CN103613126B - A kind of method and system removing vanadium impurity from titanic tetrachloride - Google Patents
A kind of method and system removing vanadium impurity from titanic tetrachloride Download PDFInfo
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Abstract
A kind of method and system removing vanadium impurity from titanic tetrachloride, this system is by crude titanic chloride gravitation tank, charging pump I, forced circulation pump, forced circulation pump groove, heating heat exchanger, flash tank, purification tower, condensing heat exchanger, titanium-tetrachloride storage tank, lipid acid gravitation tank, slush-pit launder and charging pump II form, method is: crude titanic chloride and lipid acid are squeezed in forced circulation pump groove, then squeeze into heating heat exchanger and carry out reduction reaction, the titanium tetrachloride slurries obtained containing dichloro vanadyl suspended solid enter flash tank, flash separation, containing dichloro vanadyl solid mud through draining into forced circulation pump groove, gaseous titanium tetrachloride enters purification tower, purification tower includes dichloro vanadyl solid mud and drains into forced circulation pump groove, and gaseous titanium tetrachloride enters condensing heat exchanger, obtains the titanium tetrachloride except vanadium.Advantage is: the fouling and the line clogging that decrease equipment; Improve production production capacity, reduce energy consumption, except vanadium efficiency is high, constant product quality.
Description
Technical field
The present invention relates to a kind of method and system removing vanadium impurity from titanic tetrachloride.
Background technology
Titanium tetrachloride is the main raw material producing titanium sponge and titanium dioxide, and the quality of titanium tetrachloride quality will directly affect the quality of titanium sponge and titanium dioxide.Usually, vanadium exists with the form of vanadium oxytrichloride in titanium tetrachloride, and its boiling point, a little less than titanium tetrachloride, adopts the method for distillation that the vanadium in crude titanic chloride is difficult to removing.
At present, thick titanium removes vanadium technique and mainly contains aluminium powder method, hydrogen sulfide method, copper wire method and organism method.Organism is except vanadium, and process operation is more stable, implements than being easier to, and both at home and abroad in recent years by popularity, especially in the U.S., Japan and other countries, generally adopts mineral oil except vanadium.In recent years technique was continued to optimize although domestic, steam consumption also has certain amplitude to reduce, but along with titanium white overall throughput popularization, mineral oil is except the production equipment floor space of vanadium is large, production production capacity is low, the consumption of steam is high, day by day highlights with the front and back unmatched contradiction of operation production capacity.
Mineral oil is except vanadium, and chemical reaction efficiency is low, and when production capacity improves, except vanadium index is unstable, and mineral oil usage quantity is high, easy blocking pipeline and interchanger, causes and produces instability.Organism, except vanadium, for ensureing the stability except vanadium index, needs to ensure that reactive system liquid has certain solid content and runs, in industry, production technique adopts liquid titanium tetrachloride heat exchange in heating coil and still, heating coil scale velocity is fast, and heat exchange efficiency is low, and the cycle of operation is short.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of interchanger good antiscale property, pipeline does not block, except vanadium efficiency is high, the method and system of the removal vanadium impurity from titanic tetrachloride of administration measure, this system device takes up an area small scale, heat exchange efficiency is high, and steam consumption is low, and production production capacity is large.
