CN106745268B - A kind of method that sol-gal process prepares niobium tungstate - Google Patents
A kind of method that sol-gal process prepares niobium tungstate Download PDFInfo
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- CN106745268B CN106745268B CN201611043023.6A CN201611043023A CN106745268B CN 106745268 B CN106745268 B CN 106745268B CN 201611043023 A CN201611043023 A CN 201611043023A CN 106745268 B CN106745268 B CN 106745268B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/006—Compounds containing, besides tungsten, two or more other elements, with the exception of oxygen or hydrogen
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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
Abstract
The method that a kind of sol-gal process of the present invention prepares niobium tungstate belongs to the technical field of inorganic material preparation process.Under hydrothermal conditions by Nb2O5It is dissolved in KOH solution, instills watery hydrochloric acid and obtain Nb (OH)5Precipitation, precipitation is added in hydrogenperoxide steam generator with citric acid, after being mixed again with ammonium metatungstate solution and solution of potassium carbonate, ethylene glycol is added as dispersant, solution ph is adjusted using ammoniacal liquor, solution heating, dehydration obtain gel, and pyrochlore constitution niobium potassium tungstate KNbWO is obtained after high-temperature heat treatment6·H2O.The present invention has the advantages that cost is low, and technique is simple, safety and environmental protection；Compared with conventional method, the particle size of products therefrom is obviously reduced.
Description
Technical field
The invention belongs to the technical field of inorganic material preparation process, and in particular to a kind of sol-gal process prepares niobium wolframic acid
The method of salt.
Background technology
Pyrochlore crystal belongs to cube center of area crystallographic system, due to its unique structure, with heat endurance is good, can carry out ion friendship
Change, be conductive, photocatalysis performance the advantages that.Niobium tungstate belongs to pyrochlore constitution, light of many scientists to niobium tungstate
Catalytic performance and dielectric properties etc. are studied.
At present, most niobium tungstate materials are synthesized using high temperature solid-state method.High temperature solid-state method needs anti-
Multiple high temperature sintering grinding, product are also easy to produce reunion, cause particle size to increase, and specific surface area reduces, and causes the ion of material to be handed over
Change and catalytic performance is limited.Not yet reported on document at present and prepare niobium tungstate KNbWO using sol-gel process6·H2O。
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of method that sol-gal process prepares niobium tungstate.
Specific technical scheme is as follows：
A kind of method that sol-gal process prepares niobium tungstate, uses Nb2O5It is 1 by mass ratio as niobium source：5：60
Nb2O5, KOH, deionized water be placed in reactor, wherein the volume of deionized water is no more than the 80% of reactor capacity, 180
DEG C reaction 48h, obtain [Nb6O19]8-The watery hydrochloric acid that concentration is 1mol/L is added dropwise to [Nb by alkaline solution as presoma6O19
]8-In alkaline solution, there is Nb (OH)5Precipitation, watery hydrochloric acid to the precipitation for continuing to be added dropwise 1mol/L is not further added by, by pelleting centrifugation
Separate, wash, be dried for standby；By obtained Nb (OH)5The hydrogenperoxide steam generator that mass fraction is 30% is added to citric acid
In, every gram of citric acid adds hydrogenperoxide steam generator >=40ml of mass fraction 30%, citric acid and Nb (OH)5Mass ratio >=5；
The amount of material after clarifying according to Nb, W, K is stirred to solution than 1：1：1 adds ammonium metatungstate and potassium carbonate, adds ethylene glycol
As dispersant, improve the stability of colloidal sol, reduce particle aggregation, using 1mol/L weak aqua ammonia adjust the pH=3 of solution~
5；Drying obtains thick colloidal sol at 80~100 DEG C, and further dehydration obtains xerogel；Having in 200~400 DEG C of removal systems
Machine thing, 700 DEG C of calcining more than 5h, pyrochlore constitution niobium potassium tungstate KNbWO is can obtain after cooling6·H2O。
In a kind of sol-gal process of the present invention prepares the method for niobium tungstate, preferably adjusted using 1mol/L weak aqua ammonia
Save the pH=3 of solution.
