CN1204297C - 在镍浸提过程中除硫的方法 - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 42
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002386 leaching Methods 0.000 title abstract description 7
- 229910052717 sulfur Inorganic materials 0.000 title abstract description 4
- 239000011593 sulfur Substances 0.000 title abstract description 4
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- 238000005363 electrowinning Methods 0.000 claims abstract description 16
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- 239000000243 solution Substances 0.000 claims description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical group [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 15
- 239000005864 Sulphur Substances 0.000 claims description 14
- 238000000605 extraction Methods 0.000 claims description 9
- 239000000292 calcium oxide Substances 0.000 claims description 8
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- 229910017052 cobalt Inorganic materials 0.000 claims description 7
- 239000010941 cobalt Substances 0.000 claims description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 6
- 239000012047 saturated solution Substances 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 4
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- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 150000002815 nickel Chemical class 0.000 claims description 2
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical group CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 claims 1
- 238000000746 purification Methods 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 3
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- 230000007935 neutral effect Effects 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 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 2
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- 230000008961 swelling Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- CZKYLWACZPRYOR-UHFFFAOYSA-N [S].OS(O)(=O)=O Chemical compound [S].OS(O)(=O)=O CZKYLWACZPRYOR-UHFFFAOYSA-N 0.000 description 1
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
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- C22B23/00—Obtaining nickel or cobalt
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Abstract
本发明涉及一种从镍处理的浸提循环例如镍冰铜浸提中除去硫的方法。根据该方法,镍电解冶金法中产生的阳极液借助钙基中和剂进行中和,其中硫以石膏的形式从浸提循环中除去。
Description
本发明涉及从浸提循环中除去硫的方法,该硫是在镍处理过程中,例如镍冰铜浸提过程中产生的。根据该方法,在镍电解冶金过程中形成的阳极液用石灰基中和剂中和,其中硫从浸提循环中以石膏的形式除去。
已知镍浓缩液首先在冶炼炉中用火法冶金处理以获得镍冰铜,其中含硫量相当高。然后,将该镍冰铜送入转炉,在其中回收到含硫量相当低的高品质镍冰铜。近来,已开始对生产镍的火法冶金处理工艺部分进行现代化,结果不再使用转炉,并且将由第一冶炼炉例如悬浮冶炼炉获得的镍冰铜直接供入湿法冶金工艺中。在第一冶炼炉中产生的炉渣通常需在电炉中进一步处理,此处生产的镍冰铜也进行进一步的湿法冶金处理。特别是在第一冶炼炉中,形成的镍冰铜的含硫量通常略高于转炉中的,因此如果在某种程度上未能小心地从浸提循环中除硫,则将增加在浸提过程中循环的硫含量,并可能导致硫溶胀(sulfur swelling)。这是硫酸盐基镍浸提工艺中的典型问题。
为了进行湿法冶金处理,碾磨镍冰铜并浸提到镍电解冶金法的阳极液中。镍冰铜的浸提是多步工艺,并包括在大气压和加压条件下的数个浸提步骤。所得到的硫酸镍溶液通过溶液提纯步骤(除钴)或引入镍电解冶金处理或在氢的帮助下还原为金属。
当将浸提镍冰铜形成的硫酸镍溶液引入电解冶金法中时,其反应如下:
