CN110724968A - Industrial production method of hydroiodic acid - Google Patents
Industrial production method of hydroiodic acid Download PDFInfo
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- CN110724968A CN110724968A CN201810780327.3A CN201810780327A CN110724968A CN 110724968 A CN110724968 A CN 110724968A CN 201810780327 A CN201810780327 A CN 201810780327A CN 110724968 A CN110724968 A CN 110724968A
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- Prior art keywords
- iodide
- tank
- soluble
- iodine
- cathode
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- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229940071870 hydroiodic acid Drugs 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000009776 industrial production Methods 0.000 title claims abstract description 19
- 239000011630 iodine Substances 0.000 claims abstract description 73
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 72
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000012528 membrane Substances 0.000 claims abstract description 55
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 29
- 239000003513 alkali Substances 0.000 claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
- 239000012266 salt solution Substances 0.000 claims abstract description 5
- 238000001308 synthesis method Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 33
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 27
- -1 iodine ions Chemical class 0.000 claims description 27
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 18
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 15
- 238000005086 pumping Methods 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 229910000510 noble metal Inorganic materials 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 8
- 229910019142 PO4 Inorganic materials 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- 230000007797 corrosion Effects 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Chemical compound [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 6
- 235000009518 sodium iodide Nutrition 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 4
- 150000004715 keto acids Chemical class 0.000 claims description 4
- XSKIUFGOTYHDLC-UHFFFAOYSA-N palladium rhodium Chemical compound [Rh].[Pd] XSKIUFGOTYHDLC-UHFFFAOYSA-N 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- CPRMKOQKXYSDML-UHFFFAOYSA-M rubidium hydroxide Chemical compound [OH-].[Rb+] CPRMKOQKXYSDML-UHFFFAOYSA-M 0.000 claims description 4
- WFUBYPSJBBQSOU-UHFFFAOYSA-M rubidium iodide Chemical compound [Rb+].[I-] WFUBYPSJBBQSOU-UHFFFAOYSA-M 0.000 claims description 4
- UAYWVJHJZHQCIE-UHFFFAOYSA-L zinc iodide Chemical compound I[Zn]I UAYWVJHJZHQCIE-UHFFFAOYSA-L 0.000 claims description 4
- UNMYWSMUMWPJLR-UHFFFAOYSA-L Calcium iodide Chemical compound [Ca+2].[I-].[I-] UNMYWSMUMWPJLR-UHFFFAOYSA-L 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 229910001640 calcium iodide Inorganic materials 0.000 claims description 3
- 229940046413 calcium iodide Drugs 0.000 claims description 3
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- CECABOMBVQNBEC-UHFFFAOYSA-K aluminium iodide Chemical compound I[Al](I)I CECABOMBVQNBEC-UHFFFAOYSA-K 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 2
- SGUXGJPBTNFBAD-UHFFFAOYSA-L barium iodide Chemical compound [I-].[I-].[Ba+2] SGUXGJPBTNFBAD-UHFFFAOYSA-L 0.000 claims description 2
- 229910001638 barium iodide Inorganic materials 0.000 claims description 2
- 229940075444 barium iodide Drugs 0.000 claims description 2
- 239000002585 base Substances 0.000 claims description 2
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims description 2
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- AVWLPUQJODERGA-UHFFFAOYSA-L cobalt(2+);diiodide Chemical compound [Co+2].[I-].[I-] AVWLPUQJODERGA-UHFFFAOYSA-L 0.000 claims description 2
- 229940076136 ferrous iodide Drugs 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- BQZGVMWPHXIKEQ-UHFFFAOYSA-L iron(ii) iodide Chemical compound [Fe+2].[I-].[I-] BQZGVMWPHXIKEQ-UHFFFAOYSA-L 0.000 claims description 2
- BLQJIBCZHWBKSL-UHFFFAOYSA-L magnesium iodide Chemical compound [Mg+2].[I-].[I-] BLQJIBCZHWBKSL-UHFFFAOYSA-L 0.000 claims description 2
- 229910001641 magnesium iodide Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 claims description 2
- 229910001866 strontium hydroxide Inorganic materials 0.000 claims description 2
- KRIJWFBRWPCESA-UHFFFAOYSA-L strontium iodide Chemical compound [Sr+2].[I-].[I-] KRIJWFBRWPCESA-UHFFFAOYSA-L 0.000 claims description 2
- 229910001643 strontium iodide Inorganic materials 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 2
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 claims description 2
- SXRIPRHXGZHSNU-UHFFFAOYSA-N iridium rhodium Chemical compound [Rh].[Ir] SXRIPRHXGZHSNU-UHFFFAOYSA-N 0.000 claims 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 9
- 239000011574 phosphorus Substances 0.000 abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000002360 explosive Substances 0.000 abstract description 3
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 abstract description 3
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 150000001450 anions Chemical class 0.000 description 21
- 150000001768 cations Chemical class 0.000 description 21
- 239000000047 product Substances 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 229910021389 graphene Inorganic materials 0.000 description 6
- 239000002699 waste material Substances 0.000 description 5
- 150000004694 iodide salts Chemical class 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- TTXIPMFMHNUMTI-UHFFFAOYSA-N [Ir].[Rh].[Ti] Chemical compound [Ir].[Rh].[Ti] TTXIPMFMHNUMTI-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- VURFVHCLMJOLKN-UHFFFAOYSA-N diphosphane Chemical compound PP VURFVHCLMJOLKN-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910000043 hydrogen iodide Inorganic materials 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- DKNPRRRKHAEUMW-UHFFFAOYSA-N Iodine aqueous Chemical compound [K+].I[I-]I DKNPRRRKHAEUMW-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010669 acid-base reaction Methods 0.000 description 1
