CN85100108A - 从铜电解阳极泥中提取金、银的萃取工艺 - Google Patents
从铜电解阳极泥中提取金、银的萃取工艺 Download PDFInfo
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Abstract
从铜电解阳极泥中提取金、银萃取工艺。本发明所属领域为贵金属提取。铜阳极泥是获取金、银的重要原料，目前不论是火法还是水法处理流程所得金、银产品，大多需要用电解法精炼，限制了金、银收率的提高。本发明提出了用二(2-乙基己基)硫醚萃取金、银的处理铜阳极泥的工艺流程，可革除电解工序，简化流程，提高收率。本发明适用从各种铜、铅阳极泥以及含金银的物料中提取金、银。流程包括如下主要工序：预处理，硝酸浸银，萃取提银，硝酸不溶渣用王水浸金，萃取提金。
Description
本发明所属领域：贵金属提取
铜电解阳极泥是电解精炼铜时得到的副产品，其中含有铜、铅、银、金、硒、碲等元素，是获取金、银的重要原料。目前，铜阳极泥的处理工艺主要分火法和水法两大类。传统的火法流程是通过硫酸化焙烧、苏打焙烧或氧化焙烧脱硒、浸铜后熔炼成金银合金，最后用电解法制取纯的银和金。火法流程工艺复杂，设备多样，返料多，损耗大，而且容易污染环境。为了提高熔炼效率，减少污染，近年来又发展了选冶联合流程，即阳极泥在脱硒、脱铜后先用浮选法富集金、银，得到的浮选精矿再行熔炼。选冶流程中的主要问题是尾矿中的金、银含量还相当高，需要作为返料处理。水法流程是使阳极泥中所含的主要元素转入水溶液后再进行分离，目前常用的是化学沉淀法。但水法得到的金、银产品一般仍需要用电解法加以精炼，因此依然不能全部摆脱火法流程的缺点。水法处理的新技术萃取法因其回收完全、分离彻底，操作迅速简便而日益受到重视。目前已有关于利用萃取法处理铜阳极泥的报导（如日本特开昭56-3630），但选用的萃取体系选择性较差。此外，银仍是用沉淀法处理。所得金银，一般还要进行电解精炼。
本发明旨在开发一项从铜电解阳极泥中用萃取法分别提取金、银的工艺，借以革除电解精炼工序，简化流程，提高效率，缩短生产周期。
本发明提出了以酸浸-萃取-反萃-还原为主要工序的从铜电解阳极泥中萃取金银的工艺流程，其特征在于先用硝酸浸出银，再用王水浸出金，然后分别进行萃取回收。本发明还提供了二（2-乙基己基）硫醚（二异辛基硫醚）作为萃取剂。兹结合流程图（图1）详细说明如下：
预处理工序 根据铜阳极泥的组成，回收元素的种类和产品形式选择合适的预处理方法。如阳极泥中的铜希望以硫酸铜形式回收时，可采取常用的硫酸化焙烧后水浸脱铜或采用在鼓空气条件下用稀硫酸脱铜的方法。如需要回收硒，可采用氧化蒸硒的方法。如无上述要求，则原泥便无需进行预处理而直接进入下一工序。
硝酸浸出工序 原泥或经预处理后的阳极泥用1∶1硝酸在70～90℃下浸出，固液比1∶2，浸出时间不少于1小时。然后过滤，浸出渣在同样条件下再浸出一次。此时铜、银、硒等转入溶液，而金、铂、锡、锑等留在渣中。浸取可采取二段逆流浸出的方式，以减少硝酸用量。铜、银浸出率均在99%以上。浸出渣用稀硝酸洗涤;浸出液的酸度调节到1N左右作为萃取银的料液。
萃取银工序 萃取有机相采用二异辛基硫醚-煤油体系，其中二异辛基硫醚的含量为40～60%（体积）。萃取时有机相和水相（料液）的体积比为1∶（1～5），两相接触时间1～4分钟，萃取级数3～4级。此时料液中的银以硝酸银硫醚络合物的形式萃入有机相内，而其它贱金属均不被萃取。银的萃取率＞99.9%。
反萃银工序 载银有机相在反萃前为了除去其中机械夹带的水相，用0.5～1N硝酸洗涤1～3次，两相接触1分钟，两相体积比（有机相∶水相）为（1～5）∶1。洗涤时有少量银被洗脱，可回入萃取段中。洗涤后的载银有机相用0.5～1.5N氢氧化铵溶液反萃2～4次，相比为（1～5）∶1，两相每次接触2分钟。此时萃入有机相内的银以银氨络离子形式转入水相。脱银后的有机相用水洗涤1～3次后回到萃取银工序复用。
