CN108070528B - A kind of recovery system and recovery method of spent resin powder - Google Patents
A kind of recovery system and recovery method of spent resin powder Download PDFInfo
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Abstract
The invention discloses a kind of recovery systems of spent resin powder, including microbial cultivation device, leaching device, sedimentation device, copper recyclable device, salt bath unit, heavy lead device, wash mill, drying device and solid-liquid separating machine, the invention also discloses a kind of recovery methods of spent resin powder, including microorganism growing step, leaching stage, subsidence stage, copper recovery stage, salt soak stage, heavy lead phase, washing stage and drying stage.Present invention reduces the periods of spent resin powder biological copper leaching, improve production efficiency, it is soaked using sodium chloride salt, the lead in spent resin powder can be effectively removed, and lead is individually recycled, it is high to leach the innoxious degree of residue, furthermore, resource circulation utilization of the invention has saved the utilization rate that resource also improves resource, has reduced production cost.
Description
Technical field
The invention belongs to bioanalysis to comprehensively utilize solid waste technical field, and in particular to a kind of recycling of spent resin powder
System and recovery method.
Background technique
With the further development of electronic technology, the period that electronic product updates constantly shortens, Waste ammunition
Quantity it is growing day by day, this causes serious harm, especially printed circuit board, copper-clad plate leftover pieces etc. to environment.Cover copper
Plate is the raw material of electronics industry, and structure includes substrate, copper foil, copper-clad plate adhesive etc., is made by wood pulp paper or glass-fiber-fabric etc.
Reinforcing material is soaked with resin, and single or double is formed coated with copper foil through hot pressing.Copper-clad plate, can be in addition to being fabricated to circuit board
For electronic products such as television set, radio, computer, computer, mobile communication.The useless copper-clad plate leftover pieces master of mechanical sorting at present
Processing method is wanted, is using the physical property difference (such as density, electrical property, magnetism, shape and surface nature) between substance come real
The separation of existing different material after recycling wherein metallic copper, but still generates a large amount of spent resin powder, mostly as offal treatment
Disposition, had not efficiently used wherein metal and Non-metallic components.Such useless copper-clad plate, printed wiring board, circuit board cracking and sorting
The spent resin powder that generates usually contains the copper of 0.5-2.0% and the lead of 0.1-1.0% after recycling metal, causes subsequent to remanufacture production
Quality is poor, seriously affects its application, and be listed according to Leaching characteristic and be accredited as National Hazard solid waste, discomfort is fit to do filling out
Bury processing.In view of wherein copper content also above averagely can development level, if metal therein can be separated and recovered, both
Metal can be obtained, and value of the Non-metallic components as packing material can be improved.Spent resin powder can only use wet-leaching at present
Method handled, although can achieve the purpose that mention copper using traditional acidleach and ammonia leaching, but at high cost, reagent consumption compared with
Greatly, and secondary pollution easy to form.
In wet-leaching technology, microbial metallurgy technique is mild and environmental-friendly etc. at low cost, simple process, reaction
Feature and be concerned.Chinese patent literature CN201880729U discloses a kind of abandoned printed circuit board recycling and processing device,
The device is designed using roller, solve the problems, such as to be superimposed between particle it is easily settled, using Acidithiobacillus
Ferroxidans and Acidithiobacillus thiooxidans biology extraction time is 3-10 days, copper content in leachate
Up to 3.5g/L, but the document does not have specific material component to analyze, and does not refer to leaching rate, and leaching cycle is too long.
Chinese patent literature CN102218437A discloses a kind of recovery method of discarded circuit board, broken wiring board warp
Copper particle and tailings are obtained after broken and gravity treatment, tailings is crushed gravity treatment again and obtains copper powder and non-metal powder, and sulphur is added in non-metal powder
Acid adjusts pH value to 1.5-3.5, is that kind of liquid carries out with Thiobacillus ferrooxidans Acidithiobacillus ferrooxidans
Bioleaching, leachate obtain tough cathode using extraction electrodeposition, and residual residue can be used as a kind of composite material.The method is to cupric
The non-metal powder for measuring 0.2-0.4% carries out Bioleaching, and solid-to-liquid ratio 1:6-1:3 extraction time 24-48 hours, is obtained
Copper content is the fiberglass resin composite material of 0.05-0.07%.But the technique is still the Bioleaching being conducted batch-wise, and strain list
One, and leaching cycle is longer.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of recovery system of spent resin powder and recycling side
Method.
