WO2022236956A1 - 金银提取剂的制备方法 - Google Patents

金银提取剂的制备方法 Download PDF

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WO2022236956A1
WO2022236956A1 PCT/CN2021/107060 CN2021107060W WO2022236956A1 WO 2022236956 A1 WO2022236956 A1 WO 2022236956A1 CN 2021107060 W CN2021107060 W CN 2021107060W WO 2022236956 A1 WO2022236956 A1 WO 2022236956A1
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gold
silver
cyanate
preparation
extractant
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PCT/CN2021/107060
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French (fr)
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吕宪俊
张雁
刘晓亮
崔铭耀
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山东科技大学
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Priority to AU2021445505A priority Critical patent/AU2021445505B2/en
Publication of WO2022236956A1 publication Critical patent/WO2022236956A1/zh
Priority to ZA2023/00856A priority patent/ZA202300856B/en

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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
    • C22B11/08—Obtaining noble metals by cyaniding
    • 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
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • 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 preparation method of a novel gold and silver extractant, belonging to the technical fields of hydrometallurgy and gold production.
  • Cyanide has long dominated gold production, but cyanide is highly toxic and poses a huge threat to the ecological environment and human health. Therefore, the research and development of non-cyanide gold extraction agents is imminent.
  • the Chinese invention patent of CN111304456A discloses a kind of environment-friendly gold extraction agent and preparation method thereof, uses 50%-60% sodium carbonate, 30%-40% urea and 10%-20% yellow blood salt sodium in the method, Heat to 800 oC - 850 oC in a closed container and keep warm for 3 - 6 hours to prepare the gold extracting agent.
  • the Chinese invention patent with the publication number CN109957664A discloses an environment-friendly gold extraction agent and its preparation method. The method is prepared from raw materials including sodium humate, soda ash, urea and gold leaching activator lead salt or manganate under high temperature conditions. to make.
  • the Chinese invention patent with the publication number CN109943731A discloses a green and environment-friendly gold extracting agent and its preparation method.
  • the gold extracting agent is prepared from 60%-70% sodium carbonate, 20%-30% cyanuric acid and the remaining auxiliary agent. Made, in which additives are sodium halides (sodium chloride and sodium iodide).
  • the Chinese invention patent with the publication number CN105671312A discloses an environment-friendly gold and silver leaching agent and a preparation method thereof.
  • the leaching agent is composed of 1-60 parts of sodium cyanate, 1-15 parts of sodium chloride, and 1-60 parts of carbonamide , 1-40 parts of yellow blood salt, 1-40 parts of tetrasodium hexacyanoferrate, 1-50 parts of soda, 1-15 parts of sodium thiosulfate in a stainless steel reactor at 450 oC-860 oC for 3.5- 5.5 h prepared.
  • the present invention proposes a preparation method of a novel gold and silver extractant.
  • a preparation method of a novel gold and silver extractant comprising the following steps:
  • the cyanate is sodium cyanate or potassium cyanate.
  • the ferrous salt is sodium ferrocyanide, potassium ferrocyanide, ferrous chloride, ferrous nitrate or ferrous sulfate.
  • the mass ratio of the cyanate and the ferrous salt is 3:0.5-3:2; further preferably, the mass ratio of the cyanate and the ferrous salt is 4:1.
  • the synthetic raw materials are sodium cyanate and potassium ferrocyanide, and the mass ratio of sodium cyanate and potassium ferrocyanide is 4:1.
  • the calcination synthesis process conditions are: air atmosphere, heating rate 5 oC/min-20 oC/min, calcination temperature 600 oC-750 oC, holding time 0.5 h-2 h.
  • the calcination temperature is more preferably 700°C.
  • the calcination synthesis process conditions are: air atmosphere, heating rate 15 oC/min, calcination temperature 700 oC, holding time 1 h.