还原银工序 含银反萃液加热至50～80℃，加入10%水合肼溶液，析出灰白色海绵银粉，陈化0.5～2小时待母液澄清后过渡，沉淀洗至洗水呈中性，干燥后即为纯银产品。纯度＞99.95%。
王水浸金工序 硝酸浸出工序产出的硝酸不溶渣用1∶1王水在60～90℃下溶解，固液比1∶1，浸出时间不少于1小时，金的浸出率＞99.9%。过滤，不溶渣用稀酸洗涤，滤液调节酸度至0.5～1.5N作为萃取金的料液。
萃取金工序 萃取有机相也采用二异辛基硫醚-煤油体系，其中二异辛基硫醚的体积含量为40～50%，相比1∶（1～5），两相接触1分钟，萃取2级。金的萃取率＞99.9%，其它贱金属留在水相残液中。
反萃金工序 载金有机相在反萃前先用0.2～0.5N盐酸洗涤1～2次，除去机械夹带的水相，相比为（1～5）∶1，每次接触0.5～1分钟。反萃用0.5～1N氢氧化钠加0.5～1M亚硫酸钠溶液，相比1∶（2～0.5），两相接触5～20分钟，反萃2次，此时金以亚硫酸根络合物形式转入水相。脱金后的有机相用稀盐酸洗涤后回到萃取金工序复用。
还原金工序 含金反萃液加热至70～80℃，加入盐酸酸化，使亚硫酸盐分解出二氧化硫，此时金即以棕色粉状沉淀析出，陈化1～2小时待溶液澄清后过滤，用稀盐酸及水洗净沉淀，干燥后即为纯金产品，纯度＞99.98%。
氨浸银工序 鉴于阳极泥中的银有少部分以氯化银的形式存在，硝酸和王水浸出时均留在渣中，故王水浸出后的不溶渣用1∶1氨水在室温下浸出2小时以上，固液比为1∶4。此时银以银氨络离子形式转入溶液，过滤后滤液并至还原银工序中。
本流程适用于从各种铜、铅阳极泥以及含银高金低的金银物料中提取金和银，可缩短工艺流程，提高金银收率，减少物料积压。
实施例 称取50克含铜11.5%，含金0.45%，含银8.0%（其中以氯化银形式存在的银为0.6%）的铜电解阳极泥，放入带回流装置的溶解器中加入100毫升1∶1硝酸，加温至80℃左右，搅拌浸出1小时后过滤。一次浸出率银为96%，铜为98.9%。泸液适当稀释，调节酸度至1N左右用4份25毫升60%二异辛基硫醚-煤油依次进行萃取，每次两相接触4分钟。萃残液中残留的总银量为1.9毫克，银的萃取率＞99.9%。载银有机相用0.5N硝酸洗涤3次，每次接触1分钟。洗涤液中共含银94.5毫克，可返回萃取段中回收。洗涤后的有机相用1N氢氧化铵溶液反萃3次，相比（1～5）∶1，视有机相内含银的多少而定。此时银完全转入氨水溶液中，反萃率＞99.9%。脱银有机相用无离子水洗涤2次，相比1∶1，然后可以重复使用。180毫升含银反萃液加热至70～80℃，加入10%水合肼溶液，使银完全沉淀，陈化约半小时溶液澄清后过滤，沉淀用水洗净，干燥，得灰白色纯银粉3.464克，纯度＞99.95%，萃取提取过程实收率＞99%。硝酸浸渣在与前述同样条件下再行浸出，滤液用作下一批物料溶解时的第一次溶解液。经过两段逆流浸出后，银的总浸出率＞99%。用稀硝酸洗涤后的硝酸浸渣在70℃左右用1∶1王水浸金，固液比为1∶1，时间约1小时，金浸出率＞99.9%。不溶渣过滤后用稀盐酸洗净，滤液和洗涤液合并，调节酸度至1N左右，用50%二异辛基硫醚-煤油萃取，相比1∶（1～5），两相接触1分钟，萃取2级，金的萃取率＞99.9%。分相后，含金有机相用0.2N稀盐酸洗涤1次，然后用1M NaOH+1M Na2SO3溶液反萃2次，相比（1～0.5）∶1，两相每次接触5分钟。此时金转入水相，反萃率＞99%。含金反萃液加热至70℃左右，加入盐酸使溶液呈强酸性，析出棕色粉状沉淀，陈化半小时后过滤，洗涤，干燥，得纯金0.222克，实收率＞98%，纯度99.98%。脱金有机相经稀盐酸和水洗涤后复用。
