CN103936063A - Method and system for recycling vanadium-containing mud generated in vanadium removal process of crude titanium tetrachloride - Google Patents
Method and system for recycling vanadium-containing mud generated in vanadium removal process of crude titanium tetrachloride Download PDFInfo
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- CN103936063A CN103936063A CN201410161573.2A CN201410161573A CN103936063A CN 103936063 A CN103936063 A CN 103936063A CN 201410161573 A CN201410161573 A CN 201410161573A CN 103936063 A CN103936063 A CN 103936063A
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Abstract
The invention provides a method and a system for recycling vanadium-containing mud generated in a vanadium removal process of crude titanium tetrachloride. The vanadium-containing mud contains titanium tetrachloride liquid and VOCl2 solid. The method comprises the steps of adding the vanadium-containing mud into a molten salt furnace, evaporating, and collecting titanium tetrachloride in the vanadium-containing mud; introducing chlorine into the vanadium-containing mud to ensure that chlorine is reacted with VOCl2 in the vanadium-containing mud, and obtaining mixed gas containing VOCl3 gas and chlorine; condensing the mixed gas to obtain VOCl3 liquid and chlorine, wherein molten salt is filled in the molten salt furnace, and the temperature of the molten salt furnace is kept at 600-750 DEG C. The recycling system is used for implementing the method, and comprises the molten salt furnace, an air supply pipe, a TiCl4 gas collecting unit and a condenser. The recycling method and recycling system, provided by the invention, are used for realizing one-time recovery of valuable elements namely titanium and vanadium in the vanadium-containing mud, and are high in yield of vanadium and titanium, and high in purity of obtained products.
Description
Technical field
The present invention relates to metallurgical environmental protection technical field, more particularly, relate to a kind of from thick TiCl
4aluminium powder is except the method that reclaims valuable element Ti and V in vanadium mud that contains producing in vanadium refining process.
Background technology
Titanium tetrachloride (TiCl
4) be produce titanium sponge and chloride process titanium dioxide must obligato raw material.Due to titaniferous materials (for example, ilmenite) there are many detrimental impurity (for example, vanadium) in the crude titanic chloride produced through retailoring, chlorination, these impurity directly affect the quality of titanium sponge, therefore, must by crude titanic chloride, purification could be for the production of titanium sponge and titanium white in addition.Because the foreign matter of vanadium in crude titanic chloride is mainly with three aluminum oxidation vanadium (VOCl
3) form existence, its boiling point (127 DEG C) is very approaching with titanium tetrachloride boiling point (136 DEG C), thereby adopts rectificating method to be difficult to vanadium to separate and remove from titanium tetrachloride, and in industrial production, the main chemical process that adopts is removed vanadium, and for example, aluminium powder is except vanadium.
Aluminium powder except vanadium technique be to do under the condition of catalyzer at aluminum chloride, with aluminium powder by TiCl
4be reduced to titanous chloride (TiCl
3), the muriate of this Low-valent Titanium is a kind of strong reductant, can with thick TiCl
4in VOCl
3effect, makes it to be reduced to VOCl
2, foreign matter of vanadium and TiCl
3between occur main chemical reactions equation as shown in the formula 1 and formula 2 shown in:
formula 1
TiCl
3(l)+VOCl
3(l)=TiCl
4(l)+VOCl
2(s) formula 2
Remove in vanadium technique VOCl at aluminium powder
3be reduced into solid-state VOCl
2, be deposited in refining mud.At present, for thick TiCl
4aluminium powder except produce in vanadium refining process containing vanadium mud, mainly to make the lime cake that the is insoluble in water slag field of banking up by adding lime, processing so the refining vanadium mud that contains not only can not reclaim valuable element vanadium, and take a large amount of land resources, cause environmental degradation, indirectly increased titanium sponge production cost.
Summary of the invention
For the deficiencies in the prior art, one of object of the present invention is to solve the one or more problems that exist in above-mentioned prior art.For example, one of object of the present invention is to provide a kind of thick TiCl of recycling
4aluminium powder except produce in vanadium refining process containing the vanadium of vanadium mud and the method for titanium.
