CN101831562A - Double-magnesium chloride pipe reactor for production of sponge titanium and production method of sponge titanium - Google Patents
Double-magnesium chloride pipe reactor for production of sponge titanium and production method of sponge titanium Download PDFInfo
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- CN101831562A CN101831562A CN200910300811A CN200910300811A CN101831562A CN 101831562 A CN101831562 A CN 101831562A CN 200910300811 A CN200910300811 A CN 200910300811A CN 200910300811 A CN200910300811 A CN 200910300811A CN 101831562 A CN101831562 A CN 101831562A
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Abstract
The invention relates to the field of production of nonferrous metallurgy sponge titanium, in particular to a double-magnesium chloride pipe reactor for production of the sponge titanium and a production method of the sponge titanium. The technical problem to be solved by the invention is to provide the double-magnesium chloride pipe reactor for production of the sponge titanium with integrated joint of reduction and distillation production. The invention further provides the production method of the sponge titanium with the integrated joint of reduction and distillation production. The double-magnesium chloride pipe reactor for production of the sponge titanium comprises a tank body (8) and a magnesium chloride main discharge pipeline (7), wherein a magnesium chloride auxiliary discharge pipeline (3) is further arranged on the tank body (8). The production method of the sponge titanium is as follows: discharging liquid magnesium chloride in the last time from the auxiliary discharge pipeline of the hot-end reactor during the magnesium reduction stage, and discharging other liquid magnesium chloride from the main discharge pipeline of the hot-end reactor. The reactor and the production method can shorten the single-furnace production cycle, improve the quality of the produced sponge titanium, greatly reduce the production cost and have broad application prospects.
Description
Technical field
The present invention relates to nonferrous metallurgy titanium sponge production field, be specifically related to the production method of a kind of double-magnesium chloride pipe reactor for production of sponge titanium and titanium sponge.
Background technology
The reaction equation of titanium sponge is: TiCl
4+ 2Mg=Ti+2MgCl
2, its production process mainly is divided into two stages, i.e. magnesium reduction stage (generate titanium and magnesium chloride) and distillation stage (removing impurity such as the magnesium that remains in the titanium sponge and magnesium chloride).
At present, the production of domestic titanium sponge is mainly two kinds of patterns: a kind of is to adopt the tandem device fabrication; Another kind is to adopt parallel device fabrication.Adopt the hot junction reactor of parallel device fabrication (promptly to go back the reactor of original production, the abbreviation hot junction) has only 1 magnesium chloride discharge tube at present, design attitude is placed fixing, also the magnesium chloride that produces during original production by the magnesium chloride discharge tube discharge, after the emptying, then hot junction reactor and cold end reactor (promptly are used to receive the reactor of reaction residual magnesium and magnesium chloride, the abbreviation cold junction) production is distilled in porthole flange butt joint, sealing at last.Its concrete production process comprises the steps:
1, the magnesium reduction stage: the magnesium of the manufacturing technique requirent amount of in the reactor of hot junction, packing in advance, be heated to certain temperature in process furnace, through repeatedly adding titanium tetrachloride and magnesium reacts, generate solid titanium and liquid magnesium chloride, the magnesium chloride of discharging need be sent into electrowinning process while hot and carry out magnesium eletrolysis production, (do not have the titanium sponge enterprise of electrolytic magnesium production process, magnesium chloride is sold as byproduct) obtains magnesium and chlorine; (magnesium is sent into also original production titanium sponge, and chlorine is sent into the chlorination production titanium tetrachloride)
2, the distillation stage (collect remaining magnesium and magnesium chlorides): before changing distillation over to and producing, the whole magnesium chlorides in the emptying reduction production process in latter stage change distillation over to by original production also then and produce, and have worked before changing distillation over to and producing:
(1) with a plurality of magnesium chlorides two-man ladle (container that is the splendid attire magnesium chloride), be contained in whole magnesium chlorides that latter stage, reduction reaction generated, because the magnesium chloride temperature of discharging is about 800 ℃, therefore, entering the magnesium chloride of two-maing ladle needs surface cool to condense, and just can slowly hang out from the condensation staving, in case spilling, magnesium chloride scalds operator, two-man ladle from the condensation staving, hang out after, the titanium sponge enterprise of electrolytic magnesium production process is arranged, then immediately magnesium chloride is sent to magnesium eletrolysis; The titanium sponge enterprise of no electrolytic magnesium production process, then will two-man ladle is placed into secure location and continues cooling, and change to sky then and two-man ladle and continue the discharging magnesium chloride, through 3～4 repeatable operation, the whole emptyings of magnesium chloride in reactor;
(2) after the interior whole emptyings of magnesium chloride of reactor, in time cool off magnesium chloride pipe, first-class blind flange is to prevent titanium products air inlet oxidation;
(3) hang out that the intravital magnesium chloride of condensation drum is two-mand ladle and the magnesium chloride support of two-maing ladle;
(4) cold end reactor is hung in the condensation staving, and dock with hot junction channel of reactor mouth flange the cold end reactor porthole;
(5) the timely good hot junction of welded seal, cold junction porthole flange, and it is qualified to hunt leak;
(6) hot junction, cold junction pathway heater are installed, pathway heater each point temperature thermocouple is installed;
(7) connect vacuum system, check vacuum system and vacuum machine equipment, the vacuum system leak detection is qualified;
(8) process furnace carry out airtight and hunt leak qualified;
(9) process furnace, pathway heater feeding temperature-raising;
(10) every preparation work has met the requirement of distilling producing process technical qualification, starts vacuum mechanical pump, enters distillation and produces.