- 230000006315 carbonylation Effects 0.000 description 1
- 238000005810 carbonylation reaction Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- RAQDACVRFCEPDA-UHFFFAOYSA-L ferrous carbonate Chemical compound [Fe+2].[O-]C([O-])=O RAQDACVRFCEPDA-UHFFFAOYSA-L 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 229910000450 iodine oxide Inorganic materials 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000012450 pharmaceutical intermediate Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- KXAHUXSHRWNTOD-UHFFFAOYSA-K rhodium(3+);triiodide Chemical compound [Rh+3].[I-].[I-].[I-] KXAHUXSHRWNTOD-UHFFFAOYSA-K 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention belongs to the field of chemical synthesis, in particular to an industrial production method of hydriodic acid, which takes iodine, soluble iodide, soluble alkali or soluble oxysalt and water as raw materials, takes an electrosynthesis unit tank consisting of an electrode, an electrode supporting component, a bipolar membrane and a tank body as synthesis equipment, produces the hydriodic acid by an electrochemical synthesis method, wherein the iodine and the soluble iodide are in a cathode tank, soluble alkali liquor or soluble oxyacid salt solution is in an anode tank, and the cathode tank and the anode tank are separated by the bipolar membrane to form a two-chamber electrochemical synthesis unit, the hydriodic acid product produced by the method has extremely high purity, and is synthesized under normal pressure without using inflammable and explosive articles such as phosphorus and the like in the production process, so that the safety of the hydriodic acid produced by the method is greatly improved, only oxygen is produced in the production process, has no pollution to the environment, and is a safe, efficient and green synthetic method for producing the hydroiodic acid.
Description
Technical Field
The invention belongs to the technical field of green synthesis of hydroiodic acid, and particularly relates to an industrial production method of hydroiodic acid.
Technical Field
Hydroiodic acid is an iodine-based inorganic strong acid and has the following uses:
(1) high-end catalyst: the primary use of hydroiodic acid is as a high efficiency catalyst for the synthesis of acetic acid by the methanol carbonylation process. Acetic acid is an important basic chemical raw material, is widely used in the fields of chemical industry, light industry, textile, medicine, printing and dyeing, rubber, pesticides, electronics, food and the like, and has important significance to national economy.
(2) Graphene and other new material fields, integrated circuit industry: graphene is a new material with great application potential and important encouragement of the country. Hydroiodic acid is used as a strong reducing agent and is used for preparing graphene films, graphene fibers, graphene-based flexible conductive materials, graphene-coated glass fibers and the like. In the integrated circuit industry, hydriodic acid is used as an etchant for integrated circuits and also in ion implantation processes in the manufacture of semiconductor devices. Hydriodic acid is also used to make perovskite-type semiconductor materials (such as thin film perovskite solar cells).
(3) Preparation of high purity iodide: hydroiodic acid is the iodine source for the preparation of high purity iodides. High-purity iodides (lithium iodide, rhodium iodide, potassium iodide, calcium iodide, etc.) are important materials indispensable in many fields such as lithium batteries, catalysts, fine chemicals, liquid crystals, semiconductors, medicines, pesticides, developers, reagents, etc. The application of hydroiodic acid changes the traditional process route for preparing iodide by directly using iodine. Taking potassium iodide as an example, the traditional method is to take iodine and potassium hydroxide as raw materials and then add iron powder and potassium carbonate or formic acid to participate in the reaction. The method has complex reaction, low yield, high impurity content of the finished product of potassium iodide, and also generates a large amount of wastes such as iron carbonate and the like which pollute the environment. The hydriodic acid is used as an iodine source to react with the potassium hydroxide, namely, the potassium iodide and the water are directly obtained, namely, the simple acid-base reaction is carried out to generate the salt and the water, and the purity of the finished product potassium iodide is greatly improved due to the fact that the substances participating in the reaction are few and the purity is high.
(4) Other uses are as follows: other uses of hydroiodic acid include: pharmaceutical intermediates, disinfectants, raw materials for dyes and perfumes, analytical reagents, reducing agents in organic chemistry, and the like.
The traditional hydroiodic acid production method is a red phosphorus method, and the specific production process comprises the steps of respectively and slowly adding iodine and red phosphorus into a reactor filled with water, reacting under the conditions of heating and stirring, and generating a solution of phosphorous acid or phosphoric acid and hydroiodic acid according to different iodine dosage. And filtering the solution after reaction, heating and distilling the filtrate, and collecting fractions at 125-130 ℃ to prepare a 57% hydriodic acid solution. If free I2 exists, adding water for dilution before distillation, heating to boil, adding 50% hypophosphorous acid until the color of iodine disappears, and distilling.
