CN103787408A - Preparation method of ammonium trifluorooxytitanate - Google Patents
Preparation method of ammonium trifluorooxytitanate Download PDFInfo
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- CN103787408A CN103787408A CN201410015903.7A CN201410015903A CN103787408A CN 103787408 A CN103787408 A CN 103787408A CN 201410015903 A CN201410015903 A CN 201410015903A CN 103787408 A CN103787408 A CN 103787408A
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- acid ammonium
- trifluoro oxygen
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Abstract
The invention provides a preparation method of ammonium trifluorooxytitanate (NH4TiOG3). The preparation method comprises the following steps: by taking ammonium fluorotitanate [(NH4)2TiF6] liquor and ammonium water (NH4OH) liquor as raw materials, mixing the ammonium fluorotitanate liquor and the ammonium water liquor, and reacting at 15-50 DEG C to obtain ammonium trifluorooxytitanate. The preparation method provided by the invention is simple and environment-friendly and low in reaction temperature. The grain size of the ammonium trifluorooxytitanate powder is less (less than 1 micron) and uniform in distribution. Furthermore, preferably, ammonium trifluorooxytitanate with the grain size which is ranged from 300nm to 600nm and uniform in distribution can be prepared by reaction at 15-35 DEG C.
Description
Technical field
The invention belongs to inorganics preparing technical field, be specifically related to a kind of trifluoro oxygen titanium acid ammonium (NH
4tiOF
3) preparation method.
Background technology
Due to titanium dioxide (TiO
2) unique physicochemical property, it has a wide range of applications in the field such as environmental protection and the energy.Theoretical calculate and experimental result all show: if increase high reactivity, { 001} crystal face, in the shared ratio in titanic oxide material surface, will contribute to improve its reactive behavior, strengthen its usefulness in various application.At present, for the preparation of { method that 001} crystal face is exposed to the titanic oxide material of outside surface mainly contains two classes: a class is by hydrofluoric acid (HF) or Neutral ammonium fluoride (NH
4f) { 001} crystal face reactive behavior, to being retained (Yang, H.G.et al.Nature, 2008,453,638-641) in final product in reduction; Another kind of is to make (Zhou, L.et al.CrystEngComm, 2013,15,5012-5015) by the topological conversion reaction of trifluoro oxygen titanium acid ammonium.Rear class methods are for last class, simpler, and noxious chemical uses still less, is likely applied to scale operation.
At present, trifluoro oxygen titanium acid ammonium is mainly by ammonium titanium fluoride ((NH
4)
2tiF
6) and boric acid (H
3bO
3) reaction makes, gained granular size differs, and shape irregularity is unfavorable for that later stage topology transforms that { 001} face is exposed to outer titanic oxide material to make.In order to control its size and shape, often need in reaction system, add tensio-active agent, this has increased again preparation cost virtually.Meanwhile, the at present prepared trifluoro oxygen of method titanium acid ammonium particle, generally large (3～5 microns) of size, cause calcining rear gained specific surface area less, and photocatalytic activity is limited, has limited its large-scale application.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, provides one to utilize ammonium titanium fluoride ((NH
4)
2tiF
6) solution and ammoniacal liquor (NH
4oH) solution is prepared trifluoro oxygen titanium acid ammonium (NH
4tiOF
3) method.The method preparation is simple, and temperature of reaction is low, the trifluoro oxygen titanium acid ammonium powder size less (1 micron following) obtaining and being evenly distributed.
The present invention is for solving the problems of the technologies described above by the following technical solutions:
A kind of trifluoro oxygen titanium acid ammonium (NH
4tiOF
3) preparation method, adopting ammonium titanium fluoride solution and ammonia soln is raw material, and ammonium titanium fluoride solution and ammonia soln are mixed, 15～50 ℃ of reactions obtain trifluoro oxygen titanium acid ammonium.
In such scheme, the described reaction times is 1～24h.
In such scheme, described ammonia soln is take the mol ratio of ammonium titanium fluoride in effective ammoniacal liquor content meter wherein and ammonium titanium fluoride solution as 1:2～4:3, and temperature of reaction is 15～35 ℃.
