CN106756052A - The Rapid recovery device and technique of a kind of uranium zircaloy chip - Google Patents
The Rapid recovery device and technique of a kind of uranium zircaloy chip Download PDFInfo
- Publication number
- CN106756052A CN106756052A CN201710021877.2A CN201710021877A CN106756052A CN 106756052 A CN106756052 A CN 106756052A CN 201710021877 A CN201710021877 A CN 201710021877A CN 106756052 A CN106756052 A CN 106756052A
- Authority
- CN
- China
- Prior art keywords
- chip
- uranium zircaloy
- uranium
- zircaloy
- recovery device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 119
- 229910001093 Zr alloy Inorganic materials 0.000 title claims abstract description 119
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 238000011084 recovery Methods 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 99
- 238000002844 melting Methods 0.000 claims abstract description 46
- 230000008018 melting Effects 0.000 claims abstract description 46
- 239000005439 thermosphere Substances 0.000 claims abstract description 16
- 238000001953 recrystallisation Methods 0.000 claims abstract description 15
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- DJOYTAUERRJRAT-UHFFFAOYSA-N 2-(n-methyl-4-nitroanilino)acetonitrile Chemical compound N#CCN(C)C1=CC=C([N+]([O-])=O)C=C1 DJOYTAUERRJRAT-UHFFFAOYSA-N 0.000 claims abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000919 ceramic Substances 0.000 claims abstract description 4
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 4
- 238000003723 Smelting Methods 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- NBWXXYPQEPQUSB-UHFFFAOYSA-N uranium zirconium Chemical compound [Zr].[Zr].[U] NBWXXYPQEPQUSB-UHFFFAOYSA-N 0.000 claims description 4
- MYDJEUINZIFHKK-UHFFFAOYSA-N 1,1,2-trichloroethane-1,2-diol Chemical compound OC(Cl)C(O)(Cl)Cl MYDJEUINZIFHKK-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 description 26
- 238000007499 fusion processing Methods 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000001965 increasing effect Effects 0.000 description 5
- 238000013461 design Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000006698 induction Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229960002415 trichloroethylene Drugs 0.000 description 2
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 206010068052 Mosaicism Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000000289 melt material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 210000003765 sex chromosome Anatomy 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
- C22B7/003—Dry processes only remelting, e.g. of chips, borings, turnings; apparatus used therefor
-
- 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
-
- 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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0208—Obtaining thorium, uranium, or other actinides obtaining uranium preliminary treatment of ores or scrap
-
- 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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0213—Obtaining thorium, uranium, or other actinides obtaining uranium by dry processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Geology (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses the Rapid recovery device and technique of a kind of uranium zircaloy chip, the Rapid recovery device is used cooperatively with microwave high-temperature high vacuum furnace, the Rapid recovery device includes heating crucible, muff and the auxiliary thermosphere being filled between the heating crucible and muff, wherein, heating crucible is made up of recrystallization SiC ceramics and inner surface is coated with calcium zirconate coating, and muff is by Al2O3It is made, auxiliary thermosphere is by ZrO2Particle or recrystallization SiC piece are constituted.The quick recovery process of the uranium zircaloy chip then carries out the recovery of uranium zircaloy chip using the Rapid recovery device of above-mentioned uranium zircaloy chip.The present invention can obviously reduce heating using power and will reduce more than half the time required to melting compared with other melting modes and device, therefore can reduce the waste of the energy, reduce the pollution caused in uranium zircaloy removal process.
Description
Technical field
The invention belongs to metallurgical technical field, more particularly, it is related to a kind of quick recovery of uranium zircaloy chip to fill
Put and technique.
Background technology
It has the features such as excellent nuclearity energy, high-melting-point, corrosion resistance to uranium zircaloy, is that the fuel can of nuclear reactor is excellent
Material selection.
Can produce the radwastes such as more chip in uranium zircaloy process, cause a large amount of wastes of raw material with
And the pollution to environment, based on induction melting, equipment operationally consumes substantial amounts of energy for the recovery of uranium bits both at home and abroad at present,
Meeting generating material and energy waste in fusion process, and there is security risk sex chromosome mosaicism.
