CN103936062A - Vanadium removal refining tower with organic matter and method for removing vanadium from crude titanium tetrachloride with organic matter - Google Patents
Vanadium removal refining tower with organic matter and method for removing vanadium from crude titanium tetrachloride with organic matter Download PDFInfo
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- CN103936062A CN103936062A CN201410160740.1A CN201410160740A CN103936062A CN 103936062 A CN103936062 A CN 103936062A CN 201410160740 A CN201410160740 A CN 201410160740A CN 103936062 A CN103936062 A CN 103936062A
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Abstract
The invention discloses a vanadium removal refining tower with an organic matter and a method for removing vanadium from crude titanium tetrachloride with the organic matter. The vanadium removal refining tower with the organic matter is a vertically arranged cylinder and comprises a fluidized mixed reaction zone, a buffer zone and a rectifying zone, wherein the fluidized mixed reaction zone is used for fluidized mixing and reaction of vanadium removal organic matters and gas to be subjected to vanadium removal and comprises a slurry outlet arranged at the bottom, an organic matter inlet arranged at the upper part of the side wall, a gas inlet arranged at the lower part of the side wall and a gas distributor arranged in the fluidized mixed reaction zone, the inlet of the gas distributor is communicated with the gas outlet to spray the gas to be subjected to vanadium removal into the fluidized mixed reaction zone; the buffer zone is connected to the fluidized mixed reaction zone and the rectifying zone; the rectifying zone is used for removing impurities from the vanadium-removed gas and comprises a gas outlet disposed on the top, a reflux feed port formed in the upper part of the side wall and a plurality of tower plates disposed in the rectifying zone. The method for removing vanadium from crude titanium tetrachloride with the organic matter performs vanadium removal by using the vanadium removal refining tower.
Description
Technical field
The present invention relates to metallurgical technology field, more particularly, relate to a kind of organism except vanadium treating tower and the crude titanic chloride organism method except vanadium.
Background technology
Crude titanic chloride is a kind of very complicated turbid solution of plurality of impurities, composition that contains, and in the production process of refining titanic chloride, the vanadium compound impurity of removing in crude titanic chloride is the important step that titanium sponge is produced.
It is at present domestic and international more advanced refine and removing vanadium technique that organism removes vanadium, and general technical process is first by thick TiCl
4with add in mixing tank and stir respectively by a certain percentage except vanadium organism (as mineral wet goods), then add and in still kettle, be heated to temperature of reaction and generate solid-state vanadium precipitation, thereby reach the object except vanadium.But in this technique, thick TiCl
4with separate with reacting by heating process except the organic mixing process of vanadium, be unfavorable for removing the serialization of vanadium, increased operating time and personnel's configuration.
Summary of the invention
For deficiency of the prior art, the object of the invention is to one or more in solving the problems of the technologies described above.
The object of the present invention is to provide and a kind ofly improve organism except the efficiency of vanadium and simplify except the organism of vanadium device is except vanadium treating tower and the crude titanic chloride organism method except vanadium.
To achieve these goals, an aspect of of the present present invention provides a kind of organism except vanadium treating tower, described treating tower is the fluidisation hybrid reaction section that vertically disposed cylindrical shell and described treating tower comprise bottom, the breeze way at middle part and the rectifying section on top, wherein, fluidisation hybrid reaction section is for mixing and react with treating the fluidisation except vanadium gas except vanadium organism, described fluidisation hybrid reaction section comprises the slurry outlet that is arranged on bottom, be arranged on the organism entrance of side wall upper part, be arranged on the gas feed of lower sidewall and be arranged on the gas distributor in fluidisation hybrid reaction section, the entrance of described gas distributor is communicated with gas feed to spray in fluidisation hybrid reaction section to be treated except vanadium gas, breeze way connects described fluidisation hybrid reaction section and rectifying section, rectifying section is for the removal of impurities except gas after vanadium, described rectifying section comprise be arranged on top pneumatic outlet, be arranged on the backflow charging opening of side wall upper part and be arranged on the polylith column plate in rectifying section.
An embodiment according to organism of the present invention except vanadium treating tower, described gas feed and organism entrance relatively arrange.
