CN113652555A - Recovery method and recovery system of aluminum-containing precious metal raw material - Google Patents
Recovery method and recovery system of aluminum-containing precious metal raw material Download PDFInfo
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- CN113652555A CN113652555A CN202110935583.7A CN202110935583A CN113652555A CN 113652555 A CN113652555 A CN 113652555A CN 202110935583 A CN202110935583 A CN 202110935583A CN 113652555 A CN113652555 A CN 113652555A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 76
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000002994 raw material Substances 0.000 title claims abstract description 75
- 239000010970 precious metal Substances 0.000 title claims abstract description 74
- 238000011084 recovery Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 73
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000001257 hydrogen Substances 0.000 claims abstract description 71
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 71
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 70
- 239000007789 gas Substances 0.000 claims abstract description 69
- 238000006243 chemical reaction Methods 0.000 claims abstract description 62
- 238000003756 stirring Methods 0.000 claims abstract description 45
- 239000007788 liquid Substances 0.000 claims abstract description 44
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 39
- 238000012544 monitoring process Methods 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- 230000001276 controlling effect Effects 0.000 claims description 4
- 239000008236 heating water Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 239000010865 sewage Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 2
- 239000002699 waste material Substances 0.000 abstract description 12
- 239000000243 solution Substances 0.000 description 46
- 239000000047 product Substances 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 238000004880 explosion Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 230000002159 abnormal effect Effects 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 206010010904 Convulsion Diseases 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000036461 convulsion Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000011152 fibreglass Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012806 monitoring device Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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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
-
- 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
-
- 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
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- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
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Abstract
The invention discloses a method for recovering an aluminum-containing precious metal raw material, which comprises the following steps: putting an aluminum-containing precious metal raw material into a first container with a plurality of water permeable holes, and then placing the first container into a second container; adding hot water to the second vessel without the precious metal raw material in the first vessel, followed by continuous stirring; after the tail gas treatment equipment is in a state of sucking and treating tail gas, starting to add reaction liquid into the second container, so that aluminum in the precious metal raw material and the reaction liquid start to react and generate hydrogen; continuously monitoring, stopping stirring and adding the reaction liquid when the monitored value exceeds a preset value, and separating the aluminum-containing precious metal raw material in the first container from the solution in the second container; and after the reaction of the aluminum-containing noble metal raw material in the first container is finished, performing solid-liquid separation to obtain a product. The invention also discloses a recovery system of the aluminum-containing precious metal raw material, which can safely recover the precious metal in the aluminum-containing waste.
Description
Technical Field
The invention relates to the technical field of precious metal recovery, in particular to a recovery method and a recovery system of an aluminum-containing precious metal raw material.
Background
In some precious metal processing or industrial manufacturing which needs to use precious metals as raw materials, waste materials mixed with precious metals and aluminum are generated, when the amount of the waste materials is large, the total amount of the precious metals contained in the waste materials is considerable, if the waste materials are directly discharged to be used as garbage disposal, the waste exists, particularly, the naturally stored metals such as platinum and ruthenium are limited in inventory and are increasingly exhausted, so that the precious metals in the recovered waste materials not only have economic benefits, but also have environmental protection benefits.
In the prior art, a common method is to adopt a suitable reaction solution to react impurities except noble metals with the reaction solution to form a liquid, and then continuously separate solid noble metals from the liquid solution. Among them, in the case of the noble metal scrap containing a large amount of aluminum, aluminum can be dissolved by using an acid or a base, and the noble metal having more stable chemical properties is difficult to react with the acid or the base.
However, most of the acid or alkali which can react with aluminum is very corrosive, and the manual operation is very dangerous. In addition, the temperature of the container is too high due to the large temperature rise in the reaction process; in addition, a large amount of hydrogen generated by the reaction is easy to gather indoors and is easy to explode, so that greater potential safety hazard is formed. Therefore, the problems bring great difficulty to the precious metal recovery of the aluminum-containing precious metal waste, and the conventional method can only adopt manual small-batch treatment, so that the personal safety of field operators is difficult to ensure, and the market recycling of large-batch waste is difficult to meet.
Disclosure of Invention
In order to overcome some defects of the prior art, the invention aims to provide a method and a system for recovering a precious metal raw material containing aluminum, which can safely recover precious metals in aluminum-containing waste materials.
