CN107841631A - The preparation method of the leachate of copper in a kind of recovery waste and old circuit board - Google Patents
The preparation method of the leachate of copper in a kind of recovery waste and old circuit board Download PDFInfo
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- CN107841631A CN107841631A CN201711257724.4A CN201711257724A CN107841631A CN 107841631 A CN107841631 A CN 107841631A CN 201711257724 A CN201711257724 A CN 201711257724A CN 107841631 A CN107841631 A CN 107841631A
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1666—Leaching with heterocyclic compounds
- C22B3/1675—Leaching with a mixture of organic agents wherein one agent at least is a heterocyclic compounds
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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
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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
- 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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Abstract
The invention discloses a kind of preparation method for reclaiming the leachate of copper in waste and old circuit board, this method comprises the following steps：Methylimidazole dissolved dilution is obtained into solution 1 in solvent 1; solute is dissolved in solvent 2 and obtains solution 2; in 40~120 DEG C of waters bath with thermostatic control and stirring environment; solution 2 is slowly added dropwise in solution 1; 8~24h of back flow reaction under nitrogen protection; by reaction product filtering and washing, drying, ionic liquid intermediate is obtained；Ionic liquid intermediate is dissolved in distilled water, the H that mass fraction is 98% is slowly dropped into distilled water2SO4Solution, 8~24h of stirring reaction at 40~120 DEG C, object ion liquid is dried to obtain after reaction product rotary evaporation is removed into distilled water；The electronic component for removing scolding tin and oxidant, acidic ion liquid are mixed, react 0.5~24h in 40~100 DEG C of waters bath with thermostatic control, stirring environment, gained filtrate is leachate after reaction product is filtered.The present invention is environmentally friendly, and leachate is reusable, and the leaching rate of copper is higher, and technique is simple.
Description
Technical field
The invention belongs to waste reclamation field, more particularly to a kind of system for reclaiming the leachate of copper in waste and old circuit board
Preparation Method.
Background technology
The recovery method of copper is numerous in waste and old circuit board, and mechanical phonograph recorder separation is although simple and easy, but the metal essence isolated
Ore deposit needs further purifying；Pyrometallurgy separation metal can produce SO2, bioxin, flue gas CO2Deng substantial amounts of poisonous and harmful gas
Body, greatly harm is produced to environmental protection；Bioleaching method, because the presence of nonmetallic phase in waste and old circuit board makes bacterium
Toxicity is present, and endangers production, the health of staff, and the method is also immature at present, from waste and old circuit board
The rate of recovery for reclaiming copper and other metals is relatively low；Supercritical fluid method can cause serious due to needing higher temperature and pressure
Reactor corrosion, and cause larger energy consumption；In field of hydrometallurgy, some strong acidic liquids can cause seriously to equipment
Corrosion, and in functional ion liquid recovery waste and old circuit board copper and during other metals it is not only green, and with higher
Copper and other noble metal yields, comprehensive benefit are notable.
In currently used ionic liquid, acid function ionic liquid to have obtained people in recent years the advantages of its own
Highest attention, turn into one of focus on research direction.Ionic liquid refer to room temperature or close at room temperature present liquid, it is complete
The salt being made up of entirely zwitterion, also referred to as low temperature molten salt, the asymmetry of organic anions and canons makes ion not in its structure
Crystal can be regularly piled into, therefore liquid is presented under normal temperature, ionic liquid is presented in discrete electrostatic interaction between zwitterion
Go out the property different from conventional liq.It is many to be now widely used for chemical synthesis, electrochemistry, extract and separate, material preparation etc.
Field.The heat endurance and poor chemical stability of chlorine aluminic acid type ionic liquid, the easy decomposed metamorphic of water is met, and corrosivity is stronger, limit
Its application is made.
The content of the invention
It is an object of the invention to provide a kind of preparation method for reclaiming the leachate of copper in waste and old circuit board, this method institute
Obtained leachate is volatile, nonflammable explosive, not oxidizable, preferable heat endurance and chemical stability, can reach green
The purpose of copper and other metals in color high efficiente callback waste and old circuit board.
