CN107385239B - Method is melted down in distillation in a kind of titanium sponge production - Google Patents
Method is melted down in distillation in a kind of titanium sponge production Download PDFInfo
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- CN107385239B CN107385239B CN201710709082.0A CN201710709082A CN107385239B CN 107385239 B CN107385239 B CN 107385239B CN 201710709082 A CN201710709082 A CN 201710709082A CN 107385239 B CN107385239 B CN 107385239B
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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
- C22B34/1218—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 titanium or titanium compounds from ores or scrap by dry processes
- C22B34/1222—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 titanium or titanium compounds from ores or scrap by dry processes using a halogen containing agent
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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
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses distillations in a kind of titanium sponge production to melt down method, is related to sponge titanium smelting technical field, comprising the following steps: (1) black furnace enters furnace；(2) low temperature deaerates；(3) high temperature constant temperature；Wherein, high temperature constant temperature is divided into the first and second two stages, and the first stage of high temperature constant temperature is 2 hours, and the low temperature deaerates to the first stage of high temperature constant temperature using roughing pump, and the second stage of high temperature constant temperature uses high-vacuum pump.Product is melted down using the distillation of the application method, chlorine root index is substantially all 0.08 hereinafter, individual event chlorine index is primes or more；Substantially the variation such as other index oxygen, nitrogen less, has part heat oxygen index also slightly to reduce, and product hierarchy is 2 grades of product or more.
Description
Technical field
The present invention relates to sponge titanium smelting technical fields, and in particular to method is melted down in distillation in a kind of titanium sponge production.
Background technique
Product can all be melted down every year in production due to chlorine high yield first portion in magnesium method titanium sponge manufacturing enterprise, chlorine height with also
Original product generation structure, distillation time, temperature, vacuum degree, water temperature control etc. are related, melt down product majority and occur in summer, winter
Season.Assay is substantially that individual event chlorine root is high before product melts down, and product hierarchy is waste product, and other impurity indexs are within 2 grades of product.
Chlorine root high product melts down rear chlorine index and is reduced to 2 grades of product (CL " 0.10%) hereinafter, still its oxygen, nitrogen impurity content increased,
Product Brinell hardness rises, and product hierarchy is essentially three, level Four product.Product is melted down according to including following sections: 1, being disassembled
Alembic discovery channel blocks；2, it finds that surface and bottom have after product takes out and does not steam net magnesium chloride largely；3, product is in oil
The a large amount of magnesium chlorides being evenly distributed are found when crush-cutting is cut.It is that titanium sponge sticks together upper surface highest that chlorine root is distributed in titanium sticks together, middle part time
It.Chloride content is high if there is hard core at middle part.High chlorine products is exposed to the atmosphere, and wherein magnesium chloride easily absorbs sky in product
Moisture in gas.If the product processing mode after water suction is improper, oxygen, nitrogen content in product can be increased again.There is aqueous magnesium chloride,
Relative density 1.56, is heated to lose the crystallization water at 95 DEG C, 135 DEG C or more start to decompose, and release chlorine by 118 DEG C of fusing point
Change hydrogen.Magnesium chloride hexahydrate is to take off water in a point several stages.Therefore, it melts down and determines to product treatment mode process and early period
Determine high chlorine products and melts down effect.
Summary of the invention
The purpose of the present invention is to provide distillations in a kind of titanium sponge production to melt down method, asks to solve above-mentioned technology
Topic.
To achieve the above object, the technical solution of the present invention is as follows:
Method is melted down in distillation in a kind of titanium sponge production, comprising the following steps:
(1) black furnace enters furnace；(2) low temperature deaerates；(3) high temperature constant temperature；Wherein, high temperature constant temperature is divided into the first and second two ranks
Section, the first stage of high temperature constant temperature are 2 hours, and the first stage that the low temperature deaerates to high temperature constant temperature uses roughing pump,
The second stage of high temperature constant temperature uses high-vacuum pump.
