CN209243190U - It is electrolysed arsine device processed - Google Patents
It is electrolysed arsine device processed Download PDFInfo
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- CN209243190U CN209243190U CN201821990303.2U CN201821990303U CN209243190U CN 209243190 U CN209243190 U CN 209243190U CN 201821990303 U CN201821990303 U CN 201821990303U CN 209243190 U CN209243190 U CN 209243190U
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Abstract
The utility model provides a kind of electrolysis arsine device processed.The electrolysis arsine device includes: cathode chamber, and the catholyte of cathode chamber is arsenic trioxide saturated aqueous solution, and the cathode of cathode chamber is non-sacrificial metal, and cathode chamber electrolysis generates the gaseous mixture comprising arsine and hydrogen；Anode chamber, the anode of anode chamber are non-sacrificial metal, and anode chamber's electrolysis generates oxygen；It is electrolysed arsine device processed further include: arsenic trioxide saturated aqueous solution supply unit, it is connected with cathode chamber, recoil gas source, is connected with arsenic trioxide saturated aqueous solution supply unit to carry out blowback to the arsenic trioxide saturated aqueous solution in arsenic trioxide saturated aqueous solution supply unit.Continue to provide the arsenic trioxide saturated aqueous solution of saturation to cathode chamber, to maintain concentration of electrolyte in electrolytic process to stablize, simultaneously using recoil gas source blowback, influence of the gases such as the arsine wherein carried secretly to electrolyte composition is avoided, control is electrolysed the ratio of obtained hydrogen and arsine.
Description
Technical field
The utility model relates to arsine preparation fields, in particular to a kind of electrolysis arsine device processed.
Background technique
Arsine electronic gas is wide in semicon industry, solar energy industry, LED industry, FPD industry and optical fiber industry
General use is the gas of a kind of hypertoxic gas, flammable explosive gas.Arsine electronic gas process is transported and is used in production, storage
All there is very big risk.For example, the 44L arsine steel cylinder that LED industry uses, can fill arsine electronic gas is 23.5kg,
If it is one square kilometre of a height of 3 meters of gas cloud that these gas leakages, which can form circumference, the mankind of this gas cloud are contacted within the scope of this
The death rate within 14 days is 50%.Reducing to the greatest extent using with storing liquid arsine steel cylinder gas is to reduce dangerous approach.
Be electrolysed preparation method arsine can using and storing to avoid a large amount of arsine gas bomb, the online of arsine may be implemented
Formula production and use need to there is no arsine in use site with regard to live electrolysis production how many arsine using how many arsine
Storage problem, the arsine raw material not being electrolysed are solid or liquid, the risk not spread in an atmosphere.
The patent application of Publication No. CN 101463485A discloses a kind of divided electrochemical cell and low cost is high-purity
Hydride gas production process is spent, is proposed as shown in Figure 1 using U-tube link catholyte pond and anode electrolysis pond, schematic diagram.
Cathode chamber enclosure 61 ' and anode chamber enclosure 71 ' are high-purity stainless steels, and anode chamber enclosure 71 ' doubles as the sun of electrolytic cell
Pole uses.Cathode chamber enclosure 61 ' and anode chamber enclosure 71 ' are connected by nonconducting nonmetallic U-shaped hose 72 ', it is ensured that outside cathode
Shell 61 ' and anode chamber enclosure 71 ' will not connection it is conductive, design electrolysis power 66 ' in this way, can only by catholyte 63 ' with
Anolyte 69 ' could be connected.In the patent of invention, actually catholyte 63 ' and anolyte 69 ' be actually
It is same mixture, i.e. the aqueous solution of KOH.It is 99% arsenic simple substance in the cathode 62 ' of the patent of invention.Energization starts to be electrolysed
Afterwards, the mixture that hydrogen and arsine can be generated on 62 ' surface of cathode of electrolytic tank, after 64 ' concentrations at the top of the electrolytic cell of cathode, by
The electrolytic cell gas control pipeline 65 ' of cathode is discharged；The inner surface of anode chamber enclosure 71 ' is exactly electrolytic anode, and oxygen is in this table
Face generates, and then converges at the top of the electrolytic cell of anode after 68 ' concentrations, is discharged by the electrolytic cell gas control pipeline 67 ' of anode.
The design of nonmetallic U-shaped hose 72 ' is to generate gas bubbles meeting in cathode chamber and anode chamber to divide cathode chamber and anode chamber
It is respectively risen to using buoyancy 64 ' and at the top of the electrolytic cell of anode 68 ' at the top of the electrolytic cell of cathode, without being mutually mixed, and
It plays isolation cathode chamber and anode chamber generates gas.
The raw material that arsine processed is electrolysed in the invention are elemental arsenic and water, and use elemental arsenic as the cathode being electrolysed,
It is the electrolysis method of sacrificing cathode.The patent of invention has the disadvantage in that
1, frequent shutdown is needed to replace cathode arsenic electrode.It, can be in the process of electrolysis due to the sacrificing cathode electrolysis method of use
In need to consume elemental arsenic cathode, it is therefore desirable to regularly replace cathode electrode.