Technical solution of the present invention is:
Remove a method for vanadium impurity from titanic tetrachloride, its concrete steps are as follows:
(1), crude titanic chloride is squeezed in forced circulation pump groove by crude titanic chloride gravitation tank by charging pump I, lipid acid is squeezed in forced circulation pump groove by lipid acid gravitation tank by charging pump II, and the mass ratio of described crude titanic chloride and lipid acid is 1100:1 ~ 1400:1;
(2), the crude titanic chloride in forced circulation pump groove and lipid acid are squeezed into heating heat exchanger by forced circulation pump and are heated to 140 DEG C ~ 170 DEG C by forced circulation pump, the flow velocity of crude titanic chloride in heating heat exchanger is 0.8m/s ~ 2.0m/s, in circulating-heating process, mix with lipid acid and carry out reduction reaction, obtain the titanium tetrachloride slurries containing dichloro vanadyl suspended solid;
(3) the titanium tetrachloride slurries, containing dichloro vanadyl suspended solid enter flash tank, flash separation under 140 DEG C ~ 170 DEG C temperature, 80kpa ~ 200kpa pressure, liquid titanium tetrachloride flash distillation is gaseous titanium tetrachloride, drain into forced circulation pump groove through the mud mouth d of flash tank by the opening for feed b of forced circulation pump groove containing dichloro vanadyl solid mud, gaseous titanium tetrachloride enters purification tower by the discharge port f of flash tank by the opening for feed h of purification tower;
(4), purification tower tower top spray titanium tetrachloride, wherein, the reflux ratio of spray is 1:5 ~ 1:15, the titanium tetrachloride secondary of flash distillation carries out reduction reaction, what obtain drains into forced circulation pump groove through the mud mouth g of purification tower by the opening for feed b of forced circulation pump groove containing dichloro vanadyl solid mud, in purification tower, gaseous titanium tetrachloride enters condensing heat exchanger by purification tower discharge port i, obtains the titanium tetrachloride except vanadium, delivers in titanium-tetrachloride storage tank and store;
(5), flash tank and purification tower enter forced circulation pump groove containing dichloro vanadyl solid mud with squeezed into the crude titanic chloride of forced circulation pump groove by charging pump I and be forced recycle pump by the lipid acid batch mixing that charging pump II squeezes into forced circulation pump groove and squeeze into heating heat exchanger and slush-pit launder respectively, wherein, the crude titanic chloride lipid acid dichloro vanadyl solid mud batch mixing squeezing into slush-pit launder is 1:5 ~ 1:20 with the mass ratio of the crude titanic chloride and fatty acid total amount of squeezing into forced circulation pump groove, crude titanic chloride in heating heat exchanger and lipid acid continue to carry out reduction reaction by step (2).
During heating heat exchanger heating, pass into high pressure steam as heating medium at the shell side of heating heat exchanger, heating steam pressure is 0.5Mpa ~ 0.8Mpa.
The unsaturated straight chain fatty acid that described lipid acid is degree of unsaturation is 1 ~ 3, carbon atom number is 10 ~ 30.
Step (2) is 10% ~ 25% containing the solid content containing dichloro vanadyl suspended solid in the titanium tetrachloride slurries of dichloro vanadyl suspended solid.
A kind of removal vanadium impurity from titanic tetrachloride system, there is crude titanic chloride gravitation tank, its special character is: described crude titanic chloride gravitation tank is connected with the opening for feed a of forced circulation pump groove by pipeline, pipeline between described crude titanic chloride gravitation tank and forced circulation pump groove is provided with charging pump I, the discharge port c of described forced circulation pump groove is connected by pipeline with heating heat exchanger, pipeline between described forced circulation pump groove and heating heat exchanger is provided with forced circulation pump, the discharge port of described forced circulation pump is also connected with slush-pit launder, described heating heat exchanger is connected with the opening for feed e of flash tank, the discharge port f of described flash tank is connected with the opening for feed h of purification tower, the mud mouth d of described flash tank is connected with the opening for feed b of forced circulation pump groove, the discharge port i of described purification tower is connected with condensing heat exchanger, described condensing heat exchanger is connected with titanium-tetrachloride storage tank, the mud mouth g of described purification tower is connected with the opening for feed b of forced circulation pump groove, the opening for feed b of described forced circulation pump groove is also connected with lipid acid gravitation tank by pipeline, pipeline between described forced circulation pump groove and lipid acid gravitation tank is provided with charging pump II.
