CN107445200A - The preparation system of nano titanium oxide - Google Patents
The preparation system of nano titanium oxide Download PDFInfo
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- CN107445200A CN107445200A CN201710692271.1A CN201710692271A CN107445200A CN 107445200 A CN107445200 A CN 107445200A CN 201710692271 A CN201710692271 A CN 201710692271A CN 107445200 A CN107445200 A CN 107445200A
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- Prior art keywords
- gas
- preparation system
- solid
- titanium tetrachloride
- outlet
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention provides a kind of preparation system of nano titanium oxide.The preparation system includes hydrogen feeding mechanism, compressed air supply system, titanium tetrachloride vapors feeding unit, combustion reaction device and cooling device.Wherein combustion reaction device is provided with the outlet of gas-solid reaction thing, combustion reaction device is connected with hydrogen feeding mechanism through hydrogen supply line, combustion reaction device is connected with the compressed air supply pipeline of compressed air supply system, and combustion reaction device is connected with titanium tetrachloride vapors feeding unit through titanium tetrachloride vapors supply line；Cooling device is provided with gas-solid reaction thing entrance, and gas-solid reaction thing entrance is connected with the outlet of gas-solid reaction thing.Reaction condition is more gentle when preparing titanium dioxide by above-mentioned preparation system, is advantageously implemented the industrialization production of titanium dioxide.Because there is provided cooling device, this make it that the particle diameter using titanium dioxide granule made from the titanium dioxide device of the application offer is smaller, and particle diameter distribution is more concentrated.
Description
Technical field
The present invention relates to inorganic metal compound field, in particular to a kind of preparation system of nano titanium oxide.
Background technology
In recent years, make its purposes more and more extensive because nano titanium oxide has very outstanding performance, annual production
Growth rate has reached more than 9%.
Nano-TiO2With most valuable optical property, fine development is all shown in auto industry and numerous areas
Prospect.Nano-TiO2Also there is very high chemical stability, heat endurance, nontoxicity, Superhydrophilic, non-migratory, and completely
It can be contacted with food, so being widely used in anti-ultraviolet material, weaving, photocatalysis catalyst, glass with clean, suncream, painting
In material, paint, ink, packaging material for food, paper industry, aerospace industry, in lithium battery.
Up to the present, nano-TiO2Preparation method can generally be divided into vapor phase method and liquid phase method.
The technique of domestic production nano titanium oxide mainly relies on liquid phase method.The advantages of liquid phase method be raw material sources it is wide,
Cost is low, equipment is simple, is easy to mass produce.But liquid phase method easily causes solid material distriution inequality, product size and shape
Shape is uneven, is drying and is easily causing interparticle reunion, particularly hard aggregation in calcination, is making the dispersiveness change of product
Difference, influence the using effect and application of product.
And the advantages of vapor phase method is that reaction speed is fast, continuous production, and product purity height, good dispersion, group can be realized
It is poly- less, surface-active it is big, product is especially suitable for fine ceramics material, catalyst material and electronic material.But gas phase reaction pair
The form of reactor, the material of equipment, mode of heating, feeding manner have very high requirement, and obtained product particle granularity
It is larger.This make it that the application of vapor phase method is limited significantly.
The content of the invention
It is a primary object of the present invention to provide a kind of preparation system of nano titanium oxide, received with solving vapor phase method preparation
The problem of grain graininess of rice titanium dioxide is larger.
To achieve these goals, one aspect of the invention provides a kind of preparation system of nano titanium oxide, including：
Hydrogen feeding mechanism；Compressed air supply system；Titanium tetrachloride vapors feeding unit；Combustion reaction device, it is anti-to be provided with gas-solid
Thing is answered to export, combustion reaction device is connected with hydrogen feeding mechanism through hydrogen supply line, and combustion reaction device is empty with compression
The compressed air supply pipeline of gas feeding mechanism is connected, and combustion reaction device is with titanium tetrachloride vapors feeding unit through four chlorinations
Titanium steam supply pipe road is connected；And cooling device, gas-solid reaction thing entrance is provided with, and gas-solid reaction thing entrance and gas-solid are anti-
Thing outlet is answered to be connected.
