CN107601564A - A kind of method of alcoholic solvent hot preparation niobic acid tin nanosphere - Google Patents
A kind of method of alcoholic solvent hot preparation niobic acid tin nanosphere Download PDFInfo
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- CN107601564A CN107601564A CN201710787301.7A CN201710787301A CN107601564A CN 107601564 A CN107601564 A CN 107601564A CN 201710787301 A CN201710787301 A CN 201710787301A CN 107601564 A CN107601564 A CN 107601564A
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- Prior art keywords
- nanosphere
- snnb
- organic alcohols
- deionized water
- sncl
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- 239000002077 nanosphere Substances 0.000 title claims abstract description 26
- 239000002904 solvent Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 17
- 230000001476 alcoholic effect Effects 0.000 title claims abstract description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 239000002253 acid Substances 0.000 title claims abstract description 7
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 30
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 30
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 30
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 20
- 150000001298 alcohols Chemical class 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims abstract description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 11
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 9
- 235000011150 stannous chloride Nutrition 0.000 claims description 9
- 239000001119 stannous chloride Substances 0.000 claims description 9
- 239000010955 niobium Substances 0.000 claims description 4
- 239000003643 water by type Substances 0.000 claims description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 abstract description 6
- 235000011187 glycerol Nutrition 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 239000008204 material by function Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
A kind of method of alcoholic solvent hot preparation niobic acid tin nanosphere, belongs to field of functional materials.Utilize SnCl2·2H2O and niobium pentaoxide (Nb2O5) powder mixing, it is tuned into starchiness, then organic alcohols (such as ethanol, isopropanol, ethylene glycol, glycerine etc.) and surfactant polyvinylpyrrolidone (PVP) are added, the metastable SnNb of thermodynamics can be made in alcohol heat treatment said mixture2O6Nanometer ball material.The SnNb of gained2O6Nanosphere has preferable application prospect in photocatalysis field.
Description
Technical field
The present invention relates to a kind of alcoholic solvent thermal synthesis niobic acid tin (SnNb2O6) nanosphere method, belong to functional material neck
Domain.
Technical background
Currently, it is particularly urgent for sewage disposal to find the new photochemical catalyst using visible ray.SnNb2O6Nanometer
Material has huge application potential in fields such as air-sensitive, catalysis, optics and power storages.But due to niobium oxide often table
Chemical inertness is revealed, property is relatively stable, therefore is unfavorable for carrying out the synthesis of niobates nano material as reaction raw materials.Compare
For, chemical synthesis in liquid phase technique easily carries out aoxidizing activation and the crystalline growth of niobates nano material of niobium raw material, special
It is not the glamour that solvent-thermal method has illustrated uniqueness in terms of the synthesis of niobates micro-structural.At present synthesis pattern it is homogeneous,
The SnNb of good dispersion2O6Nanosphere is rarely reported.By a kind of reaction environment of alcohol heat, oxygen in high temperature and high pressure environment is controlled
Change the dissolving of niobium, while using protective effect of the surfactant to crystal face, can be made in metastable SnNb2O6Nanometer
Ball powder, due to the SnNb compared to thermodynamics stable state2O7For, its oxygen content is reduced, therefore causes lattice distortion and oxygen sky
Position is increased, so that the separation of the photo-generated carrier more conducively under photocatalysis, so as to improve catalytic efficiency.Pass through such a method
The SnNb of synthesis2O6Nanosphere pattern is homogeneous, good dispersion, can be stabilized at room temperature, is led in photoelectricity, catalysis, energy storage etc.
There is preferable application prospect in domain.
The content of the invention
It is an object of the invention to provide a kind of alcoholic solvent thermal synthesis niobic acid tin (SnNb2O6) nanosphere method, beneficial to batch
Preparing has the SnNb of wide application prospect in water treatment field and catalytic field2O6Nanometer ball material, can substantially reduce cost,
Efficiency is improved, practical significance is great, and promotes the development of metastable state niobates method for crystallising, promotes the practical application of niobates to grind
Study carefully.
