CN109266862B - Method for recovering regenerated metal from waste circuit board by adopting ionic liquid - Google Patents
Method for recovering regenerated metal from waste circuit board by adopting ionic liquid Download PDFInfo
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- CN109266862B CN109266862B CN201811488233.5A CN201811488233A CN109266862B CN 109266862 B CN109266862 B CN 109266862B CN 201811488233 A CN201811488233 A CN 201811488233A CN 109266862 B CN109266862 B CN 109266862B
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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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- 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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- 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
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- 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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Abstract
The invention relates to the technical field of metal recovery, and particularly discloses a method for recovering regenerated metal from a waste circuit board by adopting ionic liquid, which comprises the steps of pretreating the waste circuit board, cutting the waste circuit board into waste circuit board fragments with the length and width of 15-20 mm; soldering tin electronic components, namely immersing the waste circuit board fragments into neutral ionic liquid, and separating the electronic components from the waste circuit board fragments; crushing, namely putting the separated waste circuit board fragments into a crusher to be crushed to obtain waste circuit board particles with the particle size of less than 5 mm; leaching, wherein the waste circuit board particles react with acidic functionalized ionic liquid; and (3) reducing the leachate, namely adding hydrazine hydrate into the leachate for reduction to obtain a metal precipitate. The technical scheme who adopts this patent has solved among the prior art when leaching old and useless circuit board, and ionic liquid use amount is great, increases the problem of the cost input of enterprise.
Description
Technical Field
The invention relates to the technical field of metal recovery, in particular to a method for recovering regenerated metal from a waste circuit board by adopting ionic liquid.
Background
In recent years, as the usage amount of electronic appliances increases, the updating speed of electronic appliances is increased, and the amount of electronic waste is increased rapidly. As an important component of electronic products, printed circuit boards are also being used, and waste printed circuit boards are also increasing rapidly with the generation of a large amount of electronic waste. The composition of the printed circuit board is complex and contains valuable metals such as copper, gold, etc., especially copper content of about 20% (w) which is higher than copper content (0.6%) in copper ore. In addition, the printed circuit board also contains heavy metals such as lead and zinc, and if the heavy metals are not properly treated, the heavy metals bring great harm to the ecological environment.
The wet leaching is an important method for recovering secondary resources in the printed circuit board, the metal recovery rate is higher, and a leaching agent is the key for determining the metal recovery efficiency of the wet leaching. The traditional leaching agent is mainly inorganic acid and is accompanied with harmful gas generation in the operation process, so the development of green and stable leaching agent in hydrometallurgy is important and urgent. Compared with the traditional leaching agent, the ionic liquid which appears in recent years has the advantages of small volatility, low vapor pressure, good thermal stability, low toxicity and the like, and is applied to the fields of hydrometallurgy and the like.
When the waste circuit board is recycled by utilizing the ionic liquid at present, the waste circuit board is generally directly crushed, and then the ionic liquid is added into crushed particles, so that although the process is simple, the process steps are few, and the recycling production efficiency is high, a plurality of electronic components are also arranged on the waste circuit board, the electronic components are connected to the circuit board in a detachable mode, and are welded on the circuit board in a tin soldering mode, and the electronic components are mainly made of non-metal materials, so that when the ionic liquid is used for leaching, the recovery rate of metal is reduced under the influence of the non-metal materials, meanwhile, the ionic liquid is greatly consumed, and the cost investment of enterprises is increased.
Disclosure of Invention
The invention provides a method for recovering regenerated metal from a waste circuit board by adopting ionic liquid, which aims to solve the problems that the use amount of the ionic liquid is large and the cost investment of an enterprise is increased when the waste circuit board is leached in the prior art.