The purpose of the invention is realized by adopting the following technical scheme:
a method for recovering an aluminum-containing precious metal raw material comprises the following steps:
feeding: putting an aluminum-containing precious metal raw material into a first container with a plurality of water permeable holes, and then placing the first container into a second container;
adding hot water: adding hot water of 50-70 ℃ into the second container, so that the hot water enters the first container through the water permeable holes, the liquid level of the hot water is less than that of the precious metal raw material in the first container, and continuously stirring after the addition is finished;
adding a reaction solution: starting a tail gas treatment device communicated with the second container, and starting to add reaction liquid into the second container after detecting that the tail gas treatment device is in a tail gas suction treatment state, so that aluminum in the precious metal raw material and the reaction liquid start to react and generate hydrogen;
safety monitoring: continuously obtaining a monitored value of at least one of the discharged tail gas and/or the hydrogen concentration above the second container, the solution temperature in the first container and the solution liquid level in the first container in all the steps, stopping stirring and adding the reaction liquid when the monitored value exceeds a preset value, and separating the aluminum-containing precious metal raw material in the first container from the solution in the second container;
unloading and recovering: and after the reaction of the aluminum-containing noble metal raw material in the first container is finished, separating the noble metal solid which cannot react from the residual solution to obtain a primary recovery product of the noble metal.
Further, a hot water pipeline is communicated with the second container, and the hot water adding step specifically comprises the following steps:
the control center controls the electromagnetic valve and the proportion regulating valve on the hot water pipeline, hot water of 50 ℃ to 70 ℃ is added into the second container at the preset total heating water amount and speed, the hot water enters the first container through the water permeable hole, the liquid level height in the second container is detected through the liquid level meter, the liquid level is enabled to be free of the precious metal raw material in the first container, and continuous stirring is started after the adding is finished.
Further, a compressed air pipeline is communicated with the second container, and in the hot water adding step, stirring is performed in an air stirring mode, wherein the air stirring specifically comprises the following steps: the control center opens the electromagnetic valve on the compressed air pipeline and inputs the compressed air into the bottom of the second container, thereby playing the role of stirring.
Furthermore, a pressure reducing valve and an oil-water separator are connected to the compressed air pipeline, and compressed air is decompressed by the pressure reducing valve and is input to the bottom of the second container after oil is separated by the oil-water separator.
Further, a reaction solution pipeline is communicated with the second container, and the step of adding the reaction solution into the second container specifically comprises the following steps:
the control center controls the electromagnetic valve and the proportion regulating valve on the reaction liquid pipeline to add the reaction liquid at the preset total acid adding amount and rate.
And further, a tail gas pipeline is communicated with the second container, the tail end of the tail gas pipeline is connected with a tail gas treatment device, and in the reaction liquid adding step, whether the tail gas treatment device is in a state of sucking and treating tail gas or not is judged by detecting the wind pressure in the tail gas pipeline.
Further, the second container is equipped with the discharge valve, and the outside is equipped with the pressure filter and communicates with the discharge valve, unload and retrieve the step and specifically include: after the reaction of the aluminum-containing noble metal raw material in the first container is finished, opening a discharge valve of the second container, starting the filter press, conveying a mixture of the noble metal solid which cannot react and the solution to the filter press for filter pressing, conveying filter-pressed sewage through a pipeline to leave centralized treatment, and carrying out refining recovery after the noble metal solid obtained by filter pressing of the filter press is a primary recovery product and washing and drying the product.
Furthermore, an exhaust fan communicated with the outside is further arranged in the space where the first container, the second container and the tail gas pipeline are located, and the exhaust fan is opened in the whole process or is opened when the monitoring value exceeds a preset value.
Further, the unloading and recovering step is followed by a production stop step as follows:
stopping adding the reaction liquid, separating the noble metal raw material in the first container from the solution in the second container, stopping stirring, and finally closing the tail gas treatment equipment.
A system for recovering an aluminum-containing precious metal source material, comprising:
the reaction device comprises a first container and a second container, wherein the first container is provided with a plurality of through holes and is used for containing an aluminum-containing precious metal raw material, and the first container is movably arranged in the second container;
a hot water pipe, which is communicated with the second container and is used for leading hot water with the temperature of 50-70 ℃ into the second container;
the reaction liquid pipeline is communicated with the second container and is used for introducing the reaction liquid into the second container;
a lifting device, the lower end of which is connected with the first container, and is used for lifting or lowering the first container so as to contact or separate the first container with or from the liquid in the second container;
a tail gas pipeline communicated with the second container and used for discharging tail gas in the second container;
the detection device comprises at least one of a liquid level sensor, a hydrogen concentration sensor and a temperature sensor, wherein the liquid level sensor detects the liquid level height in the second container, the hydrogen concentration sensor detects the hydrogen concentration right above the tail gas pipeline and/or the second container, and the temperature sensor detects the liquid temperature in the second container;
a control center electrically connected to the lifting device and the detection device, the control center configured to:
when the value detected by one of the liquid level sensor, the hydrogen concentration sensor or the temperature sensor exceeds a preset value, the device is controlled to lift the first container, so that the precious metal raw material containing aluminum in the first container is separated from the solution in the second container.
Further, an electromagnetic valve is arranged on the hot water pipeline, an electromagnetic valve is also arranged on the reaction liquid pipeline, the control center is electrically connected with the electromagnetic valve and the proportion regulating valve, and the control center is configured to:
and when the value detected by one of the liquid level sensor, the hydrogen concentration sensor or the temperature sensor exceeds a preset value, controlling the electromagnetic valve to be closed.
