CN106048242B - With method of the plateau with rectifying fire concentrate zirconium hafnium - Google Patents
With method of the plateau with rectifying fire concentrate zirconium hafnium Download PDFInfo
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- CN106048242B CN106048242B CN201610477996.4A CN201610477996A CN106048242B CN 106048242 B CN106048242 B CN 106048242B CN 201610477996 A CN201610477996 A CN 201610477996A CN 106048242 B CN106048242 B CN 106048242B
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- rectifying
- hafnium
- zirconium
- plateau
- equipment
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Classifications
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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
-
- 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
- C22B34/14—Obtaining zirconium or hafnium
-
- 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
- Y02P10/20—Recycling
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Acoustics & Sound (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of method for manufacturing nuclear grade zirconium and rich hafnium object, it is characterized in that the complete set of equipments of rectifying fire concentrate zirconium hafnium is placed on the plateau of 4500 meters of height above sea level or more.The intermediate fused salt chlorine potassium aluminate (KAlCl of most critical in the present invention4) it is directly to be made with the barium salt and kalunite of Chinese mineral products production.
Description
First, technical field：This patent belongs to the marginal technology field that Chemical Engineering Technology and metallurgical technology are combined.
2nd, background technology：China is the country for possessing highest plateau, and Qinghai-Tibet Platean, Qinghai-Tibet Railway are open to traffic, national grid
It is all Chinese unique inherent advantage to enter to hide.Under such overall background, many experiences of the soft older generation and technology are made
The present invention.
3rd, invention content：
The content of present invention designs a kind of low atmospheric pressure in utilization (Qinghai-Tibet) plateau using zirconium chloride, hafnium tetrachloride as raw material essence
Evaporate the method for production nuclear grade zirconium and core grade hafnium.Look at corresponding table of the following height above sea level with Zenith Distance pressure：
The respective value of height above sea level and Zenith Distance pressure
| Height above sea level (m) | Air pressure (kPa) |
| 0 | 101.3 |
| 100 | 100.1 |
| 200 | 98.8 |
| 300 | 97.6 |
| 400 | 96.4 |
| 500 | 95.2 |
| 1000 | 89.4 |
| 1500 | 84.0 |
| 2000 | 78.9 |
| 2500 | 72.84 |
| 3000 | 67.24 |
| 3500 | 61.64 |
| 4000 | 56.04 |
| 4500 | 55.40 |
| 5000 | 53.88 |
It can be seen that：As long as height above sea level, to certain altitude, " normal pressure " of atmospheric distillation tower can change, all operating modes are not
Become, as long as its a whole set of pyrogenic process rectifying device is moved on sufficiently high plateau, so that it may by light component to be separated and heavy constituent
Boiling point substantially reduces, this for be not the light component and heavy constituent to be separated of higher temperature feel without what, but for height
Zirconium hafnium rectifying separation is a bit of a very crux under warm operating mode：Because：350 DEG C be conduction oil watershed：More than 350 DEG C
It then has to use organic silicone oil or high pressure conduction oil (also only to 400 DEG C), also a selection is molten salt furnace.It is well-known：Selection
Fused salt or organic silicone oil or high pressure (10 atmospheric pressure) conduction oil are not only difficult to effectively control the heating accuracy of rectifying column, and make work
Skill, equipment material requirement and control difficulty greatly increase！It is big because rectifying column three can not be met if vacuum pump-down rectifying is selected
The requirement for balancing and making separation purity that nuclear grade zirconium be not achieved at all！No one ventured thinks that (also without objective condition) will be into before this patent
Set pyrogenic process rectifying device moves the height of 4500~5000m of height above sea level, only new Tibet of the today under the leader of the Chinese Communist Party to
(conditions such as traffic, electric power)：Make it possible that the complete rectifying device of normal pressure moves the plateau of 4500~5000m of height above sea level to.(such as west
5200 meters of Anduo County mean sea level is hidden, the infrastructure such as railway, electric power are completely complete).
4th, it illustrates：
Attached drawing is a production equipment flow chart shown in 4500 meters of height above sea level or more.
Two steps of technological process point carry out：
The first step carries hafnium tetrachloride (valve F is closed, and pump 2, filler stripper do not operate)
Raw material is from charging gear at regular time and quantity into tower, KAlCl4It is controlled by frequency conversion pump for liquid salts to flow, it is molten with being dissolved in
Raw material in salt constantly carries out mass-and heat-transfer, and the hafnium tetrachloride of wherein light component is made to be enriched with to tower top, heavy constituent zirconium chloride with
Molten salt deposition in bottom of towe, raw material be added to it is a certain amount of i.e. only, after zirconium chloride purity reaches requirement, with regard to frequency conversion pump for liquid salts out of service
KAlCl is added in plate column4。
Second step detaches zirconium chloride and KAlCl4
F valves are opened, operating pump 2 detaches the mixture of plate column and reboiler is defeated to filler stripper, makes original
Sub- energy level zirconium chloride is stripped with N2 into cooling separator, the KAlCl of bottom of towe4It is for use that fused salt storage tank is returned by purification.