The present invention provides a kind of recovery system of spent resin powder, including microbial cultivation device, leaching device, sedimentation dress
It sets, copper recyclable device, salt bath unit, heavy lead device, wash mill, drying device and solid-liquid separating machine；
The microbial cultivation device includes culture tank, and aeration component, pH control assembly, temperature are provided in the culture tank
Control component and biofilm filler assembly, obtained microbial culture medium enter leaching device；
The leaching device includes leaching tanks, and aeration component, pH control assembly, temperature control component are provided in the leaching tanks
And agitating paddle, the substance after leaching enter sedimentation device；
The sedimentation device includes subsider, and the cupric supernatant after sedimentation enters copper recyclable device, leaded heavy after sedimentation
Drop slag enters solid-liquid separating machine；
The copper recyclable device includes the filter device for receiving the cupric supernatant after sedimentation, receives filtered cupric filter
The extraction equipment of liquid, receives the neutralization precipitation device of extract liquor extracted, and the neutralization precipitation device includes neutralization precipitation slot
With the agitating paddle being arranged in neutralization precipitation slot, the substance after neutralization precipitation is after solid-liquid separating machine, isolated iron aluminum slag
With liquid after neutralization precipitation, liquid returns to microbial cultivation device after neutralization precipitation；
Leaded sedimentation slag after sedimentation obtains clear liquid and leaded filter residue after solid-liquid separating machine, and clear liquid returns to microorganism
Culture apparatus, leaded filter residue enter salt bath unit；
The salt bath unit includes salt immersion trough and the agitating paddle that is arranged in salt immersion trough, and the substance after salt leaching is by solid-liquid point
After disembarking, obtains leaded leachate and decopper(ing) takes off the leached mud after lead, leaded leachate enters precipitating lead device, after decopper(ing) takes off lead
Leached mud enter wash mill；
The heavy lead device includes heavy lead bath and the agitating paddle to sink in lead bath is arranged in, and the substance after heavy lead is by solid-liquid point
After disembarking, liquid after isolated concentrate of lead sulfide ore and heavy lead, sink lead after liquid return salt bath unit；
The wash mill includes sink and the agitating paddle that is arranged in sink, and the substance after washing is by solid-liquid point
After disembarking, isolated filtrate and filter residue, filtrate return to wash mill, and filter residue enters drying device；
The drying device includes drying machine, obtains resin and glass fibre after filter residue and drying.
Preferably, the solid-liquid separating machine is one of plate and frame filter press and centrifuge.
Preferably, the drying machine is one of roller drying machine, band drier and baking oven.
The present invention also provides a kind of recovery method of spent resin powder, including microorganism growing step, leaching stage settles rank
Section, copper recovery stage, salt soak stage, heavy lead phase, washing stage and drying stage,
A. the microorganism growing step, there is following steps: active bacteria is accessed in basal medium, at 30-45 DEG C
Lower aeration culture, until the cell concentration in solution reaches 108-109Filler is added in a/mL, and biofilm culture gradually starts, even
Continuous culture, obtains microbial culture medium；
B. the leaching stage, there is following steps: being according to volume mass ratio with spent resin powder by microbial culture medium
1.5-3L:1kg is stirred and evenly mixed, mixing speed 50-200rpm, and extraction temperature is 20-45 DEG C, and extraction time 2-5h is obtained
Leaching slurry；
C. the subsidence stage, there is following steps: leaching slurry is entered in subsider and is settled, obtain cupric supernatant and
Leaded sedimentation slag；
D. the copper recovery stage, there is following steps: cupric filtrate is obtained after the filtering of cupric filtrate, when copper in cupric filtrate
Concentration be 4g/L or more when, with copper extractant solution extract, extraction agent solution and cupric filtrate volume ratio be 1-2:1, extraction
Extract liquor after taking adds alkali to adjust pH to carry out neutralization precipitation, then liquid after isolated iron aluminum slag and neutralization precipitation, neutralization precipitation
Liquid returns to microbial cultivation device afterwards；
E. the salt soaks the stage, and have following steps: leaded sedimentation slag obtains clear liquid and leaded filter after solid-liquid separating machine
Slag, clear liquid return to microbial cultivation device, the sodium chloride solution that concentration is 100-250g/L are added into leaded filter residue, in room temperature
Lower leaching lead, the pH of solution are 5.5-7.0, and leaded leachate is obtained by filtration after the completion of leaching and decopper(ing) takes off the leached mud after lead；
F. the heavy lead phase, there is following steps: sodium sulfide solution reaction, mistake after having reacted being added into leaded leachate
Filter obtains liquid after concentrate of lead sulfide ore and heavy lead, and liquid returns to the salt leaching stage after heavy lead；
G. washing stage:
By washing twice, substance each time after washing separates leached mud after the de- lead of decopper(ing) after being separated by solid-liquid separation
To filtrate and filter residue, filtrate returns to wash mill, and filter residue enters drying device.
H. drying stage:
Filter residue obtains innoxious resin and glass fibre after drying.
Preferably, the composition of basal medium described in process A and respective content are as follows: ammonium sulfate 1.5-3g/L, seven water sulphur
Sour magnesium 0.25-0.5g/L, potassium hydrogen phosphate 0.5-0.8g/L, potassium chloride 0.1-0.12g/L, calcium nitrate 0.01-0.05g/L, sulphur powder
0-10g/L, ferrous sulfate heptahydrate 30-50g/L are 1.5-2 with sulphur acid for adjusting pH.
