CN1095809C - 含铁盐溶液的处理方法 - Google Patents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
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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
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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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1204—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
- C22B34/1213—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by wet processes, e.g. using leaching methods or flotation techniques
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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
- C22B47/00—Obtaining manganese
- C22B47/0018—Treating ocean floor nodules
- C22B47/0045—Treating ocean floor nodules by wet processes
- C22B47/0081—Treatment or purification of solutions, e.g. obtained by leaching
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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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- Y02P10/00—Technologies related to metal processing
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- Inorganic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
通过添加能够将可溶性锰盐转变成二氧化锰的氧化剂,和通过添加二氧化锰颗粒作为引晶剂,从而任何胶体状二氧化锰都沉积在晶种颗粒上,而去除作为含铁盐溶液的污染物存在的可溶性锰盐。
Description
本发明涉及处理铁盐和锰盐的混合物以降低混合物的锰含量,尤其是涉及硫酸盐法生产二氧化钛中产生的铁盐的处理。
在生产二氧化钛的硫酸盐法中,含钛原材料,像钛铁矿石,用硫酸浸渍形成固体物质,再用水处理,过滤,得到主要含有硫酸钛、硫酸亚铁和硫酸铁的溶液。通过添加铁将铁离子还原成亚铁离子,真空下冷却该溶液,使硫酸亚铁(通常称作绿矾)结晶析出,剩下硫酸钛溶液,再利用水解使二氧化钛从溶液中沉淀析出。可供选择地,首先沉淀出二氧化钛,再使绿矾从废液中结晶析出。
很显然,硫酸亚铁的量相对于产生的二氧化钛的量取决于原材料中铁和钛的比率。典型的数值是,对于钛铁矿(块状)约为1∶1,对于钛铁矿(砂状)约为0.71∶1,和对于钛铁矿(矿渣)约为0.15∶1。要知道,任何情况下,都会产生出大量的硫酸亚铁,发现可以对其利用,但在对它处理中涉及到环境问题。
硫酸亚铁的一个应用是作为基本材料使用,由其可制备水处理用的絮凝剂。在一种通常的方法中,将硫酸亚铁通过用硫酸和硝酸混合物溶解,氧化成硫酸铁。再添加含有胶体颗粒的水时,硫酸铁水解形成不溶的氢氧化物,再与胶体颗粒相互作用,使它们凝结。然后通过沉降和/或过滤可除去絮凝的颗粒。
副产物的进一步应用是生产氧化铁。然而,利用通常的方法却不能氧化可溶性的锰。虽然已经知道,通过进一步添加氧化剂,像过氧化物或高锰酸钾,可将可溶性的锰氧化成不溶的二氧化锰,如此生产的二氧化锰是非常细碎的胶体形式,它非常难以去除,而且去除费用昂贵,尤其是工业规模上,因此细硫酸铁产品仍含有大量的锰,使得它在以上应用中不能令人满意。
根据本发明的一个方面,提供一种受可溶性锰盐污染含铁盐溶液的处理方法,包括向溶液中添加一种能够将所述锰盐转变成二氧化锰的氧化剂,其特征在于添加二氧化锰作为引晶剂,这样,任何胶体状二氧化锰都会沉积在该晶种颗粒上,其特征还在于将二氧化锰颗粒从含铁盐溶液中分离。
按照优选的特征,在添加氧化剂之前添加引晶剂。期望晶种颗粒的平均颗粒尺寸至少为10μm,优选尺寸为30-50μm。
按照另一个优选特征,可以利用硫酸亚铁和高锰酸钾反应生产晶种颗粒。
为了降低费用,可以将由一批量处理硫酸铁溶液分离出的二氧化锰颗粒循环用作另一批量溶液的晶种颗粒。
利用通常方法处理硫酸亚铁并不必将所有的硫酸亚铁转变成硫酸铁。通常,这是不利的。而根据本发明的另一个优选方面,通过添加高锰酸钾,可以利用该残存的硫酸亚铁生产二氧化锰晶种颗粒。当然,如果存在的硫酸亚铁太少,不能产生所需量的晶种,则可以再添加硫酸亚铁。
氧化剂可以是任一种已知的氧化剂,像臭氧、过氧化物或过硫酸盐。然而,氧化剂优选是高锰酸钾,可以以饱和溶液的形式在一段时间内连续添加。