  • the reagent synthesized by the reaction when the roasting in step (3) ends, the reagent synthesized by the reaction is in a molten state (or liquid state), and it should be poured out from the crucible as soon as possible while it is hot, so as to separate; otherwise, during the cooling process, the synthetic reagent becomes It is solid, easy to adhere to the inner wall of the reaction vessel (ie crucible), and it is difficult to separate it.
  • the present invention has the following advantages: only two synthetic raw materials of cyanate and ferrous salt are used, and the roasting synthesis process is simple and easy to operate; Fast speed, low toxicity and environmental protection, low reagent cost, strong adaptability to ore, etc.
  • novel gold and silver extractant prepared by the invention can completely replace sodium cyanide to leach gold and silver ores without changing the original cyanide leaching process and equipment.
  • Fig. 1 is the preparation process flowchart of novel gold and silver extractant among the present invention.
  • the synthetic raw material of described gold and silver extractant is cyanate and ferrous salt.
  • the preparation steps of the gold and silver extractant are as follows: first, mix the raw material cyanate and ferrous salt in a certain proportion; then, place the mixed raw material in a high-temperature-resistant crucible for high-temperature roasting; The molten composition is poured out from the crucible, and cooled naturally in the air; finally, the block solid composition formed by cooling is ground into powder, and the gold and silver extractant is obtained.
  • the synthetic raw materials of the new gold and silver extractant involved in the present invention are simple in composition, low in price, and the synthesis process is easy to operate, and the synthesized gold and silver extractant has high gold and silver leaching rate, fast leaching rate, low toxicity and environmental protection, and adaptability to ores Strong and other advantages.
  • the chemical composition (wt.%) of a gold concentrate is shown in Table 1. The following gold and silver leaching experiments were conducted using this gold concentrate.
  • the ratio of raw materials has a great influence on the gold and silver leaching effect of the synthesized extractant.
  • the gold and silver leaching effect of the agent is better than that of sodium cyanide.
  • the gold leaching rate of the synthetic extractant was 98.4%, and the silver leaching rate was 95.1%, which was higher than the gold leaching rate of 91.3% and the silver leaching rate of 84.8% of sodium cyanide.
  • roasting temperature The influence of roasting temperature on the gold and silver leaching effect of the synthesized extractant is shown in Table 3.
  • the mass ratio of synthetic raw materials sodium cyanate to potassium ferrocyanide is 4:1; roasting conditions: air atmosphere, heating rate 15 oC/min, holding time 1 h. Other steps are the same as above.
  • Leaching conditions liquid-solid ratio 2.5:1, gold extraction agent concentration 0.3 wt.%, pH 11, rotational speed 600 rpm, leaching time 24h.
  • the calcination temperature has a great influence on the gold and silver leaching effect of the synthesized extractant. Too high or too low calcination temperature is not conducive to the synthesis of extractant, and the suitable calcination temperature is 700 oC.
  • Table 4 shows the effect of ferrous salt types on the gold and silver leaching effect of the synthesized extractant.
  • the mass ratio of synthetic raw materials sodium cyanate and ferrous salt is 4:1; roasting conditions: air atmosphere, heating rate 15 oC/min, roasting temperature 700 oC, holding time 1 h. Keep the rest of the preparation steps unchanged.
  • Leaching conditions liquid-solid ratio 2.5:1, gold extraction agent concentration 0.3 wt.%, pH 11, rotational speed 600 rpm, leaching time 24 h.
  • the synthesized gold and silver extractant can achieve ideal gold and silver extraction effects on both sulfide-type and oxidized gold ores, so it has strong ore adaptability.
  • gold and silver extractant can be synthesized only by using sodium cyanate and ferrous salt, and the synthesized extractant has high gold and silver leaching rate, fast leaching rate and strong adaptability to ore.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

一种金银提取剂的制备方法，包括以下步骤：（1）选取氰酸盐和亚铁盐为原料，将氰酸盐和亚铁盐混匀；（2）将混匀的原料放入耐高温坩埚中焙烧；（3）焙烧结束后，趁热将得到的熔融态合成物从坩埚中倒出，并置于空气中自然冷却；（4）冷却后，得到块状固体合成物，将块状固体合成物碎磨成粉末状，即得金银提取剂。上述方法仅使用氰酸盐和亚铁盐便可合成能够与氰化钠提金效果相媲美的低毒环保提取剂；合成原料组成简单、价格低廉，且合成过程工艺简单、易操作，所合成的金银提取剂具有金银浸出率高、浸出速率快、低毒环保、试剂成本低、对矿石适应性强等优点。

