WO2021169780A1 - 一种选择性浸出含金物料中金的金浸剂及制备方法和用途 - Google Patents

一种选择性浸出含金物料中金的金浸剂及制备方法和用途 Download PDF

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WO2021169780A1
WO2021169780A1 PCT/CN2021/075749 CN2021075749W WO2021169780A1 WO 2021169780 A1 WO2021169780 A1 WO 2021169780A1 CN 2021075749 W CN2021075749 W CN 2021075749W WO 2021169780 A1 WO2021169780 A1 WO 2021169780A1
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gold
leaching
printed circuit
agent
circuit board
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PCT/CN2021/075749
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English (en)
French (fr)
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黄瑛
李倩霞
熊振峰
葛飞
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东南大学
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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
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • C22B11/042—Recovery of noble metals from waste materials
    • C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
    • 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
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
    • C22B3/1666—Leaching with heterocyclic compounds
    • 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 relates to a gold leaching agent and a preparation method and application, in particular to a gold leaching agent for selectively leaching gold from a gold-containing material, and a preparation method and application.
  • gold As a metal with high chemical stability, high catalytic activity, good ductility, and high thermal stability, gold has always been used in important industries and scientific technologies such as currency reserves, jewelry, communication technology, chemical technology, and medical technology.
  • Garbage, industrial waste, etc. the high gold content of these gold-bearing materials has brought high potential recycling value, and the huge business opportunities hidden in it have also attracted the "gold rush".
  • waste printed circuit boards in electronic waste and anode mud in industrial waste have the characteristics of large output, high gold content, and high recycling value. If they are discarded at will, they will pollute the environment and cannot use valuable resources such as gold. Therefore, it is very important to develop a safe, efficient and environmentally friendly gold extraction technology.
  • Metallurgical technology mainly includes pyrometallurgy, hydrometallurgy, biometallurgy, etc.
  • pyrometallurgy is a technology that decomposes gold-containing materials at high temperatures. It can separate metals from other materials and recover part of the heat energy, but it will produce two Toxic and harmful by-products such as oxin, and if you want to separate gold from various metals in the later stage, it needs to be combined with hydrometallurgical technology.
  • Biometallurgy mainly uses microorganisms to recover gold from gold-containing materials, including bioleaching, biosorption and other technologies. Biometallurgy has low cost, but its recovery rate of gold is low, and it takes a long time to find suitable microorganisms. It is not possible at this stage. Wide range of applications. Hydrometallurgy is more accurate, controllable, results more predictable, and better for metal recovery. It is currently the most commonly used and most negatively promising technology.
  • the object of the invention is to provide a gold leaching agent for selectively leaching gold from a gold-containing material.
  • Another object of the present invention is to provide a method for preparing the gold leaching agent for selectively leaching gold from a gold-containing material.
  • Another object of the present invention is to provide the use of the gold leaching agent for selectively leaching gold from gold-containing materials.
  • the present invention provides a gold leaching agent for selectively leaching gold from a gold-containing material, the composition of which is a halogen-containing organic substance that is soluble in water.
  • the above-mentioned water-soluble gold leaching agent has the ability to form a halogen ion with strong coordination ability with gold in an aqueous solution, which can reduce the oxidation-reduction potential of gold after being combined with the gold surface, and make the gold easier to be oxidized;
  • the water-soluble gold leaching agent can also form strong oxidizing hypohalite ions, halide ions, and halogen free radicals in the aqueous solution, which can promote the continuous and rapid leaching of gold;
  • the above-mentioned water-soluble gold leaching agent The organic matter formed after the dehalogenation can be combined with the gold-containing complex formed after the gold is leached to stabilize the gold-containing complex.
  • the water-soluble halogen-containing organic matter includes one or a mixture of one or more of easily soluble water-soluble halogen-containing organic matter, water-soluble halogen-containing organic matter, and slightly water-soluble halogen-containing organic matter.
  • halogen is a mixture of one or more of F, Cl, Br, and I.
  • the water-soluble halogen-containing organic substance is added to the aqueous solution and stirred for dissolution.
  • the concentration of the halogen-containing organic matter in the aqueous solution is 1-600 mmol/L, preferably 10-300 mmol/L, and more preferably 25, 300 mmol/L.
  • the use of the gold leaching agent for selectively leaching gold from the gold-containing material in the selective leaching and recovery of gold from the gold-containing material in the selective leaching and recovery of gold from the gold-containing material.
  • the temperature of the leaching reaction is 5-100°C, preferably 10-50°C, and more preferably 25°C.
  • the gold-containing material is gold ore, gold-containing industrial waste, and gold-containing electronic waste.
  • the solid-liquid ratio during leaching is 1:3-1:500, preferably 1:300.
  • the non-cyanide gold leaching agent of the present invention can replace cyanide to become an efficient and inexpensive gold leaching agent, is non-toxic, does not produce secondary pollution, is environmentally friendly and efficient, and will make gold leaching a green and environmentally friendly process.
  • the preparation method of the invention is simple. Its raw materials have a wide range of sources, and have low requirements for preparation equipment, and can be promoted in a wide range of industries.
  • the gold leaching agent of the present invention has mild and rapid gold leaching conditions, can leaching gold with high selectivity, has a better gold leaching rate than most traditional leaching agents (including cyanide leaching agents), and can be used at a lower concentration and liquid-to-solid ratio.
