CN107502758A - A kind of method for producing high-purity calcium - Google Patents
A kind of method for producing high-purity calcium Download PDFInfo
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- CN107502758A CN107502758A CN201710797488.9A CN201710797488A CN107502758A CN 107502758 A CN107502758 A CN 107502758A CN 201710797488 A CN201710797488 A CN 201710797488A CN 107502758 A CN107502758 A CN 107502758A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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Abstract
This application discloses a kind of method for producing high-purity calcium, comprise the following steps：1) the first rectifying：Thick calcium raw material is placed in the first rectifier unit, first vacuumizes, and carries out multistage backflow at a temperature of being heated first, obtains thick calcium liquid, wherein, multistage backflow, which is at least more than 10 grades, to flow back；2) it is incubated：Thick calcium liquid is added in attemperator, is incubated at a temperature of being heated second；3) the second rectifying：The thick calcium liquid of insulation is added in the second rectifier unit, second is vacuumized, and rectifying is carried out at a temperature of being heated the 3rd, multistage backflow, separates and collects calcium steam, is condensed at a temperature of being heated the 4th, high-purity calcium is obtained, wherein, preferably more than 5 grades of multistage backflow flows back.The method that the application provides, technique is simple, cost is low, pollution-free, is easy to industrial applications.
Description
Technical field
The application is related to metal smelt technical field, more particularly to a kind of method for producing high-purity calcium.
Background technology
Calcium metal has the characteristics such as high elecrtonegativity, chemical property work ripple, in fields such as metallurgy, petrochemical industry, battery powers
It is widely used.High-purity calcium is the reducing agent for preparing many high pure metals and rare earth material, in atomic industry and national defence troops
Work field plays the role of indispensable.In nuclear material uranium, thorium, plutonium is produced, the purity of reducing agent calcium metal directly affects institute
The purity of nuclear material is obtained, and then influences the performance of nuclear component and complete machine.Therefore, it may be either phase to study high pure metal calcium technology of preparing
Close industry and bring economic benefit, also have immeasurable meaning to lifting China's national defense military project strength.At present, it is industrial to prepare
The method of calcium metal is mainly electrolysis and thermal reduction, and electrolysis is high to ingredient requirement, and cost is higher, thermal reduction energy consumption
Height, cost are higher, and electrolysis and the calcium metal purity of thermal reduction production are 99%-99.9%, also need further processing
The calcium metal of higher purity can be obtained.
The content of the invention
In order to solve the above technical problems, the purpose of the present invention is provides a kind of method that rectification under vacuum prepares high-purity calcium, it is raw
Production. art is simple, cost is low, pollution-free, is easy to industrial applications.
Technical scheme provided by the invention is as follows：
A kind of method for producing high-purity calcium, comprises the following steps：
1) the first rectifying：Thick calcium raw material is placed in the first rectifier unit, first vacuumizes, at a temperature of first heats
Multistage backflow is carried out, obtains thick calcium liquid, wherein, multistage backflow, which is at least more than 10 grades, to flow back；
2) it is incubated：Thick calcium liquid is added in attemperator, is incubated at a temperature of being heated second；
3) the second rectifying：The thick calcium liquid of insulation is added in the second rectifier unit, second vacuumizes, in the 3rd heating
At a temperature of carry out rectifying, multistage backflow, separate and collect calcium steam, multistage reflux condensation mode is carried out at a temperature of being heated the 4th,
High-purity calcium is obtained, wherein, preferably more than 5 grades of multistage backflow flows back.
Preferably, the thick calcium raw material is goes back protocalcium, the one or more being electrolysed in calcium.
Preferably, first rectifier unit is externally provided with collection device, collects low boiling impurity at normal temperatures.
Preferably, in the step 1), first, which is evacuated down to vacuum in the first rectifier unit, is less than or equal to 50Pa.
Preferably, in the step 1), the first heating-up temperature is 850-900 DEG C, time 4-5h.