In order to achieve the purpose, the basic scheme of the invention is as follows:
a method for recovering regenerated metal from waste circuit boards by adopting ionic liquid comprises the following steps,
the method comprises the following steps: preprocessing the waste circuit board, manually disassembling the detachable electronic components on the collected waste circuit board, and cutting the disassembled waste circuit board containing the soldering tin electronic components into waste circuit board fragments with the length and the width of 15-20 mm;
step two: soldering electronic component processing to prepare neutral [ BMIM ]][BF4]Heating the ionic liquid to 200-220 ℃, and treating the waste obtained in the step oneImmersion of old circuit board fragments into the neutral BMIM][BF4]In ionic liquids, neutralization [ BMIM ] using a mechanical stirrer][BF4]Stirring the ionic liquid until the soldering tin on the waste circuit board fragments is completely dissolved, and respectively recovering the electronic components and the waste circuit board fragments;
step three: crushing, namely putting the waste circuit board fragments recovered in the step two into a crusher to be crushed to obtain waste circuit board particles with the particle size of less than 5 mm;
step four: leaching, namely putting an acidic functionalized ionic liquid into a leaching barrel, putting the waste circuit board particles obtained in the third step into a containing barrel, putting the containing barrel into the leaching barrel, putting the acidic functionalized ionic liquid in the leaching barrel into the containing barrel, and reacting the waste circuit board particles with the acidic functionalized ionic liquid, wherein the temperature of the acidic functionalized ionic liquid is 70-80 ℃, and the leaching time is 2-3 hours;
step five: pretreating the leachate, namely taking out the accommodating barrel in the fourth step to obtain the leachate, and adding ammonia water into the leachate in the leaching barrel to ensure that the pH of the leachate is 7-9;
step six: and (4) reducing the leachate, namely adding a reducing agent into the leachate obtained in the step five for reduction for 150min, then performing centrifugal treatment to obtain a metal precipitate and waste liquid, and drying the metal precipitate at 80-120 ℃ for 8-12h to obtain metal powder.
The technical principle and the effect of the basic scheme are as follows:
1. in the pretreatment of the first step, because a part of electronic components, such as a rectifier and the like, on the waste circuit board are fixed on the circuit board in a threaded fastening mode, namely the electronic components are not welded on the circuit board in a soldering mode and cannot be separated from the circuit board in a chemical reaction mode, the part of electronic components are firstly detached in a manual mode.
2. Compared with the prior art, the whole circuit board is usually directly crushed and then leached, although the processing method is less in processes, the crushed circuit board particles still contain a large number of electronic components, and the materials of the electronic components contain a large number of inorganic nonmetallic materials, so that the prior art needs to consume more ionic solutions when the circuit board particles are leached.
In this scheme, through the dissolution that the manual work was dismantled and was carried out soldering tin with neutral ionic liquid, separate out electronic components on the old and useless circuit board, make like this and leach the step, acidic functional ionic liquid's use amount reduces.
And further, after the electronic components are disassembled from the waste circuit board in the step one, washing and drying are carried out.
Has the advantages that: because old and useless circuit board is in the in-process of long-term use, collection and stack, there is a large amount of dust on the circuit board, in order to reduce follow-up ionic liquid's use, and to the influence of circuit board leaching efficiency, can wash the circuit board earlier, later carry out the drying.
And further, blowing and drying the waste circuit board fragments separated from the electronic components in the step two for 2 hours at the temperature of 70 ℃.
Has the advantages that: the waste circuit board fragments are dried, so that the problem that in the crushing process, water-containing particles can be agglomerated, and the subsequent leaching effect is poor is solved.
Further, the acidic functionalized ionic liquid in the fourth step is: n-butyl sulfonic acid pyridine bisulfate, 1-butyl sulfonic acid-3-methylimidazole trifluoromethanesulfonate, methylimidazole bisulfate and N-butyl sulfonic acid pyridine trifluoromethanesulfonate.
Has the advantages that: the data of a plurality of experiments of the inventor show that the pyrolysis leaching effect of the composition on the waste circuit board is the best, and the efficiency is the fastest.
Further, evaporating the waste liquid in the sixth step at the temperature of 100-150 ℃, and concentrating the waste liquid to obtain a sticky liquid, thereby obtaining the recovery liquid of the acidic functionalized ionic liquid.
Has the advantages that: therefore, the waste liquid can be recycled, the resource is recycled, and the production investment of enterprises is reduced.
Drawings
FIG. 1 is a schematic partial sectional view of a waste circuit board metal leaching device provided with waste circuit board particles in the embodiment of the invention;
fig. 2 is a partially cut-away schematic view of the waste circuit board metal leaching device in the embodiment of the invention when the waste circuit board particles are not loaded.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: leaching bucket 10, liquid inlet valve 101, liquid outlet valve 102, mounting table 103, holding bucket 20, mounting section 201, elastic section 202, filtering section 203, bolt 204, through hole 205, bearing 30, stirring shaft 301, stirring rod 302, threaded section 303, nut 304, internally splined sleeve 305, electromagnet 40, shell 401.
