CN107758732A - Crude titanic chloride is refined to remove vanadium method - Google Patents
Crude titanic chloride is refined to remove vanadium method Download PDFInfo
- Publication number
- CN107758732A CN107758732A CN201711239363.0A CN201711239363A CN107758732A CN 107758732 A CN107758732 A CN 107758732A CN 201711239363 A CN201711239363 A CN 201711239363A CN 107758732 A CN107758732 A CN 107758732A
- Authority
- CN
- China
- Prior art keywords
- ticl
- vanadium
- steam
- slurry
- refined
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
- C01G23/024—Purification of tetrachloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
Refined the invention discloses a kind of crude titanic chloride and remove vanadium method, be related to titanium tetrachloride production technical field, there is provided one kind is fast except vanadium speed, and effect is good, and lower-cost crude titanic chloride is refined to remove vanadium method.This method comprises the following steps：A, the thick TiCl produced by chlorination system4Into TiCl4Storage tank stores；B、TiCl4Thick TiCl in storage tank4Into TiCl4Steam generating system produces the TiCl of high temperature4Steam；C、TiCl4Steam enters refined tower bottom；Refined tower bottom is provided with by aliphatic acid and smart TiCl4What is be mixed to form removes vanadium slurry, except vanadium slurry top is provided with column plate；TiCl4Being reacted containing foreign matter of vanadium with aliphatic acid in steam, product is stayed in except in vanadium slurry；TiCl4Steam, which continues to rise to exchange with column plate progress caloic, removes TiCl4The relatively low gaseous impurities of steam mid-boiling point obtains smart TiCl4Steam；D, smart TiCl4Steam leaves refined column overhead and cools down to obtain smart TiCl into condenser4, TiCl4Into smart TiCl4Storage tank stores.The present invention is fast except vanadium speed, obtained smart TiCl4Middle content of vanadium is low.
Description
Technical field
The present invention relates to titanium tetrachloride production technical field, more particularly to crude titanic chloride to refine and remove vanadium method.
Background technology
Crude titanic chloride refining process technology mainly has copper wire vanadium removal method, aluminium powder except vanadium method, hydrogen sulfide remove vanadium method.Copper wire removes
The shortcomings that vanadium method is the regeneration washing operation trouble of failure copper wire, and labor intensity is big, and condition is poor, and produces copper-containing wastewater dirt
Dye, it is not easy to reclaim vanadium, except vanadium cost is high, production is discontinuous.It is the superfine active aluminium powder valency used that aluminium powder, which removes the shortcomings that vanadium method,
Lattice are expensive, and have explosiveness.It is that hydrogen sulfide is severe toxicity, stench, explosive gas that hydrogen sulfide, which removes the shortcomings that vanadium method, working condition
Badly.
The content of the invention
The technical problem to be solved in the present invention is：One kind is provided except vanadium speed is fast, effect is good, lower-cost thick four chlorination
Titanium is refined to remove vanadium method.
Technical scheme for the use that solves the above problems is：Crude titanic chloride is refined except vanadium method comprises the following steps：
A, the thick TiCl produced by chlorination system4Into TiCl4Storage tank stores；
B、TiCl4Thick TiCl in storage tank4Into TiCl4Steam generating system produces the TiCl of high temperature4Steam；
C、TiCl4Steam enters refined tower bottom；Refined tower bottom is provided with by aliphatic acid and smart TiCl4It is mixed to form
Except vanadium slurry, except vanadium slurry top is provided with column plate；TiCl4Being reacted containing foreign matter of vanadium with aliphatic acid in steam, product
Stay in except in vanadium slurry；TiCl4Steam, which continues to rise to exchange with column plate progress caloic, removes TiCl4The relatively low gas of steam mid-boiling point
State impurity obtains smart TiCl4Steam；
D, smart TiCl4Steam leaves refined column overhead and cools down to obtain smart TiCl into condenser4, TiCl4Into smart TiCl4
Storage tank stores.
It is further：Except vanadium slurry by slurry adding apparatus is delivered to refined tower bottom, step C carry out after remove vanadium
Slurry is extracted out by slurry return mechanism and is sent into chlorination system.
