108383159A (en) * | 2018-04-11 | 2018-08-10 | 湘潭大学 | A kind of Bi2O3The preparation method and applications of nanometer sheet material |
| CN108383159B (en) * | 2018-04-11 | 2020-04-07 | 湘潭大学 | Bi2O3Preparation method and application of nanosheet material |
| CN111359658A (en) * | 2018-12-26 | 2020-07-03 | 广西大学 | Flower-shaped BiOBr loaded with organically-modified magnetic bentonite and preparation method and application thereof |
| CN110776007A (en) * | 2019-11-05 | 2020-02-11 | 北华航天工业学院 | Preparation method of ping-pong chrysanthemum-shaped lithium vanadate material |
| CN110776007B (en) * | 2019-11-05 | 2021-11-19 | 北华航天工业学院 | Preparation method of ping-pong chrysanthemum-shaped lithium vanadate material |
| CN113274499A (en) * | 2021-06-25 | 2021-08-20 | 中国药科大学 | Bionic bismuth nanoflower and preparation method and application thereof |
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Application publication date: 20180327 |