Preferably, in the step 2), the temperature of the second heating is 850-900 DEG C.
Preferably, thick calcium liquid is added in attemperator using the method for siphon, or will be protected using the method for siphon
The thick calcium liquid of temperature is added in the second rectifier unit.
Preferably, in the step 3), second, which is evacuated down to vacuum in the second rectifier unit, is less than or equal to 133Pa.
Preferably, in the step 3), the temperature of the 3rd heating is 1035-1135 DEG C.
Preferably, in the step 3), the temperature of the 4th heating is 842-970 DEG C.
In the present invention, the first rectifier unit, the second rectifier unit can use rectifying furnace, and attemperator can use insulation
Stove.Rectifier unit connects vacuum extractor respectively.Vacuum means can be set to the first rectifier unit, the second rectifier unit respectively
Put, also the first rectifier unit, the second rectifier unit can be connected to same vacuum extractor.First rectifier unit, insulation dress
Put, the connecting place of the second rectifier unit can set valve, control each device to carry out vacuum respectively, also can be true by taking out
Total valve is set at empty device, or by vacuumizing the open and close of power source, controls whole vacuum.
The method that the first distillation process of the present invention is flowed back using multistage, wherein, it is more when thick calcium raw material carries out the first rectifying
Level backflow, which is at least more than 10 grades, to flow back.10 grades of backflows refer to establish 10 grades of refluxes, i.e. reflux most in rectifier unit
10 layers are provided with well, and every layer is designed with being open, and makes the gas that the is evaporated equal repeats condensation of each layer, the process of evaporation again.It is each
The gas that layer is evaporated can be upwardly into another layer, while the liquid and can condensed flows downwardly into rectifier unit bottom.If
Multistage backflow is put, the low boiling impurity in thick calcium raw material can be removed, while ensures that calcium does not evaporate together with low boiling impurity
Come.
Attemperator is set, thick calcium liquid insulating is deposited in attemperator, can be at any time by thick calcium liquid during refining
Add in purifier so that refining process can be carried out continuously.Insulating process, which is not usually required to be passed through inert gas, to be protected
Shield, but when discharge row does not go out, inert gas discharge can be passed through.
The thick calcium liquid of the present invention is carried out in the second distillation process, and calcium steam is collected using the method for multistage backflow, wherein,
Preferably more than 5 grades of multistage backflow flows back.5 grades of backflows set 5 layers of reflux, and every layer is designed with being open, and makes what is be evaporated
Gas is in the equal repeats condensation of each layer, the process of evaporation.The gas that each layer is evaporated can be upwardly into another layer, simultaneously
The liquid and can of condensation to flow down.Multistage backflow is set, can separate with calcium boiling point similar in the impurity such as barium.The boiling point of barium compares calcium
High 70 DEG C or so of boiling point, in the second distillation process, calcium and barium can evaporate together, and because the boiling point of barium is high, barium can be prior to
Calcium condense, the purpose for establishing 5 grades of refluxes be in order to allow barium to condense, and calcium continue up evaporate, both materials due to return
Flow the effect of device and separated, condensed through the multistage isolated calcium steam that flows back into condensing unit, obtain height
Pure calcium.
The process of the present invention, technique is simple, and equipment investment is few, the calcium rate of recovery is high, cost is low, and smelting process is without dirt
Dye, to prepare high-purity calcium new technology.The method of the present invention, can remove the various impurity such as magnesium in calcium, potassium, sodium, aluminium, copper, obtain
High-purity calcium.In the present invention, when pressure is 50Pa, magnesium, potassium, the boiling point of sodium are less than the boiling point of calcium, then in a heated condition, magnesium,
The low-boiling point materials such as sodium, potassium are first evaporated, and by the multistage reflow step of the first rectifying, lower boiling impurity is removed；Then exist
In second distillation process, using the boiling point of calcium less than the high boiling substance such as aluminium, copper, using the method for multistage backflow by thick calcium liquid
In calcium steam separated with other materials, collect condensation, obtain the calcium of high-purity, by size ingot-casting into product, calcium content
More than 99.99%.