2, electrolytic process and arsine gas concentration are difficult to control.With the consumption of cathode electrode, the electrolysis area (yin of cathode
The contact area of pole electrolysis and electrolyte) it is smaller and smaller, the efficiency decline of electrolysis, this results in electrolysis control parameter and arsine gas
The yield of body is not linear relationship, is difficult accurately to control electrolytic process, it is also difficult to control hydrogen and arsine in catholyte gas
Proportionate relationship.
3, the service efficiency of elemental arsenic is low.When elemental arsenic electrolysis electrolytic efficiency shuts down replacement electricity lower than some numerical value
Pole.Elemental arsenic is caused to waste and increase the processing cost of danger wastes.
4, elemental arsenic electrode is expensive.Elemental arsenic electrode must be monocrystalline elemental arsenic can just be formed with fixed structure and
The elemental arsenic of surface area, monocrystalline needs dedicated long crystal furnace that can just grow up to crystal, needs special equipment and consumes a large amount of electric energy.
5, the gas that the structure of U-tube connection cathode chamber and anode chamber cannot be effectively isolated cathode chamber and anode chamber generates.
The solubility of oxygen is 6.3ml/l in 20 DEG C, the pure water of 100kPa, and the solubility of arsine is 230ml/l, these gases are adjoint
Electrolytic process can all be dissolved in electrolyte.When catholyte generates arsine, being dissolved into oxygen in water also can band together
Out, oxygen gas component will be limited strictly in high-purity arsine electron gas, it is desirable that otherwise < 20ppb will increase the difficulty of gas purification
And cost for purification.Anode electrolysis generate oxygen be mixed into catholyte gas arsine be the program significant deficiency, be doomed it not
Production electronics arsine gas can be used to be engineered.In addition when anode electrolysis generates oxygen, it can also take out of and be dissolved in electrolyte
Arsine gas, the gas that anode generates have to configure individual tail gas treatment device, and the oxygen after removing toxic substances could discharge, this
Increase the production cost of arsine gas.
6, moisture is difficult to remove in cathode gas.Since electrolytic process is exothermic process, the arsine and hydrogen of catholyte
Gaseous mixture in contain more vapor, the presence of these moisture influences the engineering application of arsine.
Utility model content
The main purpose of the utility model is to provide a kind of electrolysis arsine devices processed, to solve cathode in the prior art
Electrolysis area reduction the problem of causing electrolytic efficiency to decline.
To achieve the goals above, one aspect according to the present utility model provides a kind of electrolysis arsine device processed, electricity
Solution arsine device includes: cathode chamber, and the catholyte of cathode chamber is arsenic trioxide saturated aqueous solution, the cathode of cathode chamber
For non-sacrificial metal, cathode chamber electrolysis generates the gaseous mixture comprising arsine and hydrogen；Anode chamber, the anode of anode chamber are non-sacrificial
Domestic animal property metal, anode chamber's electrolysis generate oxygen；It is electrolysed arsine device processed further include: the supply of arsenic trioxide saturated aqueous solution is single
Member is connected with cathode chamber, and recoil gas source, is connected with arsenic trioxide saturated aqueous solution supply unit to be saturated to arsenic trioxide
Arsenic trioxide saturated aqueous solution in aqueous solution supply unit carries out blowback.
Further, above-mentioned arsenic trioxide saturated aqueous solution supply unit includes: arsenic trioxide saturated aqueous solution hair
Raw device, recoil gas source are connected with arsenic trioxide saturated aqueous solution generator；Liquid supply pipe；Liquid back pipe, arsenic trioxide saturated water
Solution generator, liquid supply pipe, liquid back pipe and cathode chamber constitute circulation loop.
Further, have the first blender to arsenic trioxide in above-mentioned arsenic trioxide saturated aqueous solution generator
Arsenic trioxide particle in saturated aqueous solution generator is stirred.
Further, above-mentioned arsenic trioxide saturated aqueous solution supply unit further includes the first pure water supply equipment, three oxygen
Change two arsenic saturated aqueous solution generators and is connected with the first pure water supply equipment by the first water supplying pipe.
Further, it is additionally provided with saturation liquid level sensor in above-mentioned arsenic trioxide saturated aqueous solution generator, first
The first water compensating valve is provided on water supplying pipe, saturation liquid level sensor is electrically connected with the first water compensating valve.
Further, above-mentioned cathode chamber is additionally provided with cathode liquid level sensor, is provided with solution feed pump and feed flow on liquid supply pipe
Valve, cathode liquid level sensor are electrically connected with solution feed pump and supplying valve.
Further, above-mentioned anode chamber is provided with anode liquid level sensor, and being electrolysed arsine device processed further includes the second pure water
Supply equipment, the second pure water supply equipment are connected with anode chamber by the second water supplying pipe, and the second benefit is provided on the second water supplying pipe
Water valve, anode liquid level sensor are electrically connected with the second water compensating valve.
