CN111579338A - Method for measuring gold in secondary utilization waste - Google Patents
Method for measuring gold in secondary utilization waste Download PDFInfo
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- CN111579338A CN111579338A CN202010600177.0A CN202010600177A CN111579338A CN 111579338 A CN111579338 A CN 111579338A CN 202010600177 A CN202010600177 A CN 202010600177A CN 111579338 A CN111579338 A CN 111579338A
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- G—PHYSICS
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to a method for measuring gold in secondary utilization waste, belonging to the technical field of comprehensive utilization of solid waste. The method comprises the steps of preparing waste, preparing a dilute hydrochloric acid extracting agent, mixing stannous chloride and dilute hydrochloric acid to prepare a reducing agent, taking the waste and the dilute hydrochloric acid extracting agent to carry out leaching reaction after mixing, synchronously adding a stannous chloride solution reducing agent, simultaneously heating in a water bath, taking a gold-containing waste leaching material, mixing the gold-containing waste leaching material with a cyanide-free medicament or an environment-friendly medicament or an iodine-potassium iodide gold leaching solution to carry out leaching reaction, synchronously introducing micro-nano bubbles into the cyanide-free or environment-friendly leaching reaction to obtain a gold-free waste leaching material after the leaching reaction is finished, and calculating the leaching rate of gold according to a test result. The method has the advantages that the natural solubility of the jarosite and the stannate is fully exerted, and the improvement of the recovery rate of gold minerals is facilitated; a small amount of stannous chloride mixed solution is added as a reducing agent, the reaction is more sufficient and thorough by heating in a water bath, the leaching rate of gold minerals is ensured, and the gold recovery rate is high.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of solid wastes, and particularly relates to a method for measuring gold in secondary utilization waste.
Background
With the gradual increase of the update rate of electronic products in the society, the generation rate of secondary utilization resources such as electronic garbage and the like is gradually increased. According to the relevant survey information of the domestic social environment management department: the quantity of the electronic garbage generated in China every year accounts for 60.17% of the proportion of the social garbage. Scientists have found that these electronic wastes contain a remarkable amount of "gold mine" which is a resource amount at least as much as gold obtained by mining. It is known that 50 pounds of gold and 2 million pounds of copper can be extracted from one million abandoned mobile phones if the treatment method is proper, and the method is a considerable secondary utilization resource.
However, the current situation of electronic waste treatment has a great problem, and it is known that the yield of electronic waste is 4470 ten thousand tons in 2016 worldwide, the effective recovery rate is 20%, while the environmental-friendly recovery rate of electronic waste in China is only about 10%, which is obviously lower than the average recovery rate of electronic waste worldwide. A series of problems exist in the recovery and treatment processes, firstly, the system design and the loss of a recovery system are eliminated, so that waste electronic garbage in China is in a rough state, a gray industrial chain of individual household recovery and individual workshop treatment is gradually formed, and normal enterprises are difficult to operate; then, the treatment method is improper and low in efficiency, most of the treatment methods adopted are mechanical crushing and sorting treatment methods, such as rough disassembly, strong acid extraction, random landfill, incineration, abandonment and other treatment means, and the regeneration and harmlessness of resource treatment are ignored: finally, the method for measuring the heavy metal elements in the treatment process is inaccurate, the recovery rate is low, and the precious secondary utilization resources are seriously lost.
According to the data, domestic electronic waste is large in generation base number, the effective treatment proportion is low, heavy metal element measurement methods are improper in the treatment process, the problem of large environmental pollution is brought, and the problem of resource waste is also caused. Therefore, the reasonable solid waste treatment method and the heavy metal element gold measurement method not only can carry out harmless treatment on the gold, but also can recycle the useful components in the gold to the maximum extent, meet the requirement of green chemical development and meet the requirement of the market on gold.
Disclosure of Invention
The invention provides a method for measuring gold in secondary utilization waste, aiming at utilizing the existing secondary resources to the maximum extent, effectively measuring the content of the gold in the waste and obtaining higher recovery rate.
