CN109182786A - A kind of no oxygen impurities volatilization prepares the method and device of high pure metal beryllium - Google Patents
A kind of no oxygen impurities volatilization prepares the method and device of high pure metal beryllium Download PDFInfo
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- CN109182786A CN109182786A CN201811058307.1A CN201811058307A CN109182786A CN 109182786 A CN109182786 A CN 109182786A CN 201811058307 A CN201811058307 A CN 201811058307A CN 109182786 A CN109182786 A CN 109182786A
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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
- C22B35/00—Obtaining beryllium
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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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Abstract
The present invention discloses the method for refining and device of a kind of metallic beryllium, under anaerobic, by the beryllium pearl heating containing impurity, heating temperature need to be higher than the fusing point of beryllium and the boiling point of impurity, drop is formed after the fusing of beryllium pearl to emerge and drop down from the side aperture of upper portion crucible, during drippage, impurity element volatilization obtains refining beryllium；Adjustable support (8) length for adjusting raw material crucible changes the volatilization time；Used side-wall hole crucible, adjustable support in the method for refining of metallic beryllium；The present invention can effectively deviate from the impurity content of Li, Pb, Mg, K, Zn in pure beryllium, improve pure beryllium grade.
Description
Technical field
The present invention relates to a kind of method of refining of metallic beryllium and devices, belong to metallurgy and Material Field.
Background technique
Metallic beryllium is more active, and fusing point is the oxidation film passivation easy to form of the aerial metallic beryllium surface of exposure, the film
Quality is hard, closely knit, fusing point is high, and beryllium can be protected not continue to aoxidize, and can also form hard wrapping layer at high temperature, in prevention
The volatile gas in portion is excessive.This characteristic brings very big influence to vacuum volatilization impurity removal process, for effumability impurity
The big alloy of comparision contents, such as Mg impurity > 3wt% or more in 95 wt%Be, Mg steam will form huge in vacuum volatilization
Bubble break through oxidation beryllium film package, form a large amount of cavity on raw material surface, for further micro Mg volatilize provide it is logical
Road；The pure metal less for impurity content, such as Mg content < 1wt% of Be-4, Mg quantity of steam is very little in vacuum volatilization, only
The numerous micro-bubble of energy forming quantity has no ability to the package for breaking through oxidation beryllium film.Therefore using conventional intermittent reaction
Kettle executes vacuum volatilization impurity removal process, and the impurity-eliminating effect of the higher raw material of purity is not as good as the biggish raw material of impurity content.
After metallic beryllium fusing, the density of beryllium is 1.848g/cm3, the density of beryllium oxide is 3.025 g/cm3, therefore old oxygen
Changing beryllium can precipitate to form bottom wrapping layer；What industrial volatilization furnace internal environment can also be brought into containing a small amount of oxygen and raw material
The exposed metallic beryllium of oxidant meeting oxidized surface forms new beryllium oxide hard shell, and two layers of hard shell of the old and new encloses the logical of upper and lower part
Road.Existing vacuum distillation refined metals beryllium can only improve the abjection amount of volatile impurity by the method repeatedly distilled, such as
Second distillation distills ... three times, and technique is cumbersome, and effect is also bad.
Summary of the invention
In order to break through the package of surface oxidation beryllium film, a kind of method of refining of metallic beryllium will contain in oxygen-free environment
The beryllium pearl of impurity is heated, and heating temperature is higher than the fusing point of beryllium and the boiling point of impurity, when the boiling point of impurity is higher than the fusing point of beryllium, beryllium
It first melts, continues to be heated to the boiling point of impurity or more, form drop after the fusing of beryllium pearl, emerge simultaneously from the side opening of eminence raw material crucible
It drops down, during drippage, impurity volatilization obtains refining beryllium；When the boiling point of impurity is lower than the fusing point of beryllium, impurity is first
Volatilization, but volatile quantity is seldom, continues to be heated to the fusing point of beryllium or more, drop is formed after the fusing of beryllium pearl, from eminence raw material crucible
Side opening emerge and drop down, during drippage, impurity volatilization, obtain refining beryllium；Refine beryllium in the liquid state, further
Volatilization refining.