Example (b):
a method for recovering regenerated metal from waste circuit boards by adopting ionic liquid comprises the following steps:
step one, preprocessing a waste circuit board:
the collected detachable electronic components on the waste circuit board are manually detached, for example, the detached electronic components are discarded or recovered by other processing methods through components such as a rectifier fastened through threads. And washing the disassembled waste circuit board containing the soldering tin electronic components with water to remove dust, drying the waste circuit board in a blast drying oven at the temperature of 70 ℃ for 10 hours, and then cutting the dried waste circuit board into waste circuit board fragments with the length and width within the range of 15-20 mm.
Step two, soldering the electronic components:
preparing neutral ionic liquid, heating and preserving heat within the range of 200-220 ℃, wherein the neutral ionic liquid in the embodiment is 1-butyl-3-methylimidazolium tetrafluoroborate (namely [ BMIM ]][BF4]) Immersing the waste circuit board fragments obtained in the step one into neutral ionic liquid, and centering by using a mechanical stirrerAnd stirring the ionic liquid and the waste circuit board fragments until the soldering tin on the waste circuit board fragments is completely dissolved, respectively recovering the electronic components and the waste circuit board fragments, and drying the recovered waste circuit board fragments by blowing at the temperature of 70 ℃ for 2 hours.
Step three, crushing treatment:
and D, putting the waste circuit board fragments dried in the step two into a crusher to be crushed for multiple times, and obtaining waste circuit board particles with the particle size of less than 5 mm.
Step four, leaching treatment:
preparing acidic functionalized ionic liquid as a reaction medium, wherein the acidic functionalized ionic liquid in the embodiment is one or a combination of several of N-butyl sulfonic acid pyridine bisulfate, 1-butyl sulfonic acid-3-methylimidazole trifluoromethanesulfonate, methylimidazole bisulfate and N-butyl sulfonic acid pyridine trifluoromethanesulfonate, the acidic functionalized ionic liquid in the embodiment is N-butyl sulfonic acid pyridine bisulfate, the prepared acidic functionalized ionic liquid is put into a leaching barrel, the waste circuit board particles obtained in the third step are put into a containing barrel, the containing barrel is put into the leaching barrel to enable the waste circuit board particles to react with the acidic functionalized ionic liquid, wherein the temperature of the acidic functionalized ionic liquid in the leaching barrel is kept within the range of 70-80 ℃, the leaching time is within the range of 2-3 h;
step five, pretreatment of the leachate:
and D, taking out the containing barrel in the fourth step to obtain a leaching solution, and adding ammonia water into the leaching solution in the leaching barrel to keep the pH value of the leaching solution within the range of 7-9.
Step six, reducing the leachate;
adding a reducing agent into the leachate obtained in the step five for reduction for 100min, wherein the reducing agent is hydrazine hydrate in the embodiment, after the reduction is finished, performing centrifugal treatment to obtain a metal precipitate and a waste liquid, and drying the metal precipitate at 80 ℃ for 8h to obtain metal powder; in addition, the waste liquid is evaporated at the temperature of 100 ℃ to obtain the recovery liquid of the acidic functionalized ionic liquid, so that the waste liquid can be reused.
The leaching barrel and the containing barrel used in the fourth step are both arranged in the waste circuit board metal leaching device, the waste circuit board metal leaching device is basically as shown in fig. 1 and fig. 2, and comprises a frame, a leaching barrel 10 with an upward opening is fixed on the frame, a liquid inlet valve 101 is arranged on the side wall of the leaching barrel 10, a liquid outlet valve 102 is arranged at the bottom of the leaching barrel 10, an annular mounting table 103 is arranged at the top of the leaching barrel 10, a plurality of mounting holes are uniformly distributed on the mounting table 103, a containing barrel 20 is arranged in the leaching barrel 10, wherein the containing barrel 20 comprises a mounting section 201, an elastic section 202 and a magnetic filtering section 203 which are sequentially connected from top to bottom, the top of the mounting section 201 is provided with a connecting hole corresponding to the position and the size of the mounting hole, a bolt 204 is connected in the connecting hole through a thread, the elastic section 202 is made of rubber with high elasticity, and the longitudinal section of the filtering section, a plurality of through holes 205 are arranged on the side wall and the bottom of the filtering-out section 203, wherein the diameter of the through holes 205 is less than 1 mm.
The bottom of filtering out section 203 is connected with (mixing) shaft 301 through bearing 30 rotation, is equipped with the sealing washer on bearing 30, is fixed with many puddlers 302 that are located and hold bucket 20 on the (mixing) shaft 301, and (mixing) shaft 301 is kept away from puddlers 302 one end and is equipped with screw thread section 303, wherein is connected with nut 304 on the screw thread section 303, is equipped with the spline groove in nut 304's periphery, and the meshing has internal spline cover 305 on the spline groove, wherein internal spline cover 305 and frame fixed connection.