According to the method and the device for recovering the aluminum-containing noble metal raw material, the aluminum-containing noble metal raw material is loaded by the first container, the hot water and the reaction liquid are loaded by the second container, the aluminum-containing noble metal raw material can be conveniently separated from the reaction liquid, so that the reaction is stopped and the hydrogen is generated, and the safety and the controllability are stronger.
In addition, the sequence of each link of the method is very important, firstly, a large amount of hot water is added before the reaction liquid is added, and stirring is started, so that the reaction liquid is directly mixed with a large amount of hot water in a stirring state when being added, and the over-violent reaction caused by over-high acid concentration is prevented; moreover, it is in the state of suction treatment tail gas still to need to detect tail gas treatment facility earlier before adding the reaction liquid, has guaranteed normal continuous convulsions, prevents that hydrogen concentration is too high in normal production reaction.
More importantly, the safety detection step of the invention monitors the hydrogen concentration in the tail gas discharged in the whole reaction process, and can also monitor the concentration of escaped hydrogen (the hydrogen density is less than that of air, and if escaped, the escaped hydrogen inevitably flows upwards), so as to avoid the hydrogen concentration from exceeding the threshold value to reach the explosion point to threaten the safety of equipment and personnel; in addition, the temperature of the solution in the first container can be monitored, and when the temperature of the solution is too high, the reaction is proved to be too violent, and a runaway condition is possible; when the liquid level in the first container is too high, the highly corrosive reaction liquid will escape, causing danger and contamination. Corresponding to the monitoring means, once at least one monitoring value exceeds a preset value, stirring and reaction liquid adding are stopped, the noble metal raw material and the solution are separated, hydrogen and heat are stopped from the source, the harm possibly caused by continuous reaction is thoroughly avoided, and the safety degree is extremely high.
Through the guarantee of the steps, the aluminum in the aluminum-containing precious metal raw material can be basically and safely dissolved in the solution in a complete reaction manner, only the inert precious metal which cannot be reacted is left, and at the moment, the primary recovery product of the precious metal is obtained, so that the subsequent further purification treatment and recovery are facilitated.
Drawings
FIG. 1 is a flow diagram of a process for the recovery of an aluminum-containing precious metal source in accordance with the present invention;
FIG. 2 is a schematic view of a recovery system for an aluminum-containing precious metal source material according to the present invention;
FIG. 3 is an enlarged view of the first vessel of the recovery system for an aluminum-containing precious metal source of the present invention;
fig. 4 is a top view of fig. 3.
The system comprises a reaction device 1, a first container 11, a second container 12, a hot water pipeline 2, a reaction liquid pipeline 3, a reaction liquid raw material tank 31, a lifting device 4, a tail gas pipeline 5, a tail gas treatment device 51, an exhaust fan 52, a liquid level sensor 61, a hydrogen concentration sensor 62 (an alarm device), a temperature sensor 63, a control center 7, a recovery device 8, a compressed air pipeline 9, a bottom basket 111, an arch part 111a, an annular groove 111b, a lifting handle 112, a hanging ring 112a and a through hole 113.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and the detailed description, and it should be noted that any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict.
In the description of the present application, it is to be understood that the terms "center", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present application and simplifying the description, but do not indicate or imply that the referred device or element must have a particular orientation, be constructed in a particular orientation, and be operated, and thus should not be construed as limiting the present application.
The terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless otherwise specified.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may be present.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Fig. 1 shows a method for recovering an aluminum-containing noble metal raw material according to the present invention, and fig. 2 is a recovery system in which the method for recovering an aluminum-containing noble metal raw material can be used.
The method for recovering the aluminum-containing noble metal raw material comprises the following steps:
feeding: putting an aluminum-containing noble metal raw material into a first container 11 with a plurality of water permeable holes, and then placing the first container 11 into a second container 12; the aluminum-containing noble metal raw material is contained by the first container 11, the hot water and the reaction liquid are contained by the second container 12, the aluminum-containing noble metal raw material and the reaction liquid can be conveniently separated, so that the reaction is stopped and the hydrogen is generated, and the safety and the controllability are stronger. The aluminum-containing noble metal raw material referred to in the present example is a solid raw material containing aluminum and a noble metal or rare metal (e.g., platinum, ruthenium, etc.) at the same time.
