CN103555971B - Method for judging blockage of distillation channel during production of titanium sponge - Google Patents
Method for judging blockage of distillation channel during production of titanium sponge Download PDFInfo
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- CN103555971B CN103555971B CN201310525935.7A CN201310525935A CN103555971B CN 103555971 B CN103555971 B CN 103555971B CN 201310525935 A CN201310525935 A CN 201310525935A CN 103555971 B CN103555971 B CN 103555971B
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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 vacuum distillation process when relating to a kind of titanium sponge production, judge the method that distilling path blocks.
Background technology
When adopting magnesium reduction process to produce titanium sponge, usually after magnesium reduction reaction, the mode of vacuum distilling is adopted to remove magnesium chloride in titanium sponge and magnesium.In order to the magnesium chloride in titanium sponge and magnesium are distilled totally totally, high to the vacuum level requirements in reductive jar in vacuum distillation process, if distilling path blocking in the vacuum distillation process of titanium sponge, magnesium chloride then 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 production enterprise, when distilling titanium sponge, has the distilling path of 2 ~ 4% that the phenomenon of blocking occurs.
In addition, during domestic titanium sponge production enterprise employing distillation process vacuum distilling reduzate, usually only the vacuum tightness of vacuum system and the vacuum tightness of drainer is measured, and the stopping state of distilling path can not be judged exactly in the vacuum distillation process of titanium sponge, just can observe distilling path when dismantling reductive jar after only having end cycle to be distilled and whether block.And the heat of distilling path blocking needs to melt down intensification and again carries out vacuum distilling process to titanium sponge, due to the stopping state of distilling path can not be judged in time, titanium sponge is caused at temperature 950 ~ 1020 DEG C, to carry out constant-temperature vacuum distillation for a long time, the hardness of titanium sponge is caused to raise, Sponge Titanium Quality Down.
Therefore, need badly a kind of apparatus and method being convenient to judge distilling path blocking in vacuum distillation process are provided.
Summary of the invention
Can not judge whether distilling path blocks and cause titanium sponge at high temperature to produce for a long time and cause the problem of titanium sponge densification in order to solve in time in the vacuum distillation process of titanium sponge, the object of the present invention is to provide and a kind ofly can easily and effectively judge the method and apparatus that distilling path blocks in titanium sponge vacuum distillation process.
To achieve these goals, an aspect of of the present present invention provides and a kind ofly in titanium sponge vacuum distillation process, judges the device that distilling path blocks, described reductive jar is placed in distillation electric furnace, described drainer is placed in the top of reductive jar, separated by reductive jar cover between reductive jar and drainer, described reductive jar cover arranges center-aisle and reductive jar is 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 the vacuum pipe being arranged on top, described vacuum pipe is arranged the drainer vacuum measurement instrument of the vacuum tightness for measuring drainer and the vacuum system vacuum measurement instrument for the vacuum tightness of measuring vacuum system; Further, described device also comprises reductive jar vacuum measurement instrument, and described reductive jar vacuum measurement instrument is communicated with the vacuum tightness to measure reductive jar by reduction tank skin or reductive jar cover with the inside of reductive jar; Described distilling path is from the center-aisle reductive jar cover to the passage drainer and vacuum pipe junction.
According to the embodiment judging the device that distilling path blocks in titanium sponge production process of the present invention, described reduction tank skin or reductive jar cover arrange vacuum measurement hole, and described reductive jar vacuum measurement instrument is connected with described vacuum measurement hole by vacuum rubber flexible pipe.
According to the embodiment judging the device that distilling path blocks in titanium sponge production process of the present invention, without leak source and without leak source between described vacuum rubber flexible pipe and vacuum measurement hole between described reductive jar vacuum measurement instrument and vacuum rubber flexible pipe.
According to the embodiment judging the device that distilling path blocks in titanium sponge production process of the present invention, the useful range of described reductive jar vacuum measurement instrument, drainer vacuum measurement instrument, vacuum system vacuum measurement instrument is 0 ~ 10
3pa.
Present invention also offers and a kind ofly in titanium sponge production process, judge the method that distilling path blocks, described method is undertaken by said apparatus, vacuum tightness in described reductive jar when the vacuum measurement result of reductive jar and normal heat is contrasted, and judges the stopping state of distilling path according to the difference range of the vacuum measurement result of drainer and the vacuum measurement result of vacuum system.
According to the embodiment judging the method that distilling path blocks in titanium sponge production process of the present invention, when vacuum distillation time is 50 ~ 70h, if the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 50Pa of reductive jar described during normal heat, and during the difference < 5Pa of the vacuum tightness of the vacuum tightness of drainer and vacuum system, then distilling path blocks.