  • Figure 1 is a graph showing the relationship between the leaching rate of gold and other major metals in the gold finger of the printed circuit board and the time of the bromochlorohydantoin gold leaching agent in Example 1;
  • Example 2 is a graph showing the relationship between the leaching rate of gold and other major metals in the gold fingers of the printed circuit board and the time of the gold leaching agent of trichloroisocyanuric acid in Example 2;
  • Example 3 is a graph showing the relationship between the leaching rate of gold and other main metals in the gold finger of the printed circuit board and the time of the iodine succinimide immersion gold agent in Example 3.
  • Fig. 4 is a graph showing the relationship between the leaching rate of gold and other main metals in the gold fingers of the printed circuit board and the time of the bromochlorohydantoin gold leaching agent at low temperature in Example 4.
  • Fig. 5 is a graph showing the relationship between the leaching rate of gold and other main metals in the gold finger of the printed circuit board and the time of the bromochlorohydantoin gold leaching agent at a low solid-to-liquid ratio in Example 5.
  • Fig. 6 is a graph showing the relationship between the leaching rate of gold and other major metals in the gold fingers of the printed circuit board and the time of the gold leaching agent of trichloroisocyanuric acid at high temperature in Example 6.
  • Fig. 7 is a graph showing the relationship between the leaching rate of gold and other main metals in the gold finger of the printed circuit board and the time of the N-fluorobisbenzenesulfonamide gold leaching agent in Example 7.
  • bromochlorohydantoin into the aqueous solution and stir to dissolve to form a gold leaching solution with a bromochlorohydantoin concentration of 300mmol/Lol/L.
  • the bromochlorohydantoin gold leaching agent is mixed with the ground printed circuit board gold finger powder at a solid-to-liquid ratio of 1:100 to form an leaching system, and the leaching reaction is carried out at a rate of 200 rpm at 25°C.
  • ICP-OES was used to detect the gold and other major metals in the bromochlorohydantoin leaching solution of printed circuit board gold fingers and the aqua regia leaching solution of printed circuit board gold fingers. content.
  • the leaching rate is the ratio of the gold content in the clean and high-efficiency non-cyanide gold leaching agent after leaching to the gold content in the aqua regia leaching solution.
  • the leaching rate of other metals is the same as above.
  • the leaching reaction temperature was 25°C, and the solid-liquid ratio was 1:100. The results are shown in Figure 1.
  • Figure 1 shows the curve of the leaching rate of Au and Ni, Cu, Fe, and Ca in gold fingers of printed circuit boards with bromochlorohydantoin gold leaching agent over time.
  • the leaching rate of Au is also better than most traditional gold leaching agents, and under the same leaching practice, The leaching rate of Ni is 60.95%, the leaching rate of Fe is only 1.41%, the leaching rate of Ca is only 0.64%, and the leaching rate of Cu is only 18.13%. It can be seen that the leaching of Au by bromochlorohydantoin is very fast, and the leaching selectivity for Au by bromochlorohydantoin is extremely high, which can effectively separate from other metals in the gold fingers of the printed circuit board.
  • Example 2 Trichloroisocyanuric acid gold leaching agent for leaching and recovery of gold in printed circuit board gold fingers
  • the above trichloroisocyanuric acid gold leaching agent is mixed with the ground printed circuit board gold finger powder at a solid-to-liquid ratio of 1:300 to form an leaching system, and the leaching reaction is carried out at a rate of 200 rpm at 25°C.
  • ICP-OES was used to detect gold and other major metals in the trichloroisocyanuric acid leaching solution of printed circuit board gold fingers and the aqua regia leaching solution of printed circuit board gold fingers. Content.
  • the leaching rate is the ratio of the gold content in the environment-friendly and high-efficiency non-cyanide gold leaching agent after leaching to the gold content in the aqua regia leaching solution.
  • the leaching rate of other metals is the same as above.
  • the leaching reaction temperature is 25°C, and the solid-liquid ratio is 1:300.
  • the results are shown in Figure 2.
  • Figure 2 shows the curve of the leaching rate of Au, Fe, Ca, Mg, Al, and Ag in gold fingers of printed circuit boards with trichloroisocyanuric acid leaching agent over time.
  • the leaching rate of Au in the gold fingers of the printed circuit board reaches 76.55%, which is better than most traditional gold leaching agents.
  • the leaching rate of Cu is 48.98%
  • the leaching rate of Mg is only 7.11%
  • the leaching rate of Ca is only 5.38%
  • the leaching rate of Al is only 5.72%
  • the leaching rate of Fe is only 6.14%.
  • the leaching rate is only 5.48%.
  • the trichloroisocyanuric acid gold leaching agent has a high selective leaching advantage for Au, which can separate gold from other metals in the gold finger of the printed circuit board.
  • An environmentally-friendly high-efficiency non-cyanide gold leaching agent includes iodosuccinimide.
  • iodosuccinimide to the aqueous solution and stir to dissolve to form a gold leaching solution with a concentration of iodosuccinimide of 300 mmol/Lol/L.
  • the above iodosuccinimide gold leaching agent is mixed with the ground printed circuit board gold finger powder at a solid-to-liquid ratio of 1:300 to form an leaching system, and the leaching reaction is carried out at a rate of 200 rpm at 25°C.
  • ICP-OES was used to detect gold and other gold in the iodosuccinimide leaching solution of printed circuit board gold fingers and the aqua regia leaching solution of printed circuit board gold fingers. The content of the main metal.
  • the leaching rate is the ratio of the gold content in the environment-friendly and high-efficiency non-cyanide gold leaching agent after leaching to the gold content in the aqua regia leaching solution.
  • the leaching rate of other metals is the same as above.
  • the leaching reaction temperature was 25°C, and the solid-liquid ratio was 1:300. The results are shown in Figure 3.
  • Figure 3 shows the curve of the leaching rate of Au and Ni, Cu, Fe, and Ca in gold fingers of printed circuit board with iodosuccinimide gold leaching agent over time.
  • the leaching rate of metals is lower than the leaching rate of Au.
  • the leaching rate of Cu is 14.49%
  • the leaching rate of Fe is only 1.95%
  • the leaching rate of Ca is only 1.35%
  • the leaching rate of Ni is only 30.58%.
  • the iodine succinimide gold leaching agent is very fast to leaching of Au, and has a high selectivity to Au, and can effectively separate from other metals in the gold fingers of the printed circuit board.
  • Example 4 Leaching and recovery of gold in printed circuit board gold fingers by low-concentration bromochlorohydantoin gold leaching agent at low temperature
  • bromochlorohydantoin into the aqueous solution and stir to dissolve to form a gold leaching solution with bromochlorohydantoin concentration of 1mmol/Lol/L.
  • the bromochlorohydantoin gold leaching agent is mixed with the ground printed circuit board gold finger powder at a solid-to-liquid ratio of 1:500 to form an leaching system, and the leaching reaction is carried out at 5° C. and at a rate of 200 rpm.
  • ICP-OES was used to detect the gold and other major metals in the bromochlorohydantoin leaching solution of printed circuit board gold fingers and the aqua regia leaching solution of printed circuit board gold fingers. content.
  • the leaching rate is the ratio of the gold content in the clean and high-efficiency non-cyanide gold leaching agent after leaching to the gold content in the aqua regia leaching solution.
  • the leaching rate of other metals is the same as above.
  • the leaching reaction temperature is 5°C, and the solid-liquid ratio is 1:500. The results are shown in Figure 4.
  • Figure 4 shows the curve of the leaching rate of Au, Ni, Cu, Fe, and Ca in gold fingers of printed circuit boards with low concentration of bromochlorohydantoin gold leaching agent at low temperature.
  • bromochlorohydantoin into the aqueous solution and stir to dissolve to form a gold leaching solution with bromochlorohydantoin concentration of 600mmol/Lol/L.
  • the bromochlorohydantoin gold leaching agent is mixed with the ground printed circuit board gold finger powder at a solid-to-liquid ratio of 1:3 to form an leaching system, and the leaching reaction is carried out at 5° C. and at a rate of 200 rpm.
  • ICP-OES was used to detect the gold and other major metals in the bromochlorohydantoin leaching solution of printed circuit board gold fingers and the aqua regia leaching solution of printed circuit board gold fingers. content.
  • the leaching rate is the ratio of the gold content in the clean and high-efficiency non-cyanide gold leaching agent after leaching to the gold content in the aqua regia leaching solution.
  • the leaching rate of other metals is the same as above.
  • the leaching reaction temperature was 5°C, and the solid-liquid ratio was 1:3. The results are shown in Figure 5.
  • Figure 5 shows the curve of the leaching rate of Au, Ni, Cu, Fe, and Ca in printed circuit board gold fingers with bromochlorohydantoin gold leaching agent under low liquid-to-solid ratio and low temperature.
  • the bromochlorohydantoin gold leaching agent can extract a certain amount of Au under the reaction conditions of low temperature and low liquid-to-solid ratio, and the gold leaching agent has a good selectivity to Au.
  • Example 6 The leaching and recovery of gold in printed circuit board gold fingers by trichloroisocyanuric acid gold leaching agent under high temperature conditions
  • the above-mentioned trichloroisocyanuric acid gold leaching agent is mixed with the ground printed circuit board gold finger powder at a solid-to-liquid ratio of 1:300 to form an leaching system, and the leaching reaction is carried out at 100° C. and at a rate of 200 rpm.
  • ICP-OES was used to detect gold and other major metals in the trichloroisocyanuric acid leaching solution of printed circuit board gold fingers and the aqua regia leaching solution of printed circuit board gold fingers. Content.
  • the leaching rate is the ratio of the gold content in the environment-friendly and high-efficiency non-cyanide gold leaching agent after leaching to the gold content in the aqua regia leaching solution.
  • the leaching rate of other metals is the same as above.
  • the leaching reaction temperature is 100°C, and the solid-liquid ratio is 1:300. The results are shown in Figure 6.
  • Figure 6 shows the curve of the leaching rate of Au, Fe, Ni, Ca, and Cu in gold fingers of printed circuit boards under high temperature conditions with the gold leaching agent of trichloroisocyanuric acid.
  • the leaching rate of Au in the gold fingers of the printed circuit board reaches 64.56%, which is better than most traditional gold leaching agents.
  • the leaching rate of Cu is 49.17%
  • the leaching rate of Ni is only 39.59%
  • the leaching rate of Ca is only 16.34%
  • the leaching rate of Fe is only 16.23%.
  • the trichloroisocyanuric acid gold leaching agent can leached a large amount of Au in a short time under high temperature reaction conditions, and the gold leaching agent has a high selective leaching advantage for Au.
  • An environmentally-friendly high-efficiency non-cyanide gold leaching agent includes N-fluorobisbenzenesulfonamide.
  • N-fluorobisbenzenesulfonamide is added to the aqueous solution and stirred to dissolve to form a gold leaching solution with a concentration of N-fluorobisbenzenesulfonamide of 10 mmol/L.
  • N-fluorobisbenzenesulfonamide gold leaching agent is mixed with the ground printed circuit board gold finger powder at a solid-to-liquid ratio of 1:100 to form an leaching system, and the leaching reaction is carried out at a rate of 200 rpm at 25°C.
  • ICP-OES was used to detect gold and gold in the N-fluorobisbenzenesulfonamide leaching solution of printed circuit board gold fingers and the aqua regia leaching solution of printed circuit board gold fingers. The content of other major metals.
  • the leaching rate is the ratio of the gold content in the environment-friendly and high-efficiency non-cyanide gold leaching agent after leaching to the gold content in the aqua regia leaching solution.
  • the leaching rate of other metals is the same as above.
  • the leaching reaction temperature was 25°C, and the solid-liquid ratio was 1:100. The results are shown in Figure 7.
  • Figure 7 is the curve of the leaching rate of Au and Ni, Cu, Fe, and Ca in gold fingers of printed circuit boards with N-fluorobisbenzenesulfonamide gold leaching agent over time.
  • the N-fluorobisbenzenesulfonamide gold leaching agent can extract a certain amount of Au and has a high selectivity to Au.

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Abstract

一种选择性浸出含金物料中金的金浸剂及制备方法和用途。该金浸剂成分为可溶于水的含卤素有机物，可溶于水的含卤素有机物加入到水溶液中，搅拌溶解，即可。该金浸剂用于对含金物料中的金进行选择性浸出、回收。浸金剂毒性低、化学性质稳定、能够快速、温和、高选择性浸出金的浸金物质，对金的浸出率优于氰化物浸出剂等大多传统浸出剂，且浸出后二次污染小、浸出液的处理难度低，原料来源广泛，制备过程简单，对制取设备要求低，可大范围工业推广。

Description

一种选择性浸出含金物料中金的金浸剂及制备方法和用途 技术领域
本发明涉及金浸剂及制备方法和应用，特别涉及一种选择性浸出含金物料中金的金浸剂及制备方法和用途。
背景技术
作为一种化学稳定性高、催化活性高、延展性好、热稳定性高的金属，金一直以来被应用在货币储备、珠宝首饰以及通讯技术、化工技术、医疗技术等重要的工业与科学技术领域上。最早的金来源于含金矿石的开采，但是随着人类社会生活的丰富以及技术的革新，金在越来越多的应用在其他领域，也随之产生了很多金的二次来源，如电子垃圾、工业废料等，这些含金物料中高的金含量带来了很高的潜在回收价值，其间蕴藏的巨大商机也引来了“淘金热”。如电子废物中的废印刷线路板、工业废料中的阳极泥中具有产量大、含金量多、回收利用价值大的特点，如果他们随意丢弃，既会污染环境，也不能利用金等有价资源。所以开发出一种安全、高效、环保的提金技术是至关重要的。
冶金技术主要包括火法冶金、湿法冶金、生物冶金等，其中火法冶金是在高温下使含金物料高温分解的技术，可将金属与其他材料分离，同时回收部分热能，但会产生二噁英等有毒有害副产物，且如果想后期从各种金属中分离金需要与湿法冶金技术结合。生物冶金主要利用微生物回收含金物料中的金，包括生物浸出、生物吸附等技术，生物冶金技术成本低，但其对金的回收率较低，且寻找适合的微生物耗时长，现阶段还不能大范围应用。湿法冶金更准确、可控、结果更易预测、回收金属的效果更好，是目前最常被使用和最负前景的技术。
利用湿法冶金技术回收金，首先需要对含金物料中的金进行浸出，即使金经过浸出反应进入浸出液，并为下一步的溶剂萃取、离子交换、电化学回收等提供前提条件。然而传统浸出剂如氰化物、王水、硫脲等具有腐蚀性大、对金的选择性不高、毒性大、成本高、易导致二次污染等问题。其中氰化物是最常见的浸金剂，虽然已在金矿和一些二次资源中的金回收上被运用了上百年，但造成了很多的污染案例，造成了严重的河流和地下水污染等，所以亟需开发一种绿色环保且能快速选择性浸出金的技术，能够达到含金物料的资源化、无害化的处理处置目标。
发明内容
发明目的：本发明目的是提供选择性浸出含金物料中金的金浸剂。
本发明另一目的是提供所述选择性浸出含金物料中金的金浸剂的制备方法。
本发明另一目的是提供所述选择性浸出含金物料中金的金浸剂的用途。
技术方案：本发明提供一种选择性浸出含金物料中金的金浸剂，其成分为可溶于水的 含卤素有机物。
上述可溶于水的金浸剂，具有在水溶液中形成与金配位能力强的卤素离子，其与金表面结合后能降低金的氧化还原电位，使金更容易被氧化；其次，上述可溶于水的金浸剂也可以在水溶液中形成具有强氧化性的次卤酸根离子、卤酸根离子、卤素自由基，可以促使金的持续快速浸出；其次，上述可溶于水的金浸剂在脱卤素后形成的有机物能够与金被浸出后形成的含金配合物结合、稳定含金配合物。
进一步地，所述可溶于水的含卤素有机物包括易溶于水含卤素有机物、可溶于水含卤素有机物、微溶于水含卤素有机物中的一种或多种的混合物。
进一步地，所述卤素为F、Cl、Br、I中的一种或多种的混合物。
所述的选择性浸出含金物料中金的金浸剂的制备方法，将可溶于水的含卤素有机物加入到水溶液中，搅拌溶解。
进一步地，所述水溶液中含卤素有机物的浓度为1-600mmol/L，优选为10-300mmol/L，再优选为25、300mmol/L。
所述的选择性浸出含金物料中金的金浸剂在对含金物料中的金进行选择性浸出、回收中的用途。
进一步地，所述浸出反应的温度为5-100℃，优选为10-50℃，再优选为25℃。
进一步地，所述含金物料为金矿石、含金工业废料、含金电子垃圾。
进一步地，浸出时的固液比为1:3-1:500，优选为1:300。
有益效果：本发明非氰浸金剂可代替氰化物成为高效且价格低廉的金浸出剂，没有毒性，不产生二次污染，环保高效，将使金的浸出成为绿色环保的过程。本发明制备方法简单。其原料来源广泛，对制取设备要求低，可大范围工业推广。本发明的浸金剂，浸金条件温和、快速，可高选择性浸出金，对金的浸出率优于大多传统浸出剂(包括氰化物浸出剂)，且能在较低浓度和液固比条件下可以取得工业上能接受的高浸金率，且对含金物料中其他主要金属的浸出率低，可以取得对金的高选择性回收，提高金与其他金属浸出的分离度，试剂毒性低，二次污染小，对废液的处理难度低，具有广阔的实际应用前景。
附图说明
图1为实施例1中，溴氯海因浸金剂对印刷线路板金手指中金及其他主要金属的浸出率与时间的关系曲线图；
图2为实施例2中，三氯异氰尿酸浸金剂对印刷线路板金手指中金及其他主要金属的浸出率与时间的关系曲线图；
图3为实施例3中，碘代丁二酰亚胺浸金剂对印刷线路板金手指中金及其他主要金属的浸出率与时间的关系曲线图。
图4为实施例4中，溴氯海因浸金剂在低温下对印刷线路板金手指中金及其他主要金 属的浸出率与时间的关系曲线图。
图5为实施例5中，溴氯海因浸金剂在低固液比下对印刷线路板金手指中金及其他主要金属的浸出率与时间的关系曲线图。
图6为实施例6中，三氯异氰尿酸浸金剂在高温对印刷线路板金手指中金及其他主要金属的浸出率与时间的关系曲线图。
图7为实施例7中，N-氟代双苯磺酰胺浸金剂对印刷线路板金手指中金及其他主要金属的浸出率与时间的关系曲线图。
具体实施方式
实施例1溴氯海因浸金剂对印刷线路板金手指中金的浸出回收
1.其制备方法
将溴氯海因加入到水溶液中，搅拌溶解，形成溴氯海因浓度为300mmol/Lol/L的浸金液。
2.溴氯海因浸金剂对印刷线路板金手指中金及其他主要金属的浸出
将上述溴氯海因浸金剂，与经研磨后的印刷线路板金手指粉末在1:100固液比下混合形成浸出体系，在25℃下，以200rpm速率进行浸出反应。
3.测定印刷线路板金手指中金及其他主要金属的浸出率
将1g经研磨后的印刷线路板金手指粉末分别按固液比1:100和1:40加入到上述制得的溴氯海因浸金剂和新制王水中，在200rpm下反应一段时间，其中印刷线路板金手指粉末与非氰浸金剂按照实施实验设定反应一定时间，印刷线路板金手指粉末与新制王水反应6h。浸出反应结束后，进行抽滤，得到印刷线路板金手指的溴氯海因浸出液和印刷线路板金手指的王水浸出液。
印刷线路板金手指中金及其他主要金属的浸出率测定：用ICP-OES分别检测印刷线路板金手指的溴氯海因浸出液和印刷线路板金手指的王水浸出液中金及其他主要金属的含量。
本发明中，浸出率为浸出后清洁高效非氰浸金剂中金含量和王水浸出液中金含量的比。其他金属浸出率同上所述。
4.溴氯海因浸金剂对印刷线路板金手指中Au及其他主要金属的浸出率与时间的关系
浸出反应温度为25℃，固液比为1:100，结果见图1。
图1表示了溴氯海因浸金剂对印刷线路板金手指中Au及Ni,Cu,Fe,Ca的浸出率随时间变化的曲线。
可以看出浸出仅5h后，印刷线路板金手指中91.1％的Au被浸出，其浸出时间少于传统浸出剂，Au的浸出率也优于大多传统浸金剂，且在同一浸出实践下，Ni的浸出率为60.95％，Fe的浸出率仅为1.41％，Ca的浸出率仅为0.64％，Cu的浸出率仅为18.13％。可 以看出，溴氯海因浸金剂对Au的浸出非常快速，且溴氯海因浸金剂对Au的浸出选择性极高，能够有效与印刷线路板金手指中其他金属分离。
实施例2三氯异氰尿酸浸金剂对印刷线路板金手指中金的浸出回收
1.制备方法
将三氯异氰尿酸溶解在水溶液中，形成三氯异氰尿酸浓度为25mmol/Lol/L的浸金液。
2.三氯异氰尿酸浸金剂对印刷线路板金手指中金及其他主要金属的浸出
将上述三氯异氰尿酸浸金剂，与经研磨后的印刷线路板金手指粉末在1:300固液比下混合形成浸出体系，在25℃下，以200rpm速率进行浸出反应。
3.测定印刷线路板金手指中金及其他主要金属的浸出率
将0.5g经研磨后的印刷线路板金手指粉末按固液比1:300和1:40加入到上述制得的三氯异氰尿酸浸金剂和新制王水中，在200rpm下反应一段时间，其中印刷线路板金手指粉末与非氰浸金剂按照实施实验设定反应一定时间，印刷线路板金手指粉末与新制王水反应24h。浸出反应结束后，进行抽滤，得到印刷线路板金手指的三氯异氰尿酸浸出液和印刷线路板金手指的王水浸出液。
印刷线路板金手指中金及其他主要金属的浸出率测定：用ICP-OES分别检测印刷线路板金手指的三氯异氰尿酸浸出液和印刷线路板金手指的王水浸出液中金及其他主要金属的含量。
本发明中，浸出率为浸出后环保高效非氰浸金剂中金含量和王水浸出液中金含量的比。其他金属浸出率同上所述。
4.三氯异氰尿酸浸金剂对印刷线路板金手指中Au及其他主要金属的浸出率与时间的关系
浸出反应温度为25℃，固液比为1:300，结果见图2。
图2表示了三氯异氰尿酸浸金剂对印刷线路板金手指中Au及Fe,Ca,Mg,Al,Ag的浸出率随时间变化的曲线。
可以看出仅浸出5h后，印刷线路板金手指中Au的浸出率达到76.55％，优于大多传统浸金剂。在同一浸出实践下，Cu的浸出率为48.98％，Mg浸出率仅为7.11％，Ca的浸出率仅为5.38％，Al的浸出率仅为5.72％，Fe的浸出率仅为6.14％，Ag的浸出率仅为5.48％。可以看出，三氯异氰尿酸浸金剂对Au具有很高的选择性浸出优势，能够使金与印刷线路板金手指中其他金属分离。
实施例3碘代丁二酰亚胺浸金剂对印刷线路板金手指中金的浸出回收
一种环保高效非氰浸金剂包括碘代丁二酰亚胺。
1.制备方法
将碘代丁二酰亚胺加入到水溶液中，搅拌溶解，形成碘代丁二酰亚胺浓度为 300mmol/Lol/L的浸金液。
2.碘代丁二酰亚胺浸金剂对印刷线路板金手指中金及其他主要金属的浸出
将上述碘代丁二酰亚胺浸金剂，与经研磨后的印刷线路板金手指粉末在1:300固液比下混合形成浸出体系，在25℃下，以200rpm速率进行浸出反应。
3.测定印刷线路板金手指中金及其他主要金属的浸出率
将1g经研磨后的印刷线路板金手指粉末分别按固液比1:300和1:40加入到上述制得的碘代丁二酰亚胺浸金剂和新制王水中，在200rpm下反应一段时间，其中印刷线路板金手指粉末与非氰浸金剂按照实施实验设定反应一定时间，印刷线路板金手指粉末与新制王水反应6h。浸出反应结束后，进行抽滤，得到印刷线路板金手指的碘代丁二酰亚胺浸出液和印刷线路板金手指的王水浸出液。
印刷线路板金手指中金及其他主要金属的浸出率测定：用ICP-OES分别检测印刷线路板金手指的碘代丁二酰亚胺浸出液和印刷线路板金手指的王水浸出液中金及其他主要金属的含量。
本发明中，浸出率为浸出后环保高效非氰浸金剂中金含量和王水浸出液中金含量的比。其他金属浸出率同上所述。
4.碘代丁二酰亚胺浸金剂对印刷线路板金手指中Au及其他主要金属的浸出率与时间的关系
浸出反应温度为25℃，固液比为1:300，结果见图3。
图3了碘代丁二酰亚胺浸金剂对印刷线路板金手指中Au及Ni,Cu,Fe,Ca的浸出率随时间变化的曲线。
可以看出浸出仅5h后，印刷线路板金手指中45.34％的Au被浸出，其浸金速率快于传统浸出剂，并且在同一浸出实践下，碘代丁二酰亚胺浸金剂对其他金属的浸出率均低于对Au的浸出率，此时Cu的浸出率为14.49％，Fe的浸出率仅为1.95％，Ca的浸出率仅为1.35％，Ni的浸出率仅为30.58％。可以看出，碘代丁二酰亚胺浸金剂对Au的浸出非常快速，且对Au有很高的选择性，能够有效与印刷线路板金手指中其他金属分离。实施例4低浓度溴氯海因浸金剂在低温下对印刷线路板金手指中金的浸出回收
1.其制备方法
将溴氯海因加入到水溶液中，搅拌溶解，形成溴氯海因浓度为1mmol/Lol/L的浸金液。
2.溴氯海因浸金剂对印刷线路板金手指中金及其他主要金属的浸出
将上述溴氯海因浸金剂，与经研磨后的印刷线路板金手指粉末在1:500固液比下混合形成浸出体系，在5℃下，以200rpm速率进行浸出反应。
3.测定印刷线路板金手指中金及其他主要金属的浸出率
将0.5g经研磨后的印刷线路板金手指粉末分别按固液比1:500和1:40加入到上述制得 的溴氯海因浸金剂和新制王水中，在200rpm下反应一段时间，其中印刷线路板金手指粉末与非氰浸金剂按照实施实验设定反应一定时间，印刷线路板金手指粉末与新制王水反应6h。浸出反应结束后，进行抽滤，得到印刷线路板金手指的溴氯海因浸出液和印刷线路板金手指的王水浸出液。
印刷线路板金手指中金及其他主要金属的浸出率测定：用ICP-OES分别检测印刷线路板金手指的溴氯海因浸出液和印刷线路板金手指的王水浸出液中金及其他主要金属的含量。
本发明中，浸出率为浸出后清洁高效非氰浸金剂中金含量和王水浸出液中金含量的比。其他金属浸出率同上所述。
4.低浓度溴氯海因浸金剂在低温下对印刷线路板金手指中Au及其他主要金属的浸出率与时间的关系
浸出反应温度为5℃，固液比为1:500，结果见图4。
图4表示了低浓度溴氯海因浸金剂在低温下对印刷线路板金手指中Au及Ni,Cu,Fe,Ca的浸出率随时间变化的曲线。
可以看出浸出5h后，印刷线路板金手指中1.94％的Au被浸出，在同一浸出实践下，Ni的浸出率为2.20％，Fe的浸出率为0.56％，Ca的浸出率为0.25％，Cu的浸出率为6.21％。可以看出，低温反应条件下低浓度溴氯海因浸金剂能够浸出一定量的Au。
实施例5溴氯海因浸金剂在低液固比、低温下对印刷线路板金手指中金的浸出回收
1.其制备方法
将溴氯海因加入到水溶液中，搅拌溶解，形成溴氯海因浓度为600mmol/Lol/L的浸金液。
2.溴氯海因浸金剂对印刷线路板金手指中金及其他主要金属的浸出
将上述溴氯海因浸金剂，与经研磨后的印刷线路板金手指粉末在1:3固液比下混合形成浸出体系，在5℃下，以200rpm速率进行浸出反应。
3.测定印刷线路板金手指中金及其他主要金属的浸出率
将1g经研磨后的印刷线路板金手指粉末分别按固液比1:3和1:40加入到上述制得的溴氯海因浸金剂和新制王水中，在200rpm下反应一段时间，其中印刷线路板金手指粉末与非氰浸金剂按照实施实验设定反应一定时间，印刷线路板金手指粉末与新制王水反应6h。浸出反应结束后，进行抽滤，得到印刷线路板金手指的溴氯海因浸出液和印刷线路板金手指的王水浸出液。
印刷线路板金手指中金及其他主要金属的浸出率测定：用ICP-OES分别检测印刷线路板金手指的溴氯海因浸出液和印刷线路板金手指的王水浸出液中金及其他主要金属的含量。
本发明中，浸出率为浸出后清洁高效非氰浸金剂中金含量和王水浸出液中金含量的比。其他金属浸出率同上所述。
4.溴氯海因浸金剂在低液固比、低温下对印刷线路板金手指中Au及其他主要金属的浸出率与时间的关系
浸出反应温度为5℃，固液比为1:3，结果见图5。
图5表示了溴氯海因浸金剂在低液固比、低温下对印刷线路板金手指中Au及Ni,Cu,Fe,Ca的浸出率随时间变化的曲线。
可以看出浸出10h后，印刷线路板金手指中34.03％的Au被浸出，在同一浸出实践下，Ni的浸出率为45.96％，Fe的浸出率为0.15％，Ca的浸出率为0.70％，Cu的浸出率为10.97％。可以看出，低温、低液固比反应条件下溴氯海因浸金剂能够浸出一定量的Au，且改浸金剂对Au的选择性好。
实施例6三氯异氰尿酸浸金剂在高温条件下对印刷线路板金手指中金的浸出回收
1.制备方法
将三氯异氰尿酸溶解在水溶液中，形成三氯异氰尿酸浓度为25mmol/Lol/L的浸金液。
2.三氯异氰尿酸浸金剂对印刷线路板金手指中金及其他主要金属的浸出
将上述三氯异氰尿酸浸金剂，与经研磨后的印刷线路板金手指粉末在1:300固液比下混合形成浸出体系，在100℃下，以200rpm速率进行浸出反应。
3.测定印刷线路板金手指中金及其他主要金属的浸出率
将0.5g经研磨后的印刷线路板金手指粉末按固液比1:300和1:40加入到上述制得的三氯异氰尿酸浸金剂和新制王水中，在200rpm下反应一段时间，其中印刷线路板金手指粉末与非氰浸金剂按照实施实验设定反应一定时间，印刷线路板金手指粉末与新制王水反应24h。浸出反应结束后，进行抽滤，得到印刷线路板金手指的三氯异氰尿酸浸出液和印刷线路板金手指的王水浸出液。
印刷线路板金手指中金及其他主要金属的浸出率测定：用ICP-OES分别检测印刷线路板金手指的三氯异氰尿酸浸出液和印刷线路板金手指的王水浸出液中金及其他主要金属的含量。
本发明中，浸出率为浸出后环保高效非氰浸金剂中金含量和王水浸出液中金含量的比。其他金属浸出率同上所述。
4.三氯异氰尿酸浸金剂在高温条件下对印刷线路板金手指中Au及其他主要金属的浸出率与时间的关系
浸出反应温度为100℃，固液比为1:300，结果见图6。
图6表示了三氯异氰尿酸浸金剂在高温条件下对印刷线路板金手指中Au及Fe,Ni，Ca，Cu的浸出率随时间变化的曲线。
可以看出仅浸出5h后，印刷线路板金手指中Au的浸出率达到64.56％，优于大多传统浸金剂。在同一浸出实践下，Cu的浸出率为49.17％，Ni浸出率仅为39.59％，Ca的浸出率仅为16.34％，Fe的浸出率仅为16.23％。可以看出，三氯异氰尿酸浸金剂在高温的反应条件下能够在短时间内浸出大量Au，且该浸金剂对Au具有很高的选择性浸出优势。
实施例7 N-氟代双苯磺酰胺浸金剂对印刷线路板金手指中金的浸出回收
一种环保高效非氰浸金剂包括N-氟代双苯磺酰胺。
1.制备方法
将N-氟代双苯磺酰胺加入到水溶液中，搅拌溶解，形成N-氟代双苯磺酰胺胺浓度为10mmol/L的浸金液。
2.N-氟代双苯磺酰胺浸金剂对印刷线路板金手指中金及其他主要金属的浸出
将上述N-氟代双苯磺酰胺浸金剂，与经研磨后的印刷线路板金手指粉末在1:100固液比下混合形成浸出体系，在25℃下，以200rpm速率进行浸出反应。
3.测定印刷线路板金手指中金及其他主要金属的浸出率
将1g经研磨后的印刷线路板金手指粉末分别按固液比1:100和1:40加入到上述制得的N-氟代双苯磺酰胺浸金剂和新制王水中，在200rpm下反应一段时间，其中印刷线路板金手指粉末与非氰浸金剂按照实施实验设定反应一定时间，印刷线路板金手指粉末与新制王水反应6h。浸出反应结束后，进行抽滤，得到印刷线路板金手指的N-氟代双苯磺酰胺浸出液和印刷线路板金手指的王水浸出液。
印刷线路板金手指中金及其他主要金属的浸出率测定：用ICP-OES分别检测印刷线路板金手指的N-氟代双苯磺酰胺浸出液和印刷线路板金手指的王水浸出液中金及其他主要金属的含量。
本发明中，浸出率为浸出后环保高效非氰浸金剂中金含量和王水浸出液中金含量的比。其他金属浸出率同上所述。
4.N-氟代双苯磺酰胺浸金剂对印刷线路板金手指中Au及其他主要金属的浸出率与时间的关系
浸出反应温度为25℃，固液比为1:100，结果见图7。
图7为N-氟代双苯磺酰胺浸金剂对印刷线路板金手指中Au及Ni,Cu,Fe,Ca的浸出率随时间变化的曲线。
可以看出浸出10h后，印刷线路板金手指中1.67％的Au被浸出，在同一浸出实践下，Cu的浸出率为1.17％，Fe的浸出率仅为0.06％，Ca的浸出率仅为0.48％，Ni的浸出率仅为0.82％。可以看出，N-氟代双苯磺酰胺浸金剂能够浸出一定量的Au，且对Au有高的选择性。

Claims (9)

  1. 一种选择性浸出含金物料中金的金浸剂，其特征在于：其成分为可溶于水的含卤素有机物。
  2. 根据权利要求1所述的选择性浸出含金物料中金的金浸剂，其特征在于：所述可溶于水的含卤素有机物包括易溶于水含卤素有机物、可溶于水含卤素有机物、微溶于水含卤素有机物中的一种或多种的混合物。
  3. 根据权利要求1所述的选择性浸出含金物料中金的金浸剂，其特征在于：所述卤素为F、Cl、Br、I中的一种或多种的混合物。
  4. 权利要求1所述的选择性浸出含金物料中金的金浸剂的制备方法，其特征在于：将可溶于水的含卤素有机物加入到水溶液中，搅拌溶解。
  5. 根据权利要求4所述的选择性浸出含金物料中金的金浸剂的制备方法，其特征在于：所述水溶液中含卤素有机物的浓度为1-600mmol/L。
  6. 权利要求1所述的选择性浸出含金物料中金的金浸剂在对含金物料中的金进行选择性浸出、回收中的用途。
  7. 根据权利要求6所述的用途，其特征在于：所述浸出反应的温度为5-100℃。
  8. 根据权利要求6所述的用途，其特征在于：所述含金物料为金矿石、含金工业废料、含金电子垃圾。
  9. 根据权利要求6所述的用途，其特征在于：浸出时的固液比为1:3-1:500。
PCT/CN2021/075749 2020-02-25 2021-02-07 一种选择性浸出含金物料中金的金浸剂及制备方法和用途 WO2021169780A1 (zh)

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