WO2009149590A1 - 一种高硫高砷难选金精矿常压催化氧化方法 - Google Patents

一种高硫高砷难选金精矿常压催化氧化方法 Download PDF

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WO2009149590A1
WO2009149590A1 PCT/CN2008/001924 CN2008001924W WO2009149590A1 WO 2009149590 A1 WO2009149590 A1 WO 2009149590A1 CN 2008001924 W CN2008001924 W CN 2008001924W WO 2009149590 A1 WO2009149590 A1 WO 2009149590A1
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solid catalyst
acid
ore
refractory gold
gold concentrate
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PCT/CN2008/001924
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French (fr)
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李登新
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东华大学
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Priority to CA2722494A priority Critical patent/CA2722494C/en
Publication of WO2009149590A1 publication Critical patent/WO2009149590A1/zh

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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
    • 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
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • 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
    • C22B11/08—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
    • 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
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • 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 relates to a method for atmospheric pressure catalytic oxidation of high sulfur and high arsenic refractory gold concentrate. Background technique
  • the high-sulfur and high-arsenic refractory gold concentrate treatment processes mainly include pretreatment methods such as calcination oxidation method, pressure oxidation method, atmospheric pressure oxidation method, bacterial oxidation method, and nitric acid catalytic oxidation method.
  • pretreatment methods such as calcination oxidation method, pressure oxidation method, atmospheric pressure oxidation method, bacterial oxidation method, and nitric acid catalytic oxidation method.
  • the main disadvantage is that the extraction rate of precious metals such as gold, silver, platinum and palladium in refractory gold concentrates is low; the comprehensive utilization rate of other elements is also low; the environment is polluted during the process of extracting precious metals; and the process is complicated and costly .
  • the purpose of the invention is to improve the extraction rate of precious metals such as gold, silver, platinum and palladium in refractory gold concentrates and the comprehensive utilization ratio of other elements; at the same time, to reduce environmental pollution during the extraction process; and the process is simple and the equipment cost is low.
  • the present invention provides a method for atmospheric pressure catalytic oxidation of a high sulfur and high arsenic refractory gold concentrate. Its working principle is: Since most molecules have a bond energy of 25 ⁇ 35 kcal/m, and the redox potential of ozone is about 2.07V, the bond energy is 47 kcal/mole, so the ozone is enough to open most molecules.
  • the chemical bond breaks the pyrite and arsenopyrite that encases precious metals such as gold and silver to expose the precious metal.
  • iron, copper and manganese can play a catalytic role and promote the dissolution and conversion of oxygen and ozone in water.
  • the key to the invention is the use of an oxidizing agent and a catalyst, the reaction steps of which are as follows:
  • the reduced state [solid catalyst] can be reoxidized and recycled to indirectly increase the oxygen oxidation rate.
  • the oxidizing agent, the ozone is 0. 1 ⁇ 1. 0 ⁇ / ⁇ , or ozone and air, wherein the ozone is 0. 8 ⁇ 1. 2g / hour and the air is 0. 1 ⁇ L 0 cubic meters / hour, continuous stirring, forming oxidized pulp, reaction time is After 6 to 18 hours, the filtrate and the residue were filtered off to room temperature.
  • the filter residue is mixed with the calcium hydroxide solution, adjusted to a pH of 11 to 12, stirred by adding sodium cyanide for 24 hours, and filtered to extract precious metals from the filtrate.
  • the preparation process of the solid catalyst is: mixing industrial industrial iron, copper, hydrochloric acid or chlorine gas, manganese oxide, aluminum oxide, silicon oxide under normal temperature and normal pressure conditions, and mixing, in the process, if When chlorine gas is used, chlorine gas is continuously supplied to make the final product component percentage of iron 30%, chlorine 30%, oxygen 15%, copper 10%, manganese 5%, silicon 5% and aluminum 5%.
