CN103555971A - Device and method for judging blockage of distillation channel during production of titanium sponge - Google Patents
Device and method for judging blockage of distillation channel during production of titanium sponge Download PDFInfo
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- CN103555971A CN103555971A CN201310525935.7A CN201310525935A CN103555971A CN 103555971 A CN103555971 A CN 103555971A CN 201310525935 A CN201310525935 A CN 201310525935A CN 103555971 A CN103555971 A CN 103555971A
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Abstract
The invention discloses a device and a method for judging blockage of a distillation channel during production of titanium sponge. A vacuum measurement instrument of a reduction pot is arranged and is communicated with the inside of the reduction pot through a reduction pot wall or a reduction pot cover to determine the vacuum degree of the reduction pot; the determination result of the vacuum degree of the reduction pot is compared with the vacuum degree in the reduction tank during normal melting, and the blocking condition of the distillation channel is judged according to the difference range of the vacuum degree measuring result of a condensing tank and the vacuum degree measuring result of a vacuum system.
Description
Technical field
The invention belongs to technical field of non-ferrous metallurgy, more particularly, in the vacuum distillation process while relating to a kind of titanium sponge production, judge the apparatus and method that distilling path stops up.
Background technology
While adopting magnesium reduction process to produce titanium sponge, conventionally after magnesium reduction reaction, adopt the mode of vacuum distilling to remove magnesium chloride and the magnesium in titanium sponge.For the magnesium chloride in titanium sponge and the total distillation of magnesium is clean, in vacuum distillation process, to the vacuum tightness in reduction tank, require high, if distilling path stops up in the vacuum distillation process of titanium sponge, the magnesium chloride in titanium sponge or magnesium can not distill totally, and this will have a strong impact on the quality of titanium sponge.At present, domestic titanium sponge manufacturing enterprise, when distillation titanium sponge, has 2～4% distilling path that the phenomenon of stopping up occurs.
In addition, when domestic titanium sponge manufacturing enterprise adopts distillation process vacuum distilling reduzate, conventionally only measure the vacuum tightness of vacuum system and the vacuum tightness of drainer, and in the vacuum distillation process of titanium sponge, can not judge exactly the stopping state of distilling path, while only having after end cycle to be distilled dismounting reduction tank, just can observe distilling path and whether stop up.And the heat that distilling path stops up need to melt down intensification and again titanium sponge carried out to vacuum distilling processing, owing to can not judging in time the stopping state of distilling path, cause titanium sponge at 950～1020 ℃ of temperature, to carry out constant-temperature vacuum distillation for a long time, cause the hardness of titanium sponge to raise, Sponge Titanium Quality Down.
Therefore, need badly a kind of apparatus and method of being convenient to judge that in vacuum distillation process, distilling path stops up are provided.
Summary of the invention
In order solving, in the vacuum distillation process of titanium sponge, can not to judge in time whether distilling path stops up and cause titanium sponge at high temperature to produce for a long time and cause the problem of titanium sponge densification, to the object of the present invention is to provide a kind of method and apparatus that can judge easily and effectively in titanium sponge vacuum distillation process that distilling path stops up.
To achieve these goals, an aspect of of the present present invention provides a kind of device that judges that in titanium sponge vacuum distillation process distilling path stops up, described reduction tank is placed in distillation electric furnace, described drainer is placed in the top of reduction tank, between reduction tank and drainer, by reduction tank cover, separate, on described reduction tank cover, arrange center-aisle and reduction tank be communicated with by described center-aisle with drainer, described center-aisle is closed and is unlocked in vacuum distillation process in magnesiothermic reduction reaction process; Described drainer is connected with the vacuum system for vacuumizing by being arranged on the vacuum pipe at top, on described vacuum pipe, be provided for measuring drainer vacuum tightness drainer vacuum measurement instrument and for measuring the vacuum system vacuum measurement instrument of the vacuum tightness of vacuum system; And described device also comprises reduction tank vacuum measurement instrument, described reduction tank vacuum measurement instrument passes through the internal communication of reduction tank skin or reduction tank cover and reduction tank with the vacuum tightness of measurement reduction tank; Described distilling path is that center-aisle from reduction tank cover is to the passage drainer and vacuum pipe junction.
