CN105925799A - Wet metallurgy film concentration process - Google Patents
Wet metallurgy film concentration process Download PDFInfo
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- CN105925799A CN105925799A CN201610364021.0A CN201610364021A CN105925799A CN 105925799 A CN105925799 A CN 105925799A CN 201610364021 A CN201610364021 A CN 201610364021A CN 105925799 A CN105925799 A CN 105925799A
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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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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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
Abstract
The invention relates to a wet metallurgy film concentration process for concentrating metal solution extracted from wet metallurgy. The wet metallurgy film concentration process comprises the following steps: (S1) pretreatment: the metal solution is pretreated to obtain metal treatment liquid; the soluble impurity concentration in the metal treatment liquid is not higher than a first preset value; and the solid content in the metal treatment liquid is not higher than a second preset value; and (S2) concentration: second metal filtrate is concentrated by using a self-cleaning filter film to obtain metal concentration liquid. The wet metallurgy film concentration process adopts the self-cleaning filter film to perform high-power concentration for the metal treatment liquid, and is low in cost and high in concentration efficiency in the whole concentration treatment process. The concentration of the metal solution is increased to a saturated state through film concentration to realize the liquid concentration; and meanwhile, penetration liquid generated by film concentration is returned to a water reuse system for recycling, so that such advantages as environmental protection and water saving are achieved, and the cost is prominently reduced.
Description
Technical field
The present invention relates to a kind of hydrometallurgy membrance concentration technique, use membrane technology in wet method particularly to one
The technique in metallurgy, metallic solution being carried out high power concentration.
Background technology
Concentration is one of important process in hydrometallurgy, concentration conventional in existing hydrometallurgy industry
Technique mainly uses evaporation and concentration, but the following deficiency that evaporating concentrating method exists:
1. evaporation and concentration needs to heat, and expends mass energy, produces consuming cost high.
2. evaporation and concentration needs production site big, produces hardware input cost high.
3. the later stage of evaporation and concentration needs to cool down metallic solution, causes the production time long, produces
Efficiency is low.
And in recent years, membrane permeation technology is evolving, it is in fields such as food, pharmacy, the energy,
Especially there is a lot of successfully trial in water pure desalination field, but yet there are no membrane permeation technology in hydrometallurgy
The concentration technology in field is applied.
Summary of the invention
The technical problem to be solved is for the deficiencies in the prior art, it is provided that a kind of hydrometallurgy
Membrance concentration technique.
The technical scheme is that a kind of hydrometallurgy membrance concentration technique,
For concentrating hydrometallurgy is extracted the metallic solution obtained, comprise the following steps:
S1, pretreatment: described metallic solution is carried out pretreatment, obtain metal treatment fluid, described metal
Soluble impurity concentration in treatment fluid is not more than the first preset value, the solid content in described metal treatment fluid
It is not more than the second preset value;
S2, concentrates: use self-cleaning filtering film to concentrate secondary metals filtrate, obtains metal and concentrates
Liquid.
The invention has the beneficial effects as follows: metal treatment fluid is carried out by the present invention by using self-cleaning filtering film
High power concentrates, and whole concentration process cost is low, and thickening efficiency is high.By membrance concentration by metallic solution
Concentration improve to saturation, it is achieved feed liquid concentrate;The permeate that membrance concentration produces simultaneously returns water and returns
By system, can recycle, there is the advantage such as environmental protection, using water wisely, significantly reduce cost.With
Evaporation and concentration of the prior art is compared, and the present invention uses that to carry out film through the metal treatment fluid of pretreatment dense
Contracting, has the advantages such as energy resource consumption is little, low cost, intractability are little, saving time, efficiency high pollution.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in step S1, described preprocessing process includes:
Remove impurity: use ion exchange resin that described metallic solution is carried out ion exchange, obtain metal
Filtrate, makes the soluble impurity solubility in metal filtrate be not more than the first preset value;
Secondary remove impurity: use micro-filtration membrane that metal filtrate is filtered, obtain metal treatment fluid, make metal
Solid content in treatment fluid is not more than the second preset value.