The reaction equation is as follows:
2P+3I2+6H2O＝2H3PO3+6HI
2P+5I2+8H2O＝2H3PO4+10HI
as can be seen from the reaction equation, red phosphorus is needed in the method, phosphorus belongs to flammable substances, and side reactions exist in the reaction, and under the heating condition, substances such as phosphine, diphosphine tetrahydro and the like are likely to be generated, the phosphine is a highly toxic and easily spontaneous combustion gas, and the heart, the respiratory system, the kidney, the intestines and stomach, the nervous system and the liver are affected by the inhaled phosphine. The diphosphatidylethylene belongs to an easily natural substance and has certain safety risk.
The use of phosphorus also produces a waste liquid containing phosphoric acid and phosphorous acid, which is finally treated as a hazardous waste, and thus, there is a problem in terms of environmental safety.
The electrochemical synthesis method of hydroiodic acid is also reported in documents, but the synthesis reaction unit of the method has the defects of three chambers and multiple chambers, complex operation, extremely high equipment cost, difficult control and the like.
Therefore, the need for a simple, safe, environment-friendly preparation method of hydroiodic acid with low manufacturing cost and high product purity is one of the problems to be solved urgently in the field.
Disclosure of Invention
The invention takes iodine, soluble iodide, soluble alkali or soluble oxysalt and water as raw materials, the production of the hydroiodic acid is carried out by taking an electrosynthesis unit tank consisting of an electrode, an electrode supporting component, a bipolar membrane and a tank body as synthesis equipment and adopting an electrochemical synthesis method, in the production process, iodine and soluble iodide are in a cathode tank, soluble alkali liquor or soluble oxysalt is in an anode tank, the cathode tank and the anode tank are separated by a bipolar membrane to form a two-chamber electrochemical synthesis unit, the hydroiodic acid product produced by the method has extremely high purity, the synthesis is carried out under normal pressure without using inflammable and explosive materials such as phosphorus and the like in the production process, so that the safety of producing the hydroiodic acid by the method is greatly improved, only oxygen is generated in the production process, has no pollution to the environment, and is a safe, efficient and green synthetic method for producing the hydroiodic acid.
In the synthesis process, only iodine and water are subjected to chemical reaction, soluble iodide and soluble alkali solution or soluble oxysalt can be recycled, and the reaction raw materials are relatively pure, so that the purity of the target product is relatively high. The production process uses electricity as a synthesis driving force, does not use dangerous red phosphorus, and the synthesis is carried out at a lower temperature and under normal pressure, so that the safety of producing the hydroiodic acid by the method is greatly improved, waste liquid of dangerous wastes, namely phosphoric acid and phosphorous acid is not generated, the cost for treating the dangerous wastes is avoided, and the environmental protection pressure is greatly reduced.
The main technical scheme of the invention is as follows:
an industrial production method of hydroiodic acid comprises the following steps:
the invention firstly adopts an electrosynthesis unit device which comprises
(1) Two reaction chambers separated by a bipolar membrane;
(2) the cathode electrode plate and the anode electrode plate are respectively arranged on two sides of the bipolar membrane; the side of the cathode plate is provided with a cathode groove, wherein cathode liquid is put into the cathode groove, and the cathode liquid consists of aqueous solution containing iodine and soluble iodide; an anode tank is arranged on one side of the anode plate, and soluble alkali solution or soluble oxoacid salt solution is put into the anode tank to be used as anode liquid;
wherein the voltage applied between the cathode plate and the anode plate is 1-20V direct current;
the catholyte consists of: the molar ratio of iodine to soluble iodide is 1:1-1:5, the mass concentration range of iodine prepared by dissolving the iodine and the soluble iodide in pure water is 1% -50%, and the mass concentration range of iodine ions is 1% -60%; the mass concentration of the anolyte soluble alkali solution or the soluble oxoacid salt solution is 0.1 to 50 percent;
the two sides of the bipolar membrane are respectively provided with a cation membrane and an anion membrane, the anode plate faces the anion membrane of the bipolar membrane, and the cathode plate faces the cation membrane of the bipolar membrane; wherein the anion membrane can allow anions to pass through and can not allow cations to pass through; the cation membrane can allow cations to pass through and anions cannot pass through.
