CN103936062B - 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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- CN103936062B CN103936062B CN201410160740.1A CN201410160740A CN103936062B CN 103936062 B CN103936062 B CN 103936062B CN 201410160740 A CN201410160740 A CN 201410160740A CN 103936062 B CN103936062 B CN 103936062B
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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 crude titanic chloride organism are except the method for vanadium.
Background technology
Crude titanic chloride is a kind of turbid solution very complicated containing plurality of impurities, composition, and in the production process of refining titanic chloride, the vanadium compound impurity in removing crude titanic chloride is an important step of titanium sponge production.
It is refine and removing vanadium technique more advanced both at home and abroad at present that organism removes vanadium, and general technical process is first by thick TiCl
4add in mixing tank respectively by a certain percentage stir with except vanadium organism (as mineral wet goods), then add in still kettle and be heated to temperature of reaction and generate solid-state vanadium precipitation, thus reach the object except vanadium.But in this process, thick TiCl
4separate with reacting by heating process with except the organic mixing process of vanadium, be unfavorable for the serialization except vanadium, add the configuration of operating time and personnel.
Summary of the invention
For deficiency of the prior art, what the object of the invention is in solving the problems of the technologies described above is one or more.
The object of the present invention is to provide and a kind ofly improve organism except the efficiency of vanadium and to simplify except the organism of vanadium device is except vanadium treating tower and crude titanic chloride organism are except the method for 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 vertically disposed cylindrical shell and described treating tower comprises the fluidisation hybrid reaction section of bottom, the breeze way at middle part and the rectifying section on top, wherein, fluidisation hybrid reaction section is used for except vanadium organism mixes with the fluidisation treated except vanadium gas and reacts, described fluidisation hybrid reaction section comprises the slurry outlet being arranged on bottom, be arranged on the organism entrance of side wall upper part, the gas feed being arranged on lower sidewall and the gas distributor be arranged in fluidisation hybrid reaction section, the entrance of described gas distributor is communicated with gas feed to be treated except vanadium gas to spray in fluidisation hybrid reaction section, breeze way connects described fluidisation hybrid reaction section and rectifying section, rectifying section is used for the removal of impurities except gas after vanadium, the polylith column plate that described rectifying section comprises the pneumatic outlet being arranged on top, the backflow charging opening being arranged on side wall upper part and is arranged in rectifying section.
According to the embodiment of organism of the present invention except vanadium treating tower, described gas feed and organism entrance are relatively arranged.
According to the embodiment of organism of the present invention except vanadium treating tower, described gas distributor comprises 8 ~ 13 inlet pipe, every root inlet pipe is uniformly distributed 40 ~ 70 nozzles.
According to the embodiment of organism of the present invention except vanadium treating tower, the setting position of described gas distributor should be guaranteed to treat can not have described gas distributor except vanadium gas and except vanadium organism reacts the vanadium slurry sediment that contains generated.
According to the embodiment of organism of the present invention except vanadium treating tower, described gas distributor is apart from the bottom 1500 ~ 1800mm of described fluidisation hybrid reaction section.
According to the embodiment of organism of the present invention except vanadium treating tower, the quantity of described column plate is 2 ~ 10.
According to the embodiment of organism of the present invention except vanadium treating tower, treat except vanadium gas with pass into from organism entrance except vanadium organism fluidisation in fluidisation hybrid reaction section mix and react generate contain vanadium slurry sediment, described contain vanadium slurry sediment discharge from slurry outlet; Reacted treating enters rectifying section except vanadium gas, makes be separated until the higher-boiling compound in vanadium gas and obtain gas after except vanadium by regulating the temperature at rectifying section top.
Another aspect provides a kind of crude titanic chloride organism except the method for vanadium, described method adopt above-mentioned organism except vanadium treating tower carry out crude titanic chloride except vanadium.
According to the embodiment of crude titanic chloride organism of the present invention except the method for vanadium, said method comprising the steps of: by temperature be 136 ~ 142 DEG C pass into fluidisation hybrid reaction section from organism entrance except vanadium organism, again crude titanic chloride gas is sprayed into fluidisation hybrid reaction section by gas feed and gas distributor, described mix except vanadium organism and crude titanic chloride are gas fluidized and react to generate contain vanadium slurry sediment; The temperature at described rectifying section top is regulated to be 135 ~ 138 DEG C, reacted crude titanic chloride gas enters rectifying section and is separated through column plate and enters aftertreatment device from pneumatic outlet after higher-boiling compound and obtain the titanium tetrachloride after except vanadium, higher-boiling compound and regularly being discharged by slurry outlet containing vanadium slurry sediment.