Above-mentioned further scheme is used to provide the benefit that: by using ion exchange resin to remove metal
Soluble impurity in solution, can make the soluble impurity in metallic solution effectively be reduced to the first preset value
Hereinafter, even soluble impurity is all got rid of;By using micro-filtration membrane to fixing in metallic solution
Thing content carries out filtering to be removed, and the fixture content in metallic solution can be made effectively to be reduced to the second preset value
Hereinafter, even solid content all can be filtered out;By micro-filtration membrane, the float in metallic solution is intercepted,
Realize solid-liquid separation;Float is easily produced during the acidleach of hydrometallurgy, if do not got rid of,
Product quality and subsequent treatment process difficulty and cost can be affected;And owing to the materialization of float is special
Property, (for the filter press) problem easily produce filtering material blocking, frequently changing;
Utilize micro-filtration membrane the float in solution to be intercepted, it is achieved solid-liquid separation, there is precision height, intercepting efficiency
High advantage.By ion exchange resin is industrial to hydrometallurgy, effectively with micro-filtration membrane connected applications
Ensure that the product purity of hydrometallurgy, have that energy resource consumption is little, low cost, intractability are little, save
The advantage such as time, efficiency are high, pollution-free.
Further, described first preset value is 0.001-0.02%.
Further, described second preset value is 0.005-0.02g/L.
Further, described metal concentrated solution is the saturated solution of target metal ions.
Further, in a described remove impurity, every 100mL metallic solution adds the exchange of 5g-15g ion
Resin.
Above-mentioned further scheme is used to provide the benefit that: by adding in every 100mL metallic solution
5g-15g ion exchange resin, can make the soluble impurity active adsorption in metallic solution remove, such as
Ca2+、Mg2+And SiO3 2-Plasma.
Further, in described step S1, in secondary remove impurity, the aperture of micro-filtration membrane is 0.1-20 μm, mistake
The temperature of filter is 0-100 DEG C, and the pressure of filtration is 0.02-0.2MPa.
Further, in step S2, the pressure of described concentration is 5-20Mpa, and the temperature of described concentration is
0-40 DEG C, the molecular weight retained is more than 100.
Further, in step S2, the aperture of described self-cleaning filtering film is straight less than target metal ions
Footpath.
Further, in step S2, described metal treatment fluid uses cross-current flow by described self-cleaning
Filter membrane.
Above-mentioned further scheme is used to provide the benefit that: by making metal treatment fluid use cross-current flow to lead to
Cross self-cleaning filtering film, make the effect of filtration reach optimal.
Detailed description of the invention
Principle and feature to the present invention are described below, and example is served only for explaining the present invention, and
Non-for limiting the scope of the present invention.
Embodiment 1
A kind of hydrometallurgy membrance concentration technique, for carrying out extracting the metallic solution obtained in hydrometallurgy
Concentrate, comprise the following steps:
S1, pretreatment: described metallic solution is carried out pretreatment, obtain metal treatment fluid, described metal
Soluble impurity concentration in treatment fluid is not more than the first preset value, the solid content in described metal treatment fluid
Content is not more than the second preset value;
S2, concentrates: uses self-cleaning filtering film to concentrate metal treatment fluid, obtains saturated concentration
Metal concentrated solution.The aperture of described self-cleaning filtering film is less than the diameter of target metal ions.Described metal
Treatment fluid uses cross-current flow by described self-cleaning filtering film.
In step S1, described preprocessing process includes:
Remove impurity: use ion exchange resin that described metallic solution carries out ion exchange, every 100mL
Metallic solution adds 5g ion exchange resin, obtains metal filtrate, make the solubility in metal filtrate
Impurity solubility is not more than the first preset value;
Secondary remove impurity: use micro-filtration membrane that metal filtrate is filtered, obtain metal treatment fluid, make metal
Solid content in treatment fluid is not more than the second preset value.The aperture of micro-filtration membrane is 0.1 μm, filtration
Temperature is 0 DEG C, and the pressure of filtration is 0.02MPa.
In described step S2, the pressure of described concentration is 5Mpa, and the temperature of described concentration is 0 DEG C, cuts
The molecular weight stayed is 100.
The present embodiment is for different raw mineral materials, and parameter and the step of employing are the most variant, parameters
Reasonably can set according to different metal ion.The application is as a example by spodumene, to hydrometallurgy
Detailed process illustrates.The hydrometallurgy of the present embodiment uses sulfuric acid process to carry out the lithium salts in spodumene
Leaching and concentrate, spodumene is commercially available spodumene concentrate (Li2O·Al2O3·4SiO2), mainly contain oxygen
Change lithium (Li2O), silicon oxide (Al2O3) and silicon dioxide (SiO2).Specifically include following steps:
1) acidleach: pretreated spodumene breeze is immersed in sulfuric acid solution, obtains lithium sulfate leachate.
