CN114561552A - Method for recovering noble metal through atmospheric pressure plasma treatment - Google Patents
Method for recovering noble metal through atmospheric pressure plasma treatment Download PDFInfo
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- CN114561552A CN114561552A CN202210347551.XA CN202210347551A CN114561552A CN 114561552 A CN114561552 A CN 114561552A CN 202210347551 A CN202210347551 A CN 202210347551A CN 114561552 A CN114561552 A CN 114561552A
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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
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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
- C22B11/042—Recovery of noble metals from waste materials
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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Abstract
The invention discloses a method for recovering noble metals by atmospheric pressure plasma treatment, and particularly relates to the field of noble metal recovery. The method comprises the following specific steps: the method comprises the steps of placing a precious metal material containing ruthenium and iridium in an atmospheric pressure low-temperature plasma reduction device, carrying out atmospheric pressure low-temperature plasma treatment on the precious metal material under the condition of atmospheric pressure and under the atmosphere of chlorine gas by using a certain power, converting a precious metal simple substance or a precious metal oxide which is not easy to dissolve in aqua regia into a chloride which is easy to dissolve in aqua regia, and refining and purifying to obtain different precious metal chlorides. The invention adopts a novel precious metal material pretreatment mode, so that precious metals are more easily dissolved in the king water to achieve the purpose of improving the precious metal recovery efficiency. In the whole pretreatment process, the pollution to the environment is less, and the energy consumption is less; and finally, the content of noble metals ruthenium and iridium which can be dissolved in aqua regia is higher, and the method has more excellent economic benefit.
Description
The technical field is as follows:
the invention relates to a novel method for recovering noble metals by atmospheric pressure plasma treatment, which is used for the recovery treatment of the noble metals.
Background art:
the noble metal is mainly 8 metal elements such as iridium and ruthenium group metal, and the noble metal has stronger chemical stability, so that the noble metal is not easy to react with other substances. The application cost of the noble metal is higher due to the characteristics of rarity and difficult exploitation of the noble metal, so that the noble metal can be recycled through secondary recovery, the recycling of the noble metal can be effectively realized, the cost is reduced, the resources are saved, and the secondary recovery of the noble metal is an essential module in the industrial process. The main current technologies for secondary recovery of precious metals include pyrogenic treatment and wet treatment.
The basic principle of the pyrogenic process is that the noble metal is melted in other metal smelting materials or molten salts by using a metallurgical furnace for high-temperature heating and stripping of nonmetal, and then separated. The pyrogenic process has the greatest advantages of simple operation and high recovery rate. However, in comparison, the pyrogenic process treatment technology consumes more energy, causes more pollution to the environment, easily produces harmful gas and solid waste, and the treatment of harmful gas and the treatment of waste are troublesome links in the pyrogenic process technology, and particularly under the current development concept of environmental protection, the pyrogenic process treatment technology has been gradually eliminated by times.
The wet processing technology is to dissolve a metal mixture by using strong acid and other chemical substances to obtain a metal and nonmetal dissolved solution, and then reduce the metal and nonmetal dissolved solution into noble metal by using a chemical method. The wet treatment technique involves the separation of metals from the liquid phase by precipitation, displacement, ion exchange, etc. of the leachate. Compared with the pyrogenic process, the wet process technology has more diversified production processes, and different treatment technologies have different advantages, and the wet process technology is the main method for recovering precious metals at present.
The traditional wet process has the advantages of low cost, environmental protection, high efficiency and the like and is widely applied, but the recovery rate of the precious metals is low because the precious metal simple substances or oxides are difficult to dissolve in the king water.
Plasma is the fourth state of matter, macroscopically electrically neutral, and microscopically composed of positive and negative ions, free electrons, ground or excited particles. When the temperature of the neutral gas rises to a certain degree, collision occurs among particles, a large number of ionization processes are generated, and finally plasma is formed. The plasma is confined by an electric or magnetic field and has no fixed form. The particle-to-particle forces in the plasma are long range electromagnetic forces. In the range of the force path, there are a large number of particles, and self-consistent interactions occur between the particles, so that the motion of the plasma appears as a collective motion. The plasma has a large number of excited atoms (or molecules), high-energy electrons and the like which can interact with other particles, so that the plasma has active chemical properties.