According to the embodiment of 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 is separated after higher-boiling compound through column plate and enters described air cooler condensation from pneumatic outlet, makes to reflux to control the described quality except the titanium tetrachloride after vanadium through the condensed partial condensation thing of air cooler by backflow charging opening by regulating reflux ratio.
The present invention utilize fluidization technique make to treat except vanadium gas with except vanadium organic mixing reaching full and uniform state, be conducive to except vanadium Adsorption of Organic is treated, except being conducive to heat and mass transport process between gas-liquid containing vanadium component in vanadium gas, improving and remove vanadium efficiency; In addition, crude titanic chloride with except vanadium organism can mix in the same apparatus while carry out reacting by heating, decrease the agitation mixer except vanadium organism and crude titanic chloride and step, more effectively reduce the outfit of operating time and personnel, reduce the cost of refining titanic chloride, there is popularizing application prospect widely.
Accompanying drawing explanation
Fig. 1 is the structural representation of organism except vanadium treating tower of exemplary embodiment of the present.
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, organism of the present invention is described with reference to the accompanying drawings in detail except vanadium treating tower and crude titanic chloride organism are except the method for vanadium.
Fig. 1 is the structural representation of organism except vanadium treating tower of exemplary embodiment of the present.
As shown in Figure 1, according to exemplary embodiment of the present invention, described organism is vertically disposed cylindrical shell and this treating tower comprises the fluidisation hybrid reaction section 1 of bottom except 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 except vanadium organism with the fluidisation treated except vanadium gas and react, rectifying section 2 is for the removal of impurities of 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 obtained after gas removal of impurities after vanadium, avoid organism to rise sharply on the impact of physical qualities after vanadium with liquid level in time removing vanadium gas reaction 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 arranged according to Production requirement.
Below each segment structure for the treatment of tower and function are specifically described.
Fluidisation hybrid reaction section 1 comprises the slurry outlet 7 being arranged on bottom, the organism entrance 6 being arranged on side wall upper part, the gas feed 5 being arranged on lower sidewall and the gas distributor (not shown) be arranged in fluidisation hybrid reaction section 1, and the entrance of gas distributor is communicated with gas feed 5 to be treated except vanadium gas to spray in fluidisation hybrid reaction section 1.Treat to enter fluidisation hybrid reaction section 1 in via gas feed 5 and gas distributor with certain speed and certain pressure except vanadium gas, except vanadium organism then passes in fluidisation hybrid reaction section 1 from organism entrance, two kinds of materials fluidisation in fluidisation hybrid reaction section 1 mixes, direct heating removes vanadium organism and also reacts generation containing after vanadium slurry sediment to temperature of reaction or by mixed heating material to temperature of reaction, reacted gaseous mixture then directly rises and enters rectifying section 2, and gained is then 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 be guaranteed to treat can not have gas distributor except vanadium gas and except vanadium organism reacts the vanadium slurry sediment that contains generated, according to one embodiment of present invention, bottom 1500 ~ the 1800mm of gas distributor distance fluidisation hybrid reaction section 1, but the present invention is not limited thereto, can 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, every root inlet pipe is uniformly distributed 40 ~ 70 nozzles, but the present invention is not limited thereto, because gas distributor is mainly used in treating except vanadium gas uniform distribution except vanadium gas to spray in fluidisation hybrid reaction section 1 with certain speed and certain pressure and makes to enter in tower by treating, thus be conducive to treating except vanadium gas and the Homogeneous phase mixing except vanadium organism liquid, as long as can realize above-mentioned functions, the present invention does not specifically limit its structure.