The present invention is achieved in that a kind of preparation method for reclaiming the leachate of copper in waste and old circuit board, this method bag
Include following steps：
(1) methylimidazole dissolved dilution is obtained into solution 1 in solvent 1, solute is dissolved in solvent 2 and obtains solution 2,
In 40~120 DEG C of waters bath with thermostatic control and stirring environment, solution 2 is slowly added dropwise in solution 1, under nitrogen protection back flow reaction
8~24h, by reaction product filtering and washing, drying, obtain ionic liquid intermediate；Wherein, the methylimidazole, solvent 1, molten
Matter, the molal volume ratio of solvent 2 are 1mol：(50~250) mL：(0.5~2) mol：(50~250) mL, the solvent include third
Ketone, acetonitrile, the solute include bromination of n-butane, PS, monoxone；
(2) ionic liquid intermediate is dissolved in distilled water, it is 98% that mass fraction is slowly dropped into distilled water
H2SO4Solution, 8~24h of stirring reaction at 40~120 DEG C, mesh is dried to obtain after reaction product rotary evaporation is removed into distilled water
Mark ionic liquid；Wherein, the ionic liquid, distilled water, H2SO4Molal volume ratio be (0.05~0.5) mol：(50~
500)mL：(0.05~0.5) mol；
(3) will remove scolding tin electronic component and oxidant, acidic ion liquid mix, 40~100 DEG C of waters bath with thermostatic control,
Stir and 0.5~24h is reacted in environment, gained filtrate is leachate after reaction product is filtered；Wherein, the electronic component, oxygen
The mass volume ratio of agent and acidic ion liquid is (0.25~5) g：(1~10) mL：(1~10) mL.
Preferably, in step (1), the methylimidazole includes N- methylimidazoles, 1- butyl -3- methylimidazoles, 1- (3-
Sulfonic group) propyl group -3- methylimidazoles, 1- carboxymethyl -3- methylimidazoles, 1,3- dicarboxyls methylimidazole and 1- carboxymethyl -3- miaows
Azoles.
Preferably, in step (1), the methylimidazole, solvent 1, solute, the molal volume ratio of solvent 2 are
0.21mol：50mL：0.20mol：50mL.
Preferably, in step (1), the drying is that 24h is dried in 80 DEG C of vacuum drying chambers；The temperature of the water bath with thermostatic control
Spend for 60 DEG C；The time of the back flow reaction is 24h.
Preferably, in step (2), the stirring reaction 6h at 100 DEG C；The drying is to be dried in 80 DEG C of vacuum drying chambers
24h。
Preferably, in step (2), the ionic liquid, distilled water, H2SO4Molal volume ratio be 0.10mol：(50
~500) mL：0.10mol.
Preferably, in step (3), the oxidant includes the aqueous hydrogen peroxide solution that mass fraction is 30%.
Preferably, in step (3), the electronic component is the particle that crushing is 0.071~5mm particle sizes.
Preferably, in step (3), the mass volume ratio of the electronic component, oxidant and acidic ion liquid is
1g：2mL：8mL.
A kind of overcome the deficiencies in the prior art of the present invention, there is provided preparation side for reclaiming the leachate of copper in waste and old circuit board
Method.The present invention is by reacting to obtain ionic liquid the solute such as methylimidazole and bromination of n-butane, PS, monoxone
Body intermediate, then intermediate and the concentrated sulfuric acid are subjected to acidification reaction and obtain target acidic ion liquid, the ionic liquid is substantially
Respectively 1- butyl -3- methylimidazolium hydrogen sulphates salt ([BMIM] [HSO4]), 1- propane sulfonic acid base -3- methylimidazolium hydrogen sulphate salt
([PS-MIM][HSO4]), 1- carboxymethyl -3- methylimidazolium hydrogen sulphates salt ([CM-MIM] [HSO4]), 1,3- dicarboxyl methylimidazoles
Disulfate ([di-CM-IM] [HSO4]), double-(1- carboxymethyl -3- imidazoles) hexylidene disulfate ([C6(CM-IM)2]
[HSO4]2)；It is mixed to get finally by the electronic component after the ionic liquid and oxidant, crushing rich in metal ion (Cu)
Leachate.
