CN102092783A - Drying method of titanium tetrachloride settling mud - Google Patents
Drying method of titanium tetrachloride settling mud Download PDFInfo
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- CN102092783A CN102092783A CN 201010616681 CN201010616681A CN102092783A CN 102092783 A CN102092783 A CN 102092783A CN 201010616681 CN201010616681 CN 201010616681 CN 201010616681 A CN201010616681 A CN 201010616681A CN 102092783 A CN102092783 A CN 102092783A
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- ticl
- titanium tetrachloride
- mud
- drying
- spray
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Abstract
The invention relates to a drying method of titanium tetrachloride settling mud. The technical process comprises three main steps, namely spray drying, gas-solid separation and TiCl4 recycling. The method comprises the following specific steps: performing spray drying to titanium tetrachloride settling mud to form mixed gas, dedusting the mixed gas, performing forced cooling to recycle TiCl4, sending the heat-carrying gas back to the spray drying step for reuse after recycling. The method of the invention has the advantages of good drying effect, high TiCl4 recovery rate, sealed system, environmental friend and the like.
Description
Technical field
The present invention relates to a kind of titanium tetrachloride precipitation mud drying means.
Background technology
Rich titanium material adds the TiCl that the carbon reduction chlorination obtains
4Can separate out red solid sediment by nature in the liquid, i.e. titanium tetrachloride precipitation mud.Titanium tetrachloride precipitation mud accounts for the TiCl of chlorination furnace output
4The 3-5wt% of total amount of liquid.Remove high boiling metal chloride in the titanium tetrachloride precipitation mud, and outside the solidss such as oxychloride of titanium and other metals, also contain the TiCl of 55-65wt%
4In order to reclaim the titanium tetrachloride in the precipitation mud, manufacturing enterprise and scientific research institution carried out a large amount of research and trial, comprising: precipitation mud turns back to boiling chloridizing furnace, precipitation mud adds dividing plate dust-precipitator inner drying, rotary kiln drying, centrifugal drying, microwave drying etc.Though mud adds energy recovery part titanium tetrachloride in the chlorination furnace, the working of a furnace that mud adds the back fluidizing furnace is had a strong impact on.Though temperature is up to 400-500 ℃ in the dividing plate dust-precipitator, the specific surface area of mud is little, and it is short that mud adds the back heat exchanger time, the TiCl in the mud
4Have little time to volatilize and just be deposited in the bottom of dust-precipitator.Experiment showed, TiCl
4Precipitation mud adopts rotary kiln drying or centrifugal drying also unsuccessful.Though the TiCl in the microwave energy rapid heating volatilization mud
4, but microwave is at TiCl
4Penetration depth in the precipitation mud is very limited, thereby has limited TiCl
4The industrial application of precipitation mud microwave drying.
Why difficult titanium tetrachloride precipitation mud is, is not only because TiCl
4Character is special, see air or meet the water intense hydrolysis, Mao Baiyan, and emit a large amount of heat, serious to equipment corrosion, and be contain in the titanium tetrachloride mud precipitation slurry that viscosity is big, the metal oxychloride of poor thermal conductivity, strong adhesion.
TiCl
4+H
2O＝Ti(OH)Cl
3+HCl↑
TiCl
4+2H
2O＝Ti(OH)
2Cl
2+2HCl↑
TiCl
4+3H
2O＝Ti(OH)
3Cl+3HCl↑
TiCl
4+2H
2O＝TiO
2+4HCl↑
On the industrial production, precipitate the TiCl in the mud at present
4Also can't reclaim, the mode that generally adopts water to dash is handled, and this not only causes a large amount of TiCl
4Lose and cause heavy environmental protection pressure.
Summary of the invention
The objective of the invention is to reclaim the TiCl in the titanium tetrachloride precipitation mud
4, avoid because of TiCl
4The environmental pollution that hydrolysis causes, the protection environment, the rate of recovery of valuable metals such as raising Ti reduces production costs, and the invention provides a kind of titanium tetrachloride precipitation mud drying means.
Technical scheme of the present invention is:
Technological process comprises spraying drying, gas solid separation and TiCl
4Reclaim: earlier titanium tetrachloride is precipitated mud and add in the centrifugal atomizer in the spray chamber and atomize, the TiCl wherein that in the heat-carrying air-flow, forces to volatilize of the precipitation mud after the atomizing
4, obtain containing TiCl
4The mixed gas of steam and dust cools off the TiCl that reclaims wherein through pressure after the mixed gas dedusting again
4, reclaim TiCl
4Back heat-carrying gas returns spraying drying and recycles.
Titanium tetrachloride precipitation mud rotating speed is the centrifugal atomizer spraying of 5000～25000r/min.
Enter the dry-heat air intake pressure 0.05～0.25Mpa of titanium tetrachloride precipitation mud spray chamber, inlet temperature is 250～450 ℃, 80～250 ℃ of mixed gas outlet temperature.