Preferably, 100 DEG C of setting is for 2 hours simultaneously for 4 points for the step of step (2) low temperature deaerates, then
150 DEG C continue 3 hours, continue 2 hours for 300 DEG C later, last 350 DEG C 3 hours.
Preferably, 4 points are the point of the 4 control temperature set gradually from top to bottom in reduction and distillation furnace
Position, the setting of this 4 point belongs to the conventional arrangement of those skilled in the art, according to the height reasonable layout of reduction and distillation furnace.
Preferably, 4 points are set as 970 DEG C simultaneously respectively from top to bottom in step (3) high temperature constant temperature, and 990 DEG C,
940 DEG C, 920 DEG C.
Preferably, the second stage of step (3) high temperature constant temperature is 20 hours.
Preferably, further comprising the steps of before the step (1):
Titanium is sticked together first and is taken out from reactor, by titanium stick together upper epithelium and the highest bottom skin of impurity content clear up it is dry
Only；
The reactor sieve plate that titanium sticks together will be filled again to be buckled on rollover stand, removes the sundries under sieve plate；The reactor cleared up
In one layer of the sieve plate upper berth titanium that swashes, the titanium cleared up being sticked together and is put into ready reactor, top covers the one layer of titanium that swashes again,
It is assembled into distilling apparatus, leak detection is then vacuumized and reenters furnace after leak detection is qualified.Leak detection standard are as follows: distilling apparatus is put into retort
It is interior, forvacuum degree, it is desirable that the pressure of resistance vacuum gauge reaches 120pa, and distortion reciprocal of duty cycle 9.33pa/10 minutes is qualification, distillation
The requirement of distortion reciprocal of duty cycle 9.33pa/10 minutes is not achieved in pressure in device, just has to check for handling, until reaching requirement.
Preferably, the granularity of the titanium that swashes in the titanium that swashes of one layer of sieve plate upper berth is 50-100mm.
Preferably, it is 100-200mm that the top covers the granularity for the titanium that swashes in the one layer of titanium that swashes again.
Preferably, process water temperature is entirely melted down not control.
The method of the present invention has the advantages that
1, product is melted down in this technique distillation, and chlorine root index is all 0.08 hereinafter, individual event chlorine index is primes or more；It is other
Substantially the variation such as index oxygen, nitrogen less, has part heat oxygen index also slightly to reduce, product hierarchy is more than 2 grades of product；
2, it ensure that the stability for melting down product, reduce the probability that single furnace product significantly degrades.
3, product hierarchy improves, and increases the performance of enterprises.
Specific embodiment
Specific embodiments of the present invention are 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 fully disclosed to those skilled in the art.
"comprising" or " comprising " as mentioned throughout the specification and claims are an open language, therefore are answered
It is construed to " including but not limited to ".Specification subsequent descriptions are to implement better embodiment of the invention, and so description is
For the purpose of the rule of specification, the range that is not intended to limit the invention.Protection scope of the present invention is when the appended power of view
Benefit requires subject to institute's defender.
Embodiment 1
The product for needing to melt down takes work that titanium sticks together to take out from reactor by beating first, and the titanium upper epithelium cleaning that sticks together is dry
Only；The highest bottom skin of impurity content is cleaned out；The reactor sieve plate that titanium sticks together will be filled again to clear up thoroughly, reactor is on rollover stand
The sundries under sieve plate is removed in back-off.The titanium that swashes of the reactor cleared up layer overlay granularity 50mm on sieve plate, clearing up
Titanium stick together and be put into ready reactor, top covers the titanium that swashes of one layer of granularity 100mm, and the titanium sponge of appropriate granularity is to returning
The titanium sponge of furnace, which sticks together, protective effect, while absorbing titanium and sticking together the evaporation of moisture in interior institute's magnesium chloride containing, sticks together middle magnesium chloride conducive to titanium
Diffusion and filtering.It is assembled into distilling apparatus, leak detection is vacuumized, is melted down after qualified.Leak detection standard are as follows: distilling apparatus is put into distillation
In furnace, forvacuum degree, it is desirable that the pressure of resistance vacuum gauge reaches 120pa, and distortion reciprocal of duty cycle 9.33pa/10 minutes is qualification, steams
The requirement of distortion reciprocal of duty cycle 9.33pa/10 minutes is not achieved in pressure in distillation unit, just has to check for handling, and is up to reaching requirement
Only.