当在回流温度下进行时,该方法是有效的。然而,其可在70-80℃的温度下进行,即,在此温度下,硫酸亚铁溶解在硫酸/硝酸中,以致于可以直接从反应器中取液体,而不需要任何额外的加热。
根据如下实施例可以更容易地理解本发明。
实施例1
在一个90分钟的周期内,在回流下向6升纯硫酸亚铁(20gpl Fe)中加入化学计算量(30gpl)的高锰酸钾,以制备二氧化锰引晶剂。再将溶液在回流下保持60分钟,过滤出产生的固体,并用水洗涤。利用Malvern Mastersizer测量,得到43μm的平均颗粒尺寸。
实施例2
将利用硫酸盐法制备二氧化铁中获得的副产物硫酸亚铁溶解在硫酸和硝酸的混合物中,得到pH为0.5的硫酸铁液体。测定铁和锰的含量。然后将液体进行回流,添加50gpl实施例1的晶种。利用蠕动泵在90分钟周期内连续添加化学计算量的高锰酸钾,再将混合物保持回流30分钟。每30分钟取一次样品25ml,在真空下通过0.45μm过滤器过滤。对所得滤液分析其铁、锰含量。滤出的固体用水洗涤,测定颗粒尺寸。结果示于表1中。
表1
实施例3除了添加75gpl的晶种颗粒外,重复实施例2。结果示于表2中。
时间(分钟) | 锰含量(μg/g) | 铁含量(%) | 过滤时间(秒) | 颗粒尺寸(μm) |
0 | 1174 | 13.62 | 51 | 44.7 |
30 | 964 | 12.7 | 50 | 45.7 |
60 | 610 | 13 | 400 | 46.2 |
90 | 121 | 12.5 | 180 | 47.55 |
180 | <10 | 12.6 | 140 | 47 |
表2
时间(分钟) | 锰含量(μg/g) | 铁含量(%) | 过滤时间(秒) | 颗粒尺寸(μm) |
0 | 1230 | 133.3 | 53 | 41.59 |
30 | 890 | 12.7 | 28 | 41.91 |
60 | 570 | 13 | 45 | 43.25 |
90 | 120 | 12.5 | 40 | 43.17 |
180 | 50 | 12.6 | 33 | 42.74 |
实施例4
将1升实施例3的溶液置于量筒内,并使之沉降。7天后,出现透明沉清液体,它含有21μg/g的锰。
实施例5
除了从最终溶液中去除适量固体用作引晶剂外,重复实施例3。获得类似的结果。
实施例6
测量用硫酸和硝酸处理硫酸亚铁产生的溶液中的亚铁含量,如果需要,进一步添加硫酸亚铁,直到在添加化学计算量的高锰酸钾时,足以提供75gpl的二氧化锰引晶剂为止。
然后再添加一定量的高锰酸钾,如实施例2那样。使最终溶液沉降。不到25小时内形成透明沉清液体,其含有500μg/g的锰。
Claims (10)
1.一种处理由可溶性锰盐污染的含铁盐溶液的方法,包括向溶液中添加能将所述锰盐转变成二氧化锰的氧化剂,其特征在于添加二氧化锰作为引晶剂,从而任何胶体二氧化锰沉积在该晶种颗粒上,并且从含铁盐溶液中分离二氧化锰颗粒。
2.根据权利要求1的方法,其特征在于在添加氧化剂之前添加引晶剂。
3.根据权利要求1或2的方法,其特征在于晶种颗粒的平均颗粒尺寸至少为10μm。
4.根据权利要求3的方法,其中晶种颗粒的平均颗粒尺寸为30-50μm。
5.根据权利要求1的方法,其特征在于通过硫酸亚铁和高锰酸钾反应生产晶种颗粒。
6.根据权利要求1的方法,其特征在于将由溶液分离的二氧化锰颗粒进行循环,形成晶种颗粒。
7.根据权利要求1的方法,其特征在于将高锰酸钾和,如果需要,硫酸亚铁,添加到溶液中以产生晶种颗粒。
8.根据权利要求1的方法,其特征在于氧化剂为高锰酸钾。
9.根据权利要求8的方法,其特征在于以饱和溶液形式连续添加高锰酸钾。
10.根据权利要求1的方法,其特征在于溶液的温度为70-80℃。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB9703662.8 | 1997-02-21 | ||
GB9703662A GB9703662D0 (en) | 1997-02-21 | 1997-02-21 | Treatment of a solution containing iron salts |
Publications (2)
Publication Number | Publication Date |
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CN1248230A CN1248230A (zh) | 2000-03-22 |
CN1095809C true CN1095809C (zh) | 2002-12-11 |
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Application Number | Title | Priority Date | Filing Date |
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CN98802676A Expired - Fee Related CN1095809C (zh) | 1997-02-21 | 1998-02-18 | 含铁盐溶液的处理方法 |
Country Status (16)
Country | Link |
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US (1) | US6245240B1 (zh) |
EP (1) | EP1034136B1 (zh) |
JP (1) | JP2001512409A (zh) |