Adding hot water: adding hot water with the temperature of 50-70 ℃ into the second container 12, so that the hot water enters the first container 11 through the water permeable holes, the liquid level of the hot water is not higher than that of the precious metal raw material in the first container 11, and continuously stirring after the addition is finished;
adding a reaction solution: starting the tail gas treatment equipment 51 communicated with the second container 12, and starting to add reaction liquid into the second container 12 after detecting that the tail gas treatment equipment 51 is in a tail gas pumping treatment state, so that the precious gold is obtainedAluminum in the raw materials and the reaction solution start to react and generate hydrogen; before the reaction liquid is added, a large amount of hot water is added to increase the temperature, then the reaction liquid is added and mixed with the hot water through stirring, and then the reaction liquid reacts with the aluminum-containing noble metal raw material, the reaction is carried out simultaneously with the addition of the reaction liquid, the concentration of the reaction liquid is more controllable, and the waste amount is reduced. The reaction solution in this embodiment is preferably concentrated hydrochloric acid or concentrated nitric acid, wherein the concentration of the concentrated hydrochloric acid is preferably 28% to 35% by mass, especially 31%, and when the concentrated hydrochloric acid is added into hot water and then stirred, the concentrated hydrochloric acid can rapidly react with aluminum to generate hydrogen (2Al +6HCl ═ 2 AlCl)3+3H2↑)。
In the two steps, the importance of the sequence of each link on safe and smooth production is reflected, firstly, a large amount of hot water is added before the reaction liquid is added, and stirring is started, so that the reaction liquid is directly mixed with a large amount of hot water in a stirring state when being added, and the over-violent reaction caused by over-high acid concentration is prevented; moreover, it is in the state of suction treatment tail gas still to need to detect tail gas treatment facility earlier before adding the reaction liquid, has guaranteed normal continuous convulsions, prevents that hydrogen concentration is too high in normal production reaction. In the actual equipment design, switches of the equipment for controlling each link can be associated, and when the previous equipment is not normally started, the subsequent equipment cannot be normally started.
Safety monitoring: in all the steps, the monitoring values of at least one of the discharged tail gas and/or the hydrogen concentration above the second container 12, the solution temperature in the first container 11 and the solution liquid level in the first container 11 are continuously obtained, when the monitoring values exceed the preset values, stirring and adding of the reaction liquid are stopped, the aluminum-containing precious metal raw material in the first container 11 is separated from the solution in the second container 12, and in the actual operation process, the first container 11 is directly lifted upwards until the first container 11 is separated from the solution in the second container 12. Wherein the explosion limit of hydrogen is 4.0% to 75.6% (volume concentration), the present embodiment preferably controls the preset value of hydrogen concentration to be less than 1%. The preset value of the temperature of the solution in the first container 11 is preferably 90 ℃.
The hydrogen concentration in the tail gas discharged in the whole reaction process is monitored, and the concentration of escaped hydrogen (the hydrogen density is less than that of air, and the escaped hydrogen inevitably flows upwards if the escaped hydrogen exists) can be monitored from the upper part of the second container 12, so that the hydrogen concentration is prevented from exceeding a threshold value to reach an explosion point to threaten the safety of equipment and personnel; in addition, the temperature of the solution in the first container 11 can be monitored, and when the temperature of the solution is too high, the reaction is proved to be too violent, and a runaway condition is possible; when the liquid level in the first vessel 11 is too high, the highly corrosive reaction liquid will escape, causing danger and contamination. Corresponding to the monitoring means, once at least one monitoring value exceeds a preset value, stirring and reaction liquid adding are stopped, the aluminum-containing precious metal raw material is separated from the solution, hydrogen and heat are stopped from the source, the possible harm caused by continuous reaction is thoroughly avoided, and the safety degree is extremely high.
Unloading and recovering: after the reaction of the aluminum-containing noble metal raw material in the first container 11 is completed, the noble metal solid which cannot react is separated from the remaining solution, and the primary recovery product of the noble metal is obtained. Through the guarantee of the steps, the aluminum in the aluminum-containing precious metal raw material can be basically and safely dissolved in the solution in a complete reaction manner, only the inert precious metal which cannot be reacted is left, and at the moment, the primary recovery product of the precious metal is obtained, so that the subsequent further purification treatment and recovery are facilitated.
As a preferable scheme of the hot water adding step, a hot water pipe 2 is communicated with the second container 12, and the hot water adding step specifically comprises:
the control center 7 controls the electromagnetic valve and the proportional control valve on the hot water pipeline 2, and adds 50 ℃ to 70 ℃ hot water into the second container 12 at a preset total heating water amount and rate, so that the hot water enters the first container 11 through the permeable hole, and the liquid level height in the second container 12 is detected by the liquid level meter, so that the liquid level does not cover the precious metal raw material in the first container 11, and continuous stirring is started after the addition is finished. Set up solenoid valve and proportional control valve and make opening and shutting of hot water pipeline 2 more controllable and directly perceived with the flow condition, through opening and shutting of control center 7 control solenoid valve, combine flowmeter real-time detection flow size, long-range can automatic control go on with predetermined hot water total amount and speed, personnel need not to operate at the scene, and automation, accuracy and security are higher.
