CN117398959A - Device and method for producing micron-sized rutile titanium white - Google Patents
Device and method for producing micron-sized rutile titanium white Download PDFInfo
- Publication number
- CN117398959A CN117398959A CN202311510881.7A CN202311510881A CN117398959A CN 117398959 A CN117398959 A CN 117398959A CN 202311510881 A CN202311510881 A CN 202311510881A CN 117398959 A CN117398959 A CN 117398959A
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- Prior art keywords
- titanium tetrachloride
- inlet
- oxygen
- titanium
- shell
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 235000010215 titanium dioxide Nutrition 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 108
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000001301 oxygen Substances 0.000 claims abstract description 46
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 46
- 239000002245 particle Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims description 11
- 239000004408 titanium dioxide Substances 0.000 abstract description 17
- 239000013078 crystal Substances 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 238000009826 distribution Methods 0.000 abstract description 7
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 6
- 239000012530 fluid Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 239000002243 precursor Substances 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
Classifications
-
- 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
- C01G23/07—Producing by vapour phase processes, e.g. halide oxidation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
Abstract
The invention discloses a device and a method for producing micron-sized rutile titanium white, belonging to the technical field of chloridizing metallurgy. The device comprises: a hollow housing extending in an axial direction; an oxygen inlet arranged at one end of the shell; a titanium tetrachloride first inlet comprising a plurality of holes circumferentially disposed on the housing; a titanium tetrachloride second inlet axially spaced a predetermined distance from the titanium tetrachloride first inlet and including an air intake ring disposed about the periphery of the hollow housing. The device disclosed by the invention has the advantages that the titanium tetrachloride enters through two inlets, the proportion of the titanium tetrachloride feeding amount in the small hole at the front end to the total titanium tetrachloride feeding amount is small, and the proportion of the titanium tetrachloride at the inlets to the total oxygen amount is also small, so that the titanium tetrachloride at the first inlet can be well dispersed in oxygen, and meanwhile, discrete fine titanium dioxide crystal grains are generated, and the crystal grains are used as crystal seeds for oxidizing the titanium tetrachloride at the second inlet, so that micron-sized large particles are rapidly generated through surface chemical reaction, and the particle size distribution range of a product is reduced.
Description
Technical Field
The invention relates to the technical field of chloridizing metallurgy, in particular to a device and a method for producing micron-sized rutile titanium white.
Background
Titanium dioxide is considered as a white pigment with the best performance in the world at present, and is widely applied to various industrial departments and life fields such as paint, plastics, papermaking, printing ink, chemical fiber, rubber, cosmetics, enamel and the like. The unit lattice of rutile titanium white is small and compact, and the stability and the relative density are larger, so that the dielectric constant, the refractive index and the thermal conductivity are higher. The prior industrial preparation of titanium dioxide mainly comprises a sulfuric acid process and a chlorination process, and compared with the sulfuric acid process, the chlorination process titanium dioxide process has the advantages of short flow, less discharge of three wastes, high product quality and the like, and has more and more obvious advantages in titanium dioxide production.
The chloride process titanium dioxide technology is used as the first-choice engineering technology of high-grade titanium dioxide raw materials, has been rapidly developed and developed in China in recent years, and the types of titanium dioxide products have also been rapidly increased. The product has the reference from nano titanium dioxide (< 100 nanometers) to the average particle size of 0.3 micrometer, but the gas-phase titanium chloride white with the particle size of 0.3 micrometer and above has less variety and poor uniformity of particle size. The titanium white with large particle size has better infrared absorption characteristic and better application prospect. At present, the granularity of the produced titanium white is mainly controlled by adjusting the temperature of oxygen, the residence time of high temperature and the like on an industrial production line, but the method has a limited adjustable range and the particle size distribution of the obtained titanium white is wider.
Therefore, it is necessary to design an oxidation reaction apparatus and method which can control the average particle size and the particle size distribution more easily.
Disclosure of Invention
In view of the above, the present invention provides an apparatus and method for producing micro-scale rutile titanium dioxide.
According to an aspect of the present invention, there is provided an apparatus for producing micro-scale rutile titanium white, comprising:
a hollow housing extending in an axial direction;
an oxygen inlet arranged at one end of the shell;
a titanium tetrachloride first inlet comprising a plurality of holes circumferentially disposed on the housing;
a titanium tetrachloride second inlet axially spaced a predetermined distance from the titanium tetrachloride first inlet and including an air intake ring disposed about the periphery of the hollow housing.
According to one embodiment of the invention, the oxygen inlet is arranged in the center of the end face of the housing.