An embodiment according to organism of the present invention except vanadium treating tower, described gas distributor comprises 8～13 inlet pipe, is uniformly distributed 40～70 nozzles in every inlet pipe.
An embodiment according to organism of the present invention except vanadium treating tower, the setting position of described gas distributor should guarantee to treat can not have described gas distributor except vanadium gas with the vanadium slurry sediment that contains of reacting generation except vanadium organism.
An embodiment according to organism of the present invention except vanadium treating tower, the bottom 1500～1800mm of the described fluidisation hybrid reaction section of described gas distributor distance.
An embodiment according to organism of the present invention except vanadium treating tower, the quantity of described column plate is 2～10.
An embodiment according to organism of the present invention except vanadium treating tower, treat mix and react generation containing vanadium slurry sediment with the vanadium organism fluidisation in fluidisation hybrid reaction section of removing passing into from organism entrance except vanadium gas, the described vanadium slurry sediment that contains is discharged from slurry outlet; Reacted treating enters rectifying section except vanadium gas, by regulating the temperature at rectifying section top make separated until the higher-boiling compound except in vanadium gas and obtain except gas after vanadium.
Another aspect of the present invention provides the method for a kind of crude titanic chloride organism except vanadium, and described method adopts above-mentioned organism to remove the vanadium that removes that vanadium treating tower carries out crude titanic chloride.
An embodiment according to crude titanic chloride organism of the present invention except the method for vanadium, said method comprising the steps of: the vanadium organism that removes that is 136～142 ℃ by temperature passes into fluidisation hybrid reaction section from organism entrance, again crude titanic chloride gas is sprayed into fluidisation hybrid reaction section by gas feed and gas distributor, described except vanadium organism and crude titanic chloride are gas fluidized, mix and react generation contain vanadium slurry sediment;
The temperature that regulates described rectifying section top is 135～138 ℃, reacted crude titanic chloride gas enters rectifying section and after the separated higher-boiling compound of column plate, from pneumatic outlet, enters aftertreatment device and obtains except the titanium tetrachloride vanadium, higher-boiling compound and regularly discharging by slurry outlet containing vanadium slurry sediment.
An embodiment according to crude titanic chloride organism of the present invention except the method for vanadium, described aftertreatment device is air cooler, reacted crude titanic chloride gas enters rectifying section and from pneumatic outlet, enter described air cooler condensation after the separated higher-boiling compound of column plate, by regulating reflux ratio to make to reflux to control the described quality except the titanium tetrachloride after vanadium by backflow charging opening through the condensed partial condensation thing of air cooler.
The present invention utilizes fluidization technique make to wait to remove vanadium gas and remove the organic state that reaches full and uniform that mixes of vanadium, is conducive to treat that except vanadium Adsorption of Organic raising removes vanadium efficiency except containing vanadium component and being conducive to heat and mass transport process between gas-liquid in vanadium gas; In addition, crude titanic chloride carries out reacting by heating when can mix in same device with except vanadium organism, agitation mixer and step except vanadium organism and crude titanic chloride have been reduced, more effectively reduced operating time and personnel's outfit, reduce the cost of refining titanic chloride, there is popularizing application prospect widely.
Accompanying drawing explanation
Fig. 1 is that the organism of exemplary embodiment of the present is except the structural representation of vanadium treating tower.
Description of reference numerals:
1-fluidisation hybrid reaction section; 2-rectifying section, 3-pneumatic outlet, 4-backflow charging opening, 5-gas feed, 6-organism entrance, 7-slurry outlet, 8-breeze way.
Embodiment
Hereinafter, describe with reference to the accompanying drawings organism of the present invention in detail except vanadium treating tower and the crude titanic chloride organism method except vanadium.
Fig. 1 is that the organism of exemplary embodiment of the present is except the structural representation of vanadium treating tower.