电解冶金法中的电极用隔膜相互间隔开。该方法的主要特征之一是必须使特定电流穿过隔膜,从而使电解冶金法产生的硫酸不与阴极接触,否则将在阴极生成氢气而不形成镍。因此,对于特定镍量溶液流是恒定的,并产生某一恒定量的阳极液。阳极液的组成为约70g/l的Ni和45~50g/l的H2SO4。从反应式(1)可见,在电解冶金法中产生等分子的量的硫酸和析出的镍。至少部分该氧化的硫应从浸提循环中以硫酸盐的形式除去,以使镍不与该硫酸盐一起存在。
从浸提循环中除去硫通常采用钠基中和剂(碳酸钠,氢氧化钠),换句话说,根据不同情况,用氢氧化钠或苏打中和氧化的硫(硫酸)。中和的结果是产生可溶的硫酸钠,这在正常情况下应从该工艺过程中作为副产物除去。然而硫酸钠是一种有价值的产品,应将其用于商业销售,而如果不存在这种销售市场,则在中和硫时使用钠基中和剂是不经济的。
总之,在硫酸盐工艺中使用石灰的缺点是析出石膏,该石膏堵塞过滤器和隔膜布,还导致石膏层靠近热表面。
根据本发明现已形成了一种方法,其中在浸提镍冰铜中产生的至少部分硫通过将电解冶金法中的部分阳极液引入第二流进行回收,其中硫酸用某些钙基化合物,如煅石灰(CaO)或石灰石(CaCO3)进行中和。中和的溶液用石膏饱和,并且该石膏用例如萃取剂从溶液中分离出来,以使溶液中石膏的含量处于明显低于饱和的程度。将已除去部分石膏的中和阳极液送回浸提循环,优选送到除钴步骤中,在此它不会对实际的镍冰铜溶液造成负担。本发明主要的新特征从所附的权利要求书中明显可见。
在本发明的方法中,石灰沉淀过程产生出石膏的有害影响不仅可以通过沉淀和过滤溶液来防止,而且可以通过在石灰中和后立即将石膏从饱和溶液中除去来防止。除去石膏采用公知技术,例如用适当的萃取剂如DEHPA萃取,从而使溶液中的石膏含量明显低于饱和程度,这使石膏的有害影响最小化。产生的石膏沉淀物可以储存或用作建筑材料。
本发明将参照流程图1进一步描述。
浸提镍冰铜作为一个整体在流程图中简化为一个步骤,然而实际上它通常为多步工艺,并包括大气压和加压浸提步骤。用来自电解冶金法的锥形阳极液进行浸提,该阳极液为含硫酸的溶液。浸提步骤还包括回收铜和铁,并且按照常规方法进行。浸提得到的硫酸镍溶液送去除钴,而后对提纯的溶液进行电解,这根据电解冶金原理进行。
在电解冶金法中,镍作为单质纯镍在阴极上回收,并且在阳极区形成硫酸。在电解冶金过程中,溶液的镍含量降至约30g/l,而阳极液中的硫酸含量以等量增加。
部分阳极液被送回浸提步骤,而其它部分进入第二流,通过第二流将其引入单独的中和段,此处阳极液通过引入某些含钙中和剂例如细粉碎的煅石灰或石灰石进行中和。例如,如果使用煅石灰,其反应如下:
送入第二流的量优选为阳极液量的30~60%。溶液中的硫酸中和形成石膏,该石膏沉淀并从循环中滤除。
自中和过程排出的溶液饱和以石膏(Ca=500~700mg/l),并且如果将其直接送回浸提步骤,则可能有石膏在热表面和布等上沉淀的危险。为此,需用常规的萃取剂如DEHPA试剂从该溶液中萃取钙。该溶液中的石膏含量降低至明显低于饱和程度(Ca=50~150mg/l),从而避免了沉淀的危险。钙萃取中的有机相用盐酸溶液再次萃取,其中钙以氯化钙的形式除去。钙浸提后,中和的阳极液优选送入除钴步骤,如果将整个量的阳极液再循环回浸提中,在除钴步骤中镍冰铜浸提的实际浸提流保持在明显低于其应有的程度。
该方法值得一提的优点是,与现在使用的中和剂相比本方法的中和剂相当廉价有效。在电解冶金法中由特定浸提流中回收的镍量是恒定的,并且由于现在仅在适当的浸提步骤后,部分阳极液流送入来自所述冰铜浸提的浸提流中,这意味着来自浸提的溶液中的镍含量可提高到高于将整个液流再循环经过浸提步骤的情形。因此,对于特定量的溶液在浸提时待分离的镍量(δ镍g/l)可提高至高于电解冶金法中分离的情形。由于仅有部分溶液再循环回适当的浸提步骤,例如溶液的加热成本可大幅度降低。浸提设备的尺寸也可相应减少。来自电解冶金法的阳极液温度为约60℃,并且为了进行浸提,根据步骤的不同,将其加热至90~140℃。
Claims (13)
1、一种用于从镍冰铜的浸提循环中除去在镍冰铜的浸提中产生的硫的方法,该方法包括用镍电解的阳极液在数个步骤中浸提镍冰铜以形成硫酸镍溶液;提纯硫酸镍溶液,并且将经提纯的硫酸镍溶液进行镍电解以回收单质镍和含有作为硫酸的该镍冰铜的硫的阳极液;在中和步骤使用钙基中和剂中和部分阳极液的硫酸,以形成石膏饱和的溶液;在将该被中和的阳极液循环至浸出循环之前,从石膏饱和的溶液中除去石膏。
2、根据权利要求1的方法,其特征在于,使用所述钙基中和剂在中和步骤中中和部分阳极液的硫酸。
3、根据权利要求2的方法,其特征在于,使用所述钙基中和剂在中和步骤中中和30~60%的阳极液的硫酸。
4、根据权利要求1的方法,其特征在于,所述钙基中和剂是煅石灰CaO。
5.根据权利要求1的方法,其特征在于,所述钙基中和剂是石灰石CaCO3。
6、根据权利要求1的方法,其特征在于,所述钙基中和剂是煅石灰CaO和石灰石CaCO3。
7、根据权利要求1的方法,其特征在于,使用萃取剂从所述石膏饱和溶液中分离石膏,以使石膏浓度消耗至低于石膏饱和溶液的饱和浓度。
8、根据权利要求7的方法,其特征在于,所述萃取剂是二(2-乙基己基)磷酸。
9、根据权利要求7的方法,其特征在于,钙以氯化钙的形式从萃取石膏中除去。
10、根据权利要求1的方法,其特征在于,在从被中和阳极液中除去石膏以后,从已在钴去除步骤中分离出石膏的被中和的阳极液中去除钴。
11、根据权利要求7的方法,其中,在钙萃取后对被中和的阳极液进行溶液提纯。
12、根据权利要求1的方法,其中,石膏饱和溶液的钙浓度在500-700mg/l。
13、根据权利要求7的方法,其中,所述钙浓度被消耗至50-150mg/l。
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FI981760 | 1998-08-17 | ||
FI981760A FI106636B (fi) | 1998-08-17 | 1998-08-17 | Menetelmä rikin poistamiseksi nikkelikiven liuotusprosessista |
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CN1312867A CN1312867A (zh) | 2001-09-12 |
CN1204297C true CN1204297C (zh) | 2005-06-01 |
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CNB998097632A Expired - Fee Related CN1204297C (zh) | 1998-08-17 | 1999-08-12 | 在镍浸提过程中除硫的方法 |
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Country | Link |
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US (1) | US6387240B1 (zh) |