Above-mentionedly change the method that distillation produces over to by reduction and have following shortcoming at present:
1, lose time, produce and adopt single magnesium chloride pipe reactor, change the time that distillation is produced over to by reduction, under the normal circumstances, need 10～14 hours, single stove production cycle prolongs.
2, waste energy, because it is many to be reduced to distillation production process middle-chain, the length that wastes time must have a power failure and carry out operation, therefore causes furnace temperature to reduce.
3, at present because hot junction (product is arranged) high-temperature valve quality does not pass a test, situation about being not closed completely through regular meeting in welding hot junction, cold junction porthole flange process, needs to replenish a large amount of argon gas and protects product, to avoid by porthole flange air inlet oxygenated products.
4, gas leak phenomenon takes place in high-temperature valve easily; the magnesium chloride of the condition of high temperature is under the situation of emptying; titanium sponge exposes; product is easily by air nitrogenize, oxidation etc. during this time; even adopting a large amount of argon gas protects; owing to also contain foreign gases such as micro-oxygen and nitrogen in the argon gas, quality product is reduced.
5, at present, adopt the method for parallel device fabrication titanium sponge, in certain sense, also do not realize reduction, the associating of distillation production integration, that is: after also original production finished, the assembling of carrying out distillation plant again was with the production that continues, and this reality still rests on half combination producing state.
Summary of the invention
First technical problem to be solved by this invention provides a kind of double-magnesium chloride pipe reactor for production of sponge titanium that makes reduction, the associating of distillation production integration.
Double-magnesium chloride pipe reactor for production of sponge titanium of the present invention comprises tank body and magnesium chloride master discharge tube, wherein, also is provided with the secondary discharge tube of magnesium chloride on the tank body.
Adopt double-magnesium chloride pipe reactor of the present invention can add titanium tetrachloride several times and carry out reduction reaction, add titanium tetrachloride for the last time and carry out reduction reaction and be called also original production in latter stage.In the reduction production phase in early stage, the liquid magnesium chloride of generation is discharged by magnesium chloride master discharge tube earlier; Latter stage, also the liquid magnesium chloride of original production changed by the secondary discharge tube discharge of magnesium chloride.Reduce production period in latter stage, can be with as the double-magnesium chloride pipe reactor in hot junction and good as the porthole welded seal of the double-magnesium chloride pipe reactor of cold junction, and carry out preparation work before other distillation is produced.Because the hot junction reactor is malleation production at reduction phase, and magnesium chloride liquid protection titanium sponge product is arranged, just reduced, can also reduce the usage quantity of protecting simultaneously with the gas argon gas because of of the influence of problems such as equipment to quality product; And because distillation was produced between the standby period, keep the hot junction reactor also continuing ordinary production, thereby avoided having reduced power consumption, significantly reduced production cost because the furnace temperature that the power failure operation causes reduces.
Design according to the parallel device fabrication of present domestic use factory, the secondary discharge tube of magnesium chloride the position is set, get final product with the preparation work of guaranteeing safety, do not influence before distilling, (as: the porthole welded seal of hot junction and cold end reactor, the pathway heater of hot junction reactor and cold end reactor is installed, passage each point temperature thermocouple is installed, is connected vacuum system etc.).
Second technical problem to be solved by this invention provides the production method of the titanium sponge of a kind of reduction, the integrated associating of distillation production realization.
The production method of titanium sponge of the present invention, adopt parallel device fabrication, comprise magnesium reduction stage and distillation stage, it adopts above-mentioned double-magnesium chloride pipe reactor for production of sponge titanium to produce, in the magnesium reduction stage, last liquid magnesium chloride discharging is discharged by the secondary discharge tube of magnesium chloride, and remaining liquid magnesium chloride discharging is discharged by magnesium chloride master discharge tube.