According to an embodiment who judges the device that distilling path stops up in titanium sponge production process of the present invention, on described reduction tank skin or reduction tank cover, vacuum measurement hole is set, described reduction tank vacuum measurement instrument is connected with described vacuum measurement hole by vacuum rubber flexible pipe.
According to an embodiment who judges the device that distilling path stops up in titanium sponge production process of the present invention, between described reduction tank vacuum measurement instrument and vacuum rubber flexible pipe without between leak source and described vacuum rubber flexible pipe and vacuum measurement hole without leak source.
According to an embodiment who judges the device that distilling path stops up in titanium sponge production process of the present invention, the useful range of described reduction tank vacuum measurement instrument, drainer vacuum measurement instrument, vacuum system vacuum measurement instrument is 0～10
3pa.
The present invention also provides a kind of method that judges that in titanium sponge production process distilling path stops up, described method is undertaken by said apparatus, the vacuum tightness of the vacuum measurement result of reduction tank being reduced described in during with normal heat in tank contrasts, and according to the difference range of the vacuum measurement result of the vacuum measurement result of drainer and vacuum system, judges the stopping state of distilling path.
According to an embodiment who judges the method that distilling path stops up in titanium sponge production process of the present invention, when vacuum distillation time is 50～70h, if more than the time remaining 5h that the vacuum tightness of reduction tank is reduced described in during than normal heat more than the low vacuum 50Pa of tank, and during the difference < 5Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, distilling path stops up.
According to an embodiment who judges the method that distilling path stops up in titanium sponge production process of the present invention, when vacuum distillation time is during at 70～100h, if more than the time remaining 5h that the vacuum tightness of reduction tank is reduced described in during than normal heat more than the low vacuum 30Pa of tank, and during the difference < 3Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, distilling path stops up.
According to an embodiment who judges the method that distilling path stops up in titanium sponge production process of the present invention, when vacuum distillation time is when 100h is above, if more than the time remaining 5h that the vacuum tightness of reduction tank is reduced described in during than normal heat more than the low vacuum 20Pa of tank, and during the difference < 2Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, distilling path stops up.
Simple and the easy installation and removal of device result involved in the present invention, related method easily and effectively, adopt device and method of the present invention can accurately judge the distilling path stopping state in vacuum distillation process, the production cycle that makes distilling path stop up heat shortens, guarantee the rate of grade of titanium sponge, save power consumption cost, increase economic benefit.
Accompanying drawing explanation
The vacuum tightness change curve reducing when Fig. 1 is normal heat in tank.
Fig. 2 is the apparatus structure schematic diagram that judges distilling path obstruction in titanium sponge production process of exemplary embodiment of the present.
Description of reference numerals:
1-reduction tank, 2-drainer, 3-vacuum pipe, 4-reduction tank cover, 5-reduction tank vacuum measurement hole, 6-vacuum rubber flexible pipe, 7-reduction tank vacuum measurement instrument, 8-distillation electric furnace, 9-drainer vacuum measurement instrument, 10-vacuum system vacuum measurement instrument, 11-vacuum system, 12-center-aisle.
Embodiment
Below, with reference to accompanying drawing and example, describe the apparatus and method that judge that in titanium sponge vacuum distillation process distilling path stops up of the present invention in detail.
Fig. 2 is the overall structure schematic diagram that judges the device that distilling path stops up in titanium sponge vacuum distillation process of exemplary embodiment of the present.As shown in Figure 2, the titanium sponge production unit using in the present invention is reduction-distillation integrated apparatus, the inventive system comprises reduction tank 1, drainer 2 and vacuum system 11.Wherein, reduction tank 1 is the principal reaction device of magnesium reduction reaction, and reduction tank 1 is placed in distillation electric furnace 8, carries out magnesiothermic reduction reaction or distillation purification process in magnesiothermic reduction reaction or still-process to be heated.Drainer 2 is placed in the top of reduction tank 1, and drainer 2 is for storing cooling magnesium chloride or magnesium from 1 distillation of reduction tank comes up.
