CN209052750U - A kind of thermal dissociation reactor - Google Patents
A kind of thermal dissociation reactor Download PDFInfo
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- CN209052750U CN209052750U CN201821561189.1U CN201821561189U CN209052750U CN 209052750 U CN209052750 U CN 209052750U CN 201821561189 U CN201821561189 U CN 201821561189U CN 209052750 U CN209052750 U CN 209052750U
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Abstract
The utility model relates to a kind of thermal dissociation reactor and its purifies the method for thick beryllium powder ingot and prepare the mode of ultra-high purity metal beryllium, the thermal dissociation reactor includes containing iodine furnace, low-temp reaction device and high-temperature reactor, the Sheng iodine furnace to be connected to the low-temp reaction device；The low-temp reaction device is connected to the high-temperature reactor.Purify thick beryllium powder ingot with the thermal dissociation reactor, steps are as follows: thick beryllium powder and iodine being allowed to react in the thermal dissociation reactor, the mass ratio of thick beryllium powder and iodine is 5:1, generate beryllium iodide steam, thermal dissociation is decomposed into metallic beryllium and iodine vapor, collection obtains pure beryllium powder, and the pure beryllium powder is smelted into beryllium ingot in electron beam furnace.A kind of thermal dissociation reactor configuration of the utility model is reasonable, and assembly is simple, easy to use, purifies thick beryllium powder ingot using the thermal dissociation reactor, easy to operate, saves medicament, energy conservation and environmental protection is at low cost, the very high purity of beryllium.
Description
Technical field
The utility model relates to metallic beryllium purification field more particularly to a kind of thermal dissociation reactors.
Background technique
Beryllium is a kind of material that performance is more special, its certain performances especially nuclearity can be other with physical property
What metal material is irreplaceable.The density of beryllium is low, than 6 times that elasticity modulus is at least other any metals, light weight, just
Degree is big, and thermal property is good, has the excellent properties such as high-melting-point, high specific heat, high heat conductance and suitable coefficient of thermal expansion, and sound passes
It is all faster than other metals to broadcast speed.Therefore, the application range of beryllium be concentrated mainly on nuclear industry, weapon system, aerospace industry,
The fields such as X-ray instrument, electronic information, automobile industry, household electrical appliance.With gradually going deep into for research, application range
There are also expand trend.As a kind of strategic key material, a kind of pair of war has the basic strategic materials of turning meaning,
Beryllium is the mark post of national a national defence comprehensive strength and war industry development level.In civil field, beryllium is " core metal age "
Laurel.
Although the importance of beryllium be it is so significant, its technical threshold is very high, especially ultra-high purity metal beryllium, generation
Only country, one, the U.S. can produce 99.99% a small amount of metallic beryllium in boundary.They technically bottle up, any one state
Family, is all unable to get this ultra-high purity metal beryllium, only one, the U.S. exclusively enjoys.One only can be produced there are three country in the world at present
As purity 99% metallic beryllium, i.e. the U.S., China, Kazakhstan (left factory, the former Soviet Union).It is reacted according to relevant information,
Due to domestic product not high pure metal beryllium, and national defence, military project and some civilian high-end industry especially need, thus it is annual only
Well from imported from America part metals beryllium.This situation makes the national defense industry in China and military high-end manufacturing industry by very big system
About.And the high-end metallurgical technology for the superb metallic beryllium that the U.S. is grasped by them, monopolize beryllium market and words in the world
Language power.So preparing high ultra-high purity metal beryllium, for the monopolization for breaking the U.S., the Defence business in the China that runs business into strong one improves the army in China
Thing is horizontal, has very big realistic meaning.
It is industrially often used beryllium oxide at present and ammonium acid fluoride reacts and ammonium fluoberyllate is made, calcium carbonate soln, peroxide is added
Changing lead solution, ammonium polysulfide etc. makes other impurities, Mn2+Ion, CrO2 -Ion and other heavy metal precipitations are precipitated, and in vacuum
Under the conditions of condensing crystallizing, reheat decomposition prepare beryllium fluoride, then prepare metallic beryllium again.This process is various, tediously long, equipment
More, energy consumption is big, and at high cost, the impurity of introducing is more, and cleaning, the drug used is more, and production efficiency is low, the fluorine that heat resolve generates
Changing ammonium also will cause environmental pollution.
Utility model content
First technical problem to be solved in the utility model is to provide a kind of thermal dissociation reactor, the reactor configuration
Rationally, assembly is simple, purifies thick beryllium powder ingot using the thermal dissociation reactor, easy to operate, need to only control the amount of reaction raw materials
It is to collect the beryllium purified with the temperature for matching and containing iodine furnace, low-temp reaction device and high-temperature reactor, easy to use, behaviour
Make simply, to save medicament, energy conservation and environmental protection is at low cost, and the purity of beryllium can reach 99.999% and provide condition.
Second technical problem to be solved in the utility model is to provide a kind of using the thick beryllium of thermal dissociation reactor purifying
The method of powder ingot, the thermal dissociation reactor configuration that this method uses is reasonable, and assembly is simple, pure using the thermal dissociation reactor
Change thick beryllium powder ingot, easy to operate, amount and the proportion and Sheng iodine furnace, low-temp reaction device and high temperature that need to only control reaction raw materials are anti-
The temperature of device is answered to collect the beryllium purified, easy to use, easy to operate, to save medicament, energy conservation and environmental protection is at low cost,
The purity of beryllium can reach 99.999% and provide condition.
Third technical problem to be solved in the utility model is to provide a kind of mode for preparing ultra-high purity metal beryllium, this
The thermal dissociation reactor configuration that kind method uses is reasonable, and assembly is simple, and the thermal dissociation reactor is used to purify thick beryllium powder ingot, behaviour
The temperature made the amount that simply need to only control reaction raw materials and match and contain iodine furnace, low-temp reaction device and high-temperature reactor
The beryllium purified is collected, easy to use, easy to operate, to save medicament, energy conservation and environmental protection is at low cost, and the purity of beryllium can reach
99.999% provides condition.
In order to solve above-mentioned first technical problem, the utility model provides a kind of thermal dissociation reactor, the heat from
Solution reactor includes containing iodine furnace, low-temp reaction device and high-temperature reactor, the Sheng iodine furnace to be connected to the low-temp reaction device；It is described
Low-temp reaction device is connected to the high-temperature reactor.
