CN109621904A - The purification method of nickeliferous aqueous solution cleanser and nickeliferous aqueous solution - Google Patents
The purification method of nickeliferous aqueous solution cleanser and nickeliferous aqueous solution Download PDFInfo
- Publication number
- CN109621904A CN109621904A CN201811167866.6A CN201811167866A CN109621904A CN 109621904 A CN109621904 A CN 109621904A CN 201811167866 A CN201811167866 A CN 201811167866A CN 109621904 A CN109621904 A CN 109621904A
- Authority
- CN
- China
- Prior art keywords
- aqueous solution
- nickel
- nickeliferous
- nickeliferous aqueous
- compound
- Prior art date
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- Granted
Links
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 111
- 238000000034 method Methods 0.000 title claims abstract description 48
- 238000000746 purification Methods 0.000 title claims abstract description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 205
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 99
- 150000001875 compounds Chemical class 0.000 claims abstract description 43
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 claims abstract description 37
- 150000003839 salts Chemical class 0.000 claims abstract description 33
- 239000008394 flocculating agent Substances 0.000 claims abstract description 20
- 229920000768 polyamine Polymers 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 18
- 150000001341 alkaline earth metal compounds Chemical class 0.000 claims abstract description 11
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 9
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical class S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 33
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 17
- 229920000642 polymer Polymers 0.000 claims description 15
- 239000000701 coagulant Substances 0.000 claims description 13
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 9
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 8
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 7
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- IHYNKGRWCDKNEG-UHFFFAOYSA-N n-(4-bromophenyl)-2,6-dihydroxybenzamide Chemical group OC1=CC=CC(O)=C1C(=O)NC1=CC=C(Br)C=C1 IHYNKGRWCDKNEG-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Chemical class 0.000 claims description 3
- 150000001399 aluminium compounds Chemical class 0.000 claims description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 150000002506 iron compounds Chemical class 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 229910000000 metal hydroxide Inorganic materials 0.000 claims 1
- 150000004692 metal hydroxides Chemical class 0.000 claims 1
- 150000002816 nickel compounds Chemical class 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 19
- 238000012545 processing Methods 0.000 description 19
- 238000003756 stirring Methods 0.000 description 19
- 239000003153 chemical reaction reagent Substances 0.000 description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 14
- 239000001110 calcium chloride Substances 0.000 description 14
- 229910001628 calcium chloride Inorganic materials 0.000 description 14
- 238000005259 measurement Methods 0.000 description 11
- 239000002351 wastewater Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000000654 additive Substances 0.000 description 8
- 230000000996 additive effect Effects 0.000 description 8
- 150000001412 amines Chemical class 0.000 description 7
- 229910001453 nickel ion Inorganic materials 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 229920002873 Polyethylenimine Polymers 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical class NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 5
- 150000001342 alkaline earth metals Chemical class 0.000 description 5
- 125000000219 ethylidene group Chemical group [H]C(=[*])C([H])([H])[H] 0.000 description 5
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- -1 iron ion Chemical class 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000005345 coagulation Methods 0.000 description 4
- 230000015271 coagulation Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229960001124 trientine Drugs 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 description 2
- LWBPNIJBHRISSS-UHFFFAOYSA-L beryllium dichloride Chemical compound Cl[Be]Cl LWBPNIJBHRISSS-UHFFFAOYSA-L 0.000 description 2
- RFVVBBUVWAIIBT-UHFFFAOYSA-N beryllium nitrate Chemical compound [Be+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O RFVVBBUVWAIIBT-UHFFFAOYSA-N 0.000 description 2
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 2
- KQHXBDOEECKORE-UHFFFAOYSA-L beryllium sulfate Chemical compound [Be+2].[O-]S([O-])(=O)=O KQHXBDOEECKORE-UHFFFAOYSA-L 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- JGIATAMCQXIDNZ-UHFFFAOYSA-N calcium sulfide Chemical compound [Ca]=S JGIATAMCQXIDNZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000000909 electrodialysis Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- 229910001631 strontium chloride Inorganic materials 0.000 description 2
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 2
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- UBXAKNTVXQMEAG-UHFFFAOYSA-L strontium sulfate Chemical compound [Sr+2].[O-]S([O-])(=O)=O UBXAKNTVXQMEAG-UHFFFAOYSA-L 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- HTLPAEWBUABNNS-UHFFFAOYSA-L 2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate;hydron;nickel(2+) Chemical compound [Ni+2].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O HTLPAEWBUABNNS-UHFFFAOYSA-L 0.000 description 1
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- UUYQSLQNSVVXCC-UHFFFAOYSA-N CN.C(C=C)(=O)OCCN(C)C Chemical compound CN.C(C=C)(=O)OCCN(C)C UUYQSLQNSVVXCC-UHFFFAOYSA-N 0.000 description 1