According to the embodiment judging the method that distilling path blocks in titanium sponge production process of the present invention, when vacuum distillation time is at 70 ~ 100h, if the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 30Pa of reductive jar described during normal heat, and during the difference < 3Pa of the vacuum tightness of the vacuum tightness of drainer and vacuum system, then distilling path blocks.
According to the embodiment judging the method that distilling path blocks in titanium sponge production process of the present invention, when vacuum distillation time is at more than 100h, if the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 20Pa of reductive jar described during normal heat, and during the difference < 2Pa of the vacuum tightness of the vacuum tightness of drainer and vacuum system, then distilling path blocks.
Simple and the easy installation and removal of device result involved in the present invention, involved method easily and effectively, adopt the distilling path stopping state that device and method of the present invention can accurately judge in vacuum distillation process, the production cycle making distilling path block heat shortens, ensure the rate of grade of titanium sponge, save power consumption cost, increase economic benefit.
Accompanying drawing explanation
Vacuum tightness change curve when Fig. 1 is normal heat in reductive jar.
Fig. 2 be exemplary embodiment of the present in titanium sponge production process, judge the apparatus structure schematic diagram that distilling path blocks.
Description of reference numerals:
1-reductive jar, 2-drainer, 3-vacuum pipe, 4-reductive jar cover, 5-reductive jar vacuum measurement hole, 6-vacuum rubber flexible pipe, 7-reductive jar vacuum measurement instrument, 8-distill electric furnace, 9-drainer vacuum measurement instrument, 10-vacuum system vacuum measurement instrument, 11-vacuum system, 12-center-aisle.
Embodiment
Below, describe in detail with reference to accompanying drawing and example and of the present inventionly in titanium sponge vacuum distillation process, judge the apparatus and method that distilling path blocks.
Fig. 2 is the overall structure schematic diagram judging the device that distilling path blocks in titanium sponge vacuum distillation process of exemplary embodiment of the present.As shown in Figure 2, the titanium sponge production equipment used in the present invention is reduction-distillation integrated apparatus, namely the inventive system comprises reductive jar 1, drainer 2 and vacuum system 11.Wherein, reductive jar 1 is the main reactor of magnesium reduction reaction, and reductive jar 1 is placed in distillation electric furnace 8, to be carried out magnesiothermic reduction reaction or distillation purification process by heating in magnesiothermic reduction reaction or still-process.Drainer 2 is placed in the top of reductive jar 1, and drainer 2 is for storing the magnesium chloride or magnesium that cool after distillation from reductive jar 1 comes up.
Separated by reductive jar cover 4 between reductive jar 1 and drainer 2, reductive jar cover 4 is arranged center-aisle 12 and reductive jar 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 is opened in vacuum distillation process with the magnesium chloride by distilling or magnesium steam.Drainer 2 is connected with the vacuum system 11 for vacuumizing by the vacuum pipe 3 being arranged on top, and vacuum system 11 is mainly used in vacuumizing reductive jar 1 and drainer 2 processing and the maintenance of vacuum state.Vacuum pipe 3 is arranged the drainer vacuum measurement instrument 9 of the vacuum tightness for measuring drainer 2 and the vacuum system vacuum measurement instrument 10 for the vacuum tightness of measuring vacuum system 11.
Distilling path of the present invention is from the center-aisle 12 reductive jar cover 4 to the passage drainer 2 and vacuum pipe 3 junction.Cause described distilling path block because the magnesium chloride that produces in vacuum distillation process or magnesium steam easily cool the grid place being attached in center-aisle 12 or be attached to drainer 2 top and arranging, the distillation production after blocking may affect the quality of titanium sponge.Therefore, in order to accurately judge distilling path stopping state, device of the present invention also comprises reductive jar vacuum measurement instrument 7, and this reductive jar vacuum measurement instrument 7 is communicated with the vacuum tightness to measure reductive jar by reduction tank skin or reductive jar cover with the inside of reductive jar 1.According to one embodiment of present invention, reduction tank skin or reductive jar cover arrange vacuum measurement hole 5, and reductive jar vacuum measurement instrument leads to 7 mistake vacuum rubber flexible pipes 6 and is connected with vacuum measurement hole 5 and is communicated with the vacuum tightness measured in reductive jar 1 with reductive jar inside.And need ensure without leak source and also without leak source between vacuum rubber flexible pipe 6 and vacuum measurement hole 5 between reductive jar vacuum measuring gauge 7 and vacuum rubber flexible pipe 6, to guarantee the vacuum measurement accuracy of reductive jar.The range of vacuum measuring gauge 7 can be selected according to actual condition, and in an exemplary embodiment of the present invention, the useful range of described reductive jar vacuum measurement instrument, drainer vacuum measurement instrument, vacuum system vacuum measurement instrument is 0 ~ 10
3pa, and described reductive jar vacuum measurement instrument, drainer vacuum measurement instrument, vacuum system vacuum measurement instrument measure be Absolute truth reciprocal of duty cycle, reading be on the occasion of.
