CN114477285A - Method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and ammonium chromium polyvanadate prepared by method - Google Patents
Method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and ammonium chromium polyvanadate prepared by method Download PDFInfo
- Publication number
- CN114477285A CN114477285A CN202111547122.9A CN202111547122A CN114477285A CN 114477285 A CN114477285 A CN 114477285A CN 202111547122 A CN202111547122 A CN 202111547122A CN 114477285 A CN114477285 A CN 114477285A
- Authority
- CN
- China
- Prior art keywords
- vanadium
- ammonium
- polyvanadate
- chromium
- sodium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 99
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 50
- PYKNDCILXQWMJP-UHFFFAOYSA-N azane;chromium(3+) Chemical compound N.[Cr+3] PYKNDCILXQWMJP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 230000001603 reducing effect Effects 0.000 title claims abstract description 16
- 230000002378 acidificating effect Effects 0.000 title abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 49
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 30
- 239000011651 chromium Substances 0.000 claims abstract description 24
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 24
- CFVBFMMHFBHNPZ-UHFFFAOYSA-N [Na].[V] Chemical compound [Na].[V] CFVBFMMHFBHNPZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 20
- 239000010703 silicon Substances 0.000 claims abstract description 18
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 12
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000012065 filter cake Substances 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 238000002386 leaching Methods 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 8
- 239000002893 slag Substances 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 6
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 6
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 6
- 239000011593 sulfur Substances 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 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 claims description 5
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 5
- 235000010265 sodium sulphite Nutrition 0.000 claims description 5
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical group [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 claims description 5
- 229910000352 vanadyl sulfate Inorganic materials 0.000 claims description 5
- 229940041260 vanadyl sulfate Drugs 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical group O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 4
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 4
- 150000002484 inorganic compounds Chemical class 0.000 claims description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 229910021551 Vanadium(III) chloride Inorganic materials 0.000 claims description 2
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 claims description 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical class [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 2
- LOUBVQKDBZRZNQ-UHFFFAOYSA-M [O-2].[O-2].[OH-].O.[V+5] Chemical compound [O-2].[O-2].[OH-].O.[V+5] LOUBVQKDBZRZNQ-UHFFFAOYSA-M 0.000 claims description 2
- QUEDYRXQWSDKKG-UHFFFAOYSA-M [O-2].[O-2].[V+5].[OH-] Chemical compound [O-2].[O-2].[V+5].[OH-] QUEDYRXQWSDKKG-UHFFFAOYSA-M 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 2
- 238000001311 chemical methods and process Methods 0.000 claims description 2
- DYRBFMPPJATHRF-UHFFFAOYSA-N chromium silicon Chemical compound [Si].[Cr] DYRBFMPPJATHRF-UHFFFAOYSA-N 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 229910010272 inorganic material Inorganic materials 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000013067 intermediate product Substances 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 2
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- OGUCKKLSDGRKSH-UHFFFAOYSA-N oxalic acid oxovanadium Chemical compound [V].[O].C(C(=O)O)(=O)O OGUCKKLSDGRKSH-UHFFFAOYSA-N 0.000 claims description 2
- 159000000001 potassium salts Chemical class 0.000 claims description 2
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 claims description 2
- 229940001482 sodium sulfite Drugs 0.000 claims description 2
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 2
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 claims description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 2
- VLOPEOIIELCUML-UHFFFAOYSA-L vanadium(2+);sulfate Chemical compound [V+2].[O-]S([O-])(=O)=O VLOPEOIIELCUML-UHFFFAOYSA-L 0.000 claims description 2
- HQYCOEXWFMFWLR-UHFFFAOYSA-K vanadium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[V+3] HQYCOEXWFMFWLR-UHFFFAOYSA-K 0.000 claims description 2