Brief description of the drawings
, below will be to embodiment or existing in order to illustrate more clearly of the embodiment of the present application or technical scheme of the prior art
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments described in application, for those of ordinary skill in the art, on the premise of not paying creative work,
Other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the process chart that high-purity calcium is produced in the embodiment of the present invention；
Embodiment
In order that those skilled in the art more fully understand the technical scheme in the application, it is real below in conjunction with the application
The accompanying drawing in example is applied, the technical scheme in the embodiment of the present application is clearly and completely described, it is clear that described implementation
Example only some embodiments of the present application, rather than whole embodiments.It is common based on the embodiment in the application, this area
The every other embodiment that technical staff is obtained under the premise of creative work is not made, it should all belong to the application protection
Scope.
Please be as shown in figure 1, a kind of method for producing high-purity calcium of offer of the embodiment of the present invention, comprises the following steps：
1) the first rectifying：Thick calcium raw material is placed in the first rectifier unit, first vacuumizes, at a temperature of first heats
Multistage backflow is carried out, obtains thick calcium liquid, wherein, multistage backflow, which is at least more than 10 grades, to flow back；
2) it is incubated：Thick calcium liquid is added in attemperator, is incubated at a temperature of being heated second；
3) the second rectifying：The thick calcium liquid of insulation is added in the second rectifier unit, second vacuumizes, in the 3rd heating
At a temperature of carry out rectifying, multistage backflow, separate and collect calcium steam, multistage reflux condensation mode is carried out at a temperature of being heated the 4th,
High-purity calcium is obtained, wherein, preferably more than 5 grades of multistage backflow flows back.
In the present invention, the first rectifier unit, the second rectifier unit can use rectifying furnace, and attemperator can use insulation
Stove.Rectifier unit connects vacuum extractor respectively.Vacuum means can be set to the first rectifier unit, the second rectifier unit respectively
Put, also the first rectifier unit, the second rectifier unit can be connected to same vacuum extractor.First rectifier unit, insulation dress
Put, the connecting place of the second rectifier unit can set valve, control each device to carry out vacuum respectively, also can be true by taking out
Total valve is set at empty device, or by vacuumizing the open and close of power source, controls whole vacuum.
The method that the first distillation process of the present invention is flowed back using multistage, wherein, it is more when thick calcium raw material carries out the first rectifying
Level backflow, which is at least more than 10 grades, to flow back.10 grades of backflows refer to establish 10 grades of refluxes, i.e. reflux most in rectifier unit
10 layers are provided with well, and every layer is designed with being open, and makes the gas that the is evaporated equal repeats condensation of each layer, the process of evaporation again.It is each
The gas that layer is evaporated can be upwardly into another layer, while the liquid and can condensed flows downwardly into rectifier unit bottom.If
Multistage backflow is put, the low boiling impurity in thick calcium raw material can be removed, while ensures that calcium does not evaporate together with low boiling impurity
Come.
Attemperator is set, thick calcium liquid insulating is deposited in attemperator, can be at any time by thick calcium liquid during refining
Add in purifier so that refining process can be carried out continuously.Insulating process, which is not usually required to be passed through inert gas, to be protected
Shield, but when discharge row does not go out, inert gas discharge can be passed through.
The thick calcium liquid of the present invention is carried out in the second distillation process, is separated using the method for multistage backflow and is collected calcium and steamed
Vapour, wherein, preferably more than 5 grades of multistage backflow flows back.5 grades of backflows set 5 layers of reflux, and every layer is designed with being open, and makes steaming
The gas issued is in the equal repeats condensation of each layer, the process of evaporation.The gas that each layer is evaporated can be upwardly into separately
One layer, at the same condense liquid and can to flow down.Multistage backflow is set, can separate with calcium boiling point similar in the impurity such as barium.Barium
70 DEG C higher than the boiling point of calcium or so of boiling point, in the second distillation process, calcium and barium can evaporate together, because the boiling point of barium is high,
Barium can condense prior to calcium, the purpose for establishing 5 grades of refluxes be in order to allow barium to condense, and calcium continue up evaporate, both
Material is separated due to the effect of reflux, and it is cold to enter condensing unit progress through the multistage isolated calcium steam that flows back
It is solidifying, obtain high-purity calcium.
