CN104831088B - A kind of titanium sponge reduction distillation reaction unit and production technology - Google Patents
A kind of titanium sponge reduction distillation reaction unit and production technology Download PDFInfo
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Abstract
The present invention relates to a kind of technique using titanium sponge reduction distillation reaction unit to produce titanium sponge, the reaction unit that this technique uses is connected by tank body and big lid formed by flange rubber cushion, bolt group.The technique using said apparatus to produce titanium sponge is, is used as condenser, and the reaction unit of first-class blind plate on big lid central tube by last round of time, or directly will assemble, and through taking out qualified empty reaction unit in advance, after hanging in heating furnace, uses as reactor；Vacuumize two hours from row's magnesium chloride pipe, then argon filling, heating, after temperature reaches 700 DEG C, in the case of argon filling, pull down the blind plate on big lid central tube, at this, disposably add liquid magnesium；In reduction process, in charging sleeve pipe one, charging sleeve pipe two and three positions of central tube, charge pipe is installed, carries out 3 parallel chargings.The present invention can not only change titanium sponge and stick together structure, solves fine and close problem, and can also be greatly improved overall charging rate, makes distillation become easy, cycle time.
Description
Technical field
The invention belongs to titanium sponge production field, particularly to a kind of titanium sponge reduction distillation reaction unit and production technology.
Background technology
Through the development of 60 years, titanium sponge production technique gradually tended to unified: Kroll process (magnesium processes) and reduction distillation Joint Production, and equipment, production capacity are towards development of maximizing.
Titanium sponge reduction distillation operation, is the important step being produced titanium sponge by titanium tetrachloride, is the key of the quality of titanium sponge, cost control.In reaction unit, disposably add magnesium, then in reduction process, continuously add titanium tetrachloride, titanium tetrachloride after liquid magnesium and gasification react at liquid magnesium surface, generation liquid chlorine magnesium (sinking to discharge bottom reaction unit and by interruption) and the titanium of spongy (rich in capillary) of solid-state.After reduction terminates, under vacuum and the condition of high temperature, by magnesium remaining in reaction unit and magnesium chloride, distill to condenser, it is achieved the purification to titanium sponge.Titanium sponge to realize application, titanium must be sticked together broken, be pressed into electrode, vacuum arc furnace melting ingot casting, make section bar.
Titanium sponge reduction reaction is exothermic reaction, and reaction heat must transmit by the way of convection current, mass transfer from inside to outside, and distance reaction unit wall is the most remote, and heat radiation is more difficult to, and temperature is the highest.
Titanium sponge reduction produces and all uses point type charging at present, is i.e. fed in one or several some position by charge pipe.Titanium tetrachloride concentration, reduction reaction severe degree, reaction heat, all in normal distribution, i.e. closer to feed point position vertical line position, its value is the biggest.
The reaction unit that the also original production of traditional sponge titanium is used, is all drum type brake, and feed point position is in cylinder center position, therefore reaction unit center reaction heat is concentrated most, and temperature is the highest, may result in titanium sponge sintering and fine and close.
Some mechanisms carried out the exploration of feeding raw materials from more than one places, but limited by drum type brake reaction unit, feed point position can only be symmetrical around cylinder center's line, although the reaction heat of position of center line so can be reduced, but can't resolve the heat radiation of position of center line, therefore feeding raw materials from more than one places DeGrain, increases equipment making and manual operation difficulty on the contrary.
The technology of the operations such as the chlorination of current titanium sponge production the most in the world, refined, electrolysis is all relatively more open, and reduction distillation technology all takes the policy of bottling up only, and domestic also do not have technology transfer precedent.
The aspects such as the titanium sponge quality of China, integrated cost, the most do not locate inferior position, but reduction distillation unit product power consumption, titanium sponge machinability (compactness extent is the most then prone to processing) are obvious with advanced international standard gap.The most domestic all select simple equipment, production capacity to maximize, i.e. increase reaction unit diameter and height, reduce unit product power consumption；And this equipment enlarging will make product radiating condition be deteriorated, titanium sticks together, and height increases, single stove product accounts for stove overlong time, cause titanium stick together central part and bottom fine and close, machinability is deteriorated.