- 125000005287 vanadyl group Chemical group 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 235000010323 ascorbic acid Nutrition 0.000 claims 1
- 239000011668 ascorbic acid Substances 0.000 claims 1
- 229960005070 ascorbic acid Drugs 0.000 claims 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims 1
- 235000019838 diammonium phosphate Nutrition 0.000 claims 1
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 16
- 238000005406 washing Methods 0.000 abstract description 6
- 238000004537 pulping Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 38
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- VWBLQUSTSLXQON-UHFFFAOYSA-N N.[V+5] Chemical compound N.[V+5] VWBLQUSTSLXQON-UHFFFAOYSA-N 0.000 description 5
- 238000003916 acid precipitation Methods 0.000 description 5
- 229910001430 chromium ion Inorganic materials 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 5
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- -1 hydrogen ions Chemical class 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 229910003206 NH4VO3 Inorganic materials 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- XFBNFDUGOXFZMO-UHFFFAOYSA-N O.[O--].[O--].[O--].[O--].[O--].[V+5].[V+5] Chemical compound O.[O--].[O--].[O--].[O--].[O--].[V+5].[V+5] XFBNFDUGOXFZMO-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- DNWNZRZGKVWORZ-UHFFFAOYSA-N calcium oxido(dioxo)vanadium Chemical compound [Ca+2].[O-][V](=O)=O.[O-][V](=O)=O DNWNZRZGKVWORZ-UHFFFAOYSA-N 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- ALTWGIIQPLQAAM-UHFFFAOYSA-N metavanadate Chemical compound [O-][V](=O)=O ALTWGIIQPLQAAM-UHFFFAOYSA-N 0.000 description 1
- 239000006012 monoammonium phosphate Substances 0.000 description 1
- GEVPUGOOGXGPIO-UHFFFAOYSA-N oxalic acid;dihydrate Chemical compound O.O.OC(=O)C(O)=O GEVPUGOOGXGPIO-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical group [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- UPDATVKGFTVGQJ-UHFFFAOYSA-N sodium;azane Chemical group N.[Na+] UPDATVKGFTVGQJ-UHFFFAOYSA-N 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 150000003681 vanadium Chemical class 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/006—Compounds containing, besides chromium, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention relates to the field of vanadium chemical industry, in particular to a method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and ammonium chromium polyvanadate prepared by the method. The method comprises the following steps: leaching a vanadium raw material containing silicon and chromium with deionized water or alkali to obtain a sodium vanadium solution; adding acid into the sodium vanadium solution, adjusting the pH value to be neutral, adding a reducing agent, adding acid to adjust the pH value to be 2-3, adding ammonium salt, reacting at the temperature of 75-100 ℃ for 0.5-3h, filtering to obtain a vanadium precipitation filter cake after the reaction is finished, pulping and washing the filter cake with deionized water, and drying. According to the method for preparing the ammonium chromium polyvanadate by reducing the acidic precipitated vanadium, the sodium vanadium solution can be subjected to deep desiliconization to prepare the ammonium chromium polyvanadate, the silicon content in the ammonium chromium polyvanadate is as low as below 20ppm, and the ammonium chromium polyvanadate is an excellent raw material for preparing high-purity vanadium pentoxide.
Description
Technical Field
The invention relates to the field of vanadium chemical industry, in particular to a method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and ammonium chromium polyvanadate prepared by the method.
Background
The sodium vanadium solution is one of main vanadium raw materials for industrially preparing vanadium pentoxide, is a vanadium-containing solution obtained by carrying out sodium roasting-water leaching on vanadium slag obtained from vanadium titano-magnetite through a blast furnace iron-making-converter vanadium extraction process, and is mainly characterized by containing a large amount of alkali metal ions K, Na, Si and Cr, and the content range is approximately as follows: k-0.4-0.5 g/L, Na-20-50 g/L, Si-1.0-3.0 g/L, Cr-1.5-5.0 g/L, TV-30-80 g/L. The vanadium precipitation process for preparing vanadium pentoxide by taking sodium vanadium solution as a raw material and five vanadium precipitation products are respectively as follows:
the first method comprises the following steps: strongly acidic hydrolysis to precipitate vanadium-vanadium pentoxide hydrate (containing part of sodium vanadate hetero-phase). The vanadate is converted into hydrated V under the condition of pH less than or equal to 1 and boiling2O5Of hydration V2O5The hydrogen ions are partially replaced by sodium ions to form sodium vanadate impurities.