Further, above-mentioned electrolysis arsine device further includes counter-flushing pipeline, and counter-flushing pipeline includes: main flushing pipe
Road, one end are connected with recoil gas source；First rinses bye-pass, and one end is connected with main flushing pipeline, and the other end extends to three oxidations
The lower part of two arsenic saturated aqueous solution generators；Second rinses bye-pass, and one end is connected with main flushing pipeline, and the other end extends to yin
The lower part of pole room；Third rinses bye-pass, and one end is connected with main flushing pipeline, and the other end extends to the lower part of anode chamber；It rinses
Circuit is provided with vacuum pump, flush loop and arsenic trioxide saturated aqueous solution generator, cathode chamber and anode in flush loop
The cavity of the ullage of room is connected.
Further, above-mentioned electrolysis arsine device further include: cathode gas transfer pipeline, one end are connected with cathode chamber,
The other end is provided with cathode dry type tail gas treatment device；Anodic gas transfer pipeline, is connected with anode chamber, and flush loop includes:
One end of major loop, major loop is connected with cathode dry type tail gas treatment device, and vacuum pump is provided on major loop；First is returned
The one end on road, the first branch circuit is connected with major loop, and the liquid level of arsenic trioxide saturated aqueous solution generator is arranged in the other end
In the cavity of top；Second branch circuit, one end of the second branch circuit are connected with the other end of major loop, and the other end passes through cathode gas
Body transfer pipeline is connected with cathode chamber；Third branch circuit, one end of third branch circuit are connected with the other end of major loop, the other end
It is connected by anodic gas transfer pipeline with anode chamber.
Further, above-mentioned recoil gas source is source nitrogen and hydrogen source, and main flushing pipeline passes through the first connecting tube and nitrogen
Gas source is connected, and is connected by the second connecting tube with hydrogen source, and first switch valve is provided in the first connecting tube and first pressure passes
Sensor is provided with second switch valve and second pressure sensor in the second connecting tube.
Further, above-mentioned second flushing bye-pass is connected with cathode gas transfer pipeline by third connecting tube, and the
Three connecting tubes and the interface of the second flushing bye-pass are leaned on close to cathode chamber, third connecting tube and the interface of cathode gas transfer pipeline
Nearly cathode chamber is provided with third switch valve in third connecting tube.
Further, above-mentioned third rinses bye-pass and is connected with anodic gas transfer pipeline by the 4th connecting tube, and the
The interface that four connecting tubes and third rinse bye-pass is leaned on close to anode chamber, the 4th connecting tube and the interface of anodic gas transfer pipeline
Nearly anode chamber is provided with the 4th switch valve in the 4th connecting tube
Using the technical solution of the utility model, the application is using arsenic trioxide saturated aqueous solution as catholyte
Liquid, and continue to provide the arsenic trioxide saturated water of saturation to cathode chamber using arsenic trioxide saturated aqueous solution supply unit
Solution, to maintain to be stablized with concentration of electrolyte in cathode chamber in electrolytic process, while using recoil gas source to arsenic trioxide
Saturated aqueous solution carries out blowback, influence of the gases such as the arsine wherein carried secretly to electrolyte composition is avoided, to remain stable
Electrolytic efficiency, and then control the ratio for being electrolysed obtained hydrogen and arsine.Above-mentioned electrolysis arsine device can not also stop
Machine carries out the electrolysis production of arsine, extends the maintenance period for being electrolysed arsine device processed and guarantees that arsine stablizes supply.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide a further understanding of the present invention, this is practical
Novel illustrative embodiments and their description are not constituteed improper limits to the present invention for explaining the utility model.
In the accompanying drawings:
Fig. 1 shows the structural schematic diagram of electrochemical cell according to prior art；And
Fig. 2 shows a kind of electrolysis arsine apparatus structure schematic diagrams of embodiment according to the present utility model.
Wherein, the above drawings include the following reference numerals:
10, cathode chamber；11, cathode liquid level sensor；
20, anode chamber；21, anode liquid level sensor；
31, arsenic trioxide saturated aqueous solution generator；311, the first blender；312, it is saturated liquid level sensor；32, it supplies
Liquid pipe；321, solution feed pump；322, supplying valve；33, liquid back pipe；34, the first pure water supply equipment；341, the first water compensating valve；
40, the second pure water supply equipment；41, the second water compensating valve；
51, main flushing pipeline；52, first bye-pass is rinsed；53, second bye-pass is rinsed；54, third rinses bye-pass；
551, major loop；552, the first branch circuit；553, the second branch circuit；554, third branch circuit；555, vacuum pump；
61, source nitrogen；611, the first connecting tube；62, hydrogen source；621, the second connecting tube；
71, cathode gas transfer pipeline；711, arsine water eliminating equipment；712, cathode dry type tail gas treatment device；72, positive
Pole gas transfer pipeline；
80, third connecting tube；
90, the 4th connecting tube.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The utility model will be described in detail below with reference to the accompanying drawings and embodiments.
As the application background technique is analyzed, when doing cathode using elemental arsenic, with the consumption of cathode electrode, cathode
Electrolysis area (contact area of catholyte and electrolyte) is smaller and smaller, and the efficiency decline of electrolysis, this results in electrolysis control
The yield of parameter and arsine gas is not linear relationship, is difficult accurately to control electrolytic process, it is also difficult to control catholyte gas
The proportionate relationship of middle hydrogen and arsine, in order to solve this problem, this application provides a kind of electrolysis arsine devices processed.