In a kind of sol-gal process of the present invention prepares the method for niobium tungstate, every gram of Nb (OH)5Precipitation preferably uses
0.2 gram of ethylene glycol is as dispersant.
Wherein, the Nb (OH) 5 of brand-new is amorphous state, dehydration after being calcined at 1000 DEG C, is converted into Nb2O5, passes through thermogravimetric
The data that method analysis (TGA) measures determine Nb content, the foundation as quantitative calculating.
In laboratory, watery hydrochloric acid is added dropwise to [Nb6O19] with the speed of 6-10 drops/minute8-Gone in alkaline solution.
The present invention has the advantages that cost is low, and technique is simple, safety and environmental protection；Using citric acid as complexing agent, with solution
In metal ion formed complex, be advantageous to sol-gel transition, promote target product to be formed；With hydro-thermal method, high temperature solid-state
Method is compared, and the particle size of product is obviously reduced.
Brief description of the drawings
Fig. 1 is niobium potassium tungstate KNbWO made from embodiment 16·H2O x-ray diffraction pattern.
Fig. 2 is niobium potassium tungstate KNbWO made from embodiment 16·H2O stereoscan photograph.
Fig. 3 is niobium potassium tungstate KNbWO made from embodiment 26·H2O x-ray diffraction pattern.
Fig. 4 is niobium potassium tungstate KNbWO made from embodiment 36·H2O x-ray diffraction pattern.
Fig. 5 is niobium potassium tungstate KNbWO made from embodiment 46·H2O x-ray diffraction pattern.
Fig. 6 is niobium potassium tungstate KNbWO made from embodiment 46·H2O stereoscan photograph.
Fig. 7 is niobium potassium tungstate KNbWO made from embodiment 56·H2O x-ray diffraction pattern.
Fig. 8 is niobium potassium tungstate KNbWO made from embodiment 66·H2O x-ray diffraction pattern.
Fig. 9 is niobium potassium tungstate KNbWO made from embodiment 76·H2O x-ray diffraction pattern.
Figure 10 is niobium potassium tungstate KNbWO made from embodiment 86·H2O x-ray diffraction pattern.
Figure 11 is niobium potassium tungstate KNbWO made from embodiment 96·H2O x-ray diffraction pattern.
Figure 12 is niobium potassium tungstate KNbWO made from embodiment 96·H2O stereoscan photograph.
Embodiment
Embodiment 1
By 1.0gNb2O5Added with 5.0gKOH in 60ml deionized waters, load autoclave, 180 DEG C of hydro-thermal process 48
Hour, obtain [Nb6O19]8-Alkaline solution, take supernatant liquor to instill 1mol/L watery hydrochloric acid with the speed of 6-10 drops/minute and obtain
To Nb (OH)5Precipitation, by precipitation and centrifugal separation, washing, drying after not being further added by precipitation, take 0.1g Nb (OH)5Precipitation with
0.5g citric acids are dissolved in the hydrogenperoxide steam generator of 20ml mass fractions 30%, add 0.139g ammonium metatungstates, 0.039g carbonic acid
Sodium and 0.2g ethylene glycol, using 1mol/L weak aqua ammonia regulation pH=3 after stirring, remove large quantity of moisture at 80 DEG C, 400 DEG C
Lower organics removal, calcine 5 hours at 700 DEG C, obtain pyrochlore constitution niobium potassium tungstate KNbWO6·H2O。
The embodiment is highly preferred embodiment of the present invention.Fig. 1 is niobium potassium tungstate KNbWO made from the embodiment 16·H2O's
X-ray diffraction pattern.Fig. 2 is niobium potassium tungstate KNbWO made from the embodiment 16·H2O stereoscan photograph.
