CN107236965B - A kind of system preparing its oxide for electrolytic metal chloride - Google Patents
A kind of system preparing its oxide for electrolytic metal chloride Download PDFInfo
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- CN107236965B CN107236965B CN201710324559.3A CN201710324559A CN107236965B CN 107236965 B CN107236965 B CN 107236965B CN 201710324559 A CN201710324559 A CN 201710324559A CN 107236965 B CN107236965 B CN 107236965B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
Abstract
A kind of system preparing its oxide for electrolytic metal chloride, electrolysis system include that electrolytic cell is constituted, and wherein cell vessel and its internal anode electrode plate being arranged alternately and cathode electrode plate are above transverse slat；It is cathode chamber between the working face of cathode electrode plate two sides, bottom passes through the through-hole and electrolyte bath connection on transverse slat；It is anode chamber between the anode working face of anode electrode plate two sides, anode chamber is externally provided with cation-exchange membrane, is equipped with inlet tube in anode chamber and is connected to outside；Blender is equipped between anode chamber and cathode chamber；Cell vessel is equipped with outlet tube and carbon dioxide pipe；Chlorine conduit is equipped with above anode chamber；Hydrogen conduit is equipped with above cathode chamber.The higher metal carbonate of purity or oxide is made using the electrolyzer system of circulation in the present invention, and electrolysis process step is simple, high degree of automation, and product purity is high, and production cost is low, is easily mass produced.
Description
Technical field
The invention belongs to electrolysis tech fields, and in particular to a kind of to be for what electrolytic metal chloride prepared its oxide
System.
Background technique
The chloride of most metals element all higher aqueous solutions of water-soluble formation concentration, and many metal carbonates
It is then insoluble or be insoluble in water, for example, alkali earth metal, rare earth element, iron, cobalt, nickel, aluminium and gallium etc., its oxide of this dvielement
And the fields such as electronics, electric appliance, optics, instrument, metallurgy, national defence and aerospace are widely used to, preparation method is divided into fire
Method and wet process two major classes.
By taking magnesia as an example, large-scale production method of magnesium oxide has dolomite carbonizatin method, magnesite carbonizatin method etc., equips
Mainly direct-fired shaft kiln, rotary furnace, bubbling carbonizing equipment etc.；Magnesia is produced using seawater, brine as raw material, what the country used
Main method has lime (or calcined dolomite in powder) method, ammonia process (or ammonium carbonate method) and caustic soda (or soda ash) method, overall process operating environment
Difference, energy consumption is higher, high production cost.
By taking aluminium oxide as an example, Bayer process becomes the prevailing technology of production aluminium oxide, but Bayer process is to the quality of bauxite
It is required that relatively high, the production of the middle-low bauxites such as domestic many high-iron bauxite, high-sulfur bauxites and not applicable Bayer process
Technique.And mother liquid evaporation energy consumption is very big in Bayer process process, is unfavorable for energy conservation.The technique of alumina producing Bayer process is multiple
It is miscellaneous, equipment is numerous, operation it is also remarkable, the alumina product of production is also not always highly desirable.
Summary of the invention
For long flow path present in the prior art and equipment, energy consumption is high and the problems such as at high cost, the present invention provides
A kind of system preparing its oxide for electrolytic metal chloride carries out electricity to metal chloride solutions by the electrolysis system
Solution, can directly obtain the carbonate of respective metal, and can obtain the very high byproduct hydrogen of purity and chlorine, gained metal carbon
High-quality metal oxide can be obtained by calcining in hydrochlorate.