Pretreatment method particularly includes: take spodumene concentrate, to spodumene concentrate roasting at 1100 DEG C
0.5 hour, then cool to 80 DEG C, obtain spodumene calcining;Spodumene calcining is carried out ore grinding,
Particle diameter is less than the spodumene breeze of 80 mesh.
The reaction condition of acidleach is: the sulphuric acid of addition concentration 93%-98% in spodumene breeze, and
Roasting under conditions of 250 DEG C, obtains acid grog, and the residual acid weight/mass percentage composition controlling acid grog is 3%;
Adding calcium carbonate in acid grog, the addition mole of calcium carbonate is 1.1 times of residual acid mole, obtains mixed
Compound, adds water in mixture, when the pH value of mixture is 5.5, filters, admittedly contained
The lithium sulfate leachate of amount more than 10%.
2) lithium sulfate leachate employing ion exchange resin is carried out a remove impurity to process, every 100mL sulphuric acid
Lithium leachate adds 5g ion exchange resin, obtains the leachate containing lithium processed through a remove impurity.
3) membrane filtration: by step 2) through a remove impurity process the leachate containing lithium utilize micro-filtration membrane to carry out
Membrane filtration, the aperture of membrane filtration is 1 μm, and the temperature of membrane filtration is 0 DEG C, and the pressure of membrane filtration is
0.02Mpa, obtains filtrate and solid impurity.
4) membrance concentration: by step 3) filtrate that obtains utilizes self-cleaning NF membrane to carry out membrance concentration, obtains
Cross liquid and concentrated solution (lithium sulfate solution is enriched to the concentrated solution that lithium content is 50g/L), use nanofiltration
When film carries out membrance concentration, temperature is 0 DEG C, and pressure is 10Mpa, and the molecular weight retaining material is 100, will
Permeate returns Water circulation system.The flux of membrance concentration is 10-20L/h m2。
5) sinker: to step 4) concentrated solution that obtains adds soda saturated solution, make lithium carbonate precipitate,
Filter and separate lithium carbonate precipitation.
6) lithium carbonate precipitation being utilized hot wash lithium carbonate, the temperature of hot water is 40 DEG C, separates, and is dried,
Preparing finished product lithium carbonate, the purity of finished product lithium carbonate is 98%-99.2%.
Embodiment 2
A kind of hydrometallurgy membrance concentration technique, for carrying out extracting the metallic solution obtained in hydrometallurgy
Concentrate, comprise the following steps:
S1, pretreatment: described metallic solution is carried out pretreatment, obtain metal treatment fluid, described metal
Soluble impurity concentration in treatment fluid is not more than the first preset value, the solid content in described metal treatment fluid
Content is not more than the second preset value;
S2, concentrates: uses self-cleaning filtering film to concentrate metal treatment fluid, obtains saturated concentration
Metal concentrated solution.The aperture of described self-cleaning filtering film is less than the diameter of target metal ions.Described metal
Treatment fluid uses cross-current flow by described self-cleaning filtering film.
In step S1, described preprocessing process includes:
Remove impurity: use ion exchange resin that described metallic solution carries out ion exchange, every 100mL
Metallic solution adds 10g ion exchange resin, obtains metal filtrate, make the solubility in metal filtrate
Impurity solubility is not more than the first preset value;
Secondary remove impurity: use micro-filtration membrane that metal filtrate is filtered, obtain metal treatment fluid, make metal
Solid content in treatment fluid is not more than the second preset value.The aperture of micro-filtration membrane is 5 μm, secondary filter
Temperature be 40 DEG C, the pressure of secondary filter is 0.1MPa.
In described step S2, the pressure of described concentration is 15Mpa, and the temperature of described concentration is 20 DEG C,
The molecular weight retained is 200.
The present embodiment is for different raw mineral materials, and parameter and the step of employing are the most variant, parameters
Reasonably can set according to different metal ion.The application is as a example by spodumene, to hydrometallurgy
Detailed process illustrates.The hydrometallurgy of the present embodiment uses sulfuric acid process to carry out the lithium salts in spodumene
Leach and concentrate, specifically include following steps:
1) acidleach: pretreated spodumene breeze is immersed in sulfuric acid solution, obtains lithium sulfate leachate.
