CN102417206A - Preparation method of NaV2O5 crystal material with right angle morphology - Google Patents

Preparation method of NaV2O5 crystal material with right angle morphology Download PDF

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CN102417206A
CN102417206A CN2011102521993A CN201110252199A CN102417206A CN 102417206 A CN102417206 A CN 102417206A CN 2011102521993 A CN2011102521993 A CN 2011102521993A CN 201110252199 A CN201110252199 A CN 201110252199A CN 102417206 A CN102417206 A CN 102417206A
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right angle
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acid
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CN102417206B (en
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任铁真
范洪杰
郑冉
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Hebei University of Technology
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Abstract

The invention relates to a preparation method of a NaV2O5 crystal material with right angle morphology. The method comprises the following steps: a), dissolving an aromatic acid organic matter in water, adding a sodium hydroxide solution under the condition of stirring at room temperature, adding a solvent, and stirring for 40-60 minutes at room temperature so as to obtain an evenly mixed solution; b), adding ammonium metavanadate in the mixture so as to obtain a yellow and transparent mixed liquid, transferring the mixture into a stainless steel reaction kettle with a polytetrafluoroethylene lining after stirring for 3 hours, and then placing the reaction kettle in a constant-temperature drying oven of 150-200 DEG C to age for 2-60 days; and c), taking out and filtering the mixture finally obtained in the step b), drying the mixture in the constant-temperature drying oven of 40-60 DEG C so as to finally obtain the NaV2O5 crystal material with a right angle L shape. In the preparation method provided by the invention, ammonium metavanadate is adopted as a reactant, an alkaline solvent system of the organic matter in water/absolute ethyl alcohol is used, thus the preparation method is environment-friendly, has simple preparation process and utilizes simple equipment, and the obtained NaV2O5 crystal material with L shape can be used for research on nano optical devices.

