CN115406185A - Titanium tetrachloride slurry drying system and method - Google Patents
Titanium tetrachloride slurry drying system and method Download PDFInfo
- Publication number
- CN115406185A CN115406185A CN202211031254.0A CN202211031254A CN115406185A CN 115406185 A CN115406185 A CN 115406185A CN 202211031254 A CN202211031254 A CN 202211031254A CN 115406185 A CN115406185 A CN 115406185A
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- titanium tetrachloride
- drying
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B3/00—Drying solid materials or objects by processes involving the application of heat
- F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
- F26B3/06—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour flowing through the materials or objects to be dried
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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
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/005—Drying-steam generating means
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/14—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects using gases or vapours other than air or steam, e.g. inert gases
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/005—Treatment of dryer exhaust gases
- F26B25/007—Dust filtering; Exhaust dust filters
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28B—STEAM OR VAPOUR CONDENSERS
- F28B3/00—Condensers in which the steam or vapour comes into direct contact with the cooling medium
- F28B3/04—Condensers in which the steam or vapour comes into direct contact with the cooling medium by injecting cooling liquid into the steam or vapour
Abstract
The invention discloses a titanium tetrachloride mud drying system and a method. The drying system includes: the top of the drying device is provided with a titanium tetrachloride slurry inlet and a mixed gas outlet, and the bottom of the drying device is provided with a titanium tetrachloride vapor inlet; the inlet of the gas-solid separation device is connected with the mixed gas outlet; the solid collecting device is connected with the solid outlet of the gas-solid separating device; the inlet of a condensate to be condensed of the spraying and condensing device is connected with the gas outlet of the gas-solid separation device; the inlet of the titanium tetrachloride storage device is connected with the condensate outlet of the spraying and condensing device; the inlet of the object to be heated of the heat exchange device is connected with the outlet of the titanium tetrachloride storage device, and the heated object outlet of the heat exchange device is connected with the titanium tetrachloride steam inlet. The invention can improve the drying effect and effectively recover the titanium tetrachloride in the slurry.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a titanium tetrachloride mud drying system and method.
Background
The existing method for producing titanium tetrachloride is mainly a boiling chlorination method, namely a method for enriching TiO 2 After mixing the titanium raw material and the petroleum coke according to a certain proportion, adding chlorine gas to carry out closed chemical reaction in a chlorination furnace, wherein the reaction temperature is generally more than 900 ℃, obtaining titanium tetrachloride after the reaction is finished, and obtaining slurry containing the titanium tetrachloride and crude titanium tetrachloride by spray condensation and treatment of a thickener. Wherein the titanium tetrachloride slurry approximately accounts for TiCl produced by the chlorination furnace 4 3-8 wt% of the total amount of the liquid. The titanium tetrachloride slurry contains 40 to 65wt% of TiCl in addition to the high-boiling metal chloride 4 。
The titanium tetrachloride slurry contains a large amount of metal oxychloride with high viscosity, poor heat conductivity and strong adhesive force, and TiCl is added 4 The titanium tetrachloride precipitate mud has special properties, and the strong hydrolysis of air or water generates a large amount of white smoke, releases heat, seriously corrodes equipment and causes difficult treatment of the titanium tetrachloride precipitate mud.
The prior art method for treating titanium tetrachloride slurry comprises the following steps: the slurry returns to the chlorination furnace, is dried in a rotary kiln, centrifugally dried, dried by microwave, directly hydrolyzed and the like. The mud is returned to the chlorination furnace, although partial titanium tetrachloride can be recovered, the excessive mud can influence the furnace condition of the fluidized bed furnace; the rotary kiln is difficult to dry and seal, and the working environment is poor; the titanium tetrachloride is not thoroughly removed by centrifugal drying, and the equipment is difficult to operate for a long time; microwave treatment on TiCl 4 The penetration depth in the precipitated slurry is limited, and the evaporation efficiency of titanium tetrachloride is not high; direct hydrolysis leads to large amounts of TiCl 4 Loss and large environmental protection pressure.
Disclosure of Invention
The invention mainly aims to provide a titanium tetrachloride mud drying system and a method, which aim to solve the problems of incomplete drying of titanium tetrachloride mud and low drying efficiency in the prior art.
