CN109775758A - Preparation method of large-layer-spacing vanadium pentoxide - Google Patents
Preparation method of large-layer-spacing vanadium pentoxide Download PDFInfo
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- CN109775758A CN109775758A CN201811600941.3A CN201811600941A CN109775758A CN 109775758 A CN109775758 A CN 109775758A CN 201811600941 A CN201811600941 A CN 201811600941A CN 109775758 A CN109775758 A CN 109775758A
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- Prior art keywords
- vanadium pentoxide
- vanadic anhydride
- spacing
- layer
- preparation
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000009830 intercalation Methods 0.000 claims abstract description 18
- 230000002687 intercalation Effects 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 8
- 239000010935 stainless steel Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 150000003141 primary amines Chemical class 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 14
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910052720 vanadium Inorganic materials 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 13
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000011229 interlayer Substances 0.000 abstract description 5
- 239000005416 organic matter Substances 0.000 abstract description 3
- 150000003973 alkyl amines Chemical class 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000004729 solvothermal method Methods 0.000 abstract 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 4
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 229910021541 Vanadium(III) oxide Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a preparation method of large-layer-spacing vanadium pentoxide, which comprises the steps of mixing vanadium pentoxide and a primary amine intercalation according to the molar ratio of (1-2): 1, adding absolute ethyl alcohol, uniformly stirring, adding deionized water, continuously stirring, uniformly stirring, transferring the mixture into a polytetrafluoroethylene-lined stainless steel high-pressure reaction kettle, reacting at 160-180 ℃ for 120-168 hours, cooling to room temperature, centrifugally washing an obtained black product with the absolute ethyl alcohol and hexane, drying, and grinding to obtain the large-layer-spacing vanadium pentoxide. According to the invention, the long-chain organic primary alkylamine is intercalated into the vanadium pentoxide layer by a solvothermal method, so that the interlayer spacing of the vanadium pentoxide is enlarged, and the interlayer spacing of the vanadium pentoxide can be adjusted by changing the chain length of the organic matter. The vanadium pentoxide with large layer spacing has excellent physicochemical properties and extremely wide application prospect.
Description
Technical field
The invention belongs to composite organic-inorganic material technical field more particularly to a kind of system of the big layer away from vanadic anhydride
Preparation Method.
Background technique
Barium oxide and its derivative have outstanding adjustability of structure, are widely used in the fields such as catalysis and electrochemistry.
The structure and composition of barium oxide and its composite material is designed and is regulated and controled to change its chemical and physical features and cause
The extensive concern of people.Vanadic anhydride is a kind of typical two-dimensional layer compound, and interlayer can be by guest species intercalation.
One typical example is exactly lithium ion intercalation vanadic oxide, and this property makes vanadic anhydride can be used for lithium-ion electric
Pond electrode material.Therefore, a large amount of work is dedicated to studying the intercalation property of vanadic anhydride, and preparation has excellent physicochemical property
Intercalation vanadic oxide material.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of preparation method of the big layer away from vanadic anhydride, by molten
The organic primary alkylamine intercalation of long-chain is entered vanadic anhydride interlayer by agent thermal method, expands its interlamellar spacing, the interlamellar spacing of vanadic anhydride
It can be adjusted by the change organic matter chain length.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that: a kind of system of the big layer away from vanadic anhydride
Vanadic anhydride and primary amine intercalation object are (1~2) by Preparation Method in molar ratio: 1 mixing, addition absolute ethyl alcohol and stirring is uniform, so
Deionized water is added afterwards to continue to stir, mixture is transferred to polytetrafluoroethyllining lining stainless steel autoclave after mixing evenly
In, at 160~180 DEG C, 120~168h is reacted, after being cooled to room temperature, gained black product dehydrated alcohol and hexane centrifugation
Washing, drying, grinding obtain big layer away from vanadic anhydride.
The primary amine intercalation object is 1- lauryl amine or 1- cetylamine.
The vanadic anhydride molal quantity: dehydrated alcohol volume: deionized water volume is 3mmol:(1~2) ml:(2~3)
ml。
The beneficial effects of the present invention are: long-chain organic intercalation is entered by vanadic anhydride interlayer by solvent thermal reaction,
Big layer has been obtained away from vanadic anhydride material.The material has excellent physicochemical property, can be used for absorption, catalysis, electrochemistry
Equal fields.
