CN214528176U - Vanadium removal system of crude titanium tetrachloride - Google Patents

Vanadium removal system of crude titanium tetrachloride Download PDF

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Publication number
CN214528176U
CN214528176U CN202023005673.6U CN202023005673U CN214528176U CN 214528176 U CN214528176 U CN 214528176U CN 202023005673 U CN202023005673 U CN 202023005673U CN 214528176 U CN214528176 U CN 214528176U
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titanium tetrachloride
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crude titanium
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成文江
齐霁
王永和
孙德育
饶华进
杨雄武
杜严
杨英
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Bengbu Guoti Nano Material Co ltd
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Bengbu Zhongci Nano Technology Co ltd
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Abstract

The utility model relates to the technical field of titanium tetrachloride refining, in particular to a vanadium removal system of coarse titanium tetrachloride; the device comprises a coarse material storage unit, a heating unit, a cracking reduction unit, a circulating evaporation unit, a purification unit, a condensation unit and a fine material storage unit, wherein the circulating evaporation unit comprises a tank body and an underwater pump hermetically connected with the tank body; the organic matter extends from the outside and gets into the schizolysis reduction unit, the beneficial effects of the utility model are that: the refining process is simple and convenient, the separation efficiency is high, the vanadium removal effect is good, and the energy consumption of products is low.