- UNMYWSMUMWPJLR-UHFFFAOYSA-L Calcium iodide Chemical compound [Ca+2].[I-].[I-] UNMYWSMUMWPJLR-UHFFFAOYSA-L 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- FTGBMOAMUISOTM-UHFFFAOYSA-N O.O.O.[Na].C(=O)O Chemical compound O.O.O.[Na].C(=O)O FTGBMOAMUISOTM-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 description 1
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 229920006318 anionic polymer Polymers 0.000 description 1
- 229940077746 antacid containing aluminium compound Drugs 0.000 description 1
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 1
- NKQIMNKPSDEDMO-UHFFFAOYSA-L barium bromide Chemical compound [Br-].[Br-].[Ba+2] NKQIMNKPSDEDMO-UHFFFAOYSA-L 0.000 description 1
- 229910001620 barium bromide Inorganic materials 0.000 description 1
- ISFLYIRWQDJPDR-UHFFFAOYSA-L barium chlorate Chemical compound [Ba+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O ISFLYIRWQDJPDR-UHFFFAOYSA-L 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- SGUXGJPBTNFBAD-UHFFFAOYSA-L barium iodide Chemical compound [I-].[I-].[Ba+2] SGUXGJPBTNFBAD-UHFFFAOYSA-L 0.000 description 1
- 229910001638 barium iodide Inorganic materials 0.000 description 1
- 229940075444 barium iodide Drugs 0.000 description 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 1
- WAKZZMMCDILMEF-UHFFFAOYSA-H barium(2+);diphosphate Chemical compound [Ba+2].[Ba+2].[Ba+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O WAKZZMMCDILMEF-UHFFFAOYSA-H 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical compound [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 229910001621 beryllium bromide Inorganic materials 0.000 description 1
- PBKYCFJFZMEFRS-UHFFFAOYSA-L beryllium bromide Chemical compound [Be+2].[Br-].[Br-] PBKYCFJFZMEFRS-UHFFFAOYSA-L 0.000 description 1
- 229910000023 beryllium carbonate Inorganic materials 0.000 description 1
- ZBUQRSWEONVBES-UHFFFAOYSA-L beryllium carbonate Chemical compound [Be+2].[O-]C([O-])=O ZBUQRSWEONVBES-UHFFFAOYSA-L 0.000 description 1
- 229910001627 beryllium chloride Inorganic materials 0.000 description 1
- JZKFIPKXQBZXMW-UHFFFAOYSA-L beryllium difluoride Chemical compound F[Be]F JZKFIPKXQBZXMW-UHFFFAOYSA-L 0.000 description 1
- 229910001633 beryllium fluoride Inorganic materials 0.000 description 1
- JUCWKFHIHJQTFR-UHFFFAOYSA-L beryllium iodide Chemical compound [Be+2].[I-].[I-] JUCWKFHIHJQTFR-UHFFFAOYSA-L 0.000 description 1
- 229910001639 beryllium iodide Inorganic materials 0.000 description 1
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 1
- 239000001639 calcium acetate Substances 0.000 description 1
- 229960005147 calcium acetate Drugs 0.000 description 1
- 235000011092 calcium acetate Nutrition 0.000 description 1
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 description 1
- 229910000020 calcium bicarbonate Inorganic materials 0.000 description 1
- 229910001622 calcium bromide Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- WGEFECGEFUFIQW-UHFFFAOYSA-L calcium dibromide Chemical compound [Ca+2].[Br-].[Br-] WGEFECGEFUFIQW-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 229910001640 calcium iodide Inorganic materials 0.000 description 1
- 229940046413 calcium iodide Drugs 0.000 description 1
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 229940075933 dithionate Drugs 0.000 description 1
- 229960001484 edetic acid Drugs 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 description 1
- 239000002370 magnesium bicarbonate Substances 0.000 description 1
- 229910000022 magnesium bicarbonate Inorganic materials 0.000 description 1
- 235000014824 magnesium bicarbonate Nutrition 0.000 description 1
- OTCKOJUMXQWKQG-UHFFFAOYSA-L magnesium bromide Chemical compound [Mg+2].[Br-].[Br-] OTCKOJUMXQWKQG-UHFFFAOYSA-L 0.000 description 1
- 229910001623 magnesium bromide Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- QENHCSSJTJWZAL-UHFFFAOYSA-N magnesium sulfide Chemical compound [Mg+2].[S-2] QENHCSSJTJWZAL-UHFFFAOYSA-N 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- LXICEIPQWZZDRV-UHFFFAOYSA-N magnesium;sulfane Chemical compound [Mg].S LXICEIPQWZZDRV-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006385 ozonation reaction Methods 0.000 description 1
- NMCOHHUAMHYFBL-UHFFFAOYSA-N piperazine;2-piperazin-1-ylethanamine Chemical compound C1CNCCN1.NCCN1CCNCC1 NMCOHHUAMHYFBL-UHFFFAOYSA-N 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- ZOCLAPYLSUCOGI-UHFFFAOYSA-M potassium hydrosulfide Chemical compound [SH-].[K+] ZOCLAPYLSUCOGI-UHFFFAOYSA-M 0.000 description 1
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- INDBQLZJXZLFIT-UHFFFAOYSA-N primaquine Chemical compound N1=CC=CC2=CC(OC)=CC(NC(C)CCCN)=C21 INDBQLZJXZLFIT-UHFFFAOYSA-N 0.000 description 1
- 229960005179 primaquine Drugs 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- GIKWXTHTIQCTIH-UHFFFAOYSA-L radium bromide Chemical compound [Br-].[Br-].[Ra+2] GIKWXTHTIQCTIH-UHFFFAOYSA-L 0.000 description 1
- 229910001624 radium bromide Inorganic materials 0.000 description 1
- 229940075451 radium bromide Drugs 0.000 description 1
- RWRDJVNMSZYMDV-UHFFFAOYSA-L radium chloride Chemical compound [Cl-].[Cl-].[Ra+2] RWRDJVNMSZYMDV-UHFFFAOYSA-L 0.000 description 1
- 229910001630 radium chloride Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- UNHKSXOTUHOTAB-UHFFFAOYSA-N sodium;sulfane Chemical group [Na].S UNHKSXOTUHOTAB-UHFFFAOYSA-N 0.000 description 1
- YJPVTCSBVRMESK-UHFFFAOYSA-L strontium bromide Chemical compound [Br-].[Br-].[Sr+2] YJPVTCSBVRMESK-UHFFFAOYSA-L 0.000 description 1
- 229910001625 strontium bromide Inorganic materials 0.000 description 1
- 229940074155 strontium bromide Drugs 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 description 1
- 229910001866 strontium hydroxide Inorganic materials 0.000 description 1