Detailed description of the invention
Fig. 1 is X-ray diffractogram of the big layer away from vanadic anhydride prepared by the present invention.
Specific embodiment
In order to preferably illustrate the present invention, the present invention will be described combined with specific embodiments below, described implementation
Example is only a part of implementation column of the invention, is not limit the invention in any way.
Vanadic anhydride and primary amine intercalation object be by preparation method of the big layer away from vanadic anhydride of the invention in molar ratio
(1~2): 1 mixing, addition absolute ethyl alcohol and stirring is uniform, and deionized water is then added and continues to stir, after mixing evenly by mixture
It is transferred in polytetrafluoroethyllining lining stainless steel autoclave, at 160~180 DEG C, reacts 120~168h, be cooled to room
Wen Hou, gained black product dehydrated alcohol and hexane centrifuge washing, drying, grinding obtain big layer away from vanadic anhydride.
The primary amine intercalation object is 1- lauryl amine or 1- cetylamine.
The vanadic anhydride molal quantity: dehydrated alcohol volume: deionized water volume is 3mmol:(1~2) ml:(2~3)
ml。
Preparation method the present invention provides big layer away from vanadic anhydride can obtain long-chain organic intercalation by solvent-thermal method
Vanadic anhydride, interlamellar spacing significantly increases.The interlamellar spacing of vanadic anhydride can be regulated and controled by changing organic matter chain length.
Embodiment 1
2h is mixed in 15mmol vanadic anhydride, 15mmol 1- lauryl amine and 5ml dehydrated alcohol, 15ml is added and goes
Ionized water continues to stir 48h.Mixture is transferred in polytetrafluoroethyllining lining stainless steel autoclave, 180 DEG C of reactions
168h, after being cooled to room temperature, gained black product dehydrated alcohol and hexane centrifuge washing are dried in 60 DEG C of baking oven,
Grinding obtains the vanadic anhydride of lauryl amine intercalation, is product 1.
Embodiment 2
2h is mixed in 15mmol vanadic anhydride, 15mmol 1- cetylamine and 5ml dehydrated alcohol, 15ml is added and goes
Ionized water continues to stir 48h.Mixture is transferred in polytetrafluoroethyllining lining stainless steel autoclave, 180 DEG C of reactions
168h, after being cooled to room temperature, gained black product dehydrated alcohol and hexane centrifuge washing are dried in 60 DEG C of baking oven,
Grinding obtains the vanadic anhydride of cetylamine intercalation, is product 2.
Embodiment 3
2h is mixed in 15mmol vanadic anhydride, 10mmol 1- lauryl amine and 7.5ml dehydrated alcohol, is added
12.5ml deionized water continues to stir 48h.Mixture is transferred in polytetrafluoroethyllining lining stainless steel autoclave, 170
DEG C reaction 144h, after being cooled to room temperature, gained black product dehydrated alcohol and hexane centrifuge washing, in 60 DEG C of baking oven
Drying, grinding obtain the vanadic anhydride of lauryl amine intercalation, are product 3.
Embodiment 4
2h is mixed in 15mmol vanadic anhydride, 7.5mmol 1- lauryl amine and 10ml dehydrated alcohol, 10ml is added
Deionized water continues to stir 48h.Mixture is transferred in polytetrafluoroethyllining lining stainless steel autoclave, 160 DEG C of reactions
120h, after being cooled to room temperature, gained black product dehydrated alcohol and hexane centrifuge washing are dried in 60 DEG C of baking oven,
Grinding obtains the vanadic anhydride of lauryl amine intercalation, is product 4.
X-ray diffraction analysis is carried out to the product of Examples 1 to 4, wherein the X-ray diffractogram of product 1 and product 2 is as schemed
Shown in 1, according to 001 diffraction maximum position, 1 (V of product2O5-C12H25NH2) interlamellar spacing be 2.61nm, 2 (V of product2O5-
C16H33NH2) interlamellar spacing be 2.94nm.The interlamellar spacing that product 3 similarly can be obtained is 2.43nm, and the interlamellar spacing of product 4 is
2.26nm。
Embodiment described above is merely to illustrate technical idea and feature of the invention, in the art its object is to make
Technical staff it will be appreciated that the contents of the present invention and implement accordingly, patent model of the invention only cannot be limited with the present embodiment
It encloses, i.e., same changes or modifications made by all disclosed spirit are still fallen in the scope of the patents of the invention.