Description

Vanadium removal system of crude titanium tetrachloride
Technical Field
The utility model relates to a titanium tetrachloride refining technology field, concretely relates to vanadium removal system of thick titanium tetrachloride.
Background
Titanium tetrachloride (TiCl)4) Is an important intermediate product for producing sponge titanium and titanium dioxide. Unpurified technical crude TiCl4Is a reddish brown turbid liquid containing many impurities, coarse TiCl4The medium impurity component is quite complex, with vanadium being coarse TiCl4Is one of the main impurity elements, which is VOCl3In which the form is present. VOCl3The medium oxygen element can enter the titanium sponge in four times of concentration after being reduced, so that the oxygen content in the titanium sponge is increased, the Brinell hardness is increased, and the titanium sponge is degraded. In addition, titanium tetrachloride with high vanadium content is used for producing titanium dioxide, so that the titanium dioxide is colored to influence the performance of the titanium dioxide. In order to ensure the product quality of the titanium sponge and the titanium dioxide produced by the chlorination process, the crude TiCl produced by the chlorination process must be treated4And removing vanadium.
The method for removing vanadium from organic substances (such as industrial white oil and fatty acid) is the mainstream method in the current industrial production, and the common vanadium removal processes are as follows: firstly, the organic matter is mixed with high-temperature coarse TiCl4Contact and generate cracking-reduction reaction in an evaporation tank at 130-138 ℃, and the obtained TiCl4Purifying and condensing the gas to form liquid fine titanium tetrachloride and collecting the liquid fine titanium tetrachloride; secondly, a gas-liquid-solid fluidized bed is arranged at the bottom of the purifying tower, and organic matters and coarse TiCl are mixed4The gas is contacted in a purifying tower and subjected to cracking-reduction reaction in a gas-liquid-solid fluidized bed to obtain TiCl4The gas is purified and condensed to form liquid fine titanium tetrachloride which is collected.
In the two vanadium removal processes, the cracking-reduction reaction is carried out under normal pressure (0-15KPa) and at lower temperature (120-140 ℃), and the defects are that: firstly, the organic substances with various and complex compositions can not be completely cracked into activated carbon particles under the conditions of normal pressure and lower temperature, and the organic substances with incomplete cracking can be accompanied with TiCl4The gas enters a subsequent treatment procedure, and needs a downstream rectifying tower to continuously remove color and purify to separate the gas from the gas, so that the impurity removal process is multiple, and the refining cost is high; second, to TiCl4When the mixture of the refined TiCl and the organic matter is heated, saturated steam with the temperature of more than 190 ℃ is required to be used, condensed water with the temperature of more than 170 ℃ is generated, and the residual heat is not utilized, so that the refined TiCl is refined4The thermal efficiency in the process is low; and thirdly, the condensation unit is only cooled by circulating water, the saturated vapor pressure of titanium tetrachloride at 50 ℃ is 5KPa, and the yield of titanium tetrachloride is not high.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a vanadium removal system for refining coarse titanium tetrachloride, which is simple and efficient.
A vanadium removal system for crude titanium tetrachloride comprises a crude material storage unit, a heating unit, a cracking reduction unit, a circulating evaporation unit, a purification unit, a condensation unit and a refined material storage unit, wherein the circulating evaporation unit comprises a tank body and an underwater pump hermetically connected with the tank body, a material outlet of the crude material storage unit is connected with an inlet of the heating unit, a liquid inlet and a liquid outlet of the cracking reduction unit are respectively connected with an outlet of the heating unit and a material inlet of the circulating evaporation unit, a gas phase inlet III and a gas phase outlet III of the purification unit are respectively connected with a gas phase outlet II of the circulating evaporation unit and an inlet of the condensation unit, and an outlet of the condensation unit is introduced into the refined material storage unit; the organic matter extends from the outside into the cracking reduction unit.
The utility model discloses preferred technical scheme, the heating unit is including preheating unit and overheated unit, and the material entry one and the liquid phase export one of preheating the unit link to each other with the material export of coarse fodder memory cell, the liquid phase entry one of circulation evaporation unit respectively, and the liquid phase entry two, the liquid outlet of overheated unit link to each other with the submerged pump outlet end on the circulation evaporation unit, the income liquid mouth of schizolysis reduction unit respectively, and steam passes through the pipeline and links to each other with overheated unit's steam inlet, still is equipped with the steam outlet who accesss to preheating unit and go up gaseous phase entry one on the overheated unit.