Pretreatment method particularly includes: take spodumene concentrate, to spodumene concentrate roasting 2 at 1200 DEG C
Hour, then cool to 145 DEG C, obtain spodumene calcining;Spodumene calcining is carried out ore grinding, obtains grain
Footpath is less than the spodumene breeze of 80 mesh.
The reaction condition of acidleach is: add the sulphuric acid of concentration 98% in spodumene breeze, and at 300 DEG C
Under conditions of roasting, obtain acid grog, control acid grog residual acid weight/mass percentage composition be 6%;Ripe to acid
Adding calcium carbonate in material, the addition mole of calcium carbonate is 1.1 times of residual acid mole, obtains mixture,
Add water in mixture, when the pH value of mixture is 6.0, filter, obtain solid content 10%
Above lithium sulfate leachate.
2) lithium sulfate leachate employing ion exchange resin is carried out a remove impurity to process, every 100mL sulphuric acid
Lithium leachate adds 10g ion exchange resin, obtains the leachate containing lithium processed through a remove impurity.
3) membrane filtration: by step 2) through a remove impurity process the leachate containing lithium utilize micro-filtration membrane to carry out
Membrane filtration, the aperture of membrane filtration is 5 μm, and the temperature of membrane filtration is 100 DEG C, and the pressure of membrane filtration is
0.2Mpa, obtains filtrate and solid impurity.
4) membrance concentration: by step 3) filtrate that obtains utilizes self-cleaning reverse osmosis membrane to carry out membrance concentration, obtains
Permeate and concentrated solution (lithium sulfate solution is enriched to the concentrated solution that lithium content is 40g/L), use is received
When filter membrane carries out membrance concentration, temperature is 40 DEG C, and pressure is 20Mpa, and the molecular weight retaining material is 300,
Will transmit through liquid and return Water circulation system.The flux of membrance concentration is 10-20L/h m2。
5) sinker: to step 4) concentrated solution that obtains adds soda saturated solution, make lithium carbonate precipitate,
Filter and separate lithium carbonate precipitation.
6) lithium carbonate precipitation being utilized hot wash lithium carbonate, the temperature of hot water is 90 DEG C, separates, dry
Dry, prepare finished product lithium carbonate.The purity of finished product lithium carbonate is 98%-99.2%.
Embodiment 3
A kind of hydrometallurgy membrance concentration technique, for carrying out extracting the metallic solution obtained in hydrometallurgy
Concentrate, comprise the following steps:
S1, pretreatment: described metallic solution is carried out pretreatment, obtain metal treatment fluid, described metal
Soluble impurity concentration in treatment fluid is not more than the first preset value, the solid content in described metal treatment fluid
Content is not more than the second preset value;
S2, concentrates: uses self-cleaning filtering film to concentrate metal treatment fluid, obtains saturated concentration
Metal concentrated solution.The aperture of described self-cleaning filtering film is less than the diameter of target metal ions.Described metal
Treatment fluid uses cross-current flow by described self-cleaning filtering film.
In step S1, described preprocessing process includes:
Remove impurity: use ion exchange resin that described metallic solution carries out ion exchange, every 100mL
Metallic solution adds 15g ion exchange resin, obtains metal filtrate, make the solubility in metal filtrate
Impurity solubility is not more than the first preset value;
Secondary remove impurity: use micro-filtration membrane that metal filtrate is carried out secondary filter, obtain metal treatment fluid, make
Solid content in metal treatment fluid is not more than the second preset value.The aperture of micro-filtration membrane is 20 μm, two
The temperature of secondary filtration is 100 DEG C, and the pressure of secondary filter is 0.2MPa.
In described step S2, the pressure of described concentration is 20Mpa, and the temperature of described concentration is 40 DEG C,
The molecular weight retained is 300.
The present embodiment is for different raw mineral materials, and parameter and the step of employing are the most variant, parameters
Reasonably can set according to different metal ion.The application is as a example by spodumene, to hydrometallurgy
Detailed process illustrates.The hydrometallurgy of the present embodiment uses sulfuric acid process to carry out the lithium salts in spodumene
Leach and concentrate, specifically include following steps:
1) acidleach: pretreated spodumene breeze is immersed in sulfuric acid solution, obtains lithium sulfate leachate.
Pretreatment method particularly includes: take spodumene concentrate, to spodumene concentrate roasting 1 at 1150 DEG C
Hour, then cool to 120 DEG C, obtain spodumene calcining;Spodumene calcining is carried out ore grinding, obtains grain
Footpath is less than the spodumene breeze of 80 mesh.