  • the slurry of the refractory gold ore may include hydrochloric acid and sulfuric acid.
  • the invention has the advantages that: the extraction rate of precious metals such as gold and silver in the refractory gold concentrate and the comprehensive utilization ratio of other elements are improved; at the same time, the environmental pollution is reduced in the extraction process; and the process is simple and the equipment cost is low.
  • the leaching rates of gold and silver are 68 ⁇ 98.5% and 80 ⁇ 96%, respectively, and the corresponding leaching rates without direct cyanidation of the above invention steps are less than 40% and 50 ⁇ 60%, respectively.
  • Figure 1 is a flow chart of atmospheric pressure catalytic oxidation of high sulfur and high arsenic refractory gold concentrate.
  • a flow chart of atmospheric pressure catalytic oxidation of high sulfur and high arsenic refractory gold concentrate is carried out, and a sample, a water and a solid catalyst, and sulfuric acid are added in a reactor with a stirrer, and the concentration of the solid catalyst is 151. g/L, the weight ratio of ore to water is 1:10, sulfuric acid is added to pH 1, and it is configured as a slurry of refractory gold ore.
  • the preparation process of the solid catalyst is as follows: industrial iron, copper, manganese oxide, aluminum oxide, silicon oxide, uniform under normal temperature and normal pressure conditions Stirring and mixing, in the process, chlorine gas is continuously supplied to make the final product component percentage of iron 30%, chlorine 30%, oxygen 15%, copper 10%, manganese 5%, silicon 5% and aluminum 5%. .
  • the operation is the same as that in the first embodiment, wherein the solid catalyst is prepared by uniformly mixing industrial iron, copper, hydrochloric acid, manganese oxide, aluminum oxide and silicon oxide under normal temperature and normal pressure conditions.
  • the compositional percentage of the final product is 30% iron, 30% chlorine, 15% oxygen, 10% copper, and 5° manganese. , silicon 5 ° /. And aluminum 5%.
  • the solid catalyst concentration is 280 g / liter, the weight ratio of the ore sample to water is 1: 10, hydrochloric acid is added to the pH of 1, and at a temperature of 100 ° C, ozone and air are continuously introduced into the slurry.
  • the input amount is 1.2 g/hr and 0.4 m3/hr, and the reaction time is 16 hours.
  • the filter residue is mixed with the calcium hydroxide solution, adjusted to pH 12, and stirred by sodium cyanide. Filtered after 24 hours.
  • the leaching rate of gold is 98. 45%
  • the leaching rate of silver is 95. 27%.
  • the operation is the same as that in the first embodiment, wherein the solid catalyst is prepared by uniformly mixing and mixing industrial iron, copper, hydrochloric acid, manganese oxide, aluminum oxide and silicon oxide under normal temperature and normal pressure conditions.
  • the percentage by mass of the final product is 30% iron, 30% chlorine, 15% oxygen, and 10° copper. , 5% manganese, 5% silicon and 5% aluminum.
  • the solid catalyst concentration is 170 g / liter, the weight ratio of the ore sample to water is 1: 6, sulfuric acid is added to pH 3, and the solution is connected to the slurry at a temperature of 70 ° C.
  • the ozone and air are continuously introduced, and the amount of the solution is 1.0 g/hr and 0.8 m3/hr, and the reaction time is 12 hours.
  • the filter residue is mixed with the calcium hydroxide solution, and adjusted to pH 11, add cyanide
  • the sodium was stirred for 24 hours and then filtered.
  • the leaching rate of gold is 88.23%, and the leaching rate of silver is 81.02%.
  • the operation is the same as that in the first embodiment, wherein the solid catalyst is prepared by uniformly mixing and mixing industrial iron, copper, chlorine, manganese oxide, aluminum oxide and silicon oxide under normal temperature and normal pressure.
  • chlorine gas is continuously supplied to make the final product component percentage of iron 30%, chlorine 30%, oxygen 15%, copper 10%, manganese 5%, silicon 5% and aluminum 5%.
  • the solid catalyst concentration is 230 g / liter, the weight ratio of the ore sample to water is 1: 8, hydrochloric acid is added to pH 3, and at 10 (TC temperature conditions, ozone and oxygen are continuously introduced into the slurry, and the pass thereof
  • the input amount is 0.9 g/hr and 1.0 m3/hr, and the reaction time is 8 hours.
  • the filter residue is mixed with the calcium hydroxide solution, adjusted to pH 12, and stirred by sodium cyanide.
  • the leaching rate of silver is 76.2%, and the leaching rate of silver is 92.19%.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)

Description

一种高硫髙砷难选金精矿常压催化氧化方法 技术领域
本发明涉及一种高硫高砷难选金精矿常压催化氧化方法。 背景技术
高硫高砷难选金精矿处理工艺主要有焙烧氧化法、 加压氧化法、 常压氧化法、 细菌 氧化法、 硝酸催化氧化法等预处理方法。 主要缺点在于难选金精矿中金、 银、 铂、 钯等 贵金属的提取率较低； 其他元素综合利用率也较低； 在提取贵金属过程中， 对环境造成 污染； 并且工艺复杂， 成本高。
如果有一种催化剂能在气相中再生， 又在水中的溶解度很高， 它在硫化床表面还原 时阴极电位也高， 则可显著降低硫化矿氧化酸浸所需的温度和氧压， 这是湿法冶金研究 工作的一个重要方向。 发明内容
本发明的目的在于提高难选金精矿中金、 银、 铂、 钯等贵金属的提取率和其他元 素综合利用率； 同时在提取过程中， 减少环境污染； 并且工艺简单， 设备成本较低。
为了达到上述目的， 本发明提供一种高硫高砷难选金精矿常压催化氧化方法。 其 工作原理是： 由于大多数分子的化合键能量为 25〜35千卡 /摩， 而臭氧的氧化还原电势 大约是 2. 07V, 化合键能量为 47千卡 /摩， 因此臭氧足以打开多数分子的化合键， 打破 包裹金、 银等贵金属的黄铁矿和毒砂， 使贵金属裸露出来， 另外铁、 铜、 锰几种元素能 够起到催化作用和促进氧气和臭氧在水中溶解和转化作用。
本发明关键在于使用了氧化剂和催化剂， 其反应步骤如下：
03+02+还原态 [固体催化剂]—0. +氧化态 [固体催化剂]
0. +氧化态 [固体催化剂] +FeS2→FeS04+还原态 [固体催化剂]
其中还原态 [固体催化剂]可以被重新氧化而循环使用， 间接提高氧气氧化速率。
本发明具体步骤如下-
1. 在带有搅拌器的反应釜中一次性加入适量矿样、 固体催化剂和水， 固体催化 剂浓度为 151〜280克 /升， 矿样与水的重量比为 1： 6〜1： 10， 加酸至 pH值 1~3， 配置成难选金矿石的浆液。 . .
2. 在 60〜100°C的温度条件下， 向桨液中连续通入气体氧化剂， 即臭氧和氧气， 其中臭氧为 0. 8〜1. 2克 /小时和氧气为 0. 1〜1. 0立方米 /小时，或着臭氧和空气，其 中臭氧为 0. 8〜1. 2克 /小时和空气为 0. 1〜L 0立方米 /小时，连续不断搅拌，形成氧 化矿浆， 反应时间为 6〜18小时， 然后降至室温过滤得滤液和滤渣。
3. 根据传统提取工艺， 滤渣与氢氧化钙溶液混合， 调至 pH值 11〜12， 加入氰 化钠搅拌 24小时后过滤， 从滤液中提取贵金属。
所述的固体催化剂的制备工艺为： 将工业用铁、铜、盐酸或氯气、氧化锰、氧化铝、 氧化硅在常温、 常压条件下， 均匀搅拌， 混合而成， 在这过程中， 若使用氯气， 则连续 通入氯气， 使其最终产品的成分质量百分比分别为铁 30%、 氯 30%、 氧 15%、 铜 10%、 锰 5%、 硅 5%和铝 5%。
所述的难选金矿石的浆液可包括的酸为盐酸和硫酸。
本发明的优点是： 提高了难选金精矿中金、 银等贵金属的提取率和其他元素综合 利用率； 同时在提取过程中， 减少环境污染； 并且工艺简单， 设备成本较低。 按照国 标测定， 金、 银的浸出率分别为 68〜98. 5%和 80〜96%, 而未经上述发明步骤直接氰化 的对应浸出率分别为小于 40%和 50〜60%。 附图说明
图 1 为高硫高砷难选金精矿常压催化氧化工艺流程图 具体实施方式
下面结合实施例对本发明作进一步详细地阐述。
实施例 1