Summary of the invention
For overcoming drawbacks described above, the technical problem to be solved in the present invention is to provide a kind of novel structure, simple to operate, dispel the heat preferable titanium sponge reduction distillation reaction unit and production technology.
This device is connected by tank body and big lid formed by flange rubber cushion, bolt group, and tank body includes: base plate, sieve plate, row's magnesium chloride sleeve pipe, tank flange, kidney-shaped cylinder；Big lid includes: row's magnesium chloride pipe, heat-insulation layer, inner heating device, cover flange, big lid lower flange, central tube, charging sleeve pipe one, short cylinder, charging sleeve pipe two greatly.This reaction unit entirety spatially kidney ellipsoid structure, described base plate is one piece of swash plate, and oblique angle is 2～5 °, is positioned at the foot of whole device, cooperatively forms open three-dimensional kidney-shaped tank body with kidney-shaped cylinder；Described sieve plate is positioned at the top of base plate, is fixed on reaction unit kidney-shaped cylinder inboard wall by spot welding mode is unsettled, and the distance between sieve plate and base plate is 20～30；Described row's magnesium chloride pipe is L-shaped, is welded on and covers greatly, is inserted in the row's magnesium chloride sleeve pipe being welded on inside kidney-shaped cylinder circular arc one end；Under great Gai, above tank body, it is provided with heat-insulation layer, for the still-process insulation to reaction unit, reduces the thermal loss in tank body, avoid condensate to be condensate under big lid simultaneously；Described charging sleeve pipe one, charging sleeve pipe two are respectively symmetrically the center of arc being arranged at big lid lower flange two ends；Central tube is arranged on the center of big lid, is positioned in the middle of charging sleeve pipe one, charging sleeve pipe two；Inner heating device is positioned in the middle part of big lid lower flange, the periphery of central tube, is mainly used in still-process heating central tube；Flange rubber cushion is kidney ellipsoid structure, between big lid lower flange and tank flange, big lid lower flange, tank flange is tightened together by bolt group.
Described bolt group is made up of 20～30 bolts, for big lid lower flange, tank flange being fastened together.
Described short cylinder passes through welding manner, and by covering greatly flange, big lid lower flange links together.
Described reaction unit tank body width is 1.2～1.5 meters, and height is 1.5～2.5 times of width, 2～3 times of a length of width.
The gradient that described sieve plate is identical with reaction unit base plate holding, opposite direction is assembled, to ensure sieve plate upper surface level.
The technique using above-mentioned titanium sponge reduction distillation reaction unit to produce titanium sponge is:
Last round of time is used as condenser, and the reaction unit of first-class blind plate on big lid central tube, or directly will assemble, and through taking out qualified empty reaction unit in advance, after hanging in heating furnace, use as reactor；Vacuumize two hours from row's magnesium chloride pipe, then argon filling, heating, after temperature reaches 700 DEG C, in the case of argon filling, pull down the blind plate on big lid central tube, at this, disposably add liquid magnesium；In reduction process, in charging sleeve pipe one, charging sleeve pipe two and three positions of central tube, charge pipe is installed, carries out 3 parallel chargings；In big lid central tube position, charge pipe and bleeder pipe must be installed simultaneously, at the end of discharge magnesium chloride, pull up bleeder pipe plug with quick pressure releasing；With 4 thermometrics of reactor outer wall, as the foundation controlling charging rate；Start charging when reactor free surface correspondence position temperature reaches more than 750 DEG C, charging process maximum temperature must control between 750～870 DEG C；Ensure the equilibrium of three charge pipe charging rates；
After reduction process terminates, unload charge pipe, airtight with high temperature resistant packing ring and blind plate respectively on charging sleeve pipe one, charging sleeve pipe two, big lid central tube loads onto magnesium plug or high-temperature valve；To assemble and take out in advance qualified a set of empty reaction unit, and as condenser, be bolted or weld and realize reactor and couple with condenser, in condenser end connection vacuum system, carry out vacuum distillation；With outside heating furnace electric furnace heating wire 3～4 thermometrics, the foundation controlled as vapo(u)rizing temperature；After distillation terminates, being separated with condenser by reactor in the case of pressure-fired, the reactor equipped with product hangs in cooling jacket cooling；Condenser hangs in heating furnace, and the reduction distillation entering next one produces.