The polylith column plate (not shown) that rectifying section 2 comprises the pneumatic outlet 3 being arranged on top, the backflow charging opening 4 being arranged on side wall upper part and is arranged in rectifying section.Reacted treating enters in rectifying section 2 except vanadium gas, by regulate rectifying section 2 top temperature and via the separation of column plate, treat except the higher-boiling compound in vanadium gas is separated, then except gas after vanadium is then overflowed by pneumatic outlet 3 and enters aftertreatment device, higher-boiling compound then to stay in treating tower and with discharge from the slurry outlet 7 at the bottom of tower together with vanadium slurry sediment, thus complete the process of organism except vanadium.Wherein, column plate is the conventional components for the treatment of tower, it contacts for making two kinds of fluid in close and carries out the mass transter between two-phase, to reach the object of separation of liquid mixtures or components of gas mixtures, the present invention does not limit, as long as can realize basic heat exchange centrifugation the structure of column plate and quantity.According to the present invention, the quantity of column plate is 2 ~ 10.In addition, aftertreatment device of the present invention can be such as air cooler, then except the gas after vanadium enters air cooler condensation, then react by regulating reflux ratio to make to be back to continuation in treating tower through the condensed partial condensation thing of air cooler by backflow charging opening with the quality controlled except material after vanadium.
Crude titanic chloride organism of the present invention except the method for vanadium then adopt above-mentioned organism except vanadium treating tower carry out crude titanic chloride except vanadium, but above-mentioned organism except vanadium treating tower be not limited in crude titanic chloride except vanadium.
According to one embodiment of present invention, said method comprising the steps of: fluidisation hybrid reaction section will be passed into except vanadium organism from organism entrance, Heating temperature to 136 ~ 142 DEG C, again crude titanic chloride gas is sprayed into fluidisation hybrid reaction section by gas feed and gas distributor, mix except vanadium organism and crude titanic chloride are gas fluidized and react and generate containing vanadium slurry sediment; The temperature regulating rectifying section top is 135 ~ 138 DEG C, reacted crude titanic chloride gas enters rectifying section and after column plate separation higher-boiling compound, enters aftertreatment device from pneumatic outlet and obtains the titanium tetrachloride after except vanadium, higher-boiling compound and regularly being discharged by slurry outlet containing vanadium slurry sediment, thus realize to crude titanic chloride except vanadium process.
Wherein, making reaction and titanium tetrachloride gases after removal of impurities enters air cooler condensation via pneumatic outlet, making to be back in treating tower by backflow charging opening through the condensed partial condensation thing of air cooler by regulating reflux ratio to continue reaction to control the titanium tetrachloride quality after removing vanadium.The adjustment of reflux ratio specifically can realize by regulating the valve opening of return line, and the step of this adjustment reflux ratio should be carry out targetedly after being obtained by reacting the titanium tetrachloride after except vanadium and observe this shade and quality except the titanium tetrachloride after vanadium.
The present invention is described in detail below in conjunction with concrete example.
Example:
The internal diameter of the fluidisation hybrid reaction section for the treatment of tower is 4000mm, high 3500mm.The bottom 1800mm of gas distributor distance fluidisation hybrid reaction section, gas distributor comprises 9 inlet pipe and every root inlet pipe is uniformly distributed 55 nozzles.Column plate 5 is set in rectifying section.
Add except vanadium organism mineral oil by organism entrance, its flow is 0.05t/h, and will be heated to 140 DEG C; Pass into crude titanic chloride gas by gas feed and gas distributor, its flow is 10t/h.Crude titanic chloride gas enters fluidisation hybrid reaction Duan Houyu and reacts except vanadium organism and generate containing vanadium slurry sediment, reacted gas rises to rectifying section, the temperature at rectifying section top is controlled to be 137 DEG C simultaneously, after being separated via column plate, higher-boiling compound gets back to fluidisation hybrid reaction section, titanium tetrachloride gases and low-boiling compound then enter aftertreatment device from the pneumatic outlet of tower top and obtain except the titanium tetrachloride after vanadium, containing vanadium slurry sediment and higher-boiling compound then by slurry outlet discharge per hour.
Organism of the present invention, except vanadium treating tower novel structure, easy and simple to handle, has abandoned the method that conventional mixing of materials is separated with refining step, effectively reduces manning and simplified apparatus, improves production efficiency, have larger implementary value and economic results in society.
Although describe organism of the present invention except vanadium treating tower and crude titanic chloride organism are except the method for vanadium in conjunction with exemplary embodiment above, but those of ordinary skill in the art should be clear, when not departing from the spirit and scope of claim, various amendment can be carried out to above-described embodiment.