Description

A kind of right angle pattern NaV 2O 5The preparation method of crystalline material
Technical field
The present invention relates to a kind of right angle pattern NaV 2O 5The preparation method of crystalline material belongs to field of inorganic material preparing technology.
Background technology
There is various ways in inorganic, metal oxide at occurring in nature, and chemist hopes to obtain having the compound of different-shape, so that expand its Application Areas synthetic various when having difform inorganic oxide always.
In the material of report, be that main its pattern of inorganic materials has variety most at present with zinc oxide.Most synthetic materials can be found similar pattern at occurring in nature, like nanotube, nanometer flower, nano wire or the like.Have report to describe the iron oxide nano material of a kind of V of having font and Y font recently, this material is that the dehydration through ferrous hydroxide obtains.About 108 ° of its V font angle (CrystEngComm, 2010,12,1842-1849).But right angle pattern transition metal oxide material is not also reported.
The object of the invention is to provide a kind of making about NaV 2O 5MOX right angle pattern crystalline material method.Although at present to some report of crystal of this type material,, its crystal grain is little and how to exist with the nanometer rod form.We adopt a kind of simple solvent thermal synthetic route, and preparation has the NaV of right angle L type pattern in certain density alkaline solution 2O 5Crystalline material.
Summary of the invention
The object of the present invention is to provide a kind of metal oxide materials and preparation method thereof, can remedy the deficiency of existing crystal morphology with right angle crystal morphology.Synthesis device of the present invention is simple, and is easy to operate, and condition is loose, the energy is saved in less contamination, and raw material is simple and easy to, and is with low cost, and output is big, and crystalline size is controlled.
In order to achieve the above object, the present invention adopts ammonium meta-vanadate under the certain basic soln condition of organism at water/absolute ethyl alcohol, to prepare.Ammonium meta-vanadate/organic mixed solution is aging at a certain temperature, prepares the NaV with right angle crystal morphology 2O 5Experimental technique obtains to have the right angle NaV of different size through regulating alkali and organic ratio and digestion time 2O 5
Technical scheme of the present invention is:
A kind of right angle pattern NaV 2O 5The preparation method of crystalline material may further comprise the steps:
A), the aromatic acid organism is water-soluble, and every mole of aromatic acid adds the 2-6 kg water, under stirring at normal temperature, adds sodium hydroxide solution, adds solvent again, and stirring at normal temperature 40～60 minutes gets a uniform mixture;
Its material proportion is a mol ratio aromatic acid organism: sodium hydroxide=1: 3.5, and every mole of aromatic acid organism adds 2.5～5 kilograms of solvents;
B), in mixture, add ammonium meta-vanadate, obtain the yellow transparent mixed solution, stir after three hours, mixture is changed over to have in the teflon-lined stainless steel cauldron, put into 150-200 ℃ aging 2-60 days of thermostatic drying chamber;
The organic mol ratio of described ammonium meta-vanadate and aromatic acid is an ammonium meta-vanadate: aromatic acid organism=1～4: 1.
C), mixture takes out and filters, and 40-60 ℃ of thermostatic drying chamber inner drying obtains L type right angle NaV at last 2O 5Crystalline material.
Described aromatic acid organism is specially terephthalic acid, phthalic acid, trimesic acid, Pyromellitic Acid or their acid anhydrides.
The concentration of described sodium hydroxide solution is 2mol/l.
Described solvent is water, absolute ethyl alcohol or ethanolic soln.
Quality when described solvent is ethanolic soln is than water: ethanol=1: 1.
The synthetic black crystals that obtains is NaV 2O 5Material can obtain different big or small L shaped right angle NaV under different experimental conditions 2O 5Crystalline material.
Beneficial effect of the present invention is:
1. adopting ammonium meta-vanadate is reactant, uses the basic solvent system of organism at water/absolute ethyl alcohol, environmentally friendly.
2. can pass through to regulate differential responses thing/organism ratio and the consumption that changes reaction solvent water, and the crystal growth time obtains to have the NaV of difference size 2O 5Crystalline material.
3. temperature of reaction kettle is lower, can be controlled between 150-200 ℃.
4. preparation technology and equipment are simple, controlled NaV 2O 5The L shaped shape of crystalline material.
NaV 2O 5Crystal has optical property, the L shaped NaV that the present invention relates to 2O 5Crystal can be used for the research of nanocomposite optical device.
Description of drawings:
The x-ray diffraction pattern of the product that Fig. 1 obtains for the embodiment of the invention 1;
The low transmission microscopy picture of differentiating of (a) right angle crystalline of Fig. 2 embodiment of the invention 1 product, (b) be the diffraction picture of right angle crystal both direction (c), (d) be the diffraction picture at crystal twin crystal boundary place, right angle.
Fig. 3 is the embodiment of the invention 1 a product right angle crystalline ESEM picture.
Fig. 4 is the right angle crystalline opticmicroscope picture of the embodiment of the invention 2 products.
Fig. 5 is the right angle crystalline opticmicroscope picture of the embodiment of the invention 3 products.
Embodiment