Use reaction unit of the present invention to produce titanium sponge to provide the benefit that:
First, change titanium sponge and stick together structure, solve fine and close problem.Utilizing and laterally increase reaction unit size, it is achieved parallel feeding raw materials from more than one places, titanium sticks together flat, height reduction, and radiating condition improves, it is possible to decrease the temperature of tank body center, it is to avoid titanium sticks together sintering in reduction process and fine and close.
Second, feeding raw materials from more than one places, overall charging rate improves.Compared with identical single stove production capacity tradition feed way, a single point position charging rate reduces, but total charging rate can significantly improve.
3rd, distillation becomes easy, and the cycle can shorten.Reaction unit cross-sectional area and titanium stick together surface area strengthen, in still-process in the unit interval free magnesium and free magnesium chloride volatile quantity increasing；Titanium sticks together flat, and internal any position is the shortest from the stick together distance on surface of titanium, and the stick together path of middle remaining magnesium and magnesium chloride volatilization of titanium is shorter, adds short texture, and capillary is many, and distillation is easily.
Accompanying drawing explanation
Fig. 1 is the front view of reduction distillation reaction unit of the present invention；
Fig. 2 is the top view of reduction distillation reaction unit of the present invention.
In figure: 1-base plate, 2-sieve plate, 3-row's magnesium chloride sleeve pipe, 4-flange rubber cushion, 5-row's magnesium chloride pipe, 6-heat-insulation layer, 7-inner heating device, 8-bolt group, 9-cover greatly flange, 10-big lid lower flange, 11-tank flange, 12-kidney-shaped cylinder, 13-central tube, 14-charging sleeve pipe one, 15-short cylinder, 16-feed sleeve pipe two.
Detailed description of the invention
Below in conjunction with the accompanying drawings the present invention is described in detail。
The present invention is to realize equipment by horizontal increased in size to maximize, and uses parallel feeding raw materials from more than one places, had both reduced feed point vertical line position reaction heat, improves again the heat radiation of reaction unit center, thus solves titanium sponge and stick together fine and close problem.
As shown in Figure 1 and Figure 2, a kind of titanium sponge reduction distillation reaction unit, this device is connected by tank body and big lid formed by flange rubber cushion 4, bolt group 8, and tank body includes: base plate 1, sieve plate 2, row magnesium chloride sleeve pipe 3, tank flange 11, kidney-shaped cylinder 12；Big lid includes: row's magnesium chloride pipe 5, heat-insulation layer 6, inner heating device 7, cover flange 9, big lid lower flange 10, central tube 13, charging sleeve pipe 1, short cylinder 15, charging sleeve pipe 2 16 greatly.This reaction unit entirety spatially kidney ellipsoid structure, described base plate 1 is one piece of swash plate, and oblique angle is 2～5 °, is positioned at the foot of whole device, cooperatively forms open three-dimensional kidney-shaped tank body with kidney-shaped cylinder 12；Described sieve plate 2 is positioned at the top of base plate 1, is fixed on reaction unit kidney-shaped cylinder 12 inwall by spot welding mode is unsettled, and the distance between sieve plate 2 and base plate 1 is 20～30；Described row's magnesium chloride pipe 5 is L-shaped, is welded on and covers greatly, is inserted in the row's magnesium chloride sleeve pipe 3 being welded on inside kidney-shaped cylinder 12 circular arc one end；Under great Gai, above tank body, it is provided with heat-insulation layer 6, for the still-process insulation to reaction unit, reduces the thermal loss in tank body, avoid condensate to be condensate under big lid simultaneously；Described charging sleeve pipe 1, charging sleeve pipe 2 16 are respectively symmetrically the center of arc being arranged at big lid lower flange 10 two ends；Central tube 13 is arranged on the center of big lid, is positioned in the middle of charging sleeve pipe 1, charging sleeve pipe 2 16；Inner heating device 7 is positioned in the middle part of big lid lower flange 10, the periphery of central tube 13, is mainly used in still-process heating central tube 13；Flange rubber cushion 4 is in kidney ellipsoid structure, between big lid lower flange 10 and tank flange 11, big lid lower flange 10, tank flange 11 is tightened together by bolt group 8.Short cylinder 15 is by welding manner, and by covering greatly flange 9, big lid lower flange 10 links together.