- KRIJWFBRWPCESA-UHFFFAOYSA-L strontium iodide Chemical compound [Sr+2].[I-].[I-] KRIJWFBRWPCESA-UHFFFAOYSA-L 0.000 description 1
- 229910001643 strontium iodide Inorganic materials 0.000 description 1
- ZEGFMFQPWDMMEP-UHFFFAOYSA-N strontium;sulfide Chemical compound [S-2].[Sr+2] ZEGFMFQPWDMMEP-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- JOPDZQBPOWAEHC-UHFFFAOYSA-H tristrontium;diphosphate Chemical compound [Sr+2].[Sr+2].[Sr+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JOPDZQBPOWAEHC-UHFFFAOYSA-H 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The present invention relates to the purification methods of nickeliferous aqueous solution cleanser and nickeliferous aqueous solution.The present invention provides a kind of purification method of nickeliferous aqueous solution, reduces the nickel concentration of the aqueous solution containing compound and nickel with the ability being complexed with nickel.Containing in the compound of ability and the aqueous solution of nickel being complexed with nickel, add salt, the polyamines with 3~8 nitrogen-atoms, alkaline earth metal compound of aminodithioformic acid, then addition content is the inorganic flocculating agent of the content of the compound with the ability being complexed with nickel or more, then removes solid content.
Description
Technical field
The present invention relates to can be from containing with removal nickel in the compound of ability and the aqueous solution of nickel being complexed with nickel
Purification method.
Background technique
The known aqueous solution containing nickel uses following processing method: being transported to sewage treatment equipment, such as is added
Add iron ion to become alkalinity and make nickel ion etc. in the form of hydroxide with iron ion, other contained ion coprecipitations etc.
Processing, from aqueous solution separate after discharge etc..
Nickel is a kind of harmful heavy metal, and it is specified to be designated as the 1st class in chemical substance discharge assurance management promotion law
Chemical substance, the important monitoring project being set in environmental criteria relevant to water pollution, the importance of wastewater treatment mention
It is high.
However, coming from plating factory, electronic component/mechanical part manufacturing works, automobile plant, heat power station, rubbish
In the waste water of incineration plant etc. comprising the organic acids such as citric acid, gluconic acid, ethylenediamine tetra-acetic acid (hereinafter referred to as EDTA), cyanogen, amine,
Ammonia and polyphosphoric acid etc. have the compound for the ability being complexed with nickel, the example that can not be handled using hydroxide process as described above
Increase.
In contrast, being carried out not after being chemically treated it has been known that there is the compound that will have the ability being complexed with nickel to nickel
Dissolve the method for processing.However status is, even if using the oxidizing process of chlorine system reagent, electrolytic oxidation, peroxidating is for example utilized
The chemical treatment such as hydrogen-ferrous salt method, Ozonation, wet oxidation process, as existing as caused by the heavy metal element coexisted
The obstruction of oxidation reaction, oxide skin generation the problems such as, can not also carry out sufficient purified treatment.
As the technology for each Heavy Metallic Elements for including in removal waste water, propose for example by adding inorganic flocculating agent
Or organic flocculant carry out aggregation separation removal method, by electrolysis carry out removal method, using active carbon, inorganic adsorbent or
The Adsorption method of high-molecular organic material, the solid method for making waste water heating evaporation, the anti-impregnating method for having used film, electrodialysis or
Ultrafiltration etc..
Even if in the case where having used above-mentioned various methods, there is also following problems, any means be required into
The corresponding improvement of row.Such as:
(1) aggregation separation removal method: being unable to adequately process nickel,
(2) Adsorption method etc.: for example allowing to adsorb nickel, a large amount of solid component can be also generated after processing,
(3) it anti-impregnating method, electrodialysis or ultrafiltration etc.: is difficult to remove when containing organic matter in waste water, and it is handled
It is at high cost,
(4) utilize the solid method of heating evaporation: its facture is many and diverse and processing cost is high etc..
Then propose use the salt of aminodithioformic acid as the heavy metal treatment agent in waste water method (for example,
Referring to patent document 1~4).However, in method documented by these patent documents, from containing with the energy being complexed with heavy metal
The effect of the purified treatment heavy metal is insufficient in the nickel-containing waste water of the compound of power.
In addition, proposing the huge sum of money comprising having the dithionate of the polyamines of three or more amino and amine in the molecule
Belong to inorganic agent (for example, referring to patent document 5).However, in method disclosed Patent Document 5, the purified treatment effect of nickel is
Insufficient.
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2009-249399 bulletin
Patent document 2: Japanese Unexamined Patent Publication 2011-074350 bulletin
Patent document 3: Japanese Unexamined Patent Publication 2014-088477 bulletin
Patent document 4: Japanese Unexamined Patent Publication 2002-177902 bulletin
Patent document 5: No. 5272306 bulletins of Japanese Patent No.