After impurity content, drop size, temperature and pressure are fixed, the evaporation rate of impurity is also just at definite value, in order to mention
Volatilization total amount of the high impurity in dropping process, can also extend volatilization the time, by adjusting raw material crucible and residue earthenware
The distance between crucible d also just changes molten drop drop, changes Drain time, that is, impurity volatilization when
Between, low-grade metal biggish for impurity content is added by the distance between the residue crucible of increasing raw material crucible d
The long volatilization time；The lower high-grade raw material of impurity content, by the distance between the residue crucible for shortening raw material crucible
D shortens the volatilization time, improves production efficiency.
In the beryllium pearl containing impurity impurity be Zn, Mg, K, Li, Pb, one or more of.
The oxygen-free environment is that sealing space 99.9% is that inert gas or vacuum degree are less than 2mmHg.
The present invention also provides device used in the method for refining of the metallic beryllium, including inertia gas cylinder 1, valve 2, remove
Dirt device 3, vacuum pump 4, raw material crucible 6, bracket 8, heating element 10, shell 11, product crucible 15,11 top of shell are successively set
There are dust-extraction unit 3, vacuum pump 4,11 top of shell is also connected with inertia gas cylinder 1, and valve is equipped between inertia gas cylinder 1 and shell 11
2,11 inner wall of shell is equipped with heating element 10, is equipped with raw material crucible 6, bracket 8, product crucible 15, raw material earthenware inside shell 11
Crucible 6 is arranged on bracket 8, and product crucible 15 is arranged below raw material crucible 6, and 1 or more side is provided on 6 side wall of raw material crucible
Hole 12, the bottom outer diameter of raw material crucible 6 are less than the top internal diameter of product crucible 15.
The bracket 8 is telescope support, by adjusting the collapsing length of bracket 8, adjusts 6 bottom of raw material crucible and product earthenware
The distance between 15 bottom of crucible, the bar of telescope support are the telescopic rod of regular market purchase.
The heating element 10 is adding thermal resistance.
12 Edge Distance raw material crucible of side opening, the 6 bottom 1-60mm, for storing the beryllium oxide fragment to precipitate.
Beryllium pearl containing impurity is put into raw material crucible 6, the telescopic rod of bracket 8 is adjusted, makes side opening 12 apart from crucible
The distance of bottom reaches requirement, and closing of housing 11 closes the valve 2 of 1 road of inertia gas cylinder, vacuum pump 4 is opened, to shell 11
Inside vacuumizes, and extracts the air of the inside out, it is oxygen-free environment that vacuum degree, which drops to 2mmHg or less,；Or after vacuumizing, close true
Sky pump 4, opens the valve 2 of 1 road of inertia gas cylinder, allows inert gas full of inside shell 11, inert gas accounts for 99.9% or more
Also it is oxygen-free environment, opens heating element 10, to being heated inside shell 11, when the boiling point of impurity is higher than the fusing point of beryllium, beryllium
It first melts, continues to be heated to the boiling point of impurity or more, drop 14 is formed after the fusing of beryllium pearl, from the side opening 12 of eminence raw material crucible 6
It emerges and drops down, during drippage, impurity volatilization obtains refining beryllium；When the boiling point of impurity is lower than the fusing point of beryllium,
Impurity first volatilizees, but volatile quantity is seldom, continues to be heated to the fusing point of beryllium or more, drop 14 is formed after the fusing of beryllium pearl, from eminence
The side opening 12 of raw material crucible 6 emerges and drops down, and during drippage, impurity volatilization obtains refining beryllium；Beryllium is refined in liquid
Under state, further volatilization refining.
The impurity content of zinc, magnesium, lead, potassium, lithium in pure beryllium etc. can be effectively reduced in the present invention, improves pure beryllium grade.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention；
In figure: 1- inertia gas cylinder, 2- valve, 3- dust-extraction unit, 4- vacuum pump, 5- pipeline, 6- raw material crucible, the new beryllium oxide of 7- are hard
Shell, 8- bracket, 9- metallic beryllium melt, 10- heating element, 11- shell, 12- side opening, 13- beryllium oxide fragment, 14- drop, 15-
Product crucible.