The beneficial effects of the utility model are: iodine becomes steam in the Sheng iodine furnace, it is anti-that iodine vapor enters the low temperature
Device, and thick beryllium powder reaction is answered to generate beryllium iodide steam, beryllium iodide steam rises to high-temperature reactor from low-temp reaction device, in high temperature
Under the conditions of thermal dissociation occur generate metallic beryllium and iodine vapor, collection obtains pure beryllium powder.The reactor configuration is reasonable, and assembly is simple,
Thick beryllium powder ingot is purified using the thermal dissociation reactor, it is easy to operate, it need to only control the amount of reaction raw materials and match and contain iodine
The temperature of furnace, low-temp reaction device and high-temperature reactor is to collect the beryllium purified, easy to use, easy to operate, to save
Medicament, energy conservation and environmental protection is at low cost, and the purity of beryllium can reach 99.999% and provide condition.
Further, the first thermocouple is equipped in the Sheng iodine furnace；The entrance of the low-temp reaction device and the Sheng iodine furnace
Outlet；The entrance of the low-temp reaction device passes through porcelain tube and the outlet for containing iodine furnace；In the low-temp reaction device
Equipped with the second thermocouple；The outlet of the entrance of the high-temperature reactor and the low-temp reaction device；The high-temperature reactor
Entrance be connected to the outlet of the low-temp reaction device by iodine vapor hole；Third thermocouple is equipped in the high-temperature reactor.
It is using above-mentioned further beneficial effect: contains iodine furnace, low-temp reaction device and high-temperature reactor and heat respectively, pass through
Different power supply control, can accurately control the flowing of beryllium iodide steam and iodine vapor.
Further, it is equipped in the Sheng iodine furnace and contains iodine basin；Helium tube is provided with above the Sheng iodine basin；The helium tube
The entrance of the first valve control helium is equipped with the junction for containing iodine furnace；The low-temp reaction device passes through first partition and institute
It states and contains the isolation of iodine furnace；Stainless steel frame and Stainless steel basin are equipped in the low-temp reaction device；The Stainless steel basin is for holding thick beryllium
Powder；The material of the Stainless steel basin is 80% nickel and 20% evanohm；The high-temperature reactor passes through second partition and institute
State the isolation of low-temp reaction device；The first partition and the material of the second partition are ceramics；It is equipped in the high-temperature reactor
Cylinder；The Sheng iodine furnace, the low-temp reaction device, the high-temperature reactor are isolated from the outside with metal plate；The metal plate
Material is NI-Cr alloy；It is filled in the metal plate with heating bar；The metal plate external application insulating layer sealing；The insulating layer
The sealing of external application common brick layer；The insulating layer is externally provided with master switch；The master switch controls the power supply of entire reaction system.
Be using above-mentioned further beneficial effect: rationally, assembly is simple for construction, is easily installed, disassembles and maintains.
The high-temperature reactor is connect with cooler bin；The outlet of the high-temperature reactor connects with the entrance of the cooler bin
It is logical；The outlet of the high-temperature reactor is connected with the entrance of the cooler bin by pipeline；It is connected to the high-temperature reactor and institute
The pipeline for stating cooler bin is equipped with the second valve；Liquid reserve tank is connected with immediately below the cooler bin；The liquid reserve tank passes through pipeline
It is connected to the underface of the cooler bin；The side of the liquid reserve tank is connected with vacuum pump, and junction is equipped with third valve；It is described
Vacuum pump is also connected with the side for containing iodine furnace, and junction is equipped with the 4th valve.
Be using above-mentioned further beneficial effect: iodine vapor is cooling in the cooler bin, the product in the liquid reserve tank
Gather and crystallized for high-purity iodine, content is 99.99% or more, and iodine is not revealed, do not volatilize, and it is anti-can to be pumped back to low temperature by vacuum
Answering device, the reaction was continued, and almost without loss, recovery utilization rate is high, is recycled, and saves medicament, and energy conservation and environmental protection is at low cost.
Further, the cylinder has 2-3 root, for bearing the adherency of pure beryllium powder；The cylinder respectively hang on top
On hook；Tungsten wire is equipped in the cylinder；The material of the cylinder is NI-Cr alloy；Every diameter 20cm of the cylinder, it is long
80cm bears to be less than or equal to 20 kilograms of metallic beryllium powder adherency.
Be using above-mentioned further beneficial effect: cylinder done using nickel-chromium alloy, can with high temperature resistant, and will not with iodine,
Beryllium reaction, guarantees the purity of beryllium.
In order to solve above-mentioned second technical problem, the utility model provides a kind of thermal dissociation reactor and purifies
The method of thick beryllium powder ingot purifies thick beryllium powder using the thermal dissociation reactor, is smelted into beryllium ingot；The thick beryllium powder ingot of purifying
Method include the following steps: that the raw material includes thick beryllium powder and iodine step 1: preparing raw material；The thick beryllium powder and the iodine
Mass ratio be 5:1；Step 2: the thick beryllium powder and iodine is allowed to react in the thermal dissociation reactor, beryllium iodide steam is generated,
Thermal dissociation is decomposed into metallic beryllium and iodine vapor, and collection obtains pure beryllium powder；Step 3: the pure beryllium powder is smelted into beryllium ingot；Second
Walking the step of thick beryllium powder and iodine react in the thermal dissociation reactor includes: that the Stainless steel basin is put into the stainless steel
On frame；The thick beryllium powder is filled in the Stainless steel basin；The thickness of the thick beryllium powder is filled in the Stainless steel basin in 30-
50mm；The Sheng iodine basin is put into the Sheng iodine furnace；The iodine is added in the Sheng iodine basin；Start the vacuum pump, makes vacuum
Degree maintains 0.05pa；Connect the Sheng iodine furnace power supply, heat temperature raising makes iodine become steam, iodine vapor by the porcelain tube into
Enter the low-temp reaction device；The low-temp reaction device power supply is connected, heat temperature raising allows the thick beryllium powder and the iodine vapor in institute
It states and is reacted in low-temp reaction device, generate beryllium iodide steam；When the beryllium iodide steam occurs in the low-temp reaction device, institute is connected
State high-temperature reactor power supply, heat temperature raising；When the beryllium iodide steam appears in the high-temperature reactor, open described in connection
Second valve of cooler bin and the high-temperature reactor, the beryllium iodide steam thermal dissociation are decomposed into metallic beryllium and iodine vapor, from
The iodine vapor after solution pours in cooler bin, starts the cycle over flowing；When the iodine vapor thins out, the thick remaining nothing of beryllium powder
What time, reaction terminates, and closes power supply, stops heating, and collection obtains pure beryllium powder；The stopping heating being cooled to furnace temperature and drops to
350 DEG C or less；The method for obtaining pure beryllium powder of collecting is: the cylinder removed, the beryllium being adhered on barrel is scraped with scraper,
Obtain pure beryllium powder；The scraper is sharp stainless steel knife.Iodine becomes steam in the Sheng iodine furnace, and iodine vapor enters described low
Warm reactor, and thick beryllium powder reaction generate beryllium iodide steam, and beryllium iodide steam rises to high-temperature reactor from low-temp reaction device,
Hot conditions issue heat dissociation and generate metallic beryllium and iodine vapor, and collection obtains pure beryllium powder.