The shortcomings that compared to prior art and deficiency, the invention has the advantages that：
(1) caused filter residue (waste residue) is mainly the macromolecules such as epoxy resin in ionic liquid preparation process of the invention
Other inorganic additives such as organic material, glass fibre and ceramics, it is environmentally friendly；
(2) leachate of the present invention is more more environmentally-friendly than the method for copper in the recovery waste and old circuit board of routine, to health of people
Harm is smaller, the recyclable recycling of ionic liquid 20 times, is of relatively low cost, and the leaching rate of copper is higher；
(3) copper in leachate of the present invention recovery waste and old circuit board, extraction time in 0.5~24h, relatively other recovery copper
Method, organic efficiency are higher；Whole leaching process crosses control temperature at 40 DEG C~100 DEG C using water-bath, whole removal process energy
Consumption is smaller；Once reclaim, technique is simple, easy to utilize.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
(1) (17.2423g, 0.21mol) N- methylimidazoles are accurately weighed to be dissolved in 20mL acetone and be added to 250mL's
In three neck round bottom flask, it is placed in 60 DEG C of thermostat water baths；Then (27.4040g, 0.20mol) bromination of n-butane is weighed
It is dissolved in 20mL acetone, is slowly added dropwise by constant pressure funnel into three neck round bottom flask.Atmosphere of the reaction system in nitrogen
Middle carry out magnetic agitation, condensing reflux reaction 24h.It is sticky through rotating, washing and water white transparency is obtained after liquid separation after reaction terminates
Shape liquid, it is placed in 80 DEG C of vacuum drying chambers and dries 24h, products therefrom is 1- butyl -3- methylimidazole bromide ionic liquids
Body intermediate ([BMIM] Br).
(2) accurately weigh (21.9126g, 0.10mol) [BMIM] Br to be placed in single necked round bottom flask, add 30mL distillations
[BMIM] Br dissolved dilutions are finally slowly dropped into (10.0073g, 0.10mol) 98%H by water2SO4, the magnetic force under the conditions of 100 DEG C
Stirring reaction 6h, acidification reaction obtain light yellow liquid after terminating.Product is placed in 80 DEG C very after rotary evaporation removing distilled water
24h is dried in empty drying box, it is object ion liquid [BMIM] [HSO to obtain faint yellow viscous liquid4]。
(3) weigh the waste and old circuit board powder that 1g particle diameters are 0.071mm~5mm to be placed in 100mL single-necked flask, and measure
2mL hydrogen peroxide and the above-mentioned acid function ionic liquids of 8mL are taken, magneton stirring reaction 1h is used in 60 DEG C of water-baths, reaction terminates
Reaction system is filtered afterwards, and remaining solid residue and leachate are separated, obtains the leachate containing metal ion.
Embodiment 2
(1) dilution of (17.2423g, 0.21mol) N- methylimidazoles is accurately weighed to be dissolved in 20mL acetonitriles and be added to
In 250mL three neck round bottom flask, it is placed in 45 DEG C of thermostat water baths；Then (24.4276g, 0.20mol) 1,3- is weighed
Propane sultone is dissolved in 50mL acetonitriles, is slowly added dropwise by constant pressure funnel into three neck round bottom flask.Reaction system exists
The atmosphere of nitrogen uses magnetic agitation, and condensing reflux reaction 24h.Reaction obtains white powder after terminating after filtering, washing
Shape solid, it is placed in 80 DEG C of vacuum drying chambers and dries 24h.Products therefrom is 1- propane sulfonic acid base -3- methylimidazole inner salts
Ionic liquid intermediate (PS-MIM).
(2) (20.4244g, 0.10mol) PS-MIM is accurately weighed again to be placed in single necked round bottom flask, adds appropriate steaming
Distilled water dissolves PS-MIM, is finally slowly dropped into (10.0073g, 0.10mol) 98%H2SO4, the magnetic agitation under the conditions of 100 DEG C
6h is reacted, acidification reaction obtains pale yellow oily liquid after terminating.Product is placed in 80 DEG C very after rotary evaporation removing distilled water
24h is dried in empty drying box, it is object ion liquid [PS-MIM] [HSO to obtain faint yellow viscous liquid4]。
(3) weigh the waste and old circuit board powder that 1g particle diameters are 0.071mm~5mm to be placed in 100mL single-necked flask, and measure
2mL hydrogen peroxide and the above-mentioned acid function ionic liquids of 8mL are taken, magneton stirring reaction 1h is used in 60 DEG C of water-baths, reaction terminates
Reaction system is filtered afterwards, and remaining solid residue and leachate are separated, obtains the leachate containing metal ion.