After the hot water is added, a stirring step is further provided, stirring may be achieved by providing a stirring paddle in the second container 12, in this embodiment, it is preferable that the compressed air pipeline 9 is communicated with the second container 12, and in the hot water adding step, stirring is performed by using an air stirring method, where the air stirring specifically includes: the control center 7 opens the electromagnetic valve on the compressed air pipeline 9 and inputs the compressed air into the bottom of the second container 12, thereby playing the role of stirring. The air stirring does not need to be provided with moving parts such as a stirring paddle, so that the corrosion is not worried about, the air stirring is suitable for being used in the high-temperature and corrosive environment, the full contact between the reaction liquid and the aluminum-containing precious metal raw material is facilitated, and the acid dissolving effect is better. In order to avoid the introduction of impurities into the compressed air, a pressure reducing valve and an oil-water separator are connected to the compressed air pipeline, and the compressed air is decompressed by the pressure reducing valve and is separated by the oil-water separator, and then is input to the bottom of the second container 12. In addition, the addition of compressed air can also play the effect of the concentration of hydrogen in the tail gas of dilution emission for hydrogen concentration is difficult to reach the default more.
As a preferable embodiment of the reaction solution adding step, a reaction solution pipe 3 is connected to the second container 12, and the step of adding the reaction solution to the second container 12 specifically includes: the control center 7 controls the electromagnetic valve and the proportional control valve on the reaction liquid pipeline 3 to add the reaction liquid at the preset total acid adding amount and rate. Similar to the step of adding hot water, the proportion regulating valve added on the reaction liquid pipeline 3 is controlled by the control center 7, so that the reaction liquid is automatically, remotely, quantitatively and constantly added, and compared with the hot water, the reaction liquid with strong corrosivity is more favorable for improving the safety and controllability by adopting automatic control. In the adding process of the reaction liquid, the total added feeding amount is set firstly, and the flow precision requirement is lower than 1 percent/time of the total feeding amount, so that the precise control is realized, and the waste is reduced.
In addition, in order to facilitate the exhaust of the exhaust gas, an exhaust gas pipeline 5 is further provided to communicate with the second container 12, the tail end of the exhaust gas pipeline 5 is connected to an exhaust gas treatment device 51, and in the reaction liquid adding step, whether the exhaust gas treatment device 51 is in a state of sucking and treating the exhaust gas is judged by detecting the wind pressure in the exhaust gas pipeline 5. In order to avoid that the tail gas containing a large amount of hydrogen is accumulated in the second container 12, the tail gas treatment device 51 is adopted to extract and treat the formed tail gas, and therefore whether the tail gas treatment device 51 is in a normal working state or not is related to safe production, the embodiment adopts the method of detecting the wind pressure in the tail gas pipeline 5 to judge whether the tail gas treatment device 51 operates normally or not, but not to judge the opening or closing state of the tail gas treatment device 51, thereby further avoiding the risk caused by abnormal suction due to the problem of the tail gas treatment device 51, and having higher detection accuracy. Among them, the off-gas treatment device 51 is preferably a spray tower.
As a preferable scheme of the unloading recovery step, the second container 12 is provided with a discharge valve, and a filter press is arranged outside and communicated with the discharge valve, and the unloading recovery step specifically comprises: after the reaction of the aluminum-containing precious metal raw material in the first container 11 is finished, opening the discharge valve of the second container 12, starting the filter press, conveying the mixture of the unreacted precious metal solid and the solution to the filter press for filter pressing, conveying the filter-pressed sewage through a pipeline to leave the centralized treatment, and carrying out refining recovery after washing and drying the precious metal solid obtained by filter pressing of the filter press, wherein the precious metal solid is a primary recovery product. The filter press is a common solid-liquid separation device, has the advantages of stable performance, convenient operation, safety, labor saving and the like, can resist high temperature and high pressure, has certain corrosion resistance, and can bear solution with reduced corrosion after reaction. In addition, the solid precious metal materials after reaction are generally in a loose state, and the solid can be pressed into a filter cake through a filter pressing pump and collected, so that the use is simple, and the solid-liquid separation is rapid.
In addition, in order to further ensure that the concentration of the escaped hydrogen does not reach an explosion point and further enhance the safety performance, an exhaust fan 52 communicated with the outside is further arranged in a space (such as a production factory or a laboratory) where the first container 11, the second container 12 and the tail gas pipeline 5 are located, the exhaust fan 52 is opened in the whole process or is opened when the monitored value exceeds a preset value, and preferably at least 3 high-power axial flow fans are arranged on the wall surface of the space to be communicated with the outside. Because the exhaust fan 52 can force the interior of the space to rapidly exchange gas with the outside, if a whole-course opening mode is adopted, hydrogen explosion can be avoided at a large probability even if hydrogen escapes and safety monitoring fails during reaction; if the monitoring device is started again when the abnormal condition that the monitoring value exceeds the preset value occurs, the power can be saved, and the monitoring device can play a role quickly in the abnormal condition to recover to a normal state.