The purpose of the present invention is achieved by the following technical programs：
A kind of alcoholic solvent thermal synthesis niobic acid tin SnNb provided by the invention2O6The method of nanosphere, it is characterised in that including
Following steps：
(1) deionized water dissolving stannous chloride (SnCl is used first2·2H2O), and with niobium pentaoxide (Nb2O5) powder mixes
Close, be tuned into starchiness, then add organic alcohols solvent (such as ethanol, isopropanol, ethylene glycol, glycerine etc.) and surface-active
Agent polyvinylpyrrolidone (PVP)；
(2) solution obtained using step (1) is pre-reaction material, is heat-treated in closed reactor, temperature 160-
200 DEG C, processing time is 24-48 hours, and SnNb is successfully made2O6Nanosphere；
Wherein SnCl2·2H2O：Nb2O5：PVP mass ratio is (0.4-0.5):(0.2-0.4):(0.08-0.1)；Go from
The volume ratio of sub- water and organic alcohols solvent is (2-4):(8-6), and deionized water and organic alcohols total solvent volume amount are 10,
Niobium pentaoxide is per 0.2-0.4g Nb with magnitude relation with organic alcohols solvent2O5Corresponding 2-4ml deionized waters.
Wherein organic alcohols preferred alcohol.
Wherein preferably 180 DEG C of heat treatment temperature, processing time are 36 hours.
The present invention is with SnCl2·2H2O, organic alcohols, PVP are raw material, being capable of controllable preparation through alcoholic solvent heat treatment
SnNb2O6Nanosphere, this method confirm, by alcoholic solvent thermal process progress chemical regulation, to obtain metastable state niobates in the solution
Operability.
The beneficial effects of the invention are as follows：Product favorable repeatability obtained by the preparation method of the present invention, simple to operate, cost
It is low.The SnNb of gained2O6Nanosphere has preferable application prospect in photocatalysis field.
Brief description of the drawings
Fig. 1：The SnNb that embodiment 1 obtains2O6The X-ray diffractogram of nanosphere；
Fig. 2：The SnNb that embodiment 1 obtains2O6The scanning electron microscope (SEM) photograph of nanosphere；
Fig. 3：The SnNb that embodiment 1 obtains2O6The elementary analysis figure of nanosphere；
Fig. 4：The SnNb that embodiment 1 obtains2O6The TEM figures of nanosphere.
Embodiment
With reference to embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
(1) deionized water dissolving stannous chloride (SnCl is used first2·2H2O), and with niobium pentaoxide (Nb2O5) powder mixes
Close, be tuned into starchiness, then add organic alcohols (ethanol) and surfactant polyvinylpyrrolidone (PVP)；
(2) solution obtained using step (1) is pre-reaction material, in the closed reactor that volume is 20mL at heat
Reason, temperature are 160 DEG C, and processing time is 48 hours, and SnNb is successfully made2O6Nanosphere；
Wherein SnCl2·2H2O、Nb2O5, PVP dosage be respectively 0.4g, 0.4g, 0.1g；The dosage of deionized water and alcohol
Respectively 2mL, 8mL.
Embodiment 2
(1) deionized water dissolving stannous chloride (SnCl is used first2·2H2O), and with niobium pentaoxide (Nb2O5) powder mixes
Close, be tuned into starchiness, then add organic alcohols (ethanol) and surfactant polyvinylpyrrolidone (PVP)；
(2) solution obtained using step (1) is pre-reaction material, in the closed reactor that volume is 20mL at heat
Reason, temperature are 180 DEG C, and processing time is 48 hours, and SnNb is successfully made2O6Nanosphere；
Wherein SnCl2·2H2O、Nb2O5, PVP dosage be respectively 0.5g, 0.3g, 0.1g；The dosage of deionized water and alcohol
Respectively 2mL, 8mL.
Embodiment 3
(1) deionized water dissolving stannous chloride (SnCl is used first2·2H2O), and with niobium pentaoxide (Nb2O5) powder mixes
Close, be tuned into starchiness, then add organic alcohols (ethanol) and surfactant polyvinylpyrrolidone (PVP)；
(2) solution obtained using step (1) is pre-reaction material, in the closed reactor that volume is 20mL at heat
Reason, temperature are 180 DEG C, and processing time is 48 hours, and SnNb is successfully made2O6Nanosphere；
Wherein SnCl2·2H2O、Nb2O5, PVP dosage be respectively 0.4g, 0.2g, 0.08g；The use of deionized water and alcohol
Amount is respectively 2mL, 8mL.