Embodiment 3
(1) (17.2423g, 0.21mol) N- methylimidazoles dissolved dilution is accurately weighed in 20mL acetone and is added sequentially to
In 250mL three neck round bottom flask, it is placed in 60 DEG C of thermostat water baths；Then (18.8988g, 0.20mol) chloroethene is weighed
Acid is dissolved in 50mL acetone, is slowly added dropwise by constant pressure funnel into three neck round bottom flask.Reaction system is in nitrogen atmosphere
It is middle to use magnetic agitation, and back flow reaction 24h.Reaction obtains white powdery solids after terminating after filtering and washing, is put
24h is dried in 80 DEG C of vacuum drying chambers.Products therefrom is 1- carboxymethyl -3- methylimidazole villaumite ionic liquid intermediates
([CM-MIM]Cl)。
(2) weigh (17.6600g, 0.10mol) [CM-MIM] Cl to be placed in single necked round bottom flask, add appropriate distillation
Water dissolves [CM-MIM] Cl, is finally slowly dropped into (10.0073g, 0.10mol) 98%H2SO4, magnetic agitation is anti-at 100 DEG C
6h, acidification reaction is answered to obtain faint yellow viscous liquid after terminating.Product is placed in 80 DEG C very after rotary evaporation removing distilled water
24h is dried in empty drying box, it is object ion liquid [CM-MIM] [HSO to obtain faint yellow viscous liquid4]。
(3) weigh the waste and old circuit board powder that 1g particle diameters are 0.071mm~5mm to be placed in 100mL single-necked flask, and measure
2mL hydrogen peroxide and the above-mentioned acid function ionic liquids of 8mL are taken, magneton stirring reaction 1h is used in 60 DEG C of water-baths, reaction terminates
Reaction system is filtered afterwards, and remaining solid residue and leachate are separated, obtains the leachate containing metal ion.
Embodiment 4
(1) (14.2966g, 0.21mol) imidazoles is accurately weighed to be dissolved in 50mL acetone and be added to 250mL three mouthfuls of round bottoms
In flask, it is placed in 60 DEG C of thermostat water baths；Then weigh (37.7976g, 0.40mol) monoxone and be dissolved in 50mL acetone
In, it is slowly added dropwise by constant pressure funnel into three neck round bottom flask.Reaction system carries out magnetic force in the atmosphere of nitrogen and stirred
Mix, and back flow reaction 24h.Reaction obtains white powdery solids after terminating after filtering, washing, and is placed on 80 DEG C of vacuum and does
24h is dried in dry case.Products therefrom is 1,3- dicarboxyl methylimidazole villaumite ionic liquids intermediate ([di-CM-IM] Cl).
(2) (22.0609g, 0.10mol) [di-CM-IM] Cl is weighed again to be placed in single necked round bottom flask, is added appropriate
Distilled water dissolves [di-CM-IM] Cl, is finally slowly dropped into (10.0073g, 0.10mol) 98%H2SO4, under the conditions of 100 DEG C
Magnetic agitation reacts 6h, and acidification reaction obtains faint yellow viscous liquid after terminating.By product after rotary evaporation removing distilled water
It is placed in 80 DEG C of vacuum drying chambers and dries 24h, it is object ion liquid [di-CM-IM] to obtain faint yellow viscous liquid
[HSO4]。
(3) weigh the waste and old circuit board powder that 1g particle diameters are 0.071mm~5mm to be placed in 100mL single-necked flask, and measure
2mL hydrogen peroxide and the above-mentioned acid function ionic liquids of 8mL are taken, magneton stirring reaction 1h is used in 60 DEG C of water-baths, reaction terminates
Reaction system is filtered afterwards, and remaining solid residue and leachate are separated, obtains the leachate containing metal ion.