The technical scheme adopted by the invention is that the method comprises the following steps:
1) preparing waste materials;
2) mixing concentrated hydrochloric acid with water to prepare a dilute hydrochloric acid extractant with a certain concentration;
3) mixing stannous chloride with dilute hydrochloric acid, and preparing a reducing agent after the stannous chloride is completely dissolved;
4) mixing the waste material with a dilute hydrochloric acid extracting agent, carrying out leaching reaction, synchronously adding a stannous chloride solution reducing agent in the leaching reaction, simultaneously heating in a water bath, and placing the mixture after heating in the water bath for full reaction, thereby obtaining a gold-containing waste material leaching material after completing the leaching reaction;
5) mixing a cyanide-free medicament or an environment-friendly medicament with alkali liquor to prepare an extracting agent; or iodine-potassium iodide gold leaching solution;
6) and mixing the gold-containing waste leaching material with a cyanide-free medicament or an environment-friendly medicament or an iodine-potassium iodide gold leaching solution, carrying out leaching reaction, synchronously introducing micro-nano bubbles into the cyanide-free or environment-friendly leaching reaction to obtain a gold-free waste leaching material subjected to the leaching reaction, and calculating the leaching rate of gold according to a test result.
In the step 1), the waste is mainly complex salt rich in tin, jarosite and the like, the fineness of the waste is-0.074 mm, and the content of the waste is 60-80%.
In the step 2), the concentration of the prepared dilute hydrochloric acid extractant is 4.8-6 mol/L.
In the step 3), the solid-liquid ratio between the mass of the stannous chloride and the volume of the diluted hydrochloric acid is 1: 4-1: 6 g/ml and the concentration of dilute hydrochloric acid is 4.8-6 mol/L.
In the step 4), the solid-liquid ratio between the mass of the waste and the volume of the dilute hydrochloric acid extractant is 1: 10-1: 20 g/ml, wherein the solid-liquid ratio between the mass of the added waste and the volume of the added stannous chloride reducing agent is 10: 0.25-10: 0.35 g/ml, leaching reaction time of 2-3 h, water bath heating temperature of 60-100 ℃, and water bath reaction time of 1-1.5 h.
In the step 5), the concentration of the cyanide-free medicament in the medicament is 0.05-1.0 mol/L; the pH value is 10-12; the cyanide-free medicament is selected from one of amino acid, thiourea, thiosulfate and halogen.
In the step 5), the concentration of the medicament in the environment-friendly medicament is 0.05-1.0 mol/L; the pH value is 10-12; the environment-friendly medicament is selected from one of a cicada gold beneficiation agent, a minjedgkin beneficiation agent and a saint (Sandios) beneficiation agent.
In the step 5), the alkali liquor is an alkali-containing aqueous solution, and the alkali in the alkali liquor is selected from one of sodium hydroxide, calcium hydroxide and calcium oxide;
in the step 5), the iodine-potassium iodide gold leaching solution is prepared from iodine: potassium iodide: water-12: 28: 200 g/g/ml;
the solid-liquid ratio of the adding mass of the waste to the adding volume of the cyanide-free medicament in the step 6) is 1: 2-8 g/ml;
the solid-liquid ratio of the adding mass of the waste to the adding volume of the environment-friendly medicament in the step 6) is 1: 2-8 g/ml;
the solid-liquid ratio between the mass of the added waste and the volume of the iodine-potassium iodide gold leaching solution is 50: 200 g/ml, when the added mass of the waste is less than 50g, 200ml of gold leaching solution is added according to the minimum proportion.
Leaching reaction temperature of the cyanide-free medicament or the environment-friendly medicament in the step 6) is 40-80 ℃, and leaching reaction time is 24-72 h; leaching reaction of an iodine-potassium iodide system at normal temperature for 1.5-3 h;
the diameter of the micro-nano bubbles is 8 nm-8 um;
the gas-liquid mixing ratio when the micro-nano bubbles are generated is 1: 10-1: 30, of a nitrogen-containing gas;
the origin of the micro-nano bubbles is selected from one of air, oxygen or ozone.
The invention can not only carry out harmless treatment on the secondary utilization waste materials, but also recycle the useful components in the waste materials to the maximum extent, adapts to the development requirement of green chemistry and meets the requirement of the market on gold.
For the leaching process, gold in the waste is secondarily utilized, particularly the gold-containing waste of complex double salt forms wrapped gold, so that the leaching is difficult to be thorough and the recovery is complete. The method has the advantages that the recovery rate of gold in the secondary utilization waste is extremely low, the resource loss is serious, and the method for measuring gold needs to be systematically researched, so that the method enhances the reasonable and comprehensive recovery and utilization of gold. The method is beneficial to accurately determining the grade of the gold ore.