According to one aspect of the invention, a titanium tetrachloride mud drying system is provided, comprising: the drying device is provided with a titanium tetrachloride slurry inlet and a mixed gas outlet at the top, and a titanium tetrachloride vapor inlet is formed at the bottom; the inlet of the gas-solid separation device is connected with the mixed gas outlet; the solid collecting device is connected with the solid outlet of the gas-solid separation device; the inlet of condensate to be condensed of the spraying and condensing device is connected with the gas outlet of the gas-solid separation device; the inlet of the titanium tetrachloride storage device is connected with the condensate outlet of the spray condensing device; and the inlet of the object to be heated of the heat exchange device is connected with the outlet of the titanium tetrachloride storage device, and the heated object outlet of the heat exchange device is connected with the titanium tetrachloride vapor inlet.
According to one embodiment of the present invention, the titanium tetrachloride vapor inlet is provided in plural number, and the plural titanium tetrachloride vapor inlets are arranged uniformly along the circumference.
According to one embodiment of the invention, the gas-solid separation device is one or more of a sedimentation separation device, a cyclone dust collection device and a cloth bag dust collection device.
According to one embodiment of the invention, the spray condensing device adopts titanium tetrachloride liquid with the temperature lower than 0 ℃ as the spray liquid.
According to an embodiment of the invention, the drying system further comprises: and the hopper car is arranged below the drying device.
According to another aspect of the invention, there is provided a method of drying a carbon tetrachloride slurry, comprising: enabling titanium tetrachloride vapor and titanium tetrachloride slurry to enter a drying device from the bottom and the top of the drying device respectively, and drying the titanium tetrachloride slurry by using the titanium tetrachloride vapor to obtain mixed gas; carrying out gas-solid separation on the mixed gas to obtain a gas product and a solid product; spraying and condensing the gas product to obtain titanium tetrachloride liquid; heating the titanium tetrachloride liquid to obtain the titanium tetrachloride vapor for drying titanium tetrachloride slurry.
According to one embodiment of the present invention, the titanium tetrachloride vapor is allowed to enter the drying device at an inlet pressure of 0.05 to 0.2Mpa and a temperature of 150 to 400 ℃.
According to one embodiment of the invention, the outlet temperature of the mixed gas leaving the drying device is 140-250 ℃.
According to one embodiment of the invention, the gaseous products are sprayed with a titanium tetrachloride liquid having a temperature below 0 ℃.
According to one embodiment of the invention, the speed of the titanium tetrachloride slurry entering the drying device is 3-20kg/h.
According to the titanium tetrachloride mud drying system and the method provided by the embodiment of the invention, titanium tetrachloride vapor is adopted to dry titanium tetrachloride mud, the titanium tetrachloride vapor and the titanium tetrachloride mud are reversely met in the drying device, the heat exchange efficiency is high, the mud drying speed is high, and the titanium tetrachloride recovery rate is high.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 shows a schematic view of a titanium tetrachloride mud drying system according to an embodiment of the present invention;
fig. 2 shows a flow diagram of a method for drying titanium tetrachloride slurry according to an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
Fig. 1 shows a schematic view of a titanium tetrachloride mud drying system 100 according to an embodiment of the invention. As shown in fig. 1, the drying system 100 includes: the drying device 10 is provided with a titanium tetrachloride slurry inlet 12 and a mixed gas outlet 14 at the top of the drying device 10, and a titanium tetrachloride vapor inlet 16 at the bottom of the drying device 10; the inlet 22 of the gas-solid separation device 20 is connected with the mixed gas outlet 14; a solids collection device 30 connected to the solids outlet 24 of the gas-solids separation device 20; the spraying and condensing device 40, wherein an inlet 42 of the spraying and condensing device 40 to be condensed is connected with the gas outlet 26 of the gas-solid separation device 20; a titanium tetrachloride storage device 50, wherein the inlet 52 of the titanium tetrachloride storage device 50 is connected with the condensate outlet 44 of the spray condensing device 40; a heat exchanging device 60, wherein an inlet 62 of the heat exchanging device 60 for the object to be heated is connected with the outlet 54 of the titanium tetrachloride storage device 50, and an outlet 64 of the heat exchanging device 60 for the heated object is connected with the titanium tetrachloride vapor inlet 16.