Embodiment 5
(1) (14.2966g, 0.21mol) imidazoles is accurately weighed to be dissolved in 50mL acetone and be added to 250mL three mouthfuls of round bottoms
In flask, it is placed in 60 DEG C of thermostat water baths；Then (24.3970g, 0.10mol) 1,6- dibromo-hexanes are weighed to be dissolved in
In 20mL acetone, it is slowly added dropwise by constant pressure funnel into three neck round bottom flask.Reaction system is adopted in the atmosphere of nitrogen
With magnetic agitation, and condensing reflux reaction 24h.It is sticky that reaction after rotary evaporation, washing and liquid separation obtains yellowish-brown after terminating
Shape liquid, it is placed in 80 DEG C of vacuum drying chambers and dries 24h.Products therefrom is double-(3- imidazoles) hexylidene dibromo salt ion
Liquid intermediate (I) ([C6(IM)2]Br2)。
(2) (7.6026g, 0.02mol) [C is accurately weighed again6(IM)2]Br2It is placed in single necked round bottom flask, adds suitable
Distilled water is measured by [C6(IM)2]Br2Dissolve and be added in 100mL three neck round bottom flask, be placed on 60 DEG C of thermostat water baths
In；Then weigh (3.8743g, 0.041mol) monoxone to be dissolved in appropriate distilled water, by constant pressure funnel to three mouthfuls of circles
It is slowly added dropwise in the flask of bottom.Reaction system uses magnetic agitation, and condensing reflux reaction 24h in the atmosphere of nitrogen.Reaction terminates
By pale yellow oily liquid is obtained after rotary evaporation, washing and liquid separation, it is placed in 80 DEG C of vacuum drying chambers and dries 24h.
Gained yellowish-brown viscous liquid is double-(1- carboxymethyl -3- imidazoles) hexylidene dichloro ionic liquid intermediate (II) ([C6
(CM-IM)2]Cl2)。
(3) (8.1458g, 0.02mol) [C is weighed6(CM-IM)2]Cl2It is placed in single necked round bottom flask, adds appropriate steaming
Distilled water is by [C6(CM-IM)2]Cl2Dissolving, is finally slowly dropped into (2.0015g, 0.02mol) 98%H2SO4, the magnetic force at 100 DEG C
Stirring reaction 6h, acidification reaction obtain yellowish-brown oily liquids after terminating.Product is placed in 80 after rotary evaporation removing distilled water
24h is dried in DEG C vacuum drying chamber, it is object ion liquid ([C to obtain pale yellow oily liquid6(CM-IM)2][HSO4]2)。
(4) weigh the waste and old circuit board powder that 1g particle diameters are 0.071mm~5mm to be placed in 100mL single-necked flask, and measure
2mL hydrogen peroxide and the above-mentioned acid function ionic liquids of 8mL are taken, magneton stirring reaction 1h is used in 60 DEG C of water-baths, reaction terminates
Reaction system is filtered afterwards, and remaining solid residue and leachate are separated, obtains the leachate containing metal ion.
Embodiment 6
(1) 1mol 1- butyl -3- methylimidazoles dissolved dilutions are obtained into solution 1 in 50mL acetonitriles, by 50mL 1,3-
Propane sultone, which is dissolved in solvent 2, obtains solution 2, and in 40 DEG C of waters bath with thermostatic control and stirring environment, solution 2 is slowly added dropwise
In solution 1, back flow reaction 8h under nitrogen protection, by reaction product filtering and washing, 24h is dried in 80 DEG C of vacuum drying chambers, is obtained
To ionic liquid intermediate；
(2) 0.05mol ionic liquid intermediates are dissolved in 50mL distilled water, be slowly dropped into distilled water
0.05mol mass fractions are 98% H2SO4Solution, the stirring reaction 8h at 40 DEG C, reaction product rotary evaporation is removed and distilled
Water, 24h is dried in 80 DEG C of vacuum drying chambers and obtains object ion liquid；
(3) 0.25g is removed into scolding tin and crushes the electronic component and 1mL mass fractions for 0.071mm particles sizes
Mixed for 30% aqueous hydrogen peroxide solution, 1mL acidic ion liquids, react 0.5h in 40 DEG C of waters bath with thermostatic control, stirring environment,
Gained filtrate is leachate after reaction product is filtered.