Preferably, active bacteria described in process A be include thermophilic iron hook end screw rod Pseudomonas (Leptospirillum
Sp.), acidophilus Sulfobacillus (Sulfobacillus sp.) and thiobacillus ferrooxidans belong to (Acidithiobacillus sp.) and exist
One of interior microorganism with acidophilia iron oxidation characteristic is a variety of.
Preferably, active bacteria described in process A is that acidophilus iron aoxidizes hook end spirillum CS13 (Leptospirillum
Ferriphilum), acidophilus Sulfobacillus CS17 (Sulfobacillus thermossulfidooxidans), ferrous oxide sulphur
Bacillus CS 78 (Acidithiobacillus ferrooxidans) and acidophilus iron Thiobacillus CS12 (Acidithiobacillus
Ferrivorans one of) or a variety of.
Preferably, biofilm filler described in process A is the useless spent resin module that grid or silk screen encapsulate.
Preferably, extractant described in step D is hydroxy aldehyde (ketone) oximes extractant N902, M5640, CP150, LIX984
One of.
Preferably, extraction described in step D is extracted using two-stage extraction, level-one washing, level-one stripping process, when anti-
When the concentration for extracting copper in liquid is 45g/L or more, metallic copper is recycled by the way of metal electro-deposition or condensing crystallizing, it is extracted
Solution hydrogenation sodium oxide molybdena adjusts pH value to return to microculture after filtering and removing slag after 2.5-3.5.
Spent resin powder of the present invention refers to useless copper-clad plate, printed wiring board, circuit board cracking and sorting recycling metal
The spent resin powder generated afterwards.
The beneficial effects of the present invention are:
1, high-effective microorganism is cultivated in independent flow reactor, and microorganism is allowed to reach higher thin under optimum conditions
Bacteria concentration and activity enter back into spent resin powder powder leaching reactor, solve micro- life in spent resin powder bioleaching process
The low problem of object concentration, not only shortens the period of spent resin powder biological copper leaching, improves production efficiency, and phegma also can
The bacterial concentration in Leaching Systems is improved, the stability of system is improved, spent resin powder can be realized under the conditions of high solid-liquid ratio
It is continuous to leach, meet industrial requirement.It is soaked using sodium chloride salt, the lead in spent resin powder can be effectively removed, and lead is individually returned
It receives, leaches the innoxious degree height of residue, meet " household refuse landfill sites contamination control standard " (GB16889-2008) leachate
Limit value requires and " general industrial solid waste storage, disposal site contamination control standard " general work of (GB18599-2001) I class
The requirement of industry solid waste.
2, liquid returns to microbial cultivation device after the neutralization precipitation that copper recovery stage generates, and the clear liquid that the salt leaching stage generates returns
Microbial cultivation device is returned, liquid returns to the salt leaching stage after the heavy lead that heavy lead phase generates, and the cleaning solution of washing stage can recycle
It uses, has saved the utilization rate that resource also improves resource, reduced production cost.
2, using spent resin powder instead of tradition such as traditional suspended biological filler, polyurethane sponge, 3 D elastic fillers
Biofilm filler, not only save cost, and the microorganism of leaching is also tamed and adapts to useless tree in incubation
Cosmetics environment is conducive to shorten cultivation cycle, improves the leaching efficiency of copper, increases the microorganism concn in incubation, and cultivate
The loss of microorganism is not easily caused in the process, the filler of failure then may continue as process object and extracting stage is added, and reduce film
Pollute the emission problem of filler.
Acidophilus iron aoxidizes hook end spirillum CS13 (Leptospirillum ferriphilum), depositary institution: Chinese allusion quotation
Type culture collection, deposit number: CCTCCM2015010；Acidophilus Sulfobacillus CS17 (Sulfobacillus
Thermosulfidooxidans), depositary institution: China typical culture collection center, deposit number: CCTCC M 2015011；
Thiobacillus ferrooxidans CS 78 (Acidithiobacillus ferrooxidans), depositary institution: Chinese Typical Representative culture is protected
Hiding center, deposit number: CCTCCM2015016；Acidophilus iron Thiobacillus CS12 (Acidithiobacillus ferrivorans),
Depositary institution: China typical culture collection center, deposit number: CCTCC:M 2015009.
Above-mentioned iron aluminum slag and concentrate of lead sulfide ore are post-processed, and the prior art is belonged to.
Leached mud after the de- lead of above-mentioned decopper(ing) passes through resin and glass fibre that washing is dried to obtain, can be further processed
At material, belong to the prior art.
Detailed description of the invention
Fig. 1 is the device of the invention structure chart.
1 aeration component, 2pH control assembly, 3 temperature control components, 4 agitating paddles, 5 solid-liquid separating machines, 11 culture tanks, 12 biofilms are filled out
Expect component, 21 leaching tanks, 31 subsiders, 41 filter devices, 42 extraction equipments, 43 neutralization precipitation slots, 51 salt immersion troughs, 61 heavy lead
Slot, 71 sinks, 81 drying machines.