Summary of the invention
Problems to be solved by the invention
The present invention is completed in view of the aforementioned technical background, it is intended that providing: reduction, which contains, to be had and nickel is complexed
Ability compound and nickel aqueous solution nickel concentration cleanser；With used the net of the nickeliferous aqueous solution of the cleanser
Change method.
The solution to the problem
Further investigation has been repeated in the inventors of the present invention in order to solve the above problems, as a result, it has been found that: by using the present invention
Disclosed in novel nickeliferous aqueous solution purification method, so as to reduce in easy method containing with being complexed with nickel
The nickel concentration of the aqueous solution of the compound and nickel of ability, so far completes the present invention.
That is, the present invention has purport below.
[1] a kind of nickeliferous aqueous solution cleanser, which is characterized in that its 100 weight of salt relative to aminodithioformic acid
Part is measured, comprising having 20 parts by weight of polyamines of 3~8 nitrogen-atoms or more and alkaline earth metal compound to form.
[2] a kind of nickeliferous aqueous solution cleanser, which is characterized in that its 100 weight of salt relative to aminodithioformic acid
Part is measured, comprising having 20 parts by weight of polyamines of 3~8 nitrogen-atoms or more, alkaline earth metal compound and inorganic sulphide to form.
[3] the nickeliferous aqueous solution cleanser according to above-mentioned [2], which is characterized in that inorganic sulphide is hydrogen sulfide
Sodium.
[4] the nickeliferous aqueous solution cleanser according to above-mentioned [1] or [2], which is characterized in that aminodithioformic acid
Salt be aminated compounds and carbon disulfide at least one amino in the group being made of primary amino group and secondary amino group
With the reaction product of alkali metal hydroxide.
[5] the nickeliferous aqueous solution cleanser according to above-mentioned [1] or [2], which is characterized in that aminodithioformic acid
Salt be aminated compounds with 2 or more amino in the group being made of primary amino group and secondary amino group and carbon disulfide with
The reaction product of alkali metal hydroxide.
[6] the nickeliferous aqueous solution cleanser according to above-mentioned [1] or [2], which is characterized in that aminodithioformic acid
Salt be piperazine or tetren and carbon disulfide and alkali metal hydroxide reaction product.
[7] a kind of purification method of nickeliferous aqueous solution, which is characterized in that in nickeliferous aqueous solution, addition above-mentioned [1]~
Any one of [6] the nickeliferous aqueous solution cleanser described in, then removes the solid content of generation.
[8] purification method of the nickeliferous aqueous solution according to above-mentioned [7], which is characterized in that nickeliferous aqueous solution is further
Comprising having the compound for the ability being complexed with nickel.
[9] purification method of the nickeliferous aqueous solution according to above-mentioned [8], which is characterized in that there is the energy being complexed with nickel
The compound of power is the compound in the molecule with the functional group in the group for selecting free carboxyl group and amino to form.
[10] purification method of the nickeliferous aqueous solution according to any one of above-mentioned [7]~[9], which is characterized in that
Before removing solid content, inorganic flocculating agent is added.
[11] purification method of the nickeliferous aqueous solution according to any one of above-mentioned [7]~[9], which is characterized in that
Before removing solid content, inorganic flocculating agent and high polymer coagulant are added.
[12] purification method of the nickeliferous aqueous solution according to above-mentioned [10] or [11], which is characterized in that inorganic flocculation
Agent is the substance in the group being made of iron compound and aluminium compound.
The effect of invention
Even if nickeliferous aqueous solution cleanser of the invention for nickel the more difficult nickeliferous aqueous solution of purified treatment (for example,
Aqueous solution containing the compound and nickel with the ability being complexed with nickel) it also can reduce nickel concentration, therefore industrially extremely
It is useful.
Specific embodiment
The present invention is described in detail below.
Nickeliferous aqueous solution cleanser of the invention is characterized in that, 100 weight of salt relative to aminodithioformic acid
Part, comprising having 20 parts by weight of polyamines of 3~8 nitrogen-atoms or more, alkaline earth metal compound to form.
As the salt of aminodithioformic acid, do not have as long as the compound in the molecule with Dithiocarbamyl
It is particularly limited to.It such as can enumerate: make at least one amino in the group being made of primary amino group and secondary amino group
Compound obtained from aminated compounds is reacted with carbon disulfide with alkali metal hydroxide.More preferably make to have selected from by primaquine
Aminated compounds and the carbon disulfide of 2 or more amino in the group of base and secondary amino group composition reacted with alkali metal hydroxide and
Obtained compound.
As the aminated compounds at least one amino in the group being made of primary amino group and secondary amino group, specifically
Can example go out: diethylamine, piperazine, diethylenetriamines, N- (2- amino-ethyl) piperazine, trien, four ethylidene five
Amine, penten, seven ethylidene, eight amine etc..
In these, from the aspect of the process performance from nickel and the stability as compound, preferably make piperazine or
Compound obtained from tetren is reacted with carbon disulfide with alkali metal hydroxide.Wherein, for four ethylidene five
For the salt of the aminodithioformic acid of amine, the tetren as raw material only removes the linear body [reference of main component
Following formula (1)] also the composition comprising analog [referring to following formula (2)~(4)] industrially manufactures outside, therefore, institute
The salt of obtained aminodithioformic acid is also composition, has the shortcomings that become many and diverse in qualitative control.On the contrary, the two of piperazine
Such disadvantage is not present in the salt of thiocarbamic acid, particularly preferably.
As alkali metal hydroxide, from the aspect of being easy to get, particularly preferred sodium hydroxide, potassium hydroxide.