Embodiment 1: 0.210g (0.001mol) organism trimesic acid is dissolved in 5g (0.28mol) water; Normal temperature stirs down and adds 1.75ml NaOH solution (concentration is 2mol/l) after 5 minutes; Normal temperature continued stir about 15 minutes down; Add the solvent of forming by 2.5g water (0.14mol) and 2.5g (0.055mol) absolute ethyl alcohol then, obtain water white solution, at last to mixed solution and dripping 0.2339g (0.002mol) NH 4VO 3, the solution of this moment is that milk yellow is muddy, stirs after 40 minutes, and recording mixture pH is 7.5-8.0, and (mol ratio of mixture is NH 4VO 3: trimesic acid: NaOH=2: 1: 3.5; The quality of every mole of corresponding solvent of trimesic acid is 5 kilograms, water in the solvent: alcoholic acid mass ratio=1.Mixture changed over to have in the teflon-lined stainless steel cauldron, put into 180 ℃ aging two days of thermostatic drying chamber, take out mixture two days later and filter, 60 ℃ of thermostatic drying chamber inner dryings obtain L N-type waferN material at last.Fig. 1 XRD show sample is NaV 2O 5(JCPDS#70-08770, P2 1Mn (31), a=1.132nm, b=0.360nm, c=0.480nm).Crystalline diffraction such as Fig. 2; Fig. 2 a shows between the crystalline right angle area to exist with 90 ° of angle forms for the low transmission microscopy photo of differentiating, carries out selected diffraction (Fig. 2 b at two square edges respectively; C) show; Two square edges are single crystal structure, and the square edge infall is carried out selected diffraction (Fig. 2 d), can see the twin diffraction structure that diffracting spectrum exists with two square edge stacked systems.Crystal morphology such as ESEM Fig. 3, sample mainly exist with L type appearance, and the length of two square edges in edge reaches about about 500um.
Embodiment 2: 0.210g (0.001mol) organism trimesic acid is dissolved in 5g (0.28mol) water; Normal temperature stirs down and adds 1.75ml NaOH solution (2mol/l) after 5 minutes; Normal temperature continued stir about 15 minutes down; Add the solvent of forming by 2.5g (0.14mol) water and 2.5g (0.055mol) absolute ethyl alcohol then, obtain water white solution, at last to mixed solution and dripping 0.117g (0.001mol) NH 4VO 3, the solution of this moment is that milk yellow is muddy, stirs after 60 minutes, and the pH of survey is 7.5-8.0, and (mol ratio of mixture is NH 4VO 3: trimesic acid: NaOH=1: 1: 3.5; The quality of every mole of corresponding solvent of trimesic acid is 10 kilograms, water in the solvent: alcoholic acid mass ratio=1.Mixture changed over to have in the teflon-lined stainless steel cauldron; Put into 180 ℃ thermostatic drying chamber internal reaction one month, take out sample then and filter 40 ℃ of thermostatic drying chamber inner dryings; Obtain rectangular-shaped monocrystalline at last; Opticmicroscope picture (Fig. 4) shows that two square edges exist with 90 ° of angle forms, and the length of two square edges in edge reaches about 500um, the about 50um of width.
Embodiment 3: 0.210g (0.001mol) organism trimesic acid is dissolved in 2.5g (0.14mol) water; Normal temperature stirs down and adds 1.75ml NaOH solution (2mol/l) after 5 minutes; Normal temperature continued stir about 15 minutes down; Add the solvent of forming by 2.5g (0.055mol) ethanol solution then, obtain water white solution, in mixing solutions, add 0.4679g (0.004mol) NH at last 4VO 3, obtain the muddy liquid of xanchromatic, stirring and recording pH after 40 minutes is 7.0-7.2, the mol ratio of mixture is NH 4VO 3: trimesic acid: NaOH=4: 1: 3.5; The quality of every mole of corresponding solvent of trimesic acid does 2.5 KilogramMixture changed over to have in the teflon-lined stainless steel cauldron, put into 180 ℃ thermostatic drying chamber internal reaction 7 days, take out sample then and filter, 40 ℃ of thermostatic drying chamber inner dryings obtain rectangular-shaped monocrystalline at last.Opticmicroscope picture (Fig. 5) shows that two square edges exist with 90 ° of angle forms, and the length of two square edges in edge reaches about about 50um.
Embodiment 4: other experimental procedure only changes aging temperature with embodiment 1, and reaction mixture is put into 160 ℃ thermostatic drying chamber internal reaction 15 days, obtains right angle NaV 2O 5Crystal grain.
Embodiment 5: other experimental procedure is with embodiment 1, and only changing the organism trimesic acid is the organism phthalic acid, and the mol ratio 2 of ammonium meta-vanadate and phthalic acid obtains right angle NaV 2O 5Crystal grain.
Embodiment 6: other experimental procedure is with embodiment 1, and only changing the organism trimesic acid is the organism pyromellitic dianhydride, and the mol ratio 2 of ammonium meta-vanadate and pyromellitic dianhydride obtains right angle NaV 2O 5Crystal grain.
Embodiment 7: other experimental procedure is with embodiment 2, and only changing the organism trimesic acid is the organism phthalic acid, and the mol ratio 1 of ammonium meta-vanadate and organism phthalic acid obtains right angle NaV 2O 5Crystal grain.
Embodiment 8: other experimental procedure is with embodiment 3, and only changing the organism trimesic acid is pyromellitic dianhydride, the mol ratio 4 of ammonium meta-vanadate and pyromellitic dianhydride, the right angle NaV that obtains 2O 5Crystal grain.
Can find out that from top embodiment the present invention uses the organism trimesic acid, the mol ratio of ammonium meta-vanadate and trimesic acid is that 1 o'clock right angle sample throughput is the highest.Except that right angle pattern crystal, also have other pattern particle simultaneously when using phthalic acid, trimesic acid, Pyromellitic Acid or acid anhydrides, product purity reduces.Temperature of reaction can be carried out at 150～200 ℃ among the present invention, and is best with the sample topography that 180 ℃ of reactions obtain.Compare right angle pattern NaV with current techniques 2O 5The crystalline preparation temperature is lower, and right angle crystal yardstick is controlled, and product purity is high.