Between reduction tank 1 and drainer 2, by reduction tank cover 4, separate, center-aisle 12 is set on reduction tank cover 4 and reduction tank 1 is communicated with by this center-aisle 12 with drainer 2, and this center-aisle 12 is closed in magnesiothermic reduction reaction process and in vacuum distillation process, is opened with the magnesium chloride by distilling or magnesium steam.Drainer 2 is connected with the vacuum system 11 for vacuumizing by being arranged on the vacuum pipe 3 at top, and vacuum system 11 is mainly used in reduction tank 1 and drainer 2 to vacuumize the maintenance of processing and vacuum state.On vacuum pipe 3, be provided for measuring drainer 2 vacuum tightness drainer vacuum measurement instrument 9 and for measuring the vacuum system vacuum measurement instrument 10 of the vacuum tightness of vacuum system 11.
Distilling path of the present invention is that center-aisle 12 from reduction tank cover 4 is to the passage drainer 2 and vacuum pipe 3 junctions.Due to the magnesium chloride producing in vacuum distillation process or magnesium steam easily cooling be attached in center-aisle 12 or be attached to the grid place that the top of drainer 2 arranges cause described distilling path to stop up, the quality that may affect titanium sponge is produced in the distillation after obstruction.Therefore, for accurate judgement distilling path stopping state, device of the present invention also comprises reduction tank vacuum measurement instrument 7, this reduction tank vacuum measurement instrument 7 by reduction tank skin or reduction tank cover with the internal communication of reduction tank 1 to measure the vacuum tightness of reduction tank.According to one embodiment of present invention, on reduction tank skin or reduction tank cover, vacuum measurement hole 5 is set, the vacuum tightness that reduction tank vacuum measurement instrument logical 7 is crossed that vacuum rubber flexible pipe 6 is connected with vacuum measurement hole 5 and reduced in tank 1 with measurement with reduction tank internal communication.And need to guarantee between reduction tank vacuum measuring gauge 7 and vacuum rubber flexible pipe 6 without between leak source and vacuum rubber flexible pipe 6 and vacuum measurement hole 5 also without leak source, to guarantee to reduce the vacuum measurement accuracy of tank.The range of vacuum measuring gauge 7 can be selected according to actual condition, in exemplary embodiment of the present invention, the useful range of described reduction tank vacuum measurement instrument, drainer vacuum measurement instrument, vacuum system vacuum measurement instrument is 0～103Pa, and what described reduction tank vacuum measurement instrument, drainer vacuum measurement instrument, vacuum system vacuum measurement instrument were measured is Absolute truth reciprocal of duty cycle, reading be on the occasion of.
Particularly, reduzate in reduction tank 1 is in vacuum distillation process, because of magnesium chloride, magnesium and the titanium temperature under same vapour pressure different, volatility difference is separately larger, thereby thereby can utilize magnesium chloride, magnesium and titanium in vacuum distilling separating reducing product to obtain highly purified titanium sponge.The steam of magnesium chloride, magnesium can evaporate in drainer 2 by the center-aisle 12 in reduction tank cover 4 and cold being attached on condensation tank skin is collected.But in vacuum distillation process, when if distilling path is stopped up at the grid place that a large amount of magnesium chlorides, magnesium concentrate on the upper surface of reduction tank cover 4 or concentrates on the top of drainer 2, the vacuum measurement instrument 9 of drainer and the vacuum measurement instrument of vacuum system 10 are measured the vacuum tightness that can only measure drainer 2 and vacuum system 11, this is also not enough to judge the blockage of center-aisle 3, therefore also need to utilize the vacuum tightness in the reduction tank vacuum measurement instrument 7 measurement reduction tanks 1 that are arranged on reduction tank 1 further to judge, concrete determination methods is as described below.
The method that judges that in titanium sponge vacuum distillation process distilling path stops up according to the present invention is to be undertaken by above device, the vacuum measurement result of tank of being about to reduce is reduced the vacuum tightness of tank described in during with normal heat and is contrasted, and according to the difference range of the vacuum measurement result of the vacuum measurement result of drainer and vacuum system, judges the stopping state of distilling path.Specifically, vacuum tightness by real-time detection reduction tank can be grasped vacuum tightness situation wherein in real time, then the vacuum tightness data by the reduction tank with under normal circumstances contrast, and according to the difference range of the vacuum tightness of the vacuum tightness of drainer and vacuum system, can judge the stopping state of distilling path.