And the second method comprises the following steps: hydrolyzing to precipitate vanadium-red cake. The pH value is 1.5-3, the temperature is above 90 ℃, and the vanadium concentration is more than 5g/L, so that the prepared vanadium precipitation product is sodium hexametaphosphate with a molecular formula of Na2H2V6O17Or Na2O·3V2O5·H2O is commonly called red cake because of its red color.
And the third is that: precipitating vanadium-APV by acidic ammonium salt. pH of 2-3, temperature of 75-100 ℃, ammonium addition coefficient of 0.45-0.65, in terms of m (NH)3): m (V), the vanadium concentration is not required, and the prepared vanadium precipitation product is ammonium hexavanadate with the molecular formula of (NH)4)2V6O16Or 2NH3·3V2O5·H2O, commonly known as APV.
And fourthly: and precipitating vanadium-SAV by weak acid ammonium salt. pH of 4-6, temperature of normal temperature, ammonium addition coefficient of 0.3-0.4, in terms of m (NH)3): in m (V), the vanadium concentration is not too low, but the silicon content is not too high, and the prepared vanadium precipitation product is sodium ammonium decavanadate, and the molecular formula is (NH)4)6-xNaxV10O28Commonly known as SAV.
And a fifth mode: precipitating vanadium-AMV by using alkaline ammonium salt. pH of 8-9, normal temperature, ammonium addition coefficient of 0.65-1.0, in terms of m (NH)3)：m (V), the vanadium concentration is not too low, the prepared vanadium precipitation product is ammonium metavanadate, and the molecular formula is NH4VO3Commonly known as AMV.
The hydrolysis vanadium precipitation method has the advantages of short flow, simple operation, low requirement on vanadium concentration, and large fluctuation of vanadium concentration, but has the disadvantages of large acid consumption and low vanadium content in the product; the vanadium precipitation products of alkaline ammonium salt and weakly acidic ammonium salt have high purity and low acid consumption, but the vanadium concentration in the solution cannot be too low, and silicon needs to be removed, so the production cost is high; the acid ammonium salt vanadium precipitation has the advantages of hydrolysis vanadium precipitation and other ammonium salt vanadium precipitation, the process flow is simple, the production period is short, the acid consumption is low, the ammonium salt is smaller than other ammonium salt precipitation methods, the continuous industrial production is facilitated, and the product quality is higher than that of hydrolysis vanadium precipitation products.
In addition, a calcium vanadate precipitation method and an iron vanadate precipitation method are adopted, and calcium salt and iron salt are added into vanadium leachate by controlling a certain pH condition, so that vanadate is separated out in the form of vanadate or metavanadate. However, the precipitate obtained by the method can not be directly calcined to obtain vanadium pentoxide, and the technical steps of re-dissolving the precipitate and the like are also needed, so that the industrial application is very few at present.
In conclusion, although the acidic ammonium salt vanadium precipitation has many advantages, the method is only suitable for the production of metallurgical-grade vanadium pentoxide, and the silicon content in the vanadium precipitation product APV exceeds the standard due to the advantages, so that the development of high-purity vanadium pentoxide and the application field and range of the vanadium product are limited.
Disclosure of Invention
The invention aims to provide a method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and the ammonium chromium polyvanadate prepared by the method, and the method can carry out deep desilication on sodium vanadium solution containing Si and Cr so as to prepare the ammonium chromium polyvanadate with extremely low silicon content (below 20 ppm).
In order to achieve the above object, the present invention provides a method for preparing ammonium chromium polyvanadate by reducing acid precipitation vanadium, comprising the steps of:
(1) leaching a vanadium raw material containing silicon and chromium with deionized water or alkali to obtain a sodium vanadium solution;
(2) adding acid into the sodium vanadium solution, adjusting the pH value to be neutral, adding a reducing agent, adding acid to adjust the pH value to be 2-3, adding ammonium salt, and reacting, wherein the stoichiometric ratio of the reducing agent to Cr in the sodium vanadium solution is 1.2-6 according to m (NH)3): and m (V) the calculated ammonium addition coefficient is 0.45-0.65, the reaction temperature is 75-100 ℃, the reaction time is 0.5-3h, after the reaction is finished, filtering is carried out to obtain a vanadium precipitation filter cake, the filter cake is pulped and washed by deionized water, and then drying is carried out.