Embodiment 2
By 1.0gNb2O5Added with 5.0gKOH in 60ml deionized waters, load autoclave, 180 DEG C of hydro-thermal process 48
Hour, obtain [Nb6O19]8-Alkaline solution, take supernatant liquor to instill 1mol/L watery hydrochloric acid with the speed of 6-10 drops/minute and obtain
To Nb (OH)5Precipitation, by precipitation and centrifugal separation, washing, drying after not being further added by precipitation, take 0.1g Nb (OH)5Precipitation with
0.5g citric acids are dissolved in the hydrogenperoxide steam generator of 10ml mass fractions 30%, add 0.139g ammonium metatungstates, 0.039g carbonic acid
Sodium and 0.2g ethylene glycol, using 1mol/ L weak aqua ammonias regulation pH=3 after stirring, remove large quantity of moisture at 80 DEG C, 400 DEG C
Lower organics removal, calcine 5 hours at 700 DEG C, obtain pyrochlore constitution niobium potassium tungstate KNbWO6·H2O。
Compared with embodiment 1, the dosage of hydrogenperoxide steam generator is reduced to 10ml, is shown at 23 ° and deposits in XRD spectra
In miscellaneous peak.
Embodiment 3
By 1.0gNb2O5Added with 5.0gKOH in 60ml deionized waters, load autoclave, 180 DEG C of hydro-thermal process 48
Hour, obtain [Nb6O19]8-Alkaline solution, take supernatant liquor to instill 1mol/L watery hydrochloric acid with the speed of 6-10 drops/minute and obtain
To Nb (OH)5Precipitation, by precipitation and centrifugal separation, washing, drying after not being further added by precipitation, take 0.1g Nb (OH)5Precipitation with
0.5g citric acids are dissolved in the hydrogenperoxide steam generator of 20ml mass fractions 30%, add 0.139g ammonium metatungstates, 0.039g carbonic acid
Sodium and 0.2g ethylene glycol, remove large quantity of moisture at 80 DEG C after stirring, organics removal at 400 DEG C, and calcining 5 is small at 700 DEG C
When, obtain pyrochlore constitution niobium potassium tungstate KNbWO6·H2O。
Compared with embodiment 1, be not used weak aqua ammonia regulation pH value, the pH=1 of system, be shown in XRD spectra 22 ° and
Two faint miscellaneous peaks at 23 ° be present, illustrate that the pH value of system is unsuitable too low.
Embodiment 4
By 1.0gNb2O5Added with 5.0gKOH in 60ml deionized waters, load autoclave, 180 DEG C of hydro-thermal process 48
Hour, obtain [Nb6O19]8-Alkaline solution, take supernatant liquor to instill 1mol/L watery hydrochloric acid with the speed of 6-10 drops/minute and obtain
To Nb (OH)5Precipitation, by precipitation and centrifugal separation, washing, drying after not being further added by precipitation, take 0.1g Nb (OH)5Precipitation with
0.5g citric acids are dissolved in the hydrogenperoxide steam generator of 20ml mass fractions 30%, add 0.139g ammonium metatungstates, 0.039g carbonic acid
Sodium and 0.2g ethylene glycol, using 1mol/L weak aqua ammonia regulation pH=5 after stirring, remove large quantity of moisture at 80 DEG C, 400 DEG C
Lower organics removal, calcine 5 hours at 700 DEG C, obtain pyrochlore constitution niobium potassium tungstate KNbWO6·H2O。
Compared with embodiment 1, pH=5 is adjusted using weak aqua ammonia, does not find miscellaneous peak in XRD spectra, simply ESEM shines
Piece shows that the particle size that product is made is slightly larger.