The vacuum tightness change curve reducing when Fig. 1 is normal heat in tank, table 1 reduces vacuum tightness and the vacuum system fluctuation vacuum value range of vacuum tightness in tank, drainer when the normal heat, particularly, as shown in Fig. 1 and table 1, when vacuum distillation time is 50～70h, if more than the time remaining 5h that the vacuum tightness of reduction tank is reduced described in during than normal heat more than the low vacuum 50Pa of tank, during the difference < 5Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, distilling path stops up.When vacuum distillation time is during at 70～100h, if more than the time remaining 5h that the vacuum tightness of reduction tank is reduced described in during than normal heat more than the low vacuum 30Pa of tank, during the difference < 3Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, distilling path stops up.When vacuum distillation time is when 100h is above, if more than the time remaining 5h that the vacuum tightness of reduction tank is reduced described in during than normal heat more than the low vacuum 20Pa of tank, during the difference < 2Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, distilling path stops up.If there is not above situation, distilling path does not stop up, and production can be proceeded.If there is above situation, distilling path stops up, need stop immediately producing, and carries out again melting down and producing again after the cleaning of distilling path.
The fluctuation range of vacuum tightness in each assembly during the normal heat of table 1
Below in conjunction with concrete example explanation the present invention.
Example 1:
During vacuum distilling 55h, the vacuum tightness of reduction tank is 120.2Pa, continue after distillation 5h, the vacuum tightness of reduction tank is 118.9Pa, fluctuation vacuum scope is little, with reference to table 1, the time remaining that the vacuum tightness of tank of also now reducing is reduced during than normal heat more than the low vacuum 50Pa of tank more than 5h, and the difference of the vacuum tightness of drainer and the vacuum tightness of vacuum system is 1.9Pa, judgement distilling path stops up.Blowing out is produced, after dismounting reduction tank, find that distilling path stops up really, after cleaning, melt down processing, the average Brinell hardness of producing prepared titanium sponge after processing is 91, and the average Brinell hardness 115 of melting down again the titanium sponge that process for producing makes after finishing than normal production is low by 24.
Example 2:
During vacuum distilling 81h, the vacuum tightness of reduction tank becomes 59.3Pa from 30.6, continue after distillation 5h, the vacuum tightness of reduction tank is 66.7Pa, with reference to table 1, also the time remaining that the vacuum tightness of tank of now reducing is reduced during than normal heat more than the low vacuum 30Pa of tank more than 5h, and the difference of the vacuum tightness of drainer and the vacuum tightness of vacuum system is 0.9Pa, judgement distilling path stops up.Blowing out is produced, after dismounting reduction tank, find that distilling path stops up really, after cleaning, melt down processing, the average Brinell hardness of producing prepared titanium sponge after processing is 97, and the average Brinell hardness 115 of melting down again the titanium sponge that process for producing makes after finishing than normal production is low by 18.
Example 3:
During vacuum distilling 128h, the vacuum tightness of reduction tank becomes 40.7Pa from 13.3, continue after distillation 5h, the vacuum tightness 44.9Pa of reduction tank, with reference to table 1, more than the time remaining 5h that the vacuum tightness of tank of also now reducing is reduced during than normal heat more than the low vacuum 20Pa of tank, and the difference of the vacuum tightness of drainer and the vacuum tightness of vacuum system is 1.03Pa, and judgement distilling path stops up.After dismounting reduction tank, find that distilling path stops up really, after cleaning, melt down processing, the average Brinell hardness of producing prepared titanium sponge after processing is 104, and the average Brinell hardness 115 of melting down again the titanium sponge that process for producing makes after finishing than normal production is low by 11.
In sum, adopt device and method of the present invention can accurately judge the distilling path stopping state in vacuum distillation process, the production cycle that makes center-aisle stop up heat shortens, and guarantees the rate of grade of titanium sponge, saves power consumption cost, increases economic benefit.
Although illustrate and described the apparatus and method that judge that in titanium sponge vacuum distillation process distilling path stops up of the present invention above in conjunction with the embodiments, but what those skilled in the art will appreciate that is, in the situation that do not depart from the spirit and scope of the present invention that limit as claims, can make the various changes in form and details here.