The utility model discloses preferred technical scheme, be equipped with the circulating pump on the pipeline that coarse fodder storage unit and preheating unit link to each other.
The utility model discloses preferred technical scheme, be equipped with the relief pressure valve on the pipeline that circulation evaporation unit and schizolysis reduction unit link to each other.
The utility model discloses preferred technical scheme, purification unit's three liquid phase exports and links to each other with circulation evaporation unit's three liquid phase entrances.
The utility model discloses preferred technical scheme, submerged pump exit end on the circulation evaporation unit still accesss to chlorination unit's material entry three.
The utility model discloses preferred technical scheme, the condensing unit includes one-level condensing equipment and second grade condensing equipment, and one-level condensing equipment's gaseous phase entry four links to each other with gaseous phase export three, second grade condensing equipment's gaseous phase entry five respectively with gaseous phase export four of purification unit, and one-level condensing equipment's liquid phase export four and second grade condensing equipment's liquid phase export five do not lets in the beneficiated burden material storage unit.
The utility model discloses preferred technical scheme, preheating unit is the pre-heater, the thick titanium tetrachloride of the tube side internal flow of pre-heater, the comdenstion water that the shell side internal flow of pre-heater comes out through the thermal unit.
The utility model discloses preferred technical scheme, the overheated unit is the heater, and thick titanium tetrachloride of the tube side internal circulation of heater, the shell side internal circulation high temperature steam of heater.
The utility model discloses preferred technical scheme, circulation evaporation unit include the evaporimeter and with evaporimeter sealing connection's submerged pump, the pump body of submerged pump stretches into the tank cavity of evaporimeter, and on the submerged pump was fixed in the tank body of evaporimeter through the flange, submerged pump exit end was located the outside of evaporimeter.
The utility model discloses preferred technical scheme, chlorination unit is chlorination furnace.
The utility model discloses preferred technical scheme, the schizolysis reduction unit is the reductor.
The utility model discloses preferred technical scheme, purification unit is plate column or packed tower.
The utility model discloses preferred technical scheme, one-level condensing equipment is the cooler, and coolant is the circulating water.
The utility model discloses preferred technical scheme, second grade condensing equipment is the cooler, and coolant is freezing salt solution.
Compared with the prior art, the beneficial effects of the utility model reside in that: the vanadium removal system of the crude titanium tetrachloride is provided, and through the system optimization design, vanadium-containing substances in the crude titanium tetrachloride can be removed more efficiently and thoroughly, and the yield of the titanium tetrachloride can be improved. Specifically, crude titanium tetrachloride firstly enters a heating unit for heating treatment, which is beneficial to improving the temperature of materials in a cracking reduction unit, so that organic matters can be rapidly and thoroughly cracked into super-active carbon particles under the catalysis of titanium tetrachloride, vanadium oxychloride in the titanium tetrachloride is instantaneously reduced into vanadium oxychloride, and the reacted mixed substance enters a circulating evaporation unit after being decompressed, purified and condensed to obtain high-quality titanium tetrachloride. The heating unit adopts a preheating and overheating two-stage heating system, hot steam generated in the gasification process can be recycled to the preheating unit for reuse, and the utilization efficiency of waste heat is improved. The circulating evaporation unit can promote the reduction of trivalent vanadium in the crude titanium tetrachloride and promote the separation of titanium tetrachloride and solid particles through evaporation. The condensation unit adopts a circulating water and brine two-stage condensation system, so that the yield of the titanium tetrachloride is improved.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings.
Referring to the attached figure 1, the vanadium removal system for crude titanium tetrachloride comprises a crude material storage unit 10, a circulating pump 20, a preheating unit 30, a circulating evaporation unit 40, a chlorination unit 50, a superheating unit 60, a pressure reducing valve 70, a cracking reduction unit 80, a purification unit 90, a primary condensing device 100, a secondary condensing device 110 and a fine material storage unit 120, wherein the circulating evaporation unit 40 comprises a tank body and a submerged pump hermetically connected with the tank body.