It as the polyamines with 3~8 nitrogen-atoms, such as can enumerate: diethylenetriamines, N- (2- amino-ethyl) piperazine
Piperazine, trien, tetren, penten, seven ethylidene, eight amine, weight average molecular weight 300 poly- sub- second
Base imines.
The additive amount of the polyamines with 3~8 nitrogen-atoms of 100 parts by weight of salt relative to aminodithioformic acid is preferred
It is more than 20 parts by weight.More than 20 parts by weight of addition, so as to obtain sufficient nickel processing capacity.
It as alkaline earth metal compound, such as can enumerate: beryllium fluoride, beryllium chloride, beryllium bromide, beryllium iodide, beryllium oxide, hydrogen
Beryllium oxide, beryllium carbonate, beryllium nitrate, beryllium sulfate, vulcanization beryllium, calcirm-fluoride, calcium chloride, calcium bromide, calcium iodide, calcium oxide, hydroxide
Calcium, calcium carbonate, calcium bicarbonate, calcium nitrate, calcium sulfate, calcium sulfide, calcium phosphate, calcium acetate, calcium oxalate, magnesium chloride, magnesium bromide, iodine
Change magnesium, magnesia, magnesium hydroxide, magnesium carbonate, magnesium bicarbonate, magnesium nitrate, magnesium sulfate, magnesium sulfide, magnesium phosphate, magnesium acetate, fluorination
Strontium, strontium chloride, strontium bromide, strontium iodide, strontium oxide strontia, strontium hydroxide, strontium carbonate, strontium nitrate, strontium sulfate, strontium sulfide, strontium phosphate, second
Sour strontium, barium chloride, barium bromide, barium iodide, barium monoxide, barium hydroxide, barium carbonate, barium nitrate, barium sulphide, barium sulfate, barium sulphide,
Barium phosphate, barium acetate, radium chloride, radium bromide etc..In these from the aspect of being easy to get, particularly preferred calcium chloride, hydrogen-oxygen
Change calcium.
For alkaline earth metal compound, the available nickel processing capacity when 0.01g/L or more is added, in contrast, phase
5 parts by weight or more, which are added, for 100 parts by weight of salt of thiocarbamic acid is advisable, even if being added beyond 250000 parts by weight, nickel
Processing capacity is also certain, thus will increase nickel waste water processing cost when the additive amount excess of alkaline earth metal compound and without
Ji.
It as inorganic sulphide, such as can enumerate: vulcanized sodium, sodium bisulfide, potassium sulfide, potassium hydrogen sulfide, calcium sulfide, sulphur
Change hydrogen calcium, hydrogen sulfide magnesium, ammonium sulfide etc..In these from the viewpoint of economy, preferred sodium bisulfide.
Additive amount preferably 250 parts by weight of the inorganic sulphide of 100 parts by weight of salt relative to aminodithioformic acid with
On.More than 250 parts by weight of addition, available sufficient nickel processing capacity.
Cleanser of the invention is particularly useful for the purified treatment of nickeliferous aqueous solution.
The purification method of nickeliferous aqueous solution of the invention is characterized in that, in nickeliferous aqueous solution, adds this above-mentioned hair
Then bright cleanser removes the solid content of generation.Herein, comprising being fixed using cleanser of the invention in the solid content of generation
The nickel changed.
Purification method of the invention is especially more difficult to the processing of nickel (to be complexed for example, having with nickel containing nickeliferous aqueous solution
Ability compound) and the aqueous solution of nickel be particularly effective.
As the compound with the ability being complexed with nickel, without special as long as the compound for forming complex compound with nickel
It limits.Such as the compound in the molecule with the functional group in the group for selecting free carboxyl group and amino to form can be enumerated.Specifically
For can enumerate: EDTA, polyphosphoric acid etc. can be enumerated especially as the compound for forming firm complex compound with nickel
EDTA。
Salt, the polyamines and alkali with 3~8 nitrogen-atoms of each addition aminodithioformic acid are distinguished in nickeliferous aqueous solution
When earth metal compound, the sequence of addition is not particularly limited.
In order to promptly carry out the removal of solid content, preferably before removing solid content, flocculant is added.As flocculation
Agent, such as can enumerate: inorganic flocculating agent and flocculating polymer is more preferably applied in combination in inorganic flocculating agent, high polymer coagulant
Agent.
As inorganic flocculating agent, commercially available inorganic flocculating agent can be used, be not particularly limited.Such as it can enumerate: three
Aluminium compounds such as the iron compounds such as iron chloride, aluminum sulfate, polyaluminium chloride etc..
When nickeliferous aqueous solution includes the compound with the ability being complexed with nickel, the additive amount of inorganic flocculating agent is preferably set to
It is more than the content contained in nickeliferous aqueous solution with the compound for the ability being complexed with nickel.By by the addition of inorganic flocculating agent
Amount is set as the content with the compound of ability be complexed with nickel or more, aggregation increase, the aqueous solution that is easily reduced that treated
Nickel concentration to standard of drainage below.
The content of the compound with the ability being complexed with nickel in nickeliferous aqueous solution can be by carrying out such as HPLC, gas
Phase chromatography, titration etc. are analyzed to calculate the concentration of the compound with the ability being complexed with nickel in nickeliferous aqueous solution.
Commercially available high polymer coagulant can be used in high polymer coagulant, is not particularly limited.Such as it can enumerate: propylene
Acid polymer, acrylamide polymer, dimethylaminoethyl acrylate methyl ammonia polymerizable methacrylate object etc..From the aspect of aggregation performance, preferably
The acrylate copolymer of weak anionic.By adding high polymer coagulant before removing solid content, the solid content of removal
Processing becomes easy sometimes.