The reaction condition of acidleach is: add the sulphuric acid of concentration 95% in spodumene breeze, and at 280 DEG C
Under conditions of roasting, obtain acid grog, control acid grog residual acid weight/mass percentage composition be 5%;Ripe to acid
Adding calcium carbonate in material, the addition mole of calcium carbonate is 1.1 times of residual acid mole, obtains mixture,
Add water in mixture, when the pH value of mixture is 5.8, filter, obtain solid content 10%
Above lithium sulfate leachate.
2) lithium sulfate leachate employing ion exchange resin is carried out a remove impurity to process, every 100mL sulphuric acid
Lithium leachate adds 15g ion exchange resin, obtains the leachate containing lithium processed through a remove impurity.
3) membrane filtration: by step 2) through a remove impurity process the leachate containing lithium utilize micro-filtration membrane to carry out
Membrane filtration, the aperture of membrane filtration is 2 μm, and the temperature of membrane filtration is 50 DEG C, and the pressure of membrane filtration is
0.1Mpa, obtains filtrate and solid impurity.
4) membrance concentration: by step 3) filtrate that obtains utilizes self-cleaning NF membrane to carry out membrance concentration, obtains
Cross liquid and concentrated solution (lithium sulfate solution is enriched to the concentrated solution that lithium content is 45g/L), use nanofiltration
When film carries out membrance concentration, temperature is 20 DEG C, and pressure is 15Mpa, and the molecular weight retaining material is 200,
Will transmit through liquid and return Water circulation system.The flux of membrance concentration is 10-20L/h m2。
5) sinker: to step 4) concentrated solution that obtains adds soda saturated solution, make lithium carbonate precipitate,
Filter and separate lithium carbonate precipitation.
6) lithium carbonate precipitation being utilized hot wash lithium carbonate, the temperature of hot water is 60 DEG C, separates, and is dried,
Prepare finished product lithium carbonate.The purity of finished product lithium carbonate is 98%-99.2%.
The yield of finished product lithium carbonate refers to that the quality of the finished product lithium carbonate actually obtained obtains with by Theoretical Calculation
The mass percent of lithium carbonate.
The embodiment of the present invention does not has special strict for the membrane material during membrane filtration and membrance concentration
Limit.All can obtain or prepared by conventional method from commercially available.
Micro-filtration membrane is divided into inoranic membrane and organic high molecular layer according to filmogen, and inoranic membrane is divided into again pottery
Film, metal film and intermetallic compound porous material, organic high molecular layer be divided into again natural macromolecule membrane and
Synthetic polymeric membrane;Form according to film is divided into again Flat Membrane, tubular membrane, rolled film and hollow-fibre membrane;
According to masking principle, the preparation method of polymeric membrane be divided into leaching (dry-wet method), stretching hole forming method,
Phase inversion, thermic phase method, dip coating, irradiation method, surface chemical modification method, nuclear track method, power
Formation methods etc., the preparation method of inoranic membrane mainly has sol-gel process, sintering process, chemical precipitation method etc..
Apply and wider should belong to organic polymer hollow-fibre membrane, main micro-filtration membrane kind have poly-partially
Fluorothene (PVDF), polysulfones (PSF), polyacrylonitrile (PAN), polrvinyl chloride (PVC), polypropylene (PP)
Deng.
The material of NF membrane is macromolecular material, mainly polyamide (PA), polyvinyl alcohol (PvA), sulphur
Change polysulfones (sPS), sulfonated polyether sulfone (sPEs), cellulose acetate (cA) and derivant thereof etc..
Common reverse osmosis membrane materials has two big class, i.e. cellulose acetate membrane component and composite membrane elements.
(1) cellulose acetate membrane component
General cellulose generates triacetate fiber through esterification, then is hydrolyzed into mixing one, two, three through secondary
Acetate fiber.The salt rejection rate affecting film is acetyl content height then salt rejection rate with the most important factor of aquifer yield
Height, but aquifer yield is few.
Cellulose acetate membrane weakness substantially is, passage in time, and ester functional groups will hydrolyze, with
Time salt rejection rate be gradually reduced and flow increase, along with the reinforcement of hydrolysis, film is more vulnerable to microorganism and invades
Attacking, film itself also will lose its function and integrity simultaneously.