As shown in Figure 1, according to exemplary embodiment of the present invention, it is the fluidisation hybrid reaction section 1 that vertically disposed cylindrical shell and this treating tower comprise bottom that described organism removes vanadium treating tower, the breeze way 8 at middle part and the rectifying section 2 on top, wherein, fluidisation hybrid reaction section 1 is for mixing and react with treating the fluidisation except vanadium gas except vanadium organism, rectifying section 2 is for the removal of impurities except gas after vanadium, breeze way 8 is also set between fluidisation hybrid reaction section 1 and rectifying section 2 and is beneficial to collecting and falling the impurity except obtaining after gas removal of impurities after vanadium, avoid organism and liquid level when except vanadium gas reaction to rise sharply on the impact except material quality after vanadium simultaneously.According to the present invention, the diameter of fluidisation hybrid reaction section 1 is greater than the diameter of rectifying section 2, and the height of fluidisation hybrid reaction section 1 is less than the height of rectifying section 2, and concrete size can be according to Production requirement setting.
Below each segment structure and the function for the treatment of tower are specifically described.
Fluidisation hybrid reaction section 1 comprise be arranged on bottom slurry outlet 7, be arranged on side wall upper part organism entrance 6, be arranged on the gas feed 5 of lower sidewall and be arranged on the gas distributor (not shown) in fluidisation hybrid reaction section 1, the entrance of gas distributor is communicated with gas feed 5 to spray in fluidisation hybrid reaction section 1 waits to remove vanadium gas.Treat with certain speed and certain pressure, to enter in fluidisation hybrid reaction section 1 via gas feed 5 and gas distributor except vanadium gas, except vanadium organism passes in fluidisation hybrid reaction section 1 from organism entrance, two kinds of materials mix in fluidisation hybrid reaction section 1 interior fluidisation, direct heating contains after vanadium slurry sediment except vanadium organism also reacts to generate to temperature of reaction or by mixed heating material to temperature of reaction, reacted gaseous mixture directly rises and enters refining district 2, and gained is discharged from slurry outlet 7 containing vanadium slurry sediment.Preferably, gas feed 5 and organism entrance 6 relatively arrange to strengthen treating except vanadium gas and except the organic convection current mixing effect of vanadium, improve mixing uniformity and also impel sufficient reacting to carry out fully removing vanadium.
Wherein, the setting position of gas distributor should guarantee to treat can not have gas distributor except vanadium gas with the vanadium slurry sediment that contains of reacting generation except vanadium organism, according to one embodiment of present invention, gas distributor is apart from the bottom 1500～1800mm of fluidisation hybrid reaction section 1, but the invention is not restricted to this, can be according to the setting position of the size concrete arrangement gas distributor of whole treating tower.According to the present invention, gas distributor comprises 8～13 inlet pipe, in every inlet pipe, be uniformly distributed 40～70 nozzles, but the invention is not restricted to this, because gas distributor is mainly used in distributing except vanadium gas uniform except vanadium gas sprays in fluidisation hybrid reaction section 1 with certain speed and certain pressure and makes to enter treating in tower treating, thereby be conducive to treat except vanadium gas and even mixing that removes vanadium organism liquid, as long as can realize above-mentioned functions, the present invention does not specifically limit its structure.
Rectifying section 2 comprise be arranged on top pneumatic outlet 3, be arranged on the backflow charging opening 4 of side wall upper part and be arranged on the polylith column plate (not shown) in rectifying section.Reacted treating enters in rectifying section 2 except vanadium gas, by regulating the temperature at rectifying section 2 tops and via the separation of column plate, treat to be separated except the higher-boiling compound in vanadium gas, except gas after vanadium overflows by pneumatic outlet 3 and enter aftertreatment device, higher-boiling compound stay in treating tower and with together with vanadium slurry sediment, from the slurry outlet 7 at the bottom of tower, discharge, thereby complete organism except the processing of vanadium.Wherein, column plate is the conventional components for the treatment of tower, it is for making two kinds of fluid close contacts and carrying out the matter exchange between two-phase, to reach the object of separating liquid mixture or gaseous mixture component, the present invention does not limit the structure of column plate and quantity, as long as can realize basic heat exchange centrifugation.According to the present invention, the quantity of column plate is 2～10.In addition, aftertreatment device of the present invention can be for example air cooler, except the gas after vanadium enters air cooler condensation, then by regulating reflux ratio to make to be back to by backflow charging opening in treating tower and to continue reaction to control the quality except material after vanadium through the condensed partial condensation thing of air cooler.