The plasma is further divided into high-temperature plasma and low-temperature plasma, wherein the discharge modes of the low-temperature plasma mainly include glow discharge, corona discharge, dielectric barrier discharge, radio frequency discharge and the like. Glow discharge: the glow discharge is a low pressure discharge, typically less than 10mbar, and therefore the reduced electric field strength can be very high. Due to their high energy, electrons excite neutral atoms and molecules, and produce a unique glow for each gas. Corona discharge: the corona discharge is the local self-sustaining discharge of gas in a non-uniform electric field, and the gas is ionized and excited near an electrode with a small curvature radius because the local electric field intensity is higher than the ionization field intensity of the gas, so that the corona discharge is generated. Dielectric barrier discharge: dielectric Barrier Discharge (DBD), also known as "silent discharge," is a discharge at a pressure typically near atmospheric pressure (0.1 to 1 atm), with a dielectric layer (typically quartz, glass, ceramic, and polymeric materials) placed between the electrodes. Radio frequency discharge: radio Frequency (RF) discharges are also known as high frequency glow discharges. The discharge pressure is usually low. The RF field accelerates free electrons and collisions with background gas molecules, and these inelastic collisions can produce a variety of high-velocity reactive particles.
The atmospheric pressure plasma does not need vacuum conditions, the equipment manufacturing and maintenance cost is reduced, the energy consumption is low, and plasma active particles, free radicals and the like with higher concentration can be generated. The uniform atmospheric pressure discharge plasma has the advantages of high electron temperature, low ion temperature, uniform energy distribution and the like besides the advantages, so the uniform atmospheric pressure discharge plasma is widely applied to the fields of medicine, chemistry, material surface coating, film deposition, volatile organic compound treatment and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-efficiency recovery method of precious metal materials.
The technical scheme adopted by the invention is as follows:
a method for processing and recovering noble metals by atmospheric pressure plasma, wherein processing and recovering equipment comprises an atmospheric pressure plasma device consisting of a high-voltage alternating-current power supply, a transformer, a plasma reactor and a tail gas absorption bottle, a high-voltage electrode on the reactor is connected with the high-voltage power supply through a high-voltage cable, an electrode at the other end is grounded, the reactor is respectively connected with a chlorine cylinder and the tail gas absorption bottle by polytetrafluoroethylene tubes, and the method comprises the following steps:
(1) atmospheric low-temperature plasma treatment: placing a small amount of noble metal material into an atmospheric pressure plasma device, performing chlorine gas replacement under the atmospheric pressure condition, and after the gas replacement is finished, treating the noble metal material in the quartz tube by using an atmospheric pressure plasma with the power of 100 plus 500W for 0.5-5 h to obtain a pretreated noble metal material A;
(2) dissolution of precious metal material: placing the precious metal material A pretreated in the step (1) in a beaker, and mixing the precious metal material A: adding corresponding aqua regia in a mass ratio of 2: 1-1: 10, then placing on an electronic universal furnace for heating, boiling, and finally cooling at room temperature for 2 hours to obtain a precious metal filtrate B;
(3) filtering the precious metal filtrate obtained in the step (2) by using filter paper to obtain precious metal filtrate finally used for separation and refining.
The method uses the atmospheric pressure low-temperature plasma preparation technology to convert the precious metal simple substance or oxide which is difficult to dissolve in the aqua regia into the precious metal chloride which is easy to dissolve in the aqua regia.
The noble metal in the noble metal material comprises simple substances of ruthenium and iridium and oxides thereof.
After the plasma pretreatment, the dissolution rate of the noble metal material in the aqua regia can be effectively increased.
The discharge form of the low-temperature plasma is dielectric barrier discharge.
The invention has the following beneficial effects:
1. the whole experimental process is environment-friendly and efficient, the operation is simple, and the equipment manufacturing and maintenance cost is reduced;
2. the method finally improves the recovery efficiency of the noble metal by improving the dissolution rate of the noble metal in the aqua regia, and has better economic benefit.
Description of the drawings:
fig. 1 is a schematic structural view of a reaction apparatus in an embodiment according to the present invention.
Fig. 2 is a schematic structural view of an atmospheric pressure plasma device according to an embodiment of the present invention.
The specific implementation mode is as follows:
the present invention is described in further detail below with reference to examples. The following examples are merely illustrative of the present invention and should not be construed as limiting the scope of the invention. The invention is not described in the specification of specific technology or conditions, according to the field literature described in the technology or conditions or according to the product specification. The materials or equipment used are not indicated by manufacturers, and all are conventional products available by purchase.
A novel atmospheric pressure plasma process for the recovery of noble metals from a noble metal-containing feedstock containing ruthenium and iridium in solid form. Which comprises the following steps:
the method comprises the following steps: the pretreatment method comprises the following steps: (atmospheric pressure low temperature plasma processing) a small amount of noble metal materials are put into an atmospheric pressure low temperature plasma device, chlorine is led into the reaction device through a polytetrafluoroethylene tube under atmospheric pressure for chlorine replacement, and after the gas replacement is finished, the noble metal materials are reduced for 0.5h-5h by low temperature plasma. After the treatment is completed, the precious metal material is taken out.
Step two: dissolving a precious metal material: placing the noble metal material subjected to the atmospheric pressure low-temperature plasma treatment in a beaker, and mixing the noble metal material: the mass ratio of the aqua regia is 2: 1-1: adding aqua regia at a ratio of 10, heating in an electronic universal furnace, boiling, cooling at room temperature for 2 hr, and filtering with filter paper.
Step three: and analyzing the dissolution rate of the precious metal material.
The material containing the noble metal is a raw material of a noble metal simple substance or a noble metal oxide containing ruthenium and iridium.
In the first step, the replacement time of the chlorine is at least 20min,
in the second step, after the aqua regia is added, boiling is carried out on an electronic universal furnace for 15-20min,
and in the third step, the mass of the precious metal materials before and after dissolution is weighed.
By adopting the technical scheme, the novel method for recovering the noble metal by the atmospheric pressure plasma treatment, disclosed by the invention, is characterized in that a noble metal simple substance or oxide which is difficult to dissolve in the aqua regia is converted into a noble metal chloride which is easy to dissolve in the aqua regia after being treated by the chlorine plasma, so that the dissolution rate of a noble metal material in the aqua regia is improved, the recovery efficiency of the noble metal is improved, the noble metal in the noble metal material can be fully recovered and utilized, the resource waste is reduced, and the noble metal resource is recovered to the maximum extent.
Example 1:
1. a small amount of a noble metal material was taken and weighed to 1 g.
2. And (3) placing the reaction product into a low-temperature plasma device, introducing chlorine gas into the reaction device through a polytetrafluoroethylene tube under atmospheric pressure, and performing chlorine gas replacement for at least 20 min.
3. After the gas replacement is finished, a power supply part is turned on, an alternating current power supply and a transformer are turned on, and the noble metal material is subjected to low-temperature plasma 100W treatment for 0.5h in a quartz tube. The quartz tube, the stainless steel bar and the copper mesh form a dielectric barrier discharge mode. The gas washing device is used for washing away harmful gases generated in the reaction process. After the treatment is completed, the precious metal material is taken out.
4. Placing the noble metal material subjected to low-temperature plasma treatment in a beaker, and mixing the noble metal material: the mass ratio of the aqua regia is 1: 6, adding the corresponding aqua regia.
5. Heating in an electronic universal furnace, and boiling.
6. Cooling for 2h at room temperature, and then filtering with filter paper to obtain the precious metal filtrate for separation and refining.
7. The undissolved precious metal material is then weighed and compared to the precious metal material before dissolution.
Example 2:
1. a small amount of a noble metal material was taken and weighed to 1 g.
2. Placing into a low-temperature plasma device, introducing chlorine into the reaction device through a polytetrafluoroethylene tube under atmospheric pressure, and performing chlorine replacement for at least 20 min;
3. after the gas replacement is finished, a power supply part is turned on, an alternating current power supply and a transformer are turned on, and the noble metal material is subjected to low-temperature plasma 200W treatment for 0.5h in a quartz tube. The quartz tube, the stainless steel bar and the copper mesh form a dielectric barrier discharge mode. The gas washing device is used for washing away harmful gases generated in the reaction process. After the treatment is completed, the precious metal material is taken out.
4. Placing the noble metal material subjected to low-temperature plasma treatment in a beaker, and mixing the noble metal material: the mass ratio of the aqua regia is 1: 6, adding the corresponding aqua regia.
5. Heating in an electronic universal furnace, and boiling.
6. Cooling for 2h at room temperature, and then filtering with filter paper to obtain the precious metal filtrate for separation and refining.
7. The undissolved precious metal material is then weighed and compared to the precious metal material before dissolution.
Example 3:
1. a small amount of a noble metal material was taken and weighed to 1 g.
2. And (3) placing the reaction product into a low-temperature plasma device, introducing chlorine into the reaction device through a polytetrafluoroethylene tube under atmospheric pressure, and performing chlorine replacement for at least 20 min.
3. After the gas replacement is completed, the power supply part is turned on, the alternating current power supply and the transformer are turned on, and the noble metal material is subjected to low-temperature plasma 200W treatment for 1h in the quartz tube. The quartz tube, the stainless steel bar and the copper mesh form a dielectric barrier discharge mode. The gas washing device is used for washing away harmful gases generated in the reaction process. After the treatment is completed, the precious metal material is taken out.
4. Placing the noble metal material subjected to low-temperature plasma treatment in a beaker, and mixing the noble metal material: the mass ratio of the aqua regia is 1: 6, adding the corresponding aqua regia.
5. Heating in an electronic universal furnace, and boiling.
6. Cooling for 2h at room temperature, and then filtering with filter paper to obtain the precious metal filtrate for separation and refining.
7. The undissolved precious metal material is then weighed and compared to the precious metal material before dissolution.
Example 4:
1. a small amount of a noble metal material was taken and weighed to 1 g.
2. And (3) placing the reaction product into a low-temperature plasma device, introducing chlorine gas into the reaction device through a polytetrafluoroethylene tube under atmospheric pressure, and performing chlorine gas replacement for at least 20 min.
3. After the gas replacement is completed, the power supply part is turned on, the alternating current power supply and the transformer are turned on, and the noble metal material is subjected to low-temperature plasma 200W treatment for 2h in the quartz tube. The quartz tube, the stainless steel bar and the copper mesh form a dielectric barrier discharge mode. The gas washing device is used for washing away harmful gases generated in the reaction process. After the treatment is completed, the precious metal material is taken out.
4. Placing the noble metal material subjected to low-temperature plasma treatment in a beaker, and mixing the noble metal material: the mass ratio of the aqua regia is 1: 6, adding corresponding aqua regia.
5. Heating in an electronic universal furnace, and boiling.
6. Cooling for 2h at room temperature, and then filtering with filter paper to obtain the precious metal filtrate for separation and refining.
7. The undissolved precious metal material is then weighed and compared to the precious metal material before dissolution.
Example 5:
1. a small amount of precious metal material was taken and weighed 5 g.
2. And (3) placing the reaction product into a low-temperature plasma device, introducing chlorine gas into the reaction device through a polytetrafluoroethylene tube under atmospheric pressure, and performing chlorine gas replacement for at least 20 min.
3. After the gas replacement is completed, the power supply part is turned on, the alternating current power supply and the transformer are turned on, and the noble metal material is subjected to low-temperature plasma 200W treatment for 1h in the quartz tube. The quartz tube, the stainless steel bar and the copper mesh form a dielectric barrier discharge mode. The gas washing device is used for washing away harmful gases generated in the reaction process. After the treatment is completed, the precious metal material is taken out.
4. Placing the noble metal material subjected to low-temperature plasma treatment in a beaker, and mixing the noble metal material: the mass ratio of the aqua regia is 1: 6, adding corresponding aqua regia.
5. Heating in an electronic universal furnace, and boiling.
6. Cooling for 2h at room temperature, and then filtering with filter paper to obtain the precious metal filtrate for separation and refining.
7. The undissolved precious metal material is then weighed again and compared with the precious metal material before dissolution.