Embodiment 5
By 1.0gNb2O5Added with 5.0gKOH in 60ml deionized waters, load autoclave, 180 DEG C of hydro-thermal process 48
Hour, obtain [Nb6O19]8-Alkaline solution, take supernatant liquor to instill 1mol/L watery hydrochloric acid with the speed of 6-10 drops/minute and obtain
To Nb (OH)5Precipitation, by precipitation and centrifugal separation, washing, drying after not being further added by precipitation, take 0.1g Nb (OH)5Precipitation with
0.5g citric acids are dissolved in the hydrogen peroxide of 20ml mass fractions 30%, add 0.139g ammonium metatungstates, 0.039g sodium carbonate and
0.2g ethylene glycol, pH=3 is adjusted using 1mol/L weak aqua ammonia after stirring, removes large quantity of moisture at 80 DEG C, 400 DEG C are gone down
Except organic matter, calcined 5 hours at 600 DEG C, obtain pyrochlore constitution niobium potassium tungstate KNbWO6·H2O。
Compared with embodiment 1, calcining heat is reduced to 600 DEG C, is shown in XRD spectra at 23 ° and miscellaneous peak be present.
Embodiment 6
By 1.0gNb2O5Added with 5.0gKOH in 60ml deionized waters, load autoclave, 180 DEG C of hydro-thermal process 48
Hour, obtain [Nb6O19]8-Alkaline solution, take supernatant liquor to instill 1mol/L watery hydrochloric acid with the speed of 6-10 drops/minute and obtain
To Nb (OH)5Precipitation, by precipitation and centrifugal separation, washing, drying after not being further added by precipitation, take 0.1g Nb (OH)5Precipitation with
0.5g citric acids are dissolved in the hydrogenperoxide steam generator of 20ml mass fractions 30%, add 0.139g ammonium metatungstates, 0.039g carbonic acid
Sodium and 0.2g ethylene glycol, using 1mol/L weak aqua ammonia regulation pH=3 after stirring, remove large quantity of moisture at 80 DEG C, 400 DEG C
Lower organics removal, calcine 5 hours at 800 DEG C, obtain pyrochlore constitution niobium potassium tungstate KNbWO6·H2O。
Compared with embodiment 1, sintering temperature is increased to 800 DEG C, is shown in XRD spectra at 30 ° and miscellaneous peak be present.
Pure phase can not be obtained as can be seen that sintering temperature is too high or too low by embodiment 5,6 and the contrast of embodiment 1
Crystal, 700 DEG C is optimal.
Embodiment 7
By 1.0gNb2O5Added with 5.0gKOH in 60ml deionized waters, load autoclave, 180 DEG C of hydro-thermal process 48
Hour, obtain [Nb6O19]8-Alkaline solution, take supernatant liquor to instill 1mol/L watery hydrochloric acid with the speed of 6-10 drops/minute and obtain
To Nb (OH)5Precipitation, by precipitation and centrifugal separation, washing, drying after not being further added by precipitation, take 0.1g Nb (OH)5Precipitation with
0.5g citric acids are dissolved in the hydrogenperoxide steam generator of 20ml mass fractions 30%, add 0.139g ammonium metatungstates, 0.039g carbonic acid
Sodium and 0.2g ethylene glycol, using 1mol/L weak aqua ammonia regulation pH=3 after stirring, remove large quantity of moisture at 80 DEG C, 400 DEG C
Lower organics removal, calcine 4 hours at 700 DEG C, obtain pyrochlore constitution niobium potassium tungstate KNbWO6·H2O。
Compared with embodiment 1, reduce calcination time for 4 hours, be shown at 11 °, 36 ° and 43 ° and deposit in XRD spectra
In faint miscellaneous peak, illustrate that calcination time should not be too short.
Embodiment 8
By 1.0gNb2O5Added with 5.0gKOH in 60ml deionized waters, load autoclave, obtain [Nb6O19]8-'s
Alkaline solution, take supernatant liquor to instill 1mol/L watery hydrochloric acid with the speed of 6-10 drops/minute and obtain Nb (OH)5Precipitation, it is extremely heavy
Form sediment precipitation and centrifugal separation, washing, drying after not being further added by, take 0.1g Nb (OH)5Precipitation is dissolved in 20ml matter with 0.5g citric acids
In the hydrogenperoxide steam generator for measuring fraction 30%, 0.139g ammonium metatungstates, 0.039g sodium carbonate and 0.2g ethylene glycol are added, stirring is equal
Using 1mol/L weak aqua ammonia regulation pH=3 after even, large quantity of moisture is removed at 80 DEG C, organics removal at 400 DEG C, at 700 DEG C
Calcining 10 hours, obtains pyrochlore constitution niobium potassium tungstate KNbWO6·H2O。
Compared with embodiment 1, calcination time is added as 10 hours, does not find miscellaneous peak in XRD spectra, and diffraction peak intensity omits
There is reinforcement.
