CN105018960B - The concentration rectificating method of hydrogen iodide in a kind of hydroiodic acid containing iodine - Google Patents
The concentration rectificating method of hydrogen iodide in a kind of hydroiodic acid containing iodine Download PDFInfo
- Publication number
- CN105018960B CN105018960B CN201510438380.1A CN201510438380A CN105018960B CN 105018960 B CN105018960 B CN 105018960B CN 201510438380 A CN201510438380 A CN 201510438380A CN 105018960 B CN105018960 B CN 105018960B
- Authority
- CN
- China
- Prior art keywords
- hydroiodic acid
- tower
- concentration
- iodine
- rectifying column
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The concentration rectificating method of hydrogen iodide, is related to technical field of chemical separation in a kind of hydroiodic acid containing iodine.The present invention is on electrolytic electro-dialysis device, in catholyte discharging opening or at least one cathodic region of negative electrode discharging opening, bridge line is set, these bridge lines are connected with the tower body or tower reactor of rectifying column, heat preservation component and valve are carried in bridge line, the tower top of rectifying column is connected with decompressor；Due to being additionally arranged bridge line on electrolytic electro-dialysis device, so that electrolytic electro-dialysis (EED) intercouples with rectification under vacuum, HI in negative electrode feed liquid can be quickly moved out so that hydroiodic acid containing iodine avoids catholyte and HI and H in anolyte in EED concentration process2O concentration difference is too high and HI reverse migration occurs；On the other hand, anode region will promote anode region H due to the pressure with higher than cathodic region+Migration to cathodic region, be advantageous to cathodic region HI concentration, so as to substantially increase HI concentrating and separating efficiency.
Description
Technical field
The present invention relates to technical field of chemical separation, more particularly in hydroiodic acid containing iodine hydrogen iodide concentration rectificating method.
Background technology
The feed liquid of hydroiodic acid containing iodine (i.e. hydrogen iodide-iodo- water ternary solution, HI-I2-H2O, abbreviation HIx) distillation operation,
It can all be used in heat chemistry iodine-sulfur process hydrogen production by water decomposition technique, and the production technology of hydroiodic acid or hydrogen iodide (HI).In the past
Exemplified by person, in heat chemistry iodine-sulfur process hydrogen production process, the hydroiodic acid of generation is reacted by Bunsen, it is excessive due to adding
Iodine, form HI-I2-H2O things phase can isolate the hydrogen iodide prepared required for hydrogen, it is necessary to by distillation operation.
Due to the characteristic of material in itself, rectifying separation is carried out to the hydrogen iodide in HIx using current technology and is not easy to.
Due to HI and H2Mol ratio 1 can be formed between O：5 azeotrope, and Bunsen reacts what is provided in above-mentioned iodine-sulfur process technique
In HIx, HI concentration is often below azeotropic concentration, or has just reached azeotropic concentration, so if to HIx using directly distillation
Or if rectifying, although HI can be obtained, the evaporation that substantial amounts of heat energy is used for water is had, the economy of technique will significantly drop
It is low.Given this situation, domestic and international researcher propose：Electrolytic electro-dialysis (EED) concentration, the negative electrode of EED equipment are carried out to HIx first
HI concentration can be enhanced in the HIx feed liquids of area's outflow, be formed more than azeotropic, i.e. HI:H2O>1:5, like this in distillation/rectifying
During, HI can be steamed largely, and the amount of steaming of water is seldom, after optimize technique, or even can obtain pure HI gases, highly beneficial
In the raising of iodine-sulfur process technique whole efficiency.
Specifically, electrolytic electro-dialysis (Electrolysis and electrodialysis device, abbreviation
" EED ") it is a kind of high-efficiency electrochemical method for concentration, also known as ion exchange membrane electrolysis or membrane electrolysis, it is also possible to make special
Determine the electrochemistry formated of chemicals.HIx EED concrete principles are：When yin, yang the two poles of the earth have, HIx material flows are out-of-date, H+In electric field
Under effect, film is passed through through proton selective, cathodic region is entered by anode region, while occur on two-plate as bottom electrode is anti-
Should：
Anode：2I--2e→I2
Negative electrode：I2+2e→2I-
It is integrating as a result, anode region H+、I-Reduce, I2Increase, and cathodic region I2Reduce, H+、I-Increase, i.e., HI exists
Cathodic region is concentrated.When HI concentration surmounts constant boiling point and reaches specific concentration ranges, you can carry out essence to negative electrode material
Operation is evaporated, the HI-H of high HI concentration is obtained in rectifying tower top2O solution or HI gases.