Further, preparation system also includes gas solid separation unit, and gas solid separation unit is with cooling device through cooling down material
Transfer pipeline is connected, and the cooling material that gas solid separation unit is used to transfer out cooling device carries out gas solid separation.
Further, gas solid separation unit includes：Cyclone separator, be provided with cyclonic separation entrance, gas vent and
First solid outlet, and cyclonic separation entrance is connected with cooling device through cooling down material delivery pipe road；And filter, set
There are gas access, acid gas outlet and the second solid outlet, and gas access is connected with gas vent.
Further, preparation system also includes elution device, and elution device exports with acid gas to be connected through acid gas transfer pipeline.
Further, preparation system also includes water washing device, and water washing device is arranged on acid gas transfer pipeline.
Further, preparation system also includes deacidifying device, deacidifying device respectively with the first solid outlet and the second solid
Outlet is connected, and deacidifying device is used for the acid gas in the first solid outlet and the nano titanium oxide of the second solid outlet discharge
Removing.
Further, preparation system also includes grain refiner feeding mechanism, and grain refiner feeding mechanism is anti-with burning
Device is answered to be connected.
Further, preparation system also includes compound modifying agent feeding mechanism, and compound modifying agent feeding mechanism is anti-with burning
Device is answered to be connected.
Further, cooling device is water-circulating cooling device.
Further, titanium tetrachloride vapors feeding unit includes：Titanium tetrachloride feeding mechanism, and vapourizing unit, vaporization dress
Put and be connected with titanium tetrachloride feeding mechanism, vapourizing unit is used to make titanium tetrachloride solid be converted into titanium tetrachloride vapors.
Apply the technical scheme of the present invention, the oxygen in hydrogen and compressed air is burnt to obtain vapor, four chlorinations
Titanium steam obtains the gas-solid mixture containing titanium dioxide in the atmosphere reclaimed water solution of above-mentioned water vapour.Prepared by above-mentioned preparation system
Reaction condition is more gentle during titanium dioxide, thus the material of the reaction unit needed for whole course of reaction and feeding manner requirement
It is not high, so as to be advantageously implemented the industrialization production of titanium dioxide.Simultaneously because being provided with cooling device, this to use this Shen
The particle diameter of titanium dioxide granule is smaller made from the titanium dioxide device that please be provided, and particle diameter distribution is more concentrated.
Brief description of the drawings
The Figure of description for forming the part of the application is used for providing a further understanding of the present invention, and of the invention shows
Meaning property embodiment and its illustrate be used for explain the present invention, do not form inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 shows a kind of preparation system of the nano titanium oxide provided according to a kind of typical embodiment of the present invention
The schematic diagram of system；
Fig. 2 shows a kind of preparation of the nano titanium oxide provided according to another preferred embodiment of the present invention
The schematic diagram of system.
Wherein, above-mentioned accompanying drawing marks including the following drawings：
10th, hydrogen feeding mechanism；20th, compressed air supply system；30th, titanium tetrachloride vapors feeding unit；31st, four chlorination
Titanium feeding mechanism；32nd, vapourizing unit；40th, combustion reaction device；41st, grain refiner feeding mechanism；42nd, compound modifying agent supplies
Answer device；50th, cooling device；60th, gas solid separation unit；61st, cyclone separator；62nd, filter；70th, elution device；
80th, water washing device；90th, deacidifying device.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Below
Description only actually at least one exemplary embodiment is illustrative, is never used as to the present invention and its application or makes
Any restrictions.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creative work premise
Lower obtained every other embodiment, belongs to the scope of protection of the invention.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
As described by background technology, the problem of titanium dioxide nanoparticle granularity is larger made from vapor phase method.In order to
Solves above-mentioned technical problem, the invention provides a kind of preparation system of nano titanium oxide, as shown in figure 1, the preparation system
Including hydrogen feeding mechanism 10, compressed air supply system 20, titanium tetrachloride vapors feeding unit 30, the and of combustion reaction device 40
Cooling device 50.Wherein combustion reaction device 40 is provided with the outlet of gas-solid reaction thing, and combustion reaction device 40 fills with hydrogen supply
Put 10 through hydrogen supply line to be connected, combustion reaction device 40 and the compressed air supply pipeline of compressed air supply system 20
It is connected, combustion reaction device 40 is connected with titanium tetrachloride vapors feeding unit 30 through titanium tetrachloride vapors supply line；It is cold
But device 50 is provided with gas-solid reaction thing entrance, and gas-solid reaction thing entrance is connected with the outlet of gas-solid reaction thing.