Embodiment 9
By 1.0gNb2O5Added with 5.0gKOH in 60ml deionized waters, load autoclave, 180 DEG C of hydro-thermal process 48
Hour, obtain [Nb6O19]8-Alkaline solution, take supernatant liquor to instill 1mol/L watery hydrochloric acid with the speed of 6-10 drops/minute and obtain
To Nb (OH)5Precipitation, by precipitation and centrifugal separation, washing, drying after not being further added by precipitation, take 0.1g Nb (OH)5Precipitation with
0.5g citric acids are dissolved in the hydrogenperoxide steam generator of 20ml mass fractions 30%, add 0.139g ammonium metatungstates, 0.039g carbonic acid
Sodium and 0.1g ethylene glycol, using 1mol/L weak aqua ammonia regulation pH=3 after stirring, remove large quantity of moisture at 80 DEG C, 400 DEG C
Lower organics removal, calcine 5 hours at 700 DEG C, obtain pyrochlore constitution niobium potassium tungstate KNbWO6·H2O。
Compared with embodiment 1, the dosage of ethylene glycol is reduced to 0.1g, does not find miscellaneous peak in XRD spectra, simply ESEM
Photo shows the particle size increase that product is made, and has agglomeration.
Above example is to the course of work for example, not being the limit to protection scope of the present invention of the present invention
It is fixed, without departing from the inventive concept of the premise, any possible change or replacement are carried out, belong to the protection model of the present invention
Enclose.Embodiment 1,4,8,9 is positive example, and wherein embodiment 1 is most preferred embodiment, and embodiment 2,3,5,6,7 is counter-example, be used for and
What the present invention compared.
Claims (3)
1. a kind of method that sol-gal process prepares niobium tungstate, uses Nb2O5It is 1 by mass ratio as niobium source：5：60
Nb2O5, KOH, deionized water be placed in reactor, wherein the volume of deionized water is no more than the 80% of reactor capacity, 180
DEG C reaction 48h, obtain [Nb6O19]8-The watery hydrochloric acid that concentration is 1mol/L is added dropwise to [Nb by alkaline solution as presoma6O19
]8-In alkaline solution, there is Nb (OH)5Precipitation, watery hydrochloric acid to the precipitation for continuing to be added dropwise 1mol/L is not further added by, by pelleting centrifugation
Separate, wash, be dried for standby；By obtained Nb (OH)5The hydrogenperoxide steam generator that mass fraction is 30% is added to citric acid
In, every gram of citric acid adds hydrogenperoxide steam generator >=40ml of mass fraction 30%, citric acid and Nb (OH)5Mass ratio >=5；
The ratio 1 of amount of substance after clarifying according to Nb, W, K is stirred to solution：1：1 adds ammonium metatungstate and potassium carbonate, adds ethylene glycol
As dispersant, pH=3~5 of solution are adjusted using 1mol/L weak aqua ammonia；Drying obtains thick molten at 80~100 DEG C
Glue, further dehydration obtain xerogel；Organic matter in 200~400 DEG C of removal systems, 700 DEG C of calcining more than 5h, after cooling
To pyrochlore constitution niobium potassium tungstate KNbWO6·H2O。
2. the method that a kind of sol-gal process according to claim 1 prepares niobium tungstate, it is characterised in that use
The pH=3 of 1mol/L weak aqua ammonia regulation solution.
3. the method that a kind of sol-gal process according to right 1 or 2 prepares niobium tungstate, it is characterised in that every gram of Nb
(OH)5Precipitation uses 0.2 gram of ethylene glycol as dispersant.
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