WO2023097923A1 - 一种低成本贵金属离子选择性沉淀的还原剂 - Google Patents

一种低成本贵金属离子选择性沉淀的还原剂 Download PDF

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WO2023097923A1
WO2023097923A1 PCT/CN2022/080535 CN2022080535W WO2023097923A1 WO 2023097923 A1 WO2023097923 A1 WO 2023097923A1 CN 2022080535 W CN2022080535 W CN 2022080535W WO 2023097923 A1 WO2023097923 A1 WO 2023097923A1
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gold
noble metal
palladium
platinum
reducing agent
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PCT/CN2022/080535
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French (fr)
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俞嘉梅
郭嘉琪
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北京工业大学
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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
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the invention belongs to the technical field of recycling waste resources and relates to a new reducing agent for selective precipitation of noble metal (gold, platinum, palladium) ions in water.
  • precious metals gold, platinum, palladium
  • precious metals have extremely low abundance on earth, and their rarity and high price greatly limit their further commercial development and application in various fields.
  • the demand for precious metals has increased dramatically in recent years, with demand far exceeding supply.
  • the waste containing precious metals is not fully treated effectively, resulting in a large amount of precious metals being left in the waste.
  • Solids are Potential source of secondary precious metal resources.
  • metal leachate and waste processing fluid which are aqueous solutions containing large amounts of noble metal ions.
  • reagents such as hydrochloric acid, hydrochloric acid-chloride, aqua regia, and thiosulfuric acid have been applied, such as extracting precious metals from copper anode sludge, waste light-emitting diodes, and waste printed circuit boards.
  • concentration of noble metal ions in the metal leach solution usually ranges from 2 to 1000 mg/L, usually higher than other coexisting elements such as Fe(III), Cu(II), Ni(II), Zn(II), Pb(II), and Al(III) is several orders of magnitude smaller.
  • waste processing fluids are generated, including waste rinse water, electroplating solutions, etchant, etc.
  • waste processing fluids typically contain 15 to 5800 mg/L of noble metal ions, which may be greater, compatible, or less than the concentration of other coexisting elements such as Al(III), Cu(II), Ni(II), Zn( II) and Sn(IV), etc. How to separate noble metal ions from these coexisting ions is the core of the research.
  • ideal adsorbents should meet the following conditions: large surface area; high adsorption capacity and selectivity; high chemical and mechanical stability; easy separation, regeneration, and reuse; and high cost-effectiveness.
  • large surface area high adsorption capacity and selectivity
  • high chemical and mechanical stability high chemical and mechanical stability
  • easy separation, regeneration, and reuse and high cost-effectiveness.
  • no suitable ideal adsorbent has been found yet.
  • the purpose of the present invention is to selectively reduce and precipitate noble metal ions in a solution containing noble metal by using a simple, effective and low-cost reducing agent to obtain simple noble metal.
  • the reducing agent used in the present invention is one or more of amide organic compounds (such as N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMA) etc.), ethanol and methanol kind.
  • amide organic compounds such as N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMA) etc.
  • ethanol and methanol kind.
  • the method for selectively reducing the precious metal ions in the solution containing the precious metal to obtain the simple substance of the precious metal is as follows:
  • the above method is used to selectively reduce and precipitate noble metals from a solution containing noble metal ions and coexisting ions such as copper ions, aluminum ions, nickel ions, and tin ions to obtain noble metal elements.
  • the oxidation-reduction potentials of gold, platinum, and palladium in noble metals are all higher than those of other common metals (such as copper, aluminum, nickel, tin) in the noble metal-containing solution.
  • the higher the potential the stronger the oxidation and the easier the redox reaction.
  • amide organic compounds such as N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMA), etc.
  • ethanol and methanol are all reducing, and can be compared with The redox reaction of precious metals occurs, so the precious metals can be selectively precipitated in the solution.
  • Beneficial effects of the present invention almost all precious metal (gold, platinum, palladium) ions in the liquid containing precious metal can be reduced to precious metal simple substance, and then separated by filtration to obtain precious metal simple substance for recycling, which greatly shortens the recovery time of precious metal process flow.
  • Adopting the reducing agent of the present invention can obtain the highest gold recovery rate of 98.3%, the palladium recovery rate of 95.4%, and the platinum recovery rate of 94.6%, and the purity is all above 98.5% after testing.
  • the reducing agent used is easy to obtain, the price is low, the method is simple, the application cost is reduced, and large-scale production is easy to realize.
  • reducing agent amide organic compound (such as N, N-dimethylformamide (DMF), N, N-dimethylacetamide (DMA) etc.), ethanol and methanol ) is used in an amount of 30% to 80% of the amount of the solution containing noble metal ions, but the present invention is not limited to the following examples.
  • Example 1 according to the proportioning configuration gold ion solution of Au concentration 260.16mg/L, Cu concentration 203.52mg/L, Ni concentration 180.83mg/L, Al concentration 187.83mg/L, Sn concentration 198.04mg/L, get 100mL configuration solution in the bottle, add 40mL N,N-dimethylformamide (DMF), seal it, place it in a 50-degree oven and heat it for 7 hours. After 7 hours, a precipitate appears at the bottom of the bottle. After filtering, X-ray diffractometer (XRD ) was tested, which was consistent with the powder diffraction pattern of gold elemental substance. After the reaction, the supernatant was taken and tested by an inductively coupled plasma spectrometer (ICP). The results showed that the gold precipitation rate was 98.3%.
  • XRD X-ray diffractometer
  • Example 2 according to the proportioning configuration of Pd concentration 99.23mg/L, Cu concentration 203.52mg/L, Ni concentration 180.83mg/L, Al concentration 187.83mg/L, Sn concentration 198.04mg/L containing palladium ion solution, get 100mL configuration solution in the bottle, add 50mL N,N-dimethylacetamide (DMA), seal it, place it in a 60-degree oven and heat it for 10 hours. After 10 hours, a precipitate appears at the bottom of the bottle. After filtering, X-ray diffractometer (XRD ) to test, it is consistent with the powder diffraction pattern of palladium simple substance. After the reaction, the supernatant was taken for an inductively coupled plasma spectrometer (ICP) test, and the results showed that the palladium precipitation rate was 95.4%.
  • XRD X-ray diffractometer
  • Example 3 according to the proportioning configuration of Pt concentration 130.46mg/L, Cu concentration 203.52mg/L, Ni concentration 180.83mg/L, Al concentration 187.83mg/L, Sn concentration 198.04mg/L containing platinum ion solution, get 100mL configuration Put the solution in the bottle, add 40mL of ethanol, seal it, place it in a 60-degree oven and heat it for 8 hours. After 8 hours, a precipitate appears at the bottom of the bottle. After filtering, X-ray diffractometer (XRD) is used for testing, which is in line with the powder diffraction pattern of platinum. . After the reaction, the supernatant was taken for an inductively coupled plasma spectrometer (ICP) test, and the results showed that the platinum precipitation rate was 87.8%.
  • ICP inductively coupled plasma spectrometer
  • Example 4 according to the proportioning configuration of Au concentration 260.16mg/L, Pd concentration 99.23mg/L, Cu concentration 203.52mg/L, Ni concentration 180.83mg/L, Al concentration 187.83mg/L, Sn concentration 198.04mg/L Gold palladium ion solution, take 100mL of the prepared solution in the bottle, add 40mL N,N-dimethylformamide (DMF), seal it, place it in a 50-degree oven and heat it for 7 hours. After a precipitate appears at the bottom of the bottle, filter it Carry out X-ray diffractometer (XRD) to test afterward, accord with the powder diffraction pattern of simple gold. The supernatant after the reaction was taken and tested by an inductively coupled plasma spectrometer (ICP). The results showed that the gold precipitation rate was 96.7%, and the palladium precipitation rate was 91.2%.
  • XRD X-ray diffractometer