Above-mentioned EED- rectifying group technology has been obtained for the concern and accreditation of lot of domestic and international researcher, in China, day
Originally, on the iodine-sulfur process hydrogen manufacturing stand of South Korea, HI concentrating and separating has been carried out using this scheme.However as research work
Development, EED some limitations also gradually reveal, most important of which is that the HI during EED in catholyte is not
Can according to anticipation ideal style constantly, rapidly enrichment.With EED progress, HI and H in the solution of yin, yang the two poles of the earth2O's
Concentration difference is constantly lifted, specifically, HI concentration more and more higher HI in anolyte concentration in catholyte, so, in height
Under the promotion of concentration difference, H+Will be by negative electrode dialysis to anode, and the situation of water will be then on the contrary, increasingly will tend to be entered by anolyte
Enter catholyte, both the above trend, will make it that catholyte HI concentration can not be constantly improve, when the concentration difference of catholyte, anolyte
After reaching to a certain degree, or even the phenomenon that catholyte HI concentration falls after rise occurs.HI caused by above-mentioned concentration difference is reversely migrated, with
And water accelerates into the problem of cathodic region and can significantly reduce EED disposal ability, it is difficult to provides higher HI for follow-up rectifier unit
The feed liquid of concentration so that this HI separation process of EED- rectifying is difficult to effectively run, and then ties down whole iodine-sulfur process hydrogen manufacturing work
The high-efficiency operation of skill.
If suitable measure can be taken, suppress to produce excessive concentration difference between cathode and anode liquid, then can avoid above-mentioned
Problem, improve HI concentrating and separating efficiency.Substantial amounts of experimental data and theoretical calculation show that HI concentration surpasses in hydroiodic acid containing iodine
Cross HI-H2After azeotropic concentration between O, due to the violent raising of vapour pressure, its boiling point can be remarkably decreased, at reduced pressure conditions, very
Easily produce HI gases.If electrolytic electro-dialysis (EED) is coupled with rectification under vacuum according to this rule, i.e., by EED the moon
Polar region is connected with vacuum rectification tower, can just pipette out in time by the HI in catholyte, reduces the concentration between cathode and anode liquid
Difference, above-mentioned a series of problems is avoided, improve EED running efficiency.
The content of the invention
It is an object of the invention to provide a kind of concentration rectificating method of hydrogen iodide in hydroiodic acid containing iodine, by the way that electricity will be electrolysed
Dialysis (EED) is coupled with rectification under vacuum, the HI in catholyte is quickly moved out so that hydroiodic acid containing iodine is concentrated in EED
Cheng Zhong, avoid catholyte and HI and H in anolyte2O concentration differences are too high and HI reverse migration occurs, so as to improve HI concentration
Separative efficiency.
Technical scheme is as follows：
1) on electrolytic electro-dialysis device, at least one negative electrode with catholyte discharging opening or close to negative electrode discharging opening
Bridge line is set in area, and these bridge lines are connected with the tower body or tower reactor of rectifying column, and insulation portion is carried in bridge line
Part and valve, the tower top of rectifying column are connected with decompressor；
2) valve in bridge line is located at cut-off state, the high concentration of hydrogen without iodine is added into the tower reactor of rectifying column
Acid iodide, or low content of iodine, the hydroiodic acid containing iodine of high HI contents；In the high concentration of hydrogen acid iodide without iodine, HI：H2O mole
Than for 1：4.5~6.0；The low content of iodine, high HI contents hydroiodic acid containing iodine in, the mol ratio of each component is HI：H2O：I2
=1：4.5~6.0：0~0.4；
3) start the tower body and tower reactor heater of rectifying column, and the condensation reflux unit of rectifying tower top, open rectifying
The decompressor of tower top, distillation operation is carried out under total reflux mode；
4) when the hydroiodic acid backflow that rectifying column tower top condensation reflux unit can be stablized, negative electrode will be used as just to expect
The solution of hydroiodic acid containing iodine of liquid and the solution of hydroiodic acid containing iodine as the initial feed liquid of anode, are delivered to electrolytic electro-dialysis device respectively
Cathodic region and anode region, carry out electrolytic electro-dialysis operation, the discharge liquid in cathodic region is transported to rectifying column after collection
Tower body or tower reactor；
5) open and adjust the valve in bridge line, gas caused by electrolytic electro-dialysis equipment cathodic region is entered rectifying
The tower body of tower, and continue to carry out material extraction from rectifying tower top and tower reactor.
