CN110358919B - 一种酸浸分离锑铅的方法 - Google Patents
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- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 23
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 10
- 238000002386 leaching Methods 0.000 title claims abstract description 8
- 239000002253 acid Substances 0.000 title claims abstract description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 229910000978 Pb alloy Inorganic materials 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- CIWAOCMKRKRDME-UHFFFAOYSA-N tetrasodium dioxido-oxo-stibonatooxy-lambda5-stibane Chemical compound [Na+].[Na+].[Na+].[Na+].[O-][Sb]([O-])(=O)O[Sb]([O-])([O-])=O CIWAOCMKRKRDME-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000007670 refining Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- QQHJESKHUUVSIC-UHFFFAOYSA-N antimony lead Chemical compound [Sb].[Pb] QQHJESKHUUVSIC-UHFFFAOYSA-N 0.000 claims description 18
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 229910001245 Sb alloy Inorganic materials 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000003723 Smelting Methods 0.000 description 6
- 239000002893 slag Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- -1 silicon iron calcium sodium Chemical compound 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/02—Antimonates; Antimonites
- C01G30/023—Antimonates; Antimonites of ammonium, alkali or alkaline-earth metals or magnesium
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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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
本发明涉及一种酸浸分离锑铅的方法,是将锑铅合金破碎成200目以下,加入浓盐酸,搅拌条件下缓慢加入一定量双氧水,搅拌反应一段时间后,固液分离,滤液加入氢氧化钠和双氧水反应生成焦锑酸钠,滤渣熔融可直接进行铅电解精炼。本发明比起现有技术环境更友好,效率更高,回收时间更短,能耗更低,成本更低,可直接得到符合国家标准的焦锑酸钠。
Description
技术领域
本发明涉及一种酸浸分离锑铅的方法,属于有色金属湿法冶金领域。
背景技术
铅阳极泥还原熔炼初级阶段和贵铅氧化精炼初级阶段都会产生一种锑铅含量比较高的渣,工业上分别叫稀渣和锑渣,这两种渣除含锑铅外,还含有大量的硅铁钙钠,一般情况都是将渣加入还原碳粉进行还原熔炼,得到锑铅,这种情况得到锑铅合金,锑铅都有一定含量,锑占20-60%,铅占30-50%,若是直接进入铅电解精炼,锑含量太高会影响电解铅的精度,目前大部分是将锑铅进入转炉进行吹锑熔炼,使大部分的锑进入烟尘,从而达到锑铅的初步分离,剩余的锑铅锑含量比较小可以直接进入铅电解系统进行电解精炼,这种处理方法简单可靠,但是存在耗能高的缺点,高温冶炼环境恶劣。
发明内容
本发明的目的是提供一种成环境友好、能耗低的酸浸分离锑铅的方法。
本发明步骤如下:
(1)将锑铅合金破碎至200目以下的锑铅合金粉末;
(2)将步骤(1)所得锑铅合金粉末加入浓盐酸溶液中,搅拌10-30min后缓慢加入一定量双氧水,搅拌反应一定时间后过滤得滤液1和滤渣1;
(3)往步骤(2)所得滤液1搅拌条件下缓慢加入一定量的氢氧化钠和双氧水,搅拌氧化反应一定时间,过滤,滤渣即焦锑酸钠;
(4)步骤(2)所得滤渣1熔融后可直接进行铅电解精炼;
步骤(2)中盐酸浓度为5-10moL/L,反应时间为1-3h,浸出温度为室温,液固比为3-10:1,加入双氧水质量百分比为30%,加入双氧水的量为相当于把Sb单质氧化成三价锑理论量的1-1.2倍;
步骤(3)中双氧水用量为氧化溶液中三价锑所需理论量的1-1.2倍,氢氧化钠用量为中和盐酸所需量的1.5-3倍,反应时间为1-3h,反应温度为70-90℃。
所述滤渣1主要成分为Pb80-95%,Sb 1-5%。
本发明的有益效果:
(1)本发明在锑铅合金中,锑单质的还原能力强与铅单质,所以在盐酸溶液中,锑先被双氧水氧化,控制双氧水的加入量可以使锑单质被氧化而铅单质不被氧化,锑单质在浓盐酸中最先被氧化为溶于浓盐酸溶液的三价锑的多氯配合物,过滤就可以使锑与铅分离,三价锑的浓盐酸溶液加入氢氧化钠溶液和加双氧水反应生成难溶于水的焦锑酸钠;
(2)比起现有技术加入还原碳粉还原熔炼,得锑铅合金,再转炉进行吹锑熔炼的技术手段,采用加浓盐酸溶液和两次加双氧水,环境更友好,效率更高,回收时间更短,能耗更低,成本更低,可直接得到符合国家标准的焦锑酸钠。
具体实施方案
实施例1
所用锑铅合金,锑48%,铅51%;
称取100g锑铅合金粉末(粒度≤200目)加入5mol/L盐酸溶液中,液固比3:1,温度室温,搅拌20min,缓慢滴加1倍双氧水氧化锑单质为三价锑理论量的双氧水,搅拌反应2h,过滤,得滤液1和滤渣2。滤液1在搅拌条件下滴加1倍氧化溶液中三价锑所需理论量的双氧水和1.5倍中和盐酸所需理论量的氢氧化钠,氧化反应2h,温度80℃,过滤,洗涤,干燥,得到焦锑酸钠92.5g,锑含量为47.3%,锑直收率91.23%。滤渣2重54.1g,铅含量92.3%,锑含量6.35%,滤渣2可直接送铅电解工序。
Claims (1)
1.一种酸浸分离锑铅的方法,其特征在于:实施步骤如下:
(1)将锑铅合金破碎至200目以下得锑铅合金粉末;
(2)将步骤(1)所得锑铅合金粉末加入浓盐酸溶液中,搅拌10-30min后缓慢加入一定量双氧水,搅拌反应一定时间后过滤得滤液1和滤渣1;
(3)往步骤(2)所得滤液1搅拌条件下缓慢加入一定量的氢氧化钠和双氧水,搅拌氧化反应一定时间,过滤,滤渣即焦锑酸钠;
(4)步骤(2)所得滤渣1熔融后可直接进行铅电解精炼;
步骤(2)中盐酸浓度为5-10moL/L,反应时间为1-3h,浸出温度为室温,液固比为3-10:1,加入双氧水质量百分比为30%,加入双氧水的量为相当于把Sb单质氧化成三价锑理论量的1-1.2倍;
步骤(3)中双氧水用量为氧化溶液中三价锑所需理论量的1-1.2倍,氢氧化钠用量为中和盐酸所需量的1.5-3倍,反应时间为1-3h,反应温度为70-90℃。
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