Other explanations：
(1) mode of heating and heat preservation：
The accurate temperature control cooling of cooler, cooling separator conduction oil (is only applicable to the work of 4500 meters of plateau elevation or more
Skill)
Condenser water vapour or the cooling of water control temperature；
The accurate temperature control heating of reboiler conduction oil (technique for being only applicable to 4500 meters of plateau elevation or more, it is impossible to be used in
Low altitude area)；
Fused salt storage tank electrical heating or the heating of other fossil fuel energies；
Nitrogen gas generator generates hot N2 gases and is heated with electric heater；
Plate column, filler stripper, pump, pipeline etc. are kept the temperature with environment-friendly insulating material；
(2) main material and equipment：(pay attention to：It is only applicable to the configuration of 4500 meters of plateau elevation or more, it is impossible to be used in low sea
It rises sheer from level ground area)
Plate column, filler stripper do tower body with nickel-base alloy multiple tube, and matrix steel plate Q345R can meet≤475 DEG C
Industrial and mineral condition, interior cladding use lnconel600 planks.Column plate lnconel600 planks.Filler glass or ceramic packing
Ring.Fused salt storage tank, cooler, cooling separator lnconel600 planks, condenser material 904L stainless steels or nickel plate.
Since this equipment is in 4500 meters of plateau elevation or more, so all pumps are with adapting to 4500 meters of High aititude or more
Pump.
Since this equipment is in 4500 meters of plateau elevation or more, so nitrogen gas generator is also with adapting to High aititude 4500
Meter or more nitrogen gas generator.
(3) intermediate fused salt chlorine potassium aluminate (KAlCl4) preparation method：
2BaCL2+KAL(SO4)2=2BaSO4(precipitation)+KCL+ALCL3
The process alum solution must be heated to 90 degrees Celsius~100 degrees Celsius！Barium chloride is high-purity.It is obtained by filter
Blanc fixe product；Its filtrate (KCL+ALCL3) be sent to after concentration on high temperature reaction stove (kettle) and control temperature Celsius up to 500
It is more than degree！Making the two, melting is chlorine potassium aluminate (KAlCl at high temperature4)。
Then it is placed in fused salt storage tank, participates in fused salt essence gold-plating.
Claims (5)
1. a kind of method of the plateau with rectifying fire concentrate zirconium hafnium, it is characterised in that：Utilize 4500 meters of plateau elevation or more
Low atmospheric pressure, can make zirconium chloride, hafnium tetrachloride sublimation point temperature reduce, will be using zirconium chloride, hafnium tetrachloride as raw material
Rectifying fire concentrate zirconium hafnium equipment put to plateau band, the reboiler conduction oil in rectifying fire concentrate zirconium hafnium equipment is accurate
Temperature control heats.
2. a kind of the method as described in claim 1, it is characterised in that：It is board-like in the rectifying fire concentrate zirconium hafnium equipment
Tower, filler stripper do tower body with nickel-base alloy multiple tube, and the nickel-base alloy multiple tube is by matrix Q345R steel plates, interior cladding
Lnconel600 planks are made.
A kind of 3. method as claimed in claim 1 or 2, it is characterised in that：Filling out in the rectifying fire concentrate zirconium hafnium equipment
Expect that stripper uses glass filler ring.
A kind of 4. method as claimed in claim 1 or 2, it is characterised in that：Divided using nitrogen gas generator to the rectifying pyrogenic process
Add nitrogen from the filler stripper in zirconium hafnium equipment.
A kind of 5. method as claimed in claim 3, it is characterised in that：Using nitrogen gas generator to the rectifying fire concentrate zirconium
Filler stripper in hafnium equipment adds nitrogen.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510675377 | 2015-10-19 | ||
| CN2015106753771 | 2015-10-19 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106048242A CN106048242A (en) | 2016-10-26 |
| CN106048242B true CN106048242B (en) | 2018-06-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610477996.4A Active CN106048242B (en) | 2015-10-19 | 2016-06-27 | With method of the plateau with rectifying fire concentrate zirconium hafnium |
Country Status (1)
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| CN (1) | CN106048242B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108998683B (en) * | 2017-06-06 | 2020-02-21 | 安徽唯安科技新材料发展有限公司 | Method for separating zirconium oxide and hafnium oxide mixture |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4021531A (en) * | 1973-11-14 | 1977-05-03 | Ugine Aciers | Process for the separation of zirconium and hafnium tetrachlorides from mixtures thereof |
| CN1461353A (en) * | 2001-04-18 | 2003-12-10 | 塞祖锆欧洲公司 | Method for separating zirconium and hafnium tetrachloride with aid of melted solvent |
| CN1993295A (en) * | 2004-07-09 | 2007-07-04 | 欧洲塞扎斯“锆”公司 | Method for separating and purifying hafnium and zirconium |
-
2016
- 2016-06-27 CN CN201610477996.4A patent/CN106048242B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4021531A (en) * | 1973-11-14 | 1977-05-03 | Ugine Aciers | Process for the separation of zirconium and hafnium tetrachlorides from mixtures thereof |
| CN1461353A (en) * | 2001-04-18 | 2003-12-10 | 塞祖锆欧洲公司 | Method for separating zirconium and hafnium tetrachloride with aid of melted solvent |
| CN1993295A (en) * | 2004-07-09 | 2007-07-04 | 欧洲塞扎斯“锆”公司 | Method for separating and purifying hafnium and zirconium |
Non-Patent Citations (1)
| Title |
|---|
| 四氯铝酸钠或四氯铝酸铁熔融盐的生产;覃奇贤 编译;《电镀与精饰》;20050531;第27卷(第3期);第39页 * |
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| CN106048242A (en) | 2016-10-26 |
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