Beneficial effect of the present invention:
(1) lipid acid, adopted carries out except vanadium, due to its chemical property, to have decomposition rate fast, decompose the carbon dust activity produced high, in vanadium process, the effective rate of utilization of lipid acid is high, therefore, in system operation, the lipid acid amount of allocating into is low, except vanadium efficiency is high, system can be made to keep low-solid content to run and just can reach stablizing except vanadium effect, thus also reduce fouling and the line clogging of heating heat exchanger;
(2), organism lipid acid joins in well heater by forced circulation pump, saves the Preblend device of organism and crude titanic chloride, has the advantages that to take up an area small scale; Further, by the turbine effect of forced circulation pump, crude titanic chloride and the abundant premix of lipid acid can be made, prevent fouling and the line clogging of heating heat exchanger; Adopt forced circulation pump feeding and heating heat exchanger heating, can carry out reduction except vanadium at heating heat exchanger, forced circulation pump continuous print is discharged containing vanadium mud, ensure that the solid content of whole system is stablized, improve production production capacity, reduce steam consumption, make quality product more stable;
(3) flash tank is utilized, while realizing solid-liquid separation, the saturated titanium tetrachloride vapors that flash distillation produces enters purification tower condensation heat release to liquid titanium tetrachloride heating double evaporation-cooling in tower reactor, both reach gas, liquid, solid and be separated object, again reduce energy consumption, purify through secondary spraying in purification tower, except vanadium efficiency improves further, obtained titanium tetrachloride content of vanadium is less than 0.001%, iron level is less than 0.00087%, and Fe content is less than 0.0002%, and colourity is lower than 10mg/l, solid content is 0, can meet downstream industry titanium dioxide and titanium sponge production index request.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
In figure: 1-crude titanic chloride gravitation tank, 2-charging pump I, 3-forced circulation pump, 4-forced circulation pump groove, 5-heating heat exchanger, 6-flash tank, 7-purification tower, 8-condensing heat exchanger, 9-titanium-tetrachloride storage tank, 10-lipid acid gravitation tank, 11-slush-pit launder, 12-charging pump II.
Embodiment
embodiment 1
As shown in the figure, this removal vanadium impurity from titanic tetrachloride system, there is crude titanic chloride gravitation tank 1, described crude titanic chloride gravitation tank 1 is connected with the opening for feed a of forced circulation pump groove 4 by pipeline, pipeline between described crude titanic chloride gravitation tank 1 and forced circulation pump groove 4 is provided with charging pump I 2, the discharge port c of described forced circulation pump groove 4 is connected by pipeline with heating heat exchanger 5, pipeline between described forced circulation pump groove 4 and heating heat exchanger 5 is provided with forced circulation pump 3, the discharge port of described forced circulation pump 3 is also connected with slush-pit launder 11, described heating heat exchanger 5 is connected with the opening for feed e of flash tank 6, the discharge port f of described flash tank 6 is connected with the opening for feed h of purification tower 7, the mud mouth d of described flash tank 6 is connected with the opening for feed b of forced circulation pump groove 4, the discharge port i of described purification tower 7 is connected with condensing heat exchanger 8, described condensing heat exchanger 8 is connected with titanium-tetrachloride storage tank 9, the mud mouth g of described purification tower 7 is connected with the opening for feed b of forced circulation pump groove 4, the opening for feed b of described forced circulation pump groove 4 is also connected with lipid acid gravitation tank 10 by pipeline, pipeline between described forced circulation pump groove 4 and lipid acid gravitation tank 10 is provided with charging pump II 12.
During production, concrete steps are as follows:
(1), crude titanic chloride is squeezed in forced circulation pump groove 4 by crude titanic chloride gravitation tank 1 by charging pump I 2, lipid acid is squeezed in forced circulation pump groove 4 by lipid acid gravitation tank 10 by charging pump II 12, the mass ratio of described crude titanic chloride and lipid acid is 1100:1, wherein, the unsaturated straight chain fatty acid that lipid acid is degree of unsaturation is 1 ~ 3, carbon atom number is 10 ~ 30;
(2), the crude titanic chloride in forced circulation pump groove 4 is squeezed into heating heat exchanger 5 by forced circulation pump 3 and is heated to 140 DEG C by forced circulation pump 3, during heating heat exchanger heating, high pressure steam is passed into as heating medium at the shell side of heating heat exchanger, heating steam pressure is 0.8Mpa, the flow velocity of crude titanic chloride in heating heat exchanger 5 is 0.8m/s, in circulating-heating process, mix with lipid acid and carry out reduction reaction, obtain the titanium tetrachloride slurries containing dichloro vanadyl suspended solid;
(3) the titanium tetrachloride slurries, containing dichloro vanadyl suspended solid enter flash tank 6, flash separation under 140 DEG C of temperature, 80kpa pressure, liquid titanium tetrachloride flash distillation is gaseous titanium tetrachloride, drain into forced circulation pump groove 4 through the mud mouth d of flash tank 6 by the opening for feed b of forced circulation pump groove 4 containing dichloro vanadyl solid mud, gaseous titanium tetrachloride enters purification tower 7 by the discharge port f of flash tank 6 by the opening for feed h of purification tower 7;