Embodiment 4
(1) deionized water dissolving stannous chloride (SnCl is used first2·2H2O), and with niobium pentaoxide (Nb2O5) powder mixes
Close, be tuned into starchiness, then add organic alcohols (ethanol) and surfactant polyvinylpyrrolidone (PVP)；
(2) solution obtained using step (1) is pre-reaction material, in the closed reactor that volume is 20mL at heat
Reason, temperature are 180 DEG C, and processing time is 36 hours, and SnNb is successfully made2O6Nanosphere；
Wherein SnCl2·2H2O、Nb2O5, PVP dosage be respectively 0.5g, 0.3g, 0.08g；The use of deionized water and alcohol
Amount is respectively 4mL, 6mL.
Embodiment 5
(1) deionized water dissolving stannous chloride (SnCl is used first2·2H2O), and with niobium pentaoxide (Nb2O5) powder mixes
Close, be tuned into starchiness, then add organic alcohols (ethanol) and surfactant polyvinylpyrrolidone (PVP)；
(2) solution obtained using step (1) is pre-reaction material, in the closed reactor that volume is 20mL at heat
Reason, temperature are 200 DEG C, and processing time is 48 hours, and SnNb is successfully made2O6Nanosphere；
Wherein SnCl2·2H2O、Nb2O5, PVP dosage be respectively 0.5g, 0.4g, 0.1g；The dosage of deionized water and alcohol
Respectively 4mL, 6mL.
Embodiment 6
(1) deionized water dissolving stannous chloride (SnCl is used first2·2H2O), and with niobium pentaoxide (Nb2O5) powder mixes
Close, be tuned into starchiness, then add organic alcohols (ethanol) and surfactant polyvinylpyrrolidone (PVP)；
(2) solution obtained using step (1) is pre-reaction material, in the closed reactor that volume is 20mL at heat
Reason, temperature are 180 DEG C, and processing time is 48 hours, and SnNb is successfully made2O6Nanosphere；
Wherein SnCl2·2H2O、Nb2O5, PVP dosage be respectively 0.5g, 0.3g, 0.1g；The dosage of deionized water and alcohol
Respectively 1mL, 9mL.
Embodiment 7
(1) deionized water dissolving stannous chloride (SnCl is used first2·2H2O), and with niobium pentaoxide (Nb2O5) powder mixes
Close, be tuned into starchiness, then add organic alcohols (ethanol) and surfactant polyvinylpyrrolidone (PVP)；
(2) solution obtained using step (1) is pre-reaction material, in the closed reactor that volume is 20mL at heat
Reason, temperature are 180 DEG C, and processing time is 48 hours, and SnNb is successfully made2O6Nanosphere；
Wherein SnCl2·2H2O、Nb2O5, PVP dosage be respectively 0.3g, 0.2g, 0.09g；The use of deionized water and alcohol
Amount is respectively 3mL, 7mL.
SnNb prepared by the above embodiment of the present invention 2-72O6Substantially it is identical with embodiment, equal completely nanometer chondritics,
Uniform particle sizes.Isopropanol, ethylene glycol, glycerine etc. can be equally used, obtains the nanosphere containing other structures such as a small amount of sheets
Shape structure.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God and any modification made within principle, equivalent substitution and improvement etc., should be included in the scope of the protection.
Claims (5)
- A kind of 1. alcoholic solvent hot preparation niobic acid tin SnNb2O6The method of nanosphere, it is characterised in that comprise the following steps：(1) deionized water dissolving stannous chloride (SnCl is used first2·2H2O), and with niobium pentaoxide (Nb2O5) powder mixing, adjust Into starchiness, organic alcohols solvent and surfactant polyvinylpyrrolidone (PVP) are then added；(2) solution obtained using step (1) is pre-reaction material, is heat-treated in closed reactor, temperature 160-200 DEG C, processing time is 24-48 hours, and SnNb is successfully made2O6Nanosphere.
- 2. according to the method for claim 1, it is characterised in that SnCl2·2H2O：Nb2O5：PVP mass ratio is (0.4-0.5): (0.2-0.4):(0.08-0.1)；Deionized water and the volume ratio of organic alcohols solvent are (2-4):(8-6), and deionized water with Organic alcohols total solvent volume amount is 10, and niobium pentaoxide is per 0.2-0.4g Nb with magnitude relation with organic alcohols solvent2O5 Corresponding 2-4ml deionized waters.
- 3. according to the method for claim 1, it is characterised in that organic alcohols solvent is selected from ethanol, isopropanol, ethylene glycol, and the third three One or more in alcohol.
- 4. according to the method for claim 1, it is characterised in that organic alcohols solvent is ethanol.