In such scheme, in the mixed solution that described ammonium titanium fluoride solution and ammonia soln form after mixing, the volumetric molar concentration of ammonium titanium fluoride is 0.1～0.4mol/L, more preferably 0.2～0.4mol/L.
In such scheme, the described reaction times is preferably 8～16h.
In such scheme, the preparation method of described trifluoro oxygen titanium acid ammonium is precipitated centrifugal reaction solution after also comprising that reaction finishes, and then will precipitate water, absolute ethanol washing successively, the dry trifluoro oxygen titanium acid ammonium powder that obtains.
The invention has the beneficial effects as follows: the simple environmental protection of preparation method, temperature of reaction is low, the trifluoro oxygen titanium acid ammonium powder size that obtains less (1 micron following) and being evenly distributed, more preferably 15～35 ℃ can be reacted the trifluoro oxygen titanium acid ammonium for preparing particle size range 300～600nm and be evenly distributed.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the prepared trifluoro oxygen titanium acid ammonium of the embodiment of the present invention one;
Fig. 2 is the scanning electron microscope (SEM) photograph of the prepared trifluoro oxygen titanium acid ammonium of embodiment bis-;
Fig. 3 is the scanning electron microscope (SEM) photograph of the prepared trifluoro oxygen titanium acid ammonium of embodiment tri-;
In Fig. 4, A is the XRD figure of the prepared trifluoro oxygen titanium acid ammonium of the embodiment of the present invention four, and B is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3) standard x RD scheme (according to NH
4tiOF
3standard P DF card draw, NO.54-0239);
Fig. 5 is the scanning electron microscope (SEM) photograph of the prepared trifluoro oxygen titanium acid ammonium of embodiment ten.
Embodiment
For making those skilled in the art understand better technical scheme of the present invention, below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment mono-
Take 0.5939g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 2mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.3mol/L, ammonia concn is 0.2mol/L, in ammonia soln, in effective ammoniacal liquor content and ammonium titanium fluoride solution, the mol ratio of ammonium titanium fluoride is 2:3, after mixing, put into 24 ℃ of waters bath with thermostatic control, react the mixed solution that obtains containing trifluoro oxygen titanium acid ammonium after 8 hours, take out the centrifugal (6000r/min of mixed solution, 10 minutes), obtain white powder precipitation.Again white powder precipitation is added water and carry out ultrasonic dispersion washing with Ultrasonic Cleaners, recentrifuge (6000r/min after being uniformly dispersed, 10 minutes), and repeat twice of above-mentioned centrifuge washing process, finally add the ultrasonic dispersion washing of dehydrated alcohol, centrifugal (6000r/min, 10 minutes), the white powder obtaining is positioned in 60 ℃ of baking ovens and is dried 12 hours, obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, SEM schemes as shown in Figure 1, embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 500nm left and right as can be seen from Figure, mostly be square structure, and particle size distribution is even.
Embodiment bis-
Take 0.7919g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 2mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.4mol/L, ammonia concn is 0.2mol/L, after mixing, put into 24 ℃ of waters bath with thermostatic control, react after 8 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out the centrifugal (6000r/min of mixed solution, 10 minutes), obtain white powder precipitation.Again white powder precipitation is added water and carry out ultrasonic dispersion washing with Ultrasonic Cleaners, recentrifuge (6000r/min after being uniformly dispersed, 10 minutes), and repeat twice of above-mentioned centrifuge washing process, finally add the ultrasonic dispersion washing of dehydrated alcohol, centrifugal (6000r/min, 10 minutes), the white powder obtaining is positioned in 60 ℃ of baking ovens and is dried 12 hours, obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, SEM schemes as shown in Figure 2, embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 500nm left and right as can be seen from Figure, mostly be square structure, and particle size distribution is even.
Embodiment tri-
Take 0.5939g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 3mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.3mol/L, ammonia concn is 0.3mol/L, after mixing, put into 24 ℃ of waters bath with thermostatic control, react after 8 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out mixed solution centrifugal, obtain white powder precipitation.Again white powder is precipitated to water, absolute ethanol washing according to this, be drying to obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, SEM schemes as shown in Figure 3, embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 400～600nm as can be seen from Figure, mostly be square structure, and particle size distribution is even.
