CN106435175A - 一种协同酸性浸出法从钼焙砂制备钼酸铵的方法 - Google Patents
一种协同酸性浸出法从钼焙砂制备钼酸铵的方法 Download PDFInfo
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- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 57
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000011733 molybdenum Substances 0.000 title claims abstract description 48
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 title claims abstract description 33
- 229940010552 ammonium molybdate Drugs 0.000 title claims abstract description 33
- 235000018660 ammonium molybdate Nutrition 0.000 title claims abstract description 33
- 239000011609 ammonium molybdate Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002386 leaching Methods 0.000 title claims abstract description 20
- 239000002253 acid Substances 0.000 title claims abstract description 18
- 230000002195 synergetic effect Effects 0.000 title abstract 2
- 239000012074 organic phase Substances 0.000 claims abstract description 42
- 239000012535 impurity Substances 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 230000002378 acidificating effect Effects 0.000 claims abstract description 5
- 239000003085 diluting agent Substances 0.000 claims abstract description 5
- 150000002923 oximes Chemical class 0.000 claims abstract description 3
- 239000012071 phase Substances 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 19
- 238000000605 extraction Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 239000003350 kerosene Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 238000011001 backwashing Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- GZCWLCBFPRFLKL-UHFFFAOYSA-N 1-prop-2-ynoxypropan-2-ol Chemical class CC(O)COCC#C GZCWLCBFPRFLKL-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 150000001735 carboxylic acids Chemical class 0.000 claims description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- -1 phosphate ester Chemical class 0.000 abstract description 2
- 239000002893 slag Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000005416 organic matter Substances 0.000 abstract 3
- 229910019142 PO4 Inorganic materials 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 239000010452 phosphate Substances 0.000 abstract 1
- 150000003008 phosphonic acid esters Chemical class 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 14
- 229910052710 silicon Inorganic materials 0.000 description 12
- 229910052698 phosphorus Inorganic materials 0.000 description 11