- 5. according to the method for claim 1, it is characterised in that heat treatment temperature is 180 DEG C, and processing time is 36 hours.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108435191A (en) * | 2018-04-26 | 2018-08-24 | 济南大学 | A kind of SnNb2O6/ CoFe-LDH piece piece composite magnetic heterojunction structure catalyst and its preparation method and application |
| CN108910948A (en) * | 2018-08-30 | 2018-11-30 | 陕西科技大学 | A kind of niobic acid tin nanometer sheet and preparation method thereof |
| CN109133172A (en) * | 2018-08-30 | 2019-01-04 | 陕西科技大学 | A kind of niobic acid tin nanometer sheet and preparation method thereof and preparing the application in lithium battery |
| CN109231268A (en) * | 2018-08-30 | 2019-01-18 | 陕西科技大学 | A kind of amorphous niobic acid tin and preparation method thereof and preparing the application in lithium battery |
| CN110137493A (en) * | 2019-06-02 | 2019-08-16 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation method and product of a kind of oxygen defect zinc niobate negative electrode material and application |
| CN110624543A (en) * | 2019-10-06 | 2019-12-31 | 湖北工业大学 | PtRu-SnNb2O6Preparation method of two-dimensional composite material |
| CN111348683A (en) * | 2018-12-20 | 2020-06-30 | 中国科学院宁波材料技术与工程研究所 | Method for synthesizing high-crystalline tin niobate by solid phase method |
| CN112808261A (en) * | 2021-02-08 | 2021-05-18 | 长江师范学院 | Preparation method of nest-shaped niobium oxide |
| CN115055177A (en) * | 2022-06-06 | 2022-09-16 | 华中科技大学 | SnTa with oxygen vacancy defect 2 O 6-x Preparation method of nanosheet photocatalyst |
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Cited By (14)
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| CN108435191A (en) * | 2018-04-26 | 2018-08-24 | 济南大学 | A kind of SnNb2O6/ CoFe-LDH piece piece composite magnetic heterojunction structure catalyst and its preparation method and application |
| CN108435191B (en) * | 2018-04-26 | 2023-08-18 | 济南大学 | SnNb (tin-zinc-niobium) alloy 2 O 6 CoFe-LDH (CoFe-LDH) plate composite magnetic heterostructure catalyst and preparation method and application thereof |
| CN108910948A (en) * | 2018-08-30 | 2018-11-30 | 陕西科技大学 | A kind of niobic acid tin nanometer sheet and preparation method thereof |
| CN109133172A (en) * | 2018-08-30 | 2019-01-04 | 陕西科技大学 | A kind of niobic acid tin nanometer sheet and preparation method thereof and preparing the application in lithium battery |
| CN109231268A (en) * | 2018-08-30 | 2019-01-18 | 陕西科技大学 | A kind of amorphous niobic acid tin and preparation method thereof and preparing the application in lithium battery |
| CN109231268B (en) * | 2018-08-30 | 2020-10-20 | 陕西科技大学 | Amorphous tin niobate, preparation method thereof and application thereof in preparation of lithium battery |
| CN111348683A (en) * | 2018-12-20 | 2020-06-30 | 中国科学院宁波材料技术与工程研究所 | Method for synthesizing high-crystalline tin niobate by solid phase method |
| CN111348683B (en) * | 2018-12-20 | 2022-10-28 | 中国科学院宁波材料技术与工程研究所 | Method for synthesizing high-crystalline tin niobate by solid phase method |
| CN110137493A (en) * | 2019-06-02 | 2019-08-16 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation method and product of a kind of oxygen defect zinc niobate negative electrode material and application |
| CN110624543A (en) * | 2019-10-06 | 2019-12-31 | 湖北工业大学 | PtRu-SnNb2O6Preparation method of two-dimensional composite material |
| CN112808261A (en) * | 2021-02-08 | 2021-05-18 | 长江师范学院 | Preparation method of nest-shaped niobium oxide |
| CN112808261B (en) * | 2021-02-08 | 2022-09-02 | 长江师范学院 | Preparation method of nest-shaped niobium oxide |
| CN115055177A (en) * | 2022-06-06 | 2022-09-16 | 华中科技大学 | SnTa with oxygen vacancy defect 2 O 6-x Preparation method of nanosheet photocatalyst |
| CN115055177B (en) * | 2022-06-06 | 2023-02-14 | 华中科技大学 | SnTa with oxygen vacancy defect 2 O 6-x Preparation method of nanosheet photocatalyst |
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