The beneficial effects of the utility model are: the thermal dissociation reactor configuration that this method uses is reasonable, assembly is simple, makes
Purify thick beryllium powder ingot with the thermal dissociation reactor, need to only control the amount of reaction raw materials and matches and contain iodine furnace, low-temp reaction
The temperature of device and high-temperature reactor is to collect the beryllium purified, easy to use, easy to operate, to save medicament, energy-saving ring
It protects, at low cost, the purity of beryllium can reach 99.999% and provide condition.
Further, heat temperature raising first rises to 300 DEG C with 20 DEG C/min in the low-temp reaction device, and constant temperature 30 is kept to divide
Clock, then 500 DEG C are risen to 20 DEG C/min；Heat temperature raising elder generation gradient type is warming up to 500 DEG C in the high-temperature reactor, keeps permanent
Temperature 30 minutes, then 500 DEG C are risen to, it is kept for constant temperature 30 minutes, then rise to 1100 DEG C.
It is using above-mentioned further beneficial effect: this heating mode is taken, for the first time in use, needing to reactor
It is dried, is allowed to dry more thoroughly, bottom line reduces moisture content, to ensure the vacuum degree of stove.
Further, the reaction step that pure beryllium powder is smelted into beryllium ingot described in third step includes: step 1: the pure beryllium powder is sent
Into electron beam furnace；The vacuum degree of the electron beam furnace is 0.05pa；The molten speed of the electron beam furnace is
30g/ minutes；The ratio electric energy of the electron beam furnace is 0.6kg/kw.h；The pure beryllium powder is sent to electronics by vibration pusher
In beam smelting furnace；Step 2: the electron beam furnace is powered, the pure beryllium powder is fused into beryllium melt by electron gun；Third
Step: the beryllium melt flows in ingot mould, and beryllium ingot is solidified as after a period of time；The material of the ingot mould is beryllium oxide；Step 4: leading
Spindle blade is pulled, deflates, takes out the beryllium ingot；Step 5: bis- melting of Pi Ding is obtained the beryllium ingot of two meltings；It is described
The method of two meltings is that the beryllium ingot is sent in electron beam furnace, is powered, and melting again obtains the beryllium of two meltings
The beryllium melt of melt, two melting flows in the ingot mould, and the beryllium ingot of two meltings is obtained after a period of time；Step 6:
The impurity for removing the beryllium ingot surface of two melting, obtains ultra-high purity metal beryllium ingot, and purity is 99.999% or more.
It is using above-mentioned further beneficial effect: further increases the purity of metallic beryllium.Carry out electron-beam smelting it
Before, the purity of metallic beryllium can only achieve 99.99%, and the impurity of the inside is mainly the gases such as oxygen, nitrogen, hydrogen, these impurity and beryllium
Affinity is very powerful.With electron-beam smelting, under high temperature thermodynamic activity, these foreign gases can be decomposed out, molten in beryllium
Change drips, and to being solidified as in this of short duration period of beryllium ingot, these foreign gases are all not incorporated into metallic beryllium, to realize
The purity of metallic beryllium is increased to 99.999% or more by the target completely to deaerate.
In order to solve above-mentioned third technical problem, the utility model provides a kind of side for preparing ultra-high purity metal beryllium
Formula, including following method:
The method for preparing beryllium fluoride；
The method for preparing thick beryllium powder；
The method for purifying thick beryllium powder ingot.
The method of the thick beryllium powder ingot of purifying is the method for purifying thick beryllium powder ingot as elucidated before.
The beneficial effects of the utility model are: the thermal dissociation reactor configuration that this method uses is reasonable, assembly is simple, makes
Purify thick beryllium powder ingot with the thermal dissociation reactor, it is easy to operate, need to only control the amount of reaction raw materials and match and contain iodine furnace,
The temperature of low-temp reaction device and high-temperature reactor is to collect the beryllium purified, easy to use, easy to operate, to save medicine
Agent, energy conservation and environmental protection is at low cost, and the purity of beryllium can reach 99.999% and provide condition.
The method for preparing beryllium fluoride includes the following steps:
Step 1: preparing raw material, the raw material includes beryllium hydroxide and hydrofluoric acid；
Beryllium fluoride material is made step 2: the raw material is heated；
Step 3: beryllium fluoride crystal grain is made in the beryllium fluoride drying materials；
Step 4: crushing the beryllium fluoride crystal grain, beryllium fluoride powder is obtained, is saved.
The beneficial effects of the utility model are: this method prepares beryllium fluoride, the impurity of simple process, introducing is few, production
Efficiency is higher than traditional handicraft, and obtained product purity is high, and energy saving, and processing cost is low.
Based on the above technical solution, the utility model can also do following improvement.
Further, the purity of the beryllium hydroxide is big or equal to 99.8%；The mass fraction of the hydrofluoric acid is 40%.
Further, the hydrogen that purity is big or the quality and mass fraction of the beryllium hydroxide equal to 99.8% are 40%
The mass ratio of fluoric acid is 11:28.
Further, the heating means are: the heating raw material being poured into closed after reactor.
Further, the reactor is enamel reaction still.
Further, starting vacuum pump vacuumizes after the enamel reaction still is closed, until the stirring that is powered after vacuum degree 0.05Pa；
Heating is powered on after the energization stirring, and beryllium fluoride material is made.
Further, described to power on heating and be first warming up to 90 DEG C, starting vacuum pump will add thermogenetic steam to be extracted into instead
It answers in the fluid reservoir outside kettle.
Further, described to be powered stirring to power on the blender in starting reaction kettle and being stirred.
Further, the time of the stirring that is powered is 20-45 minutes.
Further, the heating raw material becomes stopping heating when thick colloidal beryllium fluoride material, makes the beryllium fluoride
Material cooling；The beryllium fluoride material is down to 40-50 DEG C.
Be using above-mentioned further beneficial effect: above-mentioned reaction condition is the parameter through testing, and can be guaranteed
Reaction is gone on smoothly.
Further, the furnace drying method is: opening the discharge gate of the enamel reaction still bottom, is taken with stainless steel support basin Sheng
The beryllium fluoride material obtained, is placed in drying box, closes the door, and beryllium fluoride crystal grain is made in electrified regulation；The stainless steel support
Basin inner lining polypropylene plate；Shelf is done with stainless steel material inside the drying box, shelf is divided into multilayer, and stainless steel support basin is just placed in
On shelf.
Be using above-mentioned further beneficial effect: beryllium fluoride has certain corrosivity, uses polypropylene board can be with corrosion resistant
Erosion, and heat-resisting to 200 DEG C, prevent erosion stainless steel from dragging basin.
