CN1032764C - 锡阳极泥提取贵金属和有价金属的方法 - Google Patents
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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
锡阳极泥提取贵金属和有价金属的方法。其方法为锡阳极泥盐酸浸出;浸出液铁粉置换;置换残液石灰中和得锡精矿,锡回收率>90%;置换渣回收铋,铋回收率>90%;盐酸浸出渣热水浸出铅,回收铅(铅浸出率>85%);热水浸出渣硫酸化焙烧,稀硫酸浸出;浸出液湿法回收提纯银,银回收率>98%,纯度99.95%;浸出渣混酸氯化,锌粉置换,湿法回收提纯金,金回收率>99%,纯度99.99%。
Description
锡阳极泥提取贵金属和有价金属的方法。本发明是关于贵金属冶金。
锡阳极泥是提取贵金属的原料之一,锡阳极泥一般组成为(%,Au除外):Au25g/T,Ag~1.5,Pb7,Sn30,Bi25,Cu5,Sb2,As2,SiO215,Fe0.07,S0.8。锡阳极泥含锡、铋高,含金,银低,成分复杂,属低银的多金属物料,而且金属性质又相近,两性元素较多,难以进行贵金属及多金属的综合回收。过去传统的处理方法是用硝酸处理锡阳极泥提取银,其残渣无成功办法处理,只好堆放。1990年6月23日中国专利申请“一种焊锡阳极泥硝酸渣提取银和金的方法”(申请号90103200.X)成功地提出一个处理焊锡阳极泥硝酸渣提取银和金的综合流程,银和金的回收率高,纯度高;但是方法还不完善,其他有价金属没有综合回收,而且锡阳极泥中金、银含量比其硝酸渣渣低得多(Au为1∶10,Ag为1∶5),锡、铋含量高得多(约高10倍),显然处理锡阳极泥比锡阳极泥硝酸渣复杂得多,不能照搬中国专利申请90103200.X的方法。
本发明的目的是在中国专利申请90103200.X方法的基础上提出锡阳极泥综合提取贵金属和有价金属的有效方法,既能有效地把银和金从废渣中提取出来,回收率高,纯度高,又能综合回收锡阳极泥中的其他有价金属,特别是锡和铋。
本发明所提供的方法,(1)是将所说的锡阳极泥物料在盐酸浓度3-5N,固体(重量,g数)∶液体(体积,ml数)=1∶5-7,温度70-95℃条件下进行浸出,最好锡阳极泥磨细至粒度<0.18mm,盐酸浓度4N,固体(重量,g数)∶液体(体积,ml数)=1∶6,温度80-90℃条件下浸出,时间3小时,As、Sb、Bi、Cu、Sn进入溶液,Au、Ag、Pb留在渣中,冷却后固液分离。(2)将(1)、所得浸出液在微热条件下用Fe粉置换,铁粉用量约30(重量)%,时间5小时,As、Sb、Bi、Cu进入置换渣,Sn留在溶液中,固液分离,置换渣回收铋,铋回收率>90%,置换液回收锡。(3)将(2)所得溶液用石灰乳中和至PH值接近中性,Sn以Sn(OH)2形式沉淀,产出锡精矿,送锡鼓风炉或反射炉熔炼产出粗锡,锡回收率>90%,中和残液含Sn、Bi、Cu<0.0004g/l,可送氯化***做氯化剂用,也可排出。(4)将(1)所得浸出渣在固体(重量,g数)∶液体(体积,ml数)=1∶7-9条件下,用热水进行二次浸出,第一次40分钟,第二次30分钟,铅富集于浸出液中(Pb浸出率>85%),Ag、Au富集于浸出渣中。(5)将(4)所得浸出渣在温度450-600℃,加浓硫酸进行硫酸化焙烧,使Ag转变Ag2SO4,最好温度为500-550℃,浓H2SO4加入量为70(重量)%,时间3小时。(6)将(5)所得硫酸化烙烧渣在硫酸浓度=0.5-5N,最好~1N,固体(重量,g数)∶液体(体积,ml数)=1∶10-20,最好1∶15,温度80-90℃条件下进行二次浸出,第一次2小时,第二次1小时,Ag进出浸入液中,Au留在渣中。(7)向(6)所得浸出液中加入盐酸处理,使Ag转变为AgCl沉淀,再用传统氨水溶解,水合肼沉淀法提纯,得纯银粉,银回收率>98%,纯度99.95%,(8)将(6)所得浸出渣在HCl+H2SO4的混酸介质,浓度最好为1NHCl+1NH2SO4,固体(重量,g数)∶液体(体积,ml数)=1∶4-8,最好=1∶7,温度60-70℃,加入NaClO3进行氯化反应,使Au进入氯化液中,NaClO3加入量为25(重量)%,分次加入,时间6小时。(9)向(8)所得氯化液,冷却后加入锌粉置换,得粗金粉,再用湿法分离提纯,得海绵金,Au纯度99.99%,直收率>99%。
本发明的优点是:1、锡阳极泥中低含量的贵金属得到有效回收,金银回收率高(Au>99%,Ag>98%)纯度高(>99.9%)。2、锡阳极泥中的有价金属锡,铋也能综合回收(锡、铋回收率>90%)。3、工艺先进、合理、技术可靠、流程简短。4、废气废水经适当处理不污染环境。