CN (1) | CN1095809C (zh) |
AU (1) | AU6107898A (zh) |
BR (1) | BR9812997A (zh) |
CA (1) | CA2281760C (zh) |
CZ (1) | CZ294573B6 (zh) |
DE (1) | DE69824443T2 (zh) |
ES (1) | ES2222571T3 (zh) |
GB (2) | GB9703662D0 (zh) |
MY (1) | MY116713A (zh) |
NO (1) | NO994008L (zh) |
PL (1) | PL335186A1 (zh) |
WO (1) | WO1998037022A1 (zh) |
ZA (1) | ZA981212B (zh) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
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FI106791B (fi) * | 1998-10-30 | 2001-04-12 | Kemira Chemicals Oy | Menetelmä käyttökelpoisten tuotteiden valmistamiseksi epäpuhtaasta ferrisulfaattiliuoksesta |
JP2001226121A (ja) * | 2000-02-17 | 2001-08-21 | Taki Chem Co Ltd | 硫酸第二鉄溶液中のマンガンの除去方法 |
JP4831589B2 (ja) * | 2000-02-17 | 2011-12-07 | 多木化学株式会社 | 硫酸第二鉄溶液の製造方法 |
JP5029982B2 (ja) * | 2005-06-07 | 2012-09-19 | 鶴見曹達株式会社 | 塩化鉄水溶液の精製法 |
US7641801B2 (en) * | 2007-02-28 | 2010-01-05 | Vale Inco Limited | Method for removing manganese from nickel laterite waste liquors |
CN103708566B (zh) * | 2013-12-26 | 2015-07-22 | 攀枝花东方钛业有限公司 | 一种提高硫酸亚铁过滤性能的方法 |
CN104162404B (zh) * | 2014-08-25 | 2017-01-25 | 北京矿冶研究总院 | 一种稀土掺杂水合氧化锰的吸附剂制备方法 |
CN109970105B (zh) * | 2019-04-24 | 2021-04-16 | 西南科技大学 | 一种湿法炼锌工艺中清洁回收铁的方法 |
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US4067789A (en) * | 1975-07-09 | 1978-01-10 | Newmont Exploration Limited | Process for manganese removal from zinc metal bearing solutions |
WO1997034836A1 (en) * | 1996-03-18 | 1997-09-25 | Kemira Chemicals Oy | A method for improving the applicability of a water treatment chemical, and a coagulant |
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US2786751A (en) * | 1954-06-09 | 1957-03-26 | Roy Tuhin Kumar | Method of separating cobalt-nickel-manganese |
DE1299567B (de) * | 1964-01-03 | 1969-07-17 | Hoechst Ag | Verfahren zum Reinigen von Abwaessern |
US3349031A (en) * | 1965-08-20 | 1967-10-24 | Calgon Corp | Method and composition for removal of manganese from water |
CA1141172A (en) * | 1978-12-20 | 1983-02-15 | Gerald L. Bolton | Removal of manganese ions from zinc and manganese containing solutions |
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1997
- 1997-02-21 GB GB9703662A patent/GB9703662D0/en active Pending
-
1998
- 1998-02-13 ZA ZA981212A patent/ZA981212B/xx unknown
- 1998-02-17 GB GB9803316A patent/GB2322365B/en not_active Expired - Fee Related
- 1998-02-18 AU AU61078/98A patent/AU6107898A/en not_active Abandoned
