CN102021600B - Method and device for producing potassium iodate through oxygen cathode non-diaphragm electrolysis - Google Patents
Method and device for producing potassium iodate through oxygen cathode non-diaphragm electrolysis Download PDFInfo
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- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 32
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 30
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 title claims abstract description 30
- 239000001230 potassium iodate Substances 0.000 title claims abstract description 30
- 235000006666 potassium iodate Nutrition 0.000 title claims abstract description 30
- 229940093930 potassium iodate Drugs 0.000 title claims abstract description 30
- 239000001301 oxygen Substances 0.000 title claims abstract description 29
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 29
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 45
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 41
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 30
- 239000012452 mother liquor Substances 0.000 claims abstract description 18
- 230000009467 reduction Effects 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005260 corrosion Methods 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 15
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 11
- 238000007254 oxidation reaction Methods 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 235000007715 potassium iodide Nutrition 0.000 claims description 6
- 229960004839 potassium iodide Drugs 0.000 claims description 6
- DPGAAOUOSQHIJH-UHFFFAOYSA-N ruthenium titanium Chemical compound [Ti].[Ru] DPGAAOUOSQHIJH-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000010411 electrocatalyst Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- DEPMYWCZAIMWCR-UHFFFAOYSA-N nickel ruthenium Chemical compound [Ni].[Ru] DEPMYWCZAIMWCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910002844 PtNi Inorganic materials 0.000 claims description 2
- 239000006230 acetylene black Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 229940005633 iodate ion Drugs 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical group [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 claims description 2
- ZACYQVZHFIYKMW-UHFFFAOYSA-N iridium titanium Chemical compound [Ti].[Ir] ZACYQVZHFIYKMW-UHFFFAOYSA-N 0.000 claims description 2
- PCLURTMBFDTLSK-UHFFFAOYSA-N nickel platinum Chemical compound [Ni].[Pt] PCLURTMBFDTLSK-UHFFFAOYSA-N 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 2
- UUWCBFKLGFQDME-UHFFFAOYSA-N platinum titanium Chemical compound [Ti].[Pt] UUWCBFKLGFQDME-UHFFFAOYSA-N 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 239000003792 electrolyte Substances 0.000 abstract description 13
- 239000012528 membrane Substances 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 7
- 230000002829 reductive effect Effects 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 125000002091 cationic group Chemical group 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- -1 iodide ions Chemical class 0.000 abstract 4
- 230000007797 corrosion Effects 0.000 abstract 1
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 24
- 239000007788 liquid Substances 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000012530 fluid Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052740 iodine Inorganic materials 0.000 description 4
- 239000011630 iodine Substances 0.000 description 4
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 2
- 229930195725 Mannitol Natural products 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000006056 electrooxidation reaction Methods 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 239000000594 mannitol Substances 0.000 description 2
- 235000010355 mannitol Nutrition 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical group [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 208000034809 Product contamination Diseases 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- OMBRFUXPXNIUCZ-UHFFFAOYSA-N dioxidonitrogen(1+) Chemical compound O=[N+]=O OMBRFUXPXNIUCZ-UHFFFAOYSA-N 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229940006461 iodide ion Drugs 0.000 description 1
- 229910000450 iodine oxide Inorganic materials 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- AFSVSXMRDKPOEW-UHFFFAOYSA-N oxidoiodine(.) Chemical compound I[O] AFSVSXMRDKPOEW-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
一种采用无隔膜电解槽电解生产碘酸钾的方法及装置，以碘化钾和氢氧化钾的混合溶液作为电解液，其中碘离子在阳极氧化形成碘酸根离子，氧气在阴极还原形成氢氧根离子，电解出液经冷却析出碘酸钾结晶，而母液在补加碘化钾和水后返回电解槽进行电解。电解槽的阴极为耗氧阴极，阳极为耐蚀非牺牲型阳极，不必使用阳离子膜或隔膜即可避免碘酸根离子在阴极的还原。该方法的显著特点是槽电压仅为0.6-1.0V左右，大大降低了能耗；整个流程循环进行，无污染物产生；再者，电解槽结构简单、无需离子膜，运行成本低。
A method and device for producing potassium iodate by electrolysis using a diaphragmless electrolytic cell, using a mixed solution of potassium iodide and potassium hydroxide as the electrolyte, wherein iodide ions are oxidized at the anode to form iodate ions, and oxygen is reduced at the cathode to form hydroxide ions , the electrolytic solution is cooled to precipitate potassium iodate crystals, and the mother liquor is returned to the electrolytic cell for electrolysis after adding potassium iodide and water. The cathode of the electrolyzer is an oxygen-consuming cathode, and the anode is a corrosion-resistant non-sacrificial anode, which can avoid the reduction of iodate ions at the cathode without using a cationic membrane or diaphragm. The salient feature of this method is that the cell voltage is only about 0.6-1.0V, which greatly reduces energy consumption; the whole process is cyclical, and no pollutants are produced; moreover, the electrolytic cell structure is simple, no ion membrane is required, and the operating cost is low.