Titanium tetrachloride vapor is introduced from the bottom of the drying device 10 and meets titanium tetrachloride slurry added from the top of the drying device 10, the titanium tetrachloride vapor and the titanium tetrachloride slurry are subjected to heat exchange, the titanium tetrachloride in the slurry is rapidly gasified to obtain mixed gas containing titanium tetrachloride vapor and dust, the mixed gas leaves from the top of the drying device 10 and is further subjected to gas-solid separation by a gas-solid separation device 20 to obtain dried products and titanium tetrachloride vapor, the newly generated titanium tetrachloride vapor is collected by a spray condensing device 40, and the dried products enter a solid collecting device 30.
The titanium tetrachloride vapor is adopted to dry the titanium tetrachloride slurry, and the titanium tetrachloride slurry and the titanium tetrachloride vapor meet in opposite directions, so that the heat exchange efficiency is high, and the slurry drying speed is high; the titanium tetrachloride content in the solid obtained by drying the slurry is less than 4wt%, and the drying effect is good; the titanium tetrachloride mud drying can be finished in a closed system, and the environment is friendly; the titanium tetrachloride vapor can also avoid introducing new impurities, and the titanium tetrachloride vapor can be obtained by heating titanium tetrachloride condensate obtained by condensation, so that the cyclic utilization is realized.
The number of titanium tetrachloride vapor inlets 16 may be one or more, and for example, may be 1 to 4. If the number of titanium tetrachloride vapor inlets 16 is plural, the plural titanium tetrachloride vapor inlets 16 are arranged uniformly along the circumference, ensuring uniform introduction and distribution of titanium tetrachloride vapor into the drying device 10.
The drying system 100 may further include: and a hopper car 70 disposed under the drying device 10 for collecting the substances dropped from the drying device 10. For example, some solids are heavier and do not exit the top of the dryer 10 with the mixed gas, but fall from the bottom of the dryer 10.
The gas-solid separation device 20 can be one or more of a sedimentation separation device, a cyclone dust collection device and a cloth bag dust collection device.
The spray condensing device 40 adopts titanium tetrachloride liquid with the temperature lower than 0 ℃ as spray liquid. Thus, good spraying and trapping effects can be ensured and the introduction of impurities can be avoided.
Fig. 2 shows a flow diagram of a method for drying titanium tetrachloride slurry according to an embodiment of the invention. As shown in fig. 2, the drying method includes:
s1, allowing titanium tetrachloride vapor and titanium tetrachloride slurry to enter a drying device from the bottom and the top of the drying device respectively, and drying the titanium tetrachloride slurry by using the titanium tetrachloride vapor to obtain mixed gas;
s2, carrying out gas-solid separation on the mixed gas to obtain a gas product and a solid product;
s3, spraying and condensing the gas product to obtain titanium tetrachloride liquid;
and S4, heating the titanium tetrachloride liquid to obtain the titanium tetrachloride vapor for drying titanium tetrachloride mud.
In some embodiments, the titanium tetrachloride vapor is introduced into the drying apparatus at an inlet pressure of 0.05 to 0.2Mpa and a temperature of 150 to 400 ℃. So that the speed of the titanium tetrachloride mud entering the drying device is 3-20kg/h. Thereby ensuring the efficient heat exchange effect between the titanium tetrachloride vapor and the titanium tetrachloride slurry and being beneficial to the rapid drying of the slurry.
In some embodiments, the exit temperature of the mixed gas from the drying device is 140 to 250 ℃ to avoid recondensation of the titanium tetrachloride vapor obtained by drying.
In some embodiments, the gaseous product is sprayed with titanium tetrachloride liquid at a temperature below 0 ℃ to ensure good spray capture and avoid the introduction of impurities
The method has the advantages of high drying efficiency, high titanium tetrachloride recovery rate, good drying effect, closed system, environmental friendliness and the like, can avoid environmental pollution caused by hydrolysis of titanium tetrachloride, improves the recovery rate of valuable metals such as titanium and the like, and reduces the production cost.
The following description is based on specific examples.
Example 1
The titanium tetrachloride mud drying system provided by the invention is used for carrying out a drying test on titanium tetrachloride mud, wherein two titanium tetrachloride steam inlets are symmetrically arranged at the center of the circle at the bottom of the drying device, and the titanium tetrachloride mud contains 42.6% of titanium tetrachloride according to the weight percentage.