According to one embodiment of the invention, the diameter of the hole of the titanium tetrachloride first inlet is 1-3 mm.
According to one embodiment of the invention, the number of the holes of the titanium tetrachloride first inlet is 9-28.
According to one embodiment of the invention, the apertures of the titanium tetrachloride first inlet extend in a radial direction.
According to one embodiment of the invention, the air inlet ring comprises:
the annular main body is coaxially fixed on the outer surface of the shell, the annular main body defines a hollow rectifying chamber, the outer wall of the annular main body is provided with a titanium tetrachloride feeding port, the annular main body is also provided with a flow guide slit for communicating the rectifying chamber with an oxygen channel in the shell, and the width of the flow guide slit is 15-80 mm.
According to one embodiment of the invention, the second inlet of titanium tetrachloride is axially spaced from the first inlet of titanium tetrachloride by a distance of 50 to 200mm.
According to one embodiment of the invention, the ratio of the hole spacing of adjacent holes of the titanium tetrachloride first inlet to the diameter of the hollow shell is 0.12 to 0.35:1.
according to another aspect of the present invention, there is provided a method for producing micro-scale rutile titanium white using the above apparatus, comprising the steps of:
supplying the combusted high temperature oxygen to an oxygen inlet of the device;
titanium tetrachloride accounting for 5% -20% of the total feeding amount is supplied into the shell of the device through a titanium tetrachloride first inlet;
supplying the remainder of the titanium tetrachloride to the housing of the apparatus via a titanium tetrachloride second inlet;
and collecting the generated micron-sized rutile titanium white particles.
According to one embodiment of the invention, the momentum ratio of titanium tetrachloride to axial oxygen fed through the titanium tetrachloride first inlet is 3-7, and the momentum ratio of titanium tetrachloride to axial oxygen fed through the titanium tetrachloride second inlet is 1.2-4.0.
By adopting the technical scheme, the device disclosed by the invention has the advantages that the titanium tetrachloride enters through the two inlets, the proportion of the titanium tetrachloride throwing amount in the small hole at the front end to the total titanium tetrachloride throwing amount is small, and the proportion of the titanium tetrachloride at the inlets to the total oxygen is also small, so that the titanium tetrachloride at the first inlet can be well dispersed in the oxygen, and meanwhile, discrete fine titanium dioxide grains are generated, and are used as seed crystals for oxidizing the titanium tetrachloride at the second inlet, so that micron-sized large particles are rapidly generated through surface chemical reaction, and the particle size distribution range of a product is reduced. Correspondingly, the method according to the invention has the same advantages.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural view of an apparatus for producing titanium white according to the prior art;
FIG. 2 is a schematic view showing the overall structure of an apparatus for producing micro-scale rutile titanium dioxide according to the present invention;
fig. 3 is a cross-sectional view of the apparatus for producing micro-scale rutile titanium dioxide of fig. 2 taken along line A-A.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Fig. 1 is a schematic structural view of an apparatus for producing titanium white according to the prior art, which generally includes a pipe A1 for supplying high-temperature oxygen, a feed ring A2 for adding titanium tetrachloride, and a reaction zone A3 located downstream as shown. High temperature oxygen enters the oxygen pipeline A1 through the oxygen inlet K1, titanium tetrachloride enters the interior of the pipeline through the titanium tetrachloride inlet K2 and is mixed with the oxygen in the pipeline to react, and the titanium tetrachloride further reacts in the downstream reaction zone A3. TiC1 4 And high temperature O 2 Upon contact, chemical reaction occurs to produce TiO 2 Precursor and reach TiO 2 Supersaturation degree capable of nucleation; then TiO 2 The precursor starts to nucleate and crystallize after accumulating to enough supersaturation; subsequently nucleated TiO 2 The precursor is continuously coagulated or sintered on the surface of the crystal nucleus in the airflow in the modes of diffusion, migration, collision and the like, so that the crystal nucleus is continuously grown. However, the existing device can only produce nano-scale titanium white but not micro-scale titanium white, and the granularity of the produced titanium white can be changed by adjusting the oxygen temperature, the high-temperature residence time and the like, but the method has a limited adjustable range and the particle size distribution of the obtained titanium white is wider.
In order to realize the production of the micron-sized rutile titanium white, the invention improves the structure of the existing device.
As shown in fig. 2, the apparatus for producing micro-scale rutile titanium white according to the present invention generally comprises a hollow shell 1 extending in an axial direction, an oxygen inlet provided at one end of the shell, a titanium tetrachloride first inlet 2, a titanium tetrachloride second inlet 3, and a reaction zone 4.