Preferably, the thick calcium raw material is goes back protocalcium, the one or more being electrolysed in calcium.
The thick calcium raw material that the present invention uses includes electrolysis calcium, goes back any one or more in protocalcium.Electrolysis calcium is electrolysis
What fused calcium chloride obtained.Also protocalcium is rectifying to obtain after being reduced with metallic aluminium in 1200 DEG C of vacuum.Be electrolysed calcium and
Also protocalcium main difference is that impurity.Also major impurity is aluminium in protocalcium.It is electrolysed in calcium, calcium chloride can be contained, and come from
Metal in some salts added for reduction calcium chloride fusing point.The method of the present invention, it can be carried out to being electrolysed calcium, going back protocalcium
Purification processes, obtain high-purity calcium.
Preferably, first rectifier unit is externally provided with collection device, collects low boiling impurity at normal temperatures.
In the present invention, collection impurity can be arranged outside the first rectifier unit, collects low boiling impurity for condensing, condensation
Temperature is normal temperature, without especially heating.
Preferably, in the step 1), first, which is evacuated down to vacuum in the first rectifier unit, is less than or equal to 50Pa.
Preferably, in the step 1), the first heating-up temperature is 850-900 DEG C, time 4-5h.
Preferably, in the step 2), the temperature of the second heating is 850-900 DEG C.
Preferably, thick calcium liquid is added in attemperator using the method for siphon, or will be protected using the method for siphon
The thick calcium liquid of temperature is added in the second rectifier unit.
In the present invention, can use siphon method by thick calcium liquid from the first rectifier unit suck attemperator, or from
Attemperator is sucked in the second rectifier unit.According to the method for siphon, then need to set pressure differential between two, it is real
Now transhipment of the thick calcium liquid between different device, into subsequent processing, without providing extra power.Set according to production scene
Put, may also set up pump and power is provided, realize the transhipment between different device of thick calcium liquid.
Can be by unit interval condensation number, to calculate the suitable delivery rate of attemperator, and to attemperator and
Valve between two rectifier units is controlled accordingly.Unit interval condensation number, mainly according to the cooling effectiveness of condensation chamber and
What evaporation efficiency together decided on.In production process, the evaporation capacity of calcium is equal to condensation number.Delivery rate is according to liquid level in rectifier unit
Meter is determined, corresponding liquid level gauge is provided with the second rectifier unit, and when liquid level is low arrives a certain degree, attemperator is to the
Two rectifier units provide material to a certain liquid level.
Preferably, in the step 3), second, which is evacuated down to vacuum in the second rectifier unit, is less than or equal to 133Pa.
Preferably, in the step 3), the temperature of the 3rd heating is 1035-1135 DEG C.
Preferably, in the step 3), the temperature of the 4th heating is 842-970 DEG C.
The process of the present invention, technique is simple, and equipment investment is few, the calcium rate of recovery is high, cost is low, and smelting process is without dirt
Dye, to prepare high-purity calcium new technology.The method of the present invention, can remove the various impurity such as magnesium in calcium, potassium, sodium, aluminium, copper, obtain
High-purity calcium.In the present invention, when pressure is 50Pa, magnesium, potassium, the boiling point of sodium are less than the boiling point of calcium, then in a heated condition, magnesium,
The low-boiling point materials such as sodium, potassium are first evaporated, and by the multistage reflow step of the first rectifying, lower boiling impurity is removed；Then exist
In second distillation process, using the boiling point of calcium less than the high boiling substance such as aluminium, copper, using the method for multistage backflow by thick calcium liquid
In calcium steam and other materials separate and collect condensation, the calcium of high-purity is obtained, by size ingot-casting into product, calcium content
More than 99.99%.
