CN109589951B - 一种用于回收溶液中金硫代硫酸根络离子的活性炭的制备方法 - Google Patents
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Abstract
本发明公开一种用于回收溶液中金硫代硫酸根络离子的活性炭的制备方法，属于贵金属回收技术领域，本发明所述方法为：称取活性炭，用去离子水洗涤除去活性炭的灰分，过滤、烘干；将活性炭放在浓度为0.05g/L~50g/L的改性溶液中于常温下搅拌浸渍，过滤干燥后得到改性活性炭；所述改性溶液为1‑甲基‑5‑巯基四氮唑溶液、1‑苯基‑5‑巯基四氮唑溶液或者这两者按任意比例混合得到的混合溶液。本发明所述方法制备的活性炭能回收溶液中的金（Au(S2O3)2 3‑），这种改性活性炭对金的最大负载量可达25.479kg/t（MMT）。本发明所述方法具有工艺简单，多余改性试剂可以回收利用，不涉及任何含氰根或重金属化学物质，无有毒有害物质外排的优点。
Description
技术领域
本发明涉及一种用于回收溶液中（Au(S2O3)2 3-）的活性炭的制备方法，属于贵重金属回收技术领域。
背景技术
在黄金提取领域，全世界目前大都采用氰化法提取黄金，但是由于氰化法中使用剧毒的氰化物，对生态环境和人类的潜在危害不可估量。近年来，大多国家和地区对氰化法提金实施了严格的管制，一些国家已经命令禁止使用氰化法提金。金矿品位的降低增加了试剂成本，再加上其他方面投入，使得氰化提金法入不敷出，举步维艰，整个黄金行业将面临空前的挑战。
硫代硫酸盐提金因具有浸金速度快、无毒、环保，易于处理氰化法难处理的复杂金矿石以及对设备无腐蚀等优点而被认为是最有产业化应用前景的非氰提金技术。但金矿中的金通过硫代硫酸盐浸出以后以（Au(S2O3)2 3-）离子的形式存在于溶液中。活性炭对Au(S2O3)2 3－的吸附能力极低，无法采用氰化提金中常用的 CIP方法进行黄金提取，因此限制了该技术的推广。为了使炭浆法可以应用到硫代硫酸盐提金体系中，找到有效的活性炭改性方法对硫代硫酸盐提金方法的实际应用和推广具有重要意义。
为了提高活性炭对Au(S2O3)2 3－的吸附能力，专利（US 8,500,847 B2）在活性炭上负载铜氰络离子，然后利用相关离子与金交换对[Au(S2O3)2]3-进行吸附，取得了一定成效。但是这种改性方法需要控制铜氰比例因而工艺比较复杂，外加在其改性过程涉及到一定量的含氰物质。因此，难以达到彻底的非氰无毒这一标准。
专利（CN 104549147 A）在活性炭上负载无毒无害的类普鲁士蓝化合物，明显改善了活性炭对硫代硫酸盐体系中金的吸附能力，但其改性过程较为复杂无法满足实际应用。
发明内容
本发明的目的在于提供一种用于回收溶液中（Au(S2O3)2 3-）（金硫代硫酸根络离子）的活性炭的制备方法，具体包括以下步骤：
（1）称取活性炭，用去离子水洗涤除去活性炭的灰分，过滤、烘干。
（2）将步骤（1）得到的活性炭放在浓度为0.05g/L ~ 50g/L的改性溶液中，于常温下搅拌浸渍，过滤干燥后得到改性活性炭。
所述改性溶液为1-甲基-5-巯基四氮唑（MMT）溶液、1-苯基-5-巯基四氮唑（PMT）溶液或者这两者按任意比例混合得到的混合溶液。
优选的，本发明步骤（2）中浸渍时间为0.5 h ~ 72 h。
优选的，本发明浸渍过程中改性溶液与活性炭的液固比为1 ~100。
本发明的有益效果为：
（1）本发明所述活性炭的改性方法工艺简单，不需要焙烧处理，使得改性成本低，金的回收率高。
（2）改性过程中所用1-甲基-5-巯基四氮唑或1-苯基-5-巯基四氮唑改性溶液可回收再次利用，不排放有毒有污染物质，对环境无有害影响。
（3）改性后的活性炭适应吸附溶液的pH范围较广，活性炭在pH≥6的范围内均有很好吸附效果；负载量高，整个改性过程中不使用或外排任何含氰根（CN-）或重金属等有毒物质。
（4）改性所得活性炭可连续使用，多次吸附后仍能保持较好的吸附效果。
具体实施方式
下面结合和具体实施例对本发明作进一步详细说明，但本发明的保护范围并不限于所述内容。
实施例1
一种用于回收溶液中（Au(S2O3)2 3-）的活性炭的制备方法，具体包括以下步骤：
（1）取10g颗粒状活性炭，用去离子水洗涤，去除粉末灰尘，过滤，40℃下烘12h。
（2）按改性溶液与活性炭的液固比为2的比例将步骤（1）得到的活性炭放在浓度为0.05g/L的改性溶液中，于常温下搅拌浸渍24 h，过滤后60℃下烘12 h得到改性活性炭；所述改性溶液为1-苯基-5-巯基四氮唑溶液。
取0.5g本实施例制备得到的活性炭加入到100mL含有硫代硫酸合金（Ⅰ）络离子（Au(S2O3)2 3-）溶液（简称吸附液）中，Au(S2O3)2 3-浓度为127ppm，pH值为7，吸附9天后，吸附率为60.2%，负载量为15.291 kg/t。
实施例2
一种用于回收溶液中（Au(S2O3)2 3-）的活性炭的制备方法，具体包括以下步骤：