Description
Technical field
The invention provides method and device that a kind of electrochemical electrolysis prepares Potassium Iodate, particularly replace existing cathode for hydrogen evolution and realize that the oxidation of no barrier film anode electrochemical prepares the method and the device of Potassium Iodate with oxygen reduction cathode.
Technical background
The industrial production process of Potassium Iodate mainly comprises Potcrate oxidation style, concentrated nitric acid oxidation method, hydrogen peroxide oxidation process and electrochemical oxidation process at present.Utilizing Potcrate iodine oxide simple substance is the main flow technology that China's Potassium Iodate is produced, but because the Potcrate oxidation needs to carry out under acidic conditions, therefore equipment material is required high; In addition, the easy and iodide ion reaction generation elemental iodine of iodate causes the loss of unnecessary iodine because of elemental iodine easily distils, and reclaims the complexity that iodine has increased subsequent handling under acidic conditions; Moreover the Potcrate oxidation style can produce a large amount of chlorine, adopts caustic soda to reclaim usually, but also exists the problem of the wasting of resources and complex procedures.Patent CN1712347A directly utilizes chlorine oxidation potassiumiodide under weak basic condition to obtain Potassium Iodate, and by product is a Repone K, has simplified equipment and has reduced by product, but will use a large amount of chlorine, therefore still has safety and pollution hidden trouble.The concentrated nitric acid oxidation method can produce a large amount of obnoxious flavour nitrogen peroxide, therefore uses fewer now.Hydrogen peroxide oxidation method possesses environmental friendliness, the simple advantage of operation, but the consumption of hydrogen peroxide is big, and cost is too high.
Directly the synthetic Potassium Iodate of electrooxidation can be cut down the number of intermediate links, and improves raw material availability, and reduces the pollution to environment.In the traditional electrical solution, be reduced, must use expensive cationic membrane to suppress diffusion for the Potassium Iodate that prevents the anode surface generation diffuses to negative electrode.Patent CN101078128A provides a kind of ion-exchange membrane electrolysis paired electrolysis to prepare the method for N.F,USP MANNITOL and Potassium Iodate, can obtain N.F,USP MANNITOL at negative electrode when anode obtains Potassium Iodate, the way that obtains two kinds of products simultaneously can reduce the cost that electrolyzer uses ionic membrane to a certain extent.Patent CN1121540A provides a kind of method of utilizing liquor kalii iodide to obtain Potassium Iodate by continuous, multistage and order electrolysis for raw material, for fear of using ionic membrane, in catholyte, added the reduction that potassium bichromate suppresses iodate in this method.But potassium bichromate itself is a kind of carcinogens, very easily causes product contamination, moreover the bath voltage of this method is 2.5～3.5V, and energy consumption is higher.
