CN107435106A - The big lid of reactor and the processing method of vacuum flask adhesion in a kind of titanium sponge production - Google Patents
The big lid of reactor and the processing method of vacuum flask adhesion in a kind of titanium sponge production Download PDFInfo
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- CN107435106A CN107435106A CN201710707820.8A CN201710707820A CN107435106A CN 107435106 A CN107435106 A CN 107435106A CN 201710707820 A CN201710707820 A CN 201710707820A CN 107435106 A CN107435106 A CN 107435106A
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- reactor
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- vacuum flask
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1268—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
- C22B34/1272—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1295—Refining, melting, remelting, working up of titanium
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- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a kind of big lid of reactor in titanium sponge production and the processing method of vacuum flask adhesion, the upper and lower of the big lid of the reactor of adhesion and vacuum flask, which is respectively mounted, needs the new reactor for oozing titanium, it is assembled into new distilling apparatus, hunt leak it is qualified after, it is evaporated in vacuo, reactor is covered greatly with the magnesium on vacuum flask, magnesium chloride with the change of temperature and vacuum, is evaporated on the inner surface of upper and lower new reactor, so as to the separation realized vacuum flask and covered greatly.This method can separate the big lid of reactor with vacuum flask in a short time, while and can makes full use of the magnesium and magnesium chloride that reactor covers greatly.
Description
Technical field
The present invention relates to technical field of production of sponge titanium, and in particular to the big lid of reactor and insulation in a kind of titanium sponge production
The processing method of bottle adhesion.
Background technology
During magnesium processes produce titanium sponge, after the reduction reaction of magnesium metal and titanium tetrachloride terminates, steamed in reduction
Evaporate and partial oxidation magnesium and metal magnesium addition are also remained in the titanium sponge in reactor.In order to this partial impurities from titanium sponge
Separate and purify titanium sponge, the reduction distillation reactor for filling titanium sponge is docked with condensation reactor, is being evaporated in vacuo
Under state, the impurity such as magnesium chloride and magnesium metal are sent into condensation reactor by the big lid of carrying pipe in condensation reactor and carried out
Condensation-crystallization, on the one hand obtain the magnesium chloride and magnesium metal of pure titanium sponge, on the other hand recyclable condensation-crystallization.Domestic institute
There is an I Xing Lu titanium sponge productions enterprise, scene can all find the big lid of reactor of adhesion, and especially season in summer in winter two is relatively more.Magnesium processes
Titanium sponge production, due to reasons such as water temperature control, temperature, vacuums, causes a large amount of magnesium to be gathered in instead in vacuum distillation process
Device is answered to cover greatly, the big lid of reactor and vacuum flask can not separate by magnesium firmly adhesion, during dismounting covering greatly with vacuum flask.Reactor
Big lid and vacuum flask are scrapped in advance, have had a strong impact on the normal production of also-steaming, standby redundancy consumption increase, titanium sponge production cost
Improve.
The content of the invention
It is an object of the invention to provide reactor in a kind of titanium sponge production it is big lid and vacuum flask adhesion processing method,
This method can separate the big lid of reactor with vacuum flask in a short time, while and can makes full use of the magnesium that reactor covers greatly
And magnesium chloride.
To achieve the above object, the present invention adopts the following technical scheme that：
The big lid of reactor and the processing method of vacuum flask adhesion, the processing method are in a kind of titanium sponge production：Will be viscous
The upper and lower of the big lid of reactor even and vacuum flask, which is respectively mounted, needs the new reactor for oozing titanium, is assembled into new distilling apparatus, examines
Leak it is qualified after, be evaporated in vacuo, reactor is covered greatly with the magnesium on vacuum flask, magnesium chloride with the change of temperature and vacuum
Change, be evaporated on the inner surface of upper and lower new reactor, so as to the separation realized vacuum flask and covered greatly.Make full use of magnesium and chlorination
Magnesium is under different vacuums, and more most than normal pressure times of evaporation rate so can be to realize quick volatilization at a lower temperature, its
It is real be exactly using magnesium and magnesium chloride in certain condition of negative pressure, the principle progress of can steam raising at a lower temperature.
