CN115584399A - 硫化亚铜在回收水体中Au(III)的应用 - Google Patents
硫化亚铜在回收水体中Au(III)的应用 Download PDFInfo
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- AQMRBJNRFUQADD-UHFFFAOYSA-N copper(I) sulfide Chemical compound [S-2].[Cu+].[Cu+] AQMRBJNRFUQADD-UHFFFAOYSA-N 0.000 title claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000011084 recovery Methods 0.000 title claims abstract description 29
- 239000010931 gold Substances 0.000 claims abstract description 57
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052737 gold Inorganic materials 0.000 claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 35
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 14
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 14
- 150000001879 copper Chemical class 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 7
- 239000012266 salt solution Substances 0.000 claims description 6
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
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- 239000010970 precious metal Substances 0.000 abstract description 3
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- 238000004134 energy conservation Methods 0.000 abstract 1
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- 239000002245 particle Substances 0.000 description 24
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- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 14
- 235000019345 sodium thiosulphate Nutrition 0.000 description 14
- 239000002253 acid Substances 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 239000010949 copper Substances 0.000 description 11
- 238000011068 loading method Methods 0.000 description 11
- 238000010521 absorption reaction Methods 0.000 description 10
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- 238000005303 weighing Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- CBMIPXHVOVTTTL-UHFFFAOYSA-N gold(3+) Chemical compound [Au+3] CBMIPXHVOVTTTL-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 238000010146 3D printing Methods 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 235000010204 pine bark Nutrition 0.000 description 1
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- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
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- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
Classifications
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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Abstract
本发明公开硫化亚铜在回收水体中Au(III)的应用,属于湿法冶金、贵金属回收领域。本发明所述方法使用硫化亚铜纳米粒子回收溶液中的Au(III),在机械搅拌下进行金吸附;本发明所述方法可高效回收水溶液中的Au(III),对酸性废液中Au(III)的回收具有较好回收效果,且具有节能环保,成本低廉等优点。
Description
技术领域
本发明涉及硫化亚铜在回收水体中Au(III)的应用,属于湿法冶金、贵重金属回收领域。
背景技术
黄金是一种贵金属,因其具有优异的导电性、导热性,良好的耐腐蚀性,使其被广泛应用在航空航天、医疗、催化、电子器件等领域,对我国经济发展和科技进步具有关键性作用。但目前黄金行业面临困局,比如:(1)虽然黄金产量逐年增加,但产量远低于消耗量,生产成本高昂;(2)供应缺口较大且金矿石品位日趋贫化,多为难处理矿石;(3)相当一部分黄金分布于印刷电路板、废催化剂、电镀残液等二次资源中,造成黄金资源的浪费。
对于二次资源中黄金的回收,混酸浸出具有显著优势:(1)Cl-、Br-等低价卤素可与金形成稳定配合物,且浸金速率更快,浸出条件更易控,溶液组分更简单,作为浸出剂的挥发性酸可循环使用;(2)二次黄金资源具有金品位高,体积小等特点,可置于具有极好耐酸性的含氟材料容器中浸出。然而浸出液中含有金(AuX4 -)及其它共存金属离子,需要对金进行分离与富集。相对而言,吸附法具有明显优势:(1)吸附剂具有一定尺寸和硬度,残液易于分离。所以,找到合适的解吸方法,则可在回收金的同时实现吸附剂循环使用,达到节约成本,减少资源浪费的目的。
目前,对于废旧电路板、催化剂、工业废水等二次黄金资源浸出液中Au(III)的富集分离,有多种新型吸附材料被报道。对于酸性溶液中的金(AuCl4 -或AuBr4 -),活性炭用作吸附剂被广泛报道,但是活性炭的负载能力和吸附选择性有限,故回收成本较高。也有研究报道,用松皮单宁树脂、氧化石墨烯、3 D打印Scavenger材料、Diaion WA21J型离子交换树脂、泡沫塑料等可实现较好金吸附效果,使金吸附量达到50 kg/t以上。上述新材料均可用于溶液中AuX4 -的吸附回收,但材料多为有机合成材料,存在价格相对高昂、制备工艺复杂,易粉化等问题,难以在实际工业中推广应用。
发明内容
本发明的目的在于提供一种硫化亚铜在回收水体中Au(III)的应用,具体为将硫化亚铜加入到含有Au(III)的水体中对金进行吸附;其具有操作简单、工艺性强等优势。
优选的,本发明所述含有Au(III)的水体的pH值为1-5,实验发现在酸性条件下,硫化亚铜能稳定存在,且对金(III)的吸附效果更好。
优选的,本发明所述硫化亚铜的制备方法为:按铜盐与硫代硫酸盐的浓度比为1:2~1:10的比例将铜盐溶液和硫代硫酸盐溶液混合反应完成,离心,烘干即得到所需硫化亚铜。
优选的,本发明所述铜盐溶液为硫酸铜溶液或者氯化铜溶液,铜盐溶液的浓度为1-15mmol/L。
优选的,本发明所述硫代硫酸盐的浓度为2-120mmol/L。
本发明以自制硫化亚铜纳米颗粒为Au(III)的吸附剂,因硫化亚铜具有热稳定性,不溶于水、丙酮、硫化铵、稀硫酸和稀盐酸等介质,在酸性条件下能稳定存在,故对金溶液有较强的适用性;且硫化亚铜纳米颗粒可采用合适的稳定剂简易调控其结构和尺寸,增强其吸附性能,故具有成本可控的优势,适宜于含金酸性废液的回收富集。
本发明的有益效果为:
(1)本发明所述金回收方法工艺简单,成本低,金的回收率高。
(2)制备得到的硫化亚铜(Cu2S)适应吸附溶液的pH范围较广,硫化亚铜在1≤pH≤5的范围内均有很好吸附效果。
(3)所用硫酸铜的浓度在15mmol/L以内,硫代硫酸钠的浓度在120 mmol/L以内,试剂需求量低,具有一定工业应用价值。
具体实施方式
下面结合具体实施方式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
本实施例采用一定浓度硫酸铜溶液和硫代硫酸钠溶液在机械搅拌下制备得到硫化亚铜纳米微粒,用于吸附水溶液中的Au(III);包括以下步骤:
(1)称取颗粒状硫酸铜0.025 g(1mmol/L),加入80mL去离子水溶解,备用。
(2)称取硫代硫酸钠0.05 g(2mmol/L),加入20mL去离子水溶解,备用。
(3)将步骤(2)中硫代硫酸钠溶液加入到(1)中硫酸铜溶液中(总体积为100mL),在200转/分钟的转速下机械搅拌24h;搅拌结束后,离心过滤所得固体微粒,置于60℃烘箱中干燥12h后取出备用。
(4)将步骤(3)中烘干的硫化亚铜(Cu2S)加入到浓度为5mg/L的四氯合金酸(HAuCl4)溶液中进行搅拌吸附;pH值为1,吸附24 h后,取样并用原子吸收分析金浓度,回收率达到100 %,负载量为33.33kg/t。
实施例2
(1)称取颗粒状硫酸铜0.050 g(2mmol/L),加入80mL去离子水溶解,备用。
(2)称取硫代硫酸钠0.496 g(20mmol/L),加入20mL去离子水溶解,备用。
(3)将步骤(2)中硫代硫酸钠溶液加入到(1)中硫酸铜溶液中(总体积为100 mL),在200转/分钟的转速下机械搅拌24 h;搅拌结束后,离心过滤所得固体微粒,置于60 ℃烘箱中干燥12 h后取出备用。
(4)将步骤(3)中烘干的硫化亚铜(Cu2S)加入到浓度为10 mg/L的四氯合金酸(HAuCl4)溶液中,进行搅拌吸附;pH值为2,吸附24 h后,取样并用原子吸收分析金浓度,回收率达到100 %,负载量为50 kg/t。
实施例3
(1)称取颗粒状硫酸铜0.125 g(5mmol/L),加入80mL去离子水溶解,备用。
(2)称取硫代硫酸钠0.372 g(15mmol/L),加入20mL去离子水溶解,备用。
(3)将步骤(2)中硫代硫酸钠溶液加入到(1)中硫酸铜溶液中(总体积为100 mL),在200转/分钟的转速下机械搅拌24 h;搅拌结束后,离心过滤所得固体微粒,置于60 ℃烘箱中干燥12 h后取出备用。
(4)称取步骤(3)中烘干的硫化亚铜(Cu2S) 0.01 g,加入到浓度为20 mg/L的四氯合金酸(HAuCl4)溶液中,进行吸附搅拌;pH值为5,吸附24 h后,取样并用原子吸收分析金浓度,回收率达到100 %,负载量为200 kg/t。
实施例4
(1)称取颗粒状氯化铜0.136g(8mmol/L),加入80mL去离子水溶解,备用。
(2)称取硫代硫酸钠0.620 g(25mmol/L),加入20mL去离子水溶解,备用。
(3)将步骤(2)中硫代硫酸钠溶液加入到(1)中氯化铜溶液中(总体积为100 mL)在200转/分钟的转速下机械搅拌24 h;搅拌结束后,离心过滤所得固体微粒,置于60 ℃烘箱中烘12 h后取出备用。
(4)称取步骤(3)中烘干的硫化亚铜(Cu2S) 0.01 g加入到浓度为50 mg/L的四氯合金酸(HAuCl4)溶液中,进行搅拌吸附;pH值为4,吸附24 h后,取样并用原子吸收分析金浓度,回收率达到100 %,负载量为500 kg/t。
实施例5
(1)称取颗粒状硫酸铜0.250 g(10mmol/L),加入80mL去离子水溶解,备用。
(2)称取硫代硫酸钠1.000 g(40mmol/L),加入20mL去离子水溶解,备用。
(3)将步骤(2)中硫代硫酸钠溶液加入到(1)中硫酸铜溶液中(总体积为100 mL)在200转/分钟的转速下机械搅拌24 h;搅拌结束后,离心过滤所得固体微粒,置于60 ℃烘箱中烘12 h后取出备用。
(4)称取步骤(3)中烘干的硫化亚铜(Cu2S) 0.01g加入到浓度为100 mg/L的四氯合金酸(HAuCl4)溶液中,进行搅拌吸附;pH值为3,吸附24 h后,取样并用原子吸收分析金浓度,回收率达到100 %,负载量为1000 kg/t。
实施例6
(1)称取颗粒状硫酸铜0.375 g(15mmol/L),加入80mL去离子水溶解,备用。
(2)称取硫代硫酸钠2.98 g(120mol/L),加入20mL去离子水溶解,备用。
(3)将步骤(2)中硫代硫酸钠溶液加入到(1)中硫酸铜溶液中(总体积为100 mL)在200转/分钟的转速下机械搅拌24 h;搅拌结束后,离心过滤所得固体微粒,置于60 ℃烘箱中干燥12 h后取出备用。
(4)称取步骤(3)中烘干的硫化亚铜(Cu2S) 0.01 g加入到浓度为200 mg/L的四氯合金酸(HAuCl4)溶液中,进行搅拌吸附;pH值为4,吸附24 h后,取样并用原子吸收分析金浓度,回收率达到100 %,负载量为2000 kg/t。
实施例7
市售硫化亚铜对金(III)的吸附性能研究
(1)称取市售硫化亚铜(Cu2S) 0.01 g(硫化亚铜购自罗恩试剂,纯度为99%)。
(2)将步骤(1)中的硫化亚铜加入到浓度为200 mg/L的四氯合金酸(HAuCl4)溶液中,进行搅拌吸附;pH值为4,吸附24 h后,取样并用原子吸收分析金浓度,回收率达到78 %,负载量为1560 kg/t。
实施例8
(1)在30 mL EDA(乙二胺)中加入颗粒状氯化铜0.170 g (10 mmol/L),在磁力搅拌下溶解,备用。
(2)称取0.23 g (0.03mol/L)硫脲,加入到步骤(1)的混合溶液中,继续搅拌2 h。
(3)将步骤(2)中混合溶液倒入50mL聚四氟乙烯反应釜中,温度保持在60℃,8 h;冷却后用蒸馏水和乙醇洗涤5-8次固体微粒,并置于60 ℃烘箱中干燥10 h得到硫化亚铜。
(4)称取步骤(3)中烘干的硫化亚铜(Cu2S) 0.01 g加入到浓度为200 mg/L的四氯合金酸(HAuCl4)溶液中,进行搅拌吸附;pH值为4,吸附24 h后,取样并用原子吸收分析金浓度,回收率达到80 %,负载量为1600 kg/t。
实施例9
(1)在30 mL EDA(乙二胺)中加入颗粒状氯化铜0.170 g (10 mmol/L),在磁力搅拌下溶解,备用。
(2)称取0.23 g (0.03mol/L)硫脲,加入到步骤(1)的混合溶液中,继续搅拌2 h。
(3)将步骤(2)中混合溶液倒入50mL聚四氟乙烯反应釜中,温度保持在80℃,8 h;冷却后用蒸馏水和乙醇洗涤5-8次固体微粒,并置于60 ℃烘箱中干燥10 h得到硫化亚铜。
(4)称取步骤(3)中烘干的硫化亚铜(Cu2S) 0.01 g加入到浓度为200 mg/L的四氯合金酸(HAuCl4)溶液中,进行搅拌吸附;pH值为4,吸附24 h后,取样并用原子吸收分析金浓度,回收率达到87 %,负载量为1740 kg/t。
实施例10
(1)在30 mL EDA(乙二胺)中加入颗粒状氯化铜0.170 g (10 mmol/L),在磁力搅拌下溶解,备用。
(2)称取0.23 g (0.03mol/L)硫脲,加入到步骤(1)的混合溶液中,继续搅拌2 h。
(3)将步骤(2)中混合溶液倒入50mL聚四氟乙烯反应釜中,温度保持在100℃,8h;冷却后用蒸馏水和乙醇洗涤5-8次固体微粒,并置于60℃烘箱中干燥10 h得到硫化亚铜。
(4)称取步骤(3)中烘干的硫化亚铜(Cu2S) 0.01 g加入到浓度为200 mg/L的四氯合金酸(HAuCl4)溶液中,进行搅拌吸附;pH值为4,吸附24 h后,取样并用原子吸收分析金浓度,回收率达到84 %,负载量为1680 kg/t。
以上对本发明的具体实施方式作了详细说明,但是本发明并不限于上述实施方式,在本领域普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下作出各种变化。
Claims (6)
1.硫化亚铜在回收水体中Au(III)的应用。
2.根据权利要求1所述硫化亚铜在回收水体中Au(III)的应用,其特征在于:将硫化亚铜加入到含有Au(III)的水体中对金进行吸附。
3.根据权利要求1所述硫化亚铜在回收水体中Au(III)的应用,其特征在于:所述含有Au(III)的水体的pH值为1-5。
4.根据权利要求1~3任意一项所述硫化亚铜在回收水体中Au(III)的应用,其特征在于:所述硫化亚铜的制备方法为:按铜盐与硫代硫酸盐的浓度比为1:2~1:10的比例将铜盐溶液和硫代硫酸盐溶液混合反应完成,离心,烘干得到所需硫化亚铜。
5.根据权利要求4所述硫化亚铜在回收水体中Au(III)的应用,其特征在于:铜盐溶液为硫酸铜溶液或者氯化铜溶液,铜盐溶液的浓度为1-15mmol/L。
6.根据权利要求4所述硫化亚铜在回收水体中Au(III)的应用,其特征在于:硫代硫酸盐的浓度为2-120mmol/L。
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