Corresponding to the sequence of opening the links, this embodiment further provides a preferable production stop step after the unloading and recovering step as follows:
stopping adding the reaction liquid, separating the noble metal raw material in the first container from the solution in the second container, stopping the main reaction, and basically stopping the generation of hydrogen; then stopping stirring to ensure that the reaction solution is always in a stirring state in the whole possible hydrogen generation link, so that the local overhigh concentration of the reaction solution and violent reaction are avoided; after the stirring is stopped, all reactions are confirmed to be stopped, no tail gas such as hydrogen is generated, and finally the tail gas treatment equipment is closed, so that the danger that the possibly generated hydrogen (for example, a small amount of reaction liquid remained on the surface of the precious metal raw material can continue to react to generate a small amount of hydrogen) is not timely discharged is avoided to the greatest extent. The equipment is closed through the step, so that the safety of the whole production till the end is ensured, and the characteristics of safety, automatic control, efficiency and safety in the whole method are reflected.
As shown in fig. 2 to 4, based on the above method for recovering an aluminum-containing precious metal raw material, the present embodiment further provides a system for recovering an aluminum-containing precious metal raw material, including:
the reaction device 1 comprises a first container 11 and a second container 12, wherein the first container 11 is provided with a plurality of through holes 113 for containing the aluminum-containing precious metal raw material, the first container 11 is movably arranged in the second container 12, and the contact and separation of the aluminum-containing precious metal material and the reaction liquid are conveniently realized by changing the position of the first container 11 in the second container 12;
a hot water pipe 2, which is communicated with the second container 12 and is used for introducing hot water of 50 ℃ to 70 ℃ into the second container 12, wherein the hot water can be used as the previous step of adding the reaction liquid and provides a temperature favorable for reaction for the reaction liquid;
a reaction liquid pipe 3, which is communicated with the second container 12 and is used for introducing the reaction liquid into the second container 12 so as to react with the aluminum in the aluminum-containing noble metal raw material in the first container 11; the reaction solution is fed from the reaction solution feed tank 31 into the reaction solution conduit 3 by pumping and then fed into the second container 12.
A lifting means 4 connected at a lower end thereof to the first container 11 for lifting or lowering the first container 11 so as to bring or separate the first container 11 into or from the liquid in the second container 12;
the tail gas pipeline 5 is communicated with the second container 12 and is used for discharging tail gas in the second container 12 so as to prevent hydrogen in the second container 12 from being discharged to form an explosive environment;
a detection device including at least one of a liquid level sensor 61, a hydrogen concentration sensor 62 and a temperature sensor 63, wherein the liquid level sensor 61 detects a liquid level height in the second container 12, the hydrogen concentration sensor 62 detects a hydrogen concentration directly above the off-gas pipe 5 and/or the second container 12, and the temperature sensor 63 detects a liquid temperature in the second container 12;
a control center 7 electrically connected to the lifting device 4 and the detection device, the control center 7 being configured to:
when the value detected by one of the liquid level sensor 61, the hydrogen concentration sensor 62 or the temperature sensor 63 exceeds a preset value, the device is controlled to lift the first container 11, so that the precious metal raw material containing aluminum in the first container 11 is separated from the solution in the second container 12.
The hydrogen concentration in the tail gas discharged in the whole reaction process is monitored, and the concentration of escaped hydrogen (the hydrogen density is less than that of air, and the escaped hydrogen inevitably flows upwards if the escaped hydrogen exists) can be monitored from the upper part of the second container 12, so that the hydrogen concentration is prevented from exceeding a threshold value to reach an explosion point to threaten the safety of equipment and personnel; in addition, the temperature of the solution in the first container 11 can be monitored, and when the temperature of the solution is too high, the reaction is proved to be too violent, and a runaway condition is possible; when the liquid level in the first vessel 11 is too high, the highly corrosive reaction liquid will escape, causing danger and contamination. Corresponding to the monitoring means, once at least one monitoring value exceeds a preset value, the aluminum-containing precious metal raw material and the solution are separated, the continuous generation of hydrogen and heat is stopped from the source, the possible harm caused by the continuous reaction is thoroughly avoided, and the safety degree is extremely high.
In addition, a recovery device 8 is also provided, the recovery device 8 is connected with a discharge valve of the second container 12 and is used for separating the non-reactive precious metal solids from the remaining solution, and a primary recovery product of the precious metal is obtained.
Preferably, an electromagnetic valve is arranged on the hot water pipeline 2, an electromagnetic valve is also arranged on the reaction liquid pipeline 3, the control center 7 is electrically connected with the electromagnetic valve and the proportional regulating valve, and the control center 7 is configured to: when the value detected by one of the liquid level sensor 61, the hydrogen concentration sensor 62 or the temperature sensor 63 exceeds a preset value, the electromagnetic valve is controlled to be closed, so that the reaction liquid is stopped from being added, and no new reaction liquid reacts with the aluminum-containing noble metal raw material. In addition, the hot water pipeline 2 and the reaction liquid pipeline 3 are also provided with proportional control valves for controlling the flow.