In a kind of typical embodiment of the application, a kind of electrolysis arsine device processed is provided, as shown in Fig. 2, the electricity
Solution arsine device includes cathode chamber 10 and anode chamber 20, and the catholyte of cathode chamber 10 is that arsenic trioxide saturation is water-soluble
Liquid, the cathode of cathode chamber 10 are non-sacrificial metal, and the electrolysis of cathode chamber 10 generates the gaseous mixture comprising arsine and hydrogen；Anode chamber
20 anode is non-sacrificial metal, and the electrolysis of anode chamber 20 generates oxygen；Being electrolysed arsine device processed further includes that arsenic trioxide is full
With aqueous solution supply unit and recoil gas source, arsenic trioxide saturated aqueous solution supply unit is connected with cathode chamber 10, back flushing air
Source is connected to three oxygen in arsenic trioxide saturated aqueous solution supply unit with arsenic trioxide saturated aqueous solution supply unit
Change two arsenic saturated aqueous solutions and carries out blowback.
In above-mentioned electrolysis arsine device, the reaction equation of anode electrolysis reaction are as follows:
6H2O→3O2g+12e-+12H+
The reactive mode of catholyte reaction are as follows:
As2O3(s)+12H++12e-→2AsH3+3H2O
The application uses arsenic trioxide saturated aqueous solution as catholyte, and uses arsenic trioxide saturated water
Solution supply unit continues to provide the arsenic trioxide saturated aqueous solution of saturation to cathode chamber 10, to maintain cathode in electrolytic process
It can be stablized with concentration of electrolyte in room 10, while blowback is carried out to arsenic trioxide saturated aqueous solution using recoil gas source, avoided
The influences of the gases to electrolyte composition such as the arsine wherein carried secretly to maintain stable electrolytic efficiency, and then control electrolysis
The ratio of obtained hydrogen and arsine.Above-mentioned electrolysis arsine device can not also shut down the electrolysis production for carrying out arsine, prolong
The long maintenance period for being electrolysed arsine device processed and guarantee arsine stablize supply.
As previously mentioned, arsenic trioxide participates in cell reaction, therefore preferably above-mentioned electrolysis arsine dress with stable concentration
The cathode for setting middle cathode chamber 10 is non-sacrificial metal.It is preferably positive in order to improve the isolation effect of cathode chamber 10 and anode chamber 20
Pole room 20 is isolated by ion semi-permeable membrane with cathode chamber 10.Also as before, anolyte is mainly that water participates in reaction, because
The anode of this preferred anodes room 20 is non-sacrificial metal, more preferably uses H2SO4Electrolytic efficiency is improved as conducting electrolyte.
Above-mentioned non-sacrificial metal selects those skilled in the art as the cathode of cathode chamber 10 and the anode of anode chamber 20, specific metal
Member can be selected according to the potential requirements that arsine is electrolysed, such as using lead metal plate as cathode, using titanium mesh
As anode, both metals are not involved in cell reaction, as non-sacrificial metal.Because using non-sacrificial metal conduct
Cathode and anode, and be all metal commonly used in the art, therefore cost is relatively low for electrolysis.And since cathode and anode are not consumed,
Therefore the problem of electrolysis area of cathode is kept constant, and is not in electrolytic efficiency decline caused by reducing due to electrolysis area.
Electrolyte is its constant concentration of the arsenic trioxide solution of saturation simultaneously, so that the ratio of hydrogen and arsine that catholyte generates
Stablize.Further, since cathode chamber 10 and anode chamber 20 being isolated using ion semi-permeable membrane, only allow hydrogen ion logical
It crosses, remaining ion and molecule do not allow to pass through, and effectively prevent oxygen and spread to cathode chamber 10, arsine gas expands to anode
It dissipates, and then simplifies the purification process of gas, reduces purification for gas cost.
In a preferred embodiment of the present application, electrolysis rate is controlled in order to further accurate, as shown in Fig. 2, above-mentioned
Arsenic trioxide saturated aqueous solution supply unit includes arsenic trioxide saturated aqueous solution generator 31, liquid supply pipe 32 and liquid back pipe
33, recoil gas source is connected with arsenic trioxide saturated aqueous solution generator 31；Arsenic trioxide saturated aqueous solution generator 31 supplies
Liquid pipe 32, liquid back pipe 33 and cathode chamber 10 constitute circulation loop.Pass through above-mentioned arsenic trioxide saturated aqueous solution supply unit packet
It includes arsenic trioxide saturated aqueous solution generator 31, liquid supply pipe 32 and liquid back pipe 33 and provides arsenic trioxide saturation to cathode chamber 10
Aqueous solution is to maintain arsenic trioxide concentration in cathode chamber 10 to stablize.
In order to stablize strength of fluid in arsenic trioxide saturated aqueous solution generator 31, preferably as shown in Fig. 2, above-mentioned three
Aoxidizing in two arsenic saturated aqueous solution generators 31 has the first blender 311 to arsenic trioxide saturated aqueous solution generator 31
In arsenic trioxide particle be stirred.