On the basis of the synthesis device, the inventor further provides a specific synthesis process:
(1) putting iodine and soluble iodide into a cathode tank, wherein the molar ratio of the iodine to the soluble iodide is 1:1-1:5, the mass concentration range of the iodine after mixing with water is 1-50%, and the mass concentration range of iodine ions is 1-60%, so that the electrosynthesis cathode solution is obtained; the molar ratio of iodine to soluble iodide may be chosen larger, but uneconomical;
(2) adding deionized water into a container, slowly adding soluble alkali solid or soluble oxysalt, continuously stirring, adjusting the mass concentration of the solution to be 0.1-50% after the soluble alkali or the soluble oxysalt is completely dissolved, and adding the solution into an anode tank to obtain the electrosynthesis anolyte; the mass concentration of the anolyte can be selected to be larger, but the effect is deteriorated;
(3) the cathode slot and the anode slot are isolated by a bipolar membrane, and an electrosynthesis power supply is started:
in the cathode tank, iodine is subjected to the action of 1-20V direct current voltage to obtain electrons, the electrons are changed into iodine ions, and the iodine ions are combined with hydrogen ions ionized from water to generate hydroiodic acid;
under the action of 1-20V direct current voltage, hydroxide radicals are transferred to the anode to lose electrons so as to generate oxygen and water;
when the current is gradually reduced from constant to light, extracting the catholyte to observe that the color is changed from black to light red, detecting the content of free iodine in the catholyte, and stopping the reaction to finish the reaction when the content of the free iodine is reduced to a certain degree and the mass fraction is less than 1% in general; the reaction may be continued until the free iodine is reduced to 0.1% and then the reaction may be terminated.
The reaction equation of the above reaction process is as follows:
anode ionization equation: 4OH－-4e－＝O2+2H2O
Cathode ionization equation: 2I2+4e-＝4I-
Between two electrodes: 4H2O＝4OH-+4H+
The general chemical reaction formula: 2I2+2H2O→4HI+O2
H between the cathode and anode composite layers of the bipolar membrane under the action of the DC electric field of the cathode and anode plates2Dissociation of O into H+And OH-and through the cation and anion membranes, respectively, as H+And a source of OH-ions at the cathode, due to I2Has a standard electrode potential of 0.5345V and a standard electrode potential of 0V for hydrogen ions, indicating I2Is more oxidizing than hydrogen ions, so that I2More readily available electrons from the cathode, I2Two electrons obtained at the cathode become 2 iodide ions, H between the iodide ions and the bipolar membrane composite layer2The hydrogen ions dissociated from O are combined into hydrogen iodide, and the hydrogen iodide becomes hydroiodic acid after being dissolved in water. At the same time, H between the anode and the bipolar membrane composite layer2OH-ions dissociated from the O migrate to the anode to be discharged to generate oxygen and water, and new hydrogen ions and hydroxide ions are continuously dissociated from the water under the direct-current electric field, so that the hydrogen ions continuously move to the cathode, the hydroxide ions move to the anode, the iodine continuously obtains electrons from the cathode and is changed into iodine ions, and current is formed between the cathode and the anode, so that the whole reaction can be continuously carried out.
Further, in order to obtain a preparation method which can be applied industrially, the inventor further optimizes the preparation method on the basis of the process to obtain the following industrial preparation method:
(1) putting iodine and soluble iodide into a catholyte circulating tank according to the mol ratio of 1:1-1:5, mixing with water to prepare a solution with the iodine mass concentration of 1-50% and the iodine ion mass concentration of 1-60%, namely the electrosynthesis catholyte;
(2) adding deionized water into a container, slowly adding soluble alkali or soluble oxysalt solid, continuously stirring, adjusting the solid to be a solution with the mass concentration of 0.1-50% after the solid is completely dissolved, and then adding the prepared solution into an anolyte circulating tank;
(3) respectively starting a cathode tank liquid circulating pump, an anode tank liquid circulating pump and an anolyte cooling circulating pump, pumping liquid in an anolyte tank and liquid in a catholyte tank into an anode tank and a cathode tank for reaction, simultaneously keeping the circulation of catholyte and anolyte, and continuously circulating catholyte between the cathode tank and the catholyte circulating tank, so that the concentration of the catholyte is ensured to be uniform, and the anolyte is continuously circulated between the anode tank and the anolyte circulating tank, so that the concentration of the anolyte is ensured to be uniform;
(4) turning on the electric synthetic power supply:
in the cathode tank, iodine is subjected to the action of 1-20V direct current voltage to obtain electrons, the electrons are changed into iodine ions, and the iodine ions are combined with hydrogen ions ionized from water to generate hydroiodic acid;
under the action of 1-20V direct current voltage, hydroxide radicals are transferred to the anode to lose electrons so as to generate oxygen and water;
when the current is gradually reduced from constant to light, extracting the catholyte to observe that the color is changed from black to light red, detecting the content of free iodine in the catholyte, and finishing the synthesis when the mass fraction of the free iodine is less than 1%;
(5) the synthesis process can properly release heat, the temperature of the material rises, and the temperature of the circulating liquid needs to be controlled between 0 and 70 ℃ through an anolyte cooler, so that the equipment is prevented from being damaged by high temperature;
(6) the synthesis process is completed under normal pressure, the evacuation port of the anode system is arranged on the anolyte circulating tank, and the generated oxygen is evacuated from the evacuation port;
(7) after the synthesis is finished, pumping the catholyte into a temporary storage tank of dilute hydriodic acid solution by a catholyte circulating pump;
(8) pumping a dilute hydriodic acid solution into a distillation kettle, starting stirring, starting heating, gradually raising the temperature of the material to 125-140 ℃, collecting front fraction into a front fraction tank for recycling, and collecting fractions at the temperature of 125-130 ℃ to obtain a product hydriodic acid;
the process is an industrial implementation process and can meet the requirement of large-scale production, the common process and the industrial production process use soluble iodide to dissolve iodine, and the soluble iodide comprises hydriodic acid, sodium iodide, potassium iodide, calcium iodide, lithium iodide, magnesium iodide, zinc iodide, aluminum iodide, ferrous iodide, rubidium iodide, cesium iodide, barium iodide, strontium iodide, titanium tetraiodide, cobalt iodide and a mixture of any several of the above in any proportion; the preferred iodides are hydriodic acid, potassium iodide and sodium iodide, and the iodides are cheap and easily obtained, so that the cost is reduced;
the soluble alkali is selected from lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide, barium hydroxide, strontium hydroxide and calcium hydroxide, or a mixture of any several of the above and any proportion, wherein the preferred alkali is potassium hydroxide, sodium hydroxide and lithium hydroxide; the soluble oxysalt comprises sulfate, phosphate, nitrate, carbonate and the like, or a mixture of any several of the sulfate, the phosphate, the nitrate, the carbonate and the like in any proportion.