Further, the beryllium fluoride material stops heating after becoming dry beryllium fluoride crystal grain, makes the beryllium fluoride crystal grain
Cooling；The beryllium fluoride crystal grain is down to 40-50 DEG C.
Further, the breaking method is: taking out stainless steel and drags basin, the beryllium fluoride crystal grain is poured into stainless steel pulverizer
It is crushed, obtains beryllium fluoride powder.
It is using above-mentioned further beneficial effect: carries out the beryllium fluoride powder that physical crushing obtains, be conducive to preparing
When the next step of ultra-high purity metal beryllium prepares thick beryllium powder, increase response area, makes to contact between raw material more sufficiently, react more equal
It is even.
Further, the store method is: beryllium fluoride powder loading woven bag being tightened sack and is saved；The braiding
Bag has plastic inner lining.
It is using above-mentioned further beneficial effect: the smashed beryllium fluoride powder knitting bagged for having plastic inner lining
It is good, and prick into sack, it is to avoid aoxidizing to reduce material and contact with air.
Further, starting vacuum pump vacuumizes after the drying box is closed the door, until electrified regulation after vacuum degree 0.05Pa.
It is using above-mentioned further beneficial effect: is dried under vacuum conditions, avoids beryllium oxide material from aoxidizing, no
It will affect and prepare the next step of ultra-high purity metal beryllium and prepare the reaction of thick beryllium powder.
Further, the drying is first warming up to 50 DEG C, is kept for constant temperature 30 minutes, then be warming up to 90 DEG C, and constant temperature 30 is kept to divide
Clock, then rise to 120 DEG C remain to dry materials until.
Be using above-mentioned further beneficial effect: beryllium oxide material just starts to be colloidal when drying, and water content is high, institute
To be first warming up to 50 DEG C, moisture is made slowly to volatilize, is conducive to drying box gas vent and vapor is discharged in time, vapor is avoided to dry
Condensation falls on beryllium fluoride material and influences quality of material in dry case.
The method for preparing thick beryllium powder includes the following steps:
Step 1: preparing reduction raw material, the reduction raw material includes beryllium fluoride and magnesium metal；
A material blob of slag is made step 2: the reduction raw material is heated；
Step 3: being crushed the material blob of slag, beryllium pearl and magnesium fluoride bits are isolated；
Step 4: crushing the beryllium pearl, thick beryllium powder is made.
The beneficial effects of the utility model are: this method prepares thick beryllium powder, can single reduction whole beryllium fluoride, section
Can be environmentally friendly, reduction rate is high, and straight gyrus yield greatly improves, and the time is short, at low cost in addition to the drug that magnesium separately adds without other.
Based on the above technical solution, the utility model can also do following improvement.
Further, the beryllium fluoride is with powdered addition；The magnesium metal is added with bulk.
Using above-mentioned further beneficial effect is: beryllium fluoride can be such that beryllium fluoride sufficiently participates in instead with powdered addition
It answers, improves beryllium fluoride reduction rate；Magnesium metal is added with bulk, and coarse granule advantageously reduces the violent intensity of reaction, facilitates control temperature
Degree.
Further, the mass ratio of the beryllium fluoride and magnesium metal is 60:31.
Be using above-mentioned further beneficial effect: the mass ratio of the beryllium fluoride and magnesium metal is the ginseng through testing
Number, can either guarantee that reduction reaction sufficiently carries out, and can control reaction speed, guarantee production safety.
Further, the method for the reduction raw material heating is heating reduction method；The heating reduction method is: by the reduction
Reduction furnace is added in raw material, closes the door, and electrified regulation heating agglomerates molten metal beryllium and magnesium fluoride and floats to furnace charge surface,
Mold is injected, is in pie after cooling, obtains a material blob of slag, the overall recovery of beryllium is 98%；The reduction furnace starts true after closing the door
Empty pumping vacuum, until electrified regulation heats up after vacuum degree 0.05Pa；The method of the electrified regulation heating is first gradient type heating
It to 650 DEG C, is kept for constant temperature 30 minutes, then be warming up to 750 DEG C, is kept for constant temperature 30 minutes, then be warming up to 800 DEG C and kept for 60 minutes,
It is warming up to 1000 DEG C again to be kept for 30 minutes, then is warming up to 1300 DEG C and is kept for 20 minutes；The reduction furnace is the high frequency of power 100kw
Furnace；The reduction furnace internal-lining is graphite crucible；The reduction furnace is having a size of 450mm.
Be using above-mentioned further beneficial effect: control gradient type heating, the reaction that each stage occurs is most suitable
Under the conditions of carry out, guarantee to react fully progresss while production safety, making metallic beryllium and magnesium metal, all thawings, metallic beryllium obtain
To be condensed into beryllium pearl and float on fluorination Serum Magnesium.
Further, the method for being crushed the material blob of slag is: the material blob of slag being broken into fritter with stainless steel hammer.
It is using above-mentioned further beneficial effect: carries out physics and be crushed rather than crush, convenient for separation beryllium pearl and fluorination
Magnesium bits.
Further, the separation method is: the fritter described in hot water digestion, is screened, is separated using sieve after digestion
Beryllium pearl and magnesium fluoride bits；The container that the hot water digestion uses is enamel reaction still；The temperature of the hot water digestion is 100
℃；The temperature of the hot water digestion is 1h；The process of the hot water digestion is with stirring.
It is using above-mentioned further beneficial effect: by sieve by the different beryllium pearl of density, granular size and magnesium fluoride
Bits screening separation.
Further, the breaking method is: the beryllium pearl that third step obtains is sent into airslide disintegrating mill and is crushed, cold soaking
After wash to neutrality, drying obtains thick beryllium powder；The beryllium pearl cleans drying before being sent into airslide disintegrating mill；The beryllium pearl is sent into gas
Nitrogen is filled with as protective gas before stream pulverizer；The beryllium pearl is sent into airslide disintegrating mill and is crushed to granular size < 1mm；It is described
The immersion liquid that cold soaking uses is concentrated nitric acid；The time of the cold soaking is 10-15 minutes；The washing methods is quick using pure water
Washing；The furnace drying method that the beryllium pearl crushes after cold soaking washing is placed in Stainless steel basin drying.
Using above-mentioned further beneficial effect is: making protective gas with nitrogen, metallic beryllium can be prevented to be oxidized.
Further, the beryllium fluoride can be recycled, and include the following steps: (1) by the isolated magnesium chloride slag
Sub and described plus thermogenetic flue dust is placed in enamel reaction still；The enamel reaction still is polypropylene material；(2) to described anti-
It answers and hydrofluoric acid is added in kettle, heat up digestion, obtains filter residue and filtrate；(3) it takes the filter residue to clean to dry, obtains dry fluorination
Magnesium；(4) beryllium oxide thick slurry is obtained after taking the filtrate to purify, reduction feedstock circulation is prepared into and uses.