(4), purification tower 7 tower top spray titanium tetrachloride, wherein, the reflux ratio of spray is 1:5, the titanium tetrachloride secondary of flash distillation carries out reduction reaction, what obtain drains into forced circulation pump groove 4 through the mud mouth g of purification tower 7 by the opening for feed b of forced circulation pump groove 4 containing dichloro vanadyl solid mud, in purification tower 7, gaseous titanium tetrachloride enters condensing heat exchanger 8 by purification tower 7 discharge port i, obtains the titanium tetrachloride except vanadium, delivers in titanium-tetrachloride storage tank 9 and stores;
(5), flash tank 6 and purification tower 7 enter forced circulation pump groove 4 containing dichloro vanadyl solid mud with squeezed into the crude titanic chloride of forced circulation pump groove 4 by charging pump I 2 and be forced recycle pump 3 by the lipid acid batch mixing that charging pump II 12 squeezes into forced circulation pump groove 4 and squeeze into heating heat exchanger 5 and slush-pit launder 11 respectively, wherein, the crude titanic chloride lipid acid dichloro vanadyl solid mud batch mixing squeezing into slush-pit launder 11 is 1:5 with the mass ratio of the crude titanic chloride and fatty acid total amount of squeezing into forced circulation pump groove 4, in (guaranteeing that containing dichloro vanadyl suspended solid solid content in step (2) is 10% ~ 15% scope fluctuation) slush-pit launder 11, mud can return continuously or by phased manner in chlorination furnace or dust-precipitator and reclaim, crude titanic chloride in heating heat exchanger 5 and lipid acid continue to carry out reduction reaction by step (2),
The titanium tetrachloride yield except vanadium that step (4) obtains is 98.2%, and steam mono-consumption is 130kg/ ton titanium tetrachloride, colourity < 10mg/L, and after testing, before and after titanium tetrachloride vanadium removal, the content of each component is as shown in table 1:
Table 1 crude titanic chloride and each constituent mass degree of titanium tetrachloride after removing vanadium
Embodiment 2
This removal vanadium impurity from titanic tetrachloride system is with embodiment 1.
During production, concrete steps are as follows:
(1), crude titanic chloride is squeezed in forced circulation pump groove 4 by crude titanic chloride gravitation tank 1 by charging pump I 2, lipid acid is squeezed in forced circulation pump groove 4 by lipid acid gravitation tank 10 by charging pump II 12, the mass ratio of described crude titanic chloride and lipid acid is 1400:1, wherein, the unsaturated straight chain fatty acid that lipid acid is degree of unsaturation is 1 ~ 3, carbon atom number is 10 ~ 30;
(2), the crude titanic chloride in forced circulation pump groove 4 is squeezed into heating heat exchanger 5 by forced circulation pump 3 and is heated to 170 DEG C by forced circulation pump 3, during heating heat exchanger heating, high pressure steam is passed into as heating medium at the shell side of heating heat exchanger, heating steam pressure is 0.6Mpa, the flow velocity of crude titanic chloride in heating heat exchanger 5 is 2.0m/s, in circulating-heating process, mix with lipid acid and carry out reduction reaction, obtain the titanium tetrachloride slurries containing dichloro vanadyl suspended solid;
(3) the titanium tetrachloride slurries, containing dichloro vanadyl suspended solid enter flash tank 6, flash separation under 170 DEG C of temperature, 130kpa pressure, liquid titanium tetrachloride flash distillation is gaseous titanium tetrachloride, drain into forced circulation pump groove 4 through the mud mouth d of flash tank 6 by the opening for feed b of forced circulation pump groove 4 containing dichloro vanadyl solid mud, gaseous titanium tetrachloride enters purification tower 7 by the discharge port f of flash tank 6 by the opening for feed h of purification tower 7;
(4), purification tower 7 tower top spray titanium tetrachloride, wherein, the reflux ratio of spray is 1:10, the titanium tetrachloride secondary of flash distillation carries out reduction reaction, what obtain drains into forced circulation pump groove 4 through the mud mouth g of purification tower 7 by the opening for feed b of forced circulation pump groove 4 containing dichloro vanadyl solid mud, in purification tower 7, gaseous titanium tetrachloride enters condensing heat exchanger 8 by purification tower 7 discharge port i, obtains the titanium tetrachloride except vanadium, delivers in titanium-tetrachloride storage tank 9 and stores;
(5), flash tank 6 and purification tower 7 enter forced circulation pump groove 4 containing dichloro vanadyl solid mud with squeezed into the crude titanic chloride of forced circulation pump groove 4 by charging pump I 2 and be forced recycle pump 3 by the lipid acid batch mixing that charging pump II 12 squeezes into forced circulation pump groove 4 and squeeze into heating heat exchanger 5 and slush-pit launder 11 respectively, wherein, the crude titanic chloride lipid acid dichloro vanadyl solid mud batch mixing squeezing into slush-pit launder 11 is 1:20 with the mass ratio of the crude titanic chloride and fatty acid total amount of squeezing into forced circulation pump groove 4, in (guaranteeing that containing dichloro vanadyl suspended solid solid content in step (2) is 20% ~ 25% scope fluctuation) slush-pit launder 11, mud can return continuously or by phased manner in chlorination furnace or dust-precipitator and reclaim, crude titanic chloride in heating heat exchanger 5 and lipid acid continue to carry out reduction reaction by step (2).