参考图 1， 为高硫高砷难选金精矿常压催化氧化工艺流程图， 在带有搅拌器的反应 釜中一次性加入矿样、 水和固体催化剂， 及硫酸， 固体催化剂浓度为 151克 /升， 矿样 与水的重量比为 1： 10， 加硫酸至 pH为 1， 配置成难选金矿石的浆液。其中固体催化剂 的制备工艺为： 将工业用铁、 铜、 氧化锰、 氧化铝、 氧化硅在常温、 常压条件下， 均匀 搅拌混合，在这过程中， 连续通入氯气，使其最终产品的成分质量百分比分别为铁 30%、 氯 30%、 氧 15%、 铜 10%、 锰 5%、 硅 5%和铝 5%。
在 90°C的温度条件下， 向浆液中连续通入臭氧和氧气， 其通入量分别为 0. 8克 /小 时和 0. 1立方米 /小时， 连续不断搅拌， 形成氧化矿桨； 反应时间为 8小时， 然后降至 室温过滤得滤液和滤渣； 根据传统提取工艺， 使滤渣与氢氧化钙溶液混合， 调至 pH值 11， 加入氰化钠搅拌 24小时后过滤， 从滤液中提取贵金属， 按照国标测定， 金的浸出 率为 82. 65%, 银的浸出率为 88. 77% 实施例 2
釆用与实施例 1完全相同的步骤操作，其中固体催化剂的制备工艺为：将工业用 铁、 铜、 盐酸、 氧化锰、 氧化铝、 氧化硅在常温、 常压条件下， 均匀搅混合， 使其最 终产品的成分质量百分比分别为铁 30%、 氯 30%、 氧 15%、 铜 10%、 锰 5°/。、 硅 5°/。和铝 5%。
其中固体催化剂浓度为 280克 /升， 矿样与水的重量比为 1： 10, 加盐酸至 pH为 1， 在 100°C的温度条件下， 向浆液中连续通入臭氧和空气， 其通入量分别为 1. 2克 / 小时和 0. 4立方米 /小时， 反应时间为 16小时， 根据传统提取工艺， 使滤渣与氢氧化 钙溶液混合， 调至 pH值 12， 加入氰化钠搅拌 24小时后过滤。 按照国标测定， 金的 浸出率为 98. 45%, 银的浸出率为 95. 27% 实施例 3
釆用与实施例 1完全相同的步骤操作，其中固体催化剂的制备工艺为：将工业用 铁、 铜、 盐酸、 氧化锰、 氧化铝、 氧化硅在常温、 常压条件下， 均匀搅拌混合， 使其 最终产品的成分质量百分比分别为铁 30%、 氯 30%、 氧 15%、 铜 10°/。、 锰 5%、 硅 5%和 铝 5%。
其中固体催化剂浓度为 170克 /升，矿样与水的重量比为 1： 6,加硫酸至 pH为 3， 在 70°C的温度条件下， 向浆液中连
续通入臭氧和空气， 其通入量分别为 1. 0克 /小时和 0. 8立方米 /小时， 反应时间为 12小时， 根据传统提取工艺， 使滤渣与氢氧化钙溶液混合， 调至 pH值 11， 加入氰化 钠搅拌 24小时后过滤。按照国标测定，金的浸出率为 68. 32%,银的浸出率为 81. 02%。 实施例 4
釆用与实施例 1完全相同的步骤操作，其中固体催化剂的制备工艺为：将工业用 铁、 铜、 氯气、 氧化锰、 氧化铝、 氧化硅在常温、 常压条件下， 均匀搅拌混合， 在这 过程中， 连续通入氯气， 使其最终产品的成分质量百分比分别为铁 30%、 氯 30%、 氧 15%、 铜 10%、 锰 5%、 硅 5%和铝 5%。
其中固体催化剂浓度为 230克 /升，矿样与水的重量比为 1： 8，加盐酸至 pH为 3, 在 10(TC的温度条件下， 向浆液中连续通入臭氧和氧气， 其通入量分别为 0. 9克 /小 时和 1. 0立方米 /小时， 反应时间为 8小时， 根据传统提取工艺， 使滤渣与氢氧化钙 溶液混合， 调至 pH值 12， 加入氰化钠搅拌 24小时后过滤。 按照国标测定， 金的浸 出率为 76. 25%, 银的浸出率为 92. 19%。