The invention has the following advantages and effects: because the process is carried out under the condition of medium acid environment, the natural solubility of the jarosite and the stannate is fully exerted, and the improvement of the recovery rate of gold minerals is facilitated; a small amount of stannous chloride mixed solution is added as a reducing agent, so that the generation of ferric iron is greatly reduced, and the possibility of forming an oxide film so as to form a package is reduced; the water bath heating ensures that the reaction is more sufficient and thorough, is favorable for smooth reaction and ensures the leaching rate of the gold mineral. The process has the advantages of simple operation, low production cost and high gold recovery rate.
Detailed Description
Example 1
The method takes the waste crushed by the circuit board of the washing machine as a sample, and the gold grade of the raw material is 30.58g/t, and the method specifically comprises the following steps:
1) grinding the crushed raw waste sample until the content of the crushed raw waste sample is 62 percent in the range of-0.074 mm;
2) proportioning dilute hydrochloric acid extractant with the concentration of 4.8 mol/L;
3) 2g of stannous chloride and 10ml of dilute hydrochloric acid with the concentration of 4.8mol/L are mixed to form a stannous chloride solution;
4) the dosage of the hydrochloric acid extractant is determined according to the solid-liquid ratio of the mass of the solid added in the waste to the volume of the dilute hydrochloric acid extractant of 1: 10 g/ml, the relative proportion is increased, the dosage of the stannous chloride reducing agent is 10: 0.25, g/ml, relative proportion increased; the leaching reaction time is 2h, the water bath heating temperature is 60 ℃, and the water bath reaction time is 1 h;
5) the environment-friendly agent is a cicada gold beneficiation agent, the concentration of the traditional Chinese medicine agent prepared from the environment-friendly extractant is 0.05mol/l, the alkali in the alkali liquor is sodium hydroxide, and the pH value is adjusted to 10;
6) the solid-liquid ratio of the adding mass of the waste to the adding volume of the cicada is 1: 2, g/ml, the reaction temperature is 50 ℃, the time is 24 hours, the air source of the micro-nano bubbles is air, and the gas-liquid mixing ratio generated by the micro-nano bubbles is 1: 10.
finally, the leaching rate of gold is calculated to reach 91.5 percent according to the test result, and a good recovery index is obtained.
Example 2
The method takes the crushed waste of the mobile phone circuit board as a sample, and the gold grade of the raw material is 38.24g/t, and the method specifically comprises the following steps:
1) grinding the crushed raw waste sample until the content of-0.074 mm accounts for 70 percent;
2) the concentration of the proportioned hydrochloric acid is 5.4 mol/L;
3) 2g of stannous chloride and 10ml of dilute hydrochloric acid with the concentration of 5.4mol/L are mixed to form a stannous chloride solution;
4) the dosage of the hydrochloric acid extractant is determined according to the solid-liquid ratio of the mass of the solid added in the waste to the volume of the dilute hydrochloric acid extractant of 1: 15 g/ml, the relative proportion is increased, and the dosage of the stannous chloride reducing agent is 10: 0.30, g/ml, relative proportion increased. The leaching reaction time is 2.5h, the water bath heating temperature is 80 ℃, and the water bath reaction time is 1.5 h;
5) the cyanogen-free agent is amino acid, the concentration of the cyanogen-free agent in the prepared cyanogen-free extracting agent is 0.2mol/l, alkali in the alkali liquor is calcium oxide, and the pH value is adjusted to be 11;
6) the solid-liquid ratio of the adding mass of the waste to the adding volume of histidine is 1: 2, g/ml, the cyanide-free reaction temperature is 70 ℃, the time is 48 hours, the gas source of the micro-nano bubbles is oxygen, and the gas-liquid mixing ratio generated by the micro-nano bubbles is 1: 20.
finally, the leaching rate of gold is calculated to reach 94.32 percent according to the test result, and a good recovery index is obtained.
Example 3
The method takes the waste material crushed by the computer circuit board as a sample, and the gold grade of the raw material is 44.61g/t, and comprises the following steps:
1) grinding the crushed raw waste sample until the content of-0.074 mm accounts for 80 percent;
2) the concentration of the proportioned hydrochloric acid is 6 mol/L;
3) 2g of stannous chloride and 10ml of dilute hydrochloric acid with the concentration of 6mol/L are mixed to form a stannous chloride solution; 4) the dosage of the hydrochloric acid extractant is determined according to the solid-liquid ratio of the mass of the solid added in the waste to the volume of the hydrochloric acid extractant of 1: 20 g/ml, relative proportion increased. The dosage of the stannous chloride reducing agent is 10 according to the solid-liquid ratio between the mass of the added waste and the volume of the added stannous chloride reducing agent: 0.35, g/ml, relative proportion increased. The leaching reaction time is 3h, the water bath heating temperature is 100 ℃, and the water bath reaction time is 1.5 h;
5) the iodine-potassium iodide gold leaching system is characterized in that the solid-liquid ratio of the solid mass added in the waste to the volume added in the gold leaching extractant is 50: 200, g/ml, relative proportion increased;
6) the reaction temperature is normal temperature and the reaction time is 2 hours;
finally, the leaching rate of gold is calculated to reach 97.83 percent according to the test result, and a good recovery index is obtained.
Example 4
5) The environment-friendly medicament is a Minjie gold extracting agent, the concentration of the medicament in the prepared environment-friendly extracting agent is 0.5mol/l, the alkali in the alkali liquor is sodium hydroxide, and the pH value is adjusted to 11;
6) the solid-liquid ratio of the added mass of the waste to the added volume of the Minjie gold reagent is 1: 5, the ratio of the water to the water is 5 g/ml,
the rest of the procedure was the same as in example 1.
Example 5
5) The environment-friendly agent is a Sandios mineral processing agent, the concentration of the agent in the prepared environment-friendly extracting agent is 1.0mol/l, the alkali in the alkali liquor is sodium hydroxide, and the pH value is adjusted to be 12;
6) the solid-liquid ratio of the added mass of the waste to the added volume of the Minjie gold reagent is 1: 8, the concentration of the active carbon in g/ml,
the rest of the procedure was the same as in example 1.
Example 6
5) The cyanogen-free agent is thiourea, the concentration of the cyanogen-free agent in the prepared cyanogen-free extracting agent is 0.5mol/l, the alkali in the alkali liquor is calcium oxide, and the pH value is adjusted to be 10;
6) the solid-liquid ratio of the adding mass of the waste to the adding volume of the thiourea is 1: 5, the ratio of the water to the water is 5 g/ml,
the rest of the procedure was the same as in example 2.
Example 7
5) The cyanide-free agent is thiosulfate, the concentration of the cyanide-free agent in the prepared cyanide-free extracting agent is 1.0mol/l, the alkali in the alkali liquor is calcium oxide, and the pH value is adjusted to be 12;
6) the solid-liquid ratio of the adding mass of the waste to the adding volume of the thiourea is 1: 8, the concentration of the active carbon in g/ml,
the rest of the procedure was the same as in example 2.
Example 8
5) The cyanogen-free agent is halogen, the concentration of the cyanogen-free agent in the prepared cyanogen-free extracting agent is 0.05mol/l, the alkali in the alkali liquor is calcium oxide, and the pH value is adjusted to be 10;
6) the solid-liquid ratio of the adding mass of the waste to the adding volume of the thiourea is 1: 5, the ratio of the water to the water is 5 g/ml,
the rest of the procedure was the same as in example 2.
Claims (10)
1. A method for measuring gold in secondary utilization waste is characterized by comprising the following steps:
1) preparing waste materials;
2) mixing concentrated hydrochloric acid with water to prepare a dilute hydrochloric acid extractant with a certain concentration;
3) mixing stannous chloride with dilute hydrochloric acid, and preparing a reducing agent after the stannous chloride is completely dissolved;
4) mixing the waste material with a dilute hydrochloric acid extracting agent, carrying out leaching reaction, synchronously adding a stannous chloride solution reducing agent in the leaching reaction, simultaneously heating in a water bath, and placing the mixture after heating in the water bath for full reaction, thereby obtaining a gold-containing waste material leaching material after completing the leaching reaction;
5) mixing a cyanide-free medicament or an environment-friendly medicament with alkali liquor to prepare an extracting agent; or iodine-potassium iodide gold leaching solution;
6) and mixing the gold-containing waste leaching material with a cyanide-free medicament or an environment-friendly medicament or an iodine-potassium iodide gold leaching solution, carrying out leaching reaction, synchronously introducing micro-nano bubbles into the cyanide-free or environment-friendly leaching reaction to obtain a gold-free waste leaching material subjected to the leaching reaction, and calculating the leaching rate of gold according to a test result.
2. The method for measuring gold in secondary used waste according to claim 1, wherein the method comprises the following steps: in the step 1), the waste is mainly complex salt rich in tin, jarosite and the like, the fineness of the waste is-0.074 mm, and the content of the waste is 60-80%.
3. The method for measuring gold in secondary used waste according to claim 1, wherein the method comprises the following steps: in the step 2), the concentration of the prepared dilute hydrochloric acid extractant is 4.8-6 mol/L.