Description

[根据细则37.2由ISA制定的发明名称]　金银提取剂的制备方法 技术领域
本发明涉及一种新型金银提取剂的制备方法，属于湿法冶金和黄金生产技术领域。
 背景技术
氰化法在黄金生产中长期占据统治地位，但氰化物具有剧毒，对生态环境和人体健康形成巨大威胁，因此，非氰金提取剂的研究和开发迫在眉睫。
近十年，在我国出现了一类能够替代氰化物的环保提金剂。公开号为CN111304456A的中国发明专利公开了一种环保提金剂及其制备方法，该方法中使用50% – 60%碳酸钠、30% – 40%尿素和10% – 20%黄血盐钠，在密闭容器中加热至800 ºC– 850 ºC、保温3 – 6 h制得提金剂。公开号为CN109957664A的中国发明专利公开了一种环保提金剂及其制备方法，该方法由原料包括腐植酸钠、纯碱和尿素及浸金活化剂铅盐或锰酸盐在高温条件下制备而成。公开号为CN109943731A的中国发明专利公开了一种绿色环保提金剂及其制备方法，该提金剂采用原料为60% – 70%碳酸钠、20% – 30%氰尿酸和余量助剂制备而成，其中助剂为卤化钠（氯化钠和碘化钠）。公开号为CN105671312A的中国发明专利公开了一种环保型黄金白银浸出剂及其制备方法，该浸出剂是由氰酸钠1– 60份、氯化钠1 – 15份、碳酰胺1 – 60份、黄血盐1 – 40份、六氰合铁酸四钠1 – 40份、苏打1 – 50份、硫代硫酸钠1 – 15份在不锈钢反应釜中经450 ºC – 860 ºC高温反应3.5 – 5.5 h制备而成。
 技术问题
此外，仍有较多其他有关环保提金剂制备方法的专利，但这些专利所涉及提金剂的合成原料均比较复杂，基本由三种及三种以上原料制备而成，这导致合成过程反应复杂，制备成本高。
 技术解决方案
基于上述技术问题，本发明提出一种新型金银提取剂的制备方法。
本发明所采用的技术解决方案是：
一种新型金银提取剂的制备方法，包括以下步骤：
    （1）选取氰酸盐和亚铁盐为原料，将氰酸盐和亚铁盐混匀；
    （2）将混匀的原料放入耐高温坩埚中焙烧；
    （3）焙烧结束后，趁热将得到的熔融态合成物从坩埚中倒出，并置于空气中自然冷却；
    （4）冷却后，得到块状固体合成物，将块状固体合成物碎磨成粉末状，即得新型金银提取剂。
优选的，所述氰酸盐为氰酸钠或氰酸钾。
优选的，所述亚铁盐为亚铁氰化钠、亚铁氰化钾、氯化亚铁、硝酸亚铁或硫酸亚铁。
优选的，所述氰酸盐和亚铁盐的质量比为3:0.5 – 3:2；进一步优选，所述氰酸盐和亚铁盐的质量比为4:1。更加优选合成原料为氰酸钠和亚铁氰化钾，且氰酸钠和亚铁氰化钾的质量比为4:1。
优选的，步骤（2）中，所述焙烧合成工艺条件为：空气气氛、升温速率5 ºC/min – 20 ºC/min、焙烧温度600 ºC – 750 ºC、保温时间0.5 h – 2 h。所述焙烧温度更加优选为700 ºC。
更加优选的，所述焙烧合成工艺条件为：空气气氛、升温速率15 ºC/min、焙烧温度700 ºC、保温时间1 h。
上述方法中，步骤（3）中焙烧结束时，反应合成的试剂为熔融态（或液态），应趁热尽快将其从坩埚中倒出，以便分离；否则，在冷却过程中，合成试剂变为固态，易粘附于反应容器（即坩埚）内壁，较难将其分离。
 有益效果
针对现有提金剂的合成原料复杂多变，至少有三种以上，进而导致合成反应过程复杂、不易调控的问题，本申请发明人经过多次实验研究发现，仅使用氰酸盐和亚铁盐便可合成能够与氰化钠提金效果相媲美的低毒环保提取剂；该合成原料价格低廉，且合成过程工艺简单、易操作。
总结来说，本发明具有如下优点：仅使用氰酸盐和亚铁盐两种合成原料，焙烧合成工艺简单、易操作；所合成的金银提取剂即提金剂金银浸出率高、浸出速率快、低毒环保、试剂成本低、对矿石适应性强等。
本发明所制得的新型金银提取剂在不改变原有氰化浸出工艺及设备的条件下，可完全替代氰化钠浸出金银矿石。
 附图说明
下面结合附图与具体实施方式对本发明作进一步说明：
图1为本发明中新型金银提取剂的制备工艺流程图。
 本发明的实施方式
如图1所示，一种新型金银提取剂的制备方法，所述金银提取剂的合成原料为氰酸盐和亚铁盐。金银提取剂的制备步骤为：首先，将原料氰酸盐和亚铁盐以一定比例混匀；然后，将混匀的原料置于耐高温坩埚中进行高温焙烧；焙烧结束后，趁热将熔融态合成物从坩埚中倒出，并在空气中自然冷却；最后，将冷却形成的块状固体合成物碎磨成粉末状，即得金银提取剂。本发明所涉及新型金银提取剂的合成原料组成简单、价格低廉，合成工艺易于操作，且所合成的金银提取剂具有金银浸出率高、浸出速率快、低毒环保、对矿石适应性强等优点。
以下结合实施例旨在进一步说明本发明，而非限制本发明。
某金精矿化学组成(wt.%)如表1所示。以下金银浸出实验均使用该金精矿进行研究。
表1
Au* Ag* Fe 2O 3 S SiO 2 CaO MgO Al 2O 3 CuO Pb ZnO
37.6 12.5 20.3 16 47.21 1.64 0.78 14.48 0.061 0.024 0.069
*单位为g/t
实施例1
根据表2中原料配比进行金银提取剂的制备及其浸出效果研究。焙烧条件：空气气氛、升温速率15 ºC/min、焙烧温度700 ºC、保温时间1 h。其他步骤同上。不改变原有氰化浸出工艺及设备。浸出条件：液固比2.5:1、提金剂（金银提取剂）浓度0.3 wt.%、pH 11、转速600 rmp、浸出时间24 h。合成原料配比及金银浸出率如下表2所示。
表2
Figure 658742dest_path_image001
由以上结果可知，原料配比对所合成提取剂的金银浸出效果影响较大，在适宜原料配比条件下（氰酸钠与亚铁氰化钾质量比为4:1），所合成提取剂的金银浸出效果优于氰化钠的。此时，合成提取剂的金浸出率为98.4%，银浸出率为95.1%，高于氰化钠的金浸出率91.3%和银浸出率84.8%。
实施例2
焙烧温度对所合成提取剂金银浸出效果的影响如表3所示。合成原料氰酸钠和亚铁氰化钾质量比为4:1；焙烧条件：空气气氛、升温速率15 ºC/min、保温时间1 h。其他步骤同上。浸出条件：液固比2.5:1、提金剂浓度0.3 wt.%、pH 11、转速600 rmp、浸出时间24h。
表3
编号 焙烧温度/ ºC 金浸出率/% 银浸出率/%
1 500 1.5 0.5
2 600 38.1 22.1
3 650 72.6 68.3
4 700 98.4 95.1
5 750 88.3 80.1
6 800 1.2 1.1
由以上结果可知，焙烧温度对所合成提取剂的金银浸出效果影响较大。过高或过低焙烧温度均不利于提取剂的合成，适宜的焙烧温度为700 ºC。
实施例3
亚铁盐种类对所合成提取剂金银浸出效果的影响如表4所示。合成原料氰酸钠和亚铁盐质量比为4:1；焙烧条件：空气气氛、升温速率15 ºC/min、焙烧温度700 ºC、保温时间1 h。保持其余制备步骤不变。浸出条件：液固比2.5:1、提金剂浓度0.3 wt.%、pH 11、转速600 rmp、浸出时间24 h。
表4
编号 亚铁盐种类 金浸出率/% 银浸出率/%
1 亚铁氰化钾 98.4 95.1
2 氯化亚铁 93.6 89.2
3 硝酸亚铁 86.3 81.5
4 硫酸亚铁 41.6 35.8
由以上结果可知，各类亚铁盐与氰酸钠均可合成具有一定金银提取效果的提取剂，但亚铁氰化钾与氰酸钠所合成金银提取剂的效果最好，金、银浸出率分别达到98.4%和95.1%。
实施例4
某金焙砂的化学组成(wt.%)如下表5所示。
表5
Au* Ag* Fe S As C Sb CaO Al 2O 3 SiO 2 K 2O Ti Zn Pb
105 14.7 23.8 2.28 3.19 0.21 0.08 1.2 13.8 38.2 1.69 0.47 0.28 0.11
*单位为g/t
使用所合成的金银提取剂对表1所示金精矿和表5所示金焙砂两种金矿进行金银浸出实验，结果如表6所示。合成原料氰酸钠和亚铁氰化钾质量比为4:1；焙烧条件：空气气氛、升温速率15 ºC/min、焙烧温度700 ºC、保温时间1 h。浸出条件：液固比2.5:1、提金剂浓度0.3 wt.%、pH 11、转速600 rmp、浸出时间24 h。
表6
编号 矿石类型 金浸出率/% 银浸出率/%
1 金精矿（硫化型） 98.4 95.1
2 金焙砂（氧化型） 99.2 97.3
由以上结果可知，所合成的金银提取剂对硫化型和氧化型金矿石均能取得理想的金银提取效果，故具有较强的矿石适应性。
综上可知，仅使用氰酸钠和亚铁盐便可合成金银提取剂，且所合成的提取剂金银浸出率高、浸出速率快、对矿石适应性强。

Claims (7)

  1. 一种新型金银提取剂的制备方法，其特征在于包括以下步骤：
        （1）选取氰酸盐和亚铁盐为原料，将氰酸盐和亚铁盐混匀；
        （2）将混匀的原料放入耐高温坩埚中焙烧；
        （3）焙烧结束后，趁热将得到的熔融态合成物从坩埚中倒出，并置于空气中自然冷却；
        （4）冷却后，得到块状固体合成物，将块状固体合成物碎磨成粉末状，即得新型金银提取剂。
  2. 根据权利要求1所述的一种新型金银提取剂的制备方法，其特征在于：所述氰酸盐为氰酸钠或氰酸钾。
  3. 根据权利要求1所述的一种新型金银提取剂的制备方法，其特征在于：所述亚铁盐为亚铁氰化钠、亚铁氰化钾、氯化亚铁、硝酸亚铁或硫酸亚铁。
  4. 根据权利要求1所述的一种新型金银提取剂的制备方法，其特征在于：所述氰酸盐和亚铁盐的质量比为3:0.5 – 3:2。
  5. 根据权利要求4所述的一种新型金银提取剂的制备方法，其特征在于：所述氰酸盐和亚铁盐的质量比为4:1。
  6. 根据权利要求1所述的一种新型金银提取剂的制备方法，其特征在于，步骤（2）中，所述焙烧合成工艺条件为：空气气氛、升温速率5 ºC/min – 20 ºC/min、焙烧温度600 ºC – 750 ºC、保温时间0.5 h – 2 h。
  7. 根据权利要求6所述的一种新型金银提取剂的制备方法，其特征在于，所述焙烧温度为700 ºC。
PCT/CN2021/107060 2021-05-14 2021-07-19 金银提取剂的制备方法 WO2022236956A1 (zh)

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CN103981374A (zh) * 2014-05-19 2014-08-13 中国科学院兰州化学物理研究所 一种环境友好型氰酸盐浸金剂的合成方法
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