The method that crude titanic chloride organism of the present invention removes vanadium adopts above-mentioned organism to remove the vanadium that removes that vanadium treating tower carries out crude titanic chloride, but above-mentioned organism removes the vanadium that removes that vanadium treating tower is not limited in crude titanic chloride.
According to one embodiment of present invention, said method comprising the steps of: will from organism entrance, pass into fluidisation hybrid reaction section except vanadium organism, Heating temperature to 136～142 ℃, again crude titanic chloride gas is sprayed into fluidisation hybrid reaction section by gas feed and gas distributor, except vanadium organism and crude titanic chloride are gas fluidized, mix and react generating containing vanadium slurry sediment; Regulating the temperature at rectifying section top is 135～138 ℃, reacted crude titanic chloride gas enters rectifying section and from pneumatic outlet, enter aftertreatment device after the separated higher-boiling compound of column plate and obtains except the titanium tetrachloride vanadium, higher-boiling compound and regularly discharging by slurry outlet containing vanadium slurry sediment, thus realize processing except vanadium crude titanic chloride.
Wherein, make the titanium tetrachloride gases after reaction removal of impurities enter air cooler condensation via pneumatic outlet, by regulating reflux ratio to make to be back to by backflow charging opening in treating tower and to continue reaction to control except the titanium tetrachloride quality after vanadium through the condensed partial condensation thing of air cooler.The adjusting of reflux ratio specifically can realize by the valve opening of adjusting return line, and the step of this adjusting reflux ratio should be to obtain carrying out targetedly except the titanium tetrachloride after vanadium and after observing this shade and quality except the titanium tetrachloride after vanadium in reaction.
Below in conjunction with concrete example, describe the present invention in detail.
Example:
The internal diameter of the fluidisation hybrid reaction section for the treatment of tower is 4000mm, high 3500mm.Gas distributor is apart from the bottom 1800mm of fluidisation hybrid reaction section, and gas distributor comprises and in 9 inlet pipe and every inlet pipe, is uniformly distributed 55 nozzles.5 of column plates are set in rectifying section.
By organism entrance, add except vanadium organism mineral oil, its flow is 0.05t/h, and it will be heated to 140 ℃; By gas feed and gas distributor, pass into crude titanic chloride gas, its flow is 10t/h.Crude titanic chloride gas enters fluidisation hybrid reaction Duan Houyu and contains vanadium slurry sediment except vanadium organism reacts and generates, reacted gas rises to rectifying section, the temperature at rectifying section top is controlled is 137 ℃ simultaneously, after column plate separation, higher-boiling compound is got back to fluidisation hybrid reaction section, titanium tetrachloride gases and low-boiling compound enter aftertreatment device and obtain except the titanium tetrachloride vanadium from the pneumatic outlet of tower top, contain vanadium slurry sediment and higher-boiling compound by slurry outlet discharge per hour.
Organism of the present invention, except vanadium treating tower novel structure, easy and simple to handle, has been abandoned the conventional mixing of materials method separated with refining step, effectively reduces manning simplified apparatus, has improved production efficiency, has larger implementary value and economic results in society.
Although described organism of the present invention except vanadium treating tower and the crude titanic chloride organism method except vanadium in conjunction with exemplary embodiment above, but those of ordinary skills should be clear, in the situation that do not depart from the spirit and scope of claim, can carry out various modifications to above-described embodiment.
Claims (10)
1. organism, except a vanadium treating tower, is characterized in that, described treating tower is fluidisation hybrid reaction section, the breeze way at middle part and the rectifying section on top that vertically disposed cylindrical shell and described treating tower comprise bottom, wherein,
Fluidisation hybrid reaction section is for mixing and react with treating the fluidisation except vanadium gas except vanadium organism, described fluidisation hybrid reaction section comprise be arranged on bottom slurry outlet, be arranged on side wall upper part organism entrance, be arranged on the gas feed of lower sidewall and be arranged on the gas distributor in fluidisation hybrid reaction section, the entrance of described gas distributor is communicated with gas feed to spray in fluidisation hybrid reaction section waits to remove vanadium gas;
Breeze way connects described fluidisation hybrid reaction section and rectifying section;
Rectifying section is for the removal of impurities except gas after vanadium, described rectifying section comprise be arranged on top pneumatic outlet, be arranged on the backflow charging opening of side wall upper part and be arranged on the polylith column plate in rectifying section.