It is using above-mentioned further beneficial effect: beryllium fluoride is recycled, improves the rate of recovery of beryllium.
Further, filters pressing after the heating digestion, digestion again after filters pressing, obtains filter residue and filtrate；The heating digestion
Time be every time 1.5 hours.
Be using above-mentioned further beneficial effect: two digestions improve leaching rate.
Further, the hydrofluoric acid mass fraction is 40%；The hydrofluoric acid is added to liquid pH value less than 0.5；It is described
If magnesium chloride bits and acidity in the digestion process of the flue dust are thin out, addition hydrofluoric acid is supplemented, allows its pH value less than 0.5.
Be using above-mentioned further beneficial effect: pH value remains less than 0.5, and the concentration of hydrofluoric acid is made to reach dissolution beryllium
Needed for grain, beryllium is dissolved in guarantee.
Further, the filtrate purification method is that calcium carbonate is added, and is stirred while adding, until pH value reaches mistake after 6.5-7
Filter, imurity-removal are added enamel reaction still and are concentrated, obtain beryllium oxide thick slurry.
Be using above-mentioned further beneficial effect: the filtrate has participated in impurity during processing, therefore carbon is added
Sour calcium, a part of impurity become carbon dioxide spilling, remaining is filtered to remove after generating oxidation calcium precipitate.
Further, the flue dust is collected into bagroom from the escape pipe of the reduction furnace by venturi-type eductors
In.
Be using above-mentioned further beneficial effect: the magnesium-reduced process of beryllium fluoride can generate some flue dust, easy to damp, Yi Jie
Flue dust is collected into bagroom by block by venturi from the escape pipe of reduction furnace, is made to keep cleaning in furnace, is collected into
Beryllium fluoride is recycled, and magnesium fluoride recycles, and improves the rate of recovery of beryllium, environmental protection and saving.
Detailed description of the invention
Fig. 1 is the mode flow chart that the utility model prepares ultra-high purity metal beryllium.
Fig. 2 is a kind of method flow diagram for preparing beryllium fluoride of the utility model.
Fig. 3 is a kind of method flow diagram for preparing thick beryllium powder of the utility model.
Fig. 4 is a kind of method flow diagram for purifying thick beryllium powder ingot of the utility model.
Fig. 5 is a kind of thermal dissociation structure of reactor schematic diagram of the utility model.
In attached drawing, parts list represented by the reference numerals are as follows:
1 cooler bin, 2 liquid reserve tanks, 3 vacuum pumps, 4 master switch, 5 hooks, 6 common brick layers, 7 insulating layers, 8 cylinders, 9 heating bars,
10 third thermocouples, 11 metal plates, 12 tungsten wires, 13 high-temperature reactors, 14 iodine vapor holes, 15 Stainless steel basins, 16 thick beryllium powder, 17
Two thermocouples, 18 porcelain tubes, 19 first thermocouples, 20 helium tubes, 21 Sheng iodine basins, 22 low-temp reaction devices, 23 Sheng iodine furnaces, 24 first
Valve, 25 second valves, 26 third valves, 27 the 4th valves, 28 second partitions, 29 first partitions.
Specific embodiment
The principles of the present invention and feature are described below, example is served only for explaining the utility model, and
It is non-to be used to limit the scope of the utility model.
As shown in Figure 1, a kind of mode for preparing ultra-high purity metal beryllium of the utility model, including following method:
The method for preparing beryllium fluoride；
The method for preparing thick beryllium powder；
The method for purifying thick beryllium powder ingot.
As shown in Fig. 2, the specific synthesis of the beryllium fluoride can be prepared by following steps:
Step 1: preparing raw material, the raw material includes beryllium hydroxide and hydrofluoric acid；
Beryllium fluoride material is made step 2: the raw material is heated；
Step 3: beryllium fluoride crystal grain is made in the beryllium fluoride drying materials；
Step 4: crushing the beryllium fluoride crystal grain, beryllium fluoride powder is obtained, is saved.
The purity of the beryllium hydroxide is big or equal to 99.8%；
The mass fraction of the hydrofluoric acid is 40%；
Purity is greatly or the quality of the beryllium hydroxide equal to 99.8% is 44kg, the hydrogen fluorine that mass fraction is 40%
The quality of acid is 112kg.
The heating means are: the heating raw material poured into closed after reactor, power on heating after the stirring that is powered,
Beryllium fluoride material is made；
The reactor is enamel reaction still；
Starting vacuum pump vacuumizes after the enamel reaction still is closed, until the stirring that is powered after vacuum degree 0.05Pa；
It is described to be powered stirring to power on the blender in starting reaction kettle, stir material under vacuum conditions
It mixes；
The time of the stirring that is powered is 20-45 minutes；
Preferably, the energization mixing time is 30 minutes.
Described to power on heating and be first warming up to 90 DEG C, starting vacuum pump will add thermogenetic steam to introduce outside reaction kettle
Cooler bin is condensed into water, along in water pipe injection fluid reservoir.
The heating raw material becomes stopping heating when thick colloidal beryllium fluoride material (about 2h), makes the beryllium fluoride
Material cooling.
The beryllium fluoride material is down to 40-50 DEG C.
The furnace drying method is: opening the discharge gate of the enamel reaction still bottom, is taken with stainless steel support basin Sheng obtained
The beryllium fluoride material, is placed in drying box, closes the door, and beryllium fluoride crystal grain is made in electrified regulation；
The stainless steel support basin inner lining polypropylene plate；
The support basin of the polypropylene material, constitution size can install material preferably can be put into vacuum oven, preferably
, the long 500mm of polypropylene magazine, wide 400mm, the high 200mm are rectangle, and 5 support basins install beryllium fluoride.
Shelf is done with stainless steel material inside the drying box, shelf is divided into multilayer, stainless steel support basin be just placed in shelf it
On.Be packed into drying box drags basin, point five layers of placement, between layers distance 100mm.
Starting vacuum pump vacuumizes after the drying box is closed the door, until electrified regulation after vacuum degree 0.05Pa；
The drying is first warming up to 50 DEG C, is kept for constant temperature 30 minutes, then be warming up to 90 DEG C, is kept for constant temperature 30 minutes, then rise
Until 120 DEG C remain to dry materials.
The beryllium fluoride material stops heating after becoming dry beryllium fluoride crystal grain, and the beryllium fluoride crystal grain is made to cool down.
The beryllium fluoride crystal grain is down to 40-50 DEG C.
Material after drying is colourless crystal grain, has part knot tying, is crushed.
The breaking method is: taking out stainless steel and drags basin, the beryllium fluoride crystal grain is poured into stainless steel pulverizer and carries out powder
It is broken, obtain beryllium fluoride powder.