Embodiment tetra-
Take 0.7919g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 3mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.4mol/L, ammonia concn is 0.3mol/L, after mixing, put into 24 ℃ of waters bath with thermostatic control, react after 8 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out the centrifugal (6000r/min of mixed solution, 10 minutes), obtain white powder precipitation.Again white powder precipitation is added water and carry out ultrasonic dispersion washing with Ultrasonic Cleaners, recentrifuge (6000r/min after being uniformly dispersed, 10 minutes), and repeat twice of above-mentioned centrifuge washing process, finally add the ultrasonic dispersion washing of dehydrated alcohol, centrifugal (6000r/min, 10 minutes), the white powder obtaining is positioned in 60 ℃ of baking ovens and is dried 12 hours, obtain trifluoro oxygen titanium acid ammonium powder.
Adopt XRD to test the prepared trifluoro oxygen titanium acid ammonium powder of the present embodiment, gained XRD figure is as shown in A in Fig. 4, with trifluoro oxygen titanium acid ammonium (NH
4tiOF
3) standard x RD figure (B) contrast find, main diffraction peak is mated completely, proved inventive embodiments gained powder is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, and obtaining embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 400～600nm, and particle size distribution is even.
Embodiment five
Take 0.5939g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 4mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.3mol/L, ammonia concn is 0.4mol/L, after mixing, put into 24 ℃ of waters bath with thermostatic control, react after 8 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out mixed solution centrifugal, obtain white powder precipitation.Again white powder is precipitated to water, absolute ethanol washing according to this, be drying to obtain trifluoro oxygen titanium acid ammonium powder.。
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, and obtaining embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 400～600nm, and particle size distribution is even.
Embodiment six
Take 0.7919g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 4mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.4mol/L, ammonia concn is 0.4mol/L, after mixing, put into 24 ℃ of waters bath with thermostatic control, react after 8 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out the centrifugal (6000r/min of mixed solution, 10 minutes), obtain white powder precipitation.Again white powder precipitation is added water and carry out ultrasonic dispersion washing with Ultrasonic Cleaners, recentrifuge (6000r/min after being uniformly dispersed, 10 minutes), and repeat twice of above-mentioned centrifuge washing process, finally add the ultrasonic dispersion washing of dehydrated alcohol, centrifugal (6000r/min, 10 minutes), the white powder obtaining is positioned in 60 ℃ of baking ovens and is dried 12 hours, obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, and obtaining embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 300～500nm, and particle size distribution is even.
Embodiment seven
Take 0.5939g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 3mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.3mol/L, ammonia concn is 0.3mol/L, after mixing, put into 24 ℃ of waters bath with thermostatic control, react after 2 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out the centrifugal (6000r/min of mixed solution, 10 minutes), obtain white powder precipitation.Again white powder precipitation is added water and carry out ultrasonic dispersion washing with Ultrasonic Cleaners, recentrifuge (6000r/min after being uniformly dispersed, 10 minutes), and repeat twice of above-mentioned centrifuge washing process, finally add the ultrasonic dispersion washing of dehydrated alcohol, centrifugal (6000r/min, 10 minutes), the white powder obtaining is positioned in 60 ℃ of baking ovens and is dried 12 hours, obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, and obtaining embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 400～600nm, and particle size distribution is even.
Embodiment eight
Take 0.5939g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 3mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.3mol/L, ammonia concn is 0.3mol/L, after mixing, put into 24 ℃ of waters bath with thermostatic control, react after 4 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out the centrifugal (6000r/min of mixed solution, 10 minutes), obtain white powder precipitation.Again white powder precipitation is added water and carry out ultrasonic dispersion washing with Ultrasonic Cleaners, recentrifuge (6000r/min after being uniformly dispersed, 10 minutes), and repeat twice of above-mentioned centrifuge washing process, finally add the ultrasonic dispersion washing of dehydrated alcohol, centrifugal (6000r/min, 10 minutes), the white powder obtaining is positioned in 60 ℃ of baking ovens and is dried 12 hours, obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, and obtaining embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 500nm left and right, and particle size distribution is even.