Sieve plate 2 when mounted, is first hung in kidney-shaped cylinder 12 by titanium sponge reduction distillation reaction unit of the present invention；After base plate 1 is set level, the most upwards sling 20～30mm, in four positions that sieve plate 2 surrounding is symmetrical, take spot welding mode, it is fixed on unsettled for sieve plate 2 on kidney-shaped cylinder 12 inwall, the degree of spot welding both to ensure to be unlikely in still-process to fall down and affect still-process and carry out, and can guarantee that again and can destroy solder joint in reduction process and not affect product and take out.To cover on tank body greatly, by flange rubber cushion 4 and bolt group 8, be assembled into a set of titanium sponge reduction distillation reaction unit.The row's magnesium chloride pipe 5 covered greatly must be inserted in the row's magnesium chloride sleeve pipe 3 being welded in kidney-shaped cylinder 12.Reaction unit of the present invention must be qualified through pre-evacuation, just can be delivered for use.Qualified complete reaction unit, is used as condenser in still-process, or is used as reactor in directly hanging in heating furnace in reduction process.
The production process producing titanium sponge is first to carry out reducing distilling again, has only to a reaction unit as reactor in reduction process；In still-process, in addition it is also necessary to a reaction unit makees condenser, by magnesium and the magnesium chloride of reactor remaining, by cooling down in being atmospherically distilled to condenser, thus the purpose of titanium sponge in reaching purified reaction device.Concretely comprise the following steps: last round of time is used as condenser, and the reaction unit of first-class blind plate on big lid central tube 13, or directly will assemble, and through taking out qualified empty reaction unit in advance, after hanging in heating furnace, use as reactor；Vacuumize two hours from row's magnesium chloride pipe 5, then argon filling, heating, after temperature reaches 700 DEG C, in the case of argon filling, pull down the blind plate on big lid central tube 13, at this, disposably add liquid magnesium；In reduction process, in charging sleeve pipe 1, charging sleeve pipe 2 16 and 13 3 positions of central tube, charge pipe is installed, carries out 3 parallel chargings；In big lid central tube 13 position, charge pipe and bleeder pipe must be installed simultaneously, at the end of discharge magnesium chloride, pull up bleeder pipe plug with quick pressure releasing；With 4 thermometrics of reactor outer wall, as the foundation controlling charging rate；Start charging when reactor free surface correspondence position temperature reaches more than 750 DEG C, charging process maximum temperature must control between 750～870 DEG C；Ensure the equilibrium of three charge pipe charging rates.
After reduction process terminates, unload charge pipe, airtight with high temperature resistant packing ring and blind plate respectively on charging sleeve pipe 1, charging sleeve pipe 2 16, big lid central tube 13 loads onto magnesium plug or high-temperature valve；To assemble and take out in advance qualified a set of empty reaction unit, and as condenser, be bolted or weld and realize reactor and couple with condenser, in condenser end connection vacuum system, carry out vacuum distillation；With outside heating furnace electric furnace heating wire 3～4 thermometrics, the foundation controlled as vapo(u)rizing temperature；After distillation terminates, being separated with condenser by reactor in the case of pressure-fired, the reactor equipped with product hangs in cooling jacket cooling；Condenser hangs in heating furnace, and the reduction distillation entering next one produces.
After the Sponge Titanium in reactor cools down, hang Kai great Gai, take out with instruments such as pneumatic picks and climb wall titanium；Then hang out titanium with steel wire rope to stick together, peel off sieve plate with pneumatic pick, and titanium sticks together the contaminated product in surface.Sticking together stance with titanium sponge, longitudinally send into hydraulic press stripping and slicing, whole titanium sticks together hybrid packed.