The titanium tetrachloride yield except vanadium that step (4) obtains is 98.5%, and steam mono-consumption is 150kg/ ton titanium tetrachloride, colourity < 10mg/L, and after testing, before and after titanium tetrachloride vanadium removal, the content of each component is as shown in table 2:
Table 2 crude titanic chloride and each constituent mass degree of titanium tetrachloride after removing vanadium
Embodiment 3
This removal vanadium impurity from titanic tetrachloride system is with embodiment 1.
During production, concrete steps are as follows:
(1), crude titanic chloride is squeezed in forced circulation pump groove 4 by crude titanic chloride gravitation tank 1 by charging pump I 2, lipid acid is squeezed in forced circulation pump groove 4 by lipid acid gravitation tank 10 by charging pump II 12, the mass ratio of described crude titanic chloride and lipid acid is 1200:1, wherein, the unsaturated straight chain fatty acid that lipid acid is degree of unsaturation is 1 ~ 3, carbon atom number is 10 ~ 30;
(2), the crude titanic chloride in forced circulation pump groove 4 is squeezed into heating heat exchanger 5 by forced circulation pump 3 and is heated to 150 DEG C by forced circulation pump 3, during heating heat exchanger heating, high pressure steam is passed into as heating medium at the shell side of heating heat exchanger, heating steam pressure is 0.5Mpa, the flow velocity of crude titanic chloride in heating heat exchanger 5 is 1.5m/s, in circulating-heating process, mix with lipid acid and carry out reduction reaction, obtain the titanium tetrachloride slurries containing dichloro vanadyl suspended solid;
(3) the titanium tetrachloride slurries, containing dichloro vanadyl suspended solid enter flash tank 6, flash separation under 155 DEG C of temperature, 200Kpa pressure, liquid titanium tetrachloride flash distillation is gaseous titanium tetrachloride, drain into forced circulation pump groove 4 through the mud mouth d of flash tank 6 by the opening for feed b of forced circulation pump groove 4 containing dichloro vanadyl solid mud, gaseous titanium tetrachloride enters purification tower 7 by the discharge port f of flash tank 6 by the opening for feed h of purification tower 7;
(4), purification tower 7 tower top spray titanium tetrachloride, wherein, the reflux ratio of spray is 1:15, the titanium tetrachloride secondary of flash distillation carries out reduction reaction, what obtain drains into forced circulation pump groove 4 through the mud mouth g of purification tower 7 by the opening for feed b of forced circulation pump groove 4 containing dichloro vanadyl solid mud, in purification tower 7, gaseous titanium tetrachloride enters condensing heat exchanger 8 by purification tower 7 discharge port i, obtains the titanium tetrachloride except vanadium, delivers in titanium-tetrachloride storage tank 9 and stores;
(5), flash tank 6 and purification tower 7 enter forced circulation pump groove 4 containing dichloro vanadyl solid mud with squeezed into the crude titanic chloride of forced circulation pump groove 4 by charging pump I 2 and be forced recycle pump 3 by the lipid acid batch mixing that charging pump II 12 squeezes into forced circulation pump groove 4 and squeeze into heating heat exchanger 5 and slush-pit launder 11 respectively, wherein, the crude titanic chloride lipid acid dichloro vanadyl solid mud batch mixing squeezing into slush-pit launder 11 is 1:12 with the mass ratio of the crude titanic chloride and fatty acid total amount of squeezing into forced circulation pump groove 4, in (guaranteeing that containing dichloro vanadyl suspended solid solid content in step (2) is 15% ~ 20% scope fluctuation) slush-pit launder 11, mud can return continuously or by phased manner in chlorination furnace or dust-precipitator and reclaim, crude titanic chloride in heating heat exchanger 5 and lipid acid continue to carry out reduction reaction by step (2).