Claims (10)
1. organism is except a vanadium treating tower, it is characterized in that, described treating tower is vertically disposed cylindrical shell and described treating tower comprises the fluidisation hybrid reaction section of bottom, the breeze way at middle part and the rectifying section on top, wherein,
Fluidisation hybrid reaction section is used for except vanadium organism mixes with the fluidisation treated except vanadium gas and reacts, described fluidisation hybrid reaction section comprises the slurry outlet being arranged on bottom, the organism entrance being arranged on side wall upper part, the gas feed being arranged on lower sidewall and the gas distributor be arranged in fluidisation hybrid reaction section, and the entrance of described gas distributor is communicated with gas feed to be treated except vanadium gas to spray in fluidisation hybrid reaction section;
Breeze way connects described fluidisation hybrid reaction section and rectifying section;
Rectifying section is used for the removal of impurities except gas after vanadium, the polylith column plate that described rectifying section comprises the pneumatic outlet being arranged on top, the backflow charging opening being arranged on side wall upper part and is arranged in rectifying section.
2. organism according to claim 1 is except vanadium treating tower, and it is characterized in that, described gas feed and organism entrance are relatively arranged.
3. organism according to claim 1 is except vanadium treating tower, and it is characterized in that, described gas distributor comprises 8 ~ 13 inlet pipe, every root inlet pipe is uniformly distributed 40 ~ 70 nozzles.
4. organism according to claim 1 is except vanadium treating tower, it is characterized in that, the setting position of described gas distributor should be guaranteed to treat can not have described gas distributor except vanadium gas and except vanadium organism reacts the vanadium slurry sediment that contains generated.
5. organism according to claim 4 is except vanadium treating tower, and it is characterized in that, described gas distributor is apart from the bottom 1500 ~ 1800mm of described fluidisation hybrid reaction section.
6. organism according to claim 1 is except vanadium treating tower, and it 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 except vanadium gas with pass into from organism entrance except vanadium organism fluidisation in fluidisation hybrid reaction section mix and react generate contain vanadium slurry sediment, described contain vanadium slurry sediment discharge from slurry outlet; Reacted treating enters rectifying section except vanadium gas, makes be separated until the higher-boiling compound in vanadium gas and obtain gas after except vanadium by regulating the temperature at rectifying section top.
8. crude titanic chloride organism is except the method for vanadium, it is characterized in that, described method adopt the organism according to any one of claim 1 to 7 except vanadium treating tower carry out crude titanic chloride except vanadium.
9. crude titanic chloride organism according to claim 8 is except the method for vanadium, it is characterized in that, said method comprising the steps of:
By temperature be 136 ~ 142 DEG C pass into fluidisation hybrid reaction section from organism entrance except vanadium organism, again crude titanic chloride gas is sprayed into fluidisation hybrid reaction section by gas feed and gas distributor, described mix except vanadium organism and crude titanic chloride are gas fluidized and react to generate contain vanadium slurry sediment;
The temperature at described rectifying section top is regulated to be 135 ~ 138 DEG C, reacted crude titanic chloride gas enters rectifying section and is separated through column plate and enters aftertreatment device from pneumatic outlet after higher-boiling compound and obtain the titanium tetrachloride after except vanadium, higher-boiling compound and regularly being discharged 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 is separated after higher-boiling compound through column plate and enters described air cooler condensation from pneumatic outlet, makes to reflux to control the described quality except the titanium tetrachloride after vanadium through the condensed partial condensation thing of air cooler by backflow charging opening by regulating reflux ratio.
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| CN201410160740.1A CN103936062B (en) | 2014-04-21 | 2014-04-21 | Vanadium removal refining tower with organic matter and method for removing vanadium from crude titanium tetrachloride with organic matter |
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| CN201410160740.1A CN103936062B (en) | 2014-04-21 | 2014-04-21 | Vanadium removal refining tower with organic matter and method for removing vanadium from crude titanium tetrachloride with organic matter |
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Families Citing this family (4)
| 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 |
| 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 |
| CN109956498B (en) * | 2019-04-29 | 2021-08-03 | 渤海大学 | Compound organic matter for efficiently removing vanadium from crude titanium tetrachloride and preparation method thereof |
| CN112410582B (en) * | 2020-10-30 | 2022-09-20 | 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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