In recent years, microwave melting with firing rate it is fast, the process time is short, energy consumption is low, it is small to environmental hazard the advantages of cause
The extensive concern of people.
The content of the invention
In order to solve above technological deficiency, the present invention is intended to provide one kind using microwave melting to carry out uranium zircaloy chip fast
Device and technique that speed is reclaimed.
An aspect of of the present present invention provides the Rapid recovery device of uranium zircaloy chip, the Rapid recovery device and microwave
High temperature high vacuum furnace is used cooperatively, and the Rapid recovery device includes heating crucible, muff and is filled in the heating crucible
Auxiliary thermosphere between muff, wherein, the heating crucible is made up of recrystallization SiC ceramics and inner surface is coated with calcium zirconate
Coating, the muff is by Al2O3It is made, the auxiliary thermosphere is by ZrO2Particle or recrystallization SiC piece are constituted.
One embodiment of Rapid recovery device according to uranium zircaloy chip of the present invention, the muff include sleeve and
Top cover, thermometer hole is provided with the top cover.
One embodiment of Rapid recovery device according to uranium zircaloy chip of the present invention, the internal diameter of the heating crucible with
The ratio of wall thickness is 12:1~10:1, the thickness of the calcium zirconate coating is 0.05~0.15mm.
One embodiment of Rapid recovery device according to uranium zircaloy chip of the present invention, the external diameter of the heating crucible with
The ratio of the internal diameter of muff is 1:1.5~1:2.
One embodiment of Rapid recovery device according to uranium zircaloy chip of the present invention, the packed height of the auxiliary thermosphere
Flushed with the top of heating crucible, the ZrO2The granularity of particle is 2~10mm, and the thickness of recrystallization SiC piece is 5~15mm.
Another aspect provides a kind of quick recovery process of uranium zircaloy chip, using above-mentioned uranium zircaloy
The Rapid recovery device of chip carries out the recovery of uranium zircaloy chip.
One embodiment of quick recovery process according to uranium zircaloy chip of the present invention, including the chip for carrying out successively is clear
Wash, shove charge, melting and come out of the stove；
It is higher than 5 × 10 in vacuum in the step of melting-2Microwave melting is carried out under the vacuum condition of Pa, including it is following
Sub-step：
Control heating power increases to maximum heating power Y with the speed of Y/10~Y/4W/min；
The maximum heating power Y is kept, until the temperature of uranium zircaloy chip reaches TIt is molten；
After uranium zircaloy chip is completely melt, control heating power is reduced to 0.6Y~0.8Y, is incubated 10~30min,
It is cooled to after room temperature to come out of the stove and obtains uranium zircaloy ingot；
Wherein, TIt is moltenIt is the fusing point of uranium zircaloy chip, DEG C；Y is maximum heating power, W；The internal diameter Ф of Y and heating crucible1
(mm) ratio is 10:1~100:1.
One embodiment of quick recovery process according to uranium zircaloy chip of the present invention, in the step of chip is cleaned,
The chip of uranium zircaloy is carried out to clean and after the washing by uranium using three passage cleaning ways of buck, trichloro ethylene, alcohol
Zircaloy chip is pressed into uranium zircaloy chip group after drying；In the step of shove charge, uranium zircaloy chip group is loaded fast
In the heating crucible of fast retracting device, Rapid recovery device is put into microwave high-temperature high vacuum furnace, is vacuumized after closing stove.
One embodiment of quick recovery process according to uranium zircaloy chip of the present invention, in the step of coming out of the stove, treats uranium
After zircaloy ingot is cooled to room temperature, it is passed through dry clean air and treats that vacuum is less than 5 × 103Vacuumized again after Pa, treat vacuum
Dry clean air is passed through again after reaching 10~100Pa, and so uranium zircaloy ingot is taken out in blow-on after 2~5 times repeatedly.