When inorganic flocculating agent and high polymer coagulant is applied in combination, the sequence for adding these flocculants is not particularly limited,
It is preferred that addition inorganic flocculating agent, then adds high polymer coagulant.
As removal solid content method, be not particularly limited, such as can enumerate: be filtered, be centrifugated and
After settling solid content, with the method for supernatant separation etc..
Embodiment
The present invention is specifically explained below, but the present invention is not limited to these embodiments to make explanations.
(analysis method)
Nickel ion concentration in aqueous solution utilizes ICP emission spectrographic analysis device (ICPE-9800, Shimadzu Seisakusho Ltd.'s strain formula
Commercial firm's system) it is measured.
Preparation example 1
The salt of aminodithioformic acid used in embodiment, comparative example is prepared according to the following method.
(preparation of the salt A of aminodithioformic acid)
Piperazine (TOSOH Co., Ltd's system) 112g and pure water 386g are mixed, then, side is stirred at 25 DEG C, in stream of nitrogen gas
Side is mixed respectively for 48 weight % potassium hydroxide 306g (Kishida Chemical Co., Ltd. system) and carbon disulfide 196g
(Kishida Chemical Co., Ltd. system) is divided into 4 parts and is alternately added dropwise.Stirring 1 hour is obtained comprising chemical formula (5) institute
The aqueous solution of the 40 weight % of compound shown.
(preparation of the salt B of aminodithioformic acid)
Tetren (TOSOH Co., Ltd's system) 159g and pure water 331g are mixed, then, at 25 DEG C, nitrogen gas
While stirring respectively by 48 weight % sodium hydroxide 281g (Kishida Chemical Co., Ltd. system) and carbon disulfide in stream
230g (Kishida Chemical Co., Ltd. system) is divided into 4 parts and is alternately added dropwise.Stirring 1 hour is obtained comprising chemical formula
(6) aqueous solution of 40 weight % of compound represented.
(the salt C of aminodithioformic acid)
As the salt C of aminodithioformic acid, using in chemical formula (7) compound represented N, N- diethyl-dithio ammonia
Middle water is added and is formed 40 of base formic acid sodium trihydrate (FUJIFILM Wako Pure Chemical Corporation system)
Weight % aqueous solution.
(polyamines)
As polyamines, TOSOH Co., Ltd's ethylene-amines below, Nippon Shokubai Co., Ltd. are used
Polyethylene imine class processed.
Ethylene diamine (hereinafter referred to as EA (2)).
Diethylenetriamines (hereinafter referred to as EA (3)).
Trien (hereinafter referred to as EA (4)).
Tetren (hereinafter referred to as EA (5)).
Penten (hereinafter referred to as EA (6)).
Seven ethylidene, eight amine (hereinafter referred to as EA (8)).
The product (hereinafter referred to as PEI (300)) of the weight average molecular weight 300 of polyethylene imine.
The product (hereinafter referred to as PEI (1800)) of the weight average molecular weight 1800 of polyethylene imine.
(alkaline earth metal compound)
As alkaline earth metal compound, the compound below of Kishida Chemical Co., Ltd. is used.
Magnesium chloride, calcium chloride, calcium hydroxide, strontium chloride, barium nitrate, barium chlorate.
(inorganic flocculating agent)
As inorganic flocculating agent, aqueous solution below is used.
Kishida Chemical Co., Ltd. polyaluminium chloride 30g is added in water and forms the aqueous solution for amounting to 100g
(30 weight % poly aluminum chloride aqueous solution).
38 weight % ferric chloride aqueous solutions of Kishida Chemical Co., Ltd. system.
(high polymer coagulant)
As high polymer coagulant, use Organo Corporation OA-23 (weak anionic polymer).
Embodiment 1
Coagulation test mixing machine (Jar Tester) is set in 500mL beaker, addition comprising nickel ion 10mg/L and
The aqueous solution 500mL of EDTA 25mg/L.Then, the salt A 500mg/ of aminodithioformic acid is added while with 150rpm stirring
L, diethylenetriamines [EA (3)] 400mg/L, calcium chloride 1g/L, adjustment pH were 11, with 150rpm stirring 1 hour.Then, add
Enter 30 weight % polyaluminium chloride (hereinafter referred to as PAC) aqueous solution 1000mg/L, adjustment pH was 7, with 150rpm stirring 5 minutes.
The pH of aqueous solution is to be adjusted to be always at defined pH using micro hydrochloric acid and sodium hydroxide.10 points are stood after stirring
Clock is filtered aqueous solution with the filter paper of Advantech Co., Ltd. 5A, the nickel concentration of measurement treated aqueous solution.It will knot
Fruit is shown in table 1.
Embodiment 2~11
The reagent of addition is changed to reagent shown in table 1 and 2, in addition to this similarly to Example 1 after measurement processing
Aqueous solution nickel concentration.These results are shown in table 1 together and 2.
[table 1]
[table 2]
As shown in Examples 1 to 88, the nickel concentration of the processing rear solution of the waste water containing EDTA can be reduced to 0.8mg/L
Below.