Further, the production method of titanium sponge of the present invention, its production process comprises the steps:
A, be the hot junction reactor with the double-magnesium chloride pipe reactor, in the reactor of hot junction, add magnesium, heating (being generally 700～850 ℃), add titanium tetrachloride several times and carry out reduction reaction, obtain solid titanium and liquid magnesium chloride, the liquid magnesium chloride is discharged by the main discharge tube of hot junction reactor, seals this pipeline then;
B, in the reactor of hot junction, continue to add titanium tetrachloride and carry out also original production in latter stage; Reduce production period latter stage, the porthole welded seal of hot junction reactor and cold end reactor is good, and carry out other distillation and produce preceding preparation work (as: pathway heater of hot junction reactor and cold end reactor is installed, passage each point temperature thermocouple is installed, connect vacuum system etc.);
C, latter stage with the liquid magnesium chloride that produces secondary this pipeline of discharge tube emptying rear enclosed by the hot junction reactor, enter distillation then and produce after also original production finishes.
The number of times that adds titanium tetrachloride in the above-mentioned a step can be determined according to producing titanium sponge process requirements amount, and to determine that titanium tetrachloride adds the method for indegree identical with routine.
Above-mentioned b step continues to add titanium tetrachloride and carries out also original production in latter stage in the reactor of hot junction, the add-on of its titanium tetrachloride, guaranteeing that reducing the porthole of production period hot junction reactor and cold end reactor in latter stage connects, and carry out the preparation work before other distillation is produced.
When above-mentioned b step is connected in the porthole with reactor and condenser; because the hot junction reactor is malleation production, and magnesium chloride liquid protection titanium sponge product is arranged, just reduced because of of the influence of problems such as equipment to quality product; simultaneously can also reduce the argon shield consumption, reduce production cost.
Wherein, the heating that heats up before distilling the production prerequisite of the pathway heater of distillation production hot junction reactor and cold end reactor to ensure that the air-flow of magnesium and magnesium chloride is unimpeded in distilling production process, is avoided obstruction, is implemented in the purpose of cold end reactor condensation.
Further, cold end reactor and hot junction reactor adopt same type equipment, the hot junction reactor that cold end reactor was produced as next time, and the cold end reactor that the hot junction reactor was produced as next time, cycle alternation uses.
Beneficial effect of the present invention is:
1, the present invention is first when adopting parallel stove to produce titanium sponge, take method with major and minor magnesium chloride pipe discharging magnesium chloride, solved by the technical barrier that reverts to distillation production direct transformation, really embody the purpose that reverts to the associating of distillation production integration, realized the practical significance of parallel equipment produce titanium sponge by combination method.
2, shortened single stove production cycle, average every stove production cycle saves time more than 12 hours.
3, eliminated product under hot state, in dismounting cool and heat ends passage flange process, to the infringement that quality product caused.
4, operator are all linked with one another in operation process, shortened long drawback of employee's activity duration.
5, owing to from reverting to the time shortening that distillation is produced, can keep hot junction reactor furnace temperature substantially, reduced power consumption, need not add a large amount of argon shield products, the consumption of having saved argon gas has significantly reduced production cost.
Description of drawings
Fig. 1 is the structural representation of double-magnesium chloride pipe reactor of the present invention, and double-magnesium chloride pipe reactor is in the reduction production phase among the figure;
Fig. 2 is the vertical view of the double-magnesium chloride pipe reactor of the present invention of Fig. 1;
Fig. 3 is the structural representation of double-magnesium chloride pipe reactor of the present invention, and reactor is in the distillation production phase among the figure, and used condenser (being cold end reactor) is the equipment of same type with the hot junction reactor;
Fig. 4 is the vertical view of Fig. 3.
1 is hot junction channel of reactor mouth among the figure, and 2 is sieve plate, and 3 is the secondary discharge tube of magnesium chloride, 4 is process furnace, and 5 is the high-temperature valve valve seat, and 6 is high-temperature valve, 7 is magnesium chloride master discharge tube, and 8 is tank body, and 9 for two-maing ladle, 10 are the support of two-maing ladle, and 11 is main magnesium chloride pipe, and 12 is secondary magnesium chloride pipe, 13 is condensation drum, and 14 is the process furnace silk, and 15 is charging opening, 16 is the porthole flange, and 17 is the porthole well heater, and 18 is vacuum pump interface (connection vacuum system).
Embodiment
Below in conjunction with embodiment the specific embodiment of the present invention is further described, does not therefore limit the present invention among the described scope of embodiments.