The invention also provides the ammonium chromium polyvanadate prepared by the method.
The invention innovatively provides a method for reducing-acid ammonium salt vanadium precipitation, which is mainly characterized in that a reducing agent is added in the acid ammonium salt vanadium precipitation process, hexavalent chromium ions are reduced into trivalent chromium ions and participate in vanadium precipitation reaction, and the obtained precipitation product is a loose and porous amorphous product and contains a large amount of trivalent chromium ions and ammonium ions, so that in the process of reducing the hexavalent chromium ions, anion functional groups are converted into cations to form a chromium ammonium polyvanadate precipitate, and the molecular formula of the chromium ammonium polyvanadate precipitate can be approximately regarded as (NH)4)2-xCrx/3V6O16. In addition, the silicon content in the conventional APV is 0.02-0.1%, the Cr content is 0.01-0.05%, the silicon content in the ammonium chromium polyvanadate prepared by the method is less than 0.002%, the Cr content is 0.5-5.0%, and the ammonium chromium polyvanadate can not be removed by simple washing, so that hexavalent chromium is reduced into trivalent chromium which actually participates in vanadium precipitation reaction, a part of chromium vanadate is formed, and meanwhile, trivalent chromium ions lose the coordination capacity with silicon, so that the silicon content in the ammonium chromium polyvanadate is lower, and the chromium content is higher than that of the conventional APV. Therefore, the reduction-acid vanadium precipitation changes the appearance, crystal form and chemical components of the precipitation product, and is a brand new vanadium precipitation product.
Compared with the prior art, the invention has the following advantages:
(1) the prepared ammonium chromium polyvanadate is different from a common vanadium precipitation product, is a flocculent amorphous precipitation product, and has extremely low silicon content which is below 20ppm in the precipitation product.
(2) The obtained ammonium chromium polyvanadate is an excellent raw material for preparing high-purity vanadium pentoxide, the high-purity vanadium pentoxide can be prepared more easily by adopting a re-dissolution method, and the preparation cost of the high-purity vanadium pentoxide can be reduced.
(3) The method has the advantages of simple and easy process, low equipment requirement and convenient operation, and is very suitable for industrial production.
Drawings
FIG. 1 is an XRD pattern of chromium ammonium polyvanadate prepared according to example 1 of the present invention;
FIG. 2 is an XRD pattern of a conventional APV prepared in accordance with comparative example 1;
FIG. 3 is an SEM photograph of ammonium chromium polyvanadate prepared according to example 1 of the present invention;
FIG. 4 is an SEM image of a conventional APV prepared according to comparative example 1;
FIG. 5 is a graph showing EDS spectrum analysis of ammonium chromium polyvanadate prepared in example 1 according to the present invention.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The method for preparing the ammonium chromium polyvanadate by reducing the acid vanadium precipitation comprises the following steps:
(1) leaching a vanadium raw material containing silicon and chromium with deionized water or alkali to obtain a sodium vanadium solution;
(2) adding acid into the sodium vanadium solution, adjusting the pH value to be neutral, adding a reducing agent, adding acid to adjust the pH value to be 2-3, adding ammonium salt, and reacting, wherein the reducing agent and the sodium areThe stoichiometric ratio of Cr in the vanadium solution is 1.2-6 according to m (NH)3): and m (V) the calculated ammonium addition coefficient is 0.45-0.65, the reaction temperature is 75-100 ℃, the reaction time is 0.5-3h, after the reaction is finished, filtering is carried out to obtain a vanadium precipitation filter cake, the filter cake is pulped and washed by deionized water, and then drying is carried out.
In step (1), the silicon-and chromium-containing vanadium raw material may be selected from at least one of the following raw materials: vanadium slag generated in the vanadium titano-magnetite smelting process, sodium-modified roasting clinker, Ammonium Polyvanadate (APV), Ammonium Metavanadate (AMV), ammonium polyvanadate Sodium (SAV), hydrolyzed red cake or other crude vanadium oxides generated in the vanadium chemical process, and vanadium slag or intermediate products containing silicon and chromium generated in the vanadium extraction process of other vanadium-containing minerals.