Embodiment nine
Take 0.5939g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 3mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.3mol/L, ammonia concn is 0.3mol/L, after mixing, put into 24 ℃ of waters bath with thermostatic control, react after 12 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out the centrifugal (6000r/min of mixed solution, 10 minutes), obtain white powder precipitation.Again white powder precipitation is added water and carry out ultrasonic dispersion washing with Ultrasonic Cleaners, recentrifuge (6000r/min after being uniformly dispersed, 10 minutes), and repeat twice of above-mentioned centrifuge washing process, finally add the ultrasonic dispersion washing of dehydrated alcohol, centrifugal (6000r/min, 10 minutes), the white powder obtaining is positioned in 60 ℃ of baking ovens and is dried 12 hours, obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, and obtaining embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 500nm left and right, and particle size distribution is even.
Embodiment ten
Take 0.5939g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 3mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.3mol/L, ammonia concn is 0.3mol/L, after mixing, put into 24 ℃ of waters bath with thermostatic control, react after 16 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out the centrifugal (6000r/min of mixed solution, 10 minutes), obtain white powder precipitation.Again white powder precipitation is added water and carry out ultrasonic dispersion washing with Ultrasonic Cleaners, recentrifuge (6000r/min after being uniformly dispersed, 10 minutes), and repeat twice of above-mentioned centrifuge washing process, finally add the ultrasonic dispersion washing of dehydrated alcohol, centrifugal (6000r/min, 10 minutes), the white powder obtaining is positioned in 60 ℃ of baking ovens and is dried 12 hours, obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, and SEM schemes as shown in Figure 5, and obtaining embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 400～600nm, and particle size distribution is even.
Embodiment 11
Take 0.7919g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 3mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.4mol/L, ammonia concn is 0.3mol/L, after mixing, put into 15 ℃ of waters bath with thermostatic control, react the mixed solution that obtains containing trifluoro oxygen titanium acid ammonium after 8 hours, taking-up mixed solution is centrifugal, obtain white powder precipitation, again white powder is precipitated to water, absolute ethanol washing according to this, be drying to obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, and obtaining embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 200～400nm, and particle size distribution is even.
Embodiment 12
Take 0.7919g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 3mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.4mol/L, ammonia concn is 0.3mol/L, after mixing, put into 35 ℃ of waters bath with thermostatic control, react after 8 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out mixed solution centrifugal, obtain white powder precipitation.Again white powder is precipitated to water, absolute ethanol washing according to this, be drying to obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, and obtaining embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 400～600nm, and particle size distribution is even.
Embodiment 13
Take 0.7919g ammonium titanium fluoride and be dissolved in and in 9mL deionized water, be made into ammonium titanium fluoride solution, in ammonium titanium fluoride solution, add 1mL ammonia soln (concentration is 3mol/L) again, in the mixed solution forming, ammonium titanium fluoride concentration is 0.4mol/L, ammonia concn is 0.3mol/L, after mixing, put into 50 ℃ of waters bath with thermostatic control, react after 8 hours and obtain the mixed solution containing trifluoro oxygen titanium acid ammonium, take out the centrifugal (6000r/min of mixed solution, 10 minutes), obtain white powder precipitation.Again white powder precipitation is added water and carry out ultrasonic dispersion washing with Ultrasonic Cleaners, recentrifuge (6000r/min after being uniformly dispersed, 10 minutes), and repeat twice of above-mentioned centrifuge washing process, finally add the ultrasonic dispersion washing of dehydrated alcohol, centrifugal (6000r/min, 10 minutes), the white powder obtaining is positioned in 60 ℃ of baking ovens and is dried 12 hours, obtain trifluoro oxygen titanium acid ammonium powder.
The sample of the present embodiment gained is tested through XRD, and obtaining sample is trifluoro oxygen titanium acid ammonium (NH
4tiOF
3).The another scanning electron microscope that adopts is tested the present embodiment gained trifluoro oxygen titanium acid ammonium powder, and obtaining embodiment of the present invention gained trifluoro oxygen titanium acid ammonium diameter of particle is 800～1000nm, and particle size distribution is even.