System of the invention is made of electrolysis system, filtration system, dissolving circulation system and calcination system, wherein electrolysis system
System is made of power supply device and electrolytic cell, and electrolytic cell includes cell vessel and its internal N number of anode electrode plate being arranged alternately
With N number of cathode electrode plate, N number of anode electrode plate and N number of cathode electrode plate are arranged above a transverse slat, anode electrode plate bottom end
It is connect with transverse slat；Each cathode electrode plate two sides are respectively equipped with a cathodic work piece, and two on the same cathode electrode plate
Region between cathodic work piece is cathode chamber, and cathode chamber bottom passes through the through-hole and electrolyte bath connection on transverse slat, cathode
Working face is fixed on transverse slat；Each anode electrode plate two sides are respectively equipped with an anode working face, the same anode electrode plate
On two anode working faces between region be anode chamber, each anode chamber is externally provided with cation-exchange membrane, anode chamber bottom
Transverse slat is connected, anode working face is fixed on transverse slat, and inlet tube is equipped in anode chamber and is connected to outside；Adjacent anode chamber and yin
Blender is equipped between pole room；The side of cell vessel is equipped with outlet tube, and bottom or side is equipped with carbon dioxide pipe；Sun
Chlorine conduit is equipped with above pole room to be connected to anode compartment；It is equipped with inside hydrogen conduit and cathode chamber and is connected to above cathode chamber.
In above-mentioned apparatus, anode electrode plate upper end jointed anode busbar plate, anode conducting bus bar plate connects direct current
Source anode；Cathode electrode plate upper end connects cathode busbar plate, and cathode busbar plate connects DC power cathode.
Cathode conductive column is evenly distributed in above-mentioned apparatus, in cathode chamber, cathode conductive column both ends are separately connected cathode electricity
Pole plate and cathodic work piece；Anode conducting column is evenly distributed in anode chamber, anode conducting column both ends are separately connected anode electrode
Plate and anode working face.
Above-mentioned cathode electrode plate, cathodic work piece, cathode conductive column, cathode busbar plate, carbon dioxide pipe
Material with hydrogen conduit is titanium-based ruthenium material；Anode electrode plate, anode working face, anode conducting column, anode conducting bus bar plate,
The material of chlorine conduit, inlet tube and outlet tube is titanium-based ruthenium material.
The material of above-mentioned transverse slat is PVC plastic, rubber or polytetrafluoro material.
The material of above-mentioned cell vessel is PVC plastic, glass or organic glass.
In above-mentioned apparatus, anode electrode plate and cathode electrode plate on transverse slat are any logarithm, i.e. N >=1；Device system tool
There are ventilation, stirring, quickly filtering and dry function, agitating mode is mechanical stirring, or is mechanical and gas coupled stir,
The effect of stirring is inhibition slot bottom precipitating and bubble dispersion, and cathodic region electrolyte adjusts concentration by filter plant, filtrate
After return to cathodic region, anode region electrolyte returns to anode region after adjusting solution concentration by dissolving tank, realizes anode and cathode electricity respectively
Solve the continuous circulation of liquid.
The application method of above-mentioned apparatus sequentially includes the following steps:
1, metal chloride solutions are added into device, make cathode chamber full of the metal chloride solutions；Pass through anode chamber
The inlet tube at top fills the metal chloride solutions in anode chamber；
2, by connecting the cathode busbar plate and anode conducting bus bar plate of DC power supply, respectively to each cathode and Ge Yang
Pole is powered and is electrolysed to the metal chloride solutions, at the same by the air inlet pipe of the carbon dioxide of bottom of electrolytic tank or side to
Carbon dioxide gas is passed through in electrolytic cell；
3, hydrogen and chlorine that cathode chamber and anode chamber's Inner electrolysis generate are passed through into hydrogen conduit respectively and chlorine conduit is received
Collection；
4, the suspension in cathode chamber and electrolytic cell is constantly extracted out, and after filtering, addition metal chloride adjusts concentration
It rejoins in electrolytic cell, realizes the recycling of solution；When electrolysis carry out in anode chamber solution concentration reduce when, by into
Liquid pipe adds new metal chloride solutions into anode chamber, and metal chloride solutions original in anode chamber are discharged, and makes sun
Solution concentration maintains to stablize in pole room；
5, by the metal carbonate precipitate being obtained by filtration washing, drying, high-temperature calcination, gained carbon dioxide gas returns to electricity
Solution preocess finally obtains respective metal oxide product.
In the above method, obtained oxide product purity >=97%.