The hydrogen concentration sensor 62 detects that the hydrogen concentration reaches 0.5% or the temperature sensor 63 detects that the temperature exceeds 80 ℃, the alarm device gives out sound and light alarm and prompts abnormity to the control center 7; when the hydrogen concentration sensor 62 detects that the hydrogen concentration reaches 1% or the temperature sensor 63 detects that the temperature exceeds 90 ℃, the alarm device continuously alarms, the control center 7 immediately controls to close the electromagnetic valve and the proportion regulating valve, and the lifting device 4 is controlled to lift the first reaction vessel, so that the aluminum-containing precious metal raw material is separated from the reaction liquid.
Preferably, the second container is externally connected with a compressed air pipeline 9, and the compressed air pipeline 9 is introduced into the bottom of the second container, so that the air stirring effect is achieved. The air stirring does not need to be provided with moving parts such as a stirring paddle, so that the corrosion is not worried about, the air stirring is suitable for being used in the high-temperature and corrosive environment, the full contact between the reaction liquid and the aluminum-containing precious metal raw material is facilitated, and the acid dissolving effect is better. In addition, the addition of compressed air can also play the effect of the concentration of hydrogen in the tail gas of dilution emission for hydrogen concentration is difficult to reach the default more.
The control center 7 is preferably a PLC control system operation station isolated from a production space, the first container 11 is preferably made of glass fiber reinforced plastic, the second container 12 is a reaction kettle, the first container 11 comprises a bottom basket 111 and a lifting handle 112, a plurality of through holes 113 are formed in the bottom and the side face of the bottom basket 111, the through holes 113 are 3mm in diameter and are uniformly distributed, the bottom end of the lifting handle 112 is connected to the bottom basket 111, a hanging ring 112a is arranged at the top end of the lifting handle 112, and the lifting device 4 is hung on the hanging ring 112a in a hooking mode. This structure facilitates the suspension, and the lifting device 4 can be lifted from above the first container 11 rather than from below, so that the lifting device is protected from the reaction solution, and the space and the entire structure inside the second container 12 are also simpler. Specifically, the inner side of the middle part of the bottom basket 111 is provided with an arch part 111a, the peripheral side of the arch part 111a is an annular groove 111b, the arch part 111a has no hole, and the bottom of the annular groove 111b is provided with a plurality of through holes 113; the handle 112 is columnar, the bottom end is connected to the center of the arch part 111a, and the top end is the hanging ring 112 a. Glass fiber reinforced plastic has low density, is corrosion resistant, can be easily molded into a complex shape, and is suitable for use in the present embodiment. The middle part of the first container 11 is protruded upwards to form a slope by the arch part 111a, and when the first container 11 is lifted by the lifting device 4, the reaction liquid can be rapidly flowed away from all directions by the omnibearing slope and separated from the precious metal raw material in the first container 11 as soon as possible, so that the reaction is rapidly stopped, and heat and hydrogen can not be generated continuously.
The device is explosion-proof electric block, and explosion-proof electric block is a special hoisting equipment, can install the position such as overhead traveling crane and portal crane, has advantages such as explosion-proof, small, easy operation, and explosion-proof electric block passes through explosion-proof shell and keeps apart electric spark and dangerous temperature and explosive danger environment on every side to avoid producing the explosion, because probably there is a large amount of hydrogen in the external environment in this embodiment, consequently adopt explosion-proof electric block can reduce hoisting equipment and cause the probability of explosion. The upward movement of the electric hoist is provided with a limit switch, the descending speed is controlled by frequency conversion when the electric hoist descends, the descending distance is controlled according to the descending time, and the time is accurate to the millisecond level.
In addition, a remote control switch and an emergency stop button are also arranged, so that in case that the control center 7 fails and cannot automatically stop, the reaction liquid can be added and the aluminum-containing precious metal raw material and the reaction liquid can be separated by pressing the switch and the emergency stop button.
In conclusion, the method and the system for recovering the aluminum-containing precious metal raw material in the embodiment have the advantages of high automation degree of the production process, convenience in operation, reduction in labor intensity of personnel, reduction in environmental pollution risks and product pollution risks, reasonable product collection, saving in production cost, and improvement in production efficiency, production safety coefficient and product quality.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (11)
1. A method for recovering an aluminum-containing precious metal raw material is characterized by comprising the following steps:
feeding: putting an aluminum-containing precious metal raw material into a first container with a plurality of water permeable holes, and then placing the first container into a second container;
adding hot water: adding hot water of 50-70 ℃ into the second container, so that the hot water enters the first container through the water permeable holes, the liquid level of the hot water is less than that of the precious metal raw material in the first container, and continuously stirring after the addition is finished;
adding a reaction solution: starting a tail gas treatment device communicated with the second container, and starting to add reaction liquid into the second container after detecting that the tail gas treatment device is in a tail gas suction treatment state, so that aluminum in the precious metal raw material and the reaction liquid start to react and generate hydrogen;
safety monitoring: continuously obtaining a monitored value of at least one of the discharged tail gas and/or the hydrogen concentration above the second container, the solution temperature in the first container and the solution liquid level in the first container in all the steps, stopping stirring and adding the reaction liquid when the monitored value exceeds a preset value, and separating the aluminum-containing precious metal raw material in the first container from the solution in the second container;
unloading and recovering: and after the reaction of the aluminum-containing noble metal raw material in the first container is finished, separating the noble metal solid which cannot react from the residual solution to obtain a primary recovery product of the noble metal.