实施例:
成分为(%,Au除外):Au25g/T,Ag~1.5,Pb7,Sn30,Bi25,Cu5,Sb2,As2,SiO215,Fe0.07,S0.8的锡阳极泥249.3Kg,经过(1)盐酸浸出:盐酸浓度4N,固体(重量,g数)∶液体(体积,ml数)1∶6,温度80-90℃,浸出时间3小时,(2)铁粉置换:温度40-60℃,铁粉用量30(重量)%,置换时间5小时;(3)中和沉淀锡:用石灰乳中和至PH=4-4.5;(4)热水浸铅,温度>90℃,固体(重量,g数)∶液体(体积,ml数)=1∶8,二次浸出(40分,30分);(5)硫酸化焙烧,温度500-550℃,固体(重量,g数)∶液体(体积,ml数)1∶0.7,时间3小时,(6)稀硫酸二次浸出,硫酸浓度1N,反应温度>85℃,固体(重量,g数)∶液体(体积,ml数)1∶15,二次浸出(2小时,1小时);(7)稀硫酸浸出液盐酸转化氯化银-氨水溶解水合肼还原沉淀银;(8)稀硫酸浸出渣氯化浸出金;1N硫酸+1N盐酸,固体(重量,g数)∶液体(体积,ml数)1∶7,氯酸钠用量25(重量)%,温度60~70℃,时间6小时;(9)氯化液锌粉置换金:常温,1公斤物料加锌15-20g;(10)粗金粉湿法分离提纯,得到纯银(纯度99.95%)3.665Kg,回收率98%;纯金(纯度99.99%)6.170g,回收率99%;Sn(OH)2精矿含Sn>48%,回收率>90%;以及铋精矿,含铋>75%,回收率>90%,铅以海绵铅形式回收,回收率75%。
Claims (5)
1、锡阳极泥提取贵金属和有价金属的方法,其特征在于:
a、将锡阳极泥在盐酸浓度=3-5N,固体(重量,g数)∶液体(体积,ml数)=1∶5~7,温度70-95℃条件下进行浸出,As、Sb、Bi、Cu、Sn等元素进入溶液,Au、Ag、Pb留在渣中,冷却后固液分离;
b、将a所得浸出液在微热条件下,用铁粉置换,铁粉用量~30(重量)%,时间5小时,使As、Sb、Bi、Cu进入置换渣,Sn留在溶液中,固液分离;
c、将b所得溶液用石灰乳中和至PH值接近中性,Sn以Sn(OH)2形式沉淀,产出锡精矿;
d、将a所得浸出渣在固体(重量,9数)∶液体(体积,ml数)=1∶7~9条件下,用热水二次浸出(40分,30分),PbCl2进入溶液中,Ag、Au富集于浸出渣中;
e、将d所得浸出渣在温度450~600℃,加浓硫酸进行硫酸化焙烧,使银转变为Ag2SO4;
f、将e所得焙烧渣在硫酸浓度0.5~5N,固体(重量,g数)∶液体(体积,ml数)=1∶10~20,温度80~90℃条件下进行二次浸出,Ag进入浸出液中,Au留在渣中;
g、将f所得浸出液用HCl处理使Ag转化为AgCl沉淀、过滤,用氨水溶解,水合肼还原沉淀得纯净海绵Ag;
h、将f所得浸出渣在HCl+H2SO4混酸介质,固体(重量,g数)∶液体(体积,ml数)=1∶4~8,温度60~70℃,用氯酸钠进行氯化反应,使Au转入溶液;
i、将h所得氯化液冷却后加入锌粉置换,置换渣为粗金,再用湿法进行分离提纯,得海绵金。
2、如权利要求1所述的锡阳极泥提取贵金属和有价金属的方法,其特征是进行1a过程时,阳极泥粒度<0.18mm,HCl浓度=4N,固体(重量,g数)∶液体(体积,ml数)=1∶6,浸出温度80~90℃,时间3小时。
3、如权利要求1所述的锡阳极泥提取贵金属和有价金属的方法,其特征是进行1e过程时,温度为500-550℃,浓硫酸加入量为70(重量)%,时间3小时。
4、如权利要求1所述的锡阳极泥提贵金属和有价金属的方法,其特征是进行1f过程时,固体(重量,g数)∶液体(体积,ml数)=1∶15,硫酸浓度~1N,第一次浸出2小时,第二次1小时。
5、如权利要求1所述的锡阳极泥提取贵金属和有价金属的方法,其特征是进行1h过程时,条件为1NHCl+1NH2SO4的混酸介质,固体(重量,g数)∶液体(体积,ml数)=1∶7,氯化时间6小时,NaClO3用量为25(重量)%,分次加入。
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CN1051114C (zh) * | 1996-10-25 | 2000-04-05 | 昆明贵金属研究所 | 铅阳极泥湿法酸浸前预处理方法 |
CN101886174B (zh) * | 2010-06-23 | 2012-08-29 | 郴州雄风稀贵金属材料股份有限公司 | 从阳极泥回收所产生的含铋物料中提炼高纯铋的工艺 |
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