CN103112888B - Titanium tetrachloride production system and method for recycling titanium tetrachloride from slurry - Google Patents
Titanium tetrachloride production system and method for recycling titanium tetrachloride from slurry Download PDFInfo
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- CN103112888B CN103112888B CN201310082842.1A CN201310082842A CN103112888B CN 103112888 B CN103112888 B CN 103112888B CN 201310082842 A CN201310082842 A CN 201310082842A CN 103112888 B CN103112888 B CN 103112888B
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Abstract
The invention provides a titanium tetrachloride production system and method for recycling titanium tetrachloride from slurry. The titanium tetrachloride production system comprises a chlorination furnace, a dust collection condenser and a slag ladle, wherein a torrential rinsing pipe is vertically arranged on the top of the dust collection condenser, the upper end of the torrential rinsing pipe is communicated with an exhaust gas outlet of the chlorination furnace, and a torrential rinsing spray head with an upward nozzle is arranged in the torrential rinsing pipe and is fixedly connected with a slurry feed pipe. The method comprises the following steps that: the slurry is fed into the slurry feed pipe and is upwards sprayed out from the torrential rinsing spray head, wherein the flow rate of the sprayed slurry is no less than 4m<3>/h; the temperature of exhaust gas at the outlet of the chlorination furnace is controlled, so that the exhaust gas reversely collides with the atomized slurry sprayed out by the torrential rinsing spray head and is torrentially rinsed and washed; solid particles separated out fall into the dust collection condenser and are removed by the system; the exhaust gas which is torrentially rinsed and washed enters the dust collection condenser, and then enters a subsequent elution system through gravity settling and temperature reduction, and formed titanium tetrachloride supernatant is filtered and then enters a product tank; and the slurry enters a slurry header tank and is reused. The titanium tetrachloride production system has high recovery rate and is easy to control in an operation process.
Description
Technical field
Invention belongs to titanium tetrachloride production recovery technology field, relates to a kind of titanium tetrachloride production system, relates in particular to one and utilizes rapids to rush washing technology, can from mud, reclaim the titanium tetrachloride production system of titanium tetrachloride; The invention still further relates to a kind of method that reclaims titanium tetrachloride mud producing from this production system.
Background technology
In crude titanic chloride production process, contained a large amount of high boiling point muriates and with air-flow entrained solid granule foreign in fluidizing chlorination outlet of still flue gas, after the condensation of gathering dust, most ofly separate with titanium tetrachloride; But there is small part dust impurity in the time of drip washing, to be condensed under titanium tetrachloride drip washing, enter in liquid crude titanium tetrachloride, through subsider solid-liquid separation, the impurity such as small part high boiling point muriate and solid particulate being suspended in liquid crude titanium tetrachloride is deposited on subsider bottom gradually, forms mud.In order to improve metal recovery rate, and the environmental pollution producing when Processing for removing mud slag, must process these mud.
Early stage titanium sponge manufacturing enterprise mainly adopts mud method of evaporation to process the mud of subsider bottom, by heating mud, make titanium tetrachloride carburation by evaporation wherein, then gaseous titanium tetrachloride is reclaimed in condensation.The deficiency of mud method of evaporation is, apparatus processing more complicated, gets into smooth and be often out of order, and whole equipment is worked again for a long time in corrosive environment, and working rate is lower; And mud can not steam too dryly in heat-processed, otherwise mud sintering easily causes evaporator shell body deformability, or makes duplex flexural deformation, and driving part displacement destroys, equipment scrapping.And while processing mud by mud method of evaporation, the rate of recovery of titanium tetrachloride is lower, is substituted gradually by the mud remelting of scrap.
Separately there is Some Enterprises by mud being returned to recovery titanium tetrachloride wherein in boiling chloridizing furnace.The mud that the mud of subsider bottom or refining step return, is delivered to sludge head tank through slag stock pump, in the time that chlorination furnace furnace temperature is too high, intermittently adds in chlorination furnace, and this working of a furnace that adds mode can change boiling chloridizing furnace, wayward in operating process.
Therefore, be badly in need of reclaiming the higher recovery that has of titanium tetrachloride a kind of mud that can produce from production process, and be easy to the production system of red-tape operati process.
Summary of the invention
The object of the invention is the deficiency and the defect that exist for existing crude titanic chloride production system, provide a kind of and there is higher recovery, be easy to red-tape operati process, can from mud, reclaim the titanium tetrachloride production system of titanium tetrachloride.
Another object of the present invention is to provide a kind of method that reclaims titanium tetrachloride mud producing from above-mentioned production system.
For achieving the above object, the technical solution adopted in the present invention is: a kind of titanium tetrachloride production system that can reclaim titanium tetrachloride from mud, the slag ladle that comprise chlorination furnace, the condenser and being located at of gathering dust gathers dust condenser bottom, the condenser overhead of gathering dust is vertically provided with rapid washing pipe, and rapid washing pipe upper end communicates with the exhanst gas outlet of chlorination furnace by flue; In rapid washing pipe, be from top to bottom provided with successively three nozzles all rapids upward rush shower nozzle, one end that rapids rushes shower nozzle and a mud feed pipe is affixed, the other end of all mud feed pipes all communicates with slag stock pump.
Another technical solution used in the present invention is: a kind of method that reclaims titanium tetrachloride mud producing from above-mentioned titanium tetrachloride production system, can not only improve the titanium tetrachloride rate of recovery, and make operating process be easy to control, the method is specifically carried out according to the following steps:
Step 1: by slag stock pump, the mud producing in titanic chloride production process is sent into mud feed pipe, and rush shower nozzle from rapids and upwards spray, and atomization, control the mud flow rate that each rapids rushes shower nozzle ejection and be not less than 4m
3/ h;
Step 2: the temperature of controlling chlorination furnace outlet flue gas is 550 ℃～600 ℃, sends into rapid washing pipe from upper end, flows from top to bottom in rapid washing pipe, rushes the mist mud reverse-impact of shower nozzle ejection with rapids, mist mud carries out rapids flushing to flue gas and washs and heat exchange;
Step 3: the solid particulate that mist mud carries out separating out when rapid flushing is washed to flue gas falls under gravity into the condenser that gathers dust, and then enters slag ladle, and removes from system; In rapid washing pipe, rinse through rapids the flue gas of washing and enter the condenser that gathers dust, after gravity settling, cooling, enter follow-up elution circuit, the titanium tetrachloride supernatant liquor of formation enters product groove after filtering; Mud enters sludge head tank, again utilizes.
Titanium tetrachloride production system of the present invention adopts multistage shower nozzle to carry out reverse rapid punching spray with strengthening slurry atomization effect, by the gas of mud liquid at high speed directive countercurrent flow, utilize the momentum of flue gas in reverse jet tube, to make washings scatter and splash, washings and flue gas reach transient equilibrium place and form stable strong turbulence foamy column.In this region, flue gas fully contacts with mud, and with the renewal of contact surface high speed, the dust in flue gas, by the liquid film of turbulent flow parcel, dissolving, enters the condenser that gathers dust, the vaporization of titanium tetrachloride mud, the titanium tetrachloride in realization recovery mud and the effect of flue gas cool-down dedusting.
Accompanying drawing explanation
Fig. 1 is the device connection diagram using in the inventive method.
Fig. 2 is the process flow sheet of the inventive method.
In figure: 1. chlorination furnace, 2. rapid washing pipe, 3. rapids rushes shower nozzle, 4. nitrogen blowback pipeline, 5. mud feed pipe, the condenser that 6. gathers dust, 7. slag ladle, 8. flow valve, 9. flue.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
As shown in Figure 1, the present invention can reclaim the titanium tetrachloride production system of titanium tetrachloride from mud, comprise chlorination furnace 1 and the condenser 6 that gathers dust, condenser 6 bottoms of gathering dust are provided with slag ladle 7, condenser 6 top verticals that gather dust are provided with rapid washing pipe 2, the upper end of rapid washing pipe 2 communicates with the exhanst gas outlet of chlorination furnace 1 by flue 9, and flue 9 is obliquely installed; In rapid washing pipe 2, be provided with successively three rapidss from top to bottom and rush shower nozzle 3, the nozzle that all rapidss rush shower nozzle 3 is all upward; One end that rapids rushes shower nozzle 3 and a mud feed pipe 5 is affixed, and the other end of all mud feed pipes 5 all communicates with slag stock pump; The one end that is provided with 4, nitrogen blowback pipelines 4 of a nitrogen blowback pipeline on a mud feed pipe 5 communicates with a corresponding mud feed pipe 5, and the other end of all nitrogen blowback pipelines 4 is all connected with nitrogen gas conveying device; On every nitrogen blowback pipeline 4, a flow valve 8 is all installed.
The mud that titanium tetrachloride production system provided by the invention can produce from production process, reclaim titanium tetrachloride, can not only improve the rate of recovery of titanium tetrachloride, and make operating process be easy to control, solved the problem existing in existing production system.The process flow sheet of this system, as shown in Figure 2, this recovery method specifically carries out according to the following steps:
Step 1: the mud producing in titanic chloride production process is sent into sludge head tank, by slag stock pump, the mud in sludge head tank is sent into mud feed pipe 5, the mud that enters mud feed pipe 5 rushes shower nozzle 3 from rapids and upwards sprays, and atomization, control each rapids and rush the mud flow rate that shower nozzle 3 sprays and be not less than 4m
3/ h; Turn-on flow rate valve 8, makes nitrogen enter mud feed pipe 5 by nitrogen blowback pipeline 4 and carries out blowback, to prevent that rapids from rushing shower nozzle 3 and mud feed pipe 5 stops up simultaneously;
Step 2: the temperature of controlling chlorination furnace outlet flue gas is 550 ℃ ~ 600 ℃, and send into rapid washing pipe 2 from rapid washing pipe 2 upper ends, flue gas flows from top to bottom in rapid washing pipe 2, rush with rapids the mist mud reverse-impact that shower nozzle 3 sprays, mist mud carries out rapid flushing when washing to flue gas, carries out heat exchange with flue gas;
Step 3: the solid particulate that mist mud carries out separating out when rapid flushing is washed to flue gas falls under gravity into the condenser 6 that gathers dust, and then enters slag ladle 7, and removes from system; Rapid washing pipe 2 is interior to be rinsed through rapids the flue gas of washing and enters the condenser 6 that gathers dust, and enters follow-up elution circuit through gravity settling, after lowering the temperature, and the titanium tetrachloride supernatant liquor of formation enters product groove after filtering; Mud enters high-order slush-pit launder, again utilizes.
Adopt production system of the present invention from mud, to reclaim titanium tetrachloride, the rate of recovery reaches 85%～92%.
At fluidizing chlorination outlet of still and gather dust and the flue 9 of inclination and 2, three grades of mud rapidss of rapid washing pipe are set between condenser rush shower nozzle 3 and be arranged in rapid washing pipe 2, and carry out the flow control of mud with flow valve 8.For preventing Hydralock, mud feed pipe 5 and rapids rush shower nozzle 3 and are provided with nitrogen blowback pipeline.Titanium tetrachloride mud enters after said system, and gaseous titanium tetrachloride wherein enters with flue gas the condenser 6 that gathers dust, and the solid impurities such as dust wherein fall into the slag ladle 7 of the condenser that gathers dust.
Production system of the present invention adopts rapid flushing to wash the dedusting of lowering the temperature, and atomizing effect is good, and efficiency of dust collection is high, the titanium tetrachloride rate of recovery is high, avoided the bad mud of atomizing effect to discharge with liquid form, contaminate environment, also can avoid furnace roof to return to the impact of mud on the working of a furnace simultaneously; Mud can spray into continuously, has realized the serialization of producing, and processing unit is simple, operational safety.
Claims (5)
1. an energy reclaims the titanium tetrachloride production system of titanium tetrachloride from mud, comprise chlorination furnace (1), the condenser that gathers dust (6) and be located at the slag ladle (7) of the condenser bottom of gathering dust, it is characterized in that, condenser (6) top vertical that gathers dust is provided with rapid washing pipe (2), and rapid washing pipe (2) upper end communicates with the exhanst gas outlet of chlorination furnace (1) by flue (9); In rapid washing pipe (2), be from top to bottom provided with successively three nozzles all rapids upward rush shower nozzle (3), it is affixed with one end of a mud feed pipe (5) that rapids rushes shower nozzle (3), the other end of all mud feed pipes (5) all communicates with slag stock pump.
2. the titanium tetrachloride production system that can reclaim titanium tetrachloride from mud according to claim 1, it is characterized in that, on a mud feed pipe (5), be provided with a nitrogen blowback pipeline (4), one end of a nitrogen blowback pipeline (4) communicates with a corresponding mud feed pipe (5), and the other end of all nitrogen blowback pipelines (4) is all connected with nitrogen gas conveying device; A flow valve (8) is all installed on every nitrogen blowback pipeline (4).
3. the titanium tetrachloride production system that can reclaim titanium tetrachloride from mud according to claim 1, is characterized in that, described flue (9) is obliquely installed.
4. a method that reclaims titanium tetrachloride in the mud that described in Accessory Right requirement 2, titanium tetrachloride production system produces, can not only improve the titanium tetrachloride rate of recovery, and makes operating process be easy to control, and it is characterized in that, the method is specifically carried out according to the following steps:
Step 1: by slag stock pump, the mud producing in titanic chloride production process is sent into mud feed pipe, and rush shower nozzle from rapids and upwards spray, and atomization, control the mud flow rate that each rapids rushes shower nozzle ejection and be not less than 4m
3/ h;
Step 2: the temperature of controlling chlorination furnace outlet flue gas is 550 ℃～600 ℃, sends into rapid washing pipe from upper end, flows from top to bottom in rapid washing pipe, rushes the mist mud reverse-impact of shower nozzle ejection with rapids, mist mud carries out rapids flushing to flue gas and washs and heat exchange;
Step 3: the solid particulate that mist mud carries out separating out when rapid flushing is washed to flue gas falls under gravity into the condenser that gathers dust, and then enters slag ladle, and removes from system; In rapid washing pipe, rinse through rapids the flue gas of washing and enter the condenser that gathers dust, after gravity settling, cooling, enter follow-up elution circuit, the titanium tetrachloride supernatant liquor of formation enters product groove after filtering; Mud enters sludge head tank, again utilizes.
5. the method that reclaims titanium tetrachloride from mud according to claim 4, it is characterized in that, when mud is sent into mud feed pipe, turn-on flow rate valve, make nitrogen enter mud feed pipe by nitrogen blowback pipeline and carry out blowback, to prevent that rapids from rushing shower nozzle and mud feed pipe stops up.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103466694B (en) * | 2013-08-16 | 2015-12-02 | 东华工程科技股份有限公司 | A kind of chloridating gas cooling system |
| CN106082315B (en) * | 2016-06-06 | 2017-05-31 | 攀钢集团攀枝花钢铁研究院有限公司 | Dual-reaction chamber low-temperature boiling chlorination furnace |
| CN107963653B (en) * | 2017-12-19 | 2019-12-31 | 中信钛业股份有限公司 | Gradient control method for temperature of molten salt chlorination system |
| CN109264775B (en) * | 2018-10-22 | 2023-06-30 | 河南龙兴钛业科技股份有限公司 | Titanium tetrachloride continuous production system with slag discharging function and energy saving characteristic |
| CN111517365B (en) * | 2020-06-10 | 2022-08-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium tetrachloride production method and system |
| CN114370835A (en) * | 2021-12-31 | 2022-04-19 | 宜宾天原海丰和泰有限公司 | Method for measuring chlorination furnace bed layer height |
| CN114636316B (en) * | 2022-03-14 | 2024-01-26 | 苏州海陆重工股份有限公司 | Waste heat recovery system matched with HISMELT smelting reduction ironmaking system |
| CN114534643B (en) * | 2022-03-16 | 2022-12-27 | 东华工程科技股份有限公司 | Titanium tetrachloride production system and method |
| CN115286036B (en) * | 2022-09-01 | 2023-10-17 | 攀钢集团攀枝花钢铁研究院有限公司 | Device and method for reducing solid content of titanium tetrachloride slurry in leaching system |
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| US2815091A (en) * | 1954-11-28 | 1957-12-03 | Thann Fab Prod Chem | Recovery of titanium tetrachloride from chlorination gases |
| NL6906832A (en) * | 1968-05-10 | 1969-11-12 | ||
| CN1199863C (en) * | 2002-07-19 | 2005-05-04 | 锦州铁合金（集团）有限责任公司钛白粉厂 | Technique and method for treating titanium tetrachloride slurry containing vanadium |
| CN101417813A (en) * | 2007-10-25 | 2009-04-29 | 贵阳铝镁设计研究院 | Recovery method and equipment of vanadium-containing slurry produced from titanic chloride refining process |
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