To achieve these goals, an aspect of of the present present invention provides the recovery method containing vanadium mud that a kind of crude titanic chloride produces except vanadium.Contain titanium tetrachloride liquid and VOCl described containing in vanadium mud
2solid, described method comprises carries out ground following steps successively: add in molten salt furnace containing vanadium mud described, to evaporate and to collect containing the titanium tetrachloride in vanadium mud; Pass into chlorine to described containing in vanadium mud, so that chlorine and the VOCl containing in vanadium mud
2reaction, obtains comprising VOCl
3the mixed gas of gas and chlorine; Mixed gas described in condensation, obtains VOCl
3liquid and chlorine; Wherein, the temperature being loaded with in described molten salt furnace in fused salt and described molten salt furnace remains on 600～750 DEG C.
According to the present invention, crude titanic chloride is except an embodiment of the recovery method containing vanadium mud of vanadium generation, and the temperature in described molten salt furnace remains on 650～700 DEG C.
The embodiment containing the recovery method of vanadium mud that crude titanic chloride produces except vanadium according to the present invention, by weight percentage, described containing navajoite slurry by aluminium powder except vanadium process produces, wherein can contain 70～85% TiCl
4, 8～10% TiCl
3, 1～3% VOCl
2and 3～8% AlCl
3.
According to the present invention, crude titanic chloride is except an embodiment of the recovery method containing vanadium mud of vanadium generation, and the mass ratio of the described intake containing vanadium mud and described chlorine can be 40:1～50:1.
According to the present invention, crude titanic chloride, except an embodiment of the recovery method containing vanadium mud of vanadium generation, is controlled described chlorine and is completed and pass in 20～30min.
According to the present invention, crude titanic chloride is except an embodiment of the recovery method containing vanadium mud of vanadium generation, and described fused salt is the mixture of NaCl and KCl.
According to the present invention, crude titanic chloride is except an embodiment of the recovery method containing vanadium mud of vanadium generation, and the mass ratio of described NaCl and KCl can be 4:6～2:8.
The embodiment containing the recovery method of vanadium mud that crude titanic chloride produces except vanadium according to the present invention, described method also comprises in described molten salt furnace and passes into rare gas element to keep fused salt and flowing containing vanadium mud.
According to the present invention, crude titanic chloride is except an embodiment of the recovery method containing vanadium mud of vanadium generation, and described mixed gas is cooled to-5～10 DEG C by described condensing steps.
The recovery system containing vanadium mud that another aspect of the present invention provides a kind of crude titanic chloride to produce except vanadium.Described recovery system comprises molten salt furnace, air-supply duct, TiCl
4gas collection unit and condenser, wherein, described molten salt furnace comprise have inner chamber body of heater, be arranged on body of heater containing vanadium mud opening for feed, the venting port that is arranged on body of heater top, fused salt and the heating unit of splendid attire in described inner chamber, described molten salt furnace can be heated to 600～700 DEG C by fused salt with containing vanadium mud; Described air-supply duct is connected with described molten salt furnace and stirs gas for pass into chlorine and inertia in described molten salt furnace, and one end that described air-supply duct is connected with described molten salt furnace is stretched under the charge level in described molten salt furnace; Described TiCl
4the inlet mouth of gas collection unit and condenser is communicated with the venting port of described molten salt furnace respectively, wherein, and described TiCl
4gas collection unit is for collecting the TiCl discharging from molten salt furnace
4gas, described condenser reclaims for condensation the VOCl discharging from molten salt furnace
3gas.
Compared with prior art, beneficial effect of the present invention comprises: in molten salt furnace, remove containing the titanium tetrachloride in vanadium mud and dichloro vanadyl simultaneously, production unit is simple, valuable element titanium and vanadium in the refining mud of disposable recovery titanium tetrachloride are realized, and the yield of vanadium and titanium is high, the product purity obtaining is high, when realization is turned waste into wealth, has solved the problem of environmental pollution bringing containing vanadium mud.
Brief description of the drawings
By the description of carrying out below in conjunction with accompanying drawing, above and other object of the present invention and feature will become apparent, wherein:
Fig. 1 shows the schematic diagram of exemplary embodiment of the present crude titanic chloride except the recovery system containing vanadium mud of vanadium generation.
Description of reference numerals:
1-molten salt furnace, 2-fused salt, 3,4-electrode, 5-air-supply duct, 6-TiCl
4gas collection unit, 7-condenser and 8-VOCl
3product stock unit.
Embodiment
Hereinafter, describe in connection with accompanying drawing and exemplary embodiment recovery method and the recovery system containing the vanadium mud that produce except vanadium according to crude titanic chloride of the present invention in detail.
