CN104004987B - The titanizing method of titanium sponge production reactor - Google Patents
The titanizing method of titanium sponge production reactor Download PDFInfo
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- CN104004987B CN104004987B CN201410272519.5A CN201410272519A CN104004987B CN 104004987 B CN104004987 B CN 104004987B CN 201410272519 A CN201410272519 A CN 201410272519A CN 104004987 B CN104004987 B CN 104004987B
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Abstract
The invention belongs to non-ferrous metal chemical industry field of smelting, it is specifically related to the titanizing method of a kind of titanium sponge production reactor. Technical problem to be solved by this invention is to provide the titanizing method of the titanium sponge production reactor of a kind of shorter, better effects if consuming time. The titanium sponge production of the present invention titanizing method of reactor first, comprises the steps: a, new reactor hot acid leaching 1-3 days, then washing and drying; B, smear useless titanium at inner wall of new reactor by inner wall surface area 30��80g/; C, in new reactor, add appropriate titanium tetrachloride and magnesium, it is warming up to 800��950 DEG C and oozes titanium; Wherein, the add-on of magnesium and titanium tetrachloride is so that titanium layer is oozed in the titanium and the formation of new reaction wall that generate. Titanizing method of the present invention to ooze titanium effect better, in the titanium sponge that the reactor after oozing titanium is produced, impurity obtains much slower; Avoid high temperature to ooze titanium new reactor is formed infringement, it is to increase ooze work-ing life of the reactor after titanium.
Description
Technical field
The invention belongs to non-ferrous metal chemical industry field of smelting, it is specifically related to the titanizing method of a kind of titanium sponge production reactor.
Background technology
Titanium sponge production main technique is at magnesium reduction-vacuum distillation method, and its ultimate principle is under the protection of argon gas, adds titanium tetrachloride and make it and reactive magnesium in reactor, generates titanium sponge and magnesium chloride, and its reaction process is comparatively complicated. Due to raw material and the product steel beam column that directly contact reactor is relevant with other in process of production, as: sieve plate, magnesium chloride pipe etc., iron contamination etc. may dissolve in raw material magnesium liquid or directly enter in finished product titanium sponge with alloy form, thus affect quality product.
Technical scheme disclosed in patent of invention CN201310039782.5: in container, put into MAGNESIUM METAL, particulate state titanium sponge and need to carry out surface treatment after 140-310 DEG C of degassed process, heat and lead to and be warming up to 990��1010 DEG C of constant temperature 9��11 hours into titanium tetrachloride. This technical scheme can effectively be formed oozes titanium layer, but the pre-treatment oozing titanium and the processing parameter that oozes titanium are not furtherd investigate by contriver at that time, and heat, reduces the work-ing life of new reactor; And leaching time is longer.
Summary of the invention
Technical problem to be solved by this invention is to provide the titanizing method of the titanium sponge production reactor of a kind of shorter, better effects if consuming time.
The titanizing method of titanium sponge production reactor disclosed in this invention comprises the steps:
A, new reactor hot acid soaks 1-3 days, then washing and drying;
B, smear useless titanium at inner wall of new reactor by inner wall surface area 30��80g/;
C, in new reactor, add appropriate titanium tetrachloride and magnesium, it is warming up to 800��950 DEG C and oozes titanium;Wherein, the add-on of magnesium and titanium tetrachloride is so that titanium layer is oozed in the titanium and the formation of new reaction wall that generate. Generally, maximum output be 12t reactor in magnesium add-on be 300��900kg, titanium tetrachloride add-on is 1200��3500kg.
The titanium particulate that in above-mentioned step c, magnesium steam and titanium tetrachloride vapors generate in reactor wall generation gas-phase reaction adheres to reactor wall; Meanwhile, the useless titanium smeared also can generate alloy with iron reaction, and strong reactor wall completes to ooze titanium.
Wherein, the magnesium that b step is used can be liquid magnesium, solid magnesium or distillation magnesium.