Specific embodiment
The recovery system and recovery method combination accompanying drawings and embodiments of a kind of spent resin powder proposed by the present invention are furtherly
It is bright as follows:
The recovery system of spent resin powder of the invention, basic structure is as shown in Figure 1, including microbial cultivation device, leaching
Device, sedimentation device, copper recyclable device, salt bath unit, heavy lead device, wash mill, drying device and equipment for separating liquid from solid.
The present invention recycles the course of work of spent resin powder using above system are as follows:
Basal medium and active bacteria are added in culture tank 11, aeration component 1 is opened, passes through 3 He of temperature control component
PH control assembly 2 controls temperature and pH respectively, until the cell concentration in solution reaches 108-109Filler, biofilm is added in a/mL
Culture, gradually starts, continuous to cultivate, and obtained microbial culture medium enters in leaching tanks 21, opens agitating paddle 4 and spent resin powder
It mixes, opens aeration component 1, temperature and pH are controlled by temperature control component 3 and pH control assembly 2 respectively, after the completion of Leach reaction
Mixture enter subsider 31, the leaded sedimentation slag after sedimentation enters in solid-liquid separating machine 5, and cupric supernatant enters filtering
Device 41, filtered cupric filtrate enter extraction equipment 42, and extract liquor extracted enters neutralization precipitation slot 43, neutralization precipitation
Substance afterwards is after solid-liquid separating machine 5, liquid after isolated iron aluminum slag and neutralization precipitation, and liquid returns to microorganism after neutralization precipitation
Culture apparatus, leaded sedimentation slag after sedimentation pass through solid-liquid separating machine, after 5, obtain clear liquid and leaded filter residue, clear liquid returns to micro- life
Object culture apparatus, leaded filter residue enter salt immersion trough 51, and the substance after salt leaching obtains leaded leachate after solid-liquid separating machine 5
Leached mud after taking off lead with decopper(ing), leaded leachate enter precipitation tank 61, and the leached mud after the de- lead of decopper(ing) enters wash mill, sinks
Substance after lead is after solid-liquid separating machine 5, liquid after isolated concentrate of lead sulfide ore and heavy lead, and liquid returns to salt leaching dress after heavy lead
Set, decopper(ing) take off lead after leached mud by sink 71 washing after after solid-liquid separating machine 5, isolated filtrate and filter residue,
Filtrate returns to wash mill, and filter residue enters drying machine 81, obtains resin and glass fibre after dry.
Embodiment 1
A. microorganism growing step:
Basal medium is configured, component content: ammonium sulfate 3g/L, epsom salt 0.5g/L, potassium hydrogen phosphate 0.8g/L,
Potassium chloride 0.12g/L, calcium nitrate 0.05g/L, ferrous sulfate heptahydrate 50g/L, sulphur powder 10g/L, with sulphur acid for adjusting pH to 2, by base
Basal culture medium is added in culture tank, and presses inoculum concentration 10% for 78 (Acidithiobacillus of Thiobacillus ferrooxidans CS
Ferrooxidans it) is inoculated into culture tank, is cultivated at 30 DEG C of temperature, until the cell concentration in solution reaches 108A/
Grid packing is added in mL, and biofilm culture, gradually starting obtains bacterial concentration 1.31 × 10 continuously with culture8Micro- life of a/mL
The oxidation-reduction potential of object culture solution, culture solution is 709mV, and design parameter is as shown in table 1.
B. leaching stage:
Microbial culture medium is imported in the leaching tanks of 100L, is that 2L:1kg addition copper content is according to volume mass ratio
0.99%, lead tolerance 0.5%, moisture content 16%, the spent resin powder powder of 150 mesh of partial size, which stirs evenly, to carry out leaching pre- open
Dynamic, mixing speed 120rpm, leaching pretrigger temperature is 30 DEG C, time 7h, monitors the pH of leachate in this process
Value, copper ion concentration simultaneously calculate leaching rate, ferrous ion concentration, iron concentration, bacterial concentration, and specific value is as shown in table 2.
Temperature in leaching tanks is controlled and is continuously leached within the scope of 25~30 DEG C, speed of agitator 200rpm, when leaching stop
Between 4h, obtain leaching slurry.
C. subsidence stage:
Leaching slurry enters in subsider, obtains cupric supernatant and leaded sedimentation slag by separation of solid and liquid.On cupric
The cupric filtrate that clear liquid obtains after filtering enters extraction equipment, settles slag through slush pump and imports solid-liquid separation system.
D. copper recovery stage:
When the concentration of copper in cupric filtrate is 4g/L or more, extracted with the N902 copper extractant solution that volume fraction is 10%
It takes, the volume ratio of the two is 1:1, is extracted using two-stage extraction, level-one washing, level-one stripping process, until in strip liquor
When the concentration of copper is 45g/L or more, metallic copper is recycled by the way of metal electro-deposition or condensing crystallizing, and raffinate solution adds
Sodium hydroxide is adjusted after pH value is 2.5-3.5, and liquid after isolated iron aluminum slag and neutralization precipitation, liquid returns to micro- life after neutralization precipitation
Object culture apparatus.