The bottom of the leaching barrel 10 is provided with an electromagnet 40 connected with a low-frequency alternating current power supply, the outside of the electromagnet 40 is provided with a protective shell 401 made of polytetrafluoroethylene, and the shell 401 is provided with a radiating pipe communicated with the outside.
After the operation personnel finishes the first step to the third step, the containing barrel 20 is fixed in the leaching barrel 10 through the bolt 204, the waste circuit board particles obtained in the third step are put into the containing barrel 20, after the particles enter the containing barrel 20, the filtering section 203 of the containing barrel 20 moves downwards under the action of the gravity of the waste circuit board particles, the elastic section 202 is stretched, then the prepared acidic functionalized ionic liquid is injected into the leaching barrel 10 through the liquid inlet valve 101, so that the liquid level of the solution can submerge the top of the elastic section 202, and the solution entering the leaching barrel 10 enters the containing barrel 20 through the through hole 205 on the filtering section 203 and contacts and reacts with the particles in the containing barrel 20.
After the solution is injected, the power supply connected with the electromagnet 40 is turned on, when the magnetic pole at the top of the electromagnet 40 is the same as the magnetic pole at the bottom of the filtering section 203, repulsion force is formed between the electromagnet 40 and the filtering section 203, so that the filtering section 203 moves upwards, the stirring shaft 301 moves upwards synchronously, because the threaded section 303 of the stirring shaft 301 is connected with the nut 304, and the nut 304 is fixedly connected to the rack through the spline, therefore, the stirring shaft 301 is in the process of moving upwards, the rotation of the nut 304 is limited by the spline, therefore, the stirring shaft 301 can rotate in the process of moving upwards, so that the stirring rod 302 stirs the waste circuit board particles in the accommodating barrel 20, and the particles can be in contact with the solution quickly to react.
When the magnetic pole at the top of the electromagnet 40 is opposite to the magnetic pole at the bottom of the filtering section 203, a suction force is formed between the electromagnet 40 and the filtering section 203, the filtering section 203 moves downwards, the stirring shaft 301 rotates reversely, so that the stirring rod 302 reversely stirs particles, and in the process of downward movement of the filtering section 203, the solution in the leaching barrel 10 is increased by downward extrusion force, so that the solution enters the accommodating barrel 20 through the through hole 205 at the bottom of the filtering section 203, the solution rapidly entering the accommodating barrel 20 can form impact force on the particles, so that the particles move upwards relative to the accommodating barrel 20 under the action of buoyancy force and impact force, so that the particles are also subjected to upward impact force when being circumferentially stirred by the stirring rod 302, and irregular movement of the particles in the accommodating barrel 20 is realized, the contact area with the solution is increased, and the reaction rate is increased.
In addition, in the reaction process of the waste circuit board particles and the solution, the metal compounds in the particles are continuously dissolved in the solution, other inorganic filter residues such as epoxy resin and other organic materials and glass fibers are remained, when the solution rapidly enters the accommodating barrel 20 through the through hole 205, the residues possibly blocked can be cleaned, in addition, after the metal compounds are continuously dissolved, the gravity of the particles in the accommodating barrel 20 is continuously reduced, the filtering section 203 continuously moves upwards until the metal compounds in the particles are completely dissolved, only the filter residues are remained in the accommodating barrel 20, and an operator only needs to take out the accommodating barrel 20 to perform reduction operation on the leaching solution in the leaching barrel 10.