4. The method for measuring gold in secondary used waste according to claim 1, wherein the method comprises the following steps: in the step 3), the solid-liquid ratio between the mass of the stannous chloride and the volume of the diluted hydrochloric acid is 1: 4-1: 6 g/ml and the concentration of dilute hydrochloric acid is 4.8-6 mol/L.
5. The method for measuring gold in secondary used waste according to claim 1, wherein the method comprises the following steps: in the step 4), the solid-liquid ratio between the mass of the waste and the volume of the dilute hydrochloric acid extractant is 1: 10-1: 20 g/ml, wherein the solid-liquid ratio between the mass of the added waste and the volume of the added stannous chloride reducing agent is 10: 0.25-10: 0.35 g/ml, leaching reaction time of 2-3 h, water bath heating temperature of 60-100 ℃, and water bath reaction time of 1-1.5 h.
6. The method for measuring gold in secondary used waste according to claim 1, wherein the method comprises the following steps: in the step 5), the concentration of the cyanide-free medicament in the medicament is 0.05-1.0 mol/L; the pH value is 10-12; the cyanide-free medicament is selected from one of amino acid, thiourea, thiosulfate and halogen.
7. The method for measuring gold in secondary used waste according to claim 1, wherein the method comprises the following steps: in the step 5), the concentration of the medicament in the environment-friendly medicament is 0.05-1.0 mol/L; the pH value is 10-12; the environment-friendly medicament is selected from one of a cicada gold beneficiation agent, a minjedgkin beneficiation agent and a saint (Sandios) beneficiation agent.
8. The method for measuring gold in secondary used waste according to claim 1, wherein the method comprises the following steps: in the step 5), the alkali liquor is an alkali-containing aqueous solution, and the alkali in the alkali liquor is selected from one of sodium hydroxide, calcium hydroxide and calcium oxide.
9. The method for measuring gold in secondary used waste according to claim 1, wherein the method comprises the following steps: in the step 5), the iodine-potassium iodide gold leaching solution is prepared from iodine: potassium iodide: water-12: 28: 200 g/g/ml.
10. The method for measuring gold in secondary used waste according to claim 1, wherein the method comprises the following steps:
the solid-liquid ratio of the adding mass of the waste to the adding volume of the cyanide-free medicament in the step 6) is 1: 2-8 g/ml;
the solid-liquid ratio of the adding mass of the waste to the adding volume of the environment-friendly medicament in the step 6) is 1: 2-8 g/ml;
the solid-liquid ratio between the mass of the waste material added in the step 6) and the volume of the iodine-potassium iodide gold leaching solution is 50: 200 g/ml, when the added mass of the waste is less than 50g, adding 200ml of gold leaching solution according to the lowest proportion;
leaching reaction temperature of the cyanide-free medicament or the environment-friendly medicament in the step 6) is 40-80 ℃, and leaching reaction time is 24-72 h; leaching reaction of an iodine-potassium iodide system at normal temperature for 1.5-3 h;
the diameter of the micro-nano bubbles is 8 nm-8 um;
the gas-liquid mixing ratio when the micro-nano bubbles are generated is 1: 10-1: 30, of a nitrogen-containing gas;
the origin of the micro-nano bubbles is selected from one of air, oxygen or ozone.
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Cited By (3)
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| CN112284959A (en) * | 2020-10-15 | 2021-01-29 | 长春黄金研究院有限公司 | Method for determining influence of gold-robbing substances in gold ore product on gold and silicate-coated gold |
| CN114047218A (en) * | 2021-10-25 | 2022-02-15 | 长春黄金研究院有限公司 | Method for measuring copper in roasted oxidizing slag |
| CN114904878A (en) * | 2022-04-08 | 2022-08-16 | 甘肃省建筑科学研究院(集团)有限公司 | Be used for green building electronic display screen heat recovery system of recycling |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112284959A (en) * | 2020-10-15 | 2021-01-29 | 长春黄金研究院有限公司 | Method for determining influence of gold-robbing substances in gold ore product on gold and silicate-coated gold |
| CN114047218A (en) * | 2021-10-25 | 2022-02-15 | 长春黄金研究院有限公司 | Method for measuring copper in roasted oxidizing slag |
| CN114904878A (en) * | 2022-04-08 | 2022-08-16 | 甘肃省建筑科学研究院(集团)有限公司 | Be used for green building electronic display screen heat recovery system of recycling |
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