- 229910052700 potassium Inorganic materials 0.000 description 10
- 229910052759 nickel Inorganic materials 0.000 description 9
- 229910021529 ammonia Inorganic materials 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000001099 ammonium carbonate Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 235000012501 ammonium carbonate Nutrition 0.000 description 3
- QUXFOKCUIZCKGS-UHFFFAOYSA-N bis(2,4,4-trimethylpentyl)phosphinic acid Chemical compound CC(C)(C)CC(C)CP(O)(=O)CC(C)CC(C)(C)C QUXFOKCUIZCKGS-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 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
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- FYNBDWDEBZXMSV-UHFFFAOYSA-N [As].[P].[Si] Chemical compound [As].[P].[Si] FYNBDWDEBZXMSV-UHFFFAOYSA-N 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011499 joint compound Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/30—Oximes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/32—Carboxylic acids
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
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- 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
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Abstract
本发明公开了一种协同酸性浸出法从钼焙砂制备钼酸铵的方法。将钼焙砂与酸、有机物共同混合，分解钼焙砂，最终钼与有机物选择性结合，进入有机相中，杂质留在渣中或水相中，同时达到了分解钼焙砂和分离杂质的目的。本发明以酸性磷酸酯类、酸性膦酸酯类、肟类等有机物与稀释剂混合得到有机相与酸共同与钼焙砂混合，实现钼焙砂和分离杂质的目的，流程短，过程简单，反应速度快，钼分解率高，杂质分离效果好。
Description
技术领域
本发明涉及一种新型的分解钼焙砂的工艺，特别涉及一种有机相与酸协同分解钼焙砂，分解钼焙砂同时除去铜、铁、硅、硫、磷等杂质制备得到钼酸铵的方法，属于钼湿法冶炼领域。
背景技术
钼焙砂中常常含有铜、铁、硅、硫、磷等杂质元素，而钼酸铵产品对上述元素含量要求极高。钼酸铵产品国家标准（GB/T 3460-2007）表明，牌号为MSA-0级产品中Ni、K、Na、Cu、Si、P元素的含量分别不高于0.003、 0.01、 0.001、 0.0003、 0.0005、 0.0005%。现有工艺采用氨溶钼焙砂制备钼酸铵，得到钼酸铵溶液再采用沉淀法、离子交换法从钼酸铵溶液中除去杂质元素；或首先对钼焙砂进行洗涤，除去杂质元素，再进行氨溶，可以提高钼酸铵产品的质量。现有方法，将浸出和净化分为两步进行，需要首先通过氨浸出，再净化除杂才能得到合格的钼酸铵溶液，或者通过除杂，再氨浸得到钼酸铵溶液；除杂工艺复杂，对于不同的杂质离子需要不同的除杂手段，对于铜、锌等金属离子需要采用硫化物沉淀法，对于磷砷硅则需要镁盐沉淀法，对于钾、钠、硫需要对钼焙砂或者钼酸铵产品进行纯水或铵盐洗涤除杂。因此现有方法存在的问题包括：流程长，除杂过程复杂，操作难度较大。
发明内容
本发明的目的是提供一种协同酸性浸出法从钼焙砂制备钼酸铵的方法。
具体步骤为：
（1）将体积比为1:100~90:10的萃取剂和稀释剂混合制得有机相。
（2）浸出：将钼焙砂、酸液和步骤（1）所得有机相混合，在5~90℃温度搅拌5~240分钟后，静置分相，得到负钼有机相和浆料，负钼有机相送至反萃工序，浆料固液分离后得到浸出渣和滤液，滤液作为酸液返回浸出；钼焙砂：酸液体积比=1:0.5~1:30；酸液：有机相体积比=1:0.1~1:20，酸液中氢离子浓度为0.1~6mol/L。
（2）反萃：将步骤（2）所得负钼有机相与浓度为0.1~12mol/L反萃剂混合，反萃后的负载有机相（O）和萃余液（A）的体积比为O/A=3/1~4/1，在20~30℃搅拌10~30分钟，得到低杂质含量的钼酸铵溶液和空有机相，低杂钼酸铵溶液用于钼酸铵制备，空有机相送至浸出。所述酸液为盐酸、硫酸、硝酸和磷酸的一种或多种。
所述萃取剂为酸性磷酸酯类、肟类和羧酸类中的一种或多种，如P204、P507、Cyanex272、LIX64和lix984。