王水不溶渣按固液比1∶2加1∶1氨水在室温下浸出1小时，过滤后用水合肼还原，得灰白色银粉0.295克。
Claims (2)
1、一种从铜电解泥中经酸浸-萃取-反萃-还原提取金、银的工艺，其特征在于先用硝酸浸出银，再用王水浸出金。
2、根据权利要求1所述的从铜电解阳极泥中提取金、银的萃取工艺，其特征在于金、银的萃取剂均为二异辛基硫醚。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85100108.4A CN1004883B (zh) | 1985-04-01 | 1985-04-01 | 从铜电解阳极泥中提取金银的萃取工艺 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85100108A true CN85100108A (zh) | 1986-07-16 |
| CN1004883B CN1004883B (zh) | 1989-07-26 |
Family
ID=4790891
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85100108.4A Expired CN1004883B (zh) | 1985-04-01 | 1985-04-01 | 从铜电解阳极泥中提取金银的萃取工艺 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1004883B (zh) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492965A (zh) * | 2011-12-17 | 2012-06-13 | 山东方泰循环金业股份有限公司 | 铜阳极泥除铜装置及其除铜方法 |
| CN102757022A (zh) * | 2012-06-26 | 2012-10-31 | 湖南华信有色金属有限公司 | 一种从铅阳极泥中提取碲产品和有价金属的工艺 |
| CN103168107A (zh) * | 2010-10-12 | 2013-06-19 | Ls-日光铜制炼株式会社 | 用于从锂二次电池废料中回收有价值金属的方法 |
-
1985
- 1985-04-01 CN CN85100108.4A patent/CN1004883B/zh not_active Expired
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103168107A (zh) * | 2010-10-12 | 2013-06-19 | Ls-日光铜制炼株式会社 | 用于从锂二次电池废料中回收有价值金属的方法 |
| US8945275B2 (en) | 2010-10-12 | 2015-02-03 | Ls-Nikko Copper Inc. | Method for recovering valuable metals from lithium secondary battery wastes |
| CN102492965A (zh) * | 2011-12-17 | 2012-06-13 | 山东方泰循环金业股份有限公司 | 铜阳极泥除铜装置及其除铜方法 |
| CN102757022A (zh) * | 2012-06-26 | 2012-10-31 | 湖南华信有色金属有限公司 | 一种从铅阳极泥中提取碲产品和有价金属的工艺 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1004883B (zh) | 1989-07-26 |
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