Titanium sponge reduction distillation reaction unit of the present invention is the width, highly by reducing reaction unit, laterally increases reaction unit length, it is achieved titanium sponge reaction unit maximizes.Reaction unit tank body width of the present invention is 1.2～1.5 meters, and height is 1.5～2.5 times of width, 2～3 times of a length of width.Reaction unit base plate 1 is swash plate, is beneficial to the collection of magnesium chloride, discharge.Sieve plate 2 and reaction unit base plate 1 keep identical gradient, and opposite direction is assembled, to ensure sieve plate 2 upper surface level.During assembling, unsettled spot welding is fixed on bottom reaction unit.Reduction process takes parallel feeding raw materials from more than one places.Reduction process uses 4 thermometrics, measures reaction unit outside wall temperature；Distillation employing 3～4 thermometrics, measure heating furnace electric furnace heating wire temperature outside.
Claims (5)
1. one kind uses the technique that titanium sponge reduction distillation reaction unit produces titanium sponge, it is characterized in that: the reduction distillation reaction unit that this processing technology is used is connected by tank body and big lid formed by flange rubber cushion (4), bolt group (8), and tank body includes: base plate (1), sieve plate (2), row's magnesium chloride sleeve pipe (3), tank flange (11), kidney-shaped cylinder (12)；Big lid includes: row's magnesium chloride pipe (5), heat-insulation layer (6), inner heating device (7), cover flange (9), big lid lower flange (10), central tube (13), charging sleeve pipe one (14), short cylinder (15), charging sleeve pipe two (16) greatly；Whole reaction unit spatially kidney ellipsoid structure, described base plate (1) is one piece of swash plate, and oblique angle is 2～5 °, is positioned at the foot of whole device, cooperatively forms open three-dimensional kidney-shaped tank body with kidney-shaped cylinder (12)；Described sieve plate (2) is positioned at the top of base plate (1), is fixed on reaction unit kidney-shaped cylinder (12) inwall by spot welding mode is unsettled, and the distance between sieve plate (2) and base plate (1) is 20～30；Described row's magnesium chloride pipe (5) is L-shaped, is welded on and covers greatly, is inserted in row's magnesium chloride sleeve pipe (3) being welded on inside kidney-shaped cylinder (12) circular arc one end；Under great Gai, above tank body, it is provided with heat-insulation layer (6), for the still-process insulation to reaction unit；Described charging sleeve pipe one (14), charging sleeve pipe two (16) are respectively symmetrically the center of arc being arranged at big lid lower flange (10) two ends；Central tube (13) is arranged on the center of big lid, is positioned in the middle of charging sleeve pipe one (14), charging sleeve pipe two (16)；Inner heating device (7) is positioned at big lid lower flange (10) middle part, the periphery of central tube (13), is mainly used in still-process heating central tube (13)；Flange rubber cushion (4), in kidney ellipsoid structure, is positioned between big lid lower flange (10) and tank flange (11), big lid lower flange (10), tank flange (11) is tightened together by bolt group (8)；
Above-mentioned titanium sponge reduction distillation reaction unit is used to produce the concretely comprising the following steps of titanium sponge:
Last round of time is used as condenser, and at the reaction unit of the upper first-class blind plate of big lid central tube (13), or directly will assemble, and through taking out qualified empty reaction unit in advance, after hanging in heating furnace, use as reactor；Vacuumize two hours from row's magnesium chloride pipe (5), then argon filling, heating, after temperature reaches 700 DEG C, in the case of argon filling, pull down the blind plate on big lid central tube (13), at this, disposably add liquid magnesium；In reduction process, in charging sleeve pipe one (14), charging sleeve pipe two (16) and (13) three positions of central tube, charge pipe is installed, carries out 3 parallel chargings；In big lid central tube (13) position, charge pipe and bleeder pipe must be installed simultaneously, at the end of discharge magnesium chloride, pull up bleeder pipe plug with quick pressure releasing；With 4 thermometrics of reactor outer wall, as the foundation controlling charging rate；Start charging when reactor free surface correspondence position temperature reaches more than 750 DEG C, charging process maximum temperature must control between 750～870 DEG C；Ensure the equilibrium of three charge pipe charging rates；
After reduction process terminates, unload charge pipe, airtight with high temperature resistant packing ring and blind plate respectively on charging sleeve pipe one (14), charging sleeve pipe two (16), big lid central tube (13) loads onto magnesium plug or high-temperature valve；To assemble and take out in advance qualified a set of empty reaction unit, and as condenser, be bolted or weld and realize reactor and couple with condenser, in condenser end connection vacuum system, carry out vacuum distillation；With outside heating furnace electric furnace heating wire 3～4 thermometrics, the foundation controlled as vapo(u)rizing temperature；After distillation terminates, being separated with condenser by reactor in the case of pressure-fired, the reactor equipped with product hangs in cooling jacket cooling；Condenser hangs in heating furnace, and the reduction distillation entering next one produces.