Embodiment 7
(1) 1mol 1,3- dicarboxyl methylimidazole dissolved dilutions are obtained into solution 1 in 250mL acetone, by 250mL chloroethenes
Acid, which is dissolved in solvent 2, obtains solution 2, and in 120 DEG C of waters bath with thermostatic control and stirring environment, solution 2 is slowly added dropwise into solution 1
In, back flow reaction 24h under nitrogen protection, by reaction product filtering and washing, 24h is dried in 80 DEG C of vacuum drying chambers, obtain from
Sub- liquid intermediate；
(2) 0.5mol ionic liquid intermediates are dissolved in 500mL distilled water, 0.5mol is slowly dropped into distilled water
Mass fraction is 98% H2SO4Solution, the stirring reaction 24h at 120 DEG C, by reaction product rotary evaporation remove distilled water, 80
24h is dried in DEG C vacuum drying chamber and obtains object ion liquid；
(3) 5g is removed into scolding tin and crushing is the electronic component of 5mm particles sizes and 10mL mass fractions are 30%
Aqueous hydrogen peroxide solution, 10mL acidic ion liquids mixing, 40~100 DEG C of waters bath with thermostatic control, stirring environment in reaction 0.5~
24h, gained filtrate is leachate after reaction product is filtered.
In various embodiments above, methylimidazole dosage can be adjusted in proper range, corresponding solvent load with it is molten
Matter dosage also can be adjusted suitably as needed.
Waste and old circuit board powder of the particle diameter in 0.071~5mm used in the disengaging step of various embodiments above can be according to need
Adjust, the dosage of oxidant and acid function ionic liquid can also adjust according to being actually needed, 40 DEG C~80 DEG C of extraction temperature
It can need to adjust according to production, 0.5~24h of time also can be suitably adjusted.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (9)
1. a kind of preparation method for reclaiming the leachate of copper in waste and old circuit board, it is characterised in that this method comprises the following steps：
(1) methylimidazole dissolved dilution is obtained into solution 1 in solvent 1, solute is dissolved in solvent 2 and obtains solution 2,40
~120 DEG C of waters bath with thermostatic control and stirring environment in, solution 2 is slowly added dropwise in solution 1, under nitrogen protection back flow reaction 8~
24h, by reaction product filtering and washing, drying, obtain ionic liquid intermediate；Wherein, the methylimidazole, solvent 1, solute,
The molal volume ratio of solvent 2 is 1mol：(50~250) mL：(0.5~2) mol：(50~250) mL, the solvent include acetone,
Acetonitrile, the solute include bromination of n-butane, PS, monoxone；
(2) ionic liquid intermediate is dissolved in distilled water, the H that mass fraction is 98% is slowly dropped into distilled water2SO4
Solution, 8~24h of stirring reaction at 40~120 DEG C, will reaction product rotary evaporation remove distilled water after be dried to obtain target from
Sub- liquid；Wherein, the ionic liquid, distilled water, H2SO4Molal volume ratio be (0.05~0.5) mol：(50~500) mL：
(0.05~0.5) mol；
(3) electronic component for removing scolding tin and oxidant, acidic ion liquid are mixed, in 40~100 DEG C of waters bath with thermostatic control, stirring
0.5~24h is reacted in environment, gained filtrate is leachate after reaction product is filtered；Wherein, the electronic component, oxidant
And the mass volume ratio of acidic ion liquid is (0.25~5) g：(1~10) mL：(1~10) mL.
2. the preparation method of the leachate of copper in waste and old circuit board is reclaimed as claimed in claim 1, it is characterised in that in step
(1) in, the methylimidazole includes N- methylimidazoles, 1- butyl -3- methylimidazoles, 1- (3- sulfonic groups) propyl group -3- methyl miaows
Azoles, 1- carboxymethyl -3- methylimidazoles, 1,3- dicarboxyls methylimidazole and 1- carboxymethyl -3- imidazoles.