E. salt soaks the stage:
Leaded sedimentation slag obtains clear liquid and leaded filter residue after solid-liquid separating machine, and clear liquid returns to microbial cultivation device,
Leaded filter residue is added in salt immersion trough to react at room temperature with the sodium chloride solution of 250g/L, and the pH of solution is 5.5, reacts 0.5h
Afterwards, leaded leachate is obtained by filtration and decopper(ing) takes off the leached mud after lead, Pb in leaded leachate2+Concentration can reach 1.3g/L.
F. heavy lead phase
Sodium sulfide solution reaction is added into leaded leachate, the amount of addition is 1.5 times of theoretical amount, after reacting 1h,
Filtering
Liquid after the concentrate of lead sulfide ore and heavy lead of lead tolerance 66% is obtained, the liquid after lead that sinks returns to salt and soaks the stage.
G. washing stage:
By washing twice, substance each time after washing separates leached mud after the de- lead of decopper(ing) after being separated by solid-liquid separation
To filtrate
And filter residue, filtrate return to wash mill, filter residue enters drying device.
H. drying stage:
Filter residue obtains the resin and mixture of glass fibers of low copper and lead content after drying.
1 microbial culture medium of table analyzes result
Table 2 leaches leachate analysis result in pre-boot process
Leaching pre-boot process, microorganism to the leaching rate of copper in spent resin powder up to 94.99%, continuous leaching process
The leaching rate of copper in Microorganism Leaching spent resin powder is up to 93% or more, the glass and epoxy resin composite material that obtain after cleaning
Middle copper content is reduced to 0.04% hereinafter, lead content is lower than 0.05%, and every heavy metal all meets " household refuse landfill sites pollution
Control standard " (GB16889-2008) leachate limit value requires and " general industrial solid waste storage, disposal site contamination control mark
It is quasi- " requirement of (GB18599-2001) I class general industrial solid waste.
Embodiment 2
A. microorganism growing step:
Configure basal medium, component content: ammonium sulfate 1.5g/L, epsom salt 0.25g/L, potassium hydrogen phosphate
0.5g/L, potassium chloride 0.1g/L, calcium nitrate 0.01g/L, ferrous sulfate heptahydrate 30g/L will be basic with sulphur acid for adjusting pH to 1.5
Culture medium is added in culture tank, and presses inoculum concentration 10% for 78 (Acidithiobacillus of Thiobacillus ferrooxidans CS
Ferrooxidans), acidophilus iron oxidation hook end spirillum CS13 (Leptospirillum ferriphilum) and acidophilus vulcanization
The mixed bacteria of bacillus CS17 (Sulfobacillus thermosulfidooxidans) is inoculated into culture tank, in temperature 45
It is cultivated at DEG C, until the cell concentration in solution reaches 108A/mL, is added grid biofilm filler, and biofilm culture gradually starts
It is continuous to match culture, obtain bacterial concentration 1 × 109The microbial culture medium of a/mL, the oxidation-reduction potential of culture solution are 703mV.
B. leaching stage:
Microbial culture medium is imported in the leaching tanks of 100L, is that 3L:1Kg addition copper content is according to volume mass ratio
1.2%, lead tolerance 1.0%, moisture content 11.62%, the spent resin powder powder of 200 mesh of partial size, which stirs evenly, to carry out leaching pre- open
Dynamic, mixing speed 150rpm, leaching pretrigger temperature is 45 DEG C, time 7h.It, will when leaching rate and cell concentration stable state
Temperature control in leaching tanks is continuously leached within the scope of 40~45 DEG C, speed of agitator 50rpm, when continuous leaching stops
Between 5h, obtain leaching slurry.
C. subsidence stage:
Leaching slurry enters in subsider, obtains cupric supernatant and leaded sedimentation slag by separation of solid and liquid.On cupric
The cupric filtrate that clear liquid obtains after filtering enters extraction equipment, and leaded sedimentation slag is then imported by slush pump and is separated by solid-liquid separation system
System.
D. copper recovery stage:
When the concentration of copper in cupric filtrate is 4g/L or more, the M5640 copper extractant solution for being 10% with volume fraction
The volume ratio of extraction, cupric filtrate and extractant is 1:2, is extracted using two-stage extraction, level-one washing, level-one stripping process
It takes, when the concentration of copper in strip liquor is 45g/L or more, recycles metal by the way of metal electro-deposition or condensing crystallizing
Otherwise copper is back to leaching tanks together with raffinate, after solution hydrogenation sodium oxide molybdena adjusting pH value extracted is 2.5-3.5, then
Liquid after isolated iron aluminum slag and neutralization precipitation, liquid returns to microbial cultivation device after neutralization precipitation.