The used heat-carrying gas of titanium tetrachloride precipitation spray drying of slip is meant one or more in dry air behind the dehumidification, nitrogen, the argon gas.
That the mixed gas that titanium tetrachloride precipitation spray drying of slip forms adopts is settlement separate, one or more method dedustings in the cyclone dust collection, bag collection.
The TiCl that titanium tetrachloride precipitation spray drying of slip forms
4Steam is with 0～-15 ℃ of liquid TiCl
4Spray captures the TiCl that reclaims wherein
4, TiCl
4Recovery back heat-carrying gas returns spraying drying and recycles.
The present invention compares with existing technology and has the following advantages and effect:
1, titanium tetrachloride precipitation spray drying of slip, TiCl
4Evaporation rate is fast, TiCl in the solids that the mud drying obtains
4Content is less than 5wt%, and drying effect is good.
2, the TiCl of titanium tetrachloride precipitation spray drying of slip formation
4Steam reclaims fully through forcing cooling, and is good in economic efficiency.
3. titanium tetrachloride precipitation spray drying of slip, and TiCl
4Be recovered in the closed system and finish, do not produce pollution, environmental friendliness.
4, in the dust that obtains of titanium tetrachloride precipitation spray drying of slip enrichment other valuable metals, help comprehensive recovery.
Embodiment
Below in conjunction with embodiment, the present invention is further described, following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1
Stir and add chlorination furnace thickener TiCl
4Precipitation mud 15kg to rotating speed be 8000r/min centrifugal atomizer internal spraying, make the dry heat-carrying gas of using with argon gas, intake pressure 0.07～the 0.11Mpa of spray chamber dry-heat air, the hot blast inlet temperature is 250～300 ℃, 80～120 ℃ of mixed gas outlet temperature, the mixed gas that spray drying of slip forms adopts cyclone dust collection, and the back mixed gas temperature of gathering dust is-5 ℃ of liquid TiCl
4Spray reclaims TiCl wherein
4The titanium tetrachloride precipitation spray-dired experimental result of mud (wt%) is as follows:
| TiCl 4 | Fe | Cl | Al | Si | Zr | Nb | |
| Mud | 63.21 | -- | -- | -- | -- | -- | -- |
| Dried slag | 3.58 | 4.89 | 25.14 | 4.07 | 0.21 | 1.53 | 1.21 |
Embodiment 2
Stir and add chlorination furnace thickener TiCl
4Precipitation mud 450kg to rotating speed be 12000r/min centrifugal atomizer internal spraying, make the dry heat-carrying gas of using with nitrogen, intake pressure 0.08～the 0.14Mpa of spray chamber dry-heat air, the hot blast inlet temperature is 260～350 ℃, 110～150 ℃ of mixed gas outlet temperature, bag collection after the mixed gas elder generation cyclone dust collection that spray drying of slip forms, the back mixed gas temperature of gathering dust is-10 ℃ of liquid TiCl
4Spray reclaims TiCl wherein
4, tail gas returns spraying drying and recycles.The titanium tetrachloride precipitation spray-dired experimental result of mud (wt%) is as follows:
| TiCl 4 | Fe | Cl | Al | Si | Zr | Nb | |
| Mud | 60.35 | -- | -- | -- | -- | -- | -- |
| Dried slag | 2.01 | 5.03 | 26.27 | 3.89 | 0.26 | 1.48 | 1.30 |
Embodiment 3
Stir and add chlorination furnace thickener TiCl
4Precipitation mud 2360kg to rotating speed be 16000r/min centrifugal atomizer internal spraying, make dry heat-carrying gas with the dry air behind the dehumidification, intake pressure 0.10～the 0.20Mpa of spray chamber dry-heat air, the hot blast inlet temperature is 280～390 ℃, 115～230 ℃ of mixed gas outlet temperature, the mixed gas that spray drying of slip forms is sent into the sedimentation of chlorination furnace dividing plate dust-precipitator and is gathered dust, and enters the condensing tower temperature after gathering dust and is-12 ℃ of liquid TiCl
4Spray reclaims TiCl wherein
4The titanium tetrachloride precipitation spray-dired experimental result of mud (wt%) is as follows:
| TiCl 4 | Fe | Cl | Al | Si | Zr | Nb | |
| Mud | 59.86 | -- | -- | -- | -- | -- | -- |
| Dried slag | 3.15 | 3.16 | 31.48 | 1.25 | 0.11 | 0.45 | 0.36 |
Claims (3)
1. a titanium tetrachloride precipitation mud drying means is characterized in that technological process comprises spraying drying, gas solid separation and TiCl
4Reclaim; Earlier titanium tetrachloride is precipitated mud and add in the centrifugal atomizer in the spray chamber and atomize, the TiCl wherein that in the heat-carrying air-flow, forces to volatilize of the precipitation mud after the atomizing
4, obtain containing TiCl
4The mixed gas of steam and dust cools off the TiCl that reclaims wherein through pressure after the mixed gas dedusting again
4, TiCl
4Recovery back heat-carrying gas returns spraying drying and recycles;
The spray rotating speed of used centrifugal atomizer of titanium tetrachloride precipitation mud is 5000～25000r/min;
Enter the dry-heat air intake pressure 0.05～0.25Mpa of titanium tetrachloride precipitation mud spray chamber, 250～450 ℃ of inlet temperatures, 80～250 ℃ of mixed gas outlet temperature;
TiCl is reclaimed in described pressure cooling
4Be meant the TiCl that spraying forms
4Steam is with 0～-15 ℃ of liquid TiCl
4Spray captures and reclaims.
2. a kind of titanium tetrachloride precipitation mud drying means according to claim 1 is characterized in that, the used heat-carrying gas of titanium tetrachloride precipitation spray drying of slip is meant one or more in dry air behind the dehumidification, nitrogen, the argon gas.
3. a kind of titanium tetrachloride precipitation mud drying means according to claim 1 is characterized in that, that the mixed gas that titanium tetrachloride precipitation spray drying of slip forms adopts is settlement separate, one or more method dedustings in the cyclone dust collection, bag collection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010616681 CN102092783A (en) | 2010-12-31 | 2010-12-31 | Drying method of titanium tetrachloride settling mud |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010616681 CN102092783A (en) | 2010-12-31 | 2010-12-31 | Drying method of titanium tetrachloride settling mud |
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| CN102092783A true CN102092783A (en) | 2011-06-15 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502801A (en) * | 2011-11-01 | 2012-06-20 | 成都易态科技有限公司 | Method for processing mixed slurry in chloridizing metallurgy as well as production process and system for titanium tetrachloride |
| CN102743945A (en) * | 2012-07-04 | 2012-10-24 | 金川集团股份有限公司 | Treating process for furnace gas of chlorination furnace used for production of titanium tetrachloride |
| CN112875746A (en) * | 2021-01-11 | 2021-06-01 | 北京诺芯环境科技有限公司 | Resourceful treatment method of waste and application thereof |
| CN113666417A (en) * | 2021-09-13 | 2021-11-19 | 攀钢集团钒钛资源股份有限公司 | Vanadium-containing slurry separation method and device |
| CN115406185A (en) * | 2022-08-26 | 2022-11-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium tetrachloride slurry drying system and method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415547A (en) * | 2002-07-19 | 2003-05-07 | 锦州铁合金(集团)股份有限公司钛白粉厂 | Technique and method for treating titanium tetrachloride slurry containing vanadium |
| WO2008091773A1 (en) * | 2007-01-22 | 2008-07-31 | Materials & Electrochemical Research Corp. | Continuous production of titanium by the metallothermic reduction of ticl4 |
| CN101417813A (en) * | 2007-10-25 | 2009-04-29 | 贵阳铝镁设计研究院 | Recovery method and equipment of vanadium-containing slurry produced from titanic chloride refining process |
| CN201417070Y (en) * | 2009-06-01 | 2010-03-03 | 王利运 | Slurry/liquid material wetness decompression reboiling spraying drying device |
-
2010
- 2010-12-31 CN CN 201010616681 patent/CN102092783A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415547A (en) * | 2002-07-19 | 2003-05-07 | 锦州铁合金(集团)股份有限公司钛白粉厂 | Technique and method for treating titanium tetrachloride slurry containing vanadium |
| WO2008091773A1 (en) * | 2007-01-22 | 2008-07-31 | Materials & Electrochemical Research Corp. | Continuous production of titanium by the metallothermic reduction of ticl4 |
| CN101417813A (en) * | 2007-10-25 | 2009-04-29 | 贵阳铝镁设计研究院 | Recovery method and equipment of vanadium-containing slurry produced from titanic chloride refining process |
| CN201417070Y (en) * | 2009-06-01 | 2010-03-03 | 王利运 | Slurry/liquid material wetness decompression reboiling spraying drying device |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502801A (en) * | 2011-11-01 | 2012-06-20 | 成都易态科技有限公司 | Method for processing mixed slurry in chloridizing metallurgy as well as production process and system for titanium tetrachloride |
| CN102743945A (en) * | 2012-07-04 | 2012-10-24 | 金川集团股份有限公司 | Treating process for furnace gas of chlorination furnace used for production of titanium tetrachloride |
| CN112875746A (en) * | 2021-01-11 | 2021-06-01 | 北京诺芯环境科技有限公司 | Resourceful treatment method of waste and application thereof |
| CN113666417A (en) * | 2021-09-13 | 2021-11-19 | 攀钢集团钒钛资源股份有限公司 | Vanadium-containing slurry separation method and device |
| CN115406185A (en) * | 2022-08-26 | 2022-11-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium tetrachloride slurry drying system and method |
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Application publication date: 20110615 |