In addition, with the use of arsenic trioxide saturated aqueous solution, in arsenic trioxide saturated aqueous solution generator 31
Arsenic trioxide saturated aqueous solution gradually consumes, in order to maintain the continuous service of device, in another preferred implementation of the application
In example, as shown in Fig. 2, above-mentioned arsenic trioxide saturated aqueous solution supply unit further includes the first pure water supply equipment 34, three oxygen
Change two arsenic saturated aqueous solution generators 31 and is connected with the first pure water supply equipment 34 by the first water supplying pipe.
In order to improve the accuracy and the degree of automation that the application is electrolysed the operation of arsine device processed, preferably as shown in Fig. 2,
It is additionally provided with saturation liquid level sensor 312 in above-mentioned arsenic trioxide saturated aqueous solution generator 31, is arranged on the first water supplying pipe
There is the first water compensating valve 341, saturation liquid level sensor 312 is electrically connected with the first water compensating valve 341.When arsenic trioxide saturated aqueous solution
When liquid level in generator 31 is lower than the minimum liquid level of saturation liquid level sensor 312, the first water compensating valve 341 is opened, the first pure water
Supply equipment 34 supplements deoxidation pure water into arsenic trioxide saturated aqueous solution generator 31.When arsenic trioxide saturated aqueous solution
When the highest that liquid level in generator 31 is higher than saturation liquid level sensor 312 limits liquid level, the first water compensating valve 341 is closed.
Similarly, in order to improve the accuracy and the degree of automation that the application is electrolysed the operation of arsine device processed, preferably such as Fig. 2
Shown, above-mentioned cathode chamber 10 is additionally provided with cathode liquid level sensor 11, and solution feed pump 321 and supplying valve are provided on liquid supply pipe 32
322, cathode liquid level sensor 11 is electrically connected with solution feed pump 321 and supplying valve 322.
Using the liquid level of 11 real-time detection cathode chamber of cathode liquid level sensor, 10 inner cathode electrolyte, when cathode level sensing
When device 11 detects the liquid level of catholyte lower than minimum liquid level, the tapping valve of catholyte will be closed, catholyte
Supplying valve 322 and solution feed pump 321 will open so that the liquid level of catholyte rises；The liquid level of catholyte is higher than most
When high liquid level highest limits, the solution feed pump 321 of catholyte is closed.When the liquid level of catholyte is located at cathode level sensing
When the highest of device 11 is limited between minimum limit, solution feed pump 321 will be opened, the supplying valve 322 and tapping valve of catholyte
It opens simultaneously, the catholyte and external arsenic trioxide saturated aqueous solution generator 31 in cathode chamber 10 recycle, supplement
The As of consumption3+Ion.When cathode liquid level sensor 11 detects the liquid level of catholyte higher than highest liquid level, drain is utilized
Extra liquid is back to arsenic trioxide saturated aqueous solution generator 31 by pipeline, which can be liquid back pipe 33,
Or the pipeline being independently arranged.
In the electrolytic process of anolyte, constantly there are oxygen discharge and hydrogen ion to generate, hydrogen ion is made in electric field
Under, passes through ion semi-permeable membrane and reach in catholyte, participate in the cell reaction of cathode solution.Anode electrolysis in the process
Liquid only has water and participates in reaction.Therefore, in order to stablize solution concentration in anode chamber 20, preferably as shown in Fig. 2, above-mentioned anode chamber 20
It is provided with anode liquid level sensor 21, being electrolysed arsine device processed further includes the second pure water supply equipment 40, and the supply of the second pure water is set
Standby 40 are connected with anode chamber 20 by the second water supplying pipe, and the second water compensating valve 41, anode level sensing are provided on the second water supplying pipe
Device 21 is electrically connected with the second water compensating valve 41.Using the height of 21 real-time measurement anolyte of anode liquid level sensor, work as anode
When electrolyte is lower than minimum place value, the second water compensating valve 41 is opened, and the deoxidation pure water in the second pure water supply equipment 40 adds to
In anolyte, when anolyte is higher than highest limit value, the second water compensating valve 41 is closed.
In addition, in order to avoid there is concentration gradient in the catholyte in cathode chamber 10, so that occurring heat in cathode chamber 10
In quantity set, preferably as shown in Fig. 2, being provided with catholyte blender in above-mentioned cathode chamber 10.For same consideration, preferably
As shown in Fig. 2, being provided with anolyte blender in above-mentioned anode chamber 20.
There are many in such a way that above-mentioned recoil gas source is to realization blowback, preferably as shown in Fig. 2, above-mentioned electrolysis arsine fills
Setting further includes counter-flushing pipeline, and counter-flushing pipeline includes that main flushing pipeline 51, first rinses the flushing bye-pass of bye-pass 52, second
53, third rinses bye-pass 54 and flush loop, and main 51 one end of flushing pipeline is connected with recoil gas source；First rinses bye-pass 52
One end is connected with main flushing pipeline 51, and the other end extends to the lower part of arsenic trioxide saturated aqueous solution generator 31；Second punching
It washes 53 one end of bye-pass to be connected with main flushing pipeline 51, the other end extends to the lower part of cathode chamber 10；Third rinses bye-pass 54
One end is connected with main flushing pipeline 51, and the other end extends to the lower part of anode chamber 20；Vacuum pump 555 is provided in flush loop,
The cavity phase of flush loop and arsenic trioxide saturated aqueous solution generator 31, cathode chamber 10 and the ullage of anode chamber 20
Even.Arsenic trioxide saturated aqueous solution generator 31, cathode chamber 10 and anode chamber 20 are carried out instead using above-mentioned counter-flushing pipeline
It blows, the gases such as the arsine wherein carried secretly, oxygen is blown out, avoid its influence to electrolyte, and when equipment needs to safeguard
Above-mentioned arsenic trioxide saturated aqueous solution generator 31, cathode chamber 10 and anode chamber 20 are carried out instead using above-mentioned counter-flushing pipeline
It blows, avoids arsine pollution problem caused by electrolyte outlet.
In one embodiment, as shown in Fig. 2, above-mentioned electrolysis arsine device further includes 71 He of cathode gas transfer pipeline
Anodic gas transfer pipeline 72,71 one end of cathode gas transfer pipeline are connected with cathode chamber 10, and the other end is provided with cathode dry type
Tail gas treatment device 712；Anodic gas transfer pipeline 72 is connected with anode chamber 20, and flush loop includes major loop 551, first
Circuit 552, the second branch circuit 553 and third branch circuit 554, one end of major loop 551 and cathode dry type tail gas treatment device 712
It is connected, vacuum pump 555 is provided on major loop 551；One end of first branch circuit 552 is connected with major loop 551, other end setting
In the cavity of the ullage of arsenic trioxide saturated aqueous solution generator 31；One end of second branch circuit 553 and major loop
551 other end is connected, and the other end is connected by cathode gas transfer pipeline 71 with cathode chamber 10；The one of third branch circuit 554
End is connected with the other end of major loop 551, and the other end is connected by anodic gas transfer pipeline 72 with anode chamber 20.Backwash gas
Body respectively to arsenic trioxide saturated aqueous solution, catholyte and anolyte carry out blowback by the oxygen wherein dissolved,
The gases such as hydrogen, arsine are taken out of and are handled using the gas that cathode dry type tail gas treatment device 712 goes out blowback, with benefit
In gas non-pollution discharge；With carry out arsenic trioxide saturated aqueous solution generator 31, cathode chamber 10 and the anode chamber of blowback
20 pressure increase stops blowback when increasing to certain pressure such as 1.5bar, using the vacuum pump 555 in flush loop into
Row vacuumizes.Repeatedly repeatedly, for example 50 times as complete by blow-back therein as possible.In order to avoid cathode chamber 10 and sun
20 pressure difference of pole room is excessive to cause ion semi-permeable membrane bubbling phenomenon occur, and cathode chamber 10 and anode chamber 20 carry out blowback simultaneously and take out true
It is empty.
In a kind of embodiment of the application, as shown in Fig. 2, above-mentioned recoil gas source is source nitrogen 61 and hydrogen source 62, and main
Flushing pipeline 51 is connected by the first connecting tube 611 with source nitrogen 61, is connected by the second connecting tube 621 with hydrogen source 62, the
It is provided with first switch valve and first pressure sensor in one connecting tube 611, is provided with second switch valve in the second connecting tube 621
With second pressure sensor.Nitrogen and hydrogen are controlled by the switch valve being arranged in the first connecting tube 611 and the second connecting tube 621
Whether gas is passed through the time, smooth using the supply of corresponding pressure sensor detection gas, to guarantee the safety of system.
In addition, in order to avoid the arsine remained in cathode gas transfer pipeline 71 and anodic gas transfer pipeline 72 causes
Pollution and waste, preferably as shown in Fig. 2, above-mentioned second rinses bye-pass 53 and cathode gas transfer pipeline 71 and pass through third company
Adapter tube 80 is connected, and third connecting tube 80 rinses the interface of bye-pass 53 close to cathode chamber 10 with second, third connecting tube 80 and
The interface of cathode gas transfer pipeline 71 is provided with third switch valve on cathode chamber 10, third connecting tube 80；Third is rinsed
Bye-pass 54 is connected with anodic gas transfer pipeline 72 by the 4th connecting tube 90, and the 4th connecting tube 90 rinses branch pipe with third
The interface on road 54 is close to anode chamber 20, and the interface of the 4th connecting tube 90 and anodic gas transfer pipeline 72 is close to anode chamber 20, and the
The 4th switch valve is provided in four connecting tubes 90.Bye-pass 53 and cathode gas transfer pipeline 71 is rinsed by second to connect by third
Adapter tube 80 is connected, and third is rinsed bye-pass 54 and is connected with anodic gas transfer pipeline 72 by the 4th connecting tube 90, to cathode
Gas transfer pipeline 71 and anodic gas transfer pipeline 72 carry out blowback, that is, realize and also simplify to the blowback of remaining arsine
The circuit design of system.