The store method is: beryllium fluoride powder loading woven bag being tightened sack and is saved.
Packaging will seal, to prevent becoming damp, totally 50 kilograms of beryllium fluoride siccative.
The woven bag has plastic inner lining.
As shown in figure 3, the specific synthesis of the thick beryllium powder can be prepared by following steps:
Step 1: preparing reduction raw material, the reduction raw material includes beryllium fluoride and magnesium metal；
A material blob of slag is made step 2: the reduction raw material is heated；
Step 3: being crushed the material blob of slag, beryllium pearl and magnesium fluoride bits are isolated；
Step 4: crushing the beryllium pearl, thick beryllium powder is made.
In the first step, the beryllium fluoride is with powdered addition；
The magnesium metal is added with bulk；
The mass ratio of the beryllium fluoride and magnesium metal is 60:31；
The quality of the beryllium fluoride is 60kg, and the quality of the magnesium metal is 31kg.
60kg beryllium fluoride powder is encased in graphite crucible, 31kg metal MAG block is then added, is stirred with clean sticking plaster
It mixes, mixes.
In second step, the method for the reduction raw material heating is heating reduction method；
The heating reduction method is: reduction furnace is added in the reduction raw material, is closed the door；The reduction furnace is power 100kw
Coreless induction furnace；The reduction furnace internal-lining is graphite crucible；The reduction furnace is having a size of 450mm；The reduction furnace starts after closing the door
Vacuum pump vacuumizes, until electrified regulation heats up after vacuum degree 0.05Pa；Electrified regulation heating, initial temperature slowly heat up, and work as temperature
When degree rises to 650 DEG C, allows it at this temperature section constant temperature 30 minutes, is then further continued for being warming up to 750 DEG C, and temperature half an hour,
Furnace temperature is directly risen to 800 DEG C later, keeps the constant temperature 60 minutes, this temperature section material reduction reaction is most fierce.Wait react
After, and furnace temperature is risen to 1300 DEG C, under this condition of high temperature, metallic beryllium and magnesium metal all melt, meanwhile, metallic beryllium obtains
With cohesion, since its density ratio magnesium fluoride is small, so agglomerating after beryllium pearl, all to float on fluorination Serum Magnesium；The gold of fusing
After category beryllium and magnesium fluoride agglomerate and float to furnace charge surface, mold is injected rapidly, and cooling after half an hour is in pie, obtains material slag
Cake, the overall recovery of beryllium are 98%；Heating furnace is vacuum high-frequency furnace, power 50kw.
Note that material should not once be added too much, too many beryllium fluoride and magnesium metal cannot be added, to control exothermic energy
And reaction speed.Its amount is restored each time preferably no more than 70 kilograms of beryllium fluoride, by operating procedure correct operation.
In third step, the method for being crushed the material blob of slag is: being broken into the material blob of slag with stainless steel hammer small
Block；
The separation method is: with fritter described in hot water digestion, screened after digestion using sieve, isolated beryllium pearl and
Magnesium fluoride bits；The container that the hot water digestion uses is enamel reaction still；The enamel reaction still is polypropylene material；It is described
The temperature of hot water digestion is 100 DEG C；The temperature of the hot water digestion is 1h；The process of the hot water digestion is with stirring.Not yet
The beryllium fluoride of reduction is dissolved into water, and magnesium fluoride is not soluble in water and beryllium pearl is retained in slag together.
According to broken bits block diameter size, gone over first with 80 mesh sieve sieve.It is trapped in object on compass screen surface all
It is beryllium pearl, the material across sieve pore is mostly magnesium fluoride, is partially the finer beryllium pearl of particle.When second screens
150 mesh sieve are chosen, screened material is mostly magnesium fluoride, and metallic beryllium is seldom, and particle is also very thin, stays on compass screen surface
Material be mostly beryllium pearl.In order to preferably separate this partial material, and it is poured into plastic tub, is added a little clear
Water is washed by rubbing with the hands with stainless steel brush, the impurity for attaching to beryllium bead surface is rubbed with the hands take off as far as possible, last to sieve again with 150 mesh sieve,
Part above beryllium pearl is stayed in, first of beryllium pearl screened is added, the part material of sieving is added to the object of magnesium fluoride
In material.
In 4th step, the breaking method is: the beryllium pearl that third step obtains is sent into airslide disintegrating mill and is crushed, cold
Washing to neutrality, drying obtains thick beryllium powder after leaching；The beryllium pearl is sent into airslide disintegrating mill and is crushed to granular size < 1mm；It is described
Beryllium pearl cleans drying before being sent into airslide disintegrating mill；The beryllium pearl is filled with nitrogen as protective gas before being sent into airslide disintegrating mill, prevents
Only it is oxidized；The beryllium powder that impact grinding obtains is polygon, and purity is relatively high, is then cleaned drying；The cold soaking makes
Immersion liquid is concentrated nitric acid；The time of the cold soaking is 10-15 minutes, during which for several times with sticking plaster agitation；The washing methods
To use pure water quick wash；The furnace drying method that the beryllium pearl crushes after cold soaking washing is placed in Stainless steel basin drying.
The beryllium fluoride can be recycled, and include the following steps:
(1) the isolated magnesium chloride bits and described plus thermogenetic flue dust are placed in enamel reaction still；Institute
It states flue dust and is collected into bagroom from the escape pipe of the reduction furnace by venturi-type eductors；
(2) hydrofluoric acid is added in Xiang Suoshu reaction kettle, heat up digestion, filters pressing, and digestion again after filters pressing obtains filter residue and filter
Liquid；The hydrofluoric acid mass fraction is 40%；The hydrofluoric acid is added to liquid pH value less than 0.5；It is described heating digestion when
Between be every time 1.5 hours；If the magnesium chloride bits and acidity in the digestion process of the flue dust are thin out, to supplement and hydrogen fluorine is added
Acid allows its pH value less than 0.5；
So through secondary digestion, the amount containing beryllium of flue dust and bits is lower than 0.1%, and leaching rate is higher than 98%；
(3) it takes the filter residue to clean to dry, obtains dry magnesium fluoride；It is cleaned and is dried, then packed, with to be vended；
(4) beryllium oxide thick slurry is obtained after taking the filtrate to purify, reduction feedstock circulation is prepared into and uses；But the inside has been mixed
Enter some impurity, it is necessary to it is purified, the filtrate purification method is that calcium carbonate is added, it stirs while adding, is heated to 80 DEG C,
A few hours are stood after sixty minutes, allow impurity natural subsidence to be separated by solid-liquid separation until pH value filters after reaching 6.5-7, imurity-removal adds
Enter the enamel reaction still to be concentrated, be added in the enamel reaction still, electrified regulation evaporates dense to 90 DEG C after vacuumizing
Contracting, until becoming thick beryllium oxide thick slurry；Discharge gate is opened, is drawn off, magnesium-reduced process is sent to be restored.