In step (2), the acid added may be sulfuric acid.
In the step (2), the reducing agent may be at least one of a vanadium-containing reducing agent, a sulfur-containing reducing agent, and an organic reducing agent. Specifically, the vanadium-containing reducing agent can be selected from vanadyl sulfate, vanadium sulfate, vanadyl dioxide, vanadium trichloride, vanadyl oxalate, vanadium dioxide, vanadium tetraoxide, vanadium trioxide and other inorganic or organic compounds containing trivalent vanadium and tetravalent vanadium. The sulfur-containing reducing agent may be selected from sulfur dioxide, sulfurous acid, sodium sulfite, sodium metabisulfite, sodium thiosulfate, hydrogen sulfide, sodium hydrosulfide and the same forms of potassium salts, ammonium salts or other compounds containing lower sulfur. The organic reducing agent can be selected from vitamin C, oxalic acid, formic acid, tartaric acid, citric acid and other organic matters with reducibility. Preferably, the reducing agent is at least one of vanadyl sulfate, sodium metabisulfite and sodium sulfite.
In step (2), the ammonium salt may be selected from one or more of ammonium sulfate, ammonium chloride, ammonium carbonate, ammonium sulfide, aqueous ammonia, monoammonium phosphate, and other ammonium group-containing inorganic compounds, and preferably ammonium sulfate.
In the step (2), the stoichiometric ratio of the reducing agent to Cr in the sodium vanadium solution is 1.2-6, such as 1.2, 3.0, 4.5, 6.0 and the like. When the dosage of the reducing agent is less than 1.2, the hexavalent chromium is not completely reduced; at levels above 6.0, non-tetravalent vanadium salt reducing agents, if used, can cause excessive reduction and loss of vanadium.
In step (2), according to m (NH)3): m (V), the coefficient of adding ammonium is 0.45-0.65, such as 0.45, 0.5, 0.55, 0.65, etc. The vanadium precipitation rate is low when the ammonium addition coefficient is low, the ammonium salt loss is high when the ammonium addition coefficient is high, and the cost is high. In the present invention, "coefficient of addition of ammonium" means NH added to ammonium salt3And the mass ratio of V in the sodium vanadium solution.
In step (2), the pH is adjusted to 2-3, such as 2, 2.3, 2.6, 3, after adding the reducing agent.
In the step (2), the reaction process after adding the ammonium salt is a vanadium precipitation process. The vanadium precipitation temperature is 75-100 deg.C, such as 75 deg.C, 85 deg.C, 95 deg.C, 100 deg.C, etc. When the vanadium precipitation temperature is low, the precipitation of APV is not facilitated, and the vanadium precipitation rate is low. The vanadium precipitation time is 0.5-3h, such as 0.5h, 1h, 2h, 3h and the like.
The invention also provides the ammonium chromium polyvanadate prepared by the method. The ammonium chromium polyvanadate has a loose porous amorphous structure, wherein the content of Cr is significantly higher than that of ordinary Ammonium Polyvanadate (APV), and the content of Cr in the ammonium chromium polyvanadate can usually reach 2-4% by mass, such as 2.45%, 2.59%, 3.22%, and 3.42%; furthermore, since deep desiliconization can be realized in the present invention, the Si content therein can be as low as 20ppm or less.
The present invention will be described in detail below by way of examples.
The sodium vanadium solution used in the following examples and comparative examples is a vanadium leaching solution obtained by sodium roasting vanadium slag generated in a vanadium titano-magnetite smelting process and then leaching the vanadium slag with deionized water, wherein Si is 1.18g/L, Cr is 2.15g/L, and TV is 43.22 g/L.
In the following examples and comparative examples, the contents of vanadium, chromium and silicon in the ammonium chromium polyvanadate were measured by inductively coupled plasma mass spectrometry (ICP-MS).