The concentration of the further soluble alkali liquor is controlled between 2 percent and 20 percent;
the electrosynthesis anode is a corrosion-resistant low oxygen evolution potential electrode, and the adopted electrosynthesis cathode is a corrosion-resistant high hydrogen evolution potential electrode; the anode plate and the cathode plate are made of graphite and titanium or are made of titanium serving as a base material and are externally plated with a corrosion-resistant noble metal plating layer, wherein the noble metal plating layer comprises ruthenium, rhodium, iridium, platinum, palladium, nickel, tantalum, gold, any noble metal and a noble metal mixed plating layer in any proportion;
on the basis, the cathode plate is preferably a titanium palladium rhodium plated electrode or a titanium iridium rhodium plated electrode or a titanium electrode, and the anode plate is preferably a titanium palladium rhodium plated electrode or a titanium iridium rhodium plated electrode.
The synthetic voltage is 2-10V; the synthesis temperature is 10-40 ℃.
In order to improve the production efficiency, the plurality of electrosynthesis unit tanks can be connected in series or in parallel, preferably in parallel, so that more capacity is provided.
In conclusion, the invention provides a brand-new industrial production method of hydroiodic acid, the hydroiodic acid produced by the method has extremely high purity, flammable and explosive materials such as phosphorus and the like are not used in the production process, the synthesis is carried out under normal pressure, the safety of producing the hydroiodic acid by the method is greatly improved, only oxygen is produced in the production process, and the method is free from environmental pollution and is a safe, efficient and green synthesis method for producing the hydroiodic acid.
Drawings
Fig. 1 is a schematic structural diagram of an electrosynthesis unit according to the present invention.
The specific implementation mode is as follows:
the technical solution of the present invention is not limited to the embodiments listed below, and includes appropriate extensions according to the content of the embodiments.
Example 1
A method suitable for the industrial production of hydroiodic acid comprises the following steps:
a. preparing catholyte, putting iodine and hydroiodic acid into a catholyte circulating tank according to the mol ratio of 1:1.2, mixing with water, adjusting the mass concentration range of iodine to be between 20 and 25 percent and the mass concentration range of iodine ions to be between 24 and 30 percent, adding 100g of iodine and 106g of hydroiodic acid with the concentration of 57 percent together, and completing preparation when the iodine is completely dissolved.
b. Preparing anolyte, adding deionized water into a container, slowly adding potassium hydroxide solid, continuously stirring, after potassium hydroxide is completely dissolved, preparing 1000g of aqueous alkali with the concentration of 5% -6%, adding the aqueous alkali into an anolyte circulating tank, and continuously recycling the anolyte.
c. Respectively starting a catholyte circulating pump and an anolyte circulating pump, controlling the temperature of anolyte by an anolyte cooling circulating pump to be between 30 and 40 ℃, starting an electrosynthesis power supply, controlling the voltage of a direct current power supply to be maintained between 2 and 3V, when the current is gradually reduced from constant to constant, extracting catholyte and observing the color, and detecting the content of free iodine in the catholyte when the color is changed from black to pale red, and after the mass fraction of the free iodine is less than 1 percent, finishing the synthesis, and pumping the catholyte into a hydriodic acid dilute solution temporary storage tank.
d. Pumping the dilute hydroiodic acid solution into a distillation kettle, and heating the dilute hydroiodic acid solution in the kettle. The material temperature is raised to 125-140 ℃, the front fraction is collected in a front fraction tank for recycling, the fraction at the temperature of 125-130 ℃ is collected to obtain 251g of a product, 166g of a front fraction containing 10% of hydriodic acid and distilled mother liquor are obtained, the total yield of iodine is more than 99%, the content of hydriodic acid products is 57.2%, and the obtained front fraction and distilled mother liquor can be used for preparing cathode liquor, and dissolved iodine returns to a production system.