The structure of double-magnesium chloride pipe reactor of the present invention as shown in Figure 1, 2, double-magnesium chloride pipe reactor of the present invention, comprise tank body 8, tank body 8 tops are provided with charging opening 15, high-temperature valve valve seat 5 and high-temperature valve 6, channel of reactor mouth 1 links to each other with tank body 1 by high-temperature valve 6, tank body 8 links to each other with the end of magnesium chloride master discharge tube 7 with the secondary discharge tube 3 of magnesium chloride respectively, and the other end of magnesium chloride master discharge tube 7 connects main magnesium chloride pipe 11, the other end auxiliary connection magnesium chloride pipe 12 of the secondary discharge tube 3 of magnesium chloride.
The employing furnace output is that the double-magnesium chloride pipe hot junction reactor of 6 tons of titanium sponges is gone back original production, and process furnace is done the vacuum seal leak test under the reactor cold state after the hot junction reactor is gone into stove, and stand the test is gone back original production.The 9000kg magnesium of in the reactor of double-magnesium chloride pipe hot junction, packing in advance, be heated to 700～850 ℃ in process furnace, through adding titanium tetrachloride 15～24 times and magnesium reacts, each titanium tetrachloride 1000～1600kg that adds, obtain solid titanium and liquid magnesium chloride, the liquid magnesium chloride is discharged by the main discharge tube of reactor, near the magnesium chloride of two-maing ladle of liquid magnesium chloride putting into will be housed then to be transported passage and transports, carry out electrolysis while hot, when entering also original production latter stage, before the last magnesium chloride of emptying, seal this pipeline immediately.
Add titanium tetrachloride 1000～1400kg at last and carry out also original production in latter stage, the liquid magnesium chloride that is produced is via the secondary discharge tube emptying of hot junction reactor, and emptying finishes and seals secondary discharge tube immediately; Utilize this preceding section of magnesium chloride emptying to reduce the production time in latter stage; in advance the magnesium chloride in the condensation drum is two-mand ladle; the support of two-maing ladle hangs out; and hang in cold end reactor (with the hot junction reactor be same kind equipment); having magnesium chloride in the reactor of hot junction can protect under the situation of product; took the road junction flange packing apart; butt joint; the good heat of welded seal; cold end reactor is crossed the road junction flange; install heat; cold end reactor is crossed channel heater; temperature thermocouple; connect vacuum system; carry out vacuum leak hunting; sealed heating furnace, every end-of-job is with warm; cold end reactor is crossed the channel heater feeding temperature-raising, controls the each point temperature of process furnace well.
Distill production sequence immediately routinely and change distillation production over to.
Magnesium and titanium tetrachloride with identical weight are produced by existing method (being the method in the background technology), with the inventive method contrast, produce 6 tons of titanium sponges with single stove and the results are shown in Table 1.
Table 1 the inventive method and existing method are produced result's contrast of titanium sponge
As can be seen from Table 1, major impurity content such as the iron in the titanium sponge that employing the inventive method is produced, oxygen all decrease than existing methods, because main foreign matter content reduces, realized the reduction of overall target Brinell hardness, improved the titanium sponge quality product, and shortened the production time, and saved costs such as argon gas, power consumption, have broad application prospects.
Claims (5)
1. double-magnesium chloride pipe reactor for production of sponge titanium comprises tank body (8) and magnesium chloride master discharge tube (7), it is characterized in that: also be provided with the secondary discharge tube (3) of magnesium chloride on the tank body (8).
2. the production method of titanium sponge, adopt parallel device fabrication, comprise magnesium reduction stage and distillation stage, it is characterized in that: adopt the described double-magnesium chloride pipe reactor for production of sponge titanium of claim 1 to produce, in the magnesium reduction stage, last liquid magnesium chloride discharging is discharged by the secondary discharge tube of magnesium chloride, and remaining liquid magnesium chloride discharging is discharged by magnesium chloride master discharge tube.
3. the production method of titanium sponge according to claim 2, it is characterized in that: production process comprises the steps:
A, be the hot junction reactor, in the reactor of hot junction, add magnesium, heating with the double-magnesium chloride pipe reactor, add titanium tetrachloride several times and carry out reduction reaction, obtain solid titanium and liquid magnesium chloride, the liquid magnesium chloride is discharged by the main discharge tube of hot junction reactor, seals this pipeline then;
B, in the reactor of hot junction, continue to add titanium tetrachloride and carry out also original production in latter stage; Reduce production period latter stage, the porthole welded seal of hot junction reactor and cold end reactor is good, and carry out preparation work before other distillation is produced;
C, latter stage with the liquid magnesium chloride that produces secondary this pipeline of discharge tube emptying rear enclosed by the hot junction reactor, enter distillation then and produce after also original production finishes.