In the method for the thick beryllium powder ingot of the purifying, first set up thermal dissociation reactor, as shown in figure 5, include contain iodine furnace 23,
Low-temp reaction device 22 and high-temperature reactor 13, the Sheng iodine furnace 23 are connected to the low-temp reaction device 22；The low-temp reaction device
22 are connected to the high-temperature reactor 13.Thick beryllium powder 16 reacts in the low-temp reaction device 22 with iodine vapor, generates beryllium iodide
Steam.Beryllium iodide steam rises to high-temperature reactor 13 from low-temp reaction device 22, and thermal dissociation occurs under the high temperature conditions, dissociation
For metallic beryllium and iodine vapor.
The high-temperature reactor 13 is connect with cooler bin 1；The underface of the cooler bin 1 is connected with liquid reserve tank 2；It is described
The side of liquid reserve tank 2 is connected with vacuum pump 3；The vacuum pump 3 is also connected with the side for containing iodine furnace 23.It is anti-in the high temperature
It answers the iodine vapor dissociated in device 13 to be stored in the liquid reserve tank 2 through the cooler bin 1 cooling, it is anti-to return to the low temperature again
It answers device 22 and crude beryllium powder to react again, synthesizes beryllium iodide, under the driving of concentration difference and temperature difference, and ascension is to the high temperature
Reactor 13, the cycle goes on, until crude beryllium powder is clean by reaction.Iodine is not revealed, and is not volatilized, and is not had theoretically
It is lossy, but still have seldom some loss when practical operation.First crude beryllium powder is disposed, and it is thick to add new a batch
Beryllium powder and iodine processed, continue to purify.
The first thermocouple 19 is equipped in the Sheng iodine furnace 23；The entrance of the low-temp reaction device 22 and the Sheng iodine furnace 23
Outlet；The second thermocouple 17 is equipped in the low-temp reaction device；The entrance and the low temperature of the high-temperature reactor 13 are anti-
Answer the outlet of device 22；The outlet of the entrance of the high-temperature reactor 13 and the low-temp reaction device 22 passes through iodine vapor hole 14
Connection；Third thermocouple 10 is equipped in the high-temperature reactor 13.Iodine furnace, low-temp reaction device and high-temperature reactor is contained to add respectively
Heat is controlled by different power supplys, the accurate flowing for controlling beryllium iodide steam and iodine vapor.
It is equipped in the Sheng iodine furnace 23 and contains iodine basin 21；The top for containing iodine basin 21 is provided with helium tube 20；The helium
Pipe 20 and the junction for containing iodine furnace 23 are equipped with the entrance of the first valve 24 control helium；The low-temp reaction device 22 passes through the
One partition 29 is isolated with the Sheng iodine furnace 23；The entrance of the low-temp reaction device 22 passes through porcelain tube 18 and the Sheng iodine furnace 23
Outlet；Stainless steel frame and Stainless steel basin 15 are equipped in the low-temp reaction device；The Stainless steel basin 15 is for holding thick beryllium
Powder 16；The high-temperature reactor 13 is isolated by second partition 28 with the low-temp reaction device 22；In the high-temperature reactor 13
Equipped with cylinder 8；The cylinder 8 has 2-3 root, for bearing the adherency of pure beryllium powder；The cylinder 8 respectively hang on the hook of top
On 5；Tungsten wire 12 is equipped in the cylinder 8；The Sheng iodine furnace 23, the low-temp reaction device 22, the gold of the high-temperature reactor 13
Belong to plate 11 to be isolated from the outside；It is filled in the metal plate 11 with heating bar 9；11 external application insulating layer 7 of the metal plate sealing；It is described
The sealing of 7 external application common brick layer 6 of insulating layer；The insulating layer 7 is externally provided with master switch 4；The master switch 4 controls entire reaction system
Power supply；The outlet of the high-temperature reactor 13 is connected to the entrance of the cooler bin 1；The outlet of the high-temperature reactor 13 with
The entrance of the cooler bin 1 is connected by pipeline；The pipeline for being connected to the high-temperature reactor 13 and the cooler bin 1 is equipped with the
Two valves 25；The liquid reserve tank 2 is connected to the underface of the cooler bin 1 by pipeline；The liquid reserve tank and the vacuum pump 3
Junction be equipped with third valve 26；The vacuum pump 3 is equipped with the 4th valve 27 with the junction for containing iodine furnace 23.
The material of the Stainless steel basin 15 is 80% nickel and 20% evanohm；The material of the cylinder 8 is NI-Cr
Alloy；The material of the metal plate 11 is NI-Cr alloy；The first partition 29 and the material of the second partition 28 are pottery
Porcelain.
Cylinder 8 every diameter 20cm, the long 80cm bear to be less than or equal to 20 kilograms of metallic beryllium powder adherency.
As shown in figure 4, purify thick beryllium powder using above-mentioned thermal dissociation reactor, be smelted into the thick beryllium powder of purifying described in beryllium ingot at
Ingot includes the following steps:
Thick beryllium powder 16 is packed into Stainless steel basin 15, then beryllium powder thickness is put into the low-temp reaction device between 30-50mm
Stainless steel frame on；The Sheng iodine basin 21 is added in iodine, the Sheng iodine basin 21 is put into the Sheng iodine furnace 23；
Vacuum pump is opened, so that vacuum degree is maintained 0.05pa, leak rate is less than 1.3 × 10-1Pa.L.S；Connect the Sheng iodine
23 power supply of furnace, heat temperature raising make iodine become steam, and iodine vapor enters the low-temp reaction device 22 by the porcelain tube 18；
The power supply of the low-temp reaction device 22 is connected, heat temperature raising, initial temperature raising speed is slow, rises with 20 DEG C per minute
Speed, a straight grip temperature are raised to 300 DEG C, then at this temperature section constant temperature 30 minutes, are further continued for heating up, just no longer rise to 500 degree
Temperature, and this temperature is kept until reaction terminates；
When beryllium iodide steam occurs in the low-temp reaction device 22, the power supply heating for connecting the high-temperature reactor 13 adds
Heat, constant temperature 30 minutes when rising to 500 DEG C, when being raised again to 800 DEG C, and constant temperature 30 minutes, 1100 degree are then risen to, this temperature is kept
Degree, until work terminates；
When beryllium iodide steam slowly rise to the high-temperature reactor 13 when, vacustat 0.05pa premise
Under, it opens into a small amount of helium, allows it to carry more beryllium iodides and enter the high-temperature reactor 13.1 He of cooler bin is also opened simultaneously
Second valve 25 of the high-temperature reactor 13 allows the iodine vapor after dissociation to pour in the cooler bin 1, starts the cycle over flowing；
The input amount of helium, it is initial smaller, but when beryllium iodide steam gradually increases, helium also increases intake therewith,
So the size of its intake, be it is directly proportional with beryllium iodide quantity of steam, adjusted according to the size of beryllium iodide vapor volume；
Because the reaction of beryllium and iodine is slower, the time needed for reaction is long, and this time operation works continuously 30
A hour；
When the iodine vapor thins out, and the thick beryllium powder 16 remains little, reaction terminates, and closes power supply, stops adding
Heat is cooled to furnace temperature and drops to 350 DEG C hereinafter, remove the cylinder 8, scraped and be adhered on barrel with sharp stainless steel spatula
Beryllium, collection obtain pure beryllium powder.