Wherein, the temperature of hot acid described in step a is 40 DEG C��60 DEG C. Contriver tests discovery, and acidleach rust cleaning can improve acid leaching efficiency while preventing reactor by acid corrosion at this temperature, shortens leaching time. Concrete, after titanium sponge production, the mixture of magnesium and magnesium chloride distills in a gaseous form, within the condenser condensation, and this product is distillation magnesium, for cost-saving, hot acid described in step a is obtained by the heat release heating acid solution in distillation magnesium condensation temperature-fall period by after reactor.
Preferably, the applying amount 40-60g/ of the useless titanium of step b in technique scheme.
Preferably, in technique scheme, described in step b, the granularity of useless titanium is 0.8mm��2mm.
Described useless titanium is the defective titanium sponge eliminated in production process.
Preferably, in order to reduce energy consumption, make full use of the resultant product after titanium sponge production, using needing the new reactor oozing titanium to collect distillation magnesium as condenser during titanium sponge production, then can add titanium tetrachloride and carry out reduction reaction and directly ooze titanium.
Wherein, the useless titanium of smearing described in step b can be smeared by the mode that titanium is oozed conventional in this area, smears as added water.
Useful effect:
1, titanizing method of the present invention to ooze titanium effect better, in the titanium sponge that the reactor after oozing titanium is produced, impurity obtains much slower;
2, titanizing method temperature of the present invention is low, avoids high temperature and oozes titanium new reactor is formed infringement, it is to increase oozes the work-ing life of the reactor after titanium;
4, titanizing method of the present invention improves the temperature of acidleach, can shorten leaching time, it is to increase acid leaching efficiency.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described scope of embodiments.
The titanizing method of titanium sponge production reactor disclosed in this invention comprises the steps:
A, new reactor hot acid soaks 1-3 days, then washing and drying;
B, smear useless titanium at inner wall of new reactor by inner wall surface area 30��80g/;
C, in new reactor, add appropriate titanium tetrachloride and magnesium, it is warming up to 800��950 DEG C and oozes titanium; Wherein, the add-on of magnesium and titanium tetrachloride is so that titanium layer is oozed in the titanium and the formation of new reaction wall that generate. Generally, maximum output be 12t reactor in magnesium add-on be 300��900kg, titanium tetrachloride add-on is 1200��3500kg.
The titanium particulate that in above-mentioned step c, magnesium steam and titanium tetrachloride vapors generate in reactor wall generation gas-phase reaction adheres to reactor wall; Meanwhile, the useless titanium smeared also can generate alloy with iron reaction, and strong reactor wall completes to ooze titanium.
Wherein, the magnesium that b step is used can be liquid magnesium, solid magnesium or distillation magnesium.
Wherein, the temperature of hot acid described in step a is 40 DEG C��60 DEG C. Contriver tests discovery, and acidleach rust cleaning can improve acid leaching efficiency while preventing reactor by acid corrosion at this temperature, shortens leaching time. Concrete, after titanium sponge production, the mixture of magnesium and magnesium chloride distills in a gaseous form, within the condenser condensation, and this product is distillation magnesium, for cost-saving, hot acid described in step a is obtained by the heat release heating acid solution in distillation magnesium condensation temperature-fall period by after reactor.
Preferably, the applying amount 40-60g/ of the useless titanium of step b in technique scheme.
Preferably, in technique scheme, described in step b, the granularity of useless titanium is 0.8mm��2mm.
Described useless titanium is the defective titanium sponge eliminated in production process.
Preferably, in order to reduce energy consumption, make full use of the resultant product after titanium sponge production, using needing the new reactor oozing titanium to collect distillation magnesium as condenser during titanium sponge production, then can add titanium tetrachloride and carry out reduction reaction and directly ooze titanium.
Wherein, the useless titanium of smearing described in step b can be smeared by the mode that titanium is oozed conventional in this area, smears as added water.
The present invention is also illustrated further by following instance, but therefore protection scope of the present invention is not limited in one embodiment.