The product index obtained is as follows:
| test item | Detecting a value |
| Content% | 57.2 |
| Burning residue | ≤0.01 |
| Chloride and bromide (in terms of Cl)% | ≤0.002 |
| Free iodine% | ≤0.06 |
| Sulfate% | ＜0.002 |
| Phosphate content% | ≤0.030 |
| Iron% | ＜0.0003 |
| Heavy metal (in Pb)% | ＜0.0005 |
| Density of | ≥1.70 |
The electrosynthesis device adopted by the process comprises two reaction chambers separated by a bipolar membrane, cathode electrode plates and anode electrode plates are respectively arranged on two sides of the bipolar membrane, one side of the cathode electrode plate is a cathode groove, and one side of the anode electrode plate is an anode groove; the two sides of the bipolar membrane are respectively provided with a cation membrane and an anion membrane, the anode plate faces the anion membrane of the bipolar membrane, and the cathode plate faces the cation membrane of the bipolar membrane;
wherein the anion membrane can allow anions to pass through and can not allow cations to pass through; the cation membrane can allow cations to pass through and anions cannot pass through.
Example 2
A method suitable for the industrial production of hydroiodic acid comprises the following steps:
a. preparing catholyte, putting iodine and potassium iodide into a catholyte circulation tank according to the mol ratio of 1:1.2, mixing with water, adjusting the mass concentration range of iodine to be between 20 and 25 percent and the mass concentration range of iodide ions to be between 24 and 30 percent, adding 100g of iodine and 80g of potassium iodide, and completing preparation when all iodine is dissolved
b. Preparing anolyte, adding deionized water into a container, slowly adding sodium hydroxide solid, continuously stirring, after sodium hydroxide is completely dissolved, preparing 1000g of aqueous alkali with the concentration of 7% -8%, adding the aqueous alkali into an anolyte circulating tank, and continuously recycling the anolyte.
c. Respectively starting a catholyte circulating pump and an anolyte circulating pump, controlling the temperature of anolyte by an anolyte cooling circulating pump to be between 20 and 30 ℃, starting an electrosynthesis power supply, controlling the voltage of a direct current power supply to be maintained between 3 and 4V, when the current is gradually reduced from constant to constant, extracting catholyte and observing the color, and detecting the content of free iodine in the catholyte when the color is changed from black to pale red, and after the mass fraction of the free iodine is less than 1 percent, finishing the synthesis, and pumping the catholyte into a hydriodic acid dilute solution temporary storage tank.
d. Pumping the dilute hydroiodic acid solution into a distillation kettle, and heating the dilute hydroiodic acid solution in the kettle. The material temperature is raised to 125-140 ℃, the front fraction is collected in a front fraction tank for recycling, the fraction at the temperature of 125-.
The product index obtained is as follows:
| test item | Detecting a value |
| Content% | 57.3 |
| Burning residue | ≤0.01 |
| Chloride and bromide (in terms of Cl)% | ≤0.002 |
| Free iodine% | ≤0.06 |
| Sulfate% | ＜0.002 |
| Phosphate content% | ≤0.030 |
| Iron% | ＜0.0003 |
| Heavy metal (in Pb)% | ＜0.0005 |
| Density of | ≥1.70 |
The electrosynthesis device adopted by the process comprises two reaction chambers separated by a bipolar membrane, cathode electrode plates and anode electrode plates are respectively arranged on two sides of the bipolar membrane, one side of the cathode electrode plate is a cathode groove, and one side of the anode electrode plate is an anode groove; the two sides of the bipolar membrane are respectively provided with a cation membrane and an anion membrane, the anode plate faces the anion membrane of the bipolar membrane, and the cathode plate faces the cation membrane of the bipolar membrane;
wherein the anion membrane can allow anions to pass through and can not allow cations to pass through; the cation membrane can allow cations to pass through and anions cannot pass through.
Example 3
A method suitable for the industrial production of hydroiodic acid comprises the following steps:
a. preparing catholyte, putting iodine and sodium iodide into a catholyte circulation tank according to the mol ratio of 1:1.3, mixing with water, adjusting the mass concentration range of iodine to be between 20 and 25 percent and the mass concentration range of iodide ions to be between 23 and 32.5 percent, adding 100g of iodine and 77g of sodium iodide together, and completing preparation when all iodine is dissolved
b. Preparing anolyte, adding deionized water into a container, slowly adding sodium sulfate solid, continuously stirring, after the sodium sulfate is completely dissolved, preparing 1000g of solution with the concentration of 5% -6%, adding the solution into an anolyte circulating tank, and continuously recycling the anolyte.
c. Respectively starting a catholyte circulating pump and an anolyte circulating pump, controlling the temperature of anolyte by an anolyte cooling circulating pump to be between 20 and 30 ℃, starting an electrosynthesis power supply, controlling the voltage of a direct current power supply to be maintained between 3 and 4V, when the current is gradually reduced from constant to constant, extracting catholyte and observing the color, and detecting the content of free iodine in the catholyte when the color is changed from black to pale red, and after the mass fraction of the free iodine is less than 1 percent, finishing the synthesis, and pumping the catholyte into a hydriodic acid dilute solution temporary storage tank.
d. Pumping the dilute hydroiodic acid solution into a distillation kettle, and heating the dilute hydroiodic acid solution in the kettle. The temperature of the material is raised to 125-140 ℃, the front fraction is collected in a front fraction tank for recycling, the fraction at the temperature of 125-.