3. the preparation method of the leachate of copper in waste and old circuit board is reclaimed as claimed in claim 1, it is characterised in that in step
(1) in, the methylimidazole, solvent 1, solute, the molal volume ratio of solvent 2 are 0.21mol：50mL：0.20mol：50mL.
4. the preparation method of the leachate of copper in waste and old circuit board is reclaimed as claimed in claim 1, it is characterised in that in step
(1) in, the drying is that 24h is dried in 80 DEG C of vacuum drying chambers；
The temperature of the water bath with thermostatic control is 60 DEG C；
The time of the back flow reaction is 24h.
5. the preparation method of the leachate of copper in waste and old circuit board is reclaimed as claimed in claim 1, it is characterised in that in step
(2) in, the stirring reaction 6h at 100 DEG C；
The drying is that 24h is dried in 80 DEG C of vacuum drying chambers.
6. the preparation method of the leachate of copper in waste and old circuit board is reclaimed as claimed in claim 1, it is characterised in that in step
(2) in, the ionic liquid, distilled water, H2SO4Molal volume ratio be 0.10mol：(50~500) mL：0.10mol.
7. the preparation method of the leachate of copper in waste and old circuit board is reclaimed as claimed in claim 1, it is characterised in that in step
(3) in, the oxidant includes the aqueous hydrogen peroxide solution that mass fraction is 30%.
8. the preparation method of the leachate of copper in waste and old circuit board is reclaimed as claimed in claim 1, it is characterised in that in step
(3) in, the electronic component is the particle that crushing is 0.071~5mm particle sizes.
9. the preparation method of the leachate of copper in waste and old circuit board is reclaimed as claimed in claim 1, it is characterised in that in step
(3) in, the mass volume ratio of the electronic component, oxidant and acidic ion liquid is 1g：2mL：8mL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711257724.4A CN107841631A (en) | 2017-12-04 | 2017-12-04 | The preparation method of the leachate of copper in a kind of recovery waste and old circuit board |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711257724.4A CN107841631A (en) | 2017-12-04 | 2017-12-04 | The preparation method of the leachate of copper in a kind of recovery waste and old circuit board |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114807611A (en) * | 2022-04-18 | 2022-07-29 | 上海第二工业大学 | Method for gently stripping circuit board metal coating and separating and recovering metal/nonmetal components in substrate |
| CN115254869A (en) * | 2022-06-07 | 2022-11-01 | 昆明理工大学 | Supercritical fluid-based method and device for extracting valuable metals from high-calcium silicon solid waste |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104928480A (en) * | 2015-07-17 | 2015-09-23 | 兰州理工大学 | Functionalized ionic liquid pyrolysis water leaching method for recovering metal from circuit board |
| CN106966898A (en) * | 2017-04-21 | 2017-07-21 | 江苏天音化工有限公司 | A kind of method that presence of acidic ionic liquid catalyst synthesizes dipropylene glycol methyl ether acetate |
-
2017
- 2017-12-04 CN CN201711257724.4A patent/CN107841631A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104928480A (en) * | 2015-07-17 | 2015-09-23 | 兰州理工大学 | Functionalized ionic liquid pyrolysis water leaching method for recovering metal from circuit board |
| CN106966898A (en) * | 2017-04-21 | 2017-07-21 | 江苏天音化工有限公司 | A kind of method that presence of acidic ionic liquid catalyst synthesizes dipropylene glycol methyl ether acetate |
Non-Patent Citations (2)
| Title |
|---|
| 李文喜等: "酸性离子液体[BMIM]HSO4的合成及其性能测定", 《辽宁化工》 * |
| 李静等: "酸性离子液体合成及其催化合成", 《生物质化学工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114807611A (en) * | 2022-04-18 | 2022-07-29 | 上海第二工业大学 | Method for gently stripping circuit board metal coating and separating and recovering metal/nonmetal components in substrate |
| CN115254869A (en) * | 2022-06-07 | 2022-11-01 | 昆明理工大学 | Supercritical fluid-based method and device for extracting valuable metals from high-calcium silicon solid waste |
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