Melt down process conditions:
(1) black furnace enters furnace；
(2) low temperature deaerates: 4 points be arranged simultaneously 100 DEG C it is for 2 hours, then continue 3 hours for 150 DEG C, later 300
DEG C continue 2 hours, last 350 DEG C continue 3 hours, and 4 points are the 4 controls temperature set gradually in reduction and distillation furnace
The point of degree；
(3) high temperature constant temperature: high temperature constant temperature is divided into the first and second two stages, and the first stage of high temperature constant temperature is 2 small
When, second stage constant temperature time 20 hours, 4 points were set as 970 DEG C simultaneously respectively from top to bottom, and 990 DEG C, 940 DEG C, 920
℃；
(4) with pump sequence: the low temperature deaerates the first stage to high temperature constant temperature using roughing pump, and the of high temperature constant temperature
Two-stage uses high-vacuum pump；
(5) whole process water temperature does not control.It is to require control water temperature, but melt down product distillation during normal furnace distillation
Just water temperature is not controlled since entering the degassing of furnace low temperature, directly amplifies water.
Embodiment 2
The product for needing to melt down takes work that titanium sticks together to take out from reactor by beating first, and the titanium upper epithelium cleaning that sticks together is dry
Only；The highest bottom skin of impurity content is cleaned out；The reactor sieve plate that titanium sticks together will be filled again to clear up thoroughly, reactor is on rollover stand
Object under sieve plate is removed in back-off.The titanium that swashes of the reactor cleared up layer overlay granularity 100mm on sieve plate, the titanium cleared up
It sticks together and is put into ready reactor, top covers the titanium that swashes of one layer of granularity 200mm.It is assembled into distilling apparatus, vacuumizes inspection
Leakage is melted down after qualified.Leak detection standard are as follows: distilling apparatus is put into retort, forvacuum degree, it is desirable that the pressure of resistance vacuum gauge
Reach 120pa, distortion reciprocal of duty cycle 9.33pa/10 minutes is qualification, and pressure is not achieved reciprocal of duty cycle 9.33pa/10 points of distortion in distilling apparatus
The requirement of clock just has to check for handling, until reaching requirement.
Melt down process conditions:
(1) black furnace enters furnace；
(2) low temperature deaerates: 4 points be arranged simultaneously 100 DEG C it is for 2 hours, then continue 3 hours for 150 DEG C, later 300
DEG C continue 2 hours, last 350 DEG C continue 3 hours；
(3) high temperature constant temperature: high temperature constant temperature is divided into the first and second two stages, and the first stage of high temperature constant temperature is 2 small
When, second stage constant temperature time 20 hours, 4 points were set as 970 DEG C simultaneously respectively from top to bottom, and 990 DEG C, 940 DEG C, 920
℃；
(4) with pump sequence: the low temperature deaerates the first stage to high temperature constant temperature using roughing pump, and the of high temperature constant temperature
Two-stage uses high-vacuum pump；
(5) whole process water temperature does not control.
Embodiment 3
The product for needing to melt down takes work that titanium sticks together to take out from reactor by beating first, and the titanium upper epithelium cleaning that sticks together is dry
Only；The highest bottom skin of impurity content is cleaned out；The reactor sieve plate that titanium sticks together will be filled again to clear up thoroughly, reactor is on rollover stand
Object under sieve plate is removed in back-off.The titanium that swashes of the reactor cleared up layer overlay granularity 75mm on sieve plate, the titanium cleared up
It sticks together and is put into ready reactor, top covers the titanium that swashes of one layer of granularity 150mm.It is assembled into distilling apparatus, vacuumizes inspection
Leakage is melted down after qualified.Leak detection standard are as follows: distilling apparatus is put into retort, forvacuum degree, it is desirable that the pressure of resistance vacuum gauge
Reach 120pa, distortion reciprocal of duty cycle 9.33pa/10 minutes is qualification, and pressure is not achieved reciprocal of duty cycle 9.33pa/10 points of distortion in distilling apparatus
The requirement of clock just has to check for handling, until reaching requirement.