It is purified by the thermal dissociation of iodine, metallic beryllium purity up to 99.99%, send electronic beam vacuum smelting, further purifies.
The pure beryllium powder is sent in furnace by vibration pusher, and the disconnecting switch of power turn-on cabinet, vacuum system is spaced apart, and 10 seconds
Manual indicator light is bright within clock, then opens the vacuum meter on instrument power cabinet, system pump down is carried out, then in power turn-on cabinet
It " pays high-voltage filament to be spaced apart " ", close again " main high pressure is spaced apart ", the DC power supply opened in instrument power cabinet carries out melting, electron gun
The pure beryllium powder is fused into beryllium melt, the beryllium melt being melted drips in ingot mould down, more than 30 minutes have been spent, melt solidification,
Beryllium ingot is cast, dummy bar is pulled, deflates, takes out the beryllium ingot；
Notice that the vacuum degree of stove keeps 0.05pa when melting, melts about 30g/ minutes per minute of speed, the electron beam is molten
The ratio electric energy of furnace is 0.6kg/kw.h.
The beryllium ingot of first of melting is done into second melting, the beryllium ingot is sent in electron beam furnace, is powered, again
Melting obtains the beryllium melt of two meltings, and the beryllium melt of two melting flows in the ingot mould, and two are obtained after a period of time
The beryllium ingot of road melting；The impurity for removing the beryllium ingot surface of two melting, obtains ultra-high purity metal beryllium ingot, and purity is
99.999% or more.
After two electron-beam smeltings, metallic beryllium impurity content is (%):
Aluminium < 2 × 10-4；
Carbon < 3 × 10-4；
Hydrogen < 0.3 × 10-4；
Molybdenum < 2 × 10-4；
Copper < 1 × 10-4；
Iron < 1 × 10-4；
Nitrogen < 2 × 10-4；
Oxygen < 5 × 10-4；
Nickel < 4 × 10-4；
Silicon < 1 × 10-4；
Titanium < 3 × 10-4；
Metallic beryllium purity > 99.999%.
Above-described embodiment is only used for illustrating the design of the utility model, rather than to the limit of the utility model rights protection
Fixed, all non-essential modifications to the present invention made by this concept should all fall into the protection scope of the utility model.
Claims (4)
1. a kind of thermal dissociation reactor, which is characterized in that the thermal dissociation reactor includes containing iodine furnace (23), low-temp reaction device
(22) it is connected to high-temperature reactor (13), the Sheng iodine furnace (23) with the low-temp reaction device (22)；The low-temp reaction device
(22) it is connected to the high-temperature reactor (13).
2. thermal dissociation reactor according to claim 1, which is characterized in that be equipped in the Sheng iodine furnace (23) and contain iodine basin
(21) and the first thermocouple (19)；
Helium tube (20) are provided with above the Sheng iodine basin (21)；
The helium tube (20) and the junction for containing iodine furnace (23) are equipped with the entrance of the first valve (24) control helium；
The low-temp reaction device (22) is isolated by first partition (29) with the Sheng iodine furnace (23)；
The entrance of the low-temp reaction device (22) passes through porcelain tube (18) and the outlet for containing iodine furnace (23)；
The second thermocouple (17), stainless steel frame and Stainless steel basin (15) are equipped in the low-temp reaction device；
The Stainless steel basin (15) is for holding thick beryllium powder (16)；
The high-temperature reactor (13) is isolated by second partition (28) with the low-temp reaction device (22)；
The entrance of the high-temperature reactor (13) is connected to the outlet of the low-temp reaction device (22) by iodine vapor hole (14)；
Third thermocouple (10), cylinder (8) are equipped in the high-temperature reactor (13)；
The cylinder (8) has 2-3 root, for bearing the adherency of pure beryllium powder；
The cylinder (8) respectively hang on the hook (5) of top；
Tungsten wire (12) are equipped in the cylinder (8)；
The Sheng iodine furnace (23), the low-temp reaction device (22), the high-temperature reactor (13) with metal plate (11) and it is extraneous every
From；
The interior heating bar of the metal plate (11) (9) filling；
Metal plate (11) external application insulating layer (7) sealing；
Insulating layer (7) external application common brick layer (6) sealing；
The insulating layer (7) is externally provided with master switch (4)；
The master switch (4) controls the power supply of entire reaction system；
The high-temperature reactor (13) connect with cooler bin (1)；
The outlet of the high-temperature reactor (13) is connected with the entrance of the cooler bin (1) by pipeline；
The pipeline for being connected to the high-temperature reactor (13) and the cooler bin (1) is equipped with the second valve (25)；
Liquid reserve tank (2) are connected with immediately below the cooler bin (1)；
The liquid reserve tank (2) is connected to the underface of the cooler bin (1) by pipeline；
The side of the liquid reserve tank (2) is connected with vacuum pump (3), and junction is equipped with third valve (26)；
The vacuum pump (3) is also connected with the side for containing iodine furnace (23), and junction is equipped with the 4th valve (27).
3. thermal dissociation reactor according to claim 2, which is characterized in that the material of the Stainless steel basin (15) is 80%
Nickel and 20% evanohm；
The material of the cylinder (8) is NI-Cr alloy；
The material of the metal plate (11) is NI-Cr alloy；
The material of the first partition (29) and the second partition (28) is ceramics.
4. thermal dissociation reactor according to claim 2, which is characterized in that described every diameter 20cm of cylinder (8), it is long
80cm bears to be less than or equal to 20 kilograms of metallic beryllium powder adherency.
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| CN109097602A (en) * | 2018-09-25 | 2018-12-28 | 陆世强 | A kind of method of thermal dissociation reactor and its thick beryllium powder ingot of purifying and the mode for preparing ultra-high purity metal beryllium |
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| CN109097602B (en) * | 2018-09-25 | 2021-03-26 | 陆世强 | Thermal dissociation reactor, method for purifying coarse beryllium powder into ingot and method for preparing ultra-high-purity metal beryllium |
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