Claims (3)
1. a kind of preparation method of the big layer away from vanadic anhydride, which is characterized in that massage vanadic anhydride and primary amine intercalation object
You are than being (1~2): 1 mixing, and addition absolute ethyl alcohol and stirring is uniform, and deionized water is then added and continues to stir, after mixing evenly will
Mixture is transferred in polytetrafluoroethyllining lining stainless steel autoclave, at 160~180 DEG C, 120~168h is reacted, to cold
But to after room temperature, gained black product dehydrated alcohol and hexane centrifuge washing, drying, grinding obtain big layer away from five oxidations two
Vanadium.
2. preparation method of the big layer away from vanadic anhydride according to claim 1, which is characterized in that the primary amine intercalation object is
1- lauryl amine or 1- cetylamine.
3. preparation method of the big layer away from vanadic anhydride according to claim 1, which is characterized in that the vanadic anhydride rubs
That number: dehydrated alcohol volume: deionized water volume is 3mmol:(1~2) ml:(2~3) ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811600941.3A CN109775758A (en) | 2018-12-26 | 2018-12-26 | Preparation method of large-layer-spacing vanadium pentoxide |
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|---|---|---|---|
| CN201811600941.3A CN109775758A (en) | 2018-12-26 | 2018-12-26 | Preparation method of large-layer-spacing vanadium pentoxide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111244463A (en) * | 2020-02-11 | 2020-06-05 | 桂林理工大学 | Preparation method and application of PEG (polyethylene glycol) intercalated double-layer vanadium pentoxide electrode material |
| CN111509225A (en) * | 2020-04-22 | 2020-08-07 | 中南大学 | Preparation method of vanadium-based positive electrode material of zinc ion battery, product and application thereof |
| CN111847510A (en) * | 2020-08-06 | 2020-10-30 | 西南石油大学 | Polyaniline in-situ polymerization intercalation vanadium pentoxide and preparation method and application thereof |
| CN113948689A (en) * | 2021-10-11 | 2022-01-18 | 桂林理工大学 | Preparation method and application of polyaniline modified vanadium-based oxide composite material |
| CN114956173A (en) * | 2022-04-14 | 2022-08-30 | 辽宁大学 | Dodecylamine modified V 2 O 5 Material, preparation method thereof and application of material as super capacitor electrode material |
| CN115259225A (en) * | 2022-04-15 | 2022-11-01 | 齐鲁工业大学 | Preparation method of hollow tubular water system zinc ion battery electrode material |
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| CN1872698A (en) * | 2006-06-14 | 2006-12-06 | 武汉理工大学 | Precursor body of Nano tube of composite oxides of multielement vanadium, and preparation method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111244463A (en) * | 2020-02-11 | 2020-06-05 | 桂林理工大学 | Preparation method and application of PEG (polyethylene glycol) intercalated double-layer vanadium pentoxide electrode material |
| CN111509225A (en) * | 2020-04-22 | 2020-08-07 | 中南大学 | Preparation method of vanadium-based positive electrode material of zinc ion battery, product and application thereof |
| CN111509225B (en) * | 2020-04-22 | 2022-06-07 | 中南大学 | Preparation method of vanadium-based positive electrode material of zinc ion battery, product and application thereof |
| CN111847510A (en) * | 2020-08-06 | 2020-10-30 | 西南石油大学 | Polyaniline in-situ polymerization intercalation vanadium pentoxide and preparation method and application thereof |
| CN113948689A (en) * | 2021-10-11 | 2022-01-18 | 桂林理工大学 | Preparation method and application of polyaniline modified vanadium-based oxide composite material |
| CN114956173A (en) * | 2022-04-14 | 2022-08-30 | 辽宁大学 | Dodecylamine modified V 2 O 5 Material, preparation method thereof and application of material as super capacitor electrode material |
| CN114956173B (en) * | 2022-04-14 | 2023-12-29 | 辽宁大学 | Dodecyl amine modified V 2 O 5 Material, preparation method thereof and application of material as supercapacitor electrode material |
| CN115259225A (en) * | 2022-04-15 | 2022-11-01 | 齐鲁工业大学 | Preparation method of hollow tubular water system zinc ion battery electrode material |
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