- 1998-02-18 DE DE1998624443 patent/DE69824443T2/de not_active Expired - Fee Related
- 1998-02-18 CA CA 2281760 patent/CA2281760C/en not_active Expired - Fee Related
- 1998-02-18 CN CN98802676A patent/CN1095809C/zh not_active Expired - Fee Related
- 1998-02-18 BR BR9812997A patent/BR9812997A/pt active Search and Examination
- 1998-02-18 PL PL33518698A patent/PL335186A1/xx unknown
- 1998-02-18 ES ES98905510T patent/ES2222571T3/es not_active Expired - Lifetime
- 1998-02-18 EP EP98905510A patent/EP1034136B1/en not_active Expired - Lifetime
- 1998-02-18 US US09/367,675 patent/US6245240B1/en not_active Expired - Lifetime
- 1998-02-18 JP JP53637798A patent/JP2001512409A/ja active Pending
- 1998-02-18 WO PCT/GB1998/000504 patent/WO1998037022A1/en active IP Right Grant
- 1998-02-18 CZ CZ19992958A patent/CZ294573B6/cs not_active IP Right Cessation
- 1998-02-19 MY MYPI9800696 patent/MY116713A/en unknown
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- 1999-08-19 NO NO994008A patent/NO994008L/no not_active Application Discontinuation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1592558A1 (de) * | 1967-11-24 | 1970-11-26 | Varta Gmbh | Aktivierter Braunstein und Verfahren zu seiner Herstellung |
US4067789A (en) * | 1975-07-09 | 1978-01-10 | Newmont Exploration Limited | Process for manganese removal from zinc metal bearing solutions |
WO1997034836A1 (en) * | 1996-03-18 | 1997-09-25 | Kemira Chemicals Oy | A method for improving the applicability of a water treatment chemical, and a coagulant |
Also Published As
Publication number | Publication date |
---|---|
DE69824443T2 (de) | 2004-10-07 |
GB9803316D0 (en) | 1998-04-15 |
BR9812997A (pt) | 2000-08-15 |
CA2281760C (en) | 2005-11-29 |
GB2322365B (en) | 2000-08-09 |
US6245240B1 (en) | 2001-06-12 |
CZ294573B6 (cs) | 2005-02-16 |
PL335186A1 (en) | 2000-04-10 |
DE69824443D1 (de) | 2004-07-15 |
GB2322365A (en) | 1998-08-26 |
CN1248230A (zh) | 2000-03-22 |
NO994008L (no) | 1999-10-21 |
MY116713A (en) | 2004-03-31 |
WO1998037022A1 (en) | 1998-08-27 |
ES2222571T3 (es) | 2005-02-01 |
EP1034136B1 (en) | 2004-06-09 |
AU6107898A (en) | 1998-09-09 |
EP1034136A1 (en) | 2000-09-13 |
JP2001512409A (ja) | 2001-08-21 |
CA2281760A1 (en) | 1998-08-27 |
ZA981212B (en) | 1998-08-20 |
GB9703662D0 (en) | 1997-04-09 |
NO994008D0 (no) | 1999-08-19 |
CZ295899A3 (cs) | 2000-01-12 |
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