Rectifying column of the present invention is packed tower；The initial feed liquid of described negative electrode, the initial feed liquid of anode and electrolysis electric osmose
The temperature control of analysis apparatus is at 90 DEG C between feed liquid bubble point temperature.
The technical characteristic of the present invention is also resided in, and filler is housed in described bridge line.
The present invention has the technique effect of advantages below and high-lighting：In the method for the invention, due in electrolysis electric osmose
Bridge line is additionally arranged on analysis apparatus so that electrolytic electro-dialysis (EED) intercouples with rectification under vacuum, can be by negative electrode feed liquid
HI is quickly moved out so that hydroiodic acid containing iodine avoids catholyte and HI and H in anolyte in EED concentration process2O concentration difference
Reverse migration too high and that HI occurs, so as to improve HI concentrating and separating efficiency.On the other hand, anode region due to higher than
The pressure in cathodic region, anode region H will be promoted+Migration to cathodic region, be advantageous to cathodic region HI concentration.Due to more than on both side
The reason for, method proposed by the present invention can increase substantially HI concentrating and separating efficiency.
Brief description of the drawings
Fig. 1 is equipment schematic diagram used in the concentration rectificating method of hydrogen iodide in a kind of hydroiodic acid containing iodine of the present invention, should
Schematic diagram is by taking the electrolytic electro-dialysis equipment with 4 units as an example.
1- cathode end plates；2- bipolar plates；3- anode end plates；Cathodic region in 4a- cathode end plates；The moon in 4b- bipolar plates
Polar region；Anode region on 5a- anode end plates；Anode region in 5b- bipolar plates；6- proton selective exchange membranes；7- pads；8- is cloudy
Pole feeding line；Feed liquid pipeline between 9- cathode electrode units；10- negative electrodes discharging pipeline；11- anode feed pipelines；Between 12- anode units
Feed liquid pipeline；13- anodes discharging pipeline；14- bridge lines；15- valves；16- cathode terminals；17- anode terminals
Embodiment
The embodiment of the present invention is elaborated below in conjunction with the accompanying drawings.
The concentration rectificating method of hydrogen iodide in hydroiodic acid containing iodine proposed by the present invention, it is in electrolytic electro-dialysis-rectifying coupling
Carried out in equipment.As shown in figure 1, electrolytic electro-dialysis device is mainly bipolar including cathode end plate 1, one or more in structure
Plate 2, and anode end plate 3.Possess in cathode end plate 1 containing the cathodic region 4a in cathode end plate, anode end plate 3 on anode end plate
Anode region 5a, and bipolar plates 2 then have cathodic region and anode region respectively in its both sides, i.e., the cathodic region 4b in bipolar plates and double
Anode region 5b on pole plate.
Between end plate and bipolar plates and between adjacent bipolar plates, there is provided proton selective exchange membrane 6 and pad
7。
The center of each pad is hollowed out, so that adjacent cathodic region and anode region are only with proton selective exchange membrane
It is separated by, by proton selective exchange membrane mass transfer occurs for catholyte and anolyte, i.e.,：It is separated by by proton selective exchange membrane,
Neighbouring cathode area and anode region form electrolytic electro-dialysis processing unit.
Pending catholyte enters electrolytic electro-dialysis device, the feed liquid pipe between cathode electrode unit from negative electrode feeding line 8
Line 9, flows through each cathodic region successively, including the cathodic region 4b on the cathodic region 4a and bipolar plates in cathode end plate, then via
Negative electrode discharging pipeline 10 is discharged.
Pending anolyte enters electrolytic electro-dialysis device, the feed liquid pipe between anode unit from anode feed pipeline 11
Line 12, flows through each anode region successively, including the anode region 5b on the anode region 5a and bipolar plates on anode end plate, then via
Anode discharging pipeline 13 is discharged.
The positive pole of dc source is connected with the anode terminal 17 of electrolytic electro-dialysis device, by the negative pole of dc source with
The cathode terminal 16 of electrolytic electro-dialysis device connects, and turns on the power power supply, then flows through the anolyte of above-mentioned anode region with flowing through
The catholyte in cathodic region, mass transfer will be occurred by proton selective exchange membrane in the presence of electric field, concentration difference etc..