Example 1
This example illustrates the preparation of ammonium chromium polyvanadate by reducing acid precipitation of vanadium according to the present invention.
Weighing 500ml of sodium vanadium solution, firstly dropwise adding sulfuric acid to adjust the pH value to be neutral, adding 4.7g of sodium metabisulfite, then dropwise adding sulfuric acid to adjust the pH value to be 2.0, then adding 30.6g of ammonium chloride, and stirring and reacting for 0.5h at 100 ℃. After the reaction is finished, filtering to obtain a vanadium precipitation product, pulping and washing the vanadium precipitation product twice by using deionized water, filtering and drying to obtain 43.2g of a target product of ammonium chromium polyvanadate, wherein the target product contains Cr-2.45%, Si less than 0.002% and V-47.04% through chemical detection. The XRD spectrum, SEM analysis diagram and EDS energy spectrum analysis diagram of the ammonium chromium polyvanadate target product are respectively shown in figure 1, figure 3 and figure 5.
Comparative example 1
The procedure of example 1 was followed except that sodium metabisulfite, the reducing agent, was not added to produce a conventional APV product containing Cr-0.042%, Si-0.046% and V-47.73% as determined by chemical methods. The XRD pattern and SEM analysis pattern of the common APV product are shown in fig. 2 and 4, respectively.
Comparing an XRD (X-ray diffraction) spectrum and an SEM (scanning Electron microscope) analysis chart of the ammonium chromium polyvanadate with those of a common APV (amorphous positive pressure vacuum), the ammonium chromium polyvanadate is a loose and porous amorphous product, and the result of EDS (electron-dispersive spectroscopy) analysis is consistent with that of chemical detection, so that the ammonium chromium polyvanadate contains a large amount of Cr; while the common APV is the layered crystal ammonium hexavanadate with the molecular formula of (NH)4)2V6O16The Cr content is significantly less. Therefore, the structure, the appearance and the components of the original APV are completely changed by adding the reducing agent in the vanadium precipitation process.
Example 2
This example illustrates the preparation of ammonium chromium polyvanadate by reducing acid precipitation of vanadium according to the present invention.
Weighing 500ml of sodium vanadium solution, firstly dropwise adding sulfuric acid to adjust the pH value to be neutral, adding 11.7g of sodium sulfite, then dropwise adding sulfuric acid to adjust the pH value to be 2.3, then adding 43.22g of ammonium sulfate, and stirring and reacting for 1h at 90 ℃. After the reaction is finished, filtering to obtain a vanadium precipitation product, pulping and washing the vanadium precipitation product twice by using deionized water, filtering and drying to obtain 41.5g of a target product of ammonium chromium polyvanadate, wherein the target product contains Cr-3.22%, Si less than 0.002% and V-47.40% by chemical detection.
Example 3
This example illustrates the preparation of ammonium chromium polyvanadate by reducing acid precipitation of vanadium according to the present invention.
Weighing 500ml of sodium vanadium solution, firstly dropwise adding sulfuric acid to adjust the pH value to be neutral, adding 98ml of vanadyl sulfate solution with the concentration of 2.85mol/L, then dropwise adding sulfuric acid to adjust the pH value to be 2.6, then adding 31.33g of ammonium carbonate, and stirring and reacting for 2 hours at 85 ℃. After the reaction is finished, filtering to obtain a vanadium precipitation product, pulping and washing the vanadium precipitation product twice by using deionized water, filtering and drying to obtain 42.6g of a target product of ammonium chromium polyvanadate, wherein the target product contains Cr-2.59%, Si less than 0.002% and V-47.82% through chemical detection.
Example 4
This example illustrates the preparation of ammonium chromium polyvanadate by reducing acid precipitation of vanadium according to the present invention.
Weighing 500ml of sodium vanadium solution, firstly dropwise adding sulfuric acid to adjust the pH value to be neutral, adding 23.5g of oxalic acid dihydrate, then dropwise adding sulfuric acid to adjust the pH value to be 3.0, then adding 66.9g of ammonium bicarbonate, and stirring and reacting for 3 hours at 75 ℃. After the reaction is finished, filtering to obtain a vanadium precipitation product, pulping and washing the vanadium precipitation product twice by using deionized water, filtering and drying to obtain 41.8g of a target product of ammonium chromium polyvanadate, wherein the target product contains Cr-3.42%, Si less than 0.002% and V-47.44% through chemical detection.