2. organism according to claim 1, except vanadium treating tower, is characterized in that, described gas feed and organism entrance relatively arrange.
3. organism according to claim 1, except vanadium treating tower, is characterized in that, described gas distributor comprises 8～13 inlet pipe, is uniformly distributed 40～70 nozzles in every inlet pipe.
4. organism according to claim 1, except vanadium treating tower, is characterized in that, the setting position of described gas distributor should guarantee to treat can not have described gas distributor except vanadium gas with the vanadium slurry sediment that contains of reacting generation except vanadium organism.
5. organism according to claim 4, except vanadium treating tower, is characterized in that, the bottom 1500～1800mm of the described fluidisation hybrid reaction section of described gas distributor distance.
6. organism according to claim 1, except vanadium treating tower, is characterized in that, the quantity of described column plate is 2～10.
7. organism according to claim 1 is except vanadium treating tower, it is characterized in that, treat mix and react generation containing vanadium slurry sediment with the vanadium organism fluidisation in fluidisation hybrid reaction section of removing passing into from organism entrance except vanadium gas, the described vanadium slurry sediment that contains is discharged from slurry outlet; Reacted treating enters rectifying section except vanadium gas, by regulating the temperature at rectifying section top make separated until the higher-boiling compound except in vanadium gas and obtain except gas after vanadium.
8. crude titanic chloride organism, except a method for vanadium, is characterized in that, described method adopts the organism described in any one in claim 1 to 7 to remove the vanadium that removes that vanadium treating tower carries out crude titanic chloride.
9. crude titanic chloride organism according to claim 8, except the method for vanadium, is characterized in that, said method comprising the steps of:
The vanadium organism that removes that is 136～142 ℃ by temperature passes into fluidisation hybrid reaction section from organism entrance, again crude titanic chloride gas is sprayed into fluidisation hybrid reaction section by gas feed and gas distributor, described except vanadium organism and crude titanic chloride are gas fluidized, mix and react generation contain vanadium slurry sediment;
The temperature that regulates described rectifying section top is 135～138 ℃, reacted crude titanic chloride gas enters rectifying section and after the separated higher-boiling compound of column plate, from pneumatic outlet, enters aftertreatment device and obtains except the titanium tetrachloride vanadium, higher-boiling compound and regularly discharging by slurry outlet containing vanadium slurry sediment.
10. crude titanic chloride organism according to claim 9 is except the method for vanadium, it is characterized in that, described aftertreatment device is air cooler, reacted crude titanic chloride gas enters rectifying section and from pneumatic outlet, enter described air cooler condensation after the separated higher-boiling compound of column plate, by regulating reflux ratio to make to reflux to control the described quality except the titanium tetrachloride after vanadium by backflow charging opening through the condensed partial condensation thing of air cooler.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107758732A (en) * | 2017-11-30 | 2018-03-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Crude titanic chloride is refined to remove vanadium method |
| CN107857295A (en) * | 2017-11-13 | 2018-03-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Organic matter removes vanadium mud energy saving resources Application way and device |
| CN109956498A (en) * | 2019-04-29 | 2019-07-02 | 渤海大学 | A kind of crude titanic chloride efficiently removes vanadium compounding organic matter and preparation method thereof |
| CN110372033A (en) * | 2019-08-19 | 2019-10-25 | 中国恩菲工程技术有限公司 | Titanium dioxide synthesis system |
| CN112410582A (en) * | 2020-10-30 | 2021-02-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Organic matter refining vanadium-removing slurry treatment process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107857295A (en) * | 2017-11-13 | 2018-03-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Organic matter removes vanadium mud energy saving resources Application way and device |
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| CN110372033A (en) * | 2019-08-19 | 2019-10-25 | 中国恩菲工程技术有限公司 | Titanium dioxide synthesis system |
| CN112410582A (en) * | 2020-10-30 | 2021-02-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Organic matter refining vanadium-removing slurry treatment process |
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