One embodiment of quick recovery process according to uranium zircaloy chip of the present invention, smelting temperature room temperature~
(0.6-0.7)TIt is moltenPreceding continuous improvement heating power, (0.6-0.7) TIt is molten~TIt is moltenKeep heating power constant, uranium zircaloy after fusing
The temperature of chip is maintained at 1.05TIt is molten~1.1TIt is molten。
The present invention carries out melting recovery to the chip of uranium zircaloy using microwave heating, and the rate of heat addition is fast, molten with other
Refining mode is compared with device, be can obviously reduce heating using power and will be reduced more than half the time required to melting, therefore can subtract
The waste of few energy, reduces the pollution caused in uranium zircaloy removal process.Additionally, present invention design is simple, with good
Heating and heat-insulating property, heating crucible, auxiliary thermosphere and muff materials are easy, and preparation price is relatively low, the resistance to urgency in fusion process
Cold anxious heat, security is preferable.The melting that the inventive method and device can not only meet uranium zircaloy chip is reclaimed, and is also applied for it
The waste recovery and alloying smelting of his metal material, with the wider scope of application.
Brief description of the drawings
Fig. 1 shows the structure of the Rapid recovery device of uranium zircaloy chip according to an illustrative embodiment of the invention
Schematic diagram.
Fig. 2 shows the knot of the Rapid recovery device of the uranium zircaloy chip according to another exemplary embodiment of the invention
Structure schematic diagram.
Description of reference numerals：
10- heating crucibles, 20- muffs, 21- sleeves, 22- top covers, 23- thermometer holes, the auxiliary thermospheres of 30-, 31-ZrO2
Grain, 32- recrystallization SiCs piece, 40- uranium zircaloy chips.
Specific embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine by any way.
Any feature disclosed in this specification, unless specifically stated otherwise, can be equivalent or with similar purpose by other
Alternative features are replaced.I.e., unless specifically stated otherwise, each feature is an example in a series of equivalent or similar characteristics
.
Heating using microwave has potential engineer applied valency as a kind of mode of heating of clean environment firendly in Metal Melting field
Value.In traditional melting mode, the mode of heating of material based on heat transfer, thermal convection current and heat radiation, the efficiency of heating surface it is low and
Substantial amounts of energy waste can be caused, heating using microwave is different from conventional method from principle, it is in microwave field by dielectric material
In polarization loss carry out overall heating, heat results from material internal rather than from external heat source, therefore fusion process
In can obtain intensification efficiency higher, material homogeneous heating and microwave heating equipment simple structure, can significantly reduce and put
Pollution problem during penetrating property material recovery.But, due to metallic reflection microwave (under normal temperature microwave in a metal penetrate depth
Degree is only 1~10 μm), it is therefore desirable to by carrying out the research and development and rational technological design of special purpose device, can just make such as uranium zirconium
The microwave melting of the metals such as alloy chip is possibly realized.
The present invention is directed to the particularity of uranium Zirconium alloy material and improves the aspects such as smelting efficiency, devises for uranium zircaloy
Device and technique that chip is quickly reclaimed, be both remarkably improved the melting organic efficiency of uranium zircaloy chip, it is also possible to reduce special
The environmental pollution caused in material removal process.
Uranium zircaloy chip of the present invention is the strip or broken produced in the machining process of uranium zircaloy part
Chip scrap.
The structure and principle first to the Rapid recovery device of uranium zircaloy chip of the present invention are described in detail below.
Fig. 1 shows the structure of the Rapid recovery device of uranium zircaloy chip according to an illustrative embodiment of the invention
Schematic diagram, Fig. 2 shows the knot of the Rapid recovery device of the uranium zircaloy chip according to another exemplary embodiment of the invention
Structure schematic diagram.
As illustrated in fig. 1 and 2, exemplary embodiment of the invention, the Rapid recovery device of the uranium zircaloy chip
Used cooperatively with microwave high-temperature high vacuum furnace, i.e., uranium zirconium is carried out together with microwave high-temperature high vacuum furnace by the Rapid recovery device
The recovery melting of alloy cutting.
Specifically, the Rapid recovery device includes heating crucible 10, muff 20 and is filled in heating crucible 10 with insulation
Set 20 between auxiliary thermosphere 30, heating crucible 10 is made up of recrystallization SiC ceramics and inner surface is coated with calcium zirconate coating in case
Only melting material reacts with crucible, and muff 20 is by Al2O3It is made, auxiliary thermosphere 30 is by ZrO2Particle or recrystallization SiC piece group
Into.Wherein, heating crucible 10 is used to contain and melting uranium zircaloy chip, and muff 20 is used to realize protecting in fusion process
Temperature, auxiliary thermosphere 30 then plays the effect that Accelerate Crucible and the chip of uranium zircaloy heat up.