It can be seen from the above examples and comparative examples that the method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium according to the present invention can realize deep desiliconization of the sodium vanadium solution to obtain ammonium chromium polyvanadate, and the content of silicon in the ammonium chromium polyvanadate is as low as 20ppm or less, which is an excellent raw material for preparing high purity vanadium pentoxide.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for preparing ammonium chromium polyvanadate by reducing acid precipitated vanadium is characterized by comprising the following steps:
(1) leaching a vanadium raw material containing silicon and chromium with deionized water or alkali to obtain a sodium vanadium solution;
(2) adding acid into the sodium vanadium solution, adjusting the pH value to be neutral, adding a reducing agent, adding acid to adjust the pH value to be 2-3, adding ammonium salt, and reacting, wherein the stoichiometric ratio of the reducing agent to Cr in the sodium vanadium solution is 1.2-6 according to m (NH)3): and m (V) the calculated ammonium addition coefficient is 0.45-0.65, the reaction temperature is 75-100 ℃, the reaction time is 0.5-3h, after the reaction is finished, filtering is carried out to obtain a vanadium precipitation filter cake, the filter cake is pulped and washed by deionized water, and then drying is carried out.
2. The method according to claim 1, wherein in step (1), the silicon-and chromium-containing vanadium raw material is selected from at least one of the following raw materials: vanadium slag generated in the vanadium titano-magnetite smelting process, sodium-modified roasting clinker, ammonium polyvanadate, ammonium metavanadate, ammonium polyvanadate sodium, hydrolytic red cake or other crude vanadium oxides generated in the vanadium chemical process, and vanadium slag or intermediate products containing silicon and chromium generated in the vanadium extraction process of other vanadium-containing minerals.
3. The method according to claim 1, wherein in step (2), the acid added for adjusting the pH is sulfuric acid.
4. The method according to claim 1, wherein in step (2), the reducing agent is at least one of a vanadium-containing reducing agent, a sulfur-containing reducing agent, and an organic reducing agent.
5. The method of claim 4, wherein the vanadium-containing reducing agent is selected from vanadyl sulfate, vanadium sulfate, vanadyl dioxide, vanadium trichloride, vanadyl oxalate, vanadium dioxide, vanadium tetraoxide, vanadium trioxide, and other inorganic or organic compounds containing trivalent vanadium, tetravalent vanadium.
6. The method of claim 4, wherein the sulfur-containing reducing agent is selected from sulfur dioxide, sulfurous acid, sodium sulfite, sodium metabisulfite, sodium thiosulfate, hydrogen sulfide, sodium hydrosulfide, and potassium salts, ammonium salts or other compounds containing lower sulfur in the same form.
7. The method as claimed in claim 4, wherein the organic reducing agent is selected from the group consisting of ascorbic acid, oxalic acid, formic acid, tartaric acid, citric acid and other organic substances having reducing properties.
8. The method of claim 4, wherein the reducing agent is at least one of vanadyl sulfate, sodium metabisulfite, and sodium sulfite.
9. The method according to claim 1, wherein the ammonium salt is selected from one or more of ammonium sulfate, ammonium chloride, ammonium carbonate, ammonium sulfide, aqueous ammonia, ammonium monohydrogen phosphate, ammonium dihydrogen phosphate, and other inorganic compounds containing ammonium groups.