Abstract

一种低成本贵金属离子选择性沉淀的还原剂，属于废弃物资源化回收技术领域。本发明通过一种简单有效、低成本的还原剂将含贵金属(金、铂、钯)溶液中贵金属(金、铂、钯)离子选择性还原沉淀出来，得到贵金属(金、铂、钯)单质。利用了氧化还原反应的基本原理，基于贵金属(金、铂、钯)的氧化还原电位比一般金属更高这一特性，使用有机还原剂选择性将废液中贵金属(金、铂、钯)离子还原为单质，进而通过过滤将其分离出来，实现回收利用，方法简单，缩短了贵金属(金、铂、钯)回收的工艺流程。所使用的还原剂方便易得，价格低廉，降低了应用成本，易于实现规模化生产。

Description

一种低成本贵金属离子选择性沉淀的还原剂 技术领域
本发明属于废弃物资源化回收技术领域，一种水中贵金属(金、铂、钯)离子选择性沉淀的新还原剂。
背景技术
金(Au)、铂(Pt)、钯(Pd)作为具有优良物理与化学性质的贵金属，对许多高科技产业来说是必不可少的，因为它们可以作为催化剂、电子产品、燃料电池、医药的原材料，它们也是为人熟知的高档饰品，具有极高的经济价值。然而，贵金属(金、铂、钯)在地球上的丰度极低，其稀有性和高价性大大限制了它的进一步商业开发和在各个领域的应用。一方面，近年来对贵金属的需求急剧增加，需求远远超过了供应。另一方面，因回收技术限制，没有充分将含贵金属的废物进行有效处理，导致大量贵金属被留存在废物中。研究人员也正在寻找新的替代品来解决当前的困境，然而，寻找贵金属的替代品将是一个漫长的过程，且它们的实际性能需要在实践中检验。因此，迫切需要探索更有效的技术，从二次资源中回收贵金属，以解决目前的问题。
固体(电子和珠宝废料、废催化剂和牙科材料、阳极泥、矿渣、粉煤灰等)、液体(金属浸出液、废加工液、工业废水等)或泥浆(污水污泥、矿山尾矿等)是潜在的二次贵金属资源的来源。贵金属离子的两个重要液体来源是金属浸出液和废加工液，它们是含有大量贵金属离子的水溶液。对于固体中贵金属浸出而言，盐酸、盐酸-氯化物、王水和硫代硫酸等试剂已被应用，如从铜阳极污泥、废发光二极管和废印刷电路板中提取贵金属。金属浸出液中的贵金属离子浓度通常为2至1000毫克/升不等，通常比其他共存元素如Fe(III)、Cu(II)、Ni(II)、Zn(II)、Pb(II)、和Al(III)小几个数量级。同时，在工业流程中，如半导体和印刷电路板制造、黄金熔化、电镀和蚀刻等，会产生各种废加工液，其中包括废冲洗水、电镀液和蚀刻剂等。与金属浸出液不同，废加工液通常含有15至5800毫克/升的贵金属离子，可能大于、兼容或小于其他共存元素的浓度，如Al(III)、Cu(II)、Ni(II)、Zn(II)和Sn(IV)等。如何将贵金属离子从这些共存离子中分离出来是研究的核心。
如今有几种回收含贵金属液体中贵金属离子的方法，如溶剂萃取、离子交换 和吸附。各有优劣，且都不尽完美。溶剂萃取法需要使用大量危险的有机溶剂，容易污染环境，而且由于需要多个萃取步骤，需要较长的时间。离子交换法虽然便宜、简单、环保，但同样分离周期长，难以洗脱。吸附法因其优异的性能和低廉的生产成本，被认为是回收溶液中贵金属离子的一种有效而经济的技术。一般来说，理想的吸附剂应满足以下条件：大的表面积；高的吸附能力和选择性；高的化学和机械稳定性；易于分离、再生和再利用；成本效益高。但是目前还没有合适的理想吸附剂被发现。
发明内容
本发明的目的是通过一种简单有效、成本低的还原剂将含贵金属溶液中贵金属离子选择性还原沉淀出来，得到贵金属单质。
本发明使用的还原剂是酰胺类有机化合物(例如N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMA)等)、乙醇和甲醇中的一种或几种。
本发明将含贵金属溶液中贵金属离子选择性还原出来，得到贵金属单质的方法如下：
(1)向含贵金属离子溶液中加入不超过溶液体积的还原剂。
(2)将盛有如上液体的容器密封，放入50-70℃烘箱中，加热保温6-10小时，即可得到贵金属单质。
上述方法用于将贵金属从含有贵金属离子和共存离子如铜离子、铝离子、镍离子、锡离子中的的溶液中选择性还原沉淀出来，得到贵金属单质。
本发明的原理：贵金属中金、铂、钯的氧化还原电位都高于含贵金属溶液中其他一般金属(例如铜、铝、镍、锡)的氧化还原电位。电位越高，氧化性越强，更容易发生氧化还原反应。在给定温度下，酰胺类有机化合物(例如N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMA)等)、乙醇和甲醇均具有还原性，可和贵金属发生氧化还原反应，因此在溶液中能够将贵金属选择性沉淀出来。
本发明的有益效果：可以将含贵金属液中几乎全部贵金属(金、铂、钯)离子还原为贵金属单质，进而通过过滤将其分离出来得到贵金属单质做到回收利用，极大缩短了贵金属回收的工艺流程。采用本发明的还原剂最高可以获得98.3％的金回收率，95.4％的钯回收率，94.6％的铂回收率，纯度经检测均在98.5％以上。 所使用的还原剂易得，价格低廉，方法简单，降低应用成本，易于实现规模化生产。
具体实施方式
下面结合实施例对本发明作进一步说明，还原剂(酰胺类有机化合物(例如N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMA)等)、乙醇和甲醇)的使用量为含贵金属离子溶液量的30％～80％，但本发明并不限于以下实例。
实例1:按照Au浓度260.16mg/L、Cu浓度203.52mg/L、Ni浓度180.83mg/L、Al浓度187.83mg/L、Sn浓度198.04mg/L的配比配置含金离子溶液，取100mL配置的溶液于瓶中，加入40mL N,N-二甲基甲酰胺(DMF)，密封，放置于50度烘箱中加热保温7小时后，瓶底出现沉淀物，过滤后进行X射线衍射仪(XRD)进行测试，符合金单质的粉末衍射图。取反应后上层清液进行电感耦合等离子光谱发生仪(ICP)测试，结果显示，金沉淀率为98.3％。
实例2:按照Pd浓度99.23mg/L、Cu浓度203.52mg/L、Ni浓度180.83mg/L、Al浓度187.83mg/L、Sn浓度198.04mg/L的配比配置含钯离子溶液，取100mL配置的溶液于瓶中，加入50mL N,N-二甲基乙酰胺(DMA)，密封，放置于60度烘箱中加热保温10小时后，瓶底出现沉淀物，过滤后进行X射线衍射仪(XRD)进行测试，符合钯单质的粉末衍射图。取反应后上层清液进行电感耦合等离子光谱发生仪(ICP)测试，结果显示，钯沉淀率为95.4％。
实例3:按照Pt浓度130.46mg/L、Cu浓度203.52mg/L、Ni浓度180.83mg/L、Al浓度187.83mg/L、Sn浓度198.04mg/L的配比配置含铂离子溶液，取100mL配置的溶液于瓶中，加入40mL乙醇，密封，放置于60度烘箱中加热保温8小时后，瓶底出现沉淀物，过滤后进行X射线衍射仪(XRD)进行测试，符合铂单质的粉末衍射图。取反应后上层清液进行电感耦合等离子光谱发生仪(ICP)测试，结果显示，铂沉淀率为87.8％。
实例4:按照Au浓度260.16mg/L、Pd浓度99.23mg/L、Cu浓度203.52mg/L、Ni浓度180.83mg/L、Al浓度187.83mg/L、Sn浓度198.04mg/L的配比配置含金钯离子溶液，取100mL配置的溶液于瓶中，加入40mL N,N-二甲基甲酰胺(DMF)，密封，放置于50度烘箱中加热保温7小时后，瓶底出现沉淀物，过滤后进行X射线衍射仪(XRD)进行测试，符合金单质的粉末衍射图。取反应后上层清液进行电感耦合等离子光谱发生仪(ICP)测试，结果显示，金沉淀率为96.7％，钯沉淀率为91.2％。

Claims (4)

  1. 一种低成本贵金属(金、铂、钯)离子选择性沉淀的还原剂的应用，其特征在于，将含贵金属(金、铂、钯)离子溶液中贵金属(金、铂、钯)选择性还原沉淀出来，得到贵金属(金、铂、钯)单质，所述的还原剂为酰胺类有机化合物(例如N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMA)等)、乙醇和甲醇中的一种或几种。
  2. 按照权利要求1所述的一种低成本贵金属(金、铂、钯)离子选择性沉淀的还原剂的应用，其特征在于，具体包括如下步骤：
    (1)向含贵金属(金、铂、钯)离子溶液中加入不超过溶液体积的还原剂；
    (2)将盛有如上液体的容器密封，放入50-70℃烘箱中，加热保温6-10小时，即可得到贵金属(金、铂、钯)单质。
  3. 按照权利要求2所述的一种低成本贵金属(金、铂、钯)离子选择性沉淀的还原剂的应用，其特征在于，还原剂的用量为不超过含贵金属(金、铂、钯)溶液量。
  4. 按照权利要求1所述的一种低成本贵金属(金、铂、钯)离子选择性沉淀的还原剂的应用，其特征在于，用于将含有贵金属(金、铂、钯)离子和其他金属离子的溶液中贵金属(金、铂、钯)离子选择性还原沉淀出来，得到贵金属(金、铂、钯)单质，其他金属离子为铜离子、铝离子、镍离子、锡离子中的一种或几种。
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