Embodiment 1
Protocalcium is gone back with thick 2 tons of calcium raw material and produces high-purity calcium.It is as shown in the table to reduce calcium component：
Table 1 reduces calcium component table
Boiling point (DEG C) under each material different pressures of table 2
| Element | Ca | B | Si | Ni | Na | Mn | Mg | K | Fe | Al | Cu | Cr | Ba |
| 133Pa | 808 | 2625 | 1665 | 1408 | 439 | 1249 | 602 | 344 | 1790 | 1472 | 1617 | 1695 | 861 |
| 1330Pa | 970 | 2957 | 1910 | 1602 | 550 | 1462 | 723 | 446 | 2045 | 1699 | 1910 | 1922 | 1044 |
1) the first rectifying：1000kg protocalcium of going back is added in the first rectifying furnace, Sealing Arrangement, vacuumizes, is extracted into
Below 50Pa, low boiling impurity is magnesium potassium sodium in raw material, and its content is respectively 1.17%, 0.01% and 0.01%, when temperature control
System 850-900 DEG C carry out 10 grades backflow, 4-5 hours can by magnesium potassium sodium largely remove, remaining magnesium potassium sodium 0.005% with
It is interior.When temperature is 800-850 DEG C, the vapour pressure of calcium, almost without the volatilization of calcium, reaches less than 133Pa and removes magnesium potassium sodium mesh
's.
2) it is incubated：After removing the low boiling impurities such as magnesium potassium sodium, the thick calcium liquid in the first rectifying furnace is sucked by siphon
Into holding furnace, holding temperature is controlled at 850-900 DEG C.Holding furnace can be sucked slightly by valve to control from the first rectifying furnace
The time of calcium liquid and speed, and the delivery rate of thick calcium liquid can be provided by Valve controlling to the second rectifying furnace.
3) the second rectifying：Eliminate low boiling impurity magnesium potassium sodium, go back the remaining impurity of protocalcium be mainly B, Si, Ni, Mn,
Fe, Al, Cu, Cr and Ba, these impurity belong to micro impurity, and are high-boiling-point impurities relative to calcium.In 1330Pa, calcium steams
Hair needs temperature to reach 970 DEG C, and at 1085 DEG C, the vaporization can of calcium reaches the industrialization production requirements of rectifying, and at this
At a temperature of, in addition to barium, the vapour pressure of other impurities is less than 50Pa, and rectification under vacuum process only calcium, barium can form steam, 1085
At a temperature of DEG C, the steam of barium is pressed with 1330Pa, the content of the barium content in high-purity calcium is less than 0.001%, it is necessary to more than 5 grades
Backflow removes barium, the condensation of isolated calcium steam, then can thoroughly remove impurity.The condition of calcium rectification under vacuum, rectification temperature
1035-1135 DEG C, not more than 1200 DEG C.In second distillation process, vacuum pump inlet residual voltage is controlled in below 1000Pa, is kept away
Exempt from residual voltage to have an impact the evaporation efficiency of calcium.The calcium steam that second rectifying furnace is evaporated enters condensing plant.The fusing point of calcium
For 842 DEG C, therefore calcium steam can be condensed into liquid by condensation temperature control at 842~970 DEG C.The high-purity calcium that will be obtained
Liquid presses size ingot-casting into product, calcium content more than 99.99%.