The compressed air that the hydrogen and compressed air supply system 20 that hydrogen feeding mechanism 10 provides provide is in combustion reaction
Burnt to obtain vapor in device 40, the titanium tetrachloride vapors that titanium tetrachloride vapors feeding unit 30 provides are steamed in above-mentioned water
The atmosphere reclaimed water solution of vapour obtains the gas-solid mixture containing titanium dioxide；Then above-mentioned gas-solid mixture is carried out through cooling device 50
Cooling obtains the nano titanium oxide of mixed type.Reaction condition is more gentle when preparing titanium dioxide by above-mentioned preparation system,
Thus the material of the reaction unit needed for whole course of reaction and feeding manner are less demanding, so as to be advantageously implemented titanium dioxide
Industrialization production.Simultaneously because being provided with cooling device 50, this to be made using the titanium dioxide device that the application provides
Titanium dioxide granule particle diameter it is smaller, and particle diameter distribution is more concentrated.
It is preferred that as shown in Fig. 2 above-mentioned titanium tetrachloride vapors feeding unit 30 includes titanium tetrachloride feeding mechanism 31 and vaporization
Device 32, wherein vapourizing unit 32 are connected with titanium tetrachloride feeding mechanism 31, for making titanium tetrachloride solid be converted into tetrachloro
Change titanium steam.
In a preferred embodiment, as shown in Fig. 2 preparation system also includes gas solid separation unit 60, gas-solid point
It is connected from unit 60 and cooling device 50 through cooling down material delivery pipe road, gas solid separation unit 60 is used for from cooling device 50
The cooling material transferred out carries out gas solid separation.Can be to the acid in the gas-solid mixture after cooling by gas solid separation unit 60
Gas separates with nano titanium oxide, and this is advantageous to handle with environmental protection acid gas in follow-up process.
In a preferred embodiment, as shown in Fig. 2 gas solid separation unit 60 includes cyclone separator 61 and mistake
Filter device 62.Cyclone separator 61 is provided with cyclonic separation entrance, gas vent and the first solid outlet, and cyclonic separation enters
Mouth is connected with cooling device 50 through cooling down material delivery pipe road；And filter 62 be provided with gas access, acid gas outlet and
Second solid outlet, and gas access is connected with gas vent.By the gas-solid mixture containing titanium dioxide nanoparticle according to
The secondary separation degree for being advantageous to improve titanium dioxide and acid gas by cyclone separator 61 and filter 62.
In a preferred embodiment, as shown in Fig. 2 above-mentioned preparation system also includes elution device 70, elution dress
Put 70 and exported with acid gas and is connected through acid gas transfer pipeline.The setting of elution device 70 can be divided from gas solid separation unit 60
The acid gas separated out is recycled, and then improves the economic effect of the present apparatus.By above-mentioned acid gas through leaching in elution device 70
Obtained concentrated hydrochloric acid is washed, remaining tail gas empties after alkali cleaning and washing.The concentrated hydrochloric acid of above-mentioned recovery can with direct marketing, or
Relieving haperacidity process can be circulated through parsing obtained anhydrous hydrogen chloride and diluted acid, diluted acid.
In a preferred embodiment, as shown in Fig. 2 above-mentioned preparation system also includes water washing device 80, washing dress
80 are put to be arranged on acid gas transfer pipeline.On acid gas transfer pipeline, set water washing device 80 will to wash away gas solid separation row
Dust in the acid gas gone out, occur to assemble and block pipeline so as to be advantageous to suppress above-mentioned acid gas in elution device 70.