Preferably, the distilling apparatus assembled will carry out forvacuum, and forvacuum degree requires that resistance vacuum gauge pressure reaches
To 120pa, mistake vacuum test is then done, distortion reciprocal of duty cycle reaches 9.33pa/10 minutes to be qualified.
Specifically, described distill is carried out in also-steaming joint stove, and also-steaming joint stove is 4 temperature controls, and temperature controlling point is arranged
It is respectively 1#, 2#, 3#, 4# point from top to bottom.
The distillation is to carry out stage by stage, specific as follows：First stage：The temperature of 1#, 2#, 3#, 4# point is 200 DEG C,
Constant temperature 2 hours, is vacuumized with water ring pump；Second stage：The temperature of 1#, 2#, 3#, 4# point is 400 DEG C, constant temperature 2 hours, uses water
Ring pumping vacuum；Phase III：1# points temperature is 950 DEG C, and 2#, 3#, 4# point temperature are 850 DEG C, constant temperature 1 hour, with low true
Empty pumping vacuum；Fourth stage：1# points temperature is 950 DEG C, and 2#, 3#, 4# point are 900 DEG C, constant temperature 3 hours, use high-vacuum pump
Vacuumize.
Preferably, whole vacuum distillation process keeps double vacuum states, i.e., all keeps vacuum in distilling apparatus and electric furnace.
Further, the furnace shell of electric furnace remains that negative pressure is not less than 0.075Mpa in vacuum distillation process.
Further, after vacuum distillation terminates, after water receiving cools down 4 hours to distilling apparatus between first using, then with direct water
Cooling 6 hours is carried out to distilling apparatus.
Also, whole course of reaction water temperature need not control, and reaction is simple, is easy to grasp.
Handled adhesion reactor it is big lid and vacuum flask after, it is necessary to the new reactor of titanium be oozed, after being used herein
It can disassemble, apply it to during titanium sponge production and go, in the production process of titanium sponge, new reactor needs to ooze
Titanium, titanium mainly exist in the form of titanium tetrachloride, so need addition magnesium to enter line replacement to it, and specific reaction is as follows：
2Mg+TiCl4=Ti+2MgCl2；
And in practical application, because the surface of new reactor has adhered to a part of Mg, so oozed in new reactor
During titanium, reduce Mg dosage, saved cost.Therefore, this method can not only solve reactor great Gai and guarantor
The problem of warm bottle adhesion, moreover it is possible to the magnesium adsorbed on new reactor is made full use of, serves unexpected technique effect.
The inventive method has the following advantages that：
1st, present application addresses due to the big lid of magnesium adhesion device and vacuum flask separation problem can not be dismantled, at the same it is indirectly right
New reactor has carried out once oozing magnesium and magnesium chloride, solves the problems, such as to have a strong impact on production due to the big lid adhesion of reactor.
2nd, because the big lid of reactor and vacuum flask are in time, it ensure that production normal operation.
3rd, the big lid of reactor and vacuum flask service life are improved, reduces big lid and vacuum flask loss, can be enterprise every year
Industry saves nearly 500,000 yuan of fund.
Brief description of the drawings
Fig. 1 is that reactor of the present invention big lid, vacuum flask and new reactor are assembled into new distilling apparatus and illustrated according to position
Figure.
In figure, the big lid of 1- vacuum flask, 2- reactors, 3- new reactors, 4- also-steam joint stove.
Embodiment
The specific embodiment of the present invention is described in more detail below.These embodiments are provided to be to be able to more thoroughly
Understand the present invention, and the scope of the present invention can be completely communicated to those skilled in the art.
"comprising" or " comprising " as mentioned in working as in specification in the whole text and claim are an open language, therefore should
It is construed to " include but be not limited to ".To implement the better embodiment of the present invention, so description is specification subsequent descriptions
For the purpose of the rule of specification, the scope of the present invention is not limited to.Protection scope of the present invention is weighed when regarding appended
Profit requires that institute's defender is defined.
Embodiment 1
The big lid of reactor and the processing method of vacuum flask adhesion, the processing method are in a kind of titanium sponge production：Will be viscous
The upper and lower of the big lid 2 of reactor even and vacuum flask 1 is respectively mounted the new reactor 3 for needing to ooze titanium, is assembled into new distilling apparatus
(such as Fig. 1), after leak detection is qualified, it is evaporated in vacuo, reactor is covered greatly with the magnesium on vacuum flask, magnesium chloride with temperature and very
The change of reciprocal of duty cycle, it is evaporated on the inner surface of upper and lower new reactor, so as to the separation realized vacuum flask and covered greatly.