Fig. 1 is the schematic diagram of exemplary embodiment of the present crude titanic chloride except the recovery system containing vanadium mud of vanadium generation.As shown in Figure 1, this recovery system comprises molten salt furnace 1, air-supply duct 5, TiCl
4gas collection unit 6, condenser 7 and VOCl
3product stock unit 8.
Wherein, molten salt furnace 1 can be by thick TiCl
4be heated to 600～750 DEG C, it comprise have inner chamber body of heater, be arranged on body of heater, be called again thermal barrier or heating medium containing vanadium mud opening for feed, the venting port that is arranged on body of heater top, the fused salt 2(of splendid attire in described inner chamber) and heating unit.Wherein, fused salt is the mixture of NaCl and KCl.Heating unit comprises Graphite Electrodes 3 and 4.Air-supply duct 5 stirs gas (for example nitrogen) for pass into chlorine and inertia in molten salt furnace 1, and one end of air-supply duct 5 is connected and stretches under the charge level in described molten salt furnace with described molten salt furnace, and the other end is communicated with external air source.TiCl
4the inlet mouth of gas collection unit 6 and condenser 7 is communicated with the venting port of molten salt furnace 1 respectively, wherein, and TiCl
4gas collection unit 6 is for collecting the TiCl discharging from molten salt furnace
4gas, in this example, adopts refining and distilling still as TiCl
4gas collection unit, refining and distilling still can be collected and refine and reclaim TiCl
4gas obtains TiCl
4product; Condenser 7 reclaims the VOCl discharging from molten salt furnace for condensation
3gas, obtains high purity VOCl
3(l) product.VOCl
3product stock unit is connected with condenser 7, the high purity VOCl obtaining for collecting condenser 7 condensations
3(l) product.
Below, describe according to an exemplary embodiment of the present invention recovery process except what vanadium produced containing the recovery system of vanadium mud in connection with above-mentioned crude titanic chloride.
This technique contains vanadium mud as raw material taking aluminium powder except what vanadium process produced, and chlorine is oxygenant, and the mixture of NaCl and KCl is heating medium (fused salt), and molten salt furnace 1 separates and VOCl as titanium tetrachloride
2the equipment of oxidation, condenser 7 is as VOCl
3recovery system.Wherein, by weight percentage, containing TiCl in vanadium mud
4content is 80～85%, TiCl
3content is 8～10%, VOCl
2content is 1～3% and AlCl
3content is 3～7%, but the invention is not restricted to this, and method of the present invention can also be processed other and comprise titanium tetrachloride liquid and VOCl except what vanadium process produced except crude titanic chloride
2solid containing vanadium mud.The mass ratio control of NaCl in heating medium and KCl is 4:6～2:8 in addition.This technique specifically comprises the following steps:
(1) heating medium (NaCl and KCl) mixed by predetermined proportion and be preheated to molten state, now temperature is 600～750 DEG C, then adds in molten salt furnace 1, and utilizes Graphite Electrodes 3 and 4 to heat to remain within the scope of 600～750 DEG C.
(2) will add in molten salt furnace containing vanadium mud, and be to be incubated 20～30min under the condition of 600～750 DEG C in temperature, to evaporate and to collect containing the titanium tetrachloride in vanadium mud, reach the object of separating titanium.
(3) pass into chlorine according to the ratio that is 40:1～50:1 containing the mass ratio of vanadium mud and chlorine, and control the speed that passes into of chlorine, to have led to chlorine in 20～30min, the chlorine passing into and the VOCl containing in vanadium mud
2solid reacts the VOCl that generates gaseous state under the temperature condition of 600～750 DEG C
3.
(4) condensation is reclaimed to the VOCl that molten salt furnace 1 is discharged
3gas passes in condenser 7, and keeping the temperature in condenser is-5～10 DEG C, obtains highly purified VOCl
3liquid and chlorine, realize VOCl
3and Cl
2separation, wherein, highly purified VOCl
3liquid is sent into VOCl
3in product stock unit 8, preserve, excessive chlorine can pass into alkali pond.