The titanium tetrachloride yield except vanadium that step (4) obtains is 97.8%, and steam mono-consumption is 160kg/ ton titanium tetrachloride, colourity < 10mg/L, and after testing, before and after titanium tetrachloride vanadium removal, the content of each component is as shown in table 3:
Table 3 crude titanic chloride and each constituent mass degree of titanium tetrachloride after removing vanadium
| TiCl 4 | Fe | Mn | V | Solid | |
| Crude titanic chloride | 98.5 | 0.087 | 0.03 | 0.26 | 0.5 |
| Titanium tetrachloride | 99.9 | ＜0.0087 | ＜0.0002 | ＜0.0004 | Nothing |
Claims (4)
1. remove a method for vanadium impurity from titanic tetrachloride, it is characterized in that: concrete steps are as follows:
(1), adopt and remove vanadium impurity from titanic tetrachloride system, there is crude titanic chloride gravitation tank, described crude titanic chloride gravitation tank is connected with the opening for feed a of forced circulation pump groove by pipeline, pipeline between described crude titanic chloride gravitation tank and forced circulation pump groove is provided with charging pump I, the discharge port c of described forced circulation pump groove is connected by pipeline with heating heat exchanger, pipeline between described forced circulation pump groove and heating heat exchanger is provided with forced circulation pump, the discharge port of described forced circulation pump is also connected with slush-pit launder, described heating heat exchanger is connected with the opening for feed e of flash tank, the discharge port f of described flash tank is connected with the opening for feed h of purification tower, the mud mouth d of described flash tank is connected with the opening for feed b of forced circulation pump groove, the discharge port i of described purification tower is connected with condensing heat exchanger, described condensing heat exchanger is connected with titanium-tetrachloride storage tank, the mud mouth g of described purification tower is connected with the opening for feed b of forced circulation pump groove, the opening for feed b of described forced circulation pump groove is also connected with lipid acid gravitation tank by pipeline, pipeline between described forced circulation pump groove and lipid acid gravitation tank is provided with charging pump II,
Crude titanic chloride is squeezed in forced circulation pump groove by crude titanic chloride gravitation tank by charging pump I, lipid acid is squeezed in forced circulation pump groove by lipid acid gravitation tank by charging pump II, and the mass ratio of described crude titanic chloride and lipid acid is 1100:1 ~ 1400:1; The unsaturated straight chain fatty acid that described lipid acid is degree of unsaturation is 1 ~ 3, carbon atom number is 10 ~ 30;
(2), the crude titanic chloride in forced circulation pump groove and lipid acid are squeezed into heating heat exchanger by forced circulation pump and are heated to 140 DEG C ~ 170 DEG C by forced circulation pump, the flow velocity of crude titanic chloride in heating heat exchanger is 0.8m/s ~ 2.0m/s, in circulating-heating process, mix with lipid acid and carry out reduction reaction, obtain the titanium tetrachloride slurries containing dichloro vanadyl suspended solid;
(3) the titanium tetrachloride slurries, containing dichloro vanadyl suspended solid enter flash tank, flash separation under 140 DEG C ~ 170 DEG C temperature, 80kpa ~ 200kpa pressure, liquid titanium tetrachloride flash distillation is gaseous titanium tetrachloride, drain into forced circulation pump groove through the mud mouth d of flash tank by the opening for feed b of forced circulation pump groove containing dichloro vanadyl solid mud, gaseous titanium tetrachloride enters purification tower by the discharge port f of flash tank by the opening for feed h of purification tower;
(4), purification tower tower top spray titanium tetrachloride, wherein, the reflux ratio of spray is 1:5 ~ 1:15, the titanium tetrachloride secondary of flash distillation carries out reduction reaction, what obtain drains into forced circulation pump groove through the mud mouth g of purification tower by the opening for feed b of forced circulation pump groove containing dichloro vanadyl solid mud, in purification tower, gaseous titanium tetrachloride enters condensing heat exchanger by purification tower discharge port i, obtains the titanium tetrachloride except vanadium, delivers in titanium-tetrachloride storage tank and store;
(5), flash tank and purification tower enter forced circulation pump groove containing dichloro vanadyl solid mud with squeezed into the crude titanic chloride of forced circulation pump groove by charging pump I and be forced recycle pump by the lipid acid batch mixing that charging pump II squeezes into forced circulation pump groove and squeeze into heating heat exchanger and slush-pit launder respectively, wherein, the crude titanic chloride lipid acid dichloro vanadyl solid mud batch mixing squeezing into slush-pit launder is 1:5 ~ 1:20 with the mass ratio of the crude titanic chloride and fatty acid total amount of squeezing into forced circulation pump groove, crude titanic chloride in heating heat exchanger and lipid acid continue to carry out reduction reaction by step (2).