The method adopts the leaching device of the waste circuit board to carry out leaching treatment, on one hand, the reaction efficiency and the contact area of the waste circuit board particles and the solution are improved, so that the metal compounds in the waste circuit board particles are dissolved out more quickly and thoroughly, and the leaching efficiency and effect are improved; on the other hand holds the setting of bucket and is convenient for leach the separation of the residue after accomplishing and leachate, and operating personnel only need take out and hold the bucket can.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (5)
1. A method for recovering regenerated metal from waste circuit boards by adopting ionic liquid is characterized by comprising the following steps: the method comprises the following steps of,
the method comprises the following steps: preprocessing the waste circuit board, manually disassembling the detachable electronic components on the collected waste circuit board, and cutting the disassembled waste circuit board containing the soldering tin electronic components into waste circuit board fragments with the length and the width of 15-20 mm;
step two: soldering electronic component processing to prepare neutral [ BMIM ]][BF4]Heating the ionic liquid to 200-220 ℃, and immersing the waste circuit board fragments obtained in the step one into the neutral BMIM][BF4]In ionic liquids, neutralization [ BMIM ] using a mechanical stirrer][BF4]Stirring the ionic liquid until the ionic liquid is usedThe soldering tin on the old circuit board fragments is completely dissolved, and the electronic components and the old circuit board fragments are respectively recovered;
step three: crushing, namely putting the waste circuit board fragments recovered in the step two into a crusher to be crushed to obtain waste circuit board particles with the particle size of less than 5 mm;
step four: leaching, namely putting an acidic functionalized ionic liquid into a leaching barrel, putting the waste circuit board particles obtained in the third step into a containing barrel, putting the containing barrel into the leaching barrel, putting the acidic functionalized ionic liquid in the leaching barrel into the containing barrel, and reacting the waste circuit board particles with the acidic functionalized ionic liquid, wherein the temperature of the acidic functionalized ionic liquid is 70-80 ℃, and the leaching time is 2-3 hours;
step five: pretreating the leachate, namely taking out the accommodating barrel in the fourth step to obtain the leachate, and adding ammonia water into the leachate in the leaching barrel to ensure that the pH of the leachate is 7-9;
step six: reducing the leachate, namely adding a reducing agent into the leachate obtained in the step five for reduction for 150min, then performing centrifugal treatment to obtain a metal precipitate and waste liquid, and drying the metal precipitate at 80-120 ℃ for 8-12h to obtain metal powder;
be equipped with the feed liquor valve on the leaching bucket lateral wall in step four, the bottom is equipped with out the liquid valve, it fixes in leaching the bucket to hold the bucket, it includes the from the top installation section that connects gradually to hold the bucket, the elasticity section with have the magnetic section of filtering out, the longitudinal section of filtering out the section is the U-shaped, lateral wall and bottom filtering out the section all are equipped with a plurality of through-holes, the bottom rotation that filters out the section is connected with the (mixing) shaft, be fixed with many puddlers that are located and hold the bucket on the (mixing) shaft, puddler one end is kept away from to the (mixing) shaft is equipped with the screw thread section, be connected with the nut on the screw thread section, the periphery of nut is equipped with the spline groove, the meshing.
2. The method for recovering the regenerated metal from the waste circuit boards by using the ionic liquid as claimed in claim 1, wherein the method comprises the following steps: and (3) washing and drying the waste circuit board in the step one after the electronic components are disassembled.
3. The method for recovering the regenerated metal from the waste circuit boards by using the ionic liquid as claimed in claim 2, wherein the method comprises the following steps: and D, drying the waste circuit board fragments separated from the electronic components in the step two by blowing at the temperature of 70 ℃ for 2 hours.
4. The method for recovering the regenerated metal from the waste circuit boards by using the ionic liquid as claimed in claim 3, wherein the method comprises the following steps: the acidic functionalized ionic liquid in the fourth step is as follows: n-butyl sulfonic acid pyridine bisulfate, 1-butyl sulfonic acid-3-methylimidazole trifluoromethanesulfonate, methylimidazole bisulfate and N-butyl sulfonic acid pyridine trifluoromethanesulfonate.
5. The method for recovering the regenerated metal from the waste circuit boards by using the ionic liquid as claimed in claim 4, wherein the method comprises the following steps: and evaporating the waste liquid in the sixth step at the temperature of 100-150 ℃, and concentrating the waste liquid to obtain a sticky liquid, thereby obtaining the recovery liquid of the acidic functionalized ionic liquid.
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| CN110369463B (en) * | 2019-08-27 | 2020-11-24 | 新沂市锡沂高新材料产业技术研究院有限公司 | Electronic waste wet processing device |
| CN111001211A (en) * | 2019-12-20 | 2020-04-14 | 北京京能清洁能源电力股份有限公司北京分公司 | Chemical treatment equipment for crystalline silicon cell fragments |
| CN111715657A (en) * | 2020-06-01 | 2020-09-29 | 安徽超越环保科技股份有限公司 | Stripping and recycling device and method for waste circuit board soldering tin material |
| CN114905112B (en) * | 2022-07-13 | 2022-10-25 | 徐州日托光伏科技有限公司 | Tin cream splendid attire jar of blowing is convenient for to stirring function |
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