Melt down process conditions:
(1) black furnace enters furnace；
(degassing of (2) low temperature: 4 points be arranged simultaneously 100 DEG C it is for 2 hours, then continue 3 hours for 150 DEG C, later 300
DEG C continue 2 hours, last 350 DEG C continue 3 hours；
(3) high temperature constant temperature: high temperature constant temperature is divided into the first and second two stages, and the first stage of high temperature constant temperature is 2 small
When, second stage constant temperature time 20 hours, 4 points were set as 970 DEG C simultaneously respectively from top to bottom, and 990 DEG C, 940 DEG C, 920
℃；
(4) with pump sequence: the low temperature deaerates the first stage to high temperature constant temperature using roughing pump, and the of high temperature constant temperature
Two-stage uses high-vacuum pump；
(5) whole process water temperature does not control.It is to require control water temperature, but melt down product distillation during normal furnace distillation
Just water temperature is not controlled since entering the degassing of furnace low temperature, directly amplifies water.
Comparative example 1
Equipment and product are not handled before melting down, while also do not covered to melting down product, specifically included following
Step: (1) black furnace enters furnace；(2) low temperature deaerates: 4 150 DEG C of point constant temperature 3 hours, then 350 DEG C of each point constant temperature 3 hours；(3) high
Warm constant temperature: 4 points are arranged 800 DEG C constant temperature 4 hours, and it is 970 DEG C that then temperature, which is arranged, in each point simultaneously respectively from top to bottom, and 990
DEG C, 960 DEG C, 950 DEG C, constant temperature time 25 hours (4) with pump sequence: low temperature degassing water ring pump, 2 before 800 DEG C and high temperature constant temperature
High-vacuum pump is used after 2 hours with roughing pump, high temperature constant temperature within a hour；(5) whole process water temperature does not control.
It is tested using 5 furnace products, as a result as follows after it is compared with comparative example 1 by taking embodiment 3 as an example:
1 result of comparative example is as follows:
Melt down the comparison of front and back index (mainly including Cl%, N%, O%, HB)
Major impurity content analysis result and product hierarchy before 1 comparative example 1 of table is melted down
2 comparative example 1 of table melts down rear major impurity content analysis result and product hierarchy
3 result of embodiment is as follows:
Melt down the comparison of front and back index (mainly including Cl%, N%, O%, HB)
Major impurity content analysis result and product hierarchy before 3 embodiment 3 of table is melted down
4 embodiment 3 of table melts down rear major impurity content analysis result and product hierarchy
As the result is shown: the oxygen index of comparative example 1 can all have certain amplitude increase, and product hierarchy is essentially 3 grades of product or 4 grades
Product, and 3 chlorine root index of embodiment is substantially all 0.08 hereinafter, individual event chlorine index is primes or more；The bases such as other index oxygen, nitrogen
This variation less, has part heat oxygen index also slightly to reduce, product hierarchy is 2 grades of product or more, therefore, using the side of the application
Method ensure that the stability for melting down product, reduce the probability significantly to degrade due to single furnace product.
Although above having used 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 are fallen within the scope of the claimed invention.
Claims (8)
1. method is melted down in distillation in a kind of titanium sponge production, which comprises the following steps:
Titanium is sticked together first and is taken out from reactor, titanium is sticked together into upper epithelium and the highest bottom skin of impurity content is cleaned out；
The reactor sieve plate that titanium sticks together will be filled again to be buckled on rollover stand, removes the sundries under sieve plate；
The reactor cleared up sticks together the titanium cleared up and is put into ready reactor in one layer of the sieve plate upper berth titanium that swashes, on
Portion covers the one layer of titanium that swashes again, is assembled into distilling apparatus, then vacuumizes leak detection and reenters furnace after leak detection is qualified and successively pass through (1)
Black furnace enters furnace；(2) low temperature deaerates；(3) high temperature constant temperature；Wherein, high temperature constant temperature is divided into the first and second two stages, high temperature constant temperature
First stage be 2 hours, the low temperature deaerates the first stage to high temperature constant temperature using roughing pump, the of high temperature constant temperature
Two-stage uses high-vacuum pump.