10. Ammonium chromium polyvanadate prepared by the method of any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111547122.9A CN114477285B (en) | 2021-12-16 | 2021-12-16 | Method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and ammonium chromium polyvanadate prepared by same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111547122.9A CN114477285B (en) | 2021-12-16 | 2021-12-16 | Method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and ammonium chromium polyvanadate prepared by same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114477285A true CN114477285A (en) | 2022-05-13 |
| CN114477285B CN114477285B (en) | 2024-03-26 |
Family
ID=81493278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111547122.9A Active CN114477285B (en) | 2021-12-16 | 2021-12-16 | Method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and ammonium chromium polyvanadate prepared by same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114477285B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015161660A1 (en) * | 2014-04-21 | 2015-10-29 | 中国科学院过程工程研究所 | Method for preparing low-silicon vanadium pentoxide from solution containing vanadium, chromium and silicon |
| CN106006732A (en) * | 2016-08-05 | 2016-10-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing ammonium polyvanadate from high concentration vanadium liquid |
| CN106629846A (en) * | 2016-11-18 | 2017-05-10 | 河钢股份有限公司承德分公司 | Method for preparing ammonium polyvanadate from sodiumizing, roasting and leaching solution |
-
2021
- 2021-12-16 CN CN202111547122.9A patent/CN114477285B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015161660A1 (en) * | 2014-04-21 | 2015-10-29 | 中国科学院过程工程研究所 | Method for preparing low-silicon vanadium pentoxide from solution containing vanadium, chromium and silicon |
| CN106006732A (en) * | 2016-08-05 | 2016-10-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing ammonium polyvanadate from high concentration vanadium liquid |
| CN106629846A (en) * | 2016-11-18 | 2017-05-10 | 河钢股份有限公司承德分公司 | Method for preparing ammonium polyvanadate from sodiumizing, roasting and leaching solution |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114477285B (en) | 2024-03-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100357361C (en) | Method for preparing high purity iron oxide yellow and iron oxide red using titanium dioxide byproduct ferrous sulfate | |
| CN102121068B (en) | Method for preparing vanadium pentoxide | |
| CN101182037B (en) | Method for reclaiming vanadium oxide from dephosphorization underflow slag | |
| CN105567964B (en) | Method for selectively reducing, separating and recycling vanadium and chrome from solution containing vanadium and chrome | |
| CN106745248B (en) | High-purity sulphuric acid vanadyl solution manufacturing method | |
| CN106987732B (en) | A method of separation and recovery vanadium chromium | |
| CN109055724B (en) | Method for extracting vanadium and chromium from chrome vanadium ore/slag | |
| CN107954474A (en) | A kind of method that vanadium product and chromium sulfate basic are produced using vanadium chromium solution | |
| CN109437299A (en) | Purification method of industrial-grade ammonium metavanadate | |
| CN114275815B (en) | Method for preparing high-purity vanadium pentoxide by reducing and precipitating sodium vanadium liquid | |
| CN108754186A (en) | The method for preparing vfanadium compound containing vanadium solution | |
| KR100406392B1 (en) | The neutralization process of waste sulphuric acid with by product from iron and steel works and the method of manufacturing gypsum with precipitate made the neutralization process | |
| CN110902728B (en) | Refining method of electronic-grade ferrous sulfate solution and electronic-grade ferrous sulfate | |
| CN104891576B (en) | A kind of preparation method of Manganous sulfate monohydrate | |
| CN102153136B (en) | Preparation method of hydrated titanium dioxide double-effect seed crystal | |
| CN104609472A (en) | Method for producing vanadium pentoxide from titanium tetrachloride refinement vanadium-removal slurry | |
| CN114477285B (en) | Method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and ammonium chromium polyvanadate prepared by same | |
| CN110343866B (en) | Method for separating vanadium and chromium from vanadium and chromium reduction slag | |
| CN114477282B (en) | Method for preparing low-silicon red cakes through reduction, hydrolysis, vanadium precipitation and desilication | |
| CN110803714A (en) | Method for producing vanadium pentoxide by vanadium-containing solution | |
| CN1030308C (en) | Process for preparation of titanate | |
| CN114394619B (en) | Method for preparing low-silicon ammonium sodium polyvanadate through reduction and vanadium precipitation desilication | |
| CN114480883B (en) | Method for preparing high-purity vanadium pentoxide by removing silicon and chromium in vanadium solution through nickel ion cooperation | |
| US2460975A (en) | Recovery of molybdenum compounds | |
| CN114314660B (en) | Method for preparing low-silicon ammonium polyvanadate through reduction vanadium precipitation and desilication |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |