CN114752966A - 一种银电解旧液的高效回用方法 - Google Patents
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Abstract
本发明公开了一种银电解旧液的高效回用方法,包括以下步骤:将银电解旧液的pH值调成2~3;向银电解旧液中添加银电解旧液质量分数2~5%的葡萄糖粉;所得的银电解旧液在太阳光或紫外光下照射10~100小时,银电解液中的银离子被还原析出银晶体;然后进行过滤,过滤得到的银粉使用硝酸制备新电解液,过滤后的滤液含少量银离子,使用氯化钠或盐酸对滤液进行沉银,再经过过滤后,滤液进行废水处理,滤渣进行银回收处理。旧电解液回用后,可将旧液中超过90%的银变成银粉重新造液,大大减少了氯化银量,减少了中间槽存,加快了银变现速度。
Description
技术领域
本发明属于稀贵金属湿法冶金领域,具体涉及一种银电解旧液的高效回用方法。
背景技术
电解法是目前银生产企业普遍采用的制银方法,通过电解法制备的银粉可以达到99.9-99.999wt%的纯度,其具有操作简单、试剂消耗少、变现周期短、产品纯度高且稳定、可回收阳极板中的铂族金属等优点。根据上游阳极泥来料特点,富集后的粗银阳极板一般含银约90%以上,其化学成分复杂,在电解过程中,部分杂质元素如钯、铜、铅、硒、碲、铋等会进入溶液,随着电解时间延长,杂质元素积累到一定浓度会在阴极析出进入银粉中,影响电解银粉的纯度。因此,采用电解法制备银粉的过程中,银电解液净化效果不仅直接影响电解银粉质量,也关系到后续电解银粉的加工成本,因此研究高效率的银电解废液循环利用技术显得非常重要。
目前传统的银电解液净化处理或循环利用技术主要包括以下几种方法:(1)氯化钠或盐酸沉淀法,用氯化钠水溶液或盐酸使银电解液废液中的银沉淀为AgCl,达到银与杂质元素分离的效果,AgCl用铁置换成粗银后返回卡尔多炉处 理,或者AgCl直接返入卡尔多炉处理,铸成阳极板再次电解;(2)置换法,用铜置换出废电解液中的银,置换出的粗银粉返入卡尔多炉熔炼成银阳极板再次电解。以上两种方法流程简单,操作方便,但存在收率不高,中间槽存大的缺点;(3)热分解法,利用硝酸与其它贱金属的分解温度不同将其分离,控制一定温度使贱金属硝酸盐分解为氧化物而硝酸银不分解,然后加热水使硝酸银溶解,而贱金属氧化物不溶于水,经固液分离硝酸银溶液可重新使用,贱金属氧化物送火法系统处理。该法存在流程长、操作繁杂、成本高、有安全隐患等缺陷;(4)水解法,用氢氧化钠调节电解液pH值,水解沉淀银电解废液中的杂质元素。利用Ag+与Cu2+、Pb2+、Bi3+、Sb3+水解pH值差异较大的原理,通过添加氢氧化钠和精确控制pH值,使得Cu2+、Pb2+、Bi3+、Sb3+杂质离子水解形成沉淀,而Ag+留在溶液中,从而实现银与杂质元素的分离。目前,水解法已成为银电解废液净化处理应用最广泛的方法。该方法的缺点是银电解液中的钠离子会不断富集,最终影响电解银粉质量,每隔一段时间电解液需更换一次。
发明内容
本发明是针对银电解过程中银电解液中杂质元素不断富集并在阴极析出影响银粉质量的问题,提供一种银电解旧液的高效回用方法,本发明方法具有流程简短,操作简便,环保效果好,循环使用的电解液纯净不含钠盐等优点
本发明采用以下技术方案:
步骤(1):向银电解旧液中加碱调节pH值成2~3;
步骤(2):向步骤(1)所得的银电解旧液中添加葡萄糖粉,添加量为银电解旧液中银离子质量的2%~5%;
步骤(3):将步骤(2)所得的银电解旧液在太阳光或紫外光下照射10~100小时,银电解旧液中的硝酸银发生分解析出银晶体;
步骤(4):将步骤(3)得到的银电解液进行过滤,过滤得到的银粉使用硝酸制备新电解液;过滤后的滤液含少量银离子,使用氯化钠或盐酸对滤液进行沉银,再经过过滤后,滤液进行废水处理,滤渣进行银回收处理。
所述银电解旧液为硝酸银混合溶液,其主要成分为Ag:55~75g/L、Pd:0.10~0.15g/L、Cu:50~55g/L、Fe:0.01~0.02g/L、Se:0.002~0.05g/L、Te:0.010~0.015g/L、Bi:0.0005~0.002 g/L、H+:0.1~0.2 mol/L。
步骤(3)中,太阳光强度为5000lx~100000lx。
步骤(3)中,紫外光波普范围是315~420nm,功率密度为10-80W/cm。
本发明的有益技术效果:
(1)与传统方法相比,该方法收率更高,流程简短。传统的银电解液回收方法常采用氯化沉银法,由于氯化银颗粒细小,部分氯化银投入炉子后飞扬进入排烟管道,导致直收率下降;
(2)该方法利用葡糖糖进行还原硝酸银,生成银单质、葡萄糖酸和二氧化氮气体,该方法可以得到纯净的电解新液,不需要彻底更换所有电解液,传统的水解法处理旧电解液,虽然分离了电解液中的部分杂质元素,但造成电解液中钠离子不断富集,最终影响银粉质量;
(3)与传统方法相比,使用光照或紫外光照射旧电解液析出银的方法更加安全高效。
附图说明
图1为本发明工艺流程图。
具体实施方式
下面结合附图和具体实施例对本发明做进一步解释说明。
实施例1
取废旧电解液3m³进行回收处理。参见表1,废旧电解液化学成分如下:
表1 废旧电解液化学成分
向3m³银电解旧液中加入20kg氢氧化钠,将银电解旧液的pH值调成2.5;向调节了pH值的银电解旧液中添加105公斤葡萄糖粉,并充分搅拌;添加葡萄糖后的银电解旧液在强太阳光下照射50小时(太阳光强度达到20000lx以上),光照过程中银电解液中的硝酸银不断发生分解析出银晶体;银电解液中硝酸银分解完成后进行过滤,过滤得到的166公斤银粉,银粉化学成分如表2 所示。
表2析出银粉化学成分
过滤后的滤液含少量银离子,使用氯化钠或盐酸等对滤液进行沉银,再经过过滤后,滤液进行废水处理,滤渣进行银回收处理。使用回收得到的银粉,再添加硝酸制备新电解液。旧电解液回收处理后,电解液中银的一次回收率达到91%以上。
实施例2
取废旧电解液5m³进行回收处理。参见表3,废旧电解液化学成分如下:
表3 废旧电解液化学成分
向5m³银电解旧液中加入38kg氢氧化钠,将银电解旧液的pH值调成2.7;向调节了pH值的银电解旧液中添加150公斤葡萄糖粉,并充分搅拌;添加葡萄糖后的银电解旧液在强太阳光下照射60小时(太阳光强度达到15000lx以上),光照过程中银电解液中的硝酸银不断发生分解析出银晶体;银电解液中硝酸银分解完成后进行过滤,过滤得到的336公斤银粉,银粉化学成分如表4 所示。
表4析出银粉化学成分
过滤后的滤液含少量银离子,使用氯化钠或盐酸等对滤液进行沉银,再经过过滤后,滤液进行废水处理,滤渣进行银回收处理。使用回收得到的银粉,再添加硝酸制备新电解液。旧电解液回收处理后,电解液中银的一次回收率达到93%以上。
Claims (4)
1.一种银电解旧液的高效回用方法,其特征在于,包括以下步骤:
步骤(1):向银电解旧液中加碱调节pH值成2~3;
步骤(2):向步骤(1)所得的银电解旧液中添加葡萄糖粉,添加量为银电解旧液中银离子质量的2%~5%;
步骤(3):将步骤(2)所得的银电解旧液在太阳光或紫外光下照射10~100小时,银电解旧液中的银离子被还原从而析出银晶体;
步骤(4):将步骤(3)得到的银电解液进行过滤,过滤得到的银粉使用硝酸制备新电解液;过滤后的滤液含少量银离子,使用氯化钠或盐酸对滤液进行沉银,再经过过滤后,滤液进行废水处理,滤渣进行银回收处理。
2.根据权利要求1所述的一种银电解旧液的高效回用方法,其特征在于,步骤(1)中,所述银电解旧液的主要化学成分:Ag:55~75g/L、Pd:0.10~0.15g/L、Cu:50~55g/L、Fe:0.01~0.02g/L、Se:0.002~0.05g/L、Te:0.010~0.015g/L、Bi:0.0005~0.002 g/L、H+:0.1~0.2mol/L。
3.根据权利要求1所述的一种银电解旧液的高效回用方法,其特征在于,步骤(3)中太阳光强度为5000lx~100000lx。
4.根据权利要求1所述的一种银电解旧液的高效回用方法,其特征在于,步骤(3)中,紫外光波谱范围是315~420nm,功率密度为10~80W/cm。
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CN102345140A (zh) * | 2011-08-17 | 2012-02-08 | 嘉兴科菲冶金科技股份有限公司 | 一种从含银废催化剂中电积回收白银的方法 |
US20200130066A1 (en) * | 2018-10-25 | 2020-04-30 | Zhi ZHAO | Photochemical synthesis of dendritic silver particles |
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