所述稀释剂磺化煤油、煤油、甲苯和260#溶剂油中的一种。
所述反萃剂为碱和盐的一种或多种，优先选择氨水、碳酸铵和碳酸氢铵中一种或多种。
本发明有益效果 ：
（1）该方法从钼焙砂制备纯钼酸铵溶液，无需按浸出与除杂两个步骤进行，而是在浸出时选择性将钼提取进行有机相中，杂质几乎完全存留在水相或渣中，再通过反萃一步直接得到高纯的钼酸铵溶液，无需繁复的除杂工序，从而将整个制备工艺过程简短、连续、致使能耗下降，效率提高， 成本降低。
（2）浸出在酸性条件进行，避免了传统氨浸出工艺过程操作环境差，氨气泄露等问题，从而改善了操作环境，减轻了氨污染。
实验结果表明，本发明能够一步得到钼酸铵溶液Mo、Ni、K、Na、Cu、Si、P浓度分别为215、 0.0005、 0.001、 0.001、 0.0003、 0.011、 0.001g/L，达到制备钼酸铵产品的要求。
具体实施方式
实施例 1：
有机相配制：体积比为30%P507+70%磺化煤油。
浸出：取50g钼焙砂（Mo、Ni、K、Na、Cu、Si、P质量百分比含量分别为50.45、 0.055、0.01、 0.05、 0.44、 2.33 、 0.21%）与200mL浓度为2mol/L的硫酸、有机相600mL混合，在20℃搅拌浸出60分钟，澄清分离得到负钼有机相，过滤浆料得到浸出渣和滤液。
反萃：负钼有机相与3.5mol/L氨水混合，O/A=4/1，在25℃搅拌10分钟，得到钼酸铵溶液和空有机相。
结果：滤渣中Mo质量百分比含量为1.23%，滤液中Mo浓度为1.20g/L钼浸出率为99.51%，得到钼酸铵溶液中Mo、Ni、K、Na、Cu、Si、P浓度分别为255.5、0.0004、 0.001、0.001、0.001、0.011、0.001g/L。
实施例 2：
有机相配制：体积比为30%cyanex272+70%磺化煤油。
浸出：取50g钼焙砂（Mo、Ni、K、Na、Cu、Si、P质量百分比含量分别为50.45、0.055、0.01、 0.05、 0.44、 2.33 、 0.21%）与100ml浓度为3mol/L的盐酸、有机相650mL混合，在30℃搅拌浸出30分钟，澄清分离得到负钼有机相，过滤浆料得到浸出渣和滤液。
反萃：负钼有机相与2.6mol/L氨水混合，O/A=3/1，在25℃搅拌10分钟，得到钼酸铵溶液和空有机相。
结果：滤渣中Mo质量百分比含量为1.01%，滤液中Mo浓度为0.71g/L钼浸出率为99.71%，得到钼酸铵溶液中Mo、Ni、K、Na、Cu、Si、P浓度分别为136.5、0.0001、 0.0005、0.001、0.001、0.009、0.001g/L。
实施例3：
有机相配制：体积比为35%P204+70%磺化煤油。
浸出：取50g钼焙砂（Mo、Ni、K、Na、Cu、Si、P质量百分比含量分别为35.11、 0.076、0.061、 0.081、 2.66、 2.43 、 0.12%）与100mL浓度为3mol/L的硫酸、有机相550mL混合，在50℃搅拌浸出40分钟，澄清分离得到负钼有机相，过滤浆料得到浸出渣和滤液。
反萃：负钼有机相与2.0mol/L氨水+0.6mol/L碳酸铵混合，O/A=4/1，在25℃搅拌15分钟，得到钼酸铵溶液和空有机相。
结果：滤渣中Mo质量百分比含量为0.77%，滤液中Mo浓度为0.95g/L，钼浸出率为99.31%，得到钼酸铵溶液中Mo、Ni、K、Na、Cu、Si、P浓度分别为148.5、0.0011、 0.0008、0.001、0.005、0.051、0.002g/L。
实施例4：
有机相配制：体积比为35%cyanex272+70%磺化煤油。
浸出：取50g钼焙砂（Mo、Ni、K、Na、Cu、Si、P含量分别为35.11、 0.076、 0.061、0.081、 2.66、 2.43 、 0.12）与100mL浓度为3mol/L的硫酸、有机相550mL混合，在35℃搅拌浸出40分钟，澄清分离得到负钼有机相，过滤浆料得到浸出渣和滤液。
反萃：负钼有机相与1.5mol/L氨水+1.6mol/L碳酸铵混合，O/A=4/1，在25℃搅拌20分钟，得到钼酸铵溶液和空有机相。
结果：滤渣中Mo质量百分比含量为0.72%，滤液中Mo浓度为0.55g/L，钼浸出率为99.36%，得到钼酸铵溶液中Mo、Ni、K、Na、Cu、Si、P浓度分别为155.5、0.0008、 0.0007、0.001、0.001、0.011、0.001g/L。
Claims (1)
1.一种协同酸性浸出法从钼焙砂制备钼酸铵的方法，其特征在于具体步骤为：
（1）将体积比为1:100~90:10的萃取剂和稀释剂混合制得有机相；
（2）浸出：将钼焙砂、酸液和步骤（1）所得有机相混合，在5~90℃温度搅拌5~240分钟后，静置分相，得到负钼有机相和浆料，负钼有机相送至反萃工序，浆料固液分离后得到浸出渣和滤液，滤液作为酸液返回浸出；钼焙砂：酸液体积比=1:0.5~1:30；酸液：有机相体积比=1:0.1~1:20，酸液中氢离子浓度为0.1~6mol/L；
（2）反萃：将步骤（2）所得负钼有机相与浓度为0.1~12mol/L反萃剂混合，反萃后的负载有机相和萃余液的体积比为3/1~4/1，在20~30℃搅拌10~30分钟，得到低杂质含量的钼酸铵溶液和空有机相，低杂钼酸铵溶液用于钼酸铵制备，空有机相送至浸出；
所述酸液为盐酸、硫酸、硝酸和磷酸的一种或多种；
所述萃取剂为酸性磷酸酯类、肟类和羧酸类中的一种或多种；
所述稀释剂磺化煤油、煤油、甲苯和260#溶剂油中的一种；
所述反萃剂为碱和盐的一种或多种。
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