Specifically, described distill is carried out in also-steaming joint stove 4, and also-steaming joint stove 4 is 4 temperature controls, and temperature controlling point is arranged
Cloth is respectively 1#, 2#, 3#, 4# point from top to bottom.
The distillation is to carry out stage by stage, specific as follows：First stage：The temperature of 1#, 2#, 3#, 4# point is 200 DEG C,
Constant temperature 2 hours, is vacuumized with water ring pump；Second stage：The temperature of 1#, 2#, 3#, 4# point is 400 DEG C, constant temperature 2 hours, uses water
Ring pumping vacuum；Phase III：1# points temperature is 950 DEG C, and 2#, 3#, 4# point temperature are 850 DEG C, constant temperature 1 hour, with low true
Empty pumping vacuum；Fourth stage：1# points temperature is 950 DEG C, and 2#, 3#, 4# point are 900 DEG C, constant temperature 3 hours, use high-vacuum pump
Vacuumize.
Embodiment 2
The big lid of reactor and the processing method of vacuum flask adhesion, the processing method are in a kind of titanium sponge production：Will be viscous
The upper and lower of the big lid 2 of reactor even and vacuum flask 1 is respectively mounted the new reactor 3 for needing to ooze titanium, is assembled into new distilling apparatus
(such as Fig. 1), after leak detection is qualified, it is evaporated in vacuo, reactor is covered greatly with the magnesium on vacuum flask, magnesium chloride with temperature and very
The change of reciprocal of duty cycle, it is evaporated on the inner surface of upper and lower new reactor, so as to the separation realized vacuum flask and covered greatly.
The distilling apparatus assembled will carry out forvacuum, and forvacuum degree requires that resistance vacuum gauge pressure reaches 120pa,
Then mistake vacuum test is done, distortion reciprocal of duty cycle reaches 9.33pa/10 minutes to be qualified.
Specifically, described distill is carried out in also-steaming joint stove, and also-steaming joint stove is 4 temperature controls, and temperature controlling point is arranged
It is respectively 1#, 2#, 3#, 4# point from top to bottom.
The distillation is to carry out stage by stage, specific as follows：First stage：The temperature of 1#, 2#, 3#, 4# point is 200 DEG C,
Constant temperature 2 hours, is vacuumized with water ring pump；Second stage：The temperature of 1#, 2#, 3#, 4# point is 400 DEG C, constant temperature 2 hours, uses water
Ring pumping vacuum；Phase III：1# points temperature is 950 DEG C, and 2#, 3#, 4# point temperature are 850 DEG C, constant temperature 1 hour, with low true
Empty pumping vacuum；Fourth stage：1# points temperature is 950 DEG C, and 2#, 3#, 4# point are 900 DEG C, constant temperature 3 hours, use high-vacuum pump
Vacuumize.
Whole vacuum distillation process keeps double vacuum states, i.e., all keeps vacuum in distilling apparatus and electric furnace.And electric furnace
Furnace shell remain that negative pressure is not less than 0.075Mpa in vacuum distillation process.
Embodiment 3
The big lid of reactor and the processing method of vacuum flask adhesion, the processing method are in a kind of titanium sponge production：Will be viscous
The upper and lower of the big lid 2 of reactor even and vacuum flask 1 is respectively mounted the new reactor 3 for needing to ooze titanium, is assembled into new distilling apparatus
(such as Fig. 1), after leak detection is qualified, it is evaporated in vacuo, reactor is covered greatly with the magnesium on vacuum flask, magnesium chloride with temperature and very
The change of reciprocal of duty cycle, it is evaporated on the inner surface of upper and lower new reactor, so as to the separation realized vacuum flask and covered greatly.
The distilling apparatus assembled will carry out forvacuum, and forvacuum degree requires that resistance vacuum gauge pressure reaches 120pa,
Then mistake vacuum test is done, distortion reciprocal of duty cycle reaches 9.33pa/10 minutes to be qualified.
