CN101691242A - Method and equipment for separating titanium tetrachloride from vanadium-containing mud - Google Patents
Method and equipment for separating titanium tetrachloride from vanadium-containing mud Download PDFInfo
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- CN101691242A CN101691242A CN200910167841A CN200910167841A CN101691242A CN 101691242 A CN101691242 A CN 101691242A CN 200910167841 A CN200910167841 A CN 200910167841A CN 200910167841 A CN200910167841 A CN 200910167841A CN 101691242 A CN101691242 A CN 101691242A
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- titanium tetrachloride
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- vanadium
- heat exchanger
- graphite heat
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Abstract
The invention discloses a method and equipment for separating titanium tetrachloride from vanadium-containing mud, which belong to the technical field of treating titanium tetrachloride vanadium-containing mud. The method and the equipment solve the problems that the heat transfer area is small in the prior method for treating the titanium tetrachloride vanadium-containing mud by using a heat source to heat the outer wall of a distillation kettle, dry slag formed nearby the heat transfer wall at the middle and final stages of distillation increases thermal resistance so as to cause difficult separation of the titanium tetrachloride in the vanadium-containing mud at the center part far from the heat transfer wall, and the utilization rate of heat energy in the distillation process is low. A graphite heat exchanger is soaked into the titanium tetrachloride vanadium-containing mud to absorb microwave, and the heat produced when the graphite heat exchanger absorbs the microwave is evenly transferred to the titanium tetrachloride vanadium-containing mud through the graphite heat exchanger so as to achieve the aim of efficiently separating the titanium tetrachloride from the vanadium-containing mud. The method and the equipment have the characteristics of high utilization rate of electrical energy and good separating effect of the titanium tetrachloride.
Description
Background technology
In the method that titanium tetrachloride is separated from contain vanadium mud, adopt the distillation method of traditional heat source heating to be confined to the still kettle wall because of heat-transfer surface, heat transfer area is little, in the middle and later periods that contains vanadium mud evaporative process, near because the dried slag of the preferential appearance heat conductive wall, cause thermal resistance to increase, make apart from the heat conductive wall titanium tetrachloride that contains in the vanadium mud far away to be difficult to be evaporated away.Therefore, there is the energy consumption height in this method, the limitation of titanium tetrachloride inferior separating effect.To contain vanadium mud and spray the into interior method of chlorination furnace, and the vanadium mud that will contain that CN1199863C announces sprays into first method of gathering dust condenser, because of existing vanadium in chlorination---the problem of refining system internal recycling enrichment, all be unwell to handle that the titanium tetrachloride refining step produces contain vanadium mud.What CN101413178A can be used to handle the titanium tetrachloride refining step contains vanadium mud, but contains in the vanadium mud VOCl in a small amount
2Sneaked in a large amount of slags that gathers dust, increased the difficulty that reclaims vanadium.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of from contain vanadium mud the method and apparatus of separating titanium tetrachloride, more specifically, provide and a kind ofly make thermal source, make microwave absorbing medium and heat-transfer medium with graphite heat exchanger, the method and apparatus of separating titanium tetrachloride from contain vanadium mud with microwave.
The titanium tetrachloride refining step removes the vanadium mud that contains that produces in the vanadium process and can be used for reclaiming vanadium, therefore, this part is contained vanadium mud adopt distillatory mode individual curing, and titanium tetrachloride is wherein thoroughly separated, and is beneficial to reclaim vanadium.Adopt the traditional heat source fractionation by distillation to contain the method for the titanium tetrachloride in the vanadium mud, the one, be subjected to the limitation of still kettle heat transfer area, especially in the middle and later periods of mud evaporative process, because near the dried slag of producing the heat conductive wall has increased thermal resistance, heat transfer efficiency is low, the power consumption height; The 2nd, the titanium tetrachloride inferior separating effect, titanium tetrachloride content is difficult to control to below 10% in the dried slag that evaporation mud obtains, and causes disadvantageous effect for the recovery vanadium.
Microwave heating has carries out characteristics such as whole heating, rapid heating and utilization of power efficient height to heated material.Microwave heating efficient just depends primarily on the ability size of material absorbing microwave in the system.Because titanium tetrachloride can not absorb microwave, therefore can not be directly by microwave heating.Titanium tetrachloride contains that solid matter in the vanadium mud has has the certain absorption microwave property, and what have can not absorb microwave fully.Because it is very little to contain in the vanadium mud solid matter particle diameter,, contain VOCl in the vanadium mud even handle through sedimentation
2, AlOCl, TiCl
3Deng the quality of solid matter still less than 10%, TiCl wherein
3Can not absorb microwave fully, the quality of material that promptly can not absorb microwave is greater than 90%.Titanium tetrachloride contains that the overwhelming majority is this factor affecting microwave absorbing efficient of material that can not absorb microwave in the vanadium mud, and therefore, adopting the microwave direct heating to contain vanadium, to contain the method separating titanium tetrachloride efficient of vanadium mud very low, do not have practical significance aborning.