The following data can be derived from examples 1 to 5:
as can be seen from the above table, the methods of plasma pretreatment of the precious metal materials to increase the precious metal recovery rate of examples 1-5 all increased the dissolution rate of the precious metal in aqua regia. The method has the advantages that the chlorine plasma is used for treating the noble metal material, so that the elementary substances or oxides of ruthenium and iridium in the noble metal material can be effectively converted into chlorides, the dissolution rate of the noble metal in the aqua regia is improved, and the recovery rate of the noble metal material is finally improved. The method has the advantages of simple operation, good leaching effect, high recovery rate and environmental friendliness; meanwhile, the experimental equipment does not need vacuum conditions, and the manufacturing and maintenance cost of the equipment is reduced.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. The utility model provides a method of atmospheric pressure plasma processing recovery noble metal, processing recovery plant includes the atmospheric pressure plasma device that high voltage AC power supply, transformer, plasma reactor, tail gas absorption bottle constitute, the reactor on the high voltage electrode pass through high tension cable and be connected with high voltage power supply, the electrode earth connection of the other end, the reactor adopts polytetrafluoroethylene pipe to connect chlorine cylinder and tail gas absorption bottle respectively, its characterized in that: the method comprises the following steps:
atmospheric pressure low-temperature plasma treatment: taking a small amount of noble metal material, placing the noble metal material into an atmospheric pressure plasma device, performing chlorine gas replacement under the atmospheric pressure condition, and after the gas replacement is finished, treating the noble metal material in the quartz tube by using 100-500W atmospheric pressure plasma for 0.5-5 h to obtain a pretreated noble metal material A;
(2) dissolution of precious metal material: placing the precious metal material A pretreated in the step (1) in a beaker, and mixing the precious metal material A: adding corresponding aqua regia according to the mass ratio of 2: 1-1: 10, then placing on an electronic universal furnace for heating, boiling, and finally cooling for 2 hours at room temperature to obtain precious metal filtrate B;
(3) filtering the precious metal filtrate obtained in the step (2) by using filter paper to obtain precious metal filtrate finally used for separation and refining.
2. The method of claim 1, wherein: the preparation method comprises the steps of converting a precious metal simple substance or oxide which is difficult to dissolve in aqua regia into a precious metal chloride which is easy to dissolve in aqua regia by using an atmospheric pressure low-temperature plasma preparation technology.
3. The method of claim 1, wherein: the noble metal in the noble metal material comprises simple substances of ruthenium and iridium and oxides thereof.
4. The method of claim 1, wherein: after the plasma pretreatment, the dissolution rate of the noble metal material in the aqua regia can be effectively increased.
5. The method of claim 1, wherein: the discharge form of the low-temperature plasma is dielectric barrier discharge.
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Citations (5)
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US20130177487A1 (en) * | 2010-06-22 | 2013-07-11 | Anglo Platinum Management Services (Proprietary) Limited | Upgrading of precious metals concentrates and residues |
CN106536766A (en) * | 2014-06-19 | 2017-03-22 | 耶达研究及发展有限公司 | Method for platinum group metals recovery from spent catalysts |
US20200063237A1 (en) * | 2018-08-21 | 2020-02-27 | Robert Ten | Method and Apparatus for Extracting High-Purity Gold from Ore |
CN111433377A (en) * | 2017-11-01 | 2020-07-17 | 耶达研究及发展有限公司 | Method for recovering and extracting gold from electronic waste or gold-containing minerals, ores and sands |
CN113430376A (en) * | 2021-07-06 | 2021-09-24 | 湖南省南铂新材料有限公司 | Method for efficiently separating noble metals in solution and preparing high-purity noble metals |
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- 2022-04-03 CN CN202210347551.XA patent/CN114561552A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US20130177487A1 (en) * | 2010-06-22 | 2013-07-11 | Anglo Platinum Management Services (Proprietary) Limited | Upgrading of precious metals concentrates and residues |
CN106536766A (en) * | 2014-06-19 | 2017-03-22 | 耶达研究及发展有限公司 | Method for platinum group metals recovery from spent catalysts |
CN111433377A (en) * | 2017-11-01 | 2020-07-17 | 耶达研究及发展有限公司 | Method for recovering and extracting gold from electronic waste or gold-containing minerals, ores and sands |
US20200063237A1 (en) * | 2018-08-21 | 2020-02-27 | Robert Ten | Method and Apparatus for Extracting High-Purity Gold from Ore |
CN113430376A (en) * | 2021-07-06 | 2021-09-24 | 湖南省南铂新材料有限公司 | Method for efficiently separating noble metals in solution and preparing high-purity noble metals |
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