It is further：Caused TiCl in step B4The temperature of steam is 160 DEG C, flow velocity 4.5m/s, and pressure is
0.6Mpa；TiCl in step C4The speed that steam enters refined tower bottom is 20T/h, and aliphatic acid in vanadium slurry is removed in treating column
Concentration is 8.5%, and except the depth of vanadium slurry is 60cm, refined tower pressure interior force be 60kPa, and temperature is 140 DEG C in treating column, refined
Column plate quantity is two to four in tower.
The beneficial effects of the invention are as follows：1 is fast except vanadium speed, obtained smart TiCl4Middle content of vanadium is extremely low, is a kind of efficient
It is refined to remove vanadium technique.2 are automatically added to and are extracted by slurry adding apparatus and slurry return mechanism and remove vanadium slurry, can avoid removing
Influence of the vanadium slurry to system, make except vanadium is carried out continuously, make except vanadium rapidly and efficiently.3 is relatively low except vanadium cost of sizing agent, can save into
This.
Brief description of the drawings
Fig. 1 is the schematic diagram of the refined equipment applied except vanadium method of crude titanic chloride；
In figure mark for：TiCl4Storage tank 1, steam generating system 2, treating column 3, add except vanadium slurry 31, column plate 32, slurry
Enter device 4, condenser 5, slurry return mechanism 6, chlorination system 7.
Embodiment
The present invention is further described with reference to the accompanying drawings and detailed description.
Crude titanic chloride is refined except vanadium method comprises the following steps：A, the thick TiCl produced by chlorination system 74Into TiCl4
Storage tank 1 stores；B、TiCl4Thick TiCl in storage tank 14Into TiCl4Steam generating system 2 produces the TiCl of high temperature4Steam；C、
TiCl4Steam enters the bottom for the treatment of column 3；The bottom for the treatment of column 3 is provided with by aliphatic acid and smart TiCl4What is be mixed to form removes vanadium slurry
31, except the top of vanadium slurry 31 is provided with column plate 32；TiCl4Being reacted containing foreign matter of vanadium with aliphatic acid in steam, product stays
In except vanadium slurry 31；TiCl4Steam, which continues to rise to exchange with the progress of column plate 32 caloic, removes TiCl4Steam mid-boiling point is relatively low
Gaseous impurities obtains smart TiCl4Steam；D, smart TiCl4Steam leaves the tower top for the treatment of column 3 and obtains essence into the cooling of condenser 5
TiCl4, TiCl4Into smart TiCl4Storage tank stores.
The impurity often having in crude titanic chloride is VOCl3、FeCl3、AlCl3.Except vanadium slurry 31 can remove it is therein
VOCl3, chemical equation is：VOCl3+ C=VCl3+CO。TiCl4Steam carries out caloic with column plate 32 and exchanges and can remove
FeCl therein3、C。
A large amount of residues can be produced after removing vanadium except vanadium slurry 31, residue is in thick, is easily tied on equipment pipe and chamber wall
Scar, equipment heat transfer is influenceed, key equipment is paralysed, influence the direct motion except vanadium and continuous operation.In order that can be suitable except vanadium process
Row and continuous operation, except vanadium slurry 31 by slurry adding apparatus 4 is delivered to the bottom for the treatment of column 3, step C carry out after except vanadium is starched
Material 32 is extracted out by slurry return mechanism 6 and is sent into chlorination system 7.
Slurry adding apparatus 4 can include pump and control valve, and reagent is pumped out by pump by storage tank, and passes through control valve
Adjust reagent feeds amount；Slurry return mechanism 6 can include pans and transfer cask, and pans, which are used to store, carrys out self-circulation system
Slurry, slurry imports transfer cask by pans, chlorination system returned by transfer cask.
Embodiment：
As shown in figure 1, a kind of refined equipment used except vanadium method of crude titanic chloride includes TiCl4Storage tank 1, steam produce
System 2, treating column 3, slurry adding apparatus 4, condenser 5 and slurry return mechanism 6；The bottom for the treatment of column 3 has by aliphatic acid and essence
TiCl4What is be mixed to form removes vanadium slurry 31, except the top of vanadium slurry 31 is provided with column plate 32；Except vanadium slurry 31 can be added by slurry
Enter device 4 and be delivered to the bottom for the treatment of column 3, except vanadium slurry 32 can be extracted out by slurry return mechanism 6 and be sent into chlorination system 7.
