CN101773859A - Preparation method of ionic liquid intercalation vanadic oxide - Google Patents
Preparation method of ionic liquid intercalation vanadic oxide Download PDFInfo
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- CN101773859A CN101773859A CN201010022658A CN201010022658A CN101773859A CN 101773859 A CN101773859 A CN 101773859A CN 201010022658 A CN201010022658 A CN 201010022658A CN 201010022658 A CN201010022658 A CN 201010022658A CN 101773859 A CN101773859 A CN 101773859A
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Abstract
The invention discloses a preparation method of ionic liquid intercalation vanadic oxide, which is characterized in that vanadic oxide (V2O5) is used as intercalation body, 1-(R1) alkyl-3-(R2) alkyl imidazole iodized salt is used as an intercalation object, and the vanadic oxide with the ionic liquid intercalation is obtained through mixing and compounding. Compared with the prior art, the invention has the simple process, greatly improves the performance of the body material, and expands the application range of the body material. In addition, the ionic liquid intercalation vanadic oxide has certain special effect absorption performance on methylene blue dye, has high mechanical strength and good fallibility, and belongs to a good catalyst.
Description
Technical field
The present invention relates to hybrid inorganic-organic synthetic material technical field, specifically a kind of preparation method of ionic liquid intercalation vanadic oxide.
Background technology
The history in existing more than 100 year of the research of intercalation chemistry, the structure of inorganic-organic intercalation compound has good regularity and designability, and the laminated body compound is combined with the intercalation object of difference in functionality, can obtain having the stratified material of property.Compare with the composite of routine, intercalation material has had obvious change on calorifics, mechanics, optics, electricity and magnetic property.Thereby the research of intercalation class lamellar compound not only had learning value on the very important basic theory, and wide practical prospect is arranged.
V
2O
5Be a kind of oxide with layer structure, its laminate is by tetragonal pyramid VO
5Be connected to form by being total to the limit and being total to the angle, the interaction between laminate and the laminate is very weak.V
2O
5This special construction can make many object species be embedded into its interlayer, forms the intercalation product.Up to now, people have successfully synthesized many intercalation composite materials based on vanadic anhydride, and according to inserting the object difference, intercalated compound is divided into ionic intercalation thing, neutral intercalation thing and polymer intercalation material.For example: alkyl viologen/V
2O
5Intercalation compound, C
6H
5CH
2NH
3 +/ V
2O
5, C
8H
17NH
3 +/ V
2O
5Plasma type intercalation thing is with V
2O
5Be main body, by changing the charged situation of interlayer, as reacting driving force, introduce the object ion and the intercalation compound that forms by electrostatic interaction, this synthetic method has solved the traditional difficult problem that the ionic object can not be inserted the electroneutral body layer in synthetic.Synthesized macrocyclic compound (crown ether and cave ether)/V by mechanism such as proton transfer and lattice associations
2O
5, N-propyl sulfonic acid aniline (SPAN)/V
2O
5Etc. neutral intercalation compound, at V
2O
5Thereby introduce neutral molecule in the layer structure and improved its physical property.Synthesized PVC (polyvinyl chloride)/V in addition
2O
5, PPY (polypyrrole)/V
2O
5, PANI (polyaniline)/V
2O
5Etc. the multiple polymers intercalation compound, main body is improved to some extent on performances such as mechanicalness, rheological characteristic, photoelectricity.
V
2O
5Intercalation compound can make full use of advantages such as its specific area is big, the surface energy is high, absorption property is good, mechanical strength is big, pliability is good when keeping original photoelectric properties, make the research of intercalation material become the focus of domestic and international research.
Summary of the invention
The preparation method that a kind of ionic liquid intercalation vanadic oxide of providing at the deficiencies in the prior art is provided, it is with ion liquid insertion, the interlamellar spacing and the specific area of material of main part have been increased, greatly improved the performance of material of main part, widened the range of application of material of main part, and methylene blue dye had certain special efficacy adsorptivity, be a kind of good catalyst.
The concrete technical scheme that realizes the object of the invention is: a kind of preparation method of ionic liquid intercalation vanadic oxide is characterized in that it is with vanadic anhydride (V
2O
5) be the intercalation main body, 1-(R
1) alkyl-3-(R
2) the alkyl imidazole salt compounded of iodine is the intercalation object, through the synthetic vanadic anhydride (V of hydridization with ionic liquid intercalation of following structure
2O
5), concrete preparation may further comprise the steps:
A, with 1-(R
1) alkyl-3-(R
2) alkyl imidazole salt compounded of iodine and vanadic anhydride (V
2O
5), pure water is mix after to put into reactor at 0.01～0.04: 0.01～0.08: 0.3～1.0 in molar ratio, reacts under 80～150 ℃ temperature 6～18 hours, reaction is cooled to room temperature after finishing;
B, the product of above-mentioned reaction used pure water and absolute ethanol washing respectively after, make vanadic anhydride (V with ionic liquid intercalation through 70～90 ℃ vacuum drying
2O
5).
Described ionic liquid 1-(R
1) alkyl-3-(R
2) the alkyl imidazole salt compounded of iodine has following structure:
R wherein
1, R
2Be C
1～C
8Alkyl.
It is simple that the present invention compared with prior art has a synthesis technique, easy to operate, reproducible results is good, ion liquid insertion has increased the interlamellar spacing and the specific area of material of main part, has greatly improved the performance of material of main part, widened the range of application of material of main part, and methylene blue dye had certain special efficacy adsorptivity, the surface can be high, absorption property is good, mechanical strength is big, pliability is good, is a kind of good catalyst.
Description of drawings
Fig. 1 is the infrared spectrogram of ionic liquid intercalation vanadic oxide
Fig. 2 is the XRD spectra of ionic liquid intercalation vanadic oxide
Fig. 3 is ionic liquid intercalation vanadic oxide, active carbon, V
2O
5Adsorption rate curve comparison diagram to methylene blue
Fig. 4 is the adsorption rate curve comparison diagram of ionic liquid intercalation vanadic oxide to methylene blue, methyl orange, rhodamine B
The specific embodiment:
The present invention is described in further detail by following specific embodiment.
Embodiment 1
Get 0.01 mole 1,3-methylimidazole metal iodide ions liquid, 0.9 mole of water and 0.06 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 80 ℃ of temperature, react 18h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 75 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
Get 0.01 mole 1,3-methylimidazole metal iodide ions liquid, 0.6 mole of water and 0.02 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 120 ℃ of temperature, react 12h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 80 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
Embodiment 3
Get 0.01 mole 1,3-methylimidazole metal iodide ions liquid, 0.3 mole of water and 0.02 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 150 ℃ of temperature, react 6h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 82 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
Embodiment 4
Get 0.04 mole 1,3-methylimidazole metal iodide ions liquid, 0.8 mole of water and 0.02 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 150 ℃ of temperature, react 18h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 85 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
Among the foregoing description 1～embodiment 41, the structure of 3-methylimidazole salt compounded of iodine is as follows:
Embodiment 5
Get 0.01 mole of 1-methyl-3-butyl imidazole metal iodide ions liquid, 0.6 mole of water and 0.02 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 120 ℃ of temperature, react 8h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 88 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
Embodiment 6
Get 0.02 mole of 1-methyl-3-butyl imidazole metal iodide ions liquid, 0.9 mole of water and 0.06 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 150 ℃ of temperature, react 18h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 80 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
Embodiment 7
Get 0.01 mole of 1-methyl-3-butyl imidazole metal iodide ions liquid, 0.6 mole of water and 0.02 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 80 ℃ of temperature, react 18h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 82 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
Embodiment 8
Get 0.01 mole of 1-methyl-3-butyl imidazole metal iodide ions liquid, 0.3 mole of water and 0.02 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 150 ℃ of temperature, react 6h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 85 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
Embodiment 9
Get 0.02 mole of 1-methyl-3-butyl imidazole metal iodide ions liquid, 0.9 mole of water and 0.06 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 100 ℃ of temperature, react 12h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 86 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
The structure of the 1-methyl among the foregoing description 5～embodiment 9-3-butyl imidazole salt compounded of iodine is as follows:
Get 0.01 mole of 1-butyl-3-octyl group iodonium imidazolide salts ionic liquid, 0.6 mole of water and 0.02 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 120 ℃ of temperature, react 8h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 78 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material
Embodiment 11
Get 0.01 mole of 1-butyl-3-octyl group iodonium imidazolide salts ionic liquid, 0.9 mole of water and 0.06 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 80 ℃ of temperature, react 18h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 80 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
Embodiment 12
Get 0.01 mole of 1-butyl-3-octyl group iodonium imidazolide salts ionic liquid, 0.3 mole of water and 0.01 mole of V
2O
5, after in beaker, stirring, changing in the polytetrafluoroethylene (PTFE) reactor and under 150 ℃ of temperature, react 12h, reaction is cooled to room temperature after finishing, and product is used pure water and absolute ethanol washing respectively for several times, then through 90 ℃ of vacuum drying, obtains the V of ionic liquid intercalation
2O
5Material.
The structure of the 1-butyl among the foregoing description 10～embodiment 12-3-octyl group iodonium imidazolide salts is as follows:
Consult accompanying drawing 1～accompanying drawing 2, to the various embodiments described above products therefrom carry out infrared spectrum, XRD composes detection, can confirm that ionic liquid well has been inserted into vanadic anhydride (V
2O
5) interlayer, in intercalation compound, exist stronger host-guest and interact, greatly improved the performance of vanadic anhydride, widened the range of application of its material, be a kind of good catalyst.
Consult accompanying drawing 3, to the various embodiments described above products therefrom respectively with active carbon, V
2O
5Adsorption rate to methylene blue compares, as can be seen through the vanadic anhydride (V of ionic liquid intercalation
2O
5) methylene blue dye is had certain special efficacy adsorptivity.
Consult accompanying drawing 4, the adsorption rate of the various embodiments described above products therefrom to methylene blue, methyl orange and rhodamine B compared, also as can be seen through the vanadic anhydride (V of ionic liquid intercalation
2O
5) methylene blue dye is had certain special efficacy adsorptivity,
More than each embodiment just the present invention will be further described, be not in order to restriction patent of the present invention, allly implement for the present invention's equivalence, all should be contained within the claim scope of patent of the present invention.
Claims (2)
1. the preparation method of an ionic liquid intercalation vanadic oxide is characterized in that with vanadic anhydride (V
2O
5) be the intercalation main body, 1-(R
1) alkyl-3-(R
2) the alkyl imidazole salt compounded of iodine is the intercalation object, through the synthetic vanadic anhydride (V of hydridization with ionic liquid intercalation of following structural formula
2O
5), concrete preparation may further comprise the steps:
A, with 1-(R
1) alkyl-3-(R
2) alkyl imidazole salt compounded of iodine and vanadic anhydride (V
2O
5), pure water is mix after to put into reactor at 0.01～0.04: 0.01～0.08: 0.3～1.0 in molar ratio, reacts under 80～150 ℃ temperature 6～18 hours, reaction is cooled to room temperature after finishing;
B, the product of above-mentioned reaction used pure water and absolute ethanol washing respectively after, make vanadic anhydride (V with ionic liquid intercalation through 70～90 ℃ vacuum drying
2O
5).
2. according to the preparation method of the described ionic liquid intercalation vanadic oxide of claim 1, it is characterized in that described 1-(R
1) alkyl-3-(R
2) structure of alkyl imidazole salt compounded of iodine is as follows:
R wherein
1, R
2Be C
1～C
8Alkyl.
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| WO2017035879A1 (en) * | 2015-09-01 | 2017-03-09 | 南方科技大学 | Method for preparing single-layer metal phosphate and applications thereof |
| CN108236921A (en) * | 2018-01-19 | 2018-07-03 | 杭州电子科技大学 | Ion liquid functionalization carbon nanomaterial with absorption property and preparation method thereof |
| CN108899534A (en) * | 2018-06-19 | 2018-11-27 | 清华大学 | A kind of preparation method of lithium ion battery capacitor positive electrode vanadium oxide |
| CN111204728A (en) * | 2020-03-10 | 2020-05-29 | 郑州中科新兴产业技术研究院 | Preparation method of ultrathin two-dimensional vanadium phosphorus oxygen composite metal oxide nanosheet |
| CN112993217A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Preparation method of organic-inorganic hybrid material based on vanadium pentoxide and application of organic-inorganic hybrid material in zinc ion battery |
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2010
- 2010-01-12 CN CN2010100226584A patent/CN101773859B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017035879A1 (en) * | 2015-09-01 | 2017-03-09 | 南方科技大学 | Method for preparing single-layer metal phosphate and applications thereof |
| CN108236921A (en) * | 2018-01-19 | 2018-07-03 | 杭州电子科技大学 | Ion liquid functionalization carbon nanomaterial with absorption property and preparation method thereof |
| CN108236921B (en) * | 2018-01-19 | 2021-06-01 | 杭州电子科技大学 | Ionic liquid functionalized carbon nano material with adsorption performance and preparation method thereof |
| CN108899534A (en) * | 2018-06-19 | 2018-11-27 | 清华大学 | A kind of preparation method of lithium ion battery capacitor positive electrode vanadium oxide |
| CN112993217A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Preparation method of organic-inorganic hybrid material based on vanadium pentoxide and application of organic-inorganic hybrid material in zinc ion battery |
| CN111204728A (en) * | 2020-03-10 | 2020-05-29 | 郑州中科新兴产业技术研究院 | Preparation method of ultrathin two-dimensional vanadium phosphorus oxygen composite metal oxide nanosheet |
| CN111204728B (en) * | 2020-03-10 | 2021-09-24 | 辽宁盛泽精细化工科技有限公司 | Preparation method of ultrathin two-dimensional vanadium phosphorus oxygen composite metal oxide nanosheet |
| CN115259222A (en) * | 2022-06-14 | 2022-11-01 | 苏州科技大学 | Intercalation vanadate composite nano material and preparation method and application thereof |
| CN115259222B (en) * | 2022-06-14 | 2023-11-14 | 苏州科技大学 | Intercalation vanadate composite nano material and preparation method and application thereof |
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