2. method is melted down in distillation in a kind of titanium sponge production according to claim 1, which is characterized in that the step (2)
100 DEG C of setting is for 2 hours simultaneously for 4 points for the step of low temperature deaerates, and then continues 3 hours for 150 DEG C, and 300 DEG C later
Continue 2 hours, last 350 DEG C continue 3 hours, and 4 points are the 4 control temperature set gradually in reduction and distillation furnace
Point.
3. method is melted down in distillation in a kind of titanium sponge production according to claim 1 or 2, which is characterized in that the step
(3) 4 points are set as 970 DEG C, 990 DEG C, 940 DEG C, 920 DEG C simultaneously respectively from top to bottom in high temperature constant temperature.
4. method is melted down in distillation in a kind of titanium sponge production according to claim 3, which is characterized in that the step (3)
The second stage of high temperature constant temperature is 20 hours.
5. method is melted down in distillation in a kind of titanium sponge production according to claim 1, which is characterized in that described on sieve plate
The granularity for the titanium that swashes in one layer of titanium that swashes of paving is 50-100mm.
6. method is melted down in distillation in a kind of titanium sponge production according to claim 5, which is characterized in that cover again on the top
The granularity for the titanium that swashes in one layer of titanium that swashes of lid is 100-200mm.
7. method is melted down in distillation in a kind of titanium sponge production according to claim 6, which is characterized in that entirely melt down process
Water temperature does not control.
8. method is melted down in distillation in a kind of titanium sponge production according to claim 1, which is characterized in that leak detection standard are as follows:
Distilling apparatus is put into retort, forvacuum degree, it is desirable that the pressure of resistance vacuum gauge reaches 120pa, is distorted reciprocal of duty cycle 9.33pa/
10 minutes are qualification, and the requirement of distortion reciprocal of duty cycle 9.33pa/10 minutes is not achieved in pressure in distilling apparatus, just have to check for handling,
Until reaching requirement.
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| CN103740951A (en) * | 2013-12-26 | 2014-04-23 | 攀钢集团钛业有限责任公司 | Treatment method of standard exceeding of content of chlorine in titanium sponge |
| CN103882245A (en) * | 2012-12-21 | 2014-06-25 | 攀钢集团钛业有限责任公司 | Magnesium refining method and titanium sponge preparation method |
| CN104911375A (en) * | 2015-06-12 | 2015-09-16 | 罗时雨 | Crushing-free production technique of sponge titanium |
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2017
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|---|---|---|---|---|
| US6475428B1 (en) * | 2001-04-21 | 2002-11-05 | Joseph T. Fraval | Method of producing titanium powder |
| JP2003193151A (en) * | 2001-12-28 | 2003-07-09 | Nikko Materials Co Ltd | Method for recovering titanium from titanium-containing scrap |
| CN201587972U (en) * | 2009-08-11 | 2010-09-22 | 遵义钛业股份有限公司 | Reduction distillation device for producing titanium sponge |
| CN102181670A (en) * | 2011-04-25 | 2011-09-14 | 东北大学 | Method for preparing titanium sponge through magnesium and chlorine recycling |
| CN103882245A (en) * | 2012-12-21 | 2014-06-25 | 攀钢集团钛业有限责任公司 | Magnesium refining method and titanium sponge preparation method |
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Effective date of registration: 20201224 Address after: 620800 No. 618, south section of Gongye West 1st Road, Qinglong Street, Pengshan District, Meishan City, Sichuan Province Patentee after: SICHUAN JINGZHAOHONG TECHNOLOGY Co.,Ltd. Address before: Room 107-95, block a, zhuanqiang economic Park, 138 zhuyuanli, zhuanqiang Town, Gaochun District, Nanjing City, Jiangsu Province, 211300 Patentee before: Zhonghong supply chain management (Nanjing) Co., Ltd |