Claims (8)
1. in titanium sponge production process, judge the device that distilling path stops up, it is characterized in that, described device comprises reduction tank, drainer and vacuum system, wherein,
Described reduction tank is placed in distillation electric furnace, described drainer is placed in the top of reduction tank, between reduction tank and drainer, by reduction tank cover, separate, on described reduction tank cover, arrange center-aisle and reduction tank be communicated with by described center-aisle with drainer, described center-aisle is closed and is unlocked in vacuum distillation process in magnesiothermic reduction reaction process;
Described drainer is connected with the vacuum system for vacuumizing by being arranged on the vacuum pipe at top, on described vacuum pipe, be provided for measuring drainer vacuum tightness drainer vacuum measurement instrument and for measuring the vacuum system vacuum measurement instrument of the vacuum tightness of vacuum system;
And described device also comprises reduction tank vacuum measurement instrument, described reduction tank vacuum measurement instrument passes through the internal communication of reduction tank skin or reduction tank cover and reduction tank with the vacuum tightness of measurement reduction tank;
Described distilling path is that center-aisle from reduction tank cover is to the passage drainer and vacuum pipe junction.
2. the device that judges that in titanium sponge production process distilling path stops up according to claim 1, it is characterized in that, on described reduction tank skin or reduction tank cover, vacuum measurement hole is set, described reduction tank vacuum measurement instrument is connected with described vacuum measurement hole by vacuum rubber flexible pipe.
3. the device that judges that in titanium sponge production process distilling path stops up according to claim 2, it is characterized in that, between described reduction tank vacuum measurement instrument and vacuum rubber flexible pipe without between leak source and described vacuum rubber flexible pipe and vacuum measurement hole without leak source.
4. the device that judges that in titanium sponge production process distilling path stops up according to claim 1, is characterized in that, the useful range of described reduction tank vacuum measurement instrument, drainer vacuum measurement instrument, vacuum system vacuum measurement instrument is 0～10
3pa.
5. a method that judges that in titanium sponge production process distilling path stops up, it is characterized in that, described method is undertaken by the device described in any one in claim 1 to 4, and, the vacuum tightness of the vacuum measurement result of reduction tank being reduced described in during with normal heat in tank contrasts, and according to the difference range of the vacuum measurement result of the vacuum measurement result of drainer and vacuum system, judges the stopping state of distilling path.
6. the method that judges that in titanium sponge production process distilling path stops up according to claim 5, it is characterized in that, when vacuum distillation time is 50～70h, if more than the time remaining 5h that the vacuum tightness of reduction tank is reduced described in during than normal heat more than the low vacuum 50Pa of tank, and during the difference < 5Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, distilling path stops up.
7. the method that judges that in titanium sponge production process distilling path stops up according to claim 5, it is characterized in that, when vacuum distillation time is during at 70～100h, if more than the time remaining 5h that the vacuum tightness of reduction tank is reduced described in during than normal heat more than the low vacuum 30Pa of tank, and during the difference < 3Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, distilling path stops up.
8. the method that judges that in titanium sponge production process distilling path stops up according to claim 5, it is characterized in that, when vacuum distillation time is when 100h is above, if more than the time remaining 5h that the vacuum tightness of reduction tank is reduced described in during than normal heat more than the low vacuum 20Pa of tank, and during the difference < 2Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, distilling path stops up.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106086442A (en) * | 2016-07-27 | 2016-11-09 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method preventing titanium sponge vacuum distilling channel blockage |
| CN106191470A (en) * | 2016-08-16 | 2016-12-07 | 云南冶金新立钛业有限公司 | Manufacture the method for controlling security of titanium sponge |
| CN107523704A (en) * | 2017-08-17 | 2017-12-29 | 东方弗瑞德（北京）科技有限公司 | Reactor covers greatly magnesium chloride pipe passage processing method in a kind of titanium sponge production |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106086442A (en) * | 2016-07-27 | 2016-11-09 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method preventing titanium sponge vacuum distilling channel blockage |
| CN106191470A (en) * | 2016-08-16 | 2016-12-07 | 云南冶金新立钛业有限公司 | Manufacture the method for controlling security of titanium sponge |
| CN107523704A (en) * | 2017-08-17 | 2017-12-29 | 东方弗瑞德（北京）科技有限公司 | Reactor covers greatly magnesium chloride pipe passage processing method in a kind of titanium sponge production |
| CN107523704B (en) * | 2017-08-17 | 2019-03-08 | 东方弗瑞德（北京）科技有限公司 | Reactor covers greatly magnesium chloride pipe channel processing method in a kind of titanium sponge production |
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