The product index obtained is as follows:
| test item | Detecting a value |
| Content% | 57.1 |
| Burning residue | ≤0.01 |
| Chloride and bromide (in terms of Cl)% | ≤0.002 |
| Free iodine% | ≤0.06 |
| Sulfate% | ＜0.002 |
| Phosphate content% | ≤0.030 |
| Iron% | ＜0.0003 |
| Heavy metal (in Pb)% | ＜0.0005 |
| Density of | ≥1.70 |
The electrosynthesis device adopted by the process comprises two reaction chambers separated by a bipolar membrane, cathode electrode plates and anode electrode plates are respectively arranged on two sides of the bipolar membrane, one side of the cathode electrode plate is a cathode groove, and one side of the anode electrode plate is an anode groove; the two sides of the bipolar membrane are respectively provided with a cation membrane and an anion membrane, the anode plate faces the anion membrane of the bipolar membrane, and the cathode plate faces the cation membrane of the bipolar membrane;
wherein the anion membrane can allow anions to pass through and can not allow cations to pass through; the cation membrane can allow cations to pass through and anions cannot pass through.
Claims (10)
1. An industrial production method of hydroiodic acid is characterized in that an electrochemical synthesis method is adopted, and an electrochemical synthesis unit device comprises:
(1) two reaction chambers separated by a bipolar membrane;
(2) the cathode electrode plate and the anode electrode plate are respectively arranged on two sides of the bipolar membrane; the side of the cathode plate is provided with a cathode groove, wherein cathode liquid is put into the cathode groove, and the cathode liquid consists of aqueous solution containing iodine and soluble iodide; an anode tank is arranged on one side of the anode plate, and soluble alkali solution or soluble oxoacid salt solution is put into the anode tank to be used as anode liquid;
wherein the voltage applied between the cathode plate and the anode plate is 1-20V direct current;
the catholyte consists of: the molar ratio of iodine to soluble iodide is 1:1-1:5, the mass concentration range of iodine prepared by dissolving the iodine and the soluble iodide in pure water is 1% -50%, and the mass concentration range of iodine ions is 1% -60%; the mass concentration of the anolyte soluble alkali solution or the soluble oxoacid salt solution is 0.1 to 50 percent;
after applying a voltage to the plates, the following reactions occur:
anode ionization equation: 4OH－-4e－＝O2+2H2O
Cathode ionization equation: 2I2+4e-＝4I-
Between two electrodes: 4H2O＝4OH-+4H+
The general chemical reaction formula: 2I2+2H2O→4HI+O2。
When the current is gradually reduced from constant to light, extracting the catholyte to observe that the color is changed from black to light red, detecting the content of free iodine in the catholyte, and stopping reaction after the mass fraction of the free iodine is less than 1%.
2. The industrial production method of hydroiodic acid according to claim 1, which comprises the steps of: the method comprises the following steps:
(1) putting iodine and soluble iodide into a catholyte circulating tank according to the mol ratio of 1:1-1:5, mixing with water to prepare a solution with the iodine mass concentration of 1-50% and the iodine ion mass concentration of 1-60%, namely the electrosynthesis catholyte;
(2) adding deionized water into a container, slowly adding soluble alkali or soluble oxysalt solid, continuously stirring, adjusting the mass concentration of the solution to be 0.1-50% after the soluble alkali or the soluble oxysalt is completely dissolved, and then adding the prepared soluble alkali liquor or the prepared soluble oxysalt solution into an anolyte circulating tank;
(3) respectively starting a cathode tank liquid circulating pump, an anode tank liquid circulating pump and an anolyte cooling circulating pump, pumping liquid in an anolyte tank and liquid in a catholyte tank into an anode tank and a cathode tank for reaction, simultaneously keeping the circulation of catholyte and anolyte, and continuously circulating catholyte between the cathode tank and the catholyte circulating tank, so that the concentration of the catholyte is ensured to be uniform, and the anolyte is continuously circulated between the anode tank and the anolyte circulating tank, so that the concentration of the anolyte is ensured to be uniform;
(4) turning on an electric synthesis power supply:
in the cathode tank, iodine is subjected to the action of 1-20V direct current voltage to obtain electrons, the electrons are changed into iodine ions, and the iodine ions are combined with hydrogen ions ionized from water to generate hydroiodic acid;
under the action of 1-20V direct current voltage, hydroxide radicals are transferred to the anode to lose electrons so as to generate oxygen and water;
when the current is gradually reduced from constant to light, extracting the catholyte to observe that the color is changed from black to light red, detecting the content of free iodine in the catholyte, and finishing the synthesis when the mass fraction of the free iodine is less than 1%;
(5) the synthesis process can properly release heat, the temperature of the material rises, and the temperature of the circulating liquid needs to be controlled between 0 and 70 ℃ through an anolyte cooler, so that the equipment is prevented from being damaged by high temperature;
(6) the synthesis process is completed under normal pressure, the evacuation port of the anode system is arranged on the anolyte circulating tank, and the generated oxygen is evacuated from the evacuation port;
(7) after the synthesis is finished, pumping the catholyte into a temporary storage tank of dilute hydriodic acid solution by a catholyte circulating pump;
(8) pumping the dilute hydriodic acid solution into a distillation kettle, starting stirring, starting heating, gradually raising the temperature of the material to 125-140 ℃, collecting front fraction into a front fraction tank for recycling, and collecting the fraction at the temperature of 125-130 ℃ to obtain the product hydriodic acid.