（1）取4g粉末活性炭，用去离子水洗涤，过滤，110℃下烘1h。
（2）按改性溶液与活性炭的液固比为5的比例将步骤（1）得到的活性炭放在浓度为50g/L的改性溶液中，于常温下搅拌浸渍48h，然后将上清液倾出，去离子水洗后，过滤，80℃下烘12h得到改性活性炭；所述改性溶液为1-甲基-5-巯基四氮唑和1-苯基-5-巯基四氮唑的混合溶液，混合溶液中PMT的MMT质量比为1:1。
取0.5g本实施例制备得到的活性炭加入到100mL模拟的含有硫代硫酸合金（Ⅰ）络离子（Au(S2O3)2 3-）溶液中，其中含Au(S2O3)2 3-浓度为154.05ppm，pH值为6，吸附9天后，吸附达到饱和，吸附率为82.7%，饱和负载量达到了25.479kg/t。
实施例3
一种用于回收溶液中（Au(S2O3)2 3-）的活性炭的制备方法，具体包括以下步骤：
（1）取2g颗粒状椰壳活性炭用去离子水洗净，过滤，110℃下烘1h。
（2）按改性溶液与活性炭的液固比为100的比例将步骤（1）得到的活性炭放在浓度为25g/L的改性溶液中，于常温下搅拌浸渍6 h，然后将上清液倾出，用去离子水洗涤、过滤，60℃下烘12h得到改性活性炭，所述改性溶液为1-甲基-5-巯基四氮唑和1-苯基-5-巯基四氮唑的混合溶液，混合溶液中PMT的MMT质量比为1:10。
以某含金约为2.67g/t的矿石浸出液为例，浸出液中含有二硫代硫酸合金(Ⅰ)（Au(S2O3)2 3-）的浓度为12mg/L，含Cu2+浓度为5mmol/L，含NH3/NH4 +浓度为3 mol/L，pH为11；取1g本实施例所得活性炭加入到100mL硫代硫酸盐的浸出液中，常温搅拌吸附48小时后过滤，该活性炭吸附金的回收率为100%，负载量为1.2kg/t。
实施例4
一种用于回收溶液中（Au(S2O3)2 3-）的活性炭的制备方法，具体包括以下步骤：
（1）取5g颗粒状椰壳活性炭用去离子水洗涤，去除粉末灰尘，过滤，110℃下烘1h。
（2）按改性溶液与活性炭的液固比为40的比例将步骤（1）得到的活性炭放在浓度为10g/L的改性溶液中，于常温下搅拌浸渍72 h，然后将上清液倾出，去离子水洗涤后30℃下烘12h得到改性活性炭；所述改性溶液为1-甲基-5-巯基四氮唑溶液。
取1g本实施例制备得到的活性炭加入到100mL含有硫代硫酸合金（Ⅰ）络离子（Au(S2O3)2 3-）溶液中，Au(S2O3)2 3-浓度为12.484ppm，pH值为9，吸附24小时后，滤出活性炭放入下一个同样的的吸附液中，共重复吸附五次；第一次吸附率为96.6%；第二次为72.8%；第三次为56.56%；第四次为43.19%；第五次为44.44%；总负载量为3.915kg/t。
Claims (3)
1.一种用于回收溶液中金硫代硫酸根络离子的活性炭的制备方法，其特征在于，具体包括以下步骤：
（1）称取活性炭，用去离子水洗涤除去活性炭的灰分，过滤、烘干；
（2）将步骤（1）得到的活性炭放在浓度为0.05g/L ~ 50g/L的改性溶液中，于常温下搅拌浸渍，过滤干燥后得到改性活性炭；
所述改性溶液为1-甲基-5-巯基四氮唑溶液、1-苯基-5-巯基四氮唑溶液或两者按任意比例混合得到的混合溶液。
2.根据权利要求1所述方法，其特征在于：步骤（2）中浸渍时间为0.5 h ~ 72 h。
3.根据权利要求1所述方法，其特征在于：浸渍过程中改性溶液与活性炭的液固比为1~100。
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| CN109825702B (zh) * | 2019-04-18 | 2021-04-23 | 中国有色桂林矿产地质研究院有限公司 | 用活性炭从连多硫酸盐浸金贵液中富集回收金的方法 |
| CN109930009B (zh) * | 2019-04-18 | 2021-04-13 | 中国有色桂林矿产地质研究院有限公司 | 用活性炭从含硫无氰浸金贵液中富集回收金的方法 |
| CN111004922A (zh) * | 2019-12-12 | 2020-04-14 | 昆明理工大学 | 一种回收硫代硫酸盐体系中金的方法 |
| CN111841492A (zh) * | 2020-06-19 | 2020-10-30 | 昆明理工大学 | 一种用于吸附回收[Au(S2O3)2]3-离子的炭质材料的制备方法 |
| CN111889068A (zh) * | 2020-06-19 | 2020-11-06 | 昆明理工大学 | 一种用于吸附回收[Au(S2O3)2]3-络离子的活性炭的改性方法 |
| CN112375919B (zh) * | 2020-11-02 | 2022-07-08 | 昆明理工大学 | 一种直接回收硫代硫酸盐体系中金的方法 |
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