In the above method, the process conditions of electrolysis are as follows: temperature is 10 ~ 90 DEG C, is electrolysed as direct current, tank voltage >=2.2V,
Current density is 0.01 ~ 0.60A/cm2。
In the above method, carbon dioxide is reacted with hydroxyl in electrolyte (or metal hydroxides), in conjunction in anode chamber
Enter the metal cation in catholyte through cation-exchange membrane, generates metal carbonate precipitate；Electrolytic etching of metal liquid stream passes through after going out
Filter plant, filtrate enter dissolving tank to be recycled as supplement electrolyte, and the carbonate being obtained by filtration obtains after calcining
Metal oxide.
Compared with prior art, present invention has the advantage that:
(1) the higher metal carbonate of purity or oxide, electrolysis is made using the electrolyzer system of circulation in the present invention
Processing step is simple, high degree of automation, and product purity is high, and production cost is low, is easily mass produced；
(2) metal carbonate of generation is quickly moved out electrolytic cell and enters filtration system by method of the invention, reduces gold
Belong to the secondary dissolution of carbonate or the anti-amount for being dissolved in electrolyte, obtains carbonate products to greatest extent；
(3) in the device of the invention use process, cathode and anode generates purer hydrogen and chlorine respectively, can be done
It is dry, collect using as byproduct.
Detailed description of the invention
Fig. 1 is a kind of master that electrolytic cell part in the system of its oxide is prepared for electrolytic metal chloride of the invention
Depending on the schematic diagram of the section structure；
Fig. 2 is the top view of system shown in Figure 1；
Fig. 3 is a kind of overall system architecture schematic diagram that its oxide is prepared for electrolytic metal chloride of the invention；
In figure, 1. cell vessels, 2. transverse slats, 3. anode electrode plates, 4. cathode electrode plates, 5. anode working faces, 6. yin
Pole working face, 7. anode conducting columns, 8. cathode conductive columns, 9. cation-exchange membranes, 10. chlorine conduits, 11. hydrogen conduits,
12. anode inlet tube, 13. blenders, 14. slot bottom carbon dioxide pipes, 15. slot side carbon dioxide pipes, 16. cathodes go out
Liquid pipe, 17.CO2Air accumulator, 18. gas flowmeters, 19. cathode chambers, 20. anode chambers, 21. first dissolving tanks, 22. first pumps,
23. DC power supply, 24. filters, 25. drying boxes, 26. second dissolving tanks, 27. second pumps.
Specific embodiment
In the embodiment of the present invention by taking magnesium chloride as an example, solution electrolysis is carried out in the electrolysis unit.
System of systems of the invention has the function of that ventilation, stirring, quickly filtering and calcining, agitating mode are stirred for machinery
It mixes, or is mechanical and gas coupled stir, the effect of stirring is to inhibit slot bottom precipitating and bubble dispersion, cathodic region electrolysis
Liquid is by filter plant, and filtrate returns to cathodic region after adjusting concentration, after anode region electrolyte adjusts solution concentration by dissolving tank
Anode region is returned to, realizes the continuous circulation of anode and cathode electrolyte respectively.
The titanium-based ruthenium material used in the embodiment of the present invention is commercial products.
The cation-exchange membrane used in I of the embodiment of the present invention is commercial products.