The Rapid recovery device universality of said structure and material is stronger, with good heating and heat-insulating property, heating
Crucible 10, auxiliary thermosphere 30 and muff 20 are drawn materials easily and preparation price is relatively low, the resistance to rapid heat cycle in fusion process, safety
Property preferably, be advantageously implemented the microwave melting of metal.Wherein, the good material of heating crucible selection absorbing property, can make melting
Heating initial stage whole device has heating rate higher；It is good using absorbing property but the heating effect of heating crucible is limited
Auxiliary thermosphere can further improve smelting efficiency；Muff may insure the heating effect of heating crucible and uranium zircaloy chip,
Its requirement is that not only had thermal insulation but also had wave, and microwave may pass through muff and act on heating crucible therein and chip
On.
Wherein, muff 20 includes sleeve 21 and top cover 22, after uranium zircaloy chip 40 is put into heating crucible 10,
Heating crucible 10 is put into the sleeve 21 of muff 20 and follow-up recycling is carried out by top cover 22.Preferably,
Thermometer hole 23 is provided with top cover 22, to facilitate the material to the inside to carry out infrared measurement of temperature.
According to a preferred embodiment of the invention, the internal diameter of heating crucible 10 and the ratio of wall thickness are 12:1~10:1, zirconic acid
The thickness of calcium coating is 0.05~0.15mm；The external diameter of heating crucible 10 is 1 with the ratio of the internal diameter of muff 20:1.5~1:
2；The packed height of auxiliary thermosphere 30 is flushed with the top of heating crucible 10, ZrO2The granularity of particle 31 is 2~10mm, recrystallization
The thickness of SiC pieces is 5~15mm.
Invention also provides the quick recovery process of uranium zircaloy chip, the technique uses above-mentioned uranium zircaloy chip
Rapid recovery device carry out the recovery of uranium zircaloy chip.
Exemplary embodiment of the invention, the quick recovery process includes the chip cleaning for carrying out successively, shove charge, melts
Refine and come out of the stove.Wherein, present invention process it is critical only that in fusion process by under higher vacuum to heating using microwave work(
The regulation and control of rate improve melting organic efficiency and obtain preferable Smelting Effect.
Specifically, it is higher than 5 × 10 in vacuum in the step of melting-2Microwave melting is carried out under the vacuum condition of Pa.Should
Fusion process includes following sub-step：
1) control heating power increases to maximum heating power Y with the speed of Y/10~Y/4W/min.In this sub-step,
Heating power is continuously increased can accelerate fusion process, but increase can not be too big, and otherwise device microwave reflection is more, causes power
Waste.
2) maximum heating power Y is kept, until the temperature of uranium zircaloy chip reaches TIt is molten.Wherein, maximum heating power Y
Size depends on specific melting material, when device and the timing of material one, then Y value determination.
3) after uranium zircaloy chip is completely melt, control heating power is reduced to 0.6Y~0.8Y, and insulation 10~
30min, is cooled to after room temperature to come out of the stove and obtains uranium zircaloy ingot；Preferably, with the rate reduction heating power of 1/2Y~Y.Protecting
During temperature, the temperature of uranium zircaloy chip is maintained at 1.05T after fusingIt is molten~1.1TIt is molten.Because absorbing property becomes after melt material
Well, it is necessary to suitably reduce power to prevent melt intensification too high, wherein, the smelting temperature of material is general more slightly higher than the fusing point of material
Some.
Wherein, TIt is moltenIt is the fusing point of uranium zircaloy chip, DEG C；Y is maximum heating power, W；The internal diameter Ф of Y and heating crucible1
(mm) ratio is 10:1~100:1.