(2) composite membrane element
The main support structure of composite membrane is the polyester non-woven after being calendered machine calendering, and its surface is without pine
Staple in bulk and hard smooth, due to polyester non-woven the most irregularly and the most loose, uncomfortable cooperation
For the bottom of salt barrier layer, thus micropore engineering plastics polysulfones is cast on non-woven fabric surface, polysulfones
The hole on layer surface controls at about 15nm, and barrier layer uses the aromatic polyamides of high-crosslinking-degree, and thickness is about
At 0.2um.High-crosslinking-degree aromatic polyamides is polymerized by benzene three acyl chlorides and phenylenediamine.
Different membrane filtration apertures, the interception rate of solid particle is the most different, but the aperture of the most not membrane filtration
The smaller the better, aborning, in addition it is also necessary to consider production efficiency.For the aperture of different membrane filtrations, right
The interception rate of solid particle and production efficiency are tested, and concrete operations are: on the basis of embodiment 1
Adjusting the aperture of membrane filtration, other parameter and step are constant.Result of the test such as table 1.
Experimental result according to table 1, it can be seen that aperture is the least, the granule interception rate of solid is the highest,
When aperture is between 0.1-5 micron, solid particle interception rate all can reach more than 90%, especially hole
Footpath is between 0.1-1 micron, and solid particle interception rate all can reach 99.9%.But, inventor exists
Finding in research, aperture is between 0.1-1 micron, and flux is the lowest, and filtration time is longer and easily blocks
Misgivings hole, makes the yield decline of the finished product lithium carbonate prepared, cost raise.Therefore, after considering,
By the aperture of membrane filtration between 1-5 micron, the flux of membrane filtration now is 0.6-0.8m3/h·㎡
Can ensure that solid particle interception rate is effective, flux is good, the yield of finished product lithium carbonate high, finished product simultaneously
The purity of lithium carbonate is high.
The solid particle interception rate in the different membrane filtration aperture of table 1
For different metallic solutions, the ion exchange resin of employing is the most different, and the application mainly will be from
Sub-exchange resin is applied in hydrometallurgy, the metal lixiviating solution (the most above-mentioned metallic solution) of hydrometallurgy
Typically containing more cation impurity, such as calcium ion, magnesium ion etc., therefore, the application uses sun
Ion exchange resin, owing to resin has Selective adsorption, therefore, metal lixiviating solution in this application
In, high valence ion is generally preferentially adsorbed, and the absorption of ion is more weak, at the similar ion of same valency at a low price
In, being adsorbed of the ion being relatively large in diameter is relatively strong, and lithium ion is generally finally selected, therefore, and the application
Cation exchange resin is used to be removed by the cation-adsorption in lithium ion lixiviating solution.And at every 100mL
Lithium ion extracting solution adds 5g-15g ion exchange resin, it is ensured that effectively remove soluble metal
While impurity, moreover it is possible to ensure to be removed by lithium ion.
The present invention carries out high power concentration to metal treatment fluid, at whole concentration by using self-cleaning filtering film
Reason process cost is low, and thickening efficiency is high.By membrance concentration, the concentration of metallic solution is improved to saturation,
Realize feed liquid to concentrate;The permeate that membrance concentration produces simultaneously returns Water circulation system, can recycle,
There is the advantage such as environmental protection, using water wisely, significantly reduce cost.With evaporation and concentration phase of the prior art
Ratio, the present invention uses and carries out membrance concentration through the metal treatment fluid of pretreatment, has that energy resource consumption is little, becomes
This is low, intractability is little, save the advantage such as time, efficiency high pollution.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all in the present invention
Spirit and principle within, any modification, equivalent substitution and improvement etc. made, should be included in this
Within bright protection domain.
Claims (10)
1. a hydrometallurgy membrance concentration technique, it is characterised in that for extracting in hydrometallurgy
To metallic solution concentrate, comprise the following steps:
S1, pretreatment: described metallic solution is carried out pretreatment, obtain metal treatment fluid, described metal
Soluble impurity concentration in treatment fluid is not more than the first preset value, the solid content in described metal treatment fluid
Content is not more than the second preset value;
S2, concentrates: uses self-cleaning filtering film to concentrate metal treatment fluid, obtains metal concentrated solution.