During production, the thick TiCl that is produced by chlorination system 74Into TiCl4Storage tank 1 stores, by TiCl4Tetrachloro in storage tank 1
Change titanium pump and enter the high temperature titanium tetrachloride vapors that steam generating system 2 generates 160 DEG C, steam flow rate 4.5m/s, pressure 0.6Mpa；Production
Raw titanium tetrachloride vapors with 20T/h speed import the bottom for the treatment of column 3 with except vanadium slurry 31 contacts；Aliphatic acid is except vanadium slurry
Concentration in 31 is controlled 8.5%；The Stress control for the treatment of column 3 is in 75kPa, treating column 3 except the liquid level of vanadium slurry 31 controls
140 DEG C of temperature in 60cm, tower, the smart tetrachloro of raising is exchanged except the titanium tetrachloride vapors after vanadium carry out caloic by 4 column plates 32
Change titanium quality；Refined titanic chloride steam overflows into condenser 5 through tower top and condensed, and finally obtains refined titanic chloride liquid；This is
System can be by TiCl4In content of vanadium be refined to 0.0001%, TiCl by 0.5%4Yield is more than 98%, system continuous operating time
More than 3 years.
Claims (3)
1. crude titanic chloride is refined to remove vanadium method, it is characterised in that：Comprise the following steps：
A, the thick TiCl produced by chlorination system (7)4Into TiCl4Storage tank (1) stores；
B、TiCl4Thick TiCl in storage tank (1)4Into TiCl4Steam generating system (2) produces the TiCl of high temperature4Steam；
C、TiCl4Steam enters treating column (3) bottom；Treating column (3) bottom is provided with by aliphatic acid and smart TiCl4It is mixed to form
Remove vanadium slurry (31), except being provided with column plate (32) above vanadium slurry (31)；TiCl4Being sent out containing foreign matter of vanadium and aliphatic acid in steam
Raw reaction, product are stayed in except in vanadium slurry (31)；TiCl4Steam continues to rise exchanges removal with column plate (32) progress caloic
TiCl4The relatively low gaseous impurities of steam mid-boiling point obtains smart TiCl4Steam；
D, smart TiCl4Steam leaves treating column (3) tower top and obtains smart TiCl into condenser (5) cooling4, TiCl4Into smart TiCl4
Storage tank stores.
2. crude titanic chloride according to claim 1 is refined to remove vanadium method, it is characterised in that：Except vanadium slurry (31) passes through slurry
Material adding apparatus (4) is delivered to treating column (3) bottom, step C carry out after except vanadium slurry (32) passes through slurry return mechanism (6)
Extract out and be sent into chlorination system (7).
3. crude titanic chloride according to claim 1 is refined to remove vanadium method, it is characterised in that：Caused TiCl in step B4
The temperature of steam is 160 DEG C, flow velocity 4.5m/s, pressure 0.6Mpa；TiCl in step C4Steam enters treating column (3) bottom
Speed be 20T/h, the concentration that aliphatic acid in vanadium slurry (31) is removed in treating column (3) is 8.5%, except the depth of vanadium slurry (31)
For 60cm, treating column (3) interior pressure is 60kPa, and treating column (3) interior temperature is 140 DEG C, treating column (3) interior column plate (32) quantity
For two to four.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711239363.0A CN107758732A (en) | 2017-11-30 | 2017-11-30 | Crude titanic chloride is refined to remove vanadium method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711239363.0A CN107758732A (en) | 2017-11-30 | 2017-11-30 | Crude titanic chloride is refined to remove vanadium method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107758732A true CN107758732A (en) | 2018-03-06 |
Family
ID=61276586
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711239363.0A Pending CN107758732A (en) | 2017-11-30 | 2017-11-30 | Crude titanic chloride is refined to remove vanadium method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107758732A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589880A (en) * | 2019-10-12 | 2019-12-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium removal method for titanium tetrachloride refined organic matter |
| KR20210085314A (en) * | 2019-12-30 | 2021-07-08 | 고등기술연구원연구조합 | Manufacturing apparatus of refining titanium tetrachloride and manufacturing method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103613126A (en) * | 2013-11-20 | 2014-03-05 | 锦州钛业有限公司 | Method and system for removing vanadium impurities in titanium tetrachloride |
| CN103641160A (en) * | 2013-12-02 | 2014-03-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Coarse titanium tetrachloride vanadium removal device and method |