Embodiment 1
The overall system architecture of magnesia is produced for electrolytic metal chloride solution as shown in figure 3, by electrolysis system, mistake
Filter system, dissolving circulation system and calcination system are constituted, including CO2Gas cylinder 17, gas flowmeter 18, the first dissolving tank 21, the
One pump 22, DC power supply 23, filter 24, drying box 25, the second dissolving tank 26 and the second pump 27；Wherein electrolysis system is by power supply
Device and electrolytic cell are constituted；CO2Gas cylinder 17 is connected to by gas flowmeter 18 with cathode chamber 19, cathode chamber 19 and first pump 22,
First dissolving tank 21 and filter 24 constitute circulation loop, and drying box 25 is used to receive the solid material of the generation of filter 24；Sun
Pole room 20 and the second dissolving tank 26 and the second pump 27 constitute circulation loop；
The structure of electrolytic cell part as shown in Figure 1, top view as shown in Fig. 2, include cell vessel 1 and its it is internal alternately
3 anode electrode plate 3 and 3 cathode electrode plates 4 being arranged, anode electrode plate 3 and cathode electrode plate 4 are arranged in a transverse slat 2
Top, 3 bottom end of anode electrode plate are connect with transverse slat 2；Each 4 two sides of cathode electrode plate are respectively equipped with a cathodic work piece 6, together
The region between two cathodic work pieces 6 on one cathode electrode plate 4 is cathode chamber 19, and 19 bottom of cathode chamber passes through transverse slat 2
On through-hole and electrolyte bath connection, cathodic work piece 6 is fixed on transverse slat 2；
Each 3 two sides of anode electrode plate are respectively equipped with an anode working face 5, and two on the same anode electrode plate 3
Region between anode working face 5 is anode chamber 20, and each anode chamber 20 is externally provided with cation-exchange membrane 9,20 bottom of anode chamber
Transverse slat 2 is connected, anode working face 5 is fixed on transverse slat 2, and anode inlet tube 12 is equipped in anode chamber 20 and is connected to outside；It is adjacent
Anode chamber 20 and cathode chamber 19 between be equipped with blender 13；The side of cell vessel 1 be equipped with cathode outlet tube 16, bottom and
Side is respectively equipped with slot bottom carbon dioxide pipe 14 and slot side carbon dioxide pipe 15；It is led above anode chamber 20 equipped with chlorine
It is connected to inside pipe 10 and anode chamber 20；It is equipped with inside hydrogen conduit 11 and cathode chamber 19 and is connected to above cathode chamber 19；
3 upper end jointed anode busbar plate of anode electrode plate, anode conducting bus bar plate connect 23 anode of DC power supply；Yin
Electrode plate 4 upper end in pole connects cathode busbar plate, and cathode busbar plate connects 23 cathode of DC power supply；
Cathode conductive column 8 is evenly distributed in cathode chamber 19,8 both ends of cathode conductive column are separately connected 4 He of cathode electrode plate
Cathodic work piece 6；Anode conducting column 7 is evenly distributed in anode chamber 20,7 both ends of anode conducting column are separately connected anode electrode plate
3 and anode working face 5；
Cathode electrode plate, cathodic work piece, cathode conductive column, cathode busbar plate, carbon dioxide pipe and hydrogen
The material of conduit is titanium-based ruthenium material；Anode electrode plate, anode working face, anode conducting column, anode conducting bus bar plate, chlorine are led
The material of pipe, inlet tube and outlet tube is titanium-based ruthenium material；
The material of transverse slat is PVC plastic；
The material of cell vessel is PVC plastic；
Using above system electrolysis 10% magnesium chloride brine method the following steps are included:
1. metal chloride solutions are added into electrolytic cell, make in cathode chamber and electrolytic cell full of metal chloride solutions；
Metal chloride solutions are filled in anode chamber by the inlet tube at the top of anode chamber；
2. by the cathode busbar plate and anode conducting bus bar plate of connection DC power supply, respectively to each cathode and respectively
Anodal closure is electrolysed metal chloride solutions, controls current density in 0.1A/cm2, while by bottom of electrolytic tank or
The air inlet pipe of the carbon dioxide of side is passed through carbon dioxide gas into electrolytic cell；
3. hydrogen, the chlorine that cathode chamber, anode chamber's Inner electrolysis generate are passed through hydrogen conduit, chlorine catheter collection respectively；
4. the suspension in cathode chamber and electrolytic cell is constantly extracted out, after filtering, addition magnesium chloride adjustment concentration is again
It is added in electrolytic cell, realizes the recycling of magnesium chloride；When electrolysis, which is carried out to solution concentration in anode chamber, to be reduced, pass through feed liquor
Pipe adds new metal chloride solutions into anode chamber, and metal chloride solutions original in anode chamber are discharged, and makes anode
Indoor solution concentration maintains to stablize；
6. by the magnesium carbonate being obtained by filtration washing, drying, high-temperature calcination, gained carbon dioxide gas returns to electrolytic process,
Finally obtain magnesium oxide product；
Obtained magnesium oxide product whiteness >=97, purity >=99.5%.
Embodiment 2
With embodiment 1, difference is system structure:
(1) electrolytic cell 1 and its 5 anodes and 5 cathodes of inside；
(2) side of cell vessel is equipped with slot side carbon dioxide pipe；
(3) material of transverse slat is rubber；
(4) material of cell vessel is glass.