Since electrolytic process is exothermic process, steamed in the arsine of catholyte and the gaseous mixture of hydrogen containing more water
Gas, the presence of these moisture influences the engineering application of arsine, in order to solve this problem, as shown in Fig. 2, it is preferred that above-mentioned cathode gas
Arsine water eliminating equipment 711 is provided with and communicated on body transfer pipeline 71, arsine water eliminating equipment 711 has liquid water out, liquid
State water out is connected with arsenic trioxide saturated aqueous solution supply unit.
It is preferred that above-mentioned arsine water eliminating equipment 711 includes liquid water eliminating equipment and vaporous water eliminating equipment, wherein liquid
Water out is arranged on liquid water eliminating equipment, and arsine vaporous water eliminating equipment is arranged under arsine liquid water eliminating equipment
Trip.
Entrainment of water vapour in the gaseous mixture of arsine and hydrogen that cathode generates, by arsine water water removal device to gaseous mixture
In vapor be removed in depth, and then effectively control the influence that vapor applies arsine.Wherein, it is removed using liquid water
The temperature of the cooling arsine of wetting system and hydrogen mixed gas can get rid of 99.9% moisture to 3 DEG C.At this moment the vapor removed
In the form of liquid water agglomerate, due in liquid water dissolved with severe toxicity arsine gas, the liquid water be unable to direct emission but
It is back to use in arsenic trioxide saturated solution supply unit and continues to use, saved cost of material and liquid water removing toxic substances cost.
Moisture content in gaseous mixture is further reduced to 50ppb or less using vaporous water eliminating equipment.Above-mentioned vaporous water eliminating equipment
The water removal device for being equipped with molecular sieve can be selected to utilize molecular sieve absorption water removal.In addition, in order to guarantee that arsine electrolysis is uninterrupted
It carries out, two vaporous water eliminating equipments in parallel is preferably provided with and communicated on cathode gas transfer pipeline 71.Two vaporous waters are gone
Except the Redundancy Design of equipment the using and the reserved, when so that one of vaporous water eliminating equipment being overhauled or regenerated, it is electrolysed arsenic processed
Alkane device is not shut down.
It can be seen from the above description that the above embodiments of the utility model achieve the following technical effects:
The application uses arsenic trioxide saturated aqueous solution as catholyte, and uses arsenic trioxide saturated water
Solution supply unit continues to provide the arsenic trioxide saturated aqueous solution of saturation to cathode chamber, to maintain cathode chamber in electrolytic process
It can be stablized with concentration of electrolyte in 10, while blowback is carried out to arsenic trioxide saturated aqueous solution using recoil gas source, avoided
Influence of the gases such as the arsine wherein carried secretly to electrolyte composition to maintain stable electrolytic efficiency, and then controls electrolysis institute
The ratio of obtained hydrogen and arsine.Above-mentioned electrolysis arsine device can not also shut down the electrolysis production for carrying out arsine, extend
It is electrolysed the maintenance period of arsine device processed and guarantees that arsine stablizes supply.
The above descriptions are merely preferred embodiments of the present invention, is not intended to limit the utility model, for this
For the technical staff in field, various modifications and changes may be made to the present invention.It is all in the spirit and principles of the utility model
Within, any modification, equivalent replacement, improvement and so on should be included within the scope of protection of this utility model.
Claims (10)
1. a kind of electrolysis arsine device processed, the electrolysis arsine device processed include:
Cathode chamber (10), the catholyte of the cathode chamber (10) are arsenic trioxide saturated aqueous solution, the cathode chamber
(10) cathode is non-sacrificial metal, and cathode chamber (10) electrolysis generates the gaseous mixture comprising arsine and hydrogen；
Anode chamber (20), the anode of the anode chamber (20) are non-sacrificial metal, and anode chamber (20) electrolysis generates oxygen；
It is characterized in that, the electrolysis arsine device processed further include:
Arsenic trioxide saturated aqueous solution supply unit is connected with the cathode chamber (10),
Recoil gas source, is connected with the arsenic trioxide saturated aqueous solution supply unit water-soluble to be saturated to the arsenic trioxide
Arsenic trioxide saturated aqueous solution in liquid supply unit carries out blowback.
2. electrolysis arsine device processed according to claim 1, which is characterized in that the arsenic trioxide saturated aqueous solution supplies
The unit is answered to include:
Arsenic trioxide saturated aqueous solution generator (31), the recoil gas source and the arsenic trioxide saturated aqueous solution occur
Device (31) is connected；
Liquid supply pipe (32)；
Liquid back pipe (33), the arsenic trioxide saturated aqueous solution generator (31), the liquid supply pipe (32), the liquid back pipe
(33) circulation loop is constituted with the cathode chamber (10).
3. electrolysis arsine device processed according to claim 2, which is characterized in that the arsenic trioxide saturated aqueous solution supplies
Answering unit further includes the first pure water supply equipment (34), the arsenic trioxide saturated aqueous solution generator (31) and described first
Pure water supply equipment (34) is connected by the first water supplying pipe.
4. electrolysis arsine device processed according to claim 3, which is characterized in that the arsenic trioxide saturated aqueous solution hair
It is additionally provided with saturation liquid level sensor (312) in raw device (31), is provided with the first water compensating valve (341) on first water supplying pipe,
The saturation liquid level sensor (312) is electrically connected with first water compensating valve (341).