Adding titanium tetrachloride slurry from the top of the drying device at a rate of 3kg/h; titanium tetrachloride vapor enters from the bottom of the drying device, the inlet pressure is 0.05-0.1 Mpa, and the temperature is 160-200 ℃; the outlet temperature of the mixed gas is 140-160 ℃. Collecting dust in the mixed gas by cyclone, and spraying and condensing the mixed gas by liquid titanium tetrachloride at the temperature of-4 ℃ after dust collection.
At the end of the test, the titanium tetrachloride content in the dried product of titanium tetrachloride slurry was found to be 3.9% by weight.
Example 2
The titanium tetrachloride mud drying system is adopted to carry out a drying test on the titanium tetrachloride mud, wherein two titanium tetrachloride steam inlets are symmetrically arranged at the center of the circle at the bottom of a drying device, and the titanium tetrachloride mud contains 51.5 percent by weight of titanium tetrachloride.
Titanium tetrachloride slurry is added from the top of the drying device at a rate of 9kg/h; titanium tetrachloride steam enters from the bottom of the drying device, the inlet pressure is 0.1-0.15 Mpa, and the temperature is 200-300 ℃; the outlet temperature of the mixed gas is 140-200 ℃. Collecting dust in the mixed gas by cyclone, and spraying and condensing the mixed gas by liquid titanium tetrachloride at the temperature of-4 ℃ after dust collection.
The titanium tetrachloride content in the dried product of titanium tetrachloride slurry was 3.1% by weight as measured at the end of the test.
Example 3
The titanium tetrachloride mud drying system provided by the invention is used for carrying out a drying test on titanium tetrachloride mud, wherein two titanium tetrachloride steam inlets are symmetrically arranged at the center of the circle at the bottom of the drying device, and the titanium tetrachloride mud contains 61.3% of titanium tetrachloride according to the weight percentage.
Adding titanium tetrachloride slurry from the top of the drying device at a speed of 20kg/h; titanium tetrachloride vapor enters from the bottom of the drying device, the inlet pressure is 0.15-0.2 Mpa, and the temperature is 350-400 ℃; the outlet temperature of the mixed gas is 180-250 ℃. Collecting dust in the mixed gas by cyclone, and spraying and condensing the mixed gas by liquid titanium tetrachloride at the temperature of-4 ℃ after dust collection.
The titanium tetrachloride content in the dried product of titanium tetrachloride slurry was 2.1% by weight as measured at the end of the test.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to these examples; within the idea of an embodiment of the invention, also technical features in the above embodiment or in different embodiments may be combined and there are many other variations of the different aspects of an embodiment of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of the embodiments of the present invention are intended to be included within the scope of the embodiments of the present invention.
Claims (10)
1. A titanium tetrachloride mud drying system is characterized by comprising:
the device comprises a drying device, a gas-liquid separator and a gas-liquid separator, wherein the top of the drying device is provided with a titanium tetrachloride slurry inlet and a mixed gas outlet, and the bottom of the drying device is provided with a titanium tetrachloride vapor inlet;
the inlet of the gas-solid separation device is connected with the mixed gas outlet;
the solid collecting device is connected with the solid outlet of the gas-solid separation device;
the inlet of condensate to be condensed of the spraying and condensing device is connected with the gas outlet of the gas-solid separation device;
the inlet of the titanium tetrachloride storage device is connected with the condensate outlet of the spray condensing device;
and the inlet of the object to be heated of the heat exchange device is connected with the outlet of the titanium tetrachloride storage device, and the heated object outlet of the heat exchange device is connected with the titanium tetrachloride vapor inlet.
2. The system according to claim 1, wherein the titanium tetrachloride vapor inlet is plural in number, and the plural titanium tetrachloride vapor inlets are uniformly arranged along a circumference.
3. The system of claim 1, wherein the gas-solid separation device is one or more of a sedimentation separation device, a cyclone dust collection device and a cloth bag dust collection device.
4. The system of claim 1, wherein the spray condensing means employs titanium tetrachloride liquid having a temperature of less than 0 ℃ as the spray.
5. The system of claim 1, further comprising: and the hopper car is arranged below the drying device.
6. A method for drying carbon tetrachloride mud is characterized by comprising the following steps:
enabling titanium tetrachloride vapor and titanium tetrachloride slurry to enter a drying device from the bottom and the top of the drying device respectively, and drying the titanium tetrachloride slurry by using the titanium tetrachloride vapor to obtain mixed gas;
carrying out gas-solid separation on the mixed gas to obtain a gas product and a solid product;
spraying and condensing the gas product to obtain titanium tetrachloride liquid;
heating the titanium tetrachloride liquid to obtain the titanium tetrachloride vapor for drying titanium tetrachloride slurry.