Be understandable that, above embodiment is only used to principle of the present invention is described and the illustrative embodiments that adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (7)
1. a preparation method for trifluoro oxygen titanium acid ammonium, is characterized in that: adopting ammonium titanium fluoride solution and ammonia soln is raw material, and ammonium titanium fluoride solution and ammonia soln are mixed, and 15～50 ℃ of reactions obtain trifluoro oxygen titanium acid ammonium.
2. the preparation method of trifluoro oxygen titanium acid ammonium according to claim 1, is characterized in that: the described reaction times is 1～24h.
3. the preparation method of trifluoro oxygen titanium acid ammonium according to claim 1 and 2, is characterized in that: described ammonia soln is take the mol ratio of ammonium titanium fluoride in effective ammoniacal liquor content meter wherein and ammonium titanium fluoride solution as 1:2～4:3, and temperature of reaction is 15～35 ℃.
4. the preparation method of trifluoro oxygen titanium acid ammonium according to claim 3, is characterized in that: in the mixed solution that described ammonium titanium fluoride solution and ammonia soln form after mixing, the volumetric molar concentration of ammonium titanium fluoride is 0.1～0.4mol/L.
5. the preparation method of trifluoro oxygen titanium acid ammonium according to claim 4, is characterized in that: in the mixed solution that described ammonium titanium fluoride solution and ammonia soln form after mixing, the volumetric molar concentration of ammonium titanium fluoride is 0.2～0.4mol/L.
6. the preparation method of trifluoro oxygen titanium acid ammonium according to claim 3, is characterized in that: the described reaction times is 8～16h.
7. the preparation method of trifluoro oxygen titanium acid ammonium according to claim 3, is characterized in that: it is precipitated centrifugal reaction solution after also comprising that reaction finishes, and then will precipitate water, absolute ethanol washing successively, the dry trifluoro oxygen titanium acid ammonium powder that obtains.
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Cited By (4)
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| CN103991901A (en) * | 2014-06-09 | 2014-08-20 | 华中科技大学 | Method for increasing yield of ammonium oxytrifluorotitanate by using mixed solvent |
| CN105271379A (en) * | 2015-10-28 | 2016-01-27 | 南京理工大学 | Method for synthesizing non-stoichiometric oxyfluoride ammonium titanate powder on basis of chemical nitrogen fixation technology |
| CN107096561A (en) * | 2017-06-12 | 2017-08-29 | 青岛科技大学 | A kind of Pt/NH4TiOF3Porous saqima structure photochemical catalyst and preparation method thereof |
| CN111193022A (en) * | 2020-01-07 | 2020-05-22 | 东北大学秦皇岛分校 | Preparation and application of modified ammonium trifluorooxotitanate for lithium ion battery |
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| TW200736169A (en) * | 2006-03-28 | 2007-10-01 | Univ Nat Sun Yat Sen | A method for preparing titanium oxide particle incorporated with nitrogen and fluorine |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103991901A (en) * | 2014-06-09 | 2014-08-20 | 华中科技大学 | Method for increasing yield of ammonium oxytrifluorotitanate by using mixed solvent |
| CN103991901B (en) * | 2014-06-09 | 2015-09-09 | 华中科技大学 | A kind of method utilizing mixed solvent to improve trifluoro oxygen titanium acid ammonium productive rate |
| CN105271379A (en) * | 2015-10-28 | 2016-01-27 | 南京理工大学 | Method for synthesizing non-stoichiometric oxyfluoride ammonium titanate powder on basis of chemical nitrogen fixation technology |
| CN107096561A (en) * | 2017-06-12 | 2017-08-29 | 青岛科技大学 | A kind of Pt/NH4TiOF3Porous saqima structure photochemical catalyst and preparation method thereof |
| CN111193022A (en) * | 2020-01-07 | 2020-05-22 | 东北大学秦皇岛分校 | Preparation and application of modified ammonium trifluorooxotitanate for lithium ion battery |
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| CN103787408B (en) | 2015-09-09 |
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