As described above, the electrolytic electro-dialysis device shown in Fig. 1 contains 4 processing units, it is clear that can be double by increasing
Pole plate, and the pad that matches and proton selective exchange membrane obtain having the electrolytic electro-dialysis of more crosspoints to fill
Put.
In the example of fig. 1, bridge is set on the cathodic region with catholyte discharging opening, and cathodic region adjacent thereto
Adapter line 14, these bridge lines are connected with the tower body or tower reactor of rectifying column, attemperator are carried in bridge line, and install
Valve 15, filler is housed in bridge line.Above-mentioned rectifying column is packed tower, and tower top is connected with decompressor, so as to enter
Row rectification under vacuum operates.
The concentration rectificating method of hydrogen iodide, its concrete technology step are as follows in a kind of hydroiodic acid containing iodine provided by the invention：
1) on electrolytic electro-dialysis device, with catholyte discharging opening or close at least one cathodic region of negative electrode discharging opening
Upper setting bridge line, these bridge lines are connected with the tower body or tower reactor of rectifying column, and attemperator is carried in bridge line
And valve, filler is housed in bridge line.Above-mentioned rectifying column is packed tower, and tower top is connected with decompressor, so as to enter
Row rectification under vacuum operates；
2) valve described in step 1) in bridge line is located at cut-off state, adds and be free of into the tower reactor of rectifying column
The high concentration of hydrogen acid iodide of iodine, or low content of iodine, the hydroiodic acid containing iodine of high HI contents；In the high concentration of hydrogen acid iodide without iodine,
HI：H2O mol ratio is 1：4.5~6.0；The low content of iodine, high HI contents hydroiodic acid containing iodine in, the mol ratio of each component
For HI：H2O：I2=1：4.5~6.0：0~0.4；
3) start the tower body and tower reactor heater of rectifying column, and rectifying tower top condensation reflux unit, open rectifying column
The decompressor on top, distillation operation is carried out under total reflux mode；
4) when the hydroiodic acid backflow that overhead condensate reflux device can be stablized, using containing as the initial feed liquid of negative electrode
Iodine hydroiodic acid solution, and the solution of hydroiodic acid containing iodine as the initial feed liquid of anode, the moon of electrolytic electro-dialysis device is delivered to respectively
Polar region and anode region, carry out electrolytic electro-dialysis operation, and the discharge liquid in cathodic region is transported to the tower body of rectifying column after collection
Or tower reactor.The temperature control of the initial feed liquid of above-mentioned negative electrode, the initial feed liquid of anode and electrolytic electro-dialysis device is steeped at 90 DEG C to feed liquid
Between point temperature.
5) valve in opening and adjusting 1) in bridge line, enter gas caused by electrolytic electro-dialysis equipment cathodic region
Rectifying column, and continue to carry out material extraction from rectifying tower top and bottom of towe, overhead product is HI gases or the HI-H of high HI concentration2O
Solution.
As described above, the electrolytic electro-dialysis device shown in Fig. 1 contains 4 crosspoints, it is clear that can be double by increasing
Pole plate, and the pad that matches and proton selective exchange membrane obtain having the electrolytic electro-dialysis of more crosspoints to fill
Put.
In the example of fig. 1, bridge is set on the cathodic region with catholyte discharging opening, and cathodic region adjacent thereto
Adapter line 14, these bridge lines are connected with the tower body or tower reactor of rectifying column, attemperator are carried in bridge line, and install
Valve 15, filler is housed in bridge line.Above-mentioned rectifying column is packed tower, and tower top is connected with decompressor, so as to enter
Row rectification under vacuum operates.
With reference to several embodiments, the present invention is described further.
Embodiment 1
In the present embodiment, electrolytic electro-dialysis device used and the equipment shown in Fig. 1 are similar, and it contains 4 and exchanges list
Member, the exchange area of each unit, i.e., effective exchange area of proton selective exchange membrane is possessed by each unit
150cm2.In cathodic region (the i.e. cathodic region for that unit that catholyte finally flows through, and electrolysis for possessing catholyte discharging opening
The cathodic region farthest apart from catholyte entrance in electrodialysis plant), install the bridge line that internal diameter is 2cm, this root bridge pipe additional
Line is connected with the tower body of a rectifying column, and attemperator and valve are carried in bridge line, Ф 2mm* are housed in bridge line
5mm glass spring filler.
Above-mentioned rectifying column is packed tower, and tower top is furnished with decompressor, and the internal diameter of packed tower is 5cm, and built-in filler is Ф
3mm*20mm glass spring filler, bed stuffing height 1.25m；The volume of rectifying still is 1.5L, the heating equipped with power 1kW
Set.
Before starting the operation, the valve in bridge line is located at cut-off state first, adds and be free of into rectifying still
The hydroiodic acid 1.5L of iodine, the mol ratio of HI and water is HI in the hydroiodic acid：H2O=1:5.8.
Operation of driving is implemented to rectifying device, starts the tower body of rectifying column and the heater of tower reactor, and rectifying tower top
Condensation reflux unit, the decompressor of rectifying tower top is opened, operated under total reflux mode.After 30min, overhead condensation returns
The hydroiodic acid backflow that stream device can be stablized.
By the starting material HI of electrolytic electro-dialysis:H2O:I2=1:5.40:1.25 feed liquid of hydroiodic acid containing iodine is divided into two strands,
Respectively as the catholyte and anolyte of electrolytic electro-dialysis device, electrolytic electro-dialysis dress is respectively enterd with 20ml/min flow velocity
The cathodic region and anode region put, feed temperature are 100 DEG C, and the control of electrolytic electro-dialysis unit temp is 105 DEG C.Open dc source
Power supply, current strength 16A.Collect cathodic region discharge liquor respectively and anode region discharge liquor, the discharge liquid in wherein cathodic region exist
The tower reactor of rectifying column is transported to after collection.
Open and adjust the valve in bridge line, gas caused by electrolytic electro-dialysis device cathodic region is entered rectifying
Tower, and continue to carry out material extraction, overhead product HI from rectifying tower top and bottom of towe：H2O=1：4.2 hydroiodic acid solution.
Embodiment 2
In the present embodiment, electrolytic electro-dialysis device and the equipment shown in Fig. 1 are similar, but it contains 10 and exchanges list
Member, the exchange area of each unit, i.e., effective exchange area of proton selective exchange membrane is possessed by each unit
70cm2.In cathodic region (the i.e. cathodic region for that unit that catholyte finally flows through, and electrolysis for possessing catholyte discharging opening
The cathodic region farthest apart from catholyte entrance in electrodialysis plant), and a cathodic region adjacent thereto (i.e. reciprocal the of equipment
Two cathodic regions), install the bridge line that internal diameter is 3cm additional, this two bridge lines are connected with the tower body of a rectifying column,
Attemperator and valve are carried in bridge line, Ф 3mm*10mm glass spring filler is housed in bridge line.
Above-mentioned rectifying column is packed tower, and tower top is furnished with decompressor, and the internal diameter of packed tower is 5cm, and built-in filler is Ф
3mm*20mm glass spring filler, bed stuffing height 1.25m；The volume of rectifying still is 2L, the heating equipped with power 1kW
Set.
Before starting the operation, the valve in bridge line is located at cut-off state first, adds and be free of into rectifying still
The hydroiodic acid 1.5L of iodine, the mol ratio of HI and water is HI in the hydroiodic acid：H2O=1:4.9.
Operation of driving is implemented to rectifying device, starts the tower body of rectifying column and the heater of tower reactor, and rectifying tower top
Condensation reflux unit, the decompressor of rectifying tower top is opened, operated under total reflux mode.After 30min, overhead condensation returns
The hydroiodic acid backflow that stream device can be stablized.
By the starting material HI of electrolytic electro-dialysis:H2O:I2=1:5.70:1.50 feed liquid of hydroiodic acid containing iodine is divided into two strands,
Respectively as the catholyte and anolyte of electrolytic electro-dialysis device, electrolytic electro-dialysis dress is respectively enterd with 30ml/min flow velocity
The cathodic region and anode region put, feed temperature are 90 DEG C, and the control of electrolytic electro-dialysis unit temp is 95 DEG C.Dc source is opened to supply
Electricity, current strength 7.5A.Collect cathodic region discharge liquor respectively and anode region discharge liquor, the discharge liquid in wherein cathodic region are being received
The tower reactor of rectifying column is transported to after collection.
Open and adjust the valve in bridge line, gas caused by electrolytic electro-dialysis device cathodic region is entered rectifying
Tower, and continue to carry out material extraction, overhead product HI from rectifying tower top and bottom of towe：H2O=1：3.5 hydroiodic acid solution.
Embodiment 3
In the present embodiment, electrolytic electro-dialysis device and the equipment shown in Fig. 1 are similar, but it contains 15 and exchanges list
Member, the exchange area of each unit, i.e., effective exchange area of proton selective exchange membrane is possessed by each unit
200cm2.In cathodic region (the i.e. cathodic region for that unit that catholyte finally flows through, and electrolysis for possessing catholyte discharging opening
The cathodic region farthest apart from catholyte entrance in electrodialysis plant), and a cathodic region adjacent thereto (i.e. reciprocal the of equipment
Two cathodic regions), install the bridge line that internal diameter is 5cm additional, these bridge lines are connected with the tower body of a rectifying column, bridge
Attemperator and valve are carried on adapter line, Ф 3mm*10mm glass spring filler is housed in bridge line.Above-mentioned rectifying column
For packed tower, and tower top is furnished with decompressor.
The internal diameter of above-mentioned distilling filled tower is 10cm, and built-in filler is Ф 3mm*30mm glass spring filler, packing layer
Highly it is 2.0m；Rectifying still volume is 5.5L, the heating mantle equipped with power 5kW.
Before starting the operation, the valve in bridge line is located at cut-off state first, low iodine is added into rectifying still
The 3.5L of hydroiodic acid containing iodine of content, high HI contents, the mol ratio of the feed liquid each component is HI：H2O：I2=1：4.95：0.35；
Operation of driving is implemented to rectifying device, starts the tower body of rectifying column and the heater of tower reactor, and rectifying tower top
Condensation reflux unit, the decompressor of rectifying tower top is opened, operated under total reflux mode.After 35min, overhead condensation returns
The hydroiodic acid backflow that stream device can be stablized.
By the starting material HI of electrolytic electro-dialysis:H2O:I2=1:6.50:1.80 feed liquid of hydroiodic acid containing iodine is divided into two strands,
Respectively as the catholyte and anolyte of electrolytic electro-dialysis device, electrolysis electricity is delivered into respectively with 120ml/min flow velocity
The cathodic region and anode region of electrodialysis apparatus, feed temperature are 98 DEG C, and it is 98 DEG C that electrolytic electro-dialysis device, which equally controls temperature,.Open
Dc source is powered, current strength 30A.The row of cathodic region discharge liquor and anode region discharge liquor, wherein cathodic region is collected respectively
Go out the tower reactor that liquid is transported to rectifying column after collection.
Open and adjust the valve in bridge line, gas caused by electrolytic electro-dialysis device cathodic region is entered rectifying
Tower, and continue to carry out material extraction, overhead product HI from rectifying tower top and bottom of towe：H2O=1：4.2 hydroiodic acid solution.
Embodiment 4
In the present embodiment, electrolytic electro-dialysis device and the equipment shown in Fig. 1 are similar, but it contains 35 and exchanges list
Member, the exchange area of each unit, i.e., effective exchange area of proton selective exchange membrane is possessed by each unit
600cm2.In cathodic region (the i.e. cathodic region for that unit that catholyte finally flows through, and electrolysis for possessing catholyte discharging opening
The cathodic region farthest apart from catholyte entrance in electrodialysis plant), and two cathodic region (i.e. electrolytic electro-dialysis adjacent thereto
Second from the bottom and the 3rd cathodic region of device), install the bridge line that internal diameter is 8cm, these bridge lines and an essence additional
The tower body for evaporating tower is connected, and attemperator and valve are carried in bridge line, and Ф 3mm*10mm glass is housed in bridge line
Spring filler.Above-mentioned rectifying column is packed tower, and tower top is furnished with decompressor.
The internal diameter of above-mentioned distilling filled tower is 15cm, and built-in filler is Ф 3mm*30mm glass spring filler, packing layer
Highly it is 2.0m；Rectifying still volume is 15L, the heating mantle equipped with power 10kW.
Before starting the operation, the valve in bridge line is located at cut-off state first, low iodine is added into rectifying still
The 10L of hydroiodic acid containing iodine of content, high HI contents, the mol ratio of the feed liquid each component is HI：H2O：I2=1：5.2：0.2；
Operation of driving is implemented to rectifying device, starts the tower body of rectifying column and the heater of tower reactor, and rectifying tower top
Condensation reflux unit, the decompressor of rectifying tower top is opened, operated under total reflux mode.After 35min, overhead condensation returns
The hydroiodic acid backflow that stream device can be stablized.
By the negative electrode starting material of electrolytic electro-dialysis, i.e. HI:H2O:I2=1:6.20:1.90 feed liquid of hydroiodic acid containing iodine, and
Anode starting material, i.e. HI:H2O:I2=1:5.50:1.50 feed liquid of hydroiodic acid containing iodine, it is defeated with 800ml/min flow velocity difference
The cathodic region and anode region of electrolytic electro-dialysis device are sent into, feed temperature is 105 DEG C, and electrolytic electro-dialysis device controls the temperature to be
110℃.Open dc source power supply, current strength 90A.Cathodic region discharge liquor and anode region discharge liquor are collected respectively, wherein
The discharge liquid in cathodic region is transported to the tower reactor of rectifying column after collection.
Open and adjust the valve in bridge line, gas caused by electrolytic electro-dialysis device cathodic region is entered rectifying
Tower, and continue to carry out material extraction, overhead product HI from rectifying tower top and bottom of towe：H2O=1：3.9 hydroiodic acid solution.
Claims (3)
1. the concentration rectificating method of hydrogen iodide in a kind of hydroiodic acid containing iodine, it is characterised in that this method is carried out as follows：
1) on electrolytic electro-dialysis device, in catholyte discharging opening or at least one cathodic region of negative electrode discharging opening
Bridge line is set, these bridge lines are connected with the tower body or tower reactor of rectifying column, in bridge line with heat preservation component and
Valve, the tower top of rectifying column are connected with decompressor；Filler is housed in described bridge line；
2) valve in bridge line is located at cut-off state, the high concentration of hydrogen iodine without iodine is added into the tower reactor of rectifying column
Acid, or low content of iodine, the hydroiodic acid containing iodine of high HI contents；In the high concentration of hydrogen acid iodide without iodine, HI：H2O mol ratio
For 1：4.5~6.0；The low content of iodine, high HI contents hydroiodic acid containing iodine in, the mol ratio of each component is HI：H2O：I2=
1：4.5~6.0：0~0.4；
3) start the tower body and tower reactor heater of rectifying column, and the condensation reflux unit of rectifying tower top, open rectifying tower top
Decompressor, distillation operation is carried out under total reflux mode；
4) when the hydroiodic acid backflow that rectifying column tower top condensation reflux unit can be stablized, using as the initial feed liquid of negative electrode
The solution of hydroiodic acid containing iodine and the solution of hydroiodic acid containing iodine as the initial feed liquid of anode, the moon of electrolytic electro-dialysis device is delivered to respectively
Polar region and anode region, carry out electrolytic electro-dialysis operation, and the discharge liquid in cathodic region is transported to the tower body of rectifying column after collection
Or tower reactor；
5) open and adjust the valve in bridge line, gas caused by electrolytic electro-dialysis equipment cathodic region is entered rectifying column
Tower body, and continue to carry out material extraction from rectifying tower top and tower reactor.
2. the concentration rectificating method of the hydroiodic acid according to claim 1 containing iodine, it is characterised in that the rectifying column is filler
Tower.
3. the concentration rectificating method of the feed liquid of hydroiodic acid containing iodine according to claim 1 or 2, it is characterised in that described the moon
The temperature control of extremely initial feed liquid, the initial feed liquid of anode and electrolytic electro-dialysis device is at 90 DEG C between feed liquid bubble point temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510438380.1A CN105018960B (en) | 2015-07-23 | 2015-07-23 | The concentration rectificating method of hydrogen iodide in a kind of hydroiodic acid containing iodine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510438380.1A CN105018960B (en) | 2015-07-23 | 2015-07-23 | The concentration rectificating method of hydrogen iodide in a kind of hydroiodic acid containing iodine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105018960A CN105018960A (en) | 2015-11-04 |
| CN105018960B true CN105018960B (en) | 2017-11-14 |
Family
ID=54409248
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510438380.1A Active CN105018960B (en) | 2015-07-23 | 2015-07-23 | The concentration rectificating method of hydrogen iodide in a kind of hydroiodic acid containing iodine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105018960B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107904617B (en) * | 2017-11-23 | 2019-04-23 | 浙江大学 | With the method and device of electrochemical decomposition HI hydrogen manufacturing in the circulation hydrogen manufacturing of sulphur iodine |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101545114A (en) * | 2009-05-08 | 2009-09-30 | 清华大学 | Electrolysis-electrodialysis device |
| CN102847334A (en) * | 2012-09-14 | 2013-01-02 | 清华大学 | Method and apparatus for rectifying iodine-containing hydriodic acid liquid |
| CN102854082A (en) * | 2012-08-29 | 2013-01-02 | 清华大学 | Evaluation method for condensation effect of hydrogen iodide in iodine-containing hydriodic acid by using electrolysis-electrodialysis device |
| CN103212215A (en) * | 2013-04-01 | 2013-07-24 | 清华大学 | Method for rectifying iodine-containing hydriodic acid feed liquid |
| CN104085857A (en) * | 2014-06-26 | 2014-10-08 | 周海军 | New method for preparing high-purity hydroiodic acid |
-
2015
- 2015-07-23 CN CN201510438380.1A patent/CN105018960B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101545114A (en) * | 2009-05-08 | 2009-09-30 | 清华大学 | Electrolysis-electrodialysis device |
| CN102854082A (en) * | 2012-08-29 | 2013-01-02 | 清华大学 | Evaluation method for condensation effect of hydrogen iodide in iodine-containing hydriodic acid by using electrolysis-electrodialysis device |
| CN102847334A (en) * | 2012-09-14 | 2013-01-02 | 清华大学 | Method and apparatus for rectifying iodine-containing hydriodic acid liquid |
| CN103212215A (en) * | 2013-04-01 | 2013-07-24 | 清华大学 | Method for rectifying iodine-containing hydriodic acid feed liquid |
| CN104085857A (en) * | 2014-06-26 | 2014-10-08 | 周海军 | New method for preparing high-purity hydroiodic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105018960A (en) | 2015-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103145150B (en) | Technology and device for recycling sodium chloride from wastewater generated in process of producing silica sol by ion exchange method | |
| CN103709016B (en) | A kind of pervaporation method refines technique and the device of glycol dimethyl ether | |
| CN110642228B (en) | Calcium carbide method PVC mercury-containing waste acid treatment system and method for treating waste acid by using same | |
| CN104926675A (en) | Recovery process of low concentration dimethylacetamide | |
| CN106145488A (en) | Ammonia nitrogen recovery equipment and multi-section ammonia nitrogen wastewater treatment system | |
| WO2011085669A1 (en) | Low-temperature heat-driven distillation separation apparatus for evaporating aqueous solution under negative pressure and method for obtaining distilled water | |
| CN113957459A (en) | Method for producing bromine and caustic soda by electrolyzing sodium bromide through ion membrane | |
| CN105018960B (en) | The concentration rectificating method of hydrogen iodide in a kind of hydroiodic acid containing iodine | |
| CN107365258A (en) | The preparation facilities and preparation method of tetraethyl ammonium hydroxide solution | |
| CN108276315A (en) | A kind of purification process of trifluoromethanesulfonic acid | |
| CN103566614A (en) | Dimethyl sulfate rectifying tower | |
| CN104085861B (en) | A kind of device of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater and corresponding technique thereof | |
| CN108467044B (en) | Bipolar membrane electrolytic tank for preparing silica sol by pulping and electrolyzing silica powder | |
| CN206730527U (en) | A kind of Hu shaddock ped extract solution evaporation purifying plant | |
| CN110510579A (en) | A kind of device and technique parsing separating hydrogen chloride and water from hydrochloric acid | |
| CN101817513A (en) | Phosphoric acid purification device | |
| CN104787723A (en) | Technology for deeply resolving by-product hydrochloric acid to prepare hydrogen chloride | |
| CN210764418U (en) | Evaporation crystallization separation integration system | |
| CN212403459U (en) | Deep analytical equipment of olefine acid concentration | |
| CN203938481U (en) | A kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid | |
| CN107601740A (en) | A kind of graphene prepares raffinate harmless treatment and method | |
| CN207552215U (en) | A kind of NMP dewatering membranes are impregnated with gasification purifying plant | |
| CN106744720A (en) | The circulation recycling system and its operation process of trichloroacetaldehyde by-product dilute sulfuric acid | |
| CN207210519U (en) | A kind of metallic lithium vacuum distillation purification device | |
| CN105348043A (en) | Separating and recycling method and device for solvent-water mixture containing impurities prone to scale formation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |