CN105018960A - Concentrating and rectifying method for hydrogen iodide in iodine-containing hydroiodic acid - Google Patents
Concentrating and rectifying method for hydrogen iodide in iodine-containing hydroiodic acid Download PDFInfo
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Abstract
The invention discloses a concentrating and rectifying method for hydrogen iodide in iodine-containing hydroiodic acid, and relates to the technical field of chemical separation. On an electrolysis and electrodialysis device, bridging pipelines are arranged in a cathode liquid discharge hole or on at least one cathode region close to the cathode discharge hole; the bridging pipelines are connected with the tower body or the tower kettle of a rectifying tower; thermal-insulation parts and valves are arranged on the bridging pipelines; the tower top of the rectifying tower is connected with a decompressor; the bridging pipelines are additionally arranged on the electrolysis and electrodialysis device, so that electrolysis and electrodialysis device (EED) is mutually coupled with decompressing rectification for quickly removing HI in a cathode feed liquid; in an EED concentrating process of the iodine-containing hydroiodic acid, backward transfer of HI due to extremely high concentration difference between the cathode liquid and HI and H2O in the cathode liquid is avoided; on the other hand, an anode region has pressure higher than that of a cathode region, so that H<+> in the anode region is promoted to move towards the cathode region, thereby facilitating the concentration of HI in the cathode region and greatly improving the concentrating and separating efficiency of HI.
Description
Technical field
The present invention relates to technical field of chemical separation, particularly relate to the concentrated rectificating method containing hydrogen iodide in iodine hydroiodic acid HI.
Background technology
Containing iodine hydroiodic acid HI feed liquid (i.e. hydrogen iodide-iodo-water ternary solution, HI-I
2-H
2o, be called for short HIx) distillation operation, in thermochemistry iodine-sulfur process hydrogen production by water decomposition technique, and all can use in the production technique of hydroiodic acid HI or hydrogen iodide (HI).For the former, in thermochemistry iodine-sulfur process hydrogen production process, the hydroiodic acid HI relying on Bunsen reaction to generate, owing to adding excessive iodine, defines HI-I
2-H
2o thing phase, needs by distillation operation, can isolate the hydrogen iodide prepared required for hydrogen.
Due to the characteristic of material itself, current technology is adopted to carry out rectifying separation to the hydrogen iodide in HIx and be not easy.Due to HI and H
2the azeotrope of mol ratio 1:5 can be formed between O, and Bunsen reacts in the HIx provided in above-mentioned iodine-sulfur process technique, the concentration of HI is often lower than azeotropic concentration, or just reach azeotropic concentration, if therefore adopt straight run distillation or rectifying to HIx, although can obtain HI, have a large amount of heat energy and be used to evaporation of water, the economy of technique will significantly reduce.Given this situation, domestic and international investigator proposes: first carry out electrolytic electro-dialysis (EED) to HIx and concentrate, and in the HIx feed liquid of the cathodic area outflow of EED equipment, HI concentration can be enhanced, and exceedes azeotropic composition, i.e. HI:H
2o>1:5, like this in distillation/rectifying, HI can steam in a large number, and the amount of steaming of water is little, after Optimization Technology, even can obtain pure HI gas, be very beneficial for the raising of iodine-sulfur process technique whole efficiency.
Specifically, electrolytic electro-dialysis (Electrolysis and electrodialysis device, be called for short " EED ") be a kind of high-efficiency electrochemical concentration method, be also called ion exchange membrane electrolytic process or membrane electrolysis, also can be used as the electrochemical synthesis of particular chemicals.The concrete principle of EED of HIx is: when yin, yang the two poles of the earth have HIx streams out-of-date, H
+under electric field action, through proton selective through film, enter cathodic area by positive column, following electrode reaction occur on two-plate simultaneously:
Anode: 2I
--2e → I
2
Negative electrode: I
2+ 2e → 2I
-
Integrate as a result, positive column H
+, I
-reduce, I
2increase, and cathodic area I
2reduce, H
+, I
-increase, namely HI obtains concentrated in cathodic area.Surmount constant boiling point when HI concentration and reach specific concentration ranges, distillation operation can be carried out by anticathode material, obtain the HI-H of high HI concentration in rectifying tower top
2o solution or HI gas.