E. salt soaks the stage:
Leaded sedimentation slag obtains clear liquid and leaded filter residue after solid-liquid separating machine, and clear liquid returns to microbial cultivation device,
Leaded filter residue is added in leaching tanks to react at room temperature with the sodium chloride solution of 100g/L, and the pH of solution is 7, after reacting 1h,
Leaded leachate is obtained by filtration and decopper(ing) takes off the leached mud after lead, Pb in leaded leachate2+Concentration can reach 1.8g/L.
F. lead phase is precipitated
Sodium sulfide solution reaction is added into leaded leachate, the amount of addition is 1.1 times of theoretical amount, after reacting 2h,
Liquid after the concentrate of lead sulfide ore and heavy lead of lead tolerance 70% is obtained by filtration, the liquid after lead that sinks returns to salt and soaks the stage.
G. washing stage:
By washing twice, substance each time after washing separates leached mud after the de- lead of decopper(ing) after being separated by solid-liquid separation
To filtrate and filter residue, filtrate returns to wash mill, and filter residue enters drying device.
H. drying stage:
Filter residue obtains the resin and mixture of glass fibers of low copper and lead content after drying.
In leaching pretrigger, microorganism to the leaching rate of copper in spent resin powder up to 95%, it is continuous leach in the case of it is micro-
The leaching rate of copper in Bioleaching spent resin powder is up to 92% or more, the glass and epoxy resin composite material of once purged acquisition
Middle copper content be reduced to 0.06% hereinafter, lead content be lower than 0.05%.
Embodiment 3
A. microorganism growing step:
Basal medium is configured, component content: ammonium sulfate 2g/L, epsom salt 0.3g/L, potassium hydrogen phosphate 0.6g/L,
Potassium chloride 0.1g/L, calcium nitrate 0.03g/L, ferrous sulfate heptahydrate 40g/L, sulphur powder 0.2g/L will with sulphur acid for adjusting pH to 2.0
Basal medium is added in culture tank, and presses inoculum concentration 10% for acidophilus iron Thiobacillus CS12 (Acidithiobacillus
Ferrivorans) and acidophilus iron thiobacillus thiooxidant CS 78 (Acidithiobacillus ferrooxidans) is inoculated into culture
It in slot, is cultivated at 30 DEG C of temperature, until the cell concentration in solution reaches 108The spent resin mould of silk screen encapsulation is added in a/mL
Block biofilm filler, biofilm culture, gradually starting obtains bacterial concentration 1.5 × 10 continuously with culture8The microculture of a/mL
Liquid, the oxidation-reduction potential of culture solution are 706mV.
B. leaching stage:
Microbial culture medium is imported in the leaching tanks of 100L, is that 2L:1kg addition copper content is according to volume mass ratio
1.4%, lead tolerance 0.6%, moisture content 12.78%, the spent resin powder powder of -180 mesh of partial size stir evenly leach it is pre-
Starting, mixing speed 140rpm, leaching pretrigger temperature is 30 DEG C, time 7h.By the temperature control in leaching tanks 20~
It is continuously leached within the scope of 30 DEG C, speed of agitator 100rpm, leaches residence time 3h, obtain leaching slurry.
C. subsidence stage:
Leaching slurry enters in subsider, obtains cupric supernatant and leaded sedimentation slag by separation of solid and liquid.On cupric
The cupric filtrate that clear liquid obtains after filtering enters extraction equipment, and sedimentation slag then passes through slush pump and imports solid-liquid separation system.
D. copper recovery stage:
When the concentration of copper in cupric filtrate is 4g/L or more, the CP150 copper extractant solution for being 10% with volume fraction
The volume ratio of extraction, cupric filtrate and extractant is 1:1, is extracted using two-stage extraction, level-one washing, level-one stripping process
It takes, when the concentration of copper in strip liquor is 45g/L or more, recycles metal by the way of metal electro-deposition or condensing crystallizing
Otherwise copper is back to leaching tanks together with raffinate, after solution hydrogenation sodium oxide molybdena adjusting pH value extracted is 2.5-3.5, then
Liquid after isolated iron aluminum slag and neutralization precipitation, liquid returns to microbial cultivation device after neutralization precipitation.
E. salt soaks the stage:
Leaded sedimentation slag obtains clear liquid and leaded filter residue after solid-liquid separating machine, and clear liquid returns to microbial cultivation device,
Leaded filter residue is added in leaching tanks to react at room temperature with the sodium chloride solution of 150g/L, and the pH of solution is 6, after reacting 1h,
Leaded leachate is obtained by filtration and decopper(ing) takes off the leached mud after lead, Pb in leaded leachate2+Concentration can reach 1.2g/L.
F. heavy lead phase
Sodium sulfide solution reaction is added into leaded leachate, the amount of addition is 1.3 times of theoretical amount, after reacting 1h,
Liquid after the concentrate of lead sulfide ore and heavy lead of lead tolerance 68% is obtained by filtration, the liquid after lead that sinks returns to salt and soaks the stage.