Specifically, described distill is carried out in also-steaming joint stove 4, and also-steaming joint stove 4 is 4 temperature controls, and temperature controlling point is arranged
Cloth is respectively 1#, 2#, 3#, 4# point from top to bottom.
The distillation is to carry out stage by stage, specific as follows：First stage：The temperature of 1#, 2#, 3#, 4# point is 200 DEG C,
Constant temperature 2 hours, is vacuumized with water ring pump；Second stage：The temperature of 1#, 2#, 3#, 4# point is 400 DEG C, constant temperature 2 hours, uses water
Ring pumping vacuum；Phase III：1# points temperature is 950 DEG C, and 2#, 3#, 4# point temperature are 850 DEG C, constant temperature 1 hour, with low true
Empty pumping vacuum；Fourth stage：1# points temperature is 950 DEG C, and 2#, 3#, 4# point are 900 DEG C, constant temperature 3 hours, use high-vacuum pump
Vacuumize.
Whole vacuum distillation process keeps double vacuum states, i.e., all keeps vacuum in distilling apparatus and electric furnace.
Further, the furnace shell of electric furnace remains that negative pressure is not less than 0.075Mpa in vacuum distillation process.
Further, after vacuum distillation terminates, after water receiving cools down 4 hours to distilling apparatus between first using, then with direct water
Cooling 6 hours is carried out to distilling apparatus.
The big lid of reactor can be separated with vacuum flask in a short time using the method for the present invention, while and can is fully sharp
The magnesium and magnesium chloride covered greatly with reactor.The big lid of reactor and vacuum flask service life are improved, reduces big lid and insulation
Bottle loss, can be that enterprise saves nearly 500,000 yuan of fund every year.
Although above with general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (9)
1. the big lid of reactor and the processing method of vacuum flask adhesion in a kind of titanium sponge production, it is characterised in that the processing side
Method is：The upper and lower of the big lid of the reactor of adhesion and vacuum flask, which is respectively mounted, needs the new reactor for oozing titanium, is assembled into new steaming
Distillation unit, after leak detection is qualified, it is evaporated in vacuo, reactor is covered greatly with the magnesium on vacuum flask, magnesium chloride with temperature and very
The change of reciprocal of duty cycle, it is evaporated on the inner surface of upper and lower new reactor, so as to the separation realized vacuum flask and covered greatly.
2. the big lid of reactor and the processing method of vacuum flask adhesion, its feature in titanium sponge production according to claim 1
It is, the distilling apparatus assembled will carry out forvacuum, and forvacuum degree requires that resistance vacuum gauge pressure reaches 120pa, so
After do mistake vacuum test, distortion reciprocal of duty cycle reaches 9.33pa/10 minutes to be qualified.
3. the big lid of reactor and the processing method of vacuum flask adhesion, its feature in titanium sponge production according to claim 1
It is, the distillation is carried out in also-steaming joint stove, and also-steaming joint stove is 4 temperature controls, and temperature controlling point arrangement divides from top to bottom
Wei not 1#, 2#, 3#, 4# point.
4. the big lid of reactor and the processing method of vacuum flask adhesion, its feature in titanium sponge production according to claim 3
It is, the distillation is to carry out stage by stage, specific as follows：First stage：The temperature of 1#, 2#, 3#, 4# point is 200 DEG C, constant temperature
2 hours, vacuumized with water ring pump；Second stage：The temperature of 1#, 2#, 3#, 4# point is 400 DEG C, constant temperature 2 hours, uses water ring pump
Vacuumize；Phase III：1# points temperature is 950 DEG C, and 2#, 3#, 4# point temperature are 850 DEG C, constant temperature 1 hour, use roughing pump
Vacuumize；Fourth stage：1# points temperature is 950 DEG C, and 2#, 3#, 4# point are 900 DEG C, constant temperature 3 hours, true with high vacuum pumping
It is empty.
5. the big lid of reactor and the processing method of vacuum flask adhesion, its feature in titanium sponge production according to claim 1
It is, whole vacuum distillation process keeps double vacuum states, i.e., all keeps vacuum in distilling apparatus and electric furnace.
6. the big lid of reactor and the processing method of vacuum flask adhesion, its feature in titanium sponge production according to claim 5
It is, the furnace shell of electric furnace remains that negative pressure is not less than 0.075Mpa in vacuum distillation process.
7. the big lid of reactor and the processing method of vacuum flask adhesion, its feature in titanium sponge production according to claim 1
It is, after vacuum distillation terminates, after water receiving cools down 4 hours to distilling apparatus between first using, then with direct water to distilling apparatus cooling 6
Hour.
8. the big lid of reactor and the processing method of vacuum flask adhesion, its feature in titanium sponge production according to claim 1
It is, has handled after the big lid of reactor and vacuum flask of adhesion, it is necessary to the new reactor for oozing titanium disassembles, continued to use
Gone during to titanium sponge production.
9. the big lid of reactor and the processing method of vacuum flask adhesion, its feature in titanium sponge production according to claim 1
It is, whole course of reaction water temperature does not control.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710707820.8A CN107435106B (en) | 2017-08-17 | 2017-08-17 | The processing method of reactor big lid and heat protection screen adhesion in a kind of titanium sponge production |
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| CN201710707820.8A CN107435106B (en) | 2017-08-17 | 2017-08-17 | The processing method of reactor big lid and heat protection screen adhesion in a kind of titanium sponge production |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111893321A (en) * | 2020-06-23 | 2020-11-06 | 云南国钛金属股份有限公司 | Device and method for disassembling bonded large cover |
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| CN86200847U (en) * | 1986-02-14 | 1986-11-12 | 北京有色金属研究总院 | Combined reduction and distillation device for producing active metals with high melting point |
| CN2830416Y (en) * | 2005-10-11 | 2006-10-25 | 遵义钛业股份有限公司 | Still pipeline on reactor cover for preparing sponge Ti and heater thereof |
| CN201172679Y (en) * | 2007-12-12 | 2008-12-31 | 朝阳百盛锆业有限公司 | Pup joint equipment of I-typed reducing-distilling combined furnace for producing spongy titanium by magnesium method |
| CN101476102A (en) * | 2009-01-23 | 2009-07-08 | 四川恒为制钛科技有限公司 | Titanizing method of reactor for producing titanium sponge |
| CN202265602U (en) * | 2011-08-26 | 2012-06-06 | 攀钢集团有限公司 | Surface treatment system of titanium sponge reactor |
| CN104831089A (en) * | 2015-05-22 | 2015-08-12 | 罗时雨 | Series furnace device for reducing distillation and production of titanium sponge |
| CN107034435A (en) * | 2017-06-20 | 2017-08-11 | 东方弗瑞德（北京）科技有限公司 | A kind of surface titanizing technique |
-
2017
- 2017-08-17 CN CN201710707820.8A patent/CN107435106B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86200847U (en) * | 1986-02-14 | 1986-11-12 | 北京有色金属研究总院 | Combined reduction and distillation device for producing active metals with high melting point |
| CN2830416Y (en) * | 2005-10-11 | 2006-10-25 | 遵义钛业股份有限公司 | Still pipeline on reactor cover for preparing sponge Ti and heater thereof |
| CN201172679Y (en) * | 2007-12-12 | 2008-12-31 | 朝阳百盛锆业有限公司 | Pup joint equipment of I-typed reducing-distilling combined furnace for producing spongy titanium by magnesium method |
| CN101476102A (en) * | 2009-01-23 | 2009-07-08 | 四川恒为制钛科技有限公司 | Titanizing method of reactor for producing titanium sponge |
| CN202265602U (en) * | 2011-08-26 | 2012-06-06 | 攀钢集团有限公司 | Surface treatment system of titanium sponge reactor |
| CN104831089A (en) * | 2015-05-22 | 2015-08-12 | 罗时雨 | Series furnace device for reducing distillation and production of titanium sponge |
| CN107034435A (en) * | 2017-06-20 | 2017-08-11 | 东方弗瑞德（北京）科技有限公司 | A kind of surface titanizing technique |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111893321A (en) * | 2020-06-23 | 2020-11-06 | 云南国钛金属股份有限公司 | Device and method for disassembling bonded large cover |
| CN111893321B (en) * | 2020-06-23 | 2022-06-17 | 云南国钛金属股份有限公司 | Device and method for disassembling bonded large cover |
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| CN107435106B (en) | 2019-06-21 |
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