Particularly, reduzate in reductive jar 1 is in vacuum distillation process, because magnesium chloride, magnesium and the titanium temperature under same vapour pressure is different, respective volatility difference is comparatively large, thus can utilize magnesium chloride, magnesium and titanium in vacuum distilling separating reducing product thus obtain highly purified titanium sponge.The steam of magnesium chloride, magnesium can be evaporated into by the center-aisle 12 in reductive jar cover 4 in drainer 2 and cold being attached on condensation tank skin is collected.But in vacuum distillation process, if when a large amount of magnesium chloride, magnesium concentrate on the upper surface of reductive jar cover 4 or concentrate on the grid place blocking distilling path at top of drainer 2, the vacuum tightness that can only measure drainer 2 and vacuum system 11 measured by the vacuum measurement instrument 9 of drainer and the vacuum measurement instrument 10 of vacuum system, this is also not enough to the blockage judging center-aisle 3, therefore also need to utilize reductive jar vacuum measurement instrument 7 vacuum tightness measured in reductive jar 1 be arranged on reductive jar 1 to come further to judge, concrete determination methods is as described below.
The method judging that in titanium sponge vacuum distillation process distilling path blocks according to the present invention is undertaken by above device, during vacuum measurement result and normal heat by reductive jar, the vacuum tightness of described reductive jar contrasts, and judges the stopping state of distilling path according to the difference range of the vacuum measurement result of drainer and the vacuum measurement result of vacuum system.Specifically, vacuum tightness situation wherein can be grasped in real time by the vacuum tightness detecting reductive jar in real time, then by contrasting with the vacuum tightness data of reductive jar under normal circumstances, and the stopping state of distilling path can be judged according to the difference range of the vacuum tightness of drainer and the vacuum tightness of vacuum system.
Vacuum tightness change curve when Fig. 1 is normal heat in reductive jar, the vacuum tightness of vacuum tightness, drainer and vacuum system fluctuation vacuum value range in reductive jar when table 1 is normal heat, particularly, as shown in figure 1 and table 1, when vacuum distillation time is 50 ~ 70h, if the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 50Pa of reductive jar described during normal heat, during the difference < 5Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, then distilling path blocks.When vacuum distillation time is at 70 ~ 100h, if the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 30Pa of reductive jar described during normal heat, during the difference < 3Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, then distilling path blocks.When vacuum distillation time is at more than 100h, if the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 20Pa of reductive jar described during normal heat, during the difference < 2Pa of the vacuum tightness of drainer and the vacuum tightness of vacuum system, then distilling path blocks.If there is not above situation, then distilling path does not block, and production can proceed.If there is above situation, then distilling path blocks, need stop immediately producing, and again melts down again and produce after carrying out 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, the present invention is described.
Example 1:
During vacuum distilling 55h, the vacuum tightness of reductive jar is 120.2Pa, after continuing distillation 5h, the vacuum tightness of reductive jar is 118.9Pa, fluctuation vacuum scope is little, with reference to table 1, also namely now the vacuum tightness of reductive jar than time remaining more than the 5h of more than the low vacuum 50Pa of reductive jar during normal heat, and the difference of the vacuum tightness of the vacuum tightness of drainer and vacuum system is 1.9Pa, judge that distilling path blocks.Blowing out is produced, the indeed blocking of distilling path is found after dismounting reductive jar, melt down process after cleaning, the average Brinell hardness of the titanium sponge obtained by producing after process is 91, and the average Brinell hardness 115 of melting down the titanium sponge that process for producing obtains after terminating than normal production is again low by 24.
Example 2:
During vacuum distilling 81h, the vacuum tightness of reductive jar becomes 59.3Pa from 30.6, after continuing distillation 5h, the vacuum tightness of reductive jar is 66.7Pa, with reference to table 1, also namely now the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 30Pa of reductive jar during normal heat, and the difference of the vacuum tightness of the vacuum tightness of drainer and vacuum system is 0.9Pa, judge that distilling path blocks.Blowing out is produced, the indeed blocking of distilling path is found after dismounting reductive jar, melt down process after cleaning, the average Brinell hardness of the titanium sponge obtained by producing after process is 97, and the average Brinell hardness 115 of melting down the titanium sponge that process for producing obtains after terminating than normal production is again low by 18.