Use the technique that titanium sponge reduction distillation reaction unit produces titanium sponge the most according to claim 1, it is characterized in that: described bolt group (8) is made up of 20～30 bolts, for big lid lower flange (10), tank flange (11) are fastened together.
Use the technique that titanium sponge reduction distillation reaction unit produces titanium sponge the most according to claim 1, it is characterised in that: described short cylinder (15) passes through welding manner, and by covering greatly flange (9), big lid lower flange (10) links together.
Use the technique that titanium sponge reduction distillation reaction unit produces titanium sponge the most according to claim 1, it is characterised in that: described reaction unit tank body width is 1.2～1.5 meters, and height is 1.5～2.5 times of width, 2～3 times of a length of width.
Use the technique that titanium sponge reduction distillation reaction unit produces titanium sponge the most according to claim 1, it is characterised in that: described sieve plate (2) and reaction unit base plate (1) keep identical gradient, and opposite direction is assembled, to ensure sieve plate (2) upper surface level.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN107619953A (en) * | 2017-09-14 | 2018-01-23 | 遵义钛业股份有限公司 | A kind of reduction distillation reaction unit in titanium sponge production |
| CN108396144A (en) * | 2018-05-29 | 2018-08-14 | 遵义钛业股份有限公司 | A kind of reduction apparatus during titanium sponge production |
| CN109084834B (en) * | 2018-07-05 | 2020-08-07 | 东北大学 | Liquid level and temperature measuring device suitable for titanium sponge reduction reaction |
| CN108754184A (en) * | 2018-08-29 | 2018-11-06 | 遵义钛业股份有限公司 | A kind of reduction and distillation furnace of magnesium processes production titanium sponge |
| CN110714130A (en) * | 2019-12-04 | 2020-01-21 | 遵义钛业股份有限公司 | Device and process for preventing vacuum channel from being blocked in titanium sponge production |
| CN110819826A (en) * | 2019-12-10 | 2020-02-21 | 遵宝钛业有限公司 | Device for removing impurities in magnesium in titanium sponge reduction production and production process thereof |
| CN111020229B (en) * | 2019-12-24 | 2022-03-29 | 新疆湘晟新材料科技有限公司 | Energy-saving durable efficient reduction distillation integrated electric furnace for producing titanium sponge |
| CN111893323A (en) * | 2020-09-08 | 2020-11-06 | 遵义钛业股份有限公司 | Cooling large cover used in titanium sponge production |
| CN112030010A (en) * | 2020-10-10 | 2020-12-04 | 遵宝钛业有限公司 | Device for adding solid magnesium in process of producing titanium sponge by magnesium reduction method |
| CN112359229A (en) * | 2020-11-09 | 2021-02-12 | 宝钛华神钛业有限公司 | Reduction reactor for reducing blockage of distillation channel and used for producing titanium sponge |
| CN115094248B (en) * | 2022-06-16 | 2023-11-10 | 洛阳双瑞万基钛业有限公司 | Titanium sponge production facility |
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| CN201245698Y (en) * | 2008-08-29 | 2009-05-27 | 宝钛华神钛业有限公司 | Titanium sponge reactor |
| CN101831562B (en) * | 2009-03-12 | 2012-04-04 | 四川恒为制钛科技有限公司 | Double-magnesium chloride pipe reactor for production of sponge titanium and production method of sponge titanium |
| CN203065556U (en) * | 2013-01-22 | 2013-07-17 | 罗时雨 | Titanium sponge slot type reaction device |
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