Embodiment 3
With embodiment 1, difference is system structure:
(1) electrolytic cell 1 and its 1 anode and 1 cathode of inside；
(2) bottom of cell vessel is equipped with slot bottom carbon dioxide pipe；
(3) material of transverse slat is polytetrafluoro material；
(4) material of cell vessel is organic glass.
Claims (4)
1. a kind of system for preparing its oxide for electrolytic metal chloride, by electrolysis system, filtration system, dissolving circulation system
System and calcination system are constituted, including CO2Gas cylinder, gas flowmeter, the first dissolving tank, the first pump, DC power supply, filter are done
Dry case, the second dissolving tank and the second pump；Wherein electrolysis system is made of power supply device and electrolytic cell；CO2Gas cylinder passes through gas stream
Meter is connected to cathode chamber, and cathode chamber and the first pump, the first dissolving tank and filter mechanism are at circulation loop, and drying box is for receiving
The solid material that filter generates；Anode chamber and the second dissolving tank and the second pump constitute circulation loop；It is characterized by: electrolytic cell
Including cell vessel and its internal N number of anode electrode plate and N number of cathode electrode plate being arranged alternately, N number of anode electrode plate and N
A cathode electrode plate is arranged above a transverse slat, and anode electrode plate bottom end is connect with transverse slat；Each cathode electrode plate two sides point
Not She You a cathodic work piece, the region between two cathodic work pieces on the same cathode electrode plate is cathode chamber, yin
Pole room bottom is fixed on transverse slat by the through-hole and electrolyte bath connection on transverse slat, cathodic work piece；Each anode electrode
Plate two sides are respectively equipped with an anode working face, and the region between two anode working faces on the same anode electrode plate is sun
Pole room, each anode chamber are externally provided with cation-exchange membrane, and anode chamber bottom connects transverse slat, and anode working face is fixed on transverse slat,
Inlet tube is equipped in anode chamber to be connected to outside；Blender is equipped between adjacent anode chamber and cathode chamber；Cell vessel
Side is equipped with outlet tube, and bottom and/or side are equipped with carbon dioxide pipe；Chlorine conduit and anode chamber are equipped with above anode chamber
Inside connection；It is equipped with inside hydrogen conduit and cathode chamber and is connected to above cathode chamber；Cathode is evenly distributed in the cathode chamber
Conductive column, cathode conductive column both ends are separately connected cathode electrode plate and cathodic work piece；It is evenly distributed in the anode chamber
Anode conducting column, anode conducting column both ends are separately connected anode electrode plate and anode working face；N >=1.
2. a kind of system for preparing its oxide for electrolytic metal chloride according to claim 1, it is characterised in that
The anode electrode plate upper end jointed anode busbar plate, anode conducting bus bar plate connect DC power anode；Described
Cathode electrode plate upper end connects cathode busbar plate, and cathode busbar plate connects DC power cathode.
3. a kind of system for preparing its oxide for electrolytic metal chloride according to claim 1, it is characterised in that
The material of the transverse slat is PVC plastic, rubber or polytetrafluoro material.
4. a kind of system for preparing its oxide for electrolytic metal chloride according to claim 1, it is characterised in that
The material of the cell vessel is PVC plastic, glass or organic glass.
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| CN201710324559.3A CN107236965B (en) | 2017-05-10 | 2017-05-10 | A kind of system preparing its oxide for electrolytic metal chloride |
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| CN111962093A (en) * | 2020-07-06 | 2020-11-20 | 中船重工（邯郸）派瑞特种气体有限公司 | Electrolytic fluorine production stirring device and method |
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| JP5730385B2 (en) * | 2010-04-23 | 2015-06-10 | シンボル インコーポレイテッド | Method for producing lithium carbonate from lithium chloride |
| CN103173782A (en) * | 2013-04-12 | 2013-06-26 | 四川大学 | Method for preparing basic magnesium carbonate and coproducing hydrochloric acid by mineralizing CO2 (carbon dioxide) via magnesium chloride |
| CN104988529B (en) * | 2015-07-27 | 2017-03-29 | 东北大学 | With the device and method of magnesium chloride solution preparing magnesium hydroxide, hydrogen and chlorine |
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