In sum, existing electrochemical process prepares the Potassium Iodate technology, and bath voltage is high and must use ionic membrane suppressing the diffusion of iodate to the cathodic area, otherwise current efficiency will reduce, and the use of ionic membrane makes production cost remain high.
Summary of the invention
At having the shortcoming that electrochemical process prepares the Potassium Iodate technology now, the present invention is proposed.The object of the present invention is to provide a kind of less energy-consumption, pollution-free, the simple electrolytic preparation Potassium Iodate of operation method and apparatus, have bath voltage low, do not use ionic membrane, product purity height, production safety reliable characteristics.
Electrochemical preparation Potassium Iodate method of the present invention is different from prior art and is characterised in that, substitutes cathode for hydrogen evolution with oxygen reduction cathode.In the electrochemical preparation Potassium Iodate method of the present invention, it is as follows that electrochemical reaction process takes place on anode and the negative electrode in the electrolyzer:
Anode: 2I
-+ 12OH
--12e
-→ 6H
2O+2IO
3 -Φ
Θ=0.257V
Negative electrode: 3O
2+ 6H
2O+12e
-→ 12OH
-Φ
Θ=0.401V
Total reaction: 2I
-+ 3O
2→ 2IO
3 -Φ
Θ=-0.144V
The theoretical reduction potential of oxygen is higher than the iodate reduction potential, and current density reaches 4000A/m when hydrogen reduction
2Before, iodate reductive current density is compared and can be ignored, and therefore need not to use ionic membrane or barrier film can avoid iodate to be reduced at negative electrode; Consider O
2Reduction, KI oxidation need activation energy to cause cathode and anode utmost point overpotential, the solution resistance equal loss, and the actual groove pressure of electrochemical preparation Potassium Iodate is 0.6～1.0V only when using oxygen cathode, compares prior art and greatly reduces energy consumption.
The invention provides a kind of method and device of electrochemical preparation Potassium Iodate, it is characterized in that substituting cathode for hydrogen evolution with oxygen reduction cathode in the employed electrolyzer, and need not to use ionic membrane or barrier film.
The method of electrochemical preparation Potassium Iodate of the present invention is selected no diaphragm plate frame electrolyzer for use, and wherein anode is anti-corrosion non-sacrifice type anode, and material is titanium ruthenium, titanium platinum, titanium iridium, nickel ruthenium, nickel platinum, graphite or stainless steel; Negative electrode comprises existing oxygen cathode structure and other any electrode structures that can realize oxygen reduction for can realize the electrode of oxygen reduction to hydroxide ion.Existing oxygen cathode structure comprises the gentle chamber of electrode part part at least, and wherein the electrode part branch comprises eelctro-catalyst and electro-catalyst carrier, and wherein eelctro-catalyst can be Ag, Co
3O
4, MnO
2, one or more the composition in Pt and the PtNi alloy, electro-catalyst carrier can be one or more the composition in gac, acetylene black and the graphitized carbon black.
Electrochemical preparation Potassium Iodate method of the present invention specifically describes as follows:
A: the aqueous solution 1 that contains potassiumiodide 50-400g/L, potassium hydroxide 50-250g/L is preheating to the temperature identical with electrolysis temperature (25-95 ℃) in electrolytic solution reservoir 2.
B: utilize volume pump that electrolytic solution is injected in the electrolyzer 3 that keeps steady temperature (25-95 ℃) and the electrolyzer container for storing liquid 8 to hydroful by the import of electrolyzer lower end, dividing potential drop is that the oxygen of 20～50kPa is entered in the cathode air chamber spreader plate 6 by cathode air chamber upper end import, and remaining gas enters compressor from the outlet discharge and gets back to oxygen gas-holder 7.If the gas that feeds is air, then expellant gas does not need to reclaim.