Claims (5)

1. right angle pattern NaV 2O 5The preparation method of crystalline material is characterized by and may further comprise the steps:
A), the aromatic acid organism is water-soluble, and every mole of aromatic acid adds the 2-6 kg water, under stirring at normal temperature, adds sodium hydroxide solution, adds solvent again, and stirring at normal temperature 40～60 minutes gets a uniform mixture;
Its material proportion is a mol ratio aromatic acid organism: sodium hydroxide=1: 3.5, and every mole of aromatic acid organism adds 2.5～5 kilograms of solvents;
B), in mixture, add ammonium meta-vanadate, obtain the yellow transparent mixed solution, stir after three hours, mixture is changed over to have in the teflon-lined stainless steel cauldron, put into 150-200 ℃ aging 2-60 days of thermostatic drying chamber;
The organic mol ratio of described ammonium meta-vanadate and aromatic acid is an ammonium meta-vanadate: aromatic acid organism=1～4: 1;
C), mixture takes out and filters, and 40-60 ℃ of thermostatic drying chamber inner drying obtains right angle L type NaV at last 2O 5Crystalline material.
2. right angle pattern NaV as claimed in claim 1 2O 5The preparation method of crystalline material is characterized by described aromatic acid organism and is specially terephthalic acid, phthalic acid, trimesic acid, Pyromellitic Acid or their acid anhydrides.
3. right angle pattern NaV as claimed in claim 1 2O 5The preparation method of crystalline material, the concentration that it is characterized by described sodium hydroxide solution is 2mol/l.
4. right angle pattern NaV as claimed in claim 1 2O 5The preparation method of crystalline material, it is characterized by described solvent is water, absolute ethyl alcohol or ethanolic soln.
5. right angle pattern NaV as claimed in claim 4 2O 5The preparation method of crystalline material, the quality when it is characterized by described solvent and being ethanolic soln are than water: ethanol=1: 1.
CN 201110252199 2011-08-30 2011-08-30 Preparation method of NaV2O5 crystal material with right angle morphology Expired - Fee Related CN102417206B (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
RU2549421C2 (en) * 2013-09-03 2015-04-27 Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук Method of obtaining nanoneedles of sodium vanadium oxide bronze
CN106335924A (en) * 2016-08-12 2017-01-18 武汉理工大学 Preparation method of NaV2O5
CN108163891A (en) * 2018-02-06 2018-06-15 陕西科技大学 A kind of three-dimensional self assembly NaV2O5Nano-powder and preparation method and application
CN108423711A (en) * 2018-02-06 2018-08-21 陕西科技大学 A kind of tetragonal phase NaV2O5·H2O nano-sheet powders and its preparation method and application
CN110643973A (en) * 2019-11-13 2020-01-03 西安近代化学研究所 NaV2O5Preparation method of crystal film

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2549421C2 (en) * 2013-09-03 2015-04-27 Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук Method of obtaining nanoneedles of sodium vanadium oxide bronze
CN106335924A (en) * 2016-08-12 2017-01-18 武汉理工大学 Preparation method of NaV2O5
CN108163891A (en) * 2018-02-06 2018-06-15 陕西科技大学 A kind of three-dimensional self assembly NaV2O5Nano-powder and preparation method and application
CN108423711A (en) * 2018-02-06 2018-08-21 陕西科技大学 A kind of tetragonal phase NaV2O5·H2O nano-sheet powders and its preparation method and application
CN110643973A (en) * 2019-11-13 2020-01-03 西安近代化学研究所 NaV2O5Preparation method of crystal film
CN110643973B (en) * 2019-11-13 2021-11-23 西安近代化学研究所 NaV2O5Preparation method of crystal film

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