A kind of hydrometallurgy membrance concentration technique, it is characterised in that step
In S1, described preprocessing process includes:
Remove impurity: use ion exchange resin that described metallic solution is carried out ion exchange, obtain metal
Filtrate, makes the soluble impurity solubility in metal filtrate be not more than the first preset value;
Secondary remove impurity: use micro-filtration membrane that metal filtrate is filtered, obtain metal treatment fluid, make metal
Solid content in treatment fluid is not more than the second preset value.
A kind of hydrometallurgy membrance concentration technique the most according to claim 1 or claim 2, it is characterised in that
Described first preset value is 0.001-0.02%.
A kind of hydrometallurgy membrance concentration technique the most according to claim 1 or claim 2, it is characterised in that
Described second preset value is 0.005-0.02g/L.
A kind of hydrometallurgy membrance concentration technique the most according to claim 1 or claim 2, it is characterised in that
Described metal concentrated solution is the saturated solution of target metal ions.
A kind of hydrometallurgy membrance concentration technique, it is characterised in that described
In remove impurity, every 100mL metallic solution adds 5-15g ion exchange resin.
A kind of hydrometallurgy membrance concentration technique, it is characterised in that described
In step S1, in secondary remove impurity, the aperture of micro-filtration membrane is 0.1-20 μm, and the temperature of filtration is 0-100 DEG C,
The pressure filtered is 0.02-0.2MPa.
A kind of hydrometallurgy membrance concentration technique the most according to claim 1 or claim 2, it is characterised in that
In step S2, the pressure of described concentration is 5-20Mpa, and the temperature of described concentration is 0-40 DEG C, retains
Molecular weight be more than 100.
A kind of hydrometallurgy membrance concentration technique, it is characterised in that step
In S2, the aperture of described self-cleaning filtering film is less than the diameter of target metal ions.
A kind of hydrometallurgy membrance concentration technique, it is characterised in that step
In S2, described metal treatment fluid uses cross-current flow by described self-cleaning filtering film.
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108069445A (en) * | 2018-01-24 | 2018-05-25 | 四川思达能环保科技有限公司 | A kind of sodium carbonate purification and impurity removal system and its method therefor |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102070162A (en) * | 2011-01-30 | 2011-05-25 | 西安蓝晓科技有限公司 | Novel method for extracting lithium from salt lake brine |
WO2012077610A1 (en) * | 2010-12-06 | 2012-06-14 | 東レ株式会社 | Alkali metal separation and recovery method and alkali metal separation and recovery apparatus |
CN103274550A (en) * | 2013-06-17 | 2013-09-04 | 广西大学 | Brine impurity removal method in sodium chlorate production technology |
CN103738984A (en) * | 2013-12-26 | 2014-04-23 | 江苏久吾高科技股份有限公司 | Method and device for extracting bitten lithium chloride |
CN104310446A (en) * | 2014-10-17 | 2015-01-28 | 江苏久吾高科技股份有限公司 | Process and device for extracting battery grade lithium from brine |
CN104338441A (en) * | 2014-10-17 | 2015-02-11 | 南京格洛特环境工程股份有限公司 | Treatment process of lithium precipitation mother solution |
-
2016
- 2016-05-26 CN CN201610364021.0A patent/CN105925799A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012077610A1 (en) * | 2010-12-06 | 2012-06-14 | 東レ株式会社 | Alkali metal separation and recovery method and alkali metal separation and recovery apparatus |
CN102070162A (en) * | 2011-01-30 | 2011-05-25 | 西安蓝晓科技有限公司 | Novel method for extracting lithium from salt lake brine |
CN103274550A (en) * | 2013-06-17 | 2013-09-04 | 广西大学 | Brine impurity removal method in sodium chlorate production technology |
CN103738984A (en) * | 2013-12-26 | 2014-04-23 | 江苏久吾高科技股份有限公司 | Method and device for extracting bitten lithium chloride |
CN104310446A (en) * | 2014-10-17 | 2015-01-28 | 江苏久吾高科技股份有限公司 | Process and device for extracting battery grade lithium from brine |
CN104338441A (en) * | 2014-10-17 | 2015-02-11 | 南京格洛特环境工程股份有限公司 | Treatment process of lithium precipitation mother solution |
Non-Patent Citations (1)
Title |
---|
聂梅生总主编、张杰等主编: "《水工业工程设计手册 水工业工程设备》", 31 March 2000, 北京:中国建筑工业出版社 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108069445A (en) * | 2018-01-24 | 2018-05-25 | 四川思达能环保科技有限公司 | A kind of sodium carbonate purification and impurity removal system and its method therefor |
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