4. double-magnesium chloride pipe reactor according to claim 3 is produced the method for titanium sponge, it is characterized in that: the heating that heats up before distilling the production prerequisite of the pathway heater of hot junction reactor and cold end reactor.
5. double-magnesium chloride pipe reactor according to claim 3 is produced the method for titanium sponge, it is characterized in that: cold end reactor and hot junction reactor are same type equipment, the hot junction reactor that cold end reactor was produced as next time, the cold end reactor that the hot junction reactor was produced as next time, cycle alternation uses.
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| CN2009103008112A CN101831562B (en) | 2009-03-12 | 2009-03-12 | Double-magnesium chloride tube reactor for producing titanium sponge and production method of titanium sponge |
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| CN2009103008112A CN101831562B (en) | 2009-03-12 | 2009-03-12 | Double-magnesium chloride tube reactor for producing titanium sponge and production method of titanium sponge |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2618087A1 (en) * | 2012-01-18 | 2013-07-24 | Shenzhen Sunxing Light Alloys Materials Co., Ltd | Distillation equipment for producing sponge titanium |
| CN103343227A (en) * | 2013-07-29 | 2013-10-09 | 中航天赫（唐山）钛业有限公司 | Method and equipment for purifying molten magnesium during production of sponge titanium |
| CN104004987A (en) * | 2014-06-18 | 2014-08-27 | 四川恒为制钛科技有限公司 | Titanizing method of reactor for sponge titanium production |
| CN104152722A (en) * | 2014-08-13 | 2014-11-19 | 四川恒为制钛科技有限公司 | Titanium sponge double-magnesium chloride tube reactor and production method of titanium sponge |
| CN104357659A (en) * | 2014-12-09 | 2015-02-18 | 遵义钛业股份有限公司 | Vacuum ladle for adding magnesium for reduction in production of titanium sponge and discharging magnesium chloride by distillation |
| CN104831088A (en) * | 2015-05-21 | 2015-08-12 | 罗时雨 | Sponge titanium reduction distillation reactor and production technique thereof |
| CN106048258A (en) * | 2016-08-18 | 2016-10-26 | 中航天赫（唐山）钛业有限公司 | Method and device for generating magnesium chloride in titanium sponge production process through vacuum discharging manner |
| CN106916969A (en) * | 2017-01-18 | 2017-07-04 | 贵州大学 | A kind of production method 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 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1179144A (en) * | 1981-04-04 | 1984-12-11 | Hiroshi Ishizuka | Method and an apparatus for producing titanium metal from titanium tetrachloride |
| CN201151738Y (en) * | 2007-12-17 | 2008-11-19 | 贵阳铝镁设计研究院 | Reducing distillation reactor |
-
2009
- 2009-03-12 CN CN2009103008112A patent/CN101831562B/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2618087A1 (en) * | 2012-01-18 | 2013-07-24 | Shenzhen Sunxing Light Alloys Materials Co., Ltd | Distillation equipment for producing sponge titanium |
| CN103343227A (en) * | 2013-07-29 | 2013-10-09 | 中航天赫（唐山）钛业有限公司 | Method and equipment for purifying molten magnesium during production of sponge titanium |
| CN104004987A (en) * | 2014-06-18 | 2014-08-27 | 四川恒为制钛科技有限公司 | Titanizing method of reactor for sponge titanium production |
| CN104152722A (en) * | 2014-08-13 | 2014-11-19 | 四川恒为制钛科技有限公司 | Titanium sponge double-magnesium chloride tube reactor and production method of titanium sponge |
| CN104357659A (en) * | 2014-12-09 | 2015-02-18 | 遵义钛业股份有限公司 | Vacuum ladle for adding magnesium for reduction in production of titanium sponge and discharging magnesium chloride by distillation |
| CN104831088A (en) * | 2015-05-21 | 2015-08-12 | 罗时雨 | Sponge titanium reduction distillation reactor and production technique thereof |
| CN106048258A (en) * | 2016-08-18 | 2016-10-26 | 中航天赫（唐山）钛业有限公司 | Method and device for generating magnesium chloride in titanium sponge production process through vacuum discharging manner |
| CN106048258B (en) * | 2016-08-18 | 2018-04-10 | 中航天赫（唐山）钛业有限公司 | The method and device of magnesium chloride is produced during vacuum mode discharge titanium sponge production |
| CN106916969A (en) * | 2017-01-18 | 2017-07-04 | 贵州大学 | A kind of production method 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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