A material outlet 11 of the coarse material storage unit 10 is connected with a first material inlet 31 of the preheating unit 30, and a circulating pump is arranged on a connecting pipeline; a first liquid phase outlet 32 of the preheating unit 30 is connected with a first liquid phase inlet 41 of the circulating evaporation unit 40, a second liquid phase pump outlet end 42 on the circulating evaporation unit 40 is connected with a second liquid phase inlet 61 of the overheating unit 60, a liquid outlet 64 of the overheating unit 60 is connected with a liquid inlet 82 of the cracking reduction unit 80, a second liquid phase outlet 81 of the cracking reduction unit 80 is connected with a second material inlet 43 of the circulating evaporation unit 40, and a pressure reducing valve 70 is arranged on a pipeline connecting the cracking reduction unit 80 and the circulating evaporation unit 40; a second gas phase outlet 44 of the circulating evaporation unit 40 is connected with a third gas phase inlet 91 of the purification unit 90, a third gas phase outlet 92 of the purification unit 90 is connected with a fourth gas phase inlet 101 of the first-stage condensation device 100, a fourth gas phase outlet 102 of the first-stage condensation device 100 is connected with a fifth gas phase inlet 111 of the second-stage condensation device 110, and a fourth liquid phase outlet 103 of the first-stage condensation device 100 and a fifth liquid phase outlet 112 of the second-stage condensation device 110 are respectively introduced into the concentrate storage unit 120; the steam is connected with a steam inlet 63 of the gasification unit 60 through a pipeline, and a steam outlet 62 leading to a first gas phase inlet 33 on the preheating unit 30 is also arranged on the overheating unit 60; the organic matter extends into the cracking reduction unit 80 from the outside; the liquid phase outlet three 93 of the purification unit 90 is connected with the liquid phase inlet three 45 of the circulating evaporation unit 40, and the outlet end 42 of the submerged pump on the circulating evaporation unit 40 is also communicated with the material inlet three 51 of the chlorination unit 50.
Specifically, the preheating unit 30 is a preheater, crude titanium tetrachloride flows through the tube side of the preheater, and condensed water flowing out through the thermal unit 60 flows through the shell side of the preheater.
Specifically, the circulation evaporation unit 40 includes an evaporator and a submerged pump hermetically connected to the evaporator, a pump body of the submerged pump extends into a tank cavity of the evaporator, the submerged pump is fixed to the tank body of the evaporator through a flange, and an outlet end 42 of the submerged pump is located outside the evaporator.
Specifically, the chlorination unit 50 is a chlorination furnace.
Specifically, the overheating unit 60 is a heater, coarse titanium tetrachloride flows through the tube pass of the heater, and high-temperature steam flows through the shell pass of the heater.
Specifically, the cracking reduction unit 80 is a reducer.
Specifically, the purification unit 90 is a plate column or a packed column.
Specifically, the primary condensation device 100 is a cooler, and the cooling medium is circulating water.
Specifically, the secondary condensation device 110 is a cooler, the cooling medium is frozen brine, and the temperature is-10 to-25 ℃.
The working principle of the system is as follows: the crude titanium tetrachloride obtained by chlorination procedure is stored in a crude material storage unit 10, under the action of a circulating pump 20, the crude titanium tetrachloride enters a preheating unit 30 to be preliminarily heated, then enters a circulating evaporation unit 40, under the pumping action of a submerged pump, the material enters a overheating unit 60 to be heated by high-temperature saturated steam, then a liquid phase material enters a cracking reduction unit 80 to be mixed with organic matters, the organic matters are rapidly and thoroughly cracked into super-active carbon particles under the catalysis of titanium tetrachloride through temperature control, the vanadyl trichloride in the titanium tetrachloride is instantaneously reduced into vanadyl dichloride, mixed materials comprising crude titanium tetrachloride liquid, vanadyl dichloride, carbon powder, carbon monoxide and the like are formed through reaction, after the pressure is reduced by a pressure reducing valve 70, the mixed materials are converted into gas-liquid mixed phase materials, the gas-phase materials (titanium tetrachloride) enter a purifying unit 90, wherein liquid phase substances (circulating titanium tetrachloride, carbon powder, etc.) are pumped into the overheating unit 60 to be heated again under the action of the submerged pump, and the slurry enters the chlorination unit 50 to be reused. The gas phase substance in the purification unit 90 is rectified, wherein the liquid phase substance enters the conversion unit 40 to participate in the previous step circulation, wherein the gas phase substance enters the first-stage condensation device 100 and is cooled into liquid phase titanium tetrachloride under the action of circulating water, part of the gas phase substance which is not condensed enters the second-stage condensation device 110 and is cooled into liquid phase titanium tetrachloride under the action of frozen brine, and the liquid phase titanium tetrachloride obtained by the two steps of condensation is collected in the concentrate storage unit 120.