Specific embodiment
Embodiment 1
A kind of method of refining of metallic beryllium, raw material are that certain metallic beryllium Be-4 grade that Kazakhstan produces contains trace meter
The mass percentage content of Zn is 0.4 wt%, and the mass percentage content of impurity summation is 0.95 wt%, and the device of use is such as
Shown in Fig. 1, including inertia gas cylinder 1, valve 2, dust-extraction unit 3, vacuum pump 4, raw material crucible 6, bracket 8, heating element 10, shell
11, product crucible 15, is successively arranged dust-extraction unit 3, vacuum pump 4 by pipeline 5 at the top of shell 11, and 11 top of shell also passes through pipe
Road is connected with inertia gas cylinder 1, and valve 2 is equipped between inertia gas cylinder 1 and shell 11, and inertia gas cylinder 1 is provided with inert nitrogen gas,
11 inner wall of shell is equipped with heating element 10, and heating element 10 is adding thermal resistance, is equipped with raw material crucible 6, bracket inside shell 11
8, product crucible 15, raw material crucible 6 are arranged on bracket 8, and bracket 8 is telescope support, and product crucible 15 is arranged in raw material crucible 6
Lower section is provided with 2 side openings 12 on 6 side wall of raw material crucible, and the outer diameter of side opening 12 is 10mm, and the bottom outer diameter of raw material crucible 6 is small
In the top internal diameter of product crucible 15, the bottom outer diameter of raw material crucible 6 is 80mm, and the internal diameter of product crucible 15 is 100mm, side opening
12 bottom " d " apart from raw material crucible 6 is 5mm, and bottom is for storing the beryllium oxide fragment to precipitate, by adjusting bracket 8
Collapsing length, adjustment the distance between 6 bottom of raw material crucible and 15 bottom of product crucible " d " be 130mm；Specific method is such as
Under:
Metallic beryllium pearl is placed in raw material crucible 6, adjusts the telescopic rod of bracket 8, reaches side opening 12 apart from the distance of crucible bottom
To requirement, closing of housing 11 closes the valve 2 of 1 road of inertia gas cylinder, opens vacuum pump 4, to being vacuumized inside shell 11,
After vacuumizing, vacuum pump 4 is closed, opens the valve 2 of 1 road of inertia gas cylinder, allows inert gas to be full of inside shell 11, inertia
It is also oxygen-free environment that gas, which accounts for 99.9% or more i.e., and heating element 6 is internally heated shell 7, and zinc impurities are at 760mmHg
Boiling point be 907 DEG C and be lower than 1287 DEG C of fusing point of beryllium, after reaching 1287 DEG C, continue to quickly heat up to 1307 DEG C, be higher than beryllium fusing point
About 20 DEG C, this temperature is kept, the average evaporation rate of Zn is 16mg/S at this time, and fall time is 0.25 second average, melting sources
Metallic beryllium melt 9 is formed afterwards, breaks through the package of oxidation film at crucible side opening 12, drop 14 is formed under the effect of gravity, from side opening 8
It drops down, during drippage, volatile impurity zinc gasifies form metallic vapour rapidly, and 14 surface of drop is in oxygen-free environment
In not will form new oxidation film, the smooth volatilization in drip process of the zinc inside beryllium is detached from molten drop, most of metal steam
Vapour enters dust-extraction unit 3 along pump-line 5, completes cooling and gathers dust, in order to avoid impurity enters vacuum pump 2, condenses in shell on a small quantity
On 11 inner walls, the condensate in 11 inner wall of periodic cleaning shell and dust-extraction unit 3 is needed, non-volatile part falls into product crucible 15
Refining beryllium is inside obtained, and keeps liquid, wherein micro volatile impurity can also further volatilize, until raw material water clock is complete
Finish, the mass percentage of Zn drops to 0.002 wt%, the quality percentage of impurity summation in the refining beryllium in product crucible 15
Content drops to 0.15wt%, just reaches Be-2 energy level requirement, and what 6 bottom of raw material crucible saved is the oxygen of raw material beryllium bead surface
Change beryllium fragment 13, refining terminates the beryllium oxide precipitating 13 of cleaning 6 bottom of side-wall hole crucible, could charge again.
Using common rotary-vane vaccum pump, fixed kettle crucible and vacuum metallurgy furnace, volatilization vacuum degree is 1mmHg, heating temperature
Degree is 1278 DEG C, and after traditional vacuum volatilization purification, the mass percentage content of the Zn of raw material drops to 0.35 wt%, miscellaneous
The mass percentage content of matter summation drops to 0.89 wt%.