In the fusion process, present invention employs the three-stage load mode of power increase-stabilization-bust, and work as
When the temperature of uranium zircaloy chip is increased to 2/3 temperature of fusing point, its ability for absorbing microwave is remarkably reinforced, can be direct by microwave
Heating and then acquisition smelting efficiency higher and preferable Smelting Effect.Thus, the above-mentioned melting mode rate of heat addition of the invention
Hurry up, can obviously reduce heating and use power, more than half will be reduced the time required to melting, therefore the waste of the energy can be reduced and dropped
The pollution caused during low uranium zircaloy chip recycling.Due to metal microwave reflection at low temperature, it is impossible to by heating using microwave,
Therefore needing to design special frock makes it possible metallic microwave melting.Muff uses material that is adiabatic, not absorbing microwave, temperature
Microwave transparent muff is heated to heating crucible and metal when spending relatively low；Heating crucible is using the ceramic material for caning absorb microwave
Material.The chip of melting initial stage does not absorb microwave, heating using microwave heating crucible and auxiliary hot material, the intensification of uranium zircaloy chip it is main according to
Heat transfer and heat radiation by crucible material, after after temperature rising, metal material absorbs the enhancing of microwave ability, and it can be straight by microwave
Connect and heat and with the efficiency of heating surface higher.
Preferably, in the step of chip is cleaned, using buck, trichloro ethylene, alcohol three passage cleaning ways to uranium
Zircaloy chip is cleaned and is pressed into uranium zircaloy chip group after the chip of uranium zircaloy is dried after the washing.Wherein, alkali
Water may be selected the NaOH aqueous solution of dilution.
In the step of shove charge, uranium zircaloy chip group is fitted into the heating crucible 10 of Rapid recovery device, will be quick
Retracting device is put into microwave high-temperature high vacuum furnace (not shown), is vacuumized (utilize vavuum pump) to vacuum after conjunction stove and is reached 5
×10-2More than Pa.
In the step of coming out of the stove, after uranium zircaloy ingot is cooled to room temperature, it is passed through dry clean air (unlatching vent valve) and treats
Vacuum is less than 5 × 103Vacuumized again after Pa, (unlatching is put to be passed through dry clean air again after vacuum reaches 10~100Pa
Air valve), so uranium zircaloy ingot is taken out in blow-on after 2~5 times repeatedly.Because uranium zircaloy has radioactivity, in melting rear hearth
With the presence of harmful substance, the harmful substance in stove is gone to produce injury to people divided by when avoiding blow-on after vacuum several times is taken out repeatedly.
It should be understood that the above-mentioned implementation method and following examples of present invention detailed description are merely to illustrate the present invention rather than limit
The scope of the present invention processed, some nonessential improvement and tune that those skilled in the art's the above of the invention is made
It is whole to belong to protection scope of the present invention.
The Rapid recovery device and technique of uranium zircaloy chip of the present invention are made furtherly with reference to specific embodiment
It is bright.
Embodiment 1：
The present embodiment carries out the quick of uranium zircaloy chip and returns using shown in Fig. 1 and as described above Rapid recovery device
Receipts treatment, does not repeat structure herein.
Quick recovery process is comprised the following steps：
(1) chip cleaning：Uranium zircaloy (U-0.65Zr) chip is taken, is respectively cleaned successively with buck, trichloro ethylene and alcohol
One time, it is put into after removing surface oil stain and dirt in drying oven and is dried, and clean chip is pressed into 80 × 40mm of Ф with press
Uranium zircaloy chip group.
(2) shove charge：Using Fig. 1 devices, the uranium zircaloy chip group that will be pressed is put into heating crucible, heating crucible it is interior
Footpath Ф1For 80mm and wall thickness are 8mm (i.e. external diameter Ф2It is 96mm), crucible is placed in muff center position, muff internal diameter Ф3For
150mm, ZrO is put into the space between muff and heating crucible2Simultaneously highly be added to and heating crucible top for it by particle
End flushes.Then whole device is put into microwave high-temperature high vacuum furnace, stove is closed and is vacuumized, until vacuum reaches 5 × 10- 2More than Pa.
(3) melting：Microwave power supply is opened, control heating power is increased with the speed of 400W/min, uranium zircaloy chip group
Temperature rise to 850 DEG C of (2/3TIt is molten), the maximum heating power for using is 1800W, keeps power constant after increasing to 1800W, uranium
The temperature of zircaloy chip group continues to raise, the melting temperature until reaching uranium zircaloy, and control adds after material is completely melt
Thermal power is down to 1200W and finely tunes power, and the melting material temperature degree of uranium zircaloy chip group is maintained at 1310 DEG C after fusing
(1.05TIt is molten), after insulation 15min, microwave power is unloaded with the speed of 900W/min.