Comparative example 1
Coagulation test mixing machine (Jar Tester) is set in 500mL beaker, addition comprising nickel ion 10mg/L and
The aqueous solution 500mL of EDTA 25mg/L.Then, adjustment pH was 11, with 150rpm stirring 1 hour.Then, 30 weight % are added
PAC aqueous solution 1000mg/L, adjustment pH were 7, with 150rpm stirring 5 minutes.The pH of aqueous solution is using micro hydrochloric acid and hydrogen
Sodium oxide molybdena is adjusted to be always at defined pH.10 minutes are stood after stirring, with Advantech Co., Ltd. 5A's
Filter paper filters aqueous solution, the nickel concentration of measurement treated aqueous solution.Show the result in table 3.
Comparative example 2~13
The reagent of addition is changed to reagent shown in table 3 and 4, in addition to this similarly to Example 1 after measurement processing
Aqueous solution nickel concentration.These results are shown in table 3 and 4 together.
Reference example 1
Coagulation test mixing machine (Jar Tester) is set in 500mL beaker, addition comprising nickel ion 10mg/L and
The aqueous solution 500mL of EDTA 25mg/L.Then, the salt A 500mg/ of aminodithioformic acid is added while with 150rpm stirring
L, penten 400mg/L, adjustment pH were 11, with 150rpm stirring 14 hours.Then, it is water-soluble that 30 weight %PAC are added
Liquid 1000mg/L, adjustment pH were 7, with 150rpm stirring 5 minutes.The pH of aqueous solution is using micro hydrochloric acid and sodium hydroxide tune
Whole is to be always at defined pH.10 minutes are stood after stirring, with the filter paper of Advantech Co., Ltd. 5A by water
Solution filtering, the nickel concentration of measurement treated aqueous solution.Show the result in table 4.
[table 3]
[table 4]
Comparative example 1 is that addition aluminium ion is neutralized, precipitates nickel ion in the form of hydroxide together with aluminium ion
Processing method example.The nickel concentration for aqueous solution that treated is 7.0mg/L, can not reduce nickel.
Comparative example 2 and 3 is the example that only addition calcium chloride is handled.The nickel concentration for aqueous solution that treated be 4.7~
5.3mg/L can not reduce nickel.
Comparative example 4~6 is the example for being only added to the salt of aminodithioformic acid.The nickel concentration for aqueous solution that treated is
4.9~5.5mg/L can not reduce nickel.
Comparative example 7 is the example for being only added to the salt A and sodium bisulfide of aminodithioformic acid.Aqueous solution that treated
Nickel concentration is 5.2mg/L, can not reduce nickel.
Comparative example 8 is the example for being added to the salt A and calcium chloride of aminodithioformic acid.The nickel for aqueous solution that treated is dense
Degree is 4.3mg/L, reduces nickel with being unable to fully.
Comparative example 9 is the example for being only added to polyamines.It is same before the nickel concentration for aqueous solution that treated and addition reagent
The 10mg/L of value can not reduce nickel.
Comparative example 10 is the example for being added to polyamines and calcium chloride.The nickel concentration of aqueous solution that treated and addition reagent it
The preceding 10mg/L for value, can not reduce nickel.
Comparative example 11 is the example for being added to the salt A and polyamines of aminodithioformic acid.The nickel for aqueous solution that treated is dense
Degree is 3.0mg/L, reduces nickel with being unable to fully.
Comparative example 12 is the example of the EA (2) and calcium chloride that are added to outside the salt A and the scope of the invention of aminodithioformic acid
Son, the nickel concentration for aqueous solution that treated do not find have improvement to imitate to the processing of nickel compared with the comparative example 8 that EA (2) is not added
Fruit.
Comparative example 13 is the PEI (1800) and calcium chloride being added to outside the salt A and the scope of the invention of aminodithioformic acid
Example, the nickel concentration of aqueous solution that treated is 3.5mg/L, reduces nickel with being unable to fully.
Reference example 1 is that the mixing time as reagent additive amount identical with comparative example 11 and after adding reagent on is small by 1
14 hours examples of Shi Bianwei.The nickel concentration for aqueous solution that treated is almost same value with the embodiment 4 for being added to calcium chloride, but
It needs to reduce nickel concentration for a long time.
Embodiment 12~16, comparative example 14
The reagent of addition is changed to reagent shown in table 5, in addition to this measurement treated water similarly to Example 1
The nickel concentration of solution.These results are shown in table 5 together.
[table 5]
Embodiment 12~16 is the example for changing the parts by weight of polyamines within the scope of the invention and handling.Independent of
The concentration of nickel can be reduced to 1.6mg/L or less by the parts by weight of polyamines.
Comparative example 14 be added to aminodithioformic acid salt A and lower than the scope of the present invention amount polyamines example
The nickel concentration of son, aqueous solution that treated is 4.1mg/L, can not reduce nickel.
Embodiment 17~21
The reagent of addition is changed to reagent shown in table 6, in addition to this measurement treated water similarly to Example 1
The nickel concentration of solution.These results are shown in table 6 together.
[table 6]
Embodiment 17~21 is the example for changing the type of alkaline-earth metal within the scope of the invention and handling.It does not depend on
In the type of alkaline-earth metal, the concentration of nickel can be reduced to 1.0mg/L or less.
Embodiment 22~25, comparative example 15
The reagent of addition is changed to reagent shown in table 7, in addition to this measurement treated water similarly to Example 1
The nickel concentration of solution.These results are shown in table 7 together.
[table 7]
Embodiment 22~25 is the example for changing the additive amount of the calcium chloride as alkaline-earth metal and handling.Pass through addition
The calcium chloride of 0.01g/L or more, so as to which the concentration of nickel is reduced to 0.2mg/L or less.