Embodiment 1
It it is titanium sponge production reactor washing and drying after 60 DEG C of acidleach rust cleaning in 3 days of 12t by maximum output, the useless titanium 50g of 0.8mm��2mm is smeared by inwall every square metre, magnesium ingot 700kg is placed in reactor, and control temperature is 800��950 DEG C, add 2900kg titanium tetrachloride again, carry out oozing titanium reaction. Ooze after titanium terminates and namely obtain the reactor oozing titanium and completing. The reactor completing to ooze titanium reaction can carry out titanium sponge production.
Embodiment 2
It it is titanium sponge production reactor washing and drying after 60 DEG C of acidleach rust cleaning in 3 days of 12t by maximum output, new reactor is distilled after titanium sponge production the condenser of magnesium, the useless titanium 80g of 0.8mm��2mm is smeared by inwall every square metre, magnesium ingot 500kg is placed in reactor, and control temperature is 800��950 DEG C, add 2000��3000kg titanium tetrachloride again, carry out oozing titanium reaction. Ooze after titanium terminates and namely obtain the reactor oozing titanium and completing. The reactor completing to ooze titanium reaction can carry out titanium sponge production.
The production that the reactor of embodiment 1, embodiment 2 is used as titanium sponge, to be produced stable after, get the product that wherein 10 stoves are produced respectively. By analysis, in the reactor after oozing titanium according to embodiment 1 method, in the product of gained, iron level is all less than 0.03%, and wherein 7 stoves are 0.01%. In reactor after oozing titanium according to embodiment 2 method, in 10 stove products of gained, iron level is all less than 0.03%, and wherein 6 stoves are 0.01%, separately has 2 stoves to be less than 0.01%. This shows, ooze titanium required time by the inventive method shorter, ooze titanium effect better.
Claims (5)
1. the titanizing method of titanium sponge production reactor, it is characterised in that: comprise the following steps:
A, new reactor hot acid soaks 1-3 days, then washing and drying;
B, smear useless titanium at inner wall of new reactor by inner wall surface area 30��80g/;
C, in new reactor, add appropriate titanium tetrachloride and magnesium, it is warming up to 950 DEG C and oozes titanium;
Wherein, the add-on of magnesium and titanium tetrachloride is so that titanium layer is oozed in the titanium and the formation of new reaction wall that generate; The temperature of hot acid described in step a is 40 DEG C��60 DEG C; By distilling after titanium sponge production, magnesium condensation heating obtains hot acid described in step a.
2. the titanizing method of titanium sponge production reactor according to claim 1, it is characterised in that: the applying amount 40��60g/ of useless titanium in step b.
3. the titanizing method of titanium sponge production reactor according to claim 1, it is characterised in that: described in step b, the granularity of useless titanium is 0.8mm��2mm.
4. the titanizing method of titanium sponge production reactor according to claim 1, it is characterised in that: the magnesium described in step c is liquid magnesium, solid magnesium.
5. the titanizing method of titanium sponge production reactor according to claim 1, it is characterised in that: the magnesium described in step c is the distillation magnesium produced after titanium sponge production.
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| CN105970152B (en) * | 2016-07-08 | 2018-06-01 | 朝阳金达钛业股份有限公司 | The method for ooze titanium to production titanium sponge new reactor |
| CN106834747A (en) * | 2017-01-18 | 2017-06-13 | 贵州大学 | A kind of method for preparing 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 |
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| CN1283829C (en) * | 2005-06-17 | 2006-11-08 | 遵义钛业股份有限公司 | Method of producing sponge titanium by using titanium hydride powder titanizing in new reactor |
| CN101476102B (en) * | 2009-01-23 | 2012-05-30 | 四川恒为制钛科技有限公司 | Titanium leaking method for reactor for titanium sponge production |
| 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 |
| CN202272940U (en) * | 2011-08-31 | 2012-06-13 | 洛阳双瑞万基钛业有限公司 | Gasification feeding device for preparing titanium sponge |
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