In order to address the above problem, the invention provides following technical scheme:
Titanium tetrachloride is contained vanadium mud packs in the mud vaporizer that is provided with graphite heat exchanger, graphite heat exchanger is immersed in and contains in the vanadium mud, titanium tetrachloride contains vanadium mud and is evenly distributed between each heat-transfer surface of graphite heat exchanger, microwave penetrating mud evaporator wall acts on graphite heat exchanger and produces heat energy, heat energy passes to titanium tetrachloride equably by graphite heat exchanger and contains vanadium mud, the titanium tetrachloride titanium is evaporated away from contain vanadium mud efficiently, reclaim through condensation.Slag behind the separating titanium tetrachloride draws off the back as the raw material that reclaims vanadium.
This programme is made microwave absorbing medium and heat-transfer medium with graphite heat exchanger, and solve titanium tetrachloride simultaneously and contained the inefficient problem of microwave absorbing that vanadium mud microwave absorbing property difference causes, and heat even problem of transmission in mud.
What the present invention relates to contains the mud vaporizer that method adopted of separating titanium tetrachloride the vanadium mud from titanium tetrachloride, by container (1), and graphite heat exchanger (2), microwave generator (3), titanium tetrachloride vapors outlet (4), slag-drip opening (5), thermoscope (6), charging opening (7) constitutes.Graphite heat exchanger (2) places the middle and lower part in the container (1), and microwave generator (3) places the outer middle and lower part of container (1), and thermoscope (6) places in the graphite heat exchanger, and temperature controlling system links to each other with microwave generator (3).
Distance between the inwall of the outer side of graphite heat exchanger (2) and bottom surface and container (1) is respectively 5～20mm and 50～200mm.
The graphite heat exchanger one-piece construction that to be vertical direction be made of the open tubular column of several perforations, the distance between two adjacent heat-transfer surfaces of horizontal direction is 50～250mm.
In the process that titanium tetrachloride is evaporated away from contain vanadium mud, the graphite heat exchanger working temperature is 136～350 ℃.
The present invention has overcome existing titanium tetrachloride, and to contain vanadium mud evaporation technique little because of heat transfer area, particularly in the middle and later periods of mud evaporation, causes thermal resistance to increase owing to occur dried slag near the heat-transfer surface, influences the limitation of heat transfer efficiency and titanium tetrachloride separating effect.By graphite heat exchanger is set in still kettle, solved because of titanium tetrachloride can not absorb titanium tetrachloride that microwave causes contain vanadium mud should not be with the problem of microwave as thermal source, and increased heat interchanging area, improve the heat transfer benefit, and improved the effect of separating titanium tetrachloride from contain vanadium mud.
The present invention compared with prior art, utilization efficiency of heat energy improve to surpass 50%, titanium tetrachloride contains in the residue after the evaporation of vanadium mud titanium tetrachloride content less than 3%.
Description of drawings
The mud evaporation structure is seen accompanying drawing 1: mud vaporizer synoptic diagram.
Embodiment
Close slag-drip opening shown in the accompanying drawing (5), by opening for feed (7) titanium tetrachloride is contained vanadium mud and add container (1) after stipulate liquid level, close slag-drip opening (5) and opening for feed (7), start microwave generator (3), the microwave penetrating container (1) that microwave generator (3) produces acts on the titanium tetrachloride that heat transferred that graphite heat exchanger (2) produced is distributed between each heat-transfer surface and contains vanadium mud, the titanium tetrachloride that titanium tetrachloride is contained in the vanadium mud evaporates away, overflows up to titanium tetrachloride vapors outlet (4) no titanium tetrachloride vapors.The graphite heat exchanger working temperature detects by the thermo detector (6) that is arranged in the graphite heat exchanger, temperature signal feeds back to the Controlling System of microwave generator (3), when the working temperature of graphite heat exchanger (2) departed from span of control, microwave generator started or stoped work automatically.Titanium tetrachloride vapors is discharged through vapor outlet port (4), reclaims through condensation, is used to reclaim vanadium after the slag behind the separating titanium tetrachloride draws off.
Embodiment
Embodiment 1, titanium tetrachloride refining step contain vanadium and contain vanadium mud 180g (solid quality is less than 10%) and place the glass triangle bottle, with 700KW microwave oven heating 3 minutes, contain vanadium mud and rise to 35 ℃ by 25 ℃.The titanium tetrachloride refining step contains vanadium and contains vanadium mud 180g (solid quality is less than 10%) and place the glass triangle bottle, put into particle diameter 5～15mm graphite 9g simultaneously, with 700KW microwave oven heating 3 minutes, contain vanadium mud and rise to more than 136 ℃ by 25 ℃, a large amount of titanium tetrachloride vapors are overflowed.
Embodiment 2, titanium tetrachloride refining step contain vanadium and contain vanadium mud 200g (solid quality is less than 10%) and place the glass triangle bottle, with 700KW microwave oven heating 5 minutes, contain vanadium mud and rise to 41 ℃ by 25 ℃.The titanium tetrachloride refining step contains vanadium and contains vanadium mud 200g (solid quality is less than 10%) and place the glass triangle bottle, put into particle diameter 5～15mm graphite 8g simultaneously, with 700KW microwave oven heating 3 minutes, contain vanadium mud and rise to more than 136 ℃ by 25 ℃, a large amount of titanium tetrachloride vapors are overflowed.
Claims (5)
1. the method for a separating titanium tetrachloride from contain vanadium mud, it is characterized in that: titanium tetrachloride is contained vanadium mud pack in the mud vaporizer that is provided with graphite heat exchanger, titanium tetrachloride contains vanadium mud and is evenly distributed between each heat-transfer surface of graphite heat exchanger, microwave penetrating mud evaporator wall acts on graphite heat exchanger and produces heat energy, heat energy passes to titanium tetrachloride equably by graphite heat exchanger and contains vanadium mud, the titanium tetrachloride titanium is evaporated away from contain vanadium mud through condensation reclaim, the slag behind the separating titanium tetrachloride draws off the back as the raw material that reclaims vanadium.
2. according to claim 1 a kind of from contain vanadium mud the method for separating titanium tetrachloride, it is characterized in that: described graphite heat exchanger working temperature is 136～350 ℃.
3. according to claim 1 a kind of from contain vanadium mud the described mud vaporizer of the method for separating titanium tetrachloride, it is characterized in that: described mud vaporizer is by container (1), graphite heat exchanger (2), microwave generator (3), titanium tetrachloride vapors outlet (4), slag-drip opening (5), thermoscope (6), charging opening (7) constitutes.Graphite heat exchanger (2) places the middle and lower part in the container (1), and microwave generator (3) places the outer middle and lower part of container (1), and thermoscope (6) places in the graphite heat exchanger, and temperature controlling system links to each other with microwave generator (3).
According to claim 1,2 described a kind of from contain vanadium mud the method and apparatus of separating titanium tetrachloride, it is characterized in that: the distance between the inwall of the outer side of described graphite heat exchanger (2) and bottom surface and container (1) is respectively 5～20mm and 50～200mm.
According to claim 1,3 described a kind of from contain vanadium mud the method and apparatus of separating titanium tetrachloride, it is characterized in that: the described graphite heat exchanger one-piece construction that to be vertical direction be made of the open tubular column of several perforations, the distance between two adjacent heat-transfer surfaces of horizontal direction is 50～250mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910167841A CN101691242A (en) | 2009-09-30 | 2009-09-30 | Method and equipment for separating titanium tetrachloride from vanadium-containing mud |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910167841A CN101691242A (en) | 2009-09-30 | 2009-09-30 | Method and equipment for separating titanium tetrachloride from vanadium-containing mud |
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| Publication Number | Publication Date |
|---|---|
| CN101691242A true CN101691242A (en) | 2010-04-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910167841A Pending CN101691242A (en) | 2009-09-30 | 2009-09-30 | Method and equipment for separating titanium tetrachloride from vanadium-containing mud |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009999A (en) * | 2010-11-23 | 2011-04-13 | 金川集团有限公司 | Method for recovering titanium tetrachloride |
| CN102476886A (en) * | 2010-11-24 | 2012-05-30 | 攀钢集团钢铁钒钛股份有限公司 | V-containing wastewater processing method |
| CN102557124A (en) * | 2012-01-04 | 2012-07-11 | 中南大学 | Method for recovering titanium from titanium tetrachloride precipitate sludge |
| CN103613127A (en) * | 2013-11-27 | 2014-03-05 | 攀枝花钢企欣宇化工有限公司 | Recycling method of low-boiling point matters in titanium tetrachloride production |
| CN106853985A (en) * | 2015-12-08 | 2017-06-16 | 云南冶金新立钛业有限公司 | Method of the treatment containing vanadium mud |
-
2009
- 2009-09-30 CN CN200910167841A patent/CN101691242A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009999A (en) * | 2010-11-23 | 2011-04-13 | 金川集团有限公司 | Method for recovering titanium tetrachloride |
| CN102009999B (en) * | 2010-11-23 | 2012-05-30 | 金川集团有限公司 | Method for recovering titanium tetrachloride |
| CN102476886A (en) * | 2010-11-24 | 2012-05-30 | 攀钢集团钢铁钒钛股份有限公司 | V-containing wastewater processing method |
| CN102557124A (en) * | 2012-01-04 | 2012-07-11 | 中南大学 | Method for recovering titanium from titanium tetrachloride precipitate sludge |
| CN103613127A (en) * | 2013-11-27 | 2014-03-05 | 攀枝花钢企欣宇化工有限公司 | Recycling method of low-boiling point matters in titanium tetrachloride production |
| CN103613127B (en) * | 2013-11-27 | 2015-08-05 | 攀枝花钢企欣宇化工有限公司 | The recoverying and utilizing method of low boilers in titanium tetrachloride production |
| CN106853985A (en) * | 2015-12-08 | 2017-06-16 | 云南冶金新立钛业有限公司 | Method of the treatment containing vanadium mud |
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Application publication date: 20100407 |