7. The method according to claim 6, wherein the titanium tetrachloride vapor is allowed to enter the drying device at an inlet pressure of 0.05 to 0.2Mpa and a temperature of 150 to 400 ℃.
8. The method of claim 6, wherein the exit temperature of the mixed gas as it exits the drying device is 140-250 ℃.
9. The method of claim 6, wherein the gaseous product is sprayed with a titanium tetrachloride liquid having a temperature below 0 ℃.
10. The method according to claim 6, characterized in that the speed of bringing the titanium tetrachloride slurry into the drying apparatus is 3-20kg/h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211031254.0A CN115406185A (en) | 2022-08-26 | 2022-08-26 | Titanium tetrachloride slurry drying system and method |
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| CN202211031254.0A CN115406185A (en) | 2022-08-26 | 2022-08-26 | Titanium tetrachloride slurry drying system and method |
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Citations (11)
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| GB789552A (en) * | 1954-11-26 | 1958-01-22 | Farbriques De Prod Chim De Tha | Recovery of titanium tetrachloride from chlorination gases |
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| CN102092783A (en) * | 2010-12-31 | 2011-06-15 | 遵义钛业股份有限公司 | Drying method of titanium tetrachloride settling mud |
| CN102502805A (en) * | 2011-12-12 | 2012-06-20 | 中南大学 | Method for drying titanium tetrachloride precipitate sludge using molten salts |
| CN202482083U (en) * | 2011-11-01 | 2012-10-10 | 成都易态科技有限公司 | Titanium tetrachloride production system |
| CN103145179A (en) * | 2013-03-22 | 2013-06-12 | 中南大学 | Method for recovering TiCl4 from titanium tetrachloride precipitation slurry |
| CN203238052U (en) * | 2013-02-05 | 2013-10-16 | 仙桃市中星电子材料有限公司 | Device for continuously removing vanadium and discharging residue during titanium tetrachloride production |
| CN103615868A (en) * | 2013-03-12 | 2014-03-05 | 中航天赫（唐山）钛业有限公司 | Copper wire ball forced convection drying method and device |
| EP3156370A1 (en) * | 2015-10-16 | 2017-04-19 | Kronos International, Inc. | Method for the separation of valuable metal chlorides from residues from production of titanium dioxide (chloride processes) |
| CN209242698U (en) * | 2018-10-22 | 2019-08-13 | 河南龙兴钛业科技股份有限公司 | A kind of equipment recycling titanium tetrachloride from chlorination mud |
| CN112062151A (en) * | 2020-09-01 | 2020-12-11 | 洛阳双瑞万基钛业有限公司 | Titanium tetrachloride slurry drying device and drying method |
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2022
- 2022-08-26 CN CN202211031254.0A patent/CN115406185A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB789552A (en) * | 1954-11-26 | 1958-01-22 | Farbriques De Prod Chim De Tha | Recovery of titanium tetrachloride from chlorination gases |
| CN1605824A (en) * | 2003-10-08 | 2005-04-13 | 曾维兴 | Drying and pulverizing process for preparing powder material with high dispersibility |
| CN102092783A (en) * | 2010-12-31 | 2011-06-15 | 遵义钛业股份有限公司 | Drying method of titanium tetrachloride settling mud |
| CN202482083U (en) * | 2011-11-01 | 2012-10-10 | 成都易态科技有限公司 | Titanium tetrachloride production system |
| CN102502805A (en) * | 2011-12-12 | 2012-06-20 | 中南大学 | Method for drying titanium tetrachloride precipitate sludge using molten salts |
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| CN103615868A (en) * | 2013-03-12 | 2014-03-05 | 中航天赫（唐山）钛业有限公司 | Copper wire ball forced convection drying method and device |
| CN103145179A (en) * | 2013-03-22 | 2013-06-12 | 中南大学 | Method for recovering TiCl4 from titanium tetrachloride precipitation slurry |
| EP3156370A1 (en) * | 2015-10-16 | 2017-04-19 | Kronos International, Inc. | Method for the separation of valuable metal chlorides from residues from production of titanium dioxide (chloride processes) |
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