C: close electrolytic solution feed liquor volume pump, electrolytic solution carries out internal recycle in electrolyzer 3 He in the container for storing liquid 8, and circulation velocity is 5～50L/ (minm
2), on negative and positive the two poles of the earth, to switch on, current density is 500-4000A/m
2Under carry out electrolysis, 20%～40% KI is converted into KIO in the groove electrolyte inside
3Open the feed liquor volume pump then fresh electrolyte is entered in the electrolyzer, electrolyzer contains KIO simultaneously
3, KI, KOH electrolytic solution enter after the electrolysis in the reservoir 9 by upper end outlet.
D: the electrolytic solution of reservoir 8 changes KIO over to after utilizing volume pump with electrolysis
3Crystallisation by cooling separator 10, cooling temperature is-5～10 ℃, the white KIO that separates out
3Crystal is transferred to KIO
3In the fine seperator 11.KIO in the fine seperator
3Solid transfer after the frozen water washing is to KIO
3In the hold-up vessel, and the washing mother liquor is got back to KIO
3In the crystallisation by cooling separator 10.
E: contain KOH, KI, KIO by what Crystallization Separation device 10 obtained
3Mother liquor be back in the electrolytic solution reservoir 2, and add KI, KOH and less water at this, keep in the electrolytic solution reservoir 2 concentration of electrolyte within the required range.
The said process circulation is carried out, and can constantly obtain product solid K IO
3
Compare with existing electrochemical method, electrochemical preparation Potassium Iodate method and apparatus of the present invention has following advantage: owing to adopt cathodic oxygen reduction to replace cathode hydrogen evolution, bath voltage is reduced to 0.6～1.0V by 2.5 original～3.5V, greatly reduces energy consumption; In addition, need not to use ionic membrane or add potassium bichromate, can avoid the reduction of iodate ion, reduced production cost effectively, improved production efficiency at cathode surface.
Description of drawings
Fig. 1 is the device and the schematic flow sheet thereof of the alkaline aqueous solution electrolysis production Potassium Iodate of potassiumiodide of the present invention.
Wherein: 1, the KI and the KOH aqueous solution; 2, electrolytic solution feed liquor storage tank; 3, electrolysis slot number chamber; 4, anode; 5, negative electrode; 6, cathode air chamber; 7, oxygen or air gas tank; 8, electrolytic solution internal recycle container for storing liquid; 9, electrolytic solution fluid storage tank; 10, KIO
3Separating tank; 11, KIO
3Smart separating tank; 12, KIO
3The product jar.
Specific embodiment
For technical characterictic of the present invention is described better, describe below by specific embodiment, embodiment 1-example 3 is the electrolysis in batches of the little electrolyzer in laboratory, and embodiment 4, example 5 are the continuous cyclic electrolysis of amplification test.
Use sheet frame type electrolyzer, anode titanium ruthenium, negative electrode oxygen cathode, cathod catalyst are cobalt oxide, the electrode useful area is 20cm
2, preparation KI 100g/L, KOH 80g/L electrolytic solution 100ml, 45 ℃ of electrolyte temperatures, cathode air chamber aerating oxygen, current density 100mA/cm
2, electrolysis time 5h, average cell voltage 0.675V.
Electrolytic solution heating after the electrolysis is concentrated the postcooling crystallization, with the filtering solid drying that obtains, with the KIO of gained
3Solid crude product merges coarse crystallization and the two-part mother liquor of recrystallization with frozen water flushing recrystallizing and refining, and titrimetry gets KIO in the mother liquor
3Quality is 2.15g, solid K IO
3Quality is 10.38g, analyze purity 99.78%.Whole KIO
3Yield 97.2%, solid K IO
3Yield 80.52%, unit K IO
3Electrolytic power consumption 0.539kwh/kg.
Use sheet frame type electrolyzer, anode titanium ruthenium, negative electrode oxygen cathode, cathod catalyst are Co
3O
4, the electrode useful area is 20cm
2, preparation KI 180g/L, KOH 100g/L electrolytic solution 200ml, 75 ℃ of electrolyte temperatures, cathode air chamber aerating oxygen, current density 200mA/cm
2, electrolysis time 9h, average cell voltage 0.714V.
Electrolytic solution heating after the electrolysis is concentrated the postcooling crystallization, with the filtering solid drying that obtains, with the KIO of gained
3Solid crude product merges coarse crystallization and the two-part mother liquor of recrystallization with frozen water flushing recrystallizing and refining, and titrimetry gets KIO in the mother liquor
3Quality is 7.08g, solid K IO
3Quality is 38.14g, analyze purity 99.46%.Whole KIO
3Yield 97.44%, solid K IO
3Yield 82.18%.Unit K IO
3Electrolytic power consumption 0.568kwh/kg.
Use sheet frame type electrolyzer, anode nickel ruthenium, negative electrode oxygen cathode, cathod catalyst are Ag, the electrode useful area is 20cm
2, preparation KI 160g/L, KOH 100g/L electrolytic solution 200ml, 75 ℃ of electrolyte temperatures, cathode air chamber aerating oxygen, current density 200mA/cm
2, electrolysis time 8h, average cell voltage 0.764V.
Electrolytic solution heating after the electrolysis is concentrated the postcooling crystallization, with the filtering solid drying that obtains, with the KIO of gained
3Solid crude product merges coarse crystallization and the two-part mother liquor of recrystallization with frozen water flushing recrystallizing and refining, and titrimetry gets KIO in the mother liquor
3Quality is 6.71g, solid K IO
3Quality is 33.62g, analyze purity 99.92%.Whole KIO
3Yield 97.76%, solid K IO
3Yield 81.5%, unit K IO
3Electrolytic power consumption 0.606kwh/kg.
Use sheet frame type electrolyzer, anode titanium ruthenium, negative electrode oxygen cathode, cathod catalyst are Ag, the electrode useful area is 20dm
2, configuration KI 180g/L, the electrolytic solution 10L of KOH 120g/L, 75 ℃ of electrolyte temperatures, the cathode air chamber aerating oxygen, after the storage of electrolyzer electrolyte inside was full, electrolytic solution internal recycle flow velocity was 1L/min, current density 25A/dm
2, behind the 20min, fresh electrolyte enters electrolyzer with the flow velocity of 140～160ml/min, and electrolyzer contains KIO simultaneously
3, KI, KOH electrolytic solution enter in the electrolysis fluid reservoir by upper end outlet, carry up to 10L electrolytic solution and finish.Electrolysis total consuming time 70min, the reasonable opinion of actual electrolysis electricity electric weight 33.45%, average cell voltage 0.843V.
Liquid in the electrolysis fluid reservoir enters KIO
3Cooling separator 10.Crystalline KIO
3Solid transfer is to KIO
3In the smart separating tank 11, frozen water washing back purified KIO
3Solid enters in the product jar 12.Obtain KIO
3Solid oven dry back weighing is 644.32g, analyzes to such an extent that purity is 99.92%.The washing mother liquor is got back to KIO
3In the crystallisation by cooling separator 10, the mother liquor of merging 10 and 11 enters in the electrolytic solution feed liquor container for storing liquid 2, and final mother liquor is 9.53L, contains KI 127.02g/L, KIO
312.26g/L.Current efficiency 98.09%, solid K IO
3Yield 83.01%, unit K IO
3Electrolytic power consumption 0.646kwh/kg.
Above-mentioned mother liquor is added the about 500g of KI solid, and add water and be settled to 10L, the circulation of beginning next round.
Embodiment 5
Use sheet frame type electrolyzer, anode titanium ruthenium, negative electrode oxygen cathode, cathod catalyst are Ag, the electrode useful area is 20dm
2, configuration KI 160g/L, the electrolytic solution 10L of KOH 120g/L, 75 ℃ of electrolyte temperatures, the cathode air chamber aerating oxygen, after the storage of electrolyzer electrolyte inside was full, electrolytic solution internal recycle flow velocity was 0.5L/min, current density 20A/dm
2, behind the 25min, fresh electrolyte enters electrolyzer with the flow velocity of 100ml/min, and electrolyzer contains KIO simultaneously
3, KI, KOH electrolytic solution enter in the electrolysis fluid reservoir by upper end outlet, carry up to 10L electrolytic solution and finish.Electrolysis total consuming time 102min, the reasonable opinion of actual electrolysis electricity electric weight 43.87%, average cell voltage 0.908V.
Liquid in the electrolysis fluid reservoir enters KIO
3Cooling separator 10.Crystalline KIO
3Solid transfer is to KIO
3In the smart separating tank 11, frozen water washing back purified KIO
3Solid enters in the product jar 12.Obtain KIO
3Solid oven dry back weighing is 769.12g, analyzes to such an extent that purity is 99.85%.The washing mother liquor is got back to KIO
3In the crystallisation by cooling separator 10, the mother liquor of merging 10 and 11 enters in the electrolytic solution feed liquor container for storing liquid 2, and final mother liquor is 9.27L, contains KI 89.80g/L, KIO
312.31g/L.Current efficiency 97.56%, solid K IO
3Yield 84.99%, unit K IO
3Electrolytic power consumption 0.682kwh/kg.
Above-mentioned mother liquor is added the about 700g of KI solid, and add water and be settled to 10L, the circulation of beginning next round.
Claims (4)
1. the method for an electrolytic preparation Potassium Iodate, it is characterized in that wherein substituting cathode for hydrogen evolution with oxygen reduction cathode in the electrolyzer, specifically comprise: with the mixing solutions of potassiumiodide and potassium hydroxide as electrolytic solution, wherein iodide ion forms iodate ion in anodic oxidation, oxygen forms hydroxide ion in cathodic reduction, reaction solution is separated out the Potassium Iodate crystallization through cooling, carries out electrolysis and mother liquor returns electrolyzer after adding potassiumiodide and water.
2. the method for electrolytic preparation Potassium Iodate as claimed in claim 1, wherein electrolytic solution by handling equipment from bottom of electrolytic tank enter, the top flow out to form and to circulate.
3. the method for electrolytic preparation Potassium Iodate as claimed in claim 1, wherein the electrolyzer feed liquor consists of potassiumiodide 50-400g/L, and concentration of potassium hydroxide is 50-250g/L, and electrolysis temperature 25-95 ℃, current density is 500-4000A/m
2
4. used device of electrolytic preparation Potassium Iodate method as claimed in claim 1, it is characterized in that electrolyzer adopts undivided cell, wherein anode is anti-corrosion non-sacrifice type anode, and material is a kind of in titanium ruthenium, titanium platinum, titanium iridium, nickel ruthenium, nickel platinum, the graphite; Negative electrode is an oxygen reduction electrode, comprises oxygen cathode eelctro-catalyst and electro-catalyst carrier, and wherein eelctro-catalyst is Ag, Co
3O
4, MnO
2, one or more the composition in Pt and the PtNi alloy, electro-catalyst carrier is one or more the composition in gac, acetylene black and the graphitized carbon black.
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| CN109055966A (en) * | 2018-09-13 | 2018-12-21 | 北京化工大学 | A kind of chemical combined method for preparing chlorine dioxide of electrochemistry- |
| CN112030179B (en) | 2019-06-04 | 2022-06-17 | 泰安汉威集团有限公司 | Environment-friendly production process of iodate |
| RU2732691C1 (en) * | 2019-12-06 | 2020-09-22 | Федеральное государственное автономное образовательное учреждение высшего образования «Северный (Арктический) федеральный университет имени М. В. Ломоносова» | Method of obtaining potassium iodate from iodine |
| CN111394746B (en) * | 2020-04-10 | 2021-06-08 | 山东博苑医药化学股份有限公司 | Electrochemical co-production method of potassium iodate and hydroiodic acid |
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