Embodiment 2
A kind of method of refining of metallic beryllium, raw material are that certain metallic beryllium that Hunan China scenery with hills and waters mouth is produced is using Mg thermal reduction system
It is standby, contain a large amount of magnesium metals (mass percentage content is about 2-5wt%) in raw material, and contain micro lead, use and embodiment
1 identical device, the quantity of side opening 12 are 3, and the outer diameter of raw material crucible 6 is 50mm, and the internal diameter of product crucible 15 is 70mm, side
Hole 12 is 1mm apart from raw material crucible 6 " h ", different from embodiment 1, and since volatile total impurities are larger, needing to increase can
Adjust 8 length of bracket to 200mm, the distance between 15 bottom of 6 bottom of side-wall hole crucible and product crucible " d " is 150mm, is passed through
Increase molten drop distance of fall, increase the volatilization time of drop, the specific method is as follows:
Metallic beryllium pearl is placed in raw material crucible 6, adjusts the telescopic rod of bracket 8, reaches side opening 12 apart from the distance of crucible bottom
To requirement, closing of housing 11 closes the valve 2 of 1 road of inertia gas cylinder, opens vacuum pump 4, to being vacuumized inside shell 11,
Extract the air of the inside out, it is oxygen-free environment that vacuum degree, which drops to 1mmHg, and the beryllium of micro oxygen element patina forms new oxidation
Beryllium hard shell 7.The boiling point of Mg is 605 DEG C at this time, and the boiling point of lead is 977 DEG C, lower than 1287 DEG C of fusing point of beryllium, opens heating element
10, heating temperature is 1327 DEG C, is higher than about 50 DEG C of beryllium fusing point, and the average evaporation rate of impurity is 30mg/S, fall time at this time
It is 0.35 second average.Metallic beryllium is heated to up to after fusing point, is kept+50 DEG C of fusing point of volatilization temperature, is formed metal after melting sources
Beryllium melt 9 breaks through the package of oxidation film at crucible side opening 12, forms drop 14 under the effect of gravity, drops down from side opening 8,
During drippage, volatile impurity zinc gasifies form metallic vapour rapidly, and 14 surface of drop will not shape in oxygen-free environment
The oxidation film of Cheng Xin, the smooth volatilization in drip process of zinc inside beryllium are detached from molten drop, and most of metallic vapour is along pumping
Pipeline 5 enters dust-extraction unit 3, completes cooling and gathers dust, in order to avoid impurity enters vacuum pump 2, is condensed on 11 inner wall of shell on a small quantity,
The condensate in 11 inner wall of periodic cleaning shell and dust-extraction unit 3 is needed, non-volatile part falls into product crucible 15 and obtains essence
Beryllium is refined, and keeps liquid, wherein micro volatile impurity can also further volatilize, until raw material water clock finishes, inside beryllium
Micro Mg and Pb not only volatilization is detached from molten drop in drip process, into residue crucible after can also volatilize at a slow speed, it is former
The Mg content of material drops to 0.001wt%, and Pb is lower than 0.001wt%, and impurity summation drops to 0.3wt%, reaches Be-1 grades of requirements.
Refining terminates the beryllium oxide precipitating 13 of cleaning 6 bottom of side-wall hole crucible, could charge again.
After traditional vacuum volatilization purifies Drain time same as Example 2, the mass percent of the Mg of raw material contains
Amount drops to 0.95 wt%, and the mass percentage content of Pb drops to 0.005 wt%, the mass percentage content of impurity summation
Drop to 0.13 wt%, belongs to the Be of 98.8 wt% grades.
