CN101638248B - Method and system for recovering residual titanium tetrachloride in copper-wire tower - Google Patents
Method and system for recovering residual titanium tetrachloride in copper-wire tower Download PDFInfo
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- CN101638248B CN101638248B CN2008100125800A CN200810012580A CN101638248B CN 101638248 B CN101638248 B CN 101638248B CN 2008100125800 A CN2008100125800 A CN 2008100125800A CN 200810012580 A CN200810012580 A CN 200810012580A CN 101638248 B CN101638248 B CN 101638248B
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- titanium tetrachloride
- copper
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Abstract
The invention discloses a method for removing vanadium from a titanium tetrachloride copper wire, and in particular relates to a method and a system for recovering residual titanium tetrachloride in a copper-wire tower. In the method for recovering the residual titanium tetrachloride in the copper-wire tower, a breathing pipeline on the rear of a secondary condenser in the prior copper-wire tower vanadium removal process is provided with a branch and is connected with a vacuum system, the residual titanium tetrachloride in the copper-wire tower is recovered before copper-wire ball regeneration treatment, the negative pressure generated by the vacuum system makes the residual titanium tetrachloride in the copper-wire tower evaporated into a condenser by means of self vapor pressure, and the titanium tetrachloride is condensed due to the low temperature of the condenser and the secondary condenser, and is collected to a condensate buffer storage tank. The method can recover the residual titanium tetrachloride in the copper-wire tower and reduce the loss of the titanium tetrachloride to improve the recovery efficiency of materials, prolongs the service life of the copper-wire tower, and reduces the quantity of waste acid water.
Description
Technical field
The present invention relates to a kind of method of titanium tetrachloride copper wire vanadium removal, especially relate to a kind of method and system thereof that reclaims residual titanium tetrachloride in copper-wire tower.
Background technology
In the copper wire vanadium removal process, the vanadylic chloride (VOCl in the titanium tetrachloride
3) can following reaction take place with copper:
TiCl
4+Cu＝CuCl·TiCl
3
CuCl·TiCl
3+VOCl
3＝VOCl
2↓+CuCl+TiCl
4
After removing vanadium and carrying out for some time, the copper wire surface can be wrapped and loses chemically reactive by cuprous chloride and vanadyl dichloride, at this moment need carry out manipulation of regeneration to copper wire, makes its surface have chemically reactive again.Current methods is to wash copper wire balls at copper wire tower bubble, and the titanium tetrachloride and the water that remain on the copper wire balls can produce following hydrolysis reaction generation metatitanic acid and hydrochloric acid: TiCl
4+ 3H
2O=H
2TiO
3+ 4HCl.
Because hydrochloric acid (HCl) can produce pitting attack to the copper wire tower of stainless steel, can influence the copper wire tower life-span with this method, also produces a large amount of waste acid waters simultaneously.Some factory directly emits the copper wire balls that has titanium tetrachloride for protection copper wire tower; Because titanium tetrachloride and water in air branch hydrolytic reactions generate white vaporific hydrochloric acid gas; Make that Working environment is very abominable in the workshop, hydrochloric acid is also quite serious to the corrosion of workshop factory building and device outer surface simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of method that reclaims residual titanium tetrachloride in copper-wire tower, be used to prolong the life-span of copper wire tower, reduce waste acid water, improve Working environment in the workshop.
Be achieved in that a kind of method that reclaims residual titanium tetrachloride in copper-wire tower for reaching above-mentioned purpose the present invention; Respiratory siphon pass after original copper wire tower is except that secondary condenser in the vanadium technology goes out branch; And connection vacuum system; Before the copper wire balls manipulation of regeneration, reclaim titanium tetrachloride residual in the copper wire tower; The negative pressure of utilizing vacuum system to produce makes the titanium tetrachloride that remains in the copper wire tower lean on the vapour pressure of self to be evaporated to condensing surface, because the low temperature of condensing surface and secondary condenser makes titanium tetrachloride be condensed and is collected into phlegma buffering storage tank.
The method of described recovery residual titanium tetrachloride in copper-wire tower; It is heating power supply and the valve 1 and regulating valve 2 of closing still kettle 3 earlier; Open underflow valve 4 again and be expelled to a part of titanium tetrachloride in titanium tetrachloride in the still kettle 4 and the copper wire tower 6 except that titanium tetrachloride storage tank before the vanadium, close underflow valve 4 then; Shut-off valve 10 is also opened valve 12 with valve 11, starts vacuum pump 19, and the vacuum tightness of measuring according to the vacuumometer on the vacuum buffer tank 16 15 and control vacuum breaker 17 is automatically closed sky variable valve 17 automatically after vacuum tightness reaches requirement; Valve 12 places behind secondary condenser are provided with vacuumometer 13; Automatically control vacuum breaker 14 according to the vacuum tightness of measuring; Making here that vacuum tightness is neither too high lowly only (is pressed with the pass with titanium tetrachloride vapors under the differing temps; When temperature was in 10～50 ℃, vacuum tightness should be at 700～5000Pa; When temperature was in 50～136 ℃, vacuum tightness should be 5000～50000Pa); Titanium tetrachloride in the copper wire tower is at vacuum and normal temperature or be higher than under the state of normal temperature by self vapour pressure effect and become steam; Vapour temperature descends because of the heat-eliminating medium effect after steam gets into condensing surface 7 and 8; Because temperature reduction titanium tetrachloride vapors is pressed also reduction to make gaseous titanium tetrachloride be condensed into liquid state and is collected into phlegma buffering storage tank 9, recovery operation is accomplished.
Thereby the valve 11 of then opening that the vacuum tightness of described measurement is too high makes the argon gas of breathing in the piping system get into reduction vacuum tightness.
After described recovery operation is accomplished, close vacuum breaker 17, close vacuum pump 19; Open valve 11, open underflow valve 18 then, emit and possibly get in the vacuum buffer tank 16 and the titanium tetrachloride that condenses and, shut-off valve 18 again; Close vacuum breaker 14 and valve 12.
The system architecture that reclaims residual titanium tetrachloride in copper-wire tower is following: it comprises still kettle 3, copper wire tower 6, first-stage condenser 7, secondary condenser 8 and phlegma buffering storage tank 9; Wherein connect breathing pipeline place and set up branch also at secondary condenser 8 material outlet ends; This also connects vacuum system, and vacuum system is connected with vacuum pump 19.
Described vacuum system is the vacuum buffer tank 16 that is connected with branch by inlet end, be arranged on valve 12 and vacuum breaker 14 in the branch, be arranged on the valve of breathing on the pipeline 11, the underflow valve 18 that is arranged on vacuum buffer tank 16 lower ends constitutes.
Described vacuum buffer tank 16 is connected with vacuum pump 19, and the pipeline between them is provided with vacuum breaker 17.
Described vacuum buffer tank 16 is provided with vacuumometer 15.
Advantage of the present invention and effect are following:
The present invention can reclaim the titanium tetrachloride that remains in the copper wire tower, thereby the loss that has reduced titanium tetrachloride has improved the casting yield of material.Prolong the life-span of copper wire tower, reduced the spent acid water yield.
Because the titanium tetrachloride of emitting with copper wire balls reduces, the hydrochloric acid that makes the titanium tetrachloride hydrolysis reaction produce reduces.Having improved the Working environment in the workshop has also reduced because of the corrosion of hydrochloric acid gas to facilities such as the building in the workshop, equipment and pipelines simultaneously.
Description of drawings
Fig. 1 is the process flow sheet that the present invention reclaims residual titanium tetrachloride in copper-wire tower.
Fig. 2 is that existing copper wire tower removes the vanadium process flow sheet.
Among the figure: 1. valve, 2. regulating valve, 3. still kettle, 4. underflow valve, 5. surplus valve; 6. copper wire tower, 7. first-stage condenser, 8. secondary condenser, 9. phlegma buffering storage tank, 10. valve; 11. valve, 12. valves, 13. vacuumometers, 14. vacuum breakers, 15. vacuumometers; 16. vacuum buffer tank, 17. vacuum breakers, 18. underflow valves, 19. vacuum pumps.
Embodiment
As shown in Figure 1; The present invention reclaims the method for residual titanium tetrachloride in copper-wire tower; Respiratory siphon pass after original copper wire tower is except that secondary condenser in the vanadium technology goes out branch; And connection vacuum system; Before the copper wire balls manipulation of regeneration, reclaim titanium tetrachloride residual in the copper wire tower, the negative pressure of utilizing vacuum system to produce makes the titanium tetrachloride that remains in the copper wire tower lean on the vapour pressure of self to be evaporated to condensing surface, because the low temperature of condensing surface and secondary condenser makes titanium tetrachloride be condensed and is collected into phlegma buffering storage tank.
It is following that the present invention reclaims the concrete grammar of residual titanium tetrachloride in copper-wire tower: when removing after vanadium work carries out for some time, the copper wire surface passivation loses chemically reactive, at this moment needs to take out copper wire balls carry out manipulation of regeneration.Before the copper wire balls manipulation of regeneration; Close heating power supply and the valve 1 and regulating valve 2 of still kettle 3 earlier; Open underflow valve 4 again and be expelled to a part of titanium tetrachloride in titanium tetrachloride in the still kettle 4 and the copper wire tower 6 except that titanium tetrachloride storage tank before the vanadium, close underflow valve 4 then; Shut-off valve 10 is with valve 11 and open valve 12; Start vacuum pump 19; The vacuum tightness of measuring according to the vacuumometer on the vacuum buffer tank 16 15 and control vacuum breaker 17 is automatically closed sky variable valve 17 automatically after vacuum tightness reaches requirement, titanium tetrachloride vapors is pressed with the pass under vacuum requirements and the differing temps; When temperature was in 10～50 ℃, vacuum tightness should be at 700～5000Pa; When temperature was in 50～136 ℃, vacuum tightness should be at 5000～50000Pa; Valve 12 places behind secondary condenser are provided with vacuumometer 13; Automatically control vacuum breaker 14 according to the vacuum tightness of measuring; Make that vacuum tightness is neither too high low only here; Titanium tetrachloride vapors is pressed with the pass under this vacuum tightness and the differing temps, and when temperature was in 10～50 ℃, vacuum tightness should be at 700～5000Pa; When temperature was in 50～136 ℃, vacuum tightness should be at 5000～50000Pa; Thereby, the too high situation of vacuum tightness make the argon gas of breathing in the piping system get into reduction vacuum tightness if can opening valve 11; Titanium tetrachloride in the copper wire tower becomes steam by self vapour pressure effect under vacuum and normal temperature (or being higher than normal temperature) state; Vapour temperature descends because of the heat-eliminating medium effect after steam gets into condensing surface 7 and 8, because temperature reduction titanium tetrachloride vapors is pressed also reduction to make gaseous titanium tetrachloride be condensed into liquid state and is collected into phlegma buffering storage tank 9; After recovery operation is accomplished, close vacuum breaker 17, close vacuum pump 19; Open valve 11, open underflow valve 18 then, emit and possibly get in the vacuum buffer tank 16 and the titanium tetrachloride that condenses and, shut-off valve 18 again; Close vacuum breaker 14 and valve 12.
The system architecture that the present invention reclaims residual titanium tetrachloride in copper-wire tower is following: it comprises still kettle 3, copper wire tower 6, first-stage condenser 7, secondary condenser 8 and phlegma buffering storage tank 9; Wherein connect breathing pipeline place and set up branch also at secondary condenser 8 material outlet ends; This also connects vacuum system, and vacuum system is connected with vacuum pump 19.
Described vacuum system is the vacuum buffer tank 16 that is connected with branch by inlet end, be arranged on valve 12 and vacuum breaker 14 in the branch, be arranged on the valve of breathing on the pipeline 11, the underflow valve 18 that is arranged on vacuum buffer tank 16 lower ends constitutes.Vacuum buffer tank 16 is connected with vacuum pump 19, and the pipeline between them is provided with vacuum breaker 17.Vacuum buffer tank 16 is provided with vacuumometer 15.
Claims (7)
1. method that reclaims residual titanium tetrachloride in copper-wire tower; It is characterized in that the respiratory siphon pass after original copper wire tower is except that secondary condenser in the vanadium technology goes out branch; And connection vacuum system; Before the copper wire balls manipulation of regeneration, reclaim titanium tetrachloride residual in the copper wire tower; The negative pressure of utilizing vacuum system to produce makes the titanium tetrachloride that remains in the copper wire tower lean on the vapour pressure of self to be evaporated to condensing surface, because the low temperature of condensing surface and secondary condenser makes titanium tetrachloride be condensed and is collected into phlegma buffering storage tank.
2. the method for recovery residual titanium tetrachloride in copper-wire tower according to claim 1; It is characterized in that it is heating power supply and first valve (1) and the regulating valve (2) of closing still kettle (3) earlier; Open the first underflow valve (4) again and be expelled to titanium tetrachloride in the still kettle (3) and a part of titanium tetrachloride in the copper wire tower (6) except that titanium tetrachloride storage tank before the vanadium, close the first underflow valve (4) then; Close second valve (10) and the 3rd valve (11) and open the 4th valve (12), start vacuum pump (19), the vacuum tightness in the control vacuum buffer tank (16); Titanium tetrachloride in the copper wire tower (6) is at vacuum and normal temperature or be higher than under the state of normal temperature by self vapour pressure effect and become steam; Vapour temperature descends because of the heat-eliminating medium effect after steam gets into first-stage condenser (7) and secondary condenser (8); Because temperature reduction titanium tetrachloride vapors is pressed also reduction to make gaseous titanium tetrachloride be condensed into liquid state and is collected into phlegma buffering storage tank (9), recovery operation is accomplished.
3. the method for the described recovery residual titanium tetrachloride in copper-wire tower of claim 2 is characterized in that after described recovery operation is accomplished, closing second vacuum breaker (17), closes vacuum pump (19); Open the 3rd valve (11), open the second underflow valve (18) then, emit and to get in the vacuum buffer tank (16) and the titanium tetrachloride that condenses and is closed the second underflow valve (18) again; Close first vacuum breaker (14) and the 4th valve (12).
4. system that reclaims residual titanium tetrachloride in copper-wire tower; It comprises still kettle (3), copper wire tower (6), first-stage condenser (7), secondary condenser (8) and phlegma buffering storage tank (9); It is characterized in that connecting breathing pipeline place at secondary condenser (8) material outlet end sets up branch; This branch connects vacuum system, and vacuum system is connected with vacuum pump (19).
5. the system of the described recovery residual titanium tetrachloride in copper-wire tower of claim 4, it is characterized in that described vacuum system be the vacuum buffer tank (16) that is connected with branch by inlet end, be arranged on the 4th valve (12) and first vacuum breaker (14) in the branch, be arranged on the 3rd valve of breathing on the pipeline (11), the second underflow valve (18) that is arranged on vacuum buffer tank (16) lower end constitutes.
6. the system of the described recovery residual titanium tetrachloride in copper-wire tower of claim 5 is characterized in that described vacuum buffer tank (16) is connected with vacuum pump (19), and the pipeline between them is provided with second vacuum breaker (17).
7. the system of claim 5 or 6 described recovery residual titanium tetrachloride in copper-wire tower is characterized in that described vacuum buffer tank (16) is provided with second vacuumometer (15).
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|---|---|---|---|
| CN2008100125800A CN101638248B (en) | 2008-08-01 | 2008-08-01 | Method and system for recovering residual titanium tetrachloride in copper-wire tower |
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|---|---|---|---|
| CN2008100125800A CN101638248B (en) | 2008-08-01 | 2008-08-01 | Method and system for recovering residual titanium tetrachloride in copper-wire tower |
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| CN101638248A CN101638248A (en) | 2010-02-03 |
| CN101638248B true CN101638248B (en) | 2012-03-28 |
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| CN2008100125800A Active CN101638248B (en) | 2008-08-01 | 2008-08-01 | Method and system for recovering residual titanium tetrachloride in copper-wire tower |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106946286A (en) * | 2017-03-09 | 2017-07-14 | 金川集团股份有限公司 | A kind of crude titanic chloride is except the chemical reaction equipment and method of vanadium |
| CN107267765A (en) * | 2017-08-17 | 2017-10-20 | 东方弗瑞德（北京）科技有限公司 | A kind of method that copper is reclaimed from copper wire waste liquid is washed |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1904096A (en) * | 2006-07-28 | 2007-01-31 | 遵义钛业股份有限公司 | Copper wire tower having supporting device used for removing vanadium impurity in titanium tetrachloride |
| CN101205801A (en) * | 2007-11-22 | 2008-06-25 | 陈敏 | Pumping unit polish rod centralized connecting device |
-
2008
- 2008-08-01 CN CN2008100125800A patent/CN101638248B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1904096A (en) * | 2006-07-28 | 2007-01-31 | 遵义钛业股份有限公司 | Copper wire tower having supporting device used for removing vanadium impurity in titanium tetrachloride |
| CN101205801A (en) * | 2007-11-22 | 2008-06-25 | 陈敏 | Pumping unit polish rod centralized connecting device |
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|---|---|
| CN101638248A (en) | 2010-02-03 |
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