2. The method of claim 1, wherein a hot water line is connected to the second vessel, and wherein the hot water addition step comprises:
the control center controls the electromagnetic valve and the proportion regulating valve on the hot water pipeline, hot water of 50 ℃ to 70 ℃ is added into the second container at the preset total heating water amount and speed, the hot water enters the first container through the water permeable hole, the liquid level height in the second container is detected through the liquid level meter, the liquid level is enabled to be free of the precious metal raw material in the first container, and continuous stirring is started after the adding is finished.
3. The method according to claim 2, wherein a compressed air line is connected to the second vessel, and the hot water addition step is performed by stirring with air stirring, the air stirring including: the control center opens the electromagnetic valve on the compressed air pipeline and inputs the compressed air into the bottom of the second container, thereby playing the role of stirring.
4. The method according to claim 3, wherein a pressure reducing valve and an oil-water separator are connected to the compressed air line, and the compressed air is fed to the bottom of the second vessel after being subjected to pressure reduction by the pressure reducing valve and oil-water separation by the oil-water separator.
5. The method according to claim 1, wherein a reaction solution conduit is connected to the second vessel, and the step of feeding the reaction solution to the second vessel comprises:
the control center controls the electromagnetic valve and the proportion regulating valve on the reaction liquid pipeline to add the reaction liquid at the preset total acid adding amount and rate.
6. The method according to claim 1, wherein a tail gas pipe is connected to the second container, and a tail gas treatment device is connected to an end of the tail gas pipe, and wherein in the reaction liquid addition step, it is determined whether or not the tail gas treatment device is in a state of sucking the treated tail gas by detecting a wind pressure in the tail gas pipe.
7. The method for recovering an aluminum-containing noble metal source material according to claim 1, wherein the second vessel is provided with a discharge valve, and a filter press is provided outside to communicate with the discharge valve, and the discharge recovery step comprises: after the reaction of the noble metal raw material in the first container is finished, opening a discharge valve of the second container, starting the filter press, conveying a mixture of the noble metal solid which cannot react and the solution to the filter press for filter pressing, conveying filter-pressed sewage through a pipeline to leave centralized treatment, and carrying out refining recovery after the noble metal solid obtained by filter pressing of the filter press is a primary recovery product to be washed and dried.
8. The method for recovering an aluminum-containing precious metal raw material according to claim 5, wherein an exhaust fan is further provided in a space in which the first vessel, the second vessel and the exhaust gas duct are located, the exhaust fan being opened all the way or when the monitored value exceeds a preset value.
9. The method for recovering an aluminum-containing precious metal raw material according to any one of claims 1 to 8, further comprising a production stop step after the discharge recovery step, as follows:
stopping adding the reaction liquid, separating the noble metal raw material in the first container from the solution in the second container, stopping stirring, and finally closing the tail gas treatment equipment.
10. A system for recovering an aluminum-containing precious metal source material, comprising:
the reaction device comprises a first container and a second container, wherein the first container is provided with a plurality of through holes and is used for containing an aluminum-containing precious metal raw material, and the first container is movably arranged in the second container; the second container is externally connected with a hot water pipeline, a reaction liquid pipeline and a tail gas pipeline;
a lifting device, the lower end of which is connected with the first container, and is used for lifting or lowering the first container so as to contact or separate the first container with or from the liquid in the second container;
the detection device comprises at least one of a liquid level sensor, a hydrogen concentration sensor and a temperature sensor, wherein the liquid level sensor detects the liquid level height in the second container, the hydrogen concentration sensor detects the hydrogen concentration right above the tail gas pipeline and/or the second container, and the temperature sensor detects the liquid temperature in the second container;
a control center electrically connected to the lifting device and the detection device, the control center configured to:
when the value detected by one of the liquid level sensor, the hydrogen concentration sensor or the temperature sensor exceeds a preset value, the device is controlled to lift the first container, so that the precious metal raw material containing aluminum in the first container is separated from the solution in the second container.
11. The system for recycling aluminum-containing precious metal raw material according to claim 9, wherein a solenoid valve is provided on the hot water pipe, a solenoid valve is also provided on the reaction liquid pipe, the control center is electrically connected to the solenoid valve and the proportional regulating valve, and the control center is configured to:
and when the value detected by one of the liquid level sensor, the hydrogen concentration sensor or the temperature sensor exceeds a preset value, controlling the electromagnetic valve to be closed.
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