Wherein the titanium tetrachloride first inlet 2 comprises a plurality of holes circumferentially provided on the housing 1, the titanium tetrachloride second inlet 3 is axially spaced a predetermined distance from the titanium tetrachloride first inlet 2, and the titanium tetrachloride second inlet 3 comprises an air inlet ring provided at the periphery of the hollow housing 1.
The device is provided with a plurality of small holes at a preset distance on the upstream of a titanium tetrachloride gas inlet ring, titanium tetrachloride enters an oxygen fluid area through a porous inlet, a small amount of titanium tetrachloride is dispersed and reacts in a large amount of oxygen environment to form discrete crystal grains, and the concentration of titanium tetrachloride is small, and after crystal nuclei are formed, enough titanium tetrachloride is not supplied to surface chemical reaction, so that the formed fine titanium dioxide crystal grains are in a discrete state in oxygen. When the titanium tetrachloride at the annular inlet enters the reaction zone, discrete titanium dioxide crystal grains are used as seed crystals, so that the titanium tetrachloride is promoted to react on the surface of the seed crystals in an attaching way and grow up rapidly, and nano-scale rutile titanium white can be obtained.
Due to TiC1 4 And high temperature O 2 Is a rapid reaction on the order of one millisecond, and therefore thorough mixing of the reactants has a very important influence on the particle size distribution of the product. For this purpose, the number, size, jet angle, the amount of the added titanium tetrachloride and the distance between the added titanium tetrachloride and the second titanium tetrachloride inlet 3 need to be comprehensively controlled.
Since the titanium tetrachloride fed at the titanium tetrachloride first inlet 2 is mainly used for generating seed crystals and is intended to make the seed crystals discretely distributed, only a small amount of titanium tetrachloride is fed thereto, and it is ensured that the titanium tetrachloride is dispersed in an oxygen atmosphere as uniformly as possible and that a temperature gradient and a concentration gradient are not caused in an oxygen flow as much as possible so as to avoid aggregation and non-uniformity of crystal grains. For this purpose, as shown in fig. 3, in the apparatus of the present invention, the ratio of the hole spacing of adjacent holes of the titanium tetrachloride first inlet to the diameter of the hollow shell is controlled to be 0.12 to 0.35:1, the diameter of the holes is set to be 1-3 mm, the number of the holes is 9-28, and the extending direction of the holes is parallel to the radial direction of the shell so as to enable titanium tetrachloride to be projected in the radial direction. The axial distance between the second inlet 3 of titanium tetrachloride and the first inlet 2 of titanium tetrachloride may be set to 50 to 200mm.
Further, the oxygen inlet may be provided at a central position of the end face of the housing 1. The inlet ring may comprise an annular body coaxially fixed to the outer surface of the casing 1, the annular body defining a hollow flow-straightening chamber. The outer wall of the annular body is provided with a titanium tetrachloride feed port through which a substantial portion of the titanium tetrachloride is projected to the reaction zone. The annular main body is also provided with a flow guide slit for communicating the rectifying chamber with an oxygen channel in the shell, and the width of the flow guide slit is 15-80 mm.
The invention also provides a method for producing the micron-sized rutile titanium white, which generally comprises the following steps:
supplying the combusted high temperature oxygen to an oxygen inlet of the device;
titanium tetrachloride accounting for 5% -20% of the total feeding amount is supplied into a shell of the device through a titanium tetrachloride first inlet;
supplying the remainder of the titanium tetrachloride to the housing of the apparatus via a titanium tetrachloride second inlet;
and collecting the generated micron-sized rutile titanium white particles.
In some embodiments, the momentum ratio of the titanium tetrachloride to the axial oxygen fed through the titanium tetrachloride first inlet 2 is 3-7 to ensure that the titanium tetrachloride can stably enter the main fluid to a certain depth, and discrete fine titanium dioxide grains are generated under the condition of excessive oxygen. The momentum ratio of the titanium tetrachloride put in through the second titanium tetrachloride inlet 3 to the axial oxygen is 1.2-4.0, so that the titanium tetrachloride can enter the oxygen, and a large amount of reflux eddies can not be formed behind the slit, thereby preventing deterioration of flow field stability and wall sticking effect of titanium dioxide, and after the titanium tetrachloride enters the main fluid, the titanium tetrachloride enters the main fluid and undergoes surface adsorption and surface chemical reaction with fine grains in the oxygen, so that the titanium dioxide grains grow rapidly.