Example 3:
During vacuum distilling 128h, the vacuum tightness of reductive jar becomes 40.7Pa from 13.3, after continuing distillation 5h, the vacuum tightness 44.9Pa of reductive jar, with reference to table 1, also namely now the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 20Pa of reductive jar during normal heat, and the difference of the vacuum tightness of the vacuum tightness of drainer and vacuum system is 1.03Pa, judges that distilling path blocks.The indeed blocking of distilling path is found after dismounting reductive jar, process is melted down after cleaning, the average Brinell hardness of the titanium sponge obtained by producing after process is 104, and the average Brinell hardness 115 of melting down the titanium sponge that process for producing obtains after terminating than normal production is again low by 11.
In sum, adopt the distilling path stopping state that device and method of the present invention can accurately judge in vacuum distillation process, the production cycle making center-aisle block heat shortens, and ensures the rate of grade of titanium sponge, saves power consumption cost, increases economic benefit.
Of the present inventionly in titanium sponge vacuum distillation process, the apparatus and method that distilling path blocks are judged above although illustrate and describe in conjunction with the embodiments, but what those skilled in the art will appreciate that is, when not departing from the spirit and scope of the present invention as claims restriction, the various changes in form and details can be made here.
Claims (4)
1. in titanium sponge production process, judge the method that distilling path blocks, it is characterized in that, described method is by judging that in titanium sponge production process the device that distilling path blocks carries out, and described device comprises reductive jar, drainer and vacuum system, wherein,
Described reductive jar is placed in distillation electric furnace, described drainer is placed in the top of reductive jar, separated by reductive jar cover between reductive jar and drainer, described reductive jar cover arranges center-aisle and reductive jar is 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 the vacuum pipe being arranged on top, described vacuum pipe is arranged the drainer vacuum measurement instrument of the vacuum tightness for measuring drainer and the vacuum system vacuum measurement instrument for the vacuum tightness of measuring vacuum system;
Described device also comprises reductive jar vacuum measurement instrument, and described reductive jar vacuum measurement instrument is communicated with the vacuum tightness to measure reductive jar by reduction tank skin or reductive jar cover with the inside of reductive jar;
Described distilling path is from the center-aisle reductive jar cover to the passage drainer and vacuum pipe junction;
Further, the vacuum tightness in described reductive jar when the vacuum measurement result of reductive jar and normal heat is contrasted, and judge the stopping state of distilling path according to the difference range of the vacuum measurement result of drainer and the vacuum measurement result of vacuum system; When vacuum distillation time is 50 ~ 70h, if the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 50Pa of reductive jar described during normal heat, and during the difference < 5Pa of the vacuum tightness of the vacuum tightness of drainer and vacuum system, then distilling path blocks; When vacuum distillation time is at 70 ~ 100h, if the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 30Pa of reductive jar described during normal heat, and during the difference < 3Pa of the vacuum tightness of the vacuum tightness of drainer and vacuum system, then distilling path blocks; When vacuum distillation time is at more than 100h, if the vacuum tightness of reductive jar is than time remaining more than the 5h of more than the low vacuum 20Pa of reductive jar described during normal heat, and during the difference < 2Pa of the vacuum tightness of the vacuum tightness of drainer and vacuum system, then distilling path blocks.
2. according to claim 1ly in titanium sponge production process, judge the method that distilling path blocks, it is characterized in that, described reduction tank skin or reductive jar cover arrange vacuum measurement hole, and described reductive jar vacuum measurement instrument is connected with described vacuum measurement hole by vacuum rubber flexible pipe.
3. according to claim 1ly in titanium sponge production process, judge the method that distilling path blocks, it is characterized in that, without leak source and without leak source between described vacuum rubber flexible pipe and vacuum measurement hole between described reductive jar vacuum measurement instrument and vacuum rubber flexible pipe.
4. according to claim 1ly in titanium sponge production process, judge the method that distilling path blocks, it is characterized in that, the useful range of described reductive jar vacuum measurement instrument, drainer vacuum measurement instrument, vacuum system vacuum measurement instrument is 0 ~ 10
3pa.
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| CN106086442B (en) * | 2016-07-27 | 2018-04-10 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method for preventing titanium sponge vacuum distillation 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 |
| 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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