(4) come out of the stove：After uranium zircaloy ingot is cooled to room temperature, opens vent valve and be passed through a certain amount of dry clean air, treat vacuum
Spend to 5 × 103After Pa, open vavuum pump and vacuumize, after reopened after vacuum to 50Pa vent valve and continuing be passed through it is dry clean
Air, so blow-on obtains uranium zircaloy ingot after 4 times repeatedly.
Embodiment 2：
The present embodiment carries out the quick of uranium zircaloy chip and returns using shown in Fig. 2 and as described above Rapid recovery device
Receipts treatment, does not repeat structure herein.
Quick recovery process is comprised the following steps：
(1) chip cleaning：Uranium zircaloy chip is taken, with respectively cleaning one time of buck, trichloro ethylene and alcohol, surface oil is removed
It is put into after stain and dirt in drying oven and is dried, and clean chip is pressed into the uranium zircaloy chip of 100 × 50mm of Ф with press
Group.
(2) shove charge：Using Fig. 2 devices, the uranium zircaloy chip group that will be pressed is put into recrystallization SiC crucible, heats earthenware
The internal diameter Ф of crucible1For 100mm and wall thickness are 10mm, crucible is placed in muff center position, muff internal diameter Ф3It is 200mm,
Recrystallization SiC piece is put into space between muff and heating crucible, wherein, recrystallization SiC piece is total to two-layer, and thickness in monolayer is
12mm.Whole device is put into microwave high-temperature high vacuum furnace, stove is closed and is vacuumized, until vacuum reaches 5 × 10-2Pa with
On.
(3) melting：Microwave power supply is opened, control heating power is increased with the speed of 600W/min, uranium zircaloy chip group
Temperature rise to 850 DEG C of (2/3TIt is molten), the maximum heating power for using is 2400W, and holding 2400W power is constant, and uranium zircaloy is cut
The temperature of the group of considering to be worth doing continues to raise, the melting temperature until reaching uranium zircaloy, and heating power drop is controlled after material is completely melt
To 1800W and power is finely tuned, the melting material temperature degree of uranium zircaloy chip group is maintained at 1310 DEG C of (1.05T after fusingIt is molten), insulation
After 10min, microwave power is unloaded with the speed of 1200W/min.
(4) come out of the stove：After uranium zircaloy ingot is cooled to room temperature, opens vent valve and be passed through a certain amount of dry clean air, treat vacuum
Spend to 8 × 103After Pa, open vavuum pump and vacuumize, after reopened after vacuum to 20Pa vent valve and continuing be passed through it is dry clean
Air, so blow-on obtains uranium zircaloy ingot after 3 times repeatedly.
In addition, inventor also carries out uranium zircaloy to the chip of conventional induction melting uranium zircaloy and using the present invention program
The experiment parameter of chip melting is contrasted, as a result as shown in table 1.
The conventional induction melting of table 1 is contrasted with the experiment parameter of microwave melting of the present invention
Note：Wherein microwave melting use device 1, concrete technology be embodiment 1 given in, induction melting crucible size with it is micro-
Ripple melting kettle is identical.
As shown in Table 1, the present invention carries out melting recovery, the rate of heat addition using microwave heating to the chip of uranium zircaloy
Hurry up, compared with other melting modes and device, can obviously reduce heating using power and will reduce the time required to melting half with
On, therefore the waste of the energy can be reduced, reduce the pollution caused in uranium zircaloy removal process.
Also, present invention design is simple, with good heating and heat-insulating property, heating crucible, auxiliary thermosphere and muff
Materials are easy, and preparation price is relatively low, and the resistance to rapid heat cycle in fusion process, security is preferable.The inventive method and device are not only
The melting that uranium zircaloy chip can be met is reclaimed, and is also applied for the waste recovery and alloying smelting of other metal materials, is had
The wider scope of application.