2. the method for removal vanadium impurity from titanic tetrachloride according to claim 1, is characterized in that: during heating heat exchanger heating, pass into high pressure steam as heating medium at the shell side of heating heat exchanger, heating steam pressure is 0.5Mpa ~ 0.8Mpa.
3. the method for removal vanadium impurity from titanic tetrachloride according to claim 1, is characterized in that: step (2) is 10% ~ 25% containing the solid content containing dichloro vanadyl suspended solid in the titanium tetrachloride slurries of dichloro vanadyl suspended solid.
4. remove vanadium impurity from titanic tetrachloride system for one kind, there is crude titanic chloride gravitation tank, it is characterized in that: described crude titanic chloride gravitation tank is connected with the opening for feed a of forced circulation pump groove by pipeline, pipeline between described crude titanic chloride gravitation tank and forced circulation pump groove is provided with charging pump I, the discharge port c of described forced circulation pump groove is connected by pipeline with heating heat exchanger, pipeline between described forced circulation pump groove and heating heat exchanger is provided with forced circulation pump, the discharge port of described forced circulation pump is also connected with slush-pit launder, described heating heat exchanger is connected with the opening for feed e of flash tank, the discharge port f of described flash tank is connected with the opening for feed h of purification tower, the mud mouth d of described flash tank is connected with the opening for feed b of forced circulation pump groove, the discharge port i of described purification tower is connected with condensing heat exchanger, described condensing heat exchanger is connected with titanium-tetrachloride storage tank, the mud mouth g of described purification tower is connected with the opening for feed b of forced circulation pump groove, the opening for feed b of described forced circulation pump groove is also connected with lipid acid gravitation tank by pipeline, pipeline between described forced circulation pump groove and lipid acid gravitation tank is provided with charging pump II.
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| CN104058451A (en) * | 2014-07-07 | 2014-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium removing system and method for crude titanium tetrachloride refining |
| CN105271383B (en) * | 2015-11-05 | 2017-06-30 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of the organic reagent and titanium tetrachloride vanadium removal for except vanadium |
| 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 |
| CN109052462A (en) * | 2018-10-30 | 2018-12-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Crude titanic chloride purification removes vanadium method |
| CN110054217B (en) * | 2019-04-29 | 2022-01-04 | 渤海大学 | Compound organic matter for quickly removing vanadium from crude titanium tetrachloride and preparation method thereof |
| CN110040772B (en) * | 2019-04-29 | 2021-10-08 | 渤海大学 | Compound organic matter for stably removing vanadium from crude titanium tetrachloride and preparation method thereof |
| CN112645381A (en) * | 2020-12-31 | 2021-04-13 | 仙桃市中星电子材料有限公司 | Method for reducing carbon content in titanium tetrachloride |
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| US20130299335A1 (en) * | 2011-02-23 | 2013-11-14 | E I Du Pont De Nemours And Company | PURIFICATION OF TiCl4 THROUGH THE PRODUCTION OF NEW CO-PRODUCTS |
| CN103011269A (en) * | 2012-12-29 | 2013-04-03 | 锦州钛业有限公司 | Process and system for purifying titanium tetrachloride by removing vanadium |
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| CN103613126A (en) | 2014-03-05 |
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