Embodiment 3
A kind of method of refining of metallic beryllium, raw material are that certain metallic beryllium that Hunan China scenery with hills and waters mouth is produced is using Mg thermal reduction system
It is standby, contain a large amount of magnesium metals (mass percentage content is about 2-5wt%) in raw material, using device identical with embodiment, side opening
12 quantity is 3, and the outer diameter of raw material crucible 6 is 50mm, and the internal diameter of product crucible 15 is 70mm, increases side opening 12 apart from side wall
" h " Dao 60mm of aperture crucible 6, different from embodiment 1,2, the connection of 6 bottom of raw material crucible saves the oxygen of raw material beryllium bead surface
Change beryllium fragment 13, can add up charging after last time refining, without clearing up side-wall hole crucible 6.The specific method is as follows:
Metallic beryllium pearl is placed in raw material crucible 6, adjusts the telescopic rod of bracket 8, reaches side opening 12 apart from the distance of crucible bottom
To requirement, closing of housing 11 closes the valve 2 of 1 road of inertia gas cylinder, opens vacuum pump 4, to being vacuumized inside shell 11,
Extract the air of the inside out, it is oxygen-free environment that vacuum degree, which drops to 1mmHg, and the boiling point of Mg is 605 DEG C at this time, lower than the fusing point of beryllium
1287 DEG C, heating temperature is 1327 DEG C, is higher than about 50 DEG C of beryllium fusing point, and the average evaporation rate of impurity is 30mg/S at this time, is fallen
Time is 0.37 second average.Metallic beryllium is heated to up to after fusing point, is kept+50 DEG C of fusing point of volatilization temperature, is formed after melting sources
Metallic beryllium melt 9 breaks through the package of oxidation film at crucible side opening 12, forms drop 14 under the effect of gravity, under the drippage of side opening 8
Come, during drippage, volatile impurity zinc gasifies form metallic vapour rapidly, and 14 surface of drop will not in oxygen-free environment
New oxidation film is formed, the smooth volatilization in drip process of the zinc inside beryllium is detached from molten drop, and most of metallic vapour is along pumping
Feed channel 5 enters dust-extraction unit 3, completes cooling and gathers dust, in order to avoid impurity enters vacuum pump 2, condenses in 11 inner wall of shell on a small quantity
On, the condensate in 11 inner wall of periodic cleaning shell and dust-extraction unit 3 is needed, non-volatile part falls into product crucible 15 and obtains
Beryllium is refined, and keeps liquid, wherein micro volatile impurity can also further volatilize, until raw material water clock finishes, in beryllium
The micro Mg in portion not only in drip process volatilization be detached from molten drop, into residue crucible after can also volatilize at a slow speed, raw material
Mg content drop to 0.001wt%, impurity summation drops to 0.28wt%, reaches Be-1 grades of requirements.6 bottom of raw material crucible is protected
Deposit a large amount of beryllium oxide fragments 13 of Multiple depositions.
After traditional vacuum volatilization purifies Drain time same as Example 2, the mass percent of the Mg of raw material contains
Amount drops to 0.95 wt%, and the mass percentage content of impurity summation drops to 0.13 wt%, belongs to 98.8 wt% grades
Be。
Claims (3)
1. a kind of method of refining of metallic beryllium, which is characterized in that in oxygen-free environment, the beryllium pearl containing impurity is heated, heating
Temperature need to be higher than the fusing point of beryllium and the boiling point of impurity, form drop after the fusing of beryllium pearl and emerge and drip from the side wall aperture of eminence crucible
It falls, during drippage, impurity element volatilization obtains refining beryllium；Adjustable support (8) length for adjusting raw material crucible can
To change the distance between crucible (d) up and down, changes the fall time of drop, that is, change the volatilization time of impurity.
2. the method for refining of metallic beryllium according to claim 1, which is characterized in that impurity is in the beryllium pearl containing impurity
Zn, Mg, K, Li, Pb, one or more of.
3. used device in the method for refining of metallic beryllium described in claim 1, which is characterized in that inertia gas cylinder (1), shutdown
Valve (2), side-wall hole crucible crucible (6) and product crucible (15) separate up and down, and side-wall hole crucible (6) side wall is provided with one
Above through hole (12), the outer diameter of side-wall hole crucible crucible (6) are less than the internal diameter of product crucible (15), side-wall hole crucible
Right above the product crucible (15), side wall aperture (12) precipitates for storing apart from crucible bottom 1-60mm crucible (6)
Beryllium oxide fragment.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811058307.1A CN109182786B (en) | 2018-09-11 | 2018-09-11 | Method and device for preparing high-purity metal beryllium by volatilizing oxygen-free impurities |
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| CN201811058307.1A CN109182786B (en) | 2018-09-11 | 2018-09-11 | Method and device for preparing high-purity metal beryllium by volatilizing oxygen-free impurities |
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| CN113059154A (en) * | 2021-04-12 | 2021-07-02 | 钢研晟华科技股份有限公司 | Preparation method of metallic beryllium bead and metallic beryllium ingot |
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| CN113059154B (en) * | 2021-04-12 | 2022-09-16 | 钢研晟华科技股份有限公司 | Preparation method of metallic beryllium bead and metallic beryllium ingot |
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| CN109182786B (en) | 2021-12-24 |
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