Above-mentioned EED-rectifying combination process has obtained concern and the accreditation of lot of domestic and international investigator, on the iodine-sulfur process hydrogen manufacturing stand of China, Japan, Korea S, and the concentrating and separating of HI that all used this scheme to carry out.But carrying out along with research work, some limitation of EED also reveal gradually, wherein the most important thing is HI in EED process in catholyte can not according to the ideal style of anticipation constantly, enrichment rapidly.Along with the carrying out of EED, HI and H in the solution of yin, yang the two poles of the earth
2the concentration difference of O constantly promotes, and specifically, in catholyte, the concentration of HI is more and more higher than the concentration of HI in anolyte, like this, under the promotion of concentration difference, and H
+will by negative electrode dialysis to anode, the situation of water is then contrary, to more and more tend to enter catholyte by anolyte, above two kinds of trend, catholyte HI concentration will be made cannot to continue to improve, after the concentration difference of catholyte, anolyte acquires a certain degree, even there will be the phenomenon that catholyte HI concentration falls after rise.The HI that above-mentioned concentration difference causes oppositely moves, and water accelerates the remarkable processing power reducing EED of problem meeting entering cathodic area, be difficult to for subsequent fine distillation unit provides the feed liquid of higher HI concentration, make this HI separation process of EED-rectifying be difficult to effective operation, and then tie down the high-efficient operation of whole iodine-sulfur process process for making hydrogen.
If suitable measure can be taked, suppress to produce excessive concentration difference between cathode and anode liquid, then can avoid the problems referred to above, improve the concentrating and separating efficiency of HI.A large amount of experimental datas and Theoretical Calculation show, containing the concentration of HI in iodine hydroiodic acid HI more than HI-H
2after azeotropic concentration between O, due to the violent raising of vapour pressure, its boiling point can significantly decline, and at reduced pressure conditions, is easy to produce HI gas.If electrolytic electro-dialysis (EED) is coupled with rectification under vacuum according to this rule, cathodic area by EED is connected with vacuum rectification tower, just the HI in catholyte can be pipetted out in time, reduce the concentration difference between cathode and anode liquid, avoid above-mentioned series of problems, improve the running efficiency of EED.
Summary of the invention
The object of the present invention is to provide a kind of concentrated rectificating method containing hydrogen iodide in iodine hydroiodic acid HI, by electrolytic electro-dialysis (EED) is coupled with rectification under vacuum, HI in catholyte is shifted out fast, make containing iodine hydroiodic acid HI in EED concentration process, avoid HI and H in catholyte and anolyte
2o concentration difference is too high and the reverse migration of HI occurs, thus improves the concentrating and separating efficiency of HI.
Technical scheme of the present invention is as follows:
1) on electrolytic electro-dialysis device, in there is catholyte discharge port or arrange bridge line at least one cathodic area of negative electrode discharge port, tower body or the tower reactor of these bridge line and rectifying tower are connected, with heat preservation component and valve in bridge line, the tower top of rectifying tower is connected with reliever;
2) valve in bridge line is located at off condition, adds in the tower reactor of rectifying tower not containing the high concentration of hydrogen acid iodide of iodine, or low iodine content, high HI content containing iodine hydroiodic acid HI; Described not containing in the high concentration of hydrogen acid iodide of iodine, HI:H
2the mol ratio of O is 1:4.5 ~ 6.0; Containing in iodine hydroiodic acid HI of described low iodine content, high HI content, the mol ratio of each component is HI:H
2o:I2=1:4.5 ~ 6.0:0 ~ 0.4;
3) tower body and the tower reactor heating unit of rectifying tower is started, and the condensation reflux unit of rectifying tower top, open the reliever of rectifying tower top, under total reflux mode, carry out distillation operation;
4) when rectifying tower tower top condensation reflux unit can carry out stable hydroiodic acid HI backflow, using as the initial feed liquid of negative electrode containing iodine hydroiodic acid HI solution and as the initial feed liquid of anode containing iodine hydroiodic acid HI solution, be delivered to cathodic area and the positive column of electrolytic electro-dialysis device respectively, carry out electrolytic electro-dialysis operation, the expel liquid in cathodic area is transported to tower body or the tower reactor of rectifying tower after collection;
5) open and regulate the valve in bridge line, the gas that electrolytic electro-dialysis equipment cathodic area is produced enters the tower body of rectifying tower, and continues to carry out material extraction from rectifying tower top and tower reactor.