In the device, titanium tetrachloride enters through two inlets, the proportion of front-end small-hole titanium tetrachloride to the total titanium tetrachloride feeding amount is small, and the proportion of the front-end small-hole titanium tetrachloride to the total oxygen amount is also small, so that the titanium tetrachloride of the first inlet can be well dispersed in oxygen, and meanwhile, discrete fine titanium dioxide grains are generated, and the grains serve as seed crystals for oxidizing titanium tetrachloride of the second inlet, so that micron-sized large particles are rapidly generated through surface chemical reaction, and the particle size distribution range of a product is reduced.
The invention is further described below in connection with a specific production example.
The diameter of the device for producing the micron-sized rutile titanium white is 200mm, the first inlet of titanium tetrachloride is a porous inlet, the diameter of small holes is 2mm, the number of the small holes is 20, and the small hole inlets are vertical to the surface of the straight pipe; the second inlet is an annular slit inlet, and the slit width is 19mm; the titanium tetrachloride first porous inlet was 100mm from the second annular slot inlet. The proportion of titanium tetrachloride put in by the front end small hole inlet is 15% of the total titanium tetrachloride feeding amount, the momentum ratio of titanium tetrachloride put in by the small hole of the titanium tetrachloride first inlet to axial oxygen is 5, so that titanium tetrachloride can stably enter the main fluid to a certain depth, discrete fine titanium dioxide grains are generated under the condition of excessive oxygen, the momentum ratio of titanium tetrachloride put in by the second inlet to axial oxygen is 2.0, and generated titanium dioxide particles are collected. The oxidized product particle size D50 was measured to be 0.45 microns, D10 0.25 microns, and D90 0.8 microns.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (10)
1. An apparatus for producing micron-sized rutile titanium dioxide, comprising:
a hollow housing extending in an axial direction;
an oxygen inlet arranged at one end of the shell;
a titanium tetrachloride first inlet comprising a plurality of holes circumferentially disposed on the housing;
a titanium tetrachloride second inlet axially spaced a predetermined distance from the titanium tetrachloride first inlet and including an air intake ring disposed about the periphery of the hollow housing.
2. The apparatus of claim 1, wherein the oxygen inlet is disposed at a central location of an end face of the housing.
3. The apparatus of claim 1, wherein the diameter of the aperture of the titanium tetrachloride first inlet is 1 to 3mm.
4. The apparatus of claim 3 wherein the number of apertures of the titanium tetrachloride first inlet is 9 to 28.
5. The apparatus of claim 1, wherein the aperture of the titanium tetrachloride first inlet extends in a radial direction.
6. The apparatus of claim 1, wherein the air intake ring comprises:
the annular main body is coaxially fixed on the outer surface of the shell, the annular main body defines a hollow rectifying chamber, the outer wall of the annular main body is provided with a titanium tetrachloride feeding port, the annular main body is also provided with a flow guide slit for communicating the rectifying chamber with an oxygen channel in the shell, and the width of the flow guide slit is 15-80 mm.
7. The apparatus of claim 1 wherein the second inlet of titanium tetrachloride is axially spaced from the first inlet of titanium tetrachloride by a distance of 50 to 200mm.
8. The apparatus of claim 1, wherein the ratio of the hole spacing of adjacent holes of the titanium tetrachloride first inlet to the diameter of the hollow shell is from 0.12 to 0.35:1.
9. a method for producing micro-scale rutile titanium dioxide using the apparatus of any of claims 1-8, comprising the steps of:
supplying the combusted high temperature oxygen to an oxygen inlet of the device;
titanium tetrachloride accounting for 5% -20% of the total feeding amount is supplied into the shell of the device through a titanium tetrachloride first inlet;
supplying the remainder of the titanium tetrachloride to the housing of the apparatus via a titanium tetrachloride second inlet;
and collecting the generated micron-sized rutile titanium white particles.
10. The method of claim 9 wherein the momentum ratio of titanium tetrachloride to axial oxygen fed through the titanium tetrachloride first inlet is from 3 to 7 and the momentum ratio of titanium tetrachloride to axial oxygen fed through the titanium tetrachloride second inlet is from 1.2 to 4.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311510881.7A CN117398959A (en) | 2023-11-14 | 2023-11-14 | Device and method for producing micron-sized rutile titanium white |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311510881.7A CN117398959A (en) | 2023-11-14 | 2023-11-14 | Device and method for producing micron-sized rutile titanium white |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117398959A true CN117398959A (en) | 2024-01-16 |
Family
ID=89492467
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311510881.7A Pending CN117398959A (en) | 2023-11-14 | 2023-11-14 | Device and method for producing micron-sized rutile titanium white |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117398959A (en) |
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2023
- 2023-11-14 CN CN202311510881.7A patent/CN117398959A/en active Pending
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