In above-mentioned steps (1), in (3), the temperature in control molten salt furnace is 600～750 DEG C can make fused salt keep flowing, and wherein, steams TiCl in step (2)
4time, be dispersed in the fused salt of molten state containing vanadium mud, heating surface area is large and even, be beneficial to improve and steam efficiency, if do not adopt molten salt furnace and control temperature in molten salt furnace in said temperature scope, due to lower containing solid load ratio in vanadium mud, and liquid content is more and fusing point approaches, steam after liquid phase, remaining solid matter easily hardens, and causes further vanadium separating-purifying difficulty; And in the chlorination process of step (3), dichloro vanadyl is dispersed in the fused salt of molten state, there are more chance and chlorine reaction, and speed of reaction is fast under above-mentioned hot conditions, if temperature is during lower than 600 DEG C, fused salt mobility is bad, if temperature is during higher than 750 DEG C, dichloro vanadyl may steam, and it is too high to consume energy.
Preferably, in above-mentioned steps (1), in (3), the temperature of controlling in molten salt furnace is 650～700 DEG C.
Further, in described step (2) and step (3), in molten salt furnace, pass into rare gas element (for example nitrogen), keep fused salt 2 and contain flowing of vanadium mud, to mix.
First this technique evaporate the TiCl removing containing in vanadium mud
4, then utilize VOCl
2and VOCl
3different physical propertiess and chemical property, used oxygenant Cl
2vOCl in oxidation molten salt furnace
2(s) generate VOCl
3(g), VOCl
3(g) cooling formation liquid in cooling system, reaches thereby separate the object of extracting V, that is to say, makes VOCl by chlorine
2transformed to lower boiling by high boiling point, thereby reach the effect of purification.
In order to understand better above-mentioned exemplary embodiment of the present invention, below in conjunction with concrete example, it is further described.
This example adopts the molten salt furnace of 300 tons/year to process TiCl
4aluminium powder except vanadium treating process produce containing vanadium mud.Wherein, the diameter of molten salt furnace is 800mm, and power is 60kw, and type of heating is Graphite Electrodes heating, every a collection of can process 300Kg containing vanadium mud, power consumption 80kwh.
Specific embodiment is: the fused salt 600Kg that the mass ratio of (1) preparation NaCl and KCl is 4:6, and be preheated to molten state, and now temperature is 650 DEG C, in the molten salt furnace that is then injected into diameter and is, and heat maintenance temperature by Graphite Electrodes be 650 DEG C; (2) switch tail gas to refining and distilling still, be communicated with, and in molten bath, feed nitrogen by air-supply duct by refining and distilling still with the venting port of molten salt furnace, maintenance gas supply flow is 50m
3/ h then injects 300Kg containing vanadium mud in molten salt furnace, at 650 DEG C, is incubated 30min, and the tail gas obtaining (is TiCl
4gas) escape and enter refining and distilling still from venting port; (3) switch tail gas to condenser, close being connected between refining and distilling still and the venting port of molten salt furnace, and condenser is communicated with molten salt furnace venting port, reduce nitrogen flow in vapor pipe to 48m
3/ h, and start to molten bath, to pass into chlorine in vapor pipe, control chlorine flowrate is 12m
3it is 650 DEG C that/h controls temperature of reaction, continues 30min, and the tail gas obtaining (contains VOCl
3gas and chlorine) discharge and be sent to condenser from venting port and be condensed to room temperature, obtain liquid VOCl
3product.(4) increase nitrogen flow, close chlorine, inject next batch containing vanadium mud, continue next batch ground refining.Wherein, processing continuously five batches needs deslagging containing after vanadium mud, so that the fused salt liquid level in molten salt furnace returns to elemental height.
The present invention has realized valuable element titanium and the vanadium in the refining mud of disposable recovery titanium tetrachloride, wherein, and Ti yield>=95%, V yield>=85%, VOCl
3product purity>=98wt%, yield is high, and the product purity obtaining is high, especially can obtain highly purified VOCl
3, can be used for production high-quality high purity vanadium.The present invention is conducive to that efficient utilization, the technical process of resource are short, production unit is simple, be easy to realize industrialization.And refining mud belongs to high pollution thing, the present invention turns waste into wealth in realization, create profit in, solved problem of environmental pollution, there is very high economic and social benefit.
Although above by having described the present invention in conjunction with exemplary embodiment, it will be apparent to those skilled in the art that in the case of not departing from the spirit and scope that claim limits, can carry out various amendments and change to exemplary embodiment of the present invention.