Rectifying tower of the present invention is packing tower; The temperature of the initial feed liquid of described negative electrode, the initial feed liquid of anode and electrolytic electro-dialysis device controls between 90 DEG C to feed liquid bubble point temperature.
Technical characteristic of the present invention is also, in described bridge line, filler is housed.
The present invention has the following advantages and the technique effect of high-lighting: in the method for the invention, owing to having set up bridge line on electrolytic electro-dialysis device, electrolytic electro-dialysis (EED) and rectification under vacuum are intercoupled, HI in negative electrode feed liquid can be shifted out fast, make containing iodine hydroiodic acid HI in EED concentration process, avoid HI and H in catholyte and anolyte
2the concentration difference of O is too high and the reverse migration of HI occurs, thus improves the concentrating and separating efficiency of HI.On the other hand, positive column, owing to having the pressure higher than cathodic area, will promote positive column H
+to the migration in cathodic area, be conducive to the concentrated of cathodic area HI.Due to above ambilateral reason, the method that the present invention proposes can increase substantially the concentrating and separating efficiency of HI.
Accompanying drawing explanation
Fig. 1 is a kind of equipment schematic diagram used containing the concentrated rectificating method of hydrogen iodide in iodine hydroiodic acid HI of the present invention, and this schematic diagram is to have the electrolytic electro-dialysis equipment of 4 unit.
1-cathode end plate; 2-bipolar plates; 3-anode end plate; Cathodic area in 4a-cathode end plate; Cathodic area in 4b-bipolar plates; Positive column on 5a-anode end plate; Positive column in 5b-bipolar plates; 6-proton selective exchange membrane; 7-pad; 8-negative electrode feeding line; Feed liquid pipeline between 9-cathode electrode unit; 10-negative electrode discharging pipeline; 11-anode feed pipeline; Feed liquid pipeline between 12-anode unit; 13-anode discharging pipeline; 14-bridge line; 15-valve; 16-cathode terminal; 17-anode terminal
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is elaborated.
The concentrated rectificating method containing hydrogen iodide in iodine hydroiodic acid HI that the present invention proposes, carries out in electrolytic electro-dialysis-rectifying Coupling device.As shown in Figure 1, electrolytic electro-dialysis device structurally mainly comprises cathode end plate 1, one or more bipolar plates 2, and anode end plate 3.Containing the cathodic area 4a in cathode end plate in cathode end plate 1, anode end plate 3 possesses the positive column 5a on anode end plate, and bipolar plates 2 then has cathodic area and positive column respectively in its both sides, the cathodic area 4b namely in bipolar plates and the positive column 5b in bipolar plates.
Between end plate and bipolar plates and between adjacent bipolar plates, be provided with proton selective exchange membrane 6 and pad 7.
The central authorities of each pad are hollowed out, thus adjacent cathodic area and positive column are only separated by with proton selective exchange membrane, catholyte and anolyte are by proton selective exchange membrane generation mass transfer, that is: be separated by by proton selective exchange membrane, neighbouring cathode district and positive column form electrolytic electro-dialysis processing unit.
Pending catholyte enters electrolytic electro-dialysis device from negative electrode feeding line 8, via feed liquid pipeline 9 between cathode electrode unit, flow through each cathodic area successively, comprise the cathodic area 4a in cathode end plate and the cathodic area 4b in bipolar plates, then discharge via negative electrode discharging pipeline 10.
Pending anolyte enters electrolytic electro-dialysis device from anode feed pipeline 11, via feed liquid pipeline 12 between anode unit, flow through each positive column successively, comprise the positive column 5a on anode end plate and the positive column 5b in bipolar plates, then discharge via anode discharging pipeline 13.
The positive pole of direct supply is communicated with the anode terminal 17 of electrolytic electro-dialysis device, the negative pole of direct supply is communicated with the cathode terminal 16 of electrolytic electro-dialysis device, opening power is powered, then flow through the anolyte of above-mentioned positive column and flow through the catholyte in cathodic area, by under the effect of electric field, concentration difference etc., by proton selective exchange membrane generation mass transfer.
As mentioned above, the electrolytic electro-dialysis device shown in Fig. 1 contains 4 processing units, obviously, and can by increasing bipolar plates, and the pad matched and proton selective exchange membrane obtain the electrolytic electro-dialysis device with more crosspoints.
In the example of fig. 1, there is the cathodic area of catholyte discharge port, and the cathodic area be adjacent is arranging bridge line 14, tower body or the tower reactor of these bridge line and rectifying tower are connected, with attemperator in bridge line, and mounted valve 15, in bridge line, filler is housed.Above-mentioned rectifying tower is packing tower, and tower top is connected with reliever, thus can carry out rectification under vacuum operation.
A kind of concentrated rectificating method containing hydrogen iodide in iodine hydroiodic acid HI provided by the invention, its concrete technology step is as follows:
1) on electrolytic electro-dialysis device, there is catholyte discharge port or bridge line is being set at least one cathodic area of negative electrode discharge port, tower body or the tower reactor of these bridge line and rectifying tower are connected, and with attemperator and valve in bridge line, in bridge line, filler are housed.Above-mentioned rectifying tower is packing tower, and tower top is connected with reliever, thus can carry out rectification under vacuum operation;
2) by step 1) described in valve in bridge line be located at off condition, add in the tower reactor of rectifying tower not containing the high concentration of hydrogen acid iodide of iodine, or low iodine content, high HI content containing iodine hydroiodic acid HI; Described not containing in the high concentration of hydrogen acid iodide of iodine, HI:H
2the mol ratio of O is 1:4.5 ~ 6.0; Containing in iodine hydroiodic acid HI of described low iodine content, high HI content, the mol ratio of each component is HI:H
2o:I
2=1:4.5 ~ 6.0:0 ~ 0.4;
3) tower body and the tower reactor heating unit of rectifying tower is started, and rectifying tower top condensation reflux unit, open the reliever of rectifying tower top, under total reflux mode, carry out distillation operation;
4) when overhead condensate reflux device can carry out stable hydroiodic acid HI backflow, using as the initial feed liquid of negative electrode containing iodine hydroiodic acid HI solution, with as the initial feed liquid of anode containing iodine hydroiodic acid HI solution, be delivered to cathodic area and the positive column of electrolytic electro-dialysis device respectively, carry out electrolytic electro-dialysis operation, the expel liquid in cathodic area is transported to tower body or the tower reactor of rectifying tower after collection.The temperature of the initial feed liquid of above-mentioned negative electrode, the initial feed liquid of anode and electrolytic electro-dialysis device controls between 90 DEG C to feed liquid bubble point temperature.
5) open and regulate 1) in valve in bridge line, the gas that electrolytic electro-dialysis equipment cathodic area is produced enters rectifying tower, and lastingly at the bottom of rectifying tower top and tower, carries out material extraction, and overhead product is the HI-H of HI gas or high HI concentration
2o solution.
As mentioned above, the electrolytic electro-dialysis device shown in Fig. 1 contains 4 crosspoints, obviously, and can by increasing bipolar plates, and the pad matched and proton selective exchange membrane obtain the electrolytic electro-dialysis device with more crosspoints.
In the example of fig. 1, there is the cathodic area of catholyte discharge port, and the cathodic area be adjacent is arranging bridge line 14, tower body or the tower reactor of these bridge line and rectifying tower are connected, with attemperator in bridge line, and mounted valve 15, in bridge line, filler is housed.Above-mentioned rectifying tower is packing tower, and tower top is connected with reliever, thus can carry out rectification under vacuum operation.
Below in conjunction with several embodiment, the present invention is described further.
Embodiment 1
In the present embodiment, electrolytic electro-dialysis device used and the equipment shown in Fig. 1 similar, it contains 4 crosspoints, the exchange area of each unit, and effective exchange area of proton selective exchange membrane that namely each unit has is 150cm
2.In (the i.e. cathodic area of that unit that finally flows through of catholyte, cathodic area possessing catholyte discharge port, also be electrolytic electro-dialysis device middle distance catholyte entrance cathodic area farthest), install the bridge line that internal diameter is 2cm additional, this root bridge line is connected with the tower body of a rectifying tower, with attemperator and valve in bridge line, the glass spring filler of Ф 2mm*5mm is housed in bridge line.
Above-mentioned rectifying tower is packing tower, and tower top is furnished with reliever, and the internal diameter of packing tower is 5cm, and in-built filler is the glass spring filler of Ф 3mm*20mm, and bed stuffing height is 1.25m; The volume of rectifying still is 1.5L, is furnished with the heating jacket of power 1kW.
Before starting the operation, first the valve in bridge line is located at off condition, add in rectifying still not containing the hydroiodic acid HI 1.5L of iodine, in this hydroiodic acid HI, the mol ratio of HI and water is HI:H
2o=1:5.8.
Operation of driving is implemented to rectifying device, starts the tower body of rectifying tower and the heating unit of tower reactor, and rectifying tower top condensation reflux unit, open the reliever of rectifying tower top, operate under total reflux mode.After 30min, overhead condensate reflux device can carry out stable hydroiodic acid HI backflow.
By the starting material HI:H of electrolytic electro-dialysis
2o:I
2=1:5.40:1.25 is divided into two strands containing iodine hydroiodic acid HI feed liquid, respectively as catholyte and the anolyte of electrolytic electro-dialysis device, cathodic area and the positive column of electrolytic electro-dialysis device is all entered respectively with the flow velocity of 20ml/min, feed temperature is 100 DEG C, and it is 105 DEG C that electrolytic electro-dialysis unit temp controls.Open DC power supply, strength of current is 16A.Collect cathodic area liquid effluent and positive column liquid effluent respectively, wherein the expel liquid in cathodic area is transported to the tower reactor of rectifying tower after collection.
Open and regulate the valve in bridge line, the gas that electrolytic electro-dialysis device cathodic area is produced enters rectifying tower, and continues to carry out material extraction at the bottom of rectifying tower top and tower, and overhead product is HI:H
2the hydroiodic acid HI solution of O=1:4.2.
Embodiment 2
In the present embodiment, the equipment shown in electrolytic electro-dialysis device and Fig. 1 is similar, but it contains 10 crosspoints, the exchange area of each unit, and effective exchange area of proton selective exchange membrane that namely each unit has is 70cm
2.In (the i.e. cathodic area of that unit that finally flows through of catholyte, cathodic area possessing catholyte discharge port, also be electrolytic electro-dialysis device middle distance catholyte entrance cathodic area farthest), and a cathodic area adjacent thereto (i.e. the penultimate cathodic area of equipment), install the bridge line that internal diameter is 3cm additional, these two bridge line are connected with the tower body of a rectifying tower, with attemperator and valve in bridge line, the glass spring filler of Ф 3mm*10mm is housed in bridge line.
Above-mentioned rectifying tower is packing tower, and tower top is furnished with reliever, and the internal diameter of packing tower is 5cm, and in-built filler is the glass spring filler of Ф 3mm*20mm, and bed stuffing height is 1.25m; The volume of rectifying still is 2L, is furnished with the heating jacket of power 1kW.
Before starting the operation, first the valve in bridge line is located at off condition, add in rectifying still not containing the hydroiodic acid HI 1.5L of iodine, in this hydroiodic acid HI, the mol ratio of HI and water is HI:H
2o=1:4.9.
Operation of driving is implemented to rectifying device, starts the tower body of rectifying tower and the heating unit of tower reactor, and rectifying tower top condensation reflux unit, open the reliever of rectifying tower top, operate under total reflux mode.After 30min, overhead condensate reflux device can carry out stable hydroiodic acid HI backflow.
By the starting material HI:H of electrolytic electro-dialysis
2o:I
2=1:5.70:1.50 is divided into two strands containing iodine hydroiodic acid HI feed liquid, respectively as catholyte and the anolyte of electrolytic electro-dialysis device, all enter cathodic area and the positive column of electrolytic electro-dialysis device respectively with the flow velocity of 30ml/min, feed temperature is 90 DEG C, and it is 95 DEG C that electrolytic electro-dialysis unit temp controls.Open DC power supply, strength of current is 7.5A.Collect cathodic area liquid effluent and positive column liquid effluent respectively, wherein the expel liquid in cathodic area is transported to the tower reactor of rectifying tower after collection.
Open and regulate the valve in bridge line, the gas that electrolytic electro-dialysis device cathodic area is produced enters rectifying tower, and continues to carry out material extraction at the bottom of rectifying tower top and tower, and overhead product is HI:H
2the hydroiodic acid HI solution of O=1:3.5.
Embodiment 3
In the present embodiment, the equipment shown in electrolytic electro-dialysis device and Fig. 1 is similar, but it contains 15 crosspoints, the exchange area of each unit, and effective exchange area of proton selective exchange membrane that namely each unit has is 200cm
2.In (the i.e. cathodic area of that unit that finally flows through of catholyte, cathodic area possessing catholyte discharge port, also be electrolytic electro-dialysis device middle distance catholyte entrance cathodic area farthest), and a cathodic area adjacent thereto (i.e. the penultimate cathodic area of equipment), install the bridge line that internal diameter is 5cm additional, these bridge line are connected with the tower body of a rectifying tower, with attemperator and valve in bridge line, the glass spring filler of Ф 3mm*10mm is housed in bridge line.Above-mentioned rectifying tower is packing tower, and tower top is furnished with reliever.
The internal diameter of above-mentioned distilling filled tower is 10cm, and in-built filler is the glass spring filler of Ф 3mm*30mm, and bed stuffing height is 2.0m; Rectifying still volume is 5.5L, is furnished with the heating jacket of power 5kW.
Before starting the operation, first the valve in bridge line is located at off condition, add in rectifying still low iodine content, high HI content containing iodine hydroiodic acid HI 3.5L, the mol ratio of each component of this feed liquid is HI:H
2o:I
2=1:4.95:0.35;
Operation of driving is implemented to rectifying device, starts the tower body of rectifying tower and the heating unit of tower reactor, and rectifying tower top condensation reflux unit, open the reliever of rectifying tower top, operate under total reflux mode.After 35min, overhead condensate reflux device can carry out stable hydroiodic acid HI backflow.
By the starting material HI:H of electrolytic electro-dialysis
2o:I
2=1:6.50:1.80 is divided into two strands containing iodine hydroiodic acid HI feed liquid, respectively as catholyte and the anolyte of electrolytic electro-dialysis device, cathodic area and the positive column of electrolytic electro-dialysis device is all delivered into respectively with the flow velocity of 120ml/min, feed temperature is 98 DEG C, and the same control temperature of electrolytic electro-dialysis device is 98 DEG C.Open DC power supply, strength of current is 30A.Collect cathodic area liquid effluent and positive column liquid effluent respectively, wherein the expel liquid in cathodic area is transported to the tower reactor of rectifying tower after collection.
Open and regulate the valve in bridge line, the gas that electrolytic electro-dialysis device cathodic area is produced enters rectifying tower, and continues to carry out material extraction at the bottom of rectifying tower top and tower, and overhead product is HI:H
2the hydroiodic acid HI solution of O=1:4.2.
Embodiment 4
In the present embodiment, the equipment shown in electrolytic electro-dialysis device and Fig. 1 is similar, but it contains 35 crosspoints, the exchange area of each unit, and effective exchange area of proton selective exchange membrane that namely each unit has is 600cm
2.In (the i.e. cathodic area of that unit that finally flows through of catholyte, cathodic area possessing catholyte discharge port, also be electrolytic electro-dialysis device middle distance catholyte entrance cathodic area farthest), and adjacent thereto two each and every one cathodic areas (i.e. second from the bottom and the 3rd cathodic area of electrolytic electro-dialysis device), install the bridge line that internal diameter is 8cm additional, these bridge line are connected with the tower body of a rectifying tower, with attemperator and valve in bridge line, the glass spring filler of Ф 3mm*10mm is housed in bridge line.Above-mentioned rectifying tower is packing tower, and tower top is furnished with reliever.
The internal diameter of above-mentioned distilling filled tower is 15cm, and in-built filler is the glass spring filler of Ф 3mm*30mm, and bed stuffing height is 2.0m; Rectifying still volume is 15L, is furnished with the heating jacket of power 10kW.
Before starting the operation, first the valve in bridge line is located at off condition, add in rectifying still low iodine content, high HI content containing iodine hydroiodic acid HI 10L, the mol ratio of each component of this feed liquid is HI:H
2o:I
2=1:5.2:0.2;
Operation of driving is implemented to rectifying device, starts the tower body of rectifying tower and the heating unit of tower reactor, and rectifying tower top condensation reflux unit, open the reliever of rectifying tower top, operate under total reflux mode.After 35min, overhead condensate reflux device can carry out stable hydroiodic acid HI backflow.
By the negative electrode starting material of electrolytic electro-dialysis, i.e. HI:H
2o:I
2=1:6.20:1.90 contains iodine hydroiodic acid HI feed liquid, and anode starting material, i.e. HI:H
2o:I
2=1:5.50:1.50 contains iodine hydroiodic acid HI feed liquid, and be delivered into cathodic area and the positive column of electrolytic electro-dialysis device respectively with the flow velocity of 800ml/min, feed temperature is 105 DEG C, and electrolytic electro-dialysis device control temperature is 110 DEG C.Open DC power supply, strength of current is 90A.Collect cathodic area liquid effluent and positive column liquid effluent respectively, wherein the expel liquid in cathodic area is transported to the tower reactor of rectifying tower after collection.
Open and regulate the valve in bridge line, the gas that electrolytic electro-dialysis device cathodic area is produced enters rectifying tower, and continues to carry out material extraction at the bottom of rectifying tower top and tower, and overhead product is HI:H
2the hydroiodic acid HI solution of O=1:3.9.
Claims (4)
1., containing a concentrated rectificating method for hydrogen iodide in iodine hydroiodic acid HI, it is characterized in that the method is carried out as follows:
1) on electrolytic electro-dialysis device, in there is catholyte discharge port or arrange bridge line at least one cathodic area of negative electrode discharge port, tower body or the tower reactor of these bridge line and rectifying tower are connected, with heat preservation component and valve in bridge line, the tower top of rectifying tower is connected with reliever;
2) valve in bridge line is located at off condition, adds in the tower reactor of rectifying tower not containing the high concentration of hydrogen acid iodide of iodine, or low iodine content, high HI content containing iodine hydroiodic acid HI; Described not containing in the high concentration of hydrogen acid iodide of iodine, HI:H
2the mol ratio of O is 1:4.5 ~ 6.0; Containing in iodine hydroiodic acid HI of described low iodine content, high HI content, the mol ratio of each component is HI:H
2o:I2=1:4.5 ~ 6.0:0 ~ 0.4;
3) tower body and the tower reactor heating unit of rectifying tower is started, and the condensation reflux unit of rectifying tower top, open the reliever of rectifying tower top, under total reflux mode, carry out distillation operation;
4) when rectifying tower tower top condensation reflux unit can carry out stable hydroiodic acid HI backflow, using as the initial feed liquid of negative electrode containing iodine hydroiodic acid HI solution and as the initial feed liquid of anode containing iodine hydroiodic acid HI solution, be delivered to cathodic area and the positive column of electrolytic electro-dialysis device respectively, carry out electrolytic electro-dialysis operation, the expel liquid in cathodic area is transported to tower body or the tower reactor of rectifying tower after collection;
5) open and regulate the valve in bridge line, the gas that electrolytic electro-dialysis equipment cathodic area is produced enters the tower body of rectifying tower, and continues to carry out material extraction from rectifying tower top and tower reactor.
2. the concentrated rectificating method containing iodine hydroiodic acid HI according to claim 1, it is characterized in that, described rectifying tower is packing tower.
3. the concentrated rectificating method containing iodine hydroiodic acid HI feed liquid according to claim 1 and 2, it is characterized in that, the temperature of the initial feed liquid of described negative electrode, the initial feed liquid of anode and electrolytic electro-dialysis device controls between 90 DEG C to feed liquid bubble point temperature.
4. the concentrated rectificating method containing iodine hydroiodic acid HI feed liquid according to claim 1 and 2, is characterized in that, in described bridge line, filler is housed.
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| CN107904617A (en) * | 2017-11-23 | 2018-04-13 | 浙江大学 | With the method and device of electrochemical decomposition HI hydrogen manufacturing in sulphur iodine circulates hydrogen manufacturing |
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| 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 |
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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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107904617A (en) * | 2017-11-23 | 2018-04-13 | 浙江大学 | With the method and device of electrochemical decomposition HI hydrogen manufacturing in sulphur iodine circulates hydrogen manufacturing |
| 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 |
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| CN105018960B (en) | 2017-11-14 |
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