CN (1) | CN1204297C (zh) |
AP (1) | AP1188A (zh) |
AU (1) | AU759940B2 (zh) |
BR (1) | BR9915106B1 (zh) |
CA (1) | CA2340432C (zh) |
CU (1) | CU23024A3 (zh) |
FI (1) | FI106636B (zh) |
RU (1) | RU2226558C2 (zh) |
UA (1) | UA54618C2 (zh) |
WO (1) | WO2000009782A1 (zh) |
ZA (1) | ZA200101037B (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100594265C (zh) * | 2007-03-12 | 2010-03-17 | 张建玲 | 利用各种含镍原料生产电解镍的方法 |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
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RU2485190C1 (ru) * | 2011-11-10 | 2013-06-20 | Федеральное государственное бюджетное учреждение науки Институт химии и технологии редких элементов и минерального сырья им. И.В. Тананаева Кольского научного центра Российской академии наук (ИХТРЭМС КНЦ РАН) | Способ переработки никелевого штейна |
CN109628956A (zh) * | 2019-03-01 | 2019-04-16 | 阳谷祥光铜业有限公司 | 一种阴极铜的制备方法及装置 |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
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FR2131822B1 (zh) * | 1971-03-29 | 1975-07-04 | Nickel Le | |
CA1107678A (en) * | 1978-04-12 | 1981-08-25 | Kohur N. Subramanian | Nickel recovery from sulfur-deficient mattes |
FI97154C (fi) * | 1994-11-15 | 1996-10-25 | Outokumpu Eng Contract | Menetelmä nikkelikuparikiven liuottamiseksi |
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1998
- 1998-08-17 FI FI981760A patent/FI106636B/fi not_active IP Right Cessation
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1999
- 1999-08-06 AP APAP/P/1999/001617A patent/AP1188A/en active
- 1999-08-12 CA CA002340432A patent/CA2340432C/en not_active Expired - Lifetime
- 1999-08-12 WO PCT/FI1999/000672 patent/WO2000009782A1/en active IP Right Grant
- 1999-08-12 AU AU52928/99A patent/AU759940B2/en not_active Expired
- 1999-08-12 US US09/762,443 patent/US6387240B1/en not_active Expired - Lifetime
- 1999-08-12 CU CU20010042A patent/CU23024A3/es unknown
- 1999-08-12 CN CNB998097632A patent/CN1204297C/zh not_active Expired - Fee Related
- 1999-08-12 RU RU2001107120/02A patent/RU2226558C2/ru active
- 1999-08-12 BR BRPI9915106-5A patent/BR9915106B1/pt not_active IP Right Cessation
- 1999-12-08 UA UA2001031794A patent/UA54618C2/uk unknown
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN100594265C (zh) * | 2007-03-12 | 2010-03-17 | 张建玲 | 利用各种含镍原料生产电解镍的方法 |
Also Published As
Publication number | Publication date |
---|---|
WO2000009782A1 (en) | 2000-02-24 |
FI981760A (fi) | 2000-02-18 |
BR9915106A (pt) | 2001-07-24 |
FI981760A0 (fi) | 1998-08-17 |
AP1188A (en) | 2003-07-14 |
CU23024A3 (es) | 2005-02-23 |
FI106636B (fi) | 2001-03-15 |
BR9915106B1 (pt) | 2009-08-11 |
AU5292899A (en) | 2000-03-06 |
RU2226558C2 (ru) | 2004-04-10 |
CA2340432C (en) | 2007-12-11 |
CA2340432A1 (en) | 2000-02-24 |
AU759940B2 (en) | 2003-05-01 |
UA54618C2 (uk) | 2003-03-17 |
AP9901617A0 (en) | 1999-09-30 |
ZA200101037B (en) | 2002-05-03 |
CN1312867A (zh) | 2001-09-12 |
US6387240B1 (en) | 2002-05-14 |
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