3. The industrial production method of hydroiodic acid according to claim 1 or 2, which comprises: the soluble iodide is selected from one or more of hydriodic acid, sodium iodide, potassium iodide, calcium iodide, lithium iodide, magnesium iodide, zinc iodide, aluminum iodide, ferrous iodide, rubidium iodide, cesium iodide, barium iodide, strontium iodide, titanium tetraiodide and cobalt iodide, and the mixture is in any proportion.
4. The industrial production method of hydroiodic acid according to claim 3, characterized in that: the soluble iodide is preferably one or more selected from hydriodic acid, potassium iodide and sodium iodide.
5. The industrial production method of hydroiodic acid according to claim 1 or 2, which comprises: the soluble alkali is selected from one or a mixture of any several of lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide, barium hydroxide, strontium hydroxide and calcium hydroxide in any proportion; the soluble oxysalt is selected from one or a mixture of any several of soluble inorganic oxysalts such as sulfate, nitrate, phosphate and carbonate in any proportion.
6. The industrial production method of hydroiodic acid according to claim 5, which comprises the following steps: the soluble alkali is preferably potassium hydroxide or sodium hydroxide; the concentration is controlled between 1% and 20%.
7. The industrial production method of hydroiodic acid according to claim 1 or 2, which comprises: the electrosynthesis anode is a corrosion-resistant low oxygen evolution potential electrode, and the adopted electrosynthesis cathode is a corrosion-resistant high hydrogen evolution potential electrode; the anode plate and the cathode plate are made of graphite and titanium or are made of titanium serving as a base material and are externally plated with a corrosion-resistant noble metal plating layer, wherein the noble metal plating layer comprises ruthenium, rhodium, iridium, platinum, palladium, nickel, tantalum, gold, any noble metal and a noble metal mixed plating layer in any proportion.
8. The industrial production method of hydroiodic acid according to claim 1 or 2, which comprises: the cathode is preferably a titanium-plated palladium-rhodium electrode or a titanium-plated iridium-rhodium electrode or a titanium electrode, and the anode plate is preferably a titanium-plated palladium-rhodium electrode or a titanium-plated iridium-rhodium electrode.
9. The industrial production method of hydroiodic acid according to claim 1 or 2, which comprises: the synthetic direct current voltage is 2-10V; the synthesis temperature is 10-40 ℃.
10. The process for the production of hydroiodic acid according to claim 1 or 3, characterized by: in the synthesis process, a plurality of electrosynthesis unit tanks can be connected in series or in parallel, and preferably are connected in parallel.
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| CN111394746A (en) * | 2020-04-10 | 2020-07-10 | 山东博苑医药化学有限公司 | Electrochemical co-production method of potassium iodate and hydroiodic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4053376A (en) * | 1976-10-27 | 1977-10-11 | Ppg Industries, Inc. | Electrolytic production of hydrogen iodide |
| US5520793A (en) * | 1995-04-03 | 1996-05-28 | Benham Electrosynthesis Company, Inc. | Methods of producing hydrogen iodide electrochemically |
| JPH0953195A (en) * | 1995-08-18 | 1997-02-25 | Permelec Electrode Ltd | Production of hydroiodic acid |
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2018
- 2018-07-16 CN CN201810780327.3A patent/CN110724968B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4053376A (en) * | 1976-10-27 | 1977-10-11 | Ppg Industries, Inc. | Electrolytic production of hydrogen iodide |
| US5520793A (en) * | 1995-04-03 | 1996-05-28 | Benham Electrosynthesis Company, Inc. | Methods of producing hydrogen iodide electrochemically |
| JPH0953195A (en) * | 1995-08-18 | 1997-02-25 | Permelec Electrode Ltd | Production of hydroiodic acid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111394746A (en) * | 2020-04-10 | 2020-07-10 | 山东博苑医药化学有限公司 | Electrochemical co-production method of potassium iodate and hydroiodic acid |
| 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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Denomination of invention: An Industrial Production Method of Hydroiodic Acid Granted publication date: 20230623 Pledgee: Taixi sub branch of Taian Bank Co.,Ltd. Pledgor: TAIAN HANWEI GROUP Co.,Ltd. Registration number: Y2024980020367 |
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