Claims (10)
1. the recovery method containing vanadium mud that crude titanic chloride produces except vanadium, contain titanium tetrachloride liquid and VOCl described containing in vanadium mud
2solid, is characterized in that, said method comprising the steps of:
Add in molten salt furnace containing vanadium mud described, to evaporate and to collect containing the titanium tetrachloride in vanadium mud;
Pass into chlorine to described containing in vanadium mud, so that chlorine and the VOCl containing in vanadium mud
2reaction, obtains comprising VOCl
3the mixed gas of gas and chlorine;
Mixed gas described in condensation, obtains VOCl
3liquid and chlorine;
Wherein, the temperature being loaded with in described molten salt furnace in fused salt and described molten salt furnace remains on 600～750 DEG C.
2. crude titanic chloride according to claim 1, except the recovery method containing vanadium mud that vanadium produces, is characterized in that, the temperature in described molten salt furnace remains on 650～700 DEG C.
Crude titanic chloride according to claim 1 except vanadium produce containing the recovery method of vanadium mud, it is characterized in that, by weight percentage, described containing navajoite slurry by aluminium powder except vanadium process produces, wherein contain 70～85% TiCl
4, 8～10% TiCl
3, 1～3% VOCl
2and 3～8% AlCl
3.
4. crude titanic chloride according to claim 3, except the recovery method containing vanadium mud that vanadium produces, is characterized in that, the mass ratio of the described intake containing vanadium mud and described chlorine is 40:1～50:1.
5. crude titanic chloride according to claim 3, except the recovery method containing vanadium mud that vanadium produces, is characterized in that, controls described chlorine and completes and pass in 20～30min.
Crude titanic chloride according to claim 1 except vanadium produce containing the recovery method of vanadium mud, it is characterized in that, described fused salt is that the mixture of NaCl and KCl is as fused salt.
7. crude titanic chloride according to claim 6, except the recovery method containing vanadium mud that vanadium produces, is characterized in that, the mass ratio of described NaCl and KCl is 4:6～2:8.
Crude titanic chloride according to claim 1 except vanadium produce containing the recovery method of vanadium mud, it is characterized in that, described method also comprises in described molten salt furnace and passes into rare gas element to keep fused salt and flowing containing vanadium mud.
9. crude titanic chloride according to claim 1, except the recovery method containing vanadium mud that vanadium produces, is characterized in that, described mixed gas is cooled to-5～10 DEG C by described condensing steps.
10. crude titanic chloride, except the recovery system containing vanadium mud that vanadium produces, is characterized in that, described recovery system comprises molten salt furnace, air-supply duct, TiCl
4gas collection unit and condenser, wherein,
Described molten salt furnace comprise have inner chamber body of heater, be arranged on body of heater containing vanadium mud opening for feed, the venting port that is arranged on body of heater top, fused salt and the heating unit of splendid attire in described inner chamber, described molten salt furnace can be heated to 600～750 DEG C by fused salt with containing vanadium mud;
Described air-supply duct is connected with described molten salt furnace and stirs gas for pass into chlorine and inertia in described molten salt furnace, and one end that described air-supply duct is connected with described molten salt furnace is stretched under the charge level in described molten salt furnace;
Described TiCl
4the inlet mouth of gas collection unit and condenser is communicated with the venting port of described molten salt furnace respectively, wherein, and described TiCl
4gas collection unit is for collecting the TiCl discharging from molten salt furnace
4gas, described condenser reclaims for condensation the VOCl discharging from molten salt furnace
3gas.
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|---|---|---|---|
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|---|---|---|---|
| CN201410161573.2A CN103936063B (en) | 2014-04-22 | 2014-04-22 | Method and system for recycling vanadium-containing mud generated in vanadium removal process of crude titanium tetrachloride |
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| CN106946286A (en) * | 2017-03-09 | 2017-07-14 | 金川集团股份有限公司 | A kind of crude titanic chloride is except the chemical reaction equipment and method of vanadium |
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| CN115821071A (en) * | 2022-12-13 | 2023-03-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Treatment method of titanium tetrachloride vanadium-removing slurry |
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| CN106946286A (en) * | 2017-03-09 | 2017-07-14 | 金川集团股份有限公司 | A kind of crude titanic chloride is except the chemical reaction equipment and method of vanadium |
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| 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 |
| CN115821071A (en) * | 2022-12-13 | 2023-03-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Treatment method of titanium tetrachloride vanadium-removing slurry |
| CN115821071B (en) * | 2022-12-13 | 2024-08-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Treatment method of titanium tetrachloride vanadium-removing slurry |
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