In a preferred embodiment, as shown in Fig. 2 above-mentioned preparation system also includes deacidifying device 90, depickling dress
Put 90 respectively with above-mentioned first solid outlet and the second solid outlet to be connected, above-mentioned deacidifying device 90 is used to the first solid
Acid gas removing in mouth and the nano titanium oxide of the second solid outlet discharge.This is advantageous to the product for improving nano titanium oxide
Quality.Directly pack by dried titanium dioxide can, or wrapped again after surface treatment again as needed simultaneously
Dress sale.
In a preferred embodiment, as shown in Fig. 2 above-mentioned preparation system also includes grain refiner feeding mechanism
41, grain refiner feeding mechanism 41 is connected with combustion reaction device 40.The brilliant refinement of grain is added in combustion reaction device 40
Agent is advantageous to further reduce the granularity of nano titanium oxide.
In a preferred embodiment, as shown in Fig. 2 above-mentioned preparation system also includes compound modifying agent feeding mechanism
42, compound modifying agent feeding mechanism 42 is connected with combustion reaction device 40.Transformation of crystal is added in combustion reaction device 40
Agent is advantageous to make in product containing more required crystal formations.
In a preferred embodiment, as shown in Fig. 2 above-mentioned cooling device 50 is water-circulating cooling device.After reaction
About 1000 DEG C or so of gas-solid mixture temperature, it is necessary to be cooled.Using water-circulating cooling device by gas-solid mixing
Thing is cooled down, and the gas-solid mixture temperature after cooling still has about 300 DEG C or so, and this is advantageous to suppress titanium dioxide granule in height
Assemble under the conditions of temperature, so as to further reduce the particle diameter of titanium dioxide nanoparticle.It is preferred that above-mentioned cooling device 50 is anxious
Cooler, this is advantageous to the particle diameter for further reducing titanium dioxide nanoparticle.
In a preferred embodiment, as shown in Fig. 2 above-mentioned titanium tetrachloride vapors feeding unit 30 includes four chlorinations
Titanium feeding mechanism 31 and vapourizing unit 32, wherein vapourizing unit 32 are connected with titanium tetrachloride feeding mechanism 31, vapourizing unit 32
For making titanium tetrachloride solid be converted into titanium tetrachloride vapors.
As can be seen from the above description, the above embodiments of the present invention realize following technique effect：
The compressed air that the hydrogen and compressed air supply system that hydrogen feeding mechanism provides provide is in combustion reaction device
In burnt to obtain vapor, atmosphere of the titanium tetrachloride vapors that titanium tetrachloride vapors feeding unit provides in above-mentioned water vapour
Reclaimed water solution obtains the gas-solid mixture containing titanium dioxide；Then above-mentioned gas-solid mixture is cooled down through cooling device and mixed
The nano titanium oxide of mould assembly.
Reaction condition is more gentle when preparing titanium dioxide by above-mentioned preparation system, thus needed for whole course of reaction
The material and feeding manner of reaction unit are less demanding, so as to be advantageously implemented the industrialization production of titanium dioxide.Simultaneously because
There is provided cooling device, this causes the particle diameter of titanium dioxide granule made from the titanium dioxide device that is provided using the application more
It is small, and particle diameter distribution is more concentrated.
Unless specifically stated otherwise, the part and positioned opposite, the digital table of step otherwise illustrated in these embodiments
Do not limited the scope of the invention up to formula and numerical value.Simultaneously, it should be appreciated that for the ease of description, each portion shown in accompanying drawing
The size divided not is to be drawn according to the proportionate relationship of reality.For technology, side known to person of ordinary skill in the relevant
Method and equipment may be not discussed in detail, but in the appropriate case, the technology, method and apparatus should be considered as authorizing explanation
A part for book.In shown here and discussion all examples, any occurrence should be construed as merely exemplary, and
Not by way of limitation.Therefore, the other examples of exemplary embodiment can have different values.It should be noted that：Similar label
Similar terms is represented in following accompanying drawing with letter, therefore, once it is defined in a certain Xiang Yi accompanying drawing, then subsequent attached
It need not be further discussed in figure.
For the ease of description, space relative terms can be used herein, as " ... on ", " ... top ",
" ... upper surface ", " above " etc., for describing such as a device shown in the figure or feature and other devices or spy
The spatial relation of sign.It should be appreciated that space relative terms are intended to comprising the orientation except device described in figure
Outside different azimuth in use or operation.For example, if the device in accompanying drawing is squeezed, it is described as " in other devices
It will be positioned as " under other devices or construction after the device of part or construction top " or " on other devices or construction "
Side " or " under other devices or construction ".Thus, exemplary term " ... top " can include " ... top " and
" in ... lower section " two kinds of orientation.The device can also other different modes positioning (being rotated by 90 ° or in other orientation), and
And respective explanations are made to the relative description in space used herein above.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
- A kind of 1. preparation system of nano titanium oxide, it is characterised in that including：Hydrogen feeding mechanism (10)；Compressed air supply system (20)；Titanium tetrachloride vapors feeding unit (30)；Combustion reaction device (40), is provided with the outlet of gas-solid reaction thing, and the combustion reaction device (40) is supplied with the hydrogen Device (10) is connected through hydrogen supply line, and the combustion reaction device (40) passes through with the compressed air supply system (20) Compressed air supply line is connected, and the combustion reaction device (40) is with the titanium tetrachloride vapors feeding unit (30) through four Titanium chloride steam supply pipe road is connected；AndCooling device (50), gas-solid reaction thing entrance is provided with, and the gas-solid reaction thing entrance goes out with the gas-solid reaction thing Mouth is connected.
- 2. preparation system according to claim 1, it is characterised in that the preparation system also includes gas solid separation unit (60), the gas solid separation unit (60) is connected with the cooling device (50) through cooling down material delivery pipe road, the gas-solid The cooling material that separative element (60) is used to transfer out the cooling device (50) carries out gas solid separation.
- 3. preparation system according to claim 2, it is characterised in that the gas solid separation unit (60) includes：Cyclone separator (61), it is provided with cyclonic separation entrance, gas vent and the first solid outlet, and the cyclonic separation Entrance is connected with the cooling device (50) through the cooling material delivery pipe road；AndFilter (62), it is provided with gas access, acid gas outlet and the second solid outlet, and the gas access and the gas Body outlet is connected.
- 4. preparation system according to claim 3, it is characterised in that the preparation system also includes elution device (70), The elution device (70) exports with the acid gas to be connected through acid gas transfer pipeline.
- 5. preparation system according to claim 4, it is characterised in that the preparation system also includes water washing device (80), The water washing device (80) is arranged on the acid gas transfer pipeline.
- 6. preparation system according to claim 3, it is characterised in that the preparation system also includes deacidifying device (90), The deacidifying device (90) is connected with first solid outlet and second solid outlet respectively, the deacidifying device (90) acid gas in the nano titanium oxide for being used to discharge first solid outlet and second solid outlet removes.
- 7. preparation system according to any one of claim 1 to 6, it is characterised in that the preparation system also includes crystalline substance Grain fining agent feeding mechanism (41), the grain refiner feeding mechanism (41) are connected with the combustion reaction device (40).
- 8. preparation system according to claim 7, it is characterised in that the preparation system also includes compound modifying agent and supplied Device (42), the compound modifying agent feeding mechanism (42) are connected with the combustion reaction device (40).
- 9. preparation system according to claim 8, it is characterised in that the cooling device (50) is water-circulating cooling device.
- 10. preparation system according to claim 1, it is characterised in that titanium tetrachloride vapors feeding unit (30) bag Include：Titanium tetrachloride feeding mechanism (31), andVapourizing unit (32), the vapourizing unit (32) are connected with the titanium tetrachloride feeding mechanism (31), the vaporization dress (32) are put to be used to make titanium tetrachloride solid be converted into titanium tetrachloride vapors.
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Cited By (1)
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| CN111847507A (en) * | 2020-07-06 | 2020-10-30 | 南通江山农药化工股份有限公司 | Preparation process of nano titanium dioxide by gas phase method |
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Application publication date: 20171208 |