Claims (10)

1. A vanadium removal system of crude titanium tetrachloride is characterized in that: the device comprises a coarse material storage unit (10), a heating unit, a cracking reduction unit (80), a circulating evaporation unit (40), a purification unit (90), a condensation unit and a fine material storage unit (120), wherein the circulating evaporation unit (40) comprises a tank body and a submerged pump hermetically connected with the tank body, a material outlet (11) of the coarse material storage unit (10) is connected with an inlet of the heating unit, a liquid inlet (82) and a liquid outlet (81) of the cracking reduction unit (80) are respectively connected with an outlet of the heating unit and a material inlet (43) of the circulating evaporation unit (40), a gas phase inlet (91) and a gas phase outlet (92) of the purification unit (90) are respectively connected with a gas phase outlet (44) and an inlet of the condensation unit of the circulating evaporation unit (40), and an outlet of the condensation unit is communicated into the fine material storage unit (120); the organic matter extends from the outside into the cracking reduction unit (80).
2. The system for removing vanadium from crude titanium tetrachloride according to claim 1, characterized in that: the heating unit comprises a preheating unit (30) and a superheating unit (60), a first material inlet (31) and a first liquid phase outlet (32) of the preheating unit (30) are respectively connected with a first material outlet (11) of the coarse material storage unit (10) and a first liquid phase inlet (41) of the circulating evaporation unit (40), a second liquid phase inlet (61) and a second liquid phase outlet (64) of the superheating unit (60) are respectively connected with a submerged pump outlet end (42) on the circulating evaporation unit (40) and a liquid inlet (82) of the cracking reduction unit (80), steam is connected with a steam inlet (63) of the superheating unit (60) through a pipeline, and the superheating unit (60) is also provided with a steam outlet (62) leading to a first gas phase inlet (33) on the preheating unit (30).
3. The system for removing vanadium from crude titanium tetrachloride according to claim 1, characterized in that: a circulating pump (20) is arranged on a pipeline connecting the coarse material storage unit (10) and the preheating unit (30), a pressure reducing valve (70) is arranged on a pipeline connecting the circulating evaporation unit (40) and the cracking reduction unit (80), a liquid phase outlet III (93) of the purification unit (90) is connected with a liquid phase inlet III (45) of the circulating evaporation unit (40), and a submerged pump outlet end (42) on the circulating evaporation unit (40) is also communicated with a material inlet III (51) of the chlorination unit (50).
4. The system for removing vanadium from crude titanium tetrachloride according to claim 1, characterized in that: the condensation unit comprises a first-stage condensation device (100) and a second-stage condensation device (110), a gas phase inlet four (101) and a gas phase outlet four (102) of the first-stage condensation device (100) are respectively connected with a gas phase outlet three (92) of the purification unit (90) and a gas phase inlet five (111) of the second-stage condensation device (110), and a liquid phase outlet four (103) of the first-stage condensation device (100) and a liquid phase outlet five (112) of the second-stage condensation device (110) are respectively introduced into the concentrate storage unit (120).
5. The system for removing vanadium from crude titanium tetrachloride according to claim 2, characterized in that: the preheating unit (30) is a preheater, crude titanium tetrachloride flows through the tube side of the preheater, and condensed water from the heating unit (60) flows through the shell side of the preheater.
6. The system for removing vanadium from crude titanium tetrachloride according to claim 2, characterized in that: the overheating unit (60) is a heater, coarse titanium tetrachloride flows through the tube pass of the heater, and high-temperature steam flows through the shell pass of the heater.
7. The system for removing vanadium from crude titanium tetrachloride according to claim 1, characterized in that: the circulating evaporation unit (40) comprises an evaporator and a submerged pump hermetically connected with the evaporator, a pump body of the submerged pump extends into a tank cavity of the evaporator, the submerged pump is fixed on the tank body of the evaporator through a flange, and an outlet end of the submerged pump is located outside the evaporator.
8. The system for removing vanadium from crude titanium tetrachloride according to claim 3, characterized in that: the chlorination unit (50) is a chlorination furnace, the cracking reduction unit (80) is a reducer, and the purification unit (90) is a plate tower or a packed tower.
9. The system for removing vanadium from crude titanium tetrachloride according to claim 4, characterized in that: the primary condensing device (100) is a cooler, and the cooling medium is circulating water.
10. The system for removing vanadium from crude titanium tetrachloride according to claim 4, characterized in that: the secondary condensation device (110) is a cooler, and the cooling medium is frozen brine.
CN202023005673.6U 2020-12-12 2020-12-12 Vanadium removal system of crude titanium tetrachloride Active CN214528176U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112408469A (en) * 2020-12-12 2021-02-26 蚌埠中瓷纳米科技有限公司 Vanadium removal system and method for crude titanium tetrachloride

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112408469A (en) * 2020-12-12 2021-02-26 蚌埠中瓷纳米科技有限公司 Vanadium removal system and method for crude titanium tetrachloride

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Effective date of registration: 20220602

Address after: 233000 room 1007, 10th floor, Ziyang building, No. 99, Mingzhu Road, Huaishang District, Bengbu City, Anhui Province

Patentee after: Bengbu Guoti nano material Co.,Ltd.

Address before: 233000 block B, north of Donghai Avenue and east of Longjin Road, Longzihu District, Bengbu City, Anhui Province

Patentee before: Bengbu ZHONGCI Nano Technology Co.,Ltd.

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