The invention is not limited in foregoing specific embodiment.The present invention is expanded to and any in this manual disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (10)
1. a kind of Rapid recovery device of uranium zircaloy chip, it is characterised in that the Rapid recovery device is high with microwave high-temperature
Vacuum drying oven is used cooperatively, and the Rapid recovery device includes heating crucible, muff and is filled in the heating crucible with insulation
Auxiliary thermosphere between set, wherein, the heating crucible is made up of recrystallization SiC ceramics and inner surface is coated with calcium zirconate coating,
The muff is by Al2O3It is made, the auxiliary thermosphere is by ZrO2Particle or recrystallization SiC piece are constituted.
2. the Rapid recovery device of uranium zircaloy chip according to claim 1, it is characterised in that the muff includes set
Cylinder and top cover, thermometer hole is provided with the top cover.
3. the Rapid recovery device of uranium zircaloy chip according to claim 1, it is characterised in that the heating crucible it is interior
Footpath is 12 with the ratio of wall thickness:1~10:1, the thickness of the calcium zirconate coating is 0.05~0.15mm.
4. the Rapid recovery device of uranium zircaloy chip according to claim 1, it is characterised in that the heating crucible it is outer
Footpath is 1 with the ratio of the internal diameter of muff:1.5~1:2.
5. the Rapid recovery device of uranium zircaloy chip according to claim 1, it is characterised in that the filling of the auxiliary thermosphere
Height is flushed with heating crucible, the ZrO2The granularity of particle is 2~10mm, and the thickness of recrystallization SiC piece is 5~15mm.
6. a kind of quick recovery process of uranium zircaloy chip, it is characterised in that using any one of claim 1 to 5
The Rapid recovery device of uranium zircaloy chip carries out the recovery of uranium zircaloy chip.
7. the quick recovery process of uranium zircaloy chip according to claim 6, it is characterised in that including cutting for carrying out successively
Consider cleaning, shove charge, melting to be worth doing and come out of the stove；
It is higher than 5 × 10 in vacuum in the step of melting-2Microwave melting, including following sub-step are carried out under the vacuum condition of Pa
Suddenly：
Control heating power increases to maximum heating power Y with the speed of Y/10~Y/4W/min；
The maximum heating power Y is kept, until the temperature of uranium zircaloy chip reaches TIt is molten；
After uranium zircaloy chip is completely melt, control heating power is reduced to 0.6Y~0.8Y, is incubated 10~30min, cooling
Come out of the stove after to room temperature and obtain uranium zircaloy ingot；
Wherein, TIt is moltenIt is the fusing point of uranium zircaloy chip, DEG C；Y is maximum heating power, W；The internal diameter Ф of Y and heating crucible1(mm)
Ratio be 10:1~100:1.
8. the quick recovery process of uranium zircaloy chip according to claim 7, it is characterised in that the step of chip is cleaned
In, the chip of uranium zircaloy clean and after the washing will using three passage cleaning ways of buck, trichloro ethylene, alcohol
The chip of uranium zircaloy is pressed into uranium zircaloy chip group after drying；In the step of shove charge, the uranium zircaloy chip is rolled into a ball and is loaded
In the heating crucible of Rapid recovery device, Rapid recovery device is put into microwave high-temperature high vacuum furnace, is vacuumized after closing stove.
9. the quick recovery process of uranium zircaloy chip according to claim 8, it is characterised in that in the step of coming out of the stove,
After uranium zircaloy ingot is cooled to room temperature, it is passed through dry clean air and treats that vacuum is less than 5 × 103Vacuumized again after Pa, treat true
Reciprocal of duty cycle is passed through dry clean air again after reaching 10~100Pa, and so uranium zircaloy ingot is taken out in blow-on after 2~5 times repeatedly.
10. the quick recovery process of uranium zircaloy chip according to claim 7, it is characterised in that smelting temperature is in room temperature
~(0.6-0.7) TIt is moltenPreceding continuous improvement heating power, (0.6-0.7) TIt is molten~TIt is moltenKeep heating power constant, uranium zirconium is closed after fusing
The temperature of golden chip is maintained at 1.05TIt is molten~1.1TIt is molten。
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| CN114360758A (en) * | 2021-12-31 | 2022-04-15 | 中核四川环保工程有限责任公司 | Decontamination process for radioactive source tank |
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