Comparative example 15 is the example for handling the additive amount of the calcium chloride as alkaline-earth metal with 0.001g/L.Such as than
Compared with shown in example 15, it is known that when the amount for the alkaline-earth metal being applied in combination with the salt and polyamines of aminodithioformic acid is few, the reduction of nickel
Effect is low.
Embodiment 26~27
The reagent of addition is changed to reagent shown in table 8, in addition to this measurement treated water similarly to Example 1
The nickel concentration of solution.These results are shown in table 8 together.
[table 8]
Embodiment 26 and 27 is the example for changing the additive amount of inorganic sulphide and handling.The concentration of nickel can be dropped
Down to 1.2mg/L or less.
Embodiment 28
Coagulation test mixing machine (Jar Tester) is set in 500mL beaker, addition comprising nickel ion 10mg/L and
The aqueous solution 500mL of EDTA 25mg/L.Then, the salt A 500mg/ of aminodithioformic acid is added while with 150rpm stirring
L, diethylenetriamines [EA (3)] 400mg/L, calcium chloride 1g/L, adjustment pH were 11, with 150rpm stirring 1 hour.Then, add
Enter 30 weight %PAC aqueous solution 1000mg/L, adjustment pH was 7, with 150rpm stirring 5 minutes.Then, as high polymer coagulant
0.1 weight %OA-23 aqueous solution 2000mg/L is added, adjustment pH was 7, with 50rpm stirring 5 minutes.The pH of aqueous solution be using
Micro hydrochloric acid and sodium hydroxide is adjusted to be always at defined pH.10 minutes are stood after stirring, uses Advantech
The filter paper of Co., Ltd. 5A filters aqueous solution, the nickel concentration of measurement treated aqueous solution.Show the result in table 9.
Embodiment 29
30 weight %PAC aqueous solutions are changed to 38 weight % ferric chloride in aqueous solution, in addition to this similarly to Example 28
The nickel concentration of ground measurement treated aqueous solution.The results are shown in tables 9.
[table 9]
Embodiment 28 is to add the example of high polymer coagulant in embodiment 1.The nickel concentration for aqueous solution that treated with
The case where being not added with high polymer coagulant is with value, and the processing of nickel is sufficient.
Embodiment 29 is the example that ferric chloride aqueous solutions are used as inorganic flocculating agent.The nickel for aqueous solution that treated is dense
Degree is 0.2mg/L, and independent of the type of inorganic flocculating agent, the processing of nickel is sufficient.
Industrial availability
The purification method of nickeliferous aqueous solution according to the present invention, even more difficult the containing of the processing of nickel has and nickel is complexed
The compound of ability and the aqueous solution of nickel also can reduce nickel concentration, therefore the purification side as novel nickeliferous aqueous solution
Method has the processing for the nickel-containing waste water from plating factory, electronic component/mechanical part manufacturing works, automobile plant etc.
A possibility that.
Claims (12)
1. a kind of nickeliferous aqueous solution cleanser, which is characterized in that its 100 parts by weight of salt relative to aminodithioformic acid,
Comprising having 20 parts by weight of polyamines of 3~8 nitrogen-atoms or more and alkaline earth metal compound to form.
2. a kind of nickeliferous aqueous solution cleanser, which is characterized in that its 100 parts by weight of salt relative to aminodithioformic acid,
Comprising having 20 parts by weight of polyamines of 3~8 nitrogen-atoms or more, alkaline earth metal compound and inorganic sulphide to form.
3. nickeliferous aqueous solution cleanser according to claim 2, which is characterized in that inorganic sulphide is sodium bisulfide.
4. nickeliferous aqueous solution cleanser according to claim 1 or 2, which is characterized in that the salt of aminodithioformic acid
It is aminated compounds and carbon disulfide and alkali at least one amino in the group being made of primary amino group and secondary amino group
The reaction product of metal hydroxides.
5. nickeliferous aqueous solution cleanser according to claim 1 or 2, which is characterized in that the salt of aminodithioformic acid
It is aminated compounds and carbon disulfide and alkali gold with 2 or more the amino in the group being made of primary amino group and secondary amino group
Belong to the reaction product of hydroxide.
6. nickeliferous aqueous solution cleanser according to claim 1 or 2, which is characterized in that the salt of aminodithioformic acid
It is the reaction product of piperazine or tetren and carbon disulfide and alkali metal hydroxide.
7. a kind of purification method of nickeliferous aqueous solution, which is characterized in that in nickeliferous aqueous solution, add in claim 1~6 and appoint
Nickeliferous aqueous solution cleanser, then removes the solid content of generation described in one.
8. the purification method of nickeliferous aqueous solution according to claim 7, which is characterized in that nickeliferous aqueous solution further includes
Compound with the ability being complexed with nickel.
9. the purification method of nickeliferous aqueous solution according to claim 8, which is characterized in that have the ability being complexed with nickel
Compound is the compound in the molecule with the functional group in the group for selecting free carboxyl group and amino to form.
10. the purification method of nickeliferous aqueous solution according to any one of claim 7~9, which is characterized in that solid in removal
Before shape object, inorganic flocculating agent is added.
11. the purification method of nickeliferous aqueous solution according to any one of claim 7~9, which is characterized in that solid in removal
Before shape object, inorganic flocculating agent and high polymer coagulant are added.
12. the purification method of nickeliferous aqueous solution described in 0 or 11 according to claim 1, which is characterized in that inorganic flocculating agent is choosing
Substance in the group of free iron compound and aluminium compound composition.
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