Claims

权利要求
1. 一种高硫高砷难选金精矿常压催化氧化方法， 其特征在于包括如下步骤：
步骤 1、 在带有搅拌器的反应釜中一次性加入适量矿样、 固体催化剂、 酸和水， 固体催化剂浓度为 151〜280克 /升， 矿样与水的重量比为 1： 6〜1： 10， 加酸至 pH值 1〜3， 配置成难选金矿石的浆液；
步骤 2、 在 60〜100°C的温度条件下， 向浆液中连续通入气体氧化剂： 臭氧和氧 气， 其中臭氧为 0. 8〜1. 2克 /小时和氧气为 0. 1〜1. 0立方米 /小时； 或 着臭氧和空气，其中臭氧为 0. 8〜1. 2克 /小时和空气为 0. 1〜1. 0立方米 /小时， 连续不断搅拌， 形成氧化矿浆， 反应时间为 6〜18小时， 然后降 至室温过滤得滤液和滤渣；
步骤 3、 根据传统提取工艺， 滤渣与氢氧化钙溶液混合， 调至 pH值 11〜12， 加 入氰化钠搅拌 24小时后过滤， 从滤液中提取贵金属。
2. 根据权利要求 1所述的一种高硫高砷难选金精矿常压催化氧化方法，其特征在于， 步骤 1中所述的酸为盐酸或硫酸。
3.根据权利要求 1所述的一种高硫高砷难选金精矿常压催化氧化方法，其特征在于，步 骤 1中所述的固体催化剂的制备工艺为： 将工业用铁、 铜、 盐酸或氯气、 氧化锰、 氧化 铝、 氧化硅在常温、 常压条件下， 均匀搅拌混合， 在这过程中， 若使用氯气， 则连续通 入氯气， 使其最终产品的成分质量百分比分别为铁 30%、 氯 30%、 氧 15%、 铜 10%、 锰 5%、 硅 5%和铝 5%。
PCT/CN2008/001924 2008-06-13 2008-11-25 一种高硫高砷难选金精矿常压催化氧化方法 WO2009149590A1 (zh)

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CA2722494A CA2722494C (en) 2008-06-13 2008-11-25 A method for catalytic oxidation of refractory gold concentrate with high contents of sulfur and arsenic under ordinary pressure

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CN2008100389391A CN101314815B (zh) 2008-06-13 2008-06-13 一种高硫高砷难选金精矿常压催化氧化方法
CN200810038939.1 2008-06-13

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