G. washing stage:
By washing twice, substance each time after washing separates leached mud after the de- lead of decopper(ing) after being separated by solid-liquid separation
To filtrate and filter residue, filtrate returns to wash mill, and filter residue enters drying device.
H. drying stage:
Filter residue obtains the resin and mixture of glass fibers of low copper and lead content after drying.
In leaching pretrigger, microorganism to the leaching rate of copper in spent resin powder up to 93%, it is continuous leach in the case of it is micro-
The leaching rate of copper in Bioleaching spent resin powder is up to 93% or more, in the glass and epoxy resin composite material obtained after cleaning
Copper content be reduced to 0.05% hereinafter, lead content be lower than 0.05%.
Comparative example 1
It is 1.4% that copper content, which is added, the spent resin powder powder of lead tolerance 0.6%, using containing acidithiobacillus ferrooxidans
PH value be 2.5 acidic aqueous solution, leach liquid-solid ratio be 5/1 under conditions of leach spent resin powder powder 36h, it is molten to obtain copper-rich
Liquid and fiberglass resin composite material.Using LIX860N:LIX84: kerosene volume ratio=5:5:90 extractant is comparably 1, carries out 4
Stage countercurrent cascade extraction, extraction times at different levels are 10min, and extraction copper-rich solution obtains supported copper organic phase and raffinate；In phase
Under conditions of being 1, mass fraction is used to carry out the back extraction of 2 stage countercurrent tandems for 20% sulfuric acid solution, when back extraction at different levels
Between be 15min, back extraction supported copper organic phase obtain anti-stripping agent, electrodeposition anti-stripping agent obtains tough cathode.
Leachate copper content 3.5g/L in Microorganism Leaching spent resin powder, once purged acquisition copper content are 0.06%, are contained
The glass and epoxy resin composite material of lead amount 1.55%.
Embodiment 1-3 and comparative example 1 compare, and the period of spent resin powder biological copper leaching of the present invention greatly shortens, and improve life
Efficiency is produced, the stable copper leaching rate with high, and the lead in glass and epoxy resin composite material is separated, both returned
Metallic lead is utilized in receipts, but also the innoxious degree of glass fibre and epoxy resin composite material after the de- lead of decopper(ing) is high, mentions
The high quality of further processing material.
Claims (8)
1. a kind of recovery system of spent resin powder, which is characterized in that including microbial cultivation device, leaching device, sedimentation device,
Copper recyclable device, salt bath unit, heavy lead device, wash mill, drying device and solid-liquid separating machine；
The microbial cultivation device includes culture tank (11), and aeration component (1), pH control are provided in the culture tank (11)
Component (2), temperature control component (3) and biofilm filler assembly (12), obtained microbial culture medium enter leaching device；
The leaching device includes leaching tanks (21), and aeration component (1), pH control assembly are provided in the leaching tanks (21)
(2), temperature control component (3) and agitating paddle (4), the substance after leaching enter sedimentation device；
The sedimentation device includes subsider (31), and the cupric supernatant after sedimentation enters copper recyclable device, leaded heavy after sedimentation
Drop slag enters solid-liquid separating machine (5)；
The copper recyclable device includes the filter device (41) for receiving the cupric supernatant after sedimentation, receives filtered cupric filter
The extraction equipment (42) of liquid, receives the neutralization precipitation device of extract liquor extracted, and the neutralization precipitation device includes neutralizing to sink
Shallow lake slot (43) and agitating paddle (4) in neutralization precipitation slot (43) is set, the substance after neutralization precipitation passes through solid-liquid separating machine (5)
Afterwards, liquid after isolated iron aluminum slag and neutralization precipitation, liquid returns to microbial cultivation device after neutralization precipitation；
Leaded sedimentation slag after sedimentation obtains clear liquid and leaded filter residue after solid-liquid separating machine (5), and clear liquid returns to microorganism training
Device is supported, leaded filter residue enters salt bath unit；
The salt bath unit includes the agitating paddle (4) of salt immersion trough (51) and setting in salt immersion trough (51), the substance warp after salt leaching
After crossing solid-liquid separating machine (5), obtains leaded leachate and decopper(ing) takes off the leached mud after lead, leaded leachate enters precipitating lead dress
It sets, the leached mud after the de- lead of decopper(ing) enters wash mill；
The heavy lead device includes the agitating paddle (4) of heavy lead bath (61) and setting in heavy lead bath (61), the substance warp after heavy lead
After crossing solid-liquid separating machine (5), liquid after isolated concentrate of lead sulfide ore and heavy lead, sink lead after liquid return salt bath unit；
The wash mill includes the agitating paddle (4) of sink (71) and setting in sink (71), the substance warp after washing
After crossing solid-liquid separating machine (5), isolated filtrate and filter residue, filtrate return to wash mill, and filter residue enters drying device；
The drying device includes drying machine (81), obtains resin and glass fibre after filter residue and drying.
2. the recovery system of spent resin powder as described in claim 1, which is characterized in that the solid-liquid separating machine (5) is sheet frame
One of filter press and centrifuge.
3. the recovery system of spent resin powder as described in claim 1, which is characterized in that the drying machine (81) is roller drying
One of machine, band drier and baking oven.
4. a kind of recovery method of spent resin powder, including microorganism growing step, leaching stage, subsidence stage, copper recovery stage,
Salt soaks stage, heavy lead phase, washing stage and drying stage, it is characterised in that:
A. the microorganism growing step, there is following steps: accessing active bacteria in basal medium, exposes at 30-45 DEG C
Air culture is supported, until the cell concentration in solution reaches 108-109Filler is added in a/mL, and biofilm culture gradually starts, continuous to train
It supports, obtains microbial culture medium；
Active bacteria described in process A is that acidophilus iron aoxidizes hook end spirillum CS13 (Leptospirillum
Ferriphilum), depositary institution: China typical culture collection center, deposit number: CCTCCM2015010, acidophilus vulcanize bar
Bacterium CS17 (Sulfobacillus thermosulfidooxidans), depositary institution: China typical culture collection center is protected
Hiding number: CCTCC M 2015011, Thiobacillus ferrooxidans CS 78 (Acidithiobacillus ferrooxidans), preservation
Unit: China typical culture collection center, deposit number: CCTCCM2015016, acidophilus iron Thiobacillus CS12
(Acidithiobacillus ferrivorans), depositary institution: China typical culture collection center, deposit number: CCTCC:
One of M 2015009 or a variety of；
B. the leaching stage, there is following steps: according to volume mass ratio be 1.5-3L by microbial culture medium and spent resin powder:
1kg is stirred and evenly mixed, mixing speed 50-200rpm, and extraction temperature is 20-45 DEG C, extraction time 2-5h, obtains leaching slurry
Liquid；
C. the subsidence stage, there is following steps: leaching slurry is entered in subsider and is settled, and obtains cupric supernatant and leaded
Settle slag；
D. the copper recovery stage, there is following steps: cupric filtrate is obtained after cupric supernatant liquid filtering, when copper in cupric filtrate
It when concentration is 4g/L or more, is extracted with copper extractant solution, the volume ratio of extraction agent solution and cupric filtrate is 1-2:1, extraction
Extract liquor afterwards adds alkali to adjust pH to carry out neutralization precipitation, then liquid after isolated iron aluminum slag and neutralization precipitation, after neutralization precipitation
Liquid returns to microbial cultivation device；
E. the salt soaks the stage, and have following steps: leaded sedimentation slag obtains clear liquid and leaded filter residue after solid-liquid separating machine,
Clear liquid returns to microbial cultivation device, the sodium chloride solution that concentration is 100-250g/L is added into leaded filter residue, at room temperature
Lead is leached, the pH of solution is 5.5-7.0, and leaded leachate is obtained by filtration after the completion of leaching and decopper(ing) takes off the leached mud after lead；
F. the heavy lead phase, there is following steps: sodium sulfide solution reaction being added into leaded leachate, filters after having reacted
Liquid after to concentrate of lead sulfide ore and heavy lead, sink lead after liquid return salt soak the stage；
G. washing stage:
Leached mud after the de- lead of decopper(ing) by washing twice, and substance each time after washing is after being separated by solid-liquid separation, isolated filter
Liquid and filter residue, filtrate return to wash mill, and filter residue enters drying device；
H. drying stage:
Filter residue obtains innoxious resin and glass fibre after drying.
5. the recovery method of spent resin powder as claimed in claim 4, which is characterized in that basal medium described in process A
Composition and respective content are as follows: ammonium sulfate 1.5-3g/L, epsom salt 0.25-0.5g/L, potassium hydrogen phosphate 0.5-0.8g/L, chlorination
Potassium 0.1-0.12g/L, calcium nitrate 0.01-0.05g/L, ferrous sulfate heptahydrate 30-50g/L, sulphur powder 0-10g/L are adjusted with sulfuric acid
PH is 1.5-2.
6. the recovery method of spent resin powder as described in claim 4 or 5, which is characterized in that biofilm filler described in process A is
Grid or the spent resin module of silk screen encapsulation.
7. the recovery method of spent resin powder as claimed in claim 4, which is characterized in that extractant described in step D is extraction
One of agent N902, M5640, CP150, LIX984.
8. the recovery method of spent resin powder as described in claim 4 or 5, which is characterized in that extraction described in step D uses two
Grade extraction, level-one washing, level-one stripping process are extracted, when the concentration of copper in strip liquor is 45g/L or more, using metal
The mode of electrodeposition or condensing crystallizing recycles metallic copper, after solution hydrogenation sodium oxide molybdena adjusting pH value extracted is 2.5-3.5, mistake
Microculture is returned after filtering out slag.
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