5. electrolysis arsine device processed according to claim 2, which is characterized in that the cathode chamber (10) is additionally provided with cathode
Liquid level sensor (11), solution feed pump (321) and supplying valve (322) are provided on the liquid supply pipe (32), and the cathode liquid level passes
Sensor (11) is electrically connected with the solution feed pump (321) and supplying valve (322).
6. electrolysis arsine device processed according to claim 1, which is characterized in that the anode chamber (20) is provided with anolyte
Level sensor (21), the electrolysis arsine device processed further includes the second pure water supply equipment (40), and the second pure water supply is set
Standby (40) are connected with the anode chamber (20) by the second water supplying pipe, are provided with the second water compensating valve on second water supplying pipe
(41), the anode liquid level sensor (21) is electrically connected with second water compensating valve (41).
7. electrolysis arsine device processed according to any one of claim 1 to 6, which is characterized in that the electrolysis arsine processed
Device further includes counter-flushing pipeline, and the counter-flushing pipeline includes:
Main flushing pipeline (51), one end are connected with the recoil gas source；
First rinses bye-pass (52), and one end is connected with the main flushing pipeline (51), and the other end extends to three oxidation two
The lower part of arsenic saturated aqueous solution generator (31)；
Second rinses bye-pass (53), and one end is connected with the main flushing pipeline (51), and the other end extends to the cathode chamber
(10) lower part；
Third rinses bye-pass (54), and one end is connected with the main flushing pipeline (51), and the other end extends to the anode chamber
(20) lower part；
Flush loop is provided with vacuum pump (555) in the flush loop, and the flush loop and the arsenic trioxide are saturated
Water solution generator (31), the cathode chamber (10) are connected with the cavity of the ullage of the anode chamber (20).
8. electrolysis arsine device processed according to claim 7, which is characterized in that the electrolysis arsine device processed further include:
Cathode gas transfer pipeline (71), one end are connected with the cathode chamber (10), and the other end is provided at cathode dry type tail gas
It manages equipment (712)；
Anodic gas transfer pipeline (72) is connected with the anode chamber (20),
The flush loop includes:
Major loop (551), one end of the major loop (551) is connected with the cathode dry type tail gas treatment device (712), described
The vacuum pump (555) are provided on major loop (551)；
One end of first branch circuit (552), first branch circuit (552) is connected with the major loop (551), other end setting
In the cavity of the ullage of the arsenic trioxide saturated aqueous solution generator (31)；
One end of second branch circuit (553), second branch circuit (553) is connected with the other end of the major loop (551), separately
One end is connected by the cathode gas transfer pipeline (71) with the cathode chamber (10)；
One end of third branch circuit (554), the third branch circuit (554) is connected with the other end of the major loop (551), separately
One end is connected by the anodic gas transfer pipeline (72) with the anode chamber (20).
9. electrolysis according to claim 8 arsine device processed, which is characterized in that the recoil gas source for source nitrogen (61) and
Hydrogen source (62), and the main flushing pipeline (51) is connected by the first connecting tube (611) with source nitrogen (61), is connected by second
Adapter tube (621) is connected with hydrogen source (62), and the first connecting tube is provided with first switch valve and first pressure sensor on (611),
Second connecting tube is provided with second switch valve and second pressure sensor on (621).
10. electrolysis according to claim 8 arsine device processed, which is characterized in that described second rinse bye-pass (53) with
The cathode gas transfer pipeline (71) is connected by third connecting tube (80), and the third connecting tube (80) and described second
The interface of bye-pass (53) is rinsed close to the cathode chamber (10), the third connecting tube (80) and the cathode gas delivery pipe
The interface on road (71) is provided with third switch valve on the cathode chamber (10), the third connecting tube (80)；The third
It rinses bye-pass (54) and is connected with the anodic gas transfer pipeline (72) by the 4th connecting tube (90), and the 4th connection
It manages (90) and the third rinses the interface of bye-pass (54) close to the anode chamber (20), the 4th connecting tube (90) and institute
The interface for stating anodic gas transfer pipeline (72) is provided with the 4th on the anode chamber (20), the 4th connecting tube (90)
Switch valve.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821990303.2U CN209243190U (en) | 2018-11-29 | 2018-11-29 | It is electrolysed arsine device processed |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201821990303.2U CN209243190U (en) | 2018-11-29 | 2018-11-29 | It is electrolysed arsine device processed |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114438534A (en) * | 2022-01-05 | 2022-05-06 | 飞马牧场(上海)信息咨询服务有限公司 | High-purity gas preparation device and preparation method |
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2018
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114438534A (en) * | 2022-01-05 | 2022-05-06 | 飞马牧场(上海)信息咨询服务有限公司 | High-purity gas preparation device and preparation method |
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Effective date of registration: 20210210 Address after: Unit 611, unit 3, 6 / F, building 1, yard 30, Yuzhi East Road, Changping District, Beijing 102208 Patentee after: Zishi Energy Co.,Ltd. Address before: Room a129-1, No. 10, Zhongxing Road, science and Technology Park, Changping District, Beijing Patentee before: DONGTAI HI-TECH EQUIPMENT TECHNOLOGY Co.,Ltd. |