Also protocalcium purifying technique output capacity
Also it is as shown in the table to produce high-purity calcium material balance for the rectifying of protocalcium continuous vacuum：
Also protocalcium rectifying material balance table (based on 100 tons) unit：Ton
Remarks：Input and output rate：96.80%.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (10)
- A kind of 1. method for producing high-purity calcium, it is characterised in that comprise the following steps：1) the first rectifying：Thick calcium raw material is placed in the first rectifier unit, first vacuumizes, and is carried out at a temperature of being heated first Multistage backflow, obtains thick calcium liquid, wherein, multistage backflow, which is at least more than 10 grades, to flow back；2) it is incubated：Thick calcium liquid is added in attemperator, is incubated at a temperature of being heated second；3) the second rectifying：The thick calcium liquid of insulation is added in the second rectifier unit, second vacuumizes, in the temperature of the 3rd heating Lower carry out rectifying, multistage backflow, separates and collects calcium steam, is condensed at a temperature of being heated the 4th, obtains high-purity calcium, its In, preferably more than 5 grades of multistage backflow flows back.
- 2. according to the method for claim 1, it is characterised in that the thick calcium raw material is goes back protocalcium, the one kind being electrolysed in calcium It is or a variety of.
- 3. according to the method for claim 1, it is characterised in that first rectifier unit is externally provided with collection device, normal Temperature is lower to collect low boiling impurity.
- 4. according to the method for claim 1, it is characterised in that in the step 1), first is evacuated down to the first rectifying dress Put middle vacuum and be less than or equal to 50Pa.
- 5. according to the method for claim 1, it is characterised in that in the step 1), the first heating-up temperature is 850-900 DEG C, time 4-5h.
- 6. according to the method for claim 1, it is characterised in that in the step 2), the temperature of the second heating is 850-900 ℃。
- 7. according to the method for claim 1, it is characterised in that thick calcium liquid is added to by insulation dress using the method for siphon In putting, or the method for siphon is used to add the thick calcium liquid of insulation in the second rectifier unit.
- 8. according to the method for claim 1, it is characterised in that in the step 3), second is evacuated down to the second rectifying dress Put middle vacuum and be less than or equal to 133Pa.
- 9. according to the method for claim 1, it is characterised in that in the step 3), the temperature of the 3rd heating is 1035- 1135℃。
- 10. according to the method for claim 1, it is characterised in that in the step 3), the temperature of the 4th heating is 842- 970℃。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108950208A (en) * | 2018-06-04 | 2018-12-07 | 山东习尚喜新材料科技股份有限公司 | A kind of continuous production device and technique of metallic potassium |
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| CN1676638A (en) * | 2005-04-22 | 2005-10-05 | 云南省通海大方科技有限公司 | Metal antimony purifying method and apparatus |
| CN102277504A (en) * | 2011-08-19 | 2011-12-14 | 赵志强 | Process for extracting zinc and indium by rectifying hard zinc under constant pressure |
| CN103409647A (en) * | 2013-08-12 | 2013-11-27 | 无锡职业技术学院 | High-low temperature compatible metallic lithium distillation equipment and distillation method thereof |
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2017
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| JPS5499020A (en) * | 1978-01-23 | 1979-08-04 | Mitsubishi Atomic Power Ind | Extracting and recovering of tritium contained in metal sodium |
| CN1544669A (en) * | 2003-11-14 | 2004-11-10 | 昆明永年锂业有限公司 | Process for preparing high purity lithium |
| CN1676638A (en) * | 2005-04-22 | 2005-10-05 | 云南省通海大方科技有限公司 | Metal antimony purifying method and apparatus |
| CN102277504A (en) * | 2011-08-19 | 2011-12-14 | 赵志强 | Process for extracting zinc and indium by rectifying hard zinc under constant pressure |
| CN103409647A (en) * | 2013-08-12 | 2013-11-27 | 无锡职业技术学院 | High-low temperature compatible metallic lithium distillation equipment and distillation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108950208A (en) * | 2018-06-04 | 2018-12-07 | 山东习尚喜新材料科技股份有限公司 | A kind of continuous production device and technique of metallic potassium |
| CN108950208B (en) * | 2018-06-04 | 2023-09-29 | 山东习尚喜新材料科技股份有限公司 | Continuous production device and process of metal potassium |
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