| CN103936062A (en) * | 2014-04-21 | 2014-07-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium removal refining tower with organic matter and method for removing vanadium from crude titanium tetrachloride with organic matter |
| 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 |
-
2017
- 2017-11-30 CN CN201711239363.0A patent/CN107758732A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103613126A (en) * | 2013-11-20 | 2014-03-05 | 锦州钛业有限公司 | Method and system for removing vanadium impurities in titanium tetrachloride |
| CN103641160A (en) * | 2013-12-02 | 2014-03-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Coarse titanium tetrachloride vanadium removal device and method |
| CN103936062A (en) * | 2014-04-21 | 2014-07-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium removal refining tower with organic matter and method for removing vanadium from crude titanium tetrachloride with organic matter |
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| 周丽: "高含钒粗四氯化钛有机物预处理除钒工艺研究", 《钢铁钒钛》 * |
| 杜明: "粗四氯化钛脂肪酸除钒试剂的选择", 《钢铁钒钛》 * |
| 王亚峰等: "强制循环法粗四氯化钛有机物除钒工艺研究", 《广州化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589880A (en) * | 2019-10-12 | 2019-12-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium removal method for titanium tetrachloride refined organic matter |
| CN110589880B (en) * | 2019-10-12 | 2022-03-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium removal method for titanium tetrachloride refined organic matter |
| KR20210085314A (en) * | 2019-12-30 | 2021-07-08 | 고등기술연구원연구조합 | Manufacturing apparatus of refining titanium tetrachloride and manufacturing method thereof |
| KR102321997B1 (en) | 2019-12-30 | 2021-11-08 | 고등기술연구원연구조합 | Manufacturing apparatus of refining titanium tetrachloride and manufacturing method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103011269B (en) | Process and system for purifying titanium tetrachloride by removing vanadium | |
| CN104118905B (en) | The process for refining of crude titanic chloride | |
| CN109052462A (en) | Crude titanic chloride purification removes vanadium method | |
| CN103613126B (en) | A kind of method and system removing vanadium impurity from titanic tetrachloride | |
| CN109052463A (en) | A kind of purification of crude titanic chloride removes vanadium method | |
| CN107758732A (en) | Crude titanic chloride is refined to remove vanadium method | |
| CN203474481U (en) | Slurry processing device applicable to titanium tetrachloride production process | |
| CN104058451A (en) | Vanadium removing system and method for crude titanium tetrachloride refining | |
| CN103387260A (en) | Method and equipment for recovering titanium tetrachloride from refined vanadium-containing waste liquid | |
| CN107601556A (en) | Remove VOCl in crude titanic chloride3And VCl4Method | |
| CN104528650B (en) | The purification method of tail gas hydrogen chloride during a kind of chlorocarbon-52 produce | |
| CN101417813A (en) | Recovery method and equipment of vanadium-containing slurry produced from titanic chloride refining process | |
| JP5038251B2 (en) | Titanium tetrachloride distillation purification apparatus, maintenance method of the apparatus, and purification method of titanium tetrachloride using the apparatus | |
| CN103866132A (en) | Process for recovering mercury from non-ferrous metal smelting exhaust gas | |
| KR20180064753A (en) | Methods for waste water treatment of Nitrogen trifluoride(NF3) process | |
| CN104310464B (en) | A kind of titanium chloride slurry and preparation method thereof at a low price | |
| CN108946741B (en) | Process method for recovering silicon-containing high-boiling-point substance in polycrystalline silicon cold hydrogenation process and cold hydrogenation process | |
| CN109250751A (en) | Handle the method that titanium tetrachloride purification removes vanadium mud | |
| CN114735659B (en) | Method for recovering tellurium from low-temperature pressurized leaching solution of copper anode slime | |
| CN107445421A (en) | The processing method of the mud containing vanadium caused by titanium tetrachloride vanadium removal | |
| CN213680463U (en) | VCM high-boiling-point substance purification device | |
| CN111533164B (en) | Vanadium removal method for titanium tetrachloride in boiling chlorination system | |
| US3533733A (en) | Purifying crude ticl4 vapor | |
| CN214456902U (en) | Chlorination refining system | |
| CN106187676B (en) | The recovery method of distillation residual liquid in a kind of production of tetrachloro-ethylene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180306 |