CN105800819A - Method for high-efficiency separation of valuable metal ions in complex solution containing heavy metals - Google Patents
Method for high-efficiency separation of valuable metal ions in complex solution containing heavy metals Download PDFInfo
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Abstract
The invention relates to a novel method for high-efficiency separation of valuable metal ions in a complex solution containing heavy metals. According to the method, a solution rich in heavy metal ions like copper, nickel, cobalt, zinc and cadmium ions and impurity metal ions like calcium and magnesium ions is subjected to cooperative extraction by a compound extraction agent composed of Versatic 10 and Mextral984H; an organic phase obtained after extraction is subjected to reverse extraction under different acidity conditions so as to separately obtain easily-separable reverse extract rich in zinc/cadmium, easily-separable reverse extract rich in nickel/cobalt and easily-separable reverse extract rich in copper, and raffinate only containing calcium/magnesium can be directly returned to the procedure of production of the solution containing heavy metals. The whole method realizes high-efficiency recovery of valuable metal ions in the solution and reuse of all the waste water, creates considerable economic income for enterprises and achieves the purpose of zero discharge.
Description
Technical field
The present invention relates to a kind of containing the recovery method of valuable metal in various heavy waste water, be specifically related to a kind of high efficiency separation complicated containing the new technology of valuable metal ions copper, nickel cobalt, zinc/cadmium, calcium/magnesium in heavy metal solution.
Background technology
Nonferrous production process, smelting dirt Slag treatment or recycling process etc. all can produce a large amount of waste water containing heavy metal or solution.Adopt traditional Calx neutralisation or the not only possible valuable metal of large losses in waste residue of chemical precipitation method, and be difficult to the fully recovering of waste water.Such as a factory producing 100000 t electrolytic zincs per year, its electrolysis wastewater generation amount about 3～50,000 t/a, the general restriction by hydrometallurgy system zinc ion concentration, impurity concentration requirement and volume, only the electrolysis wastewater of 30%～50% can directly reclaim the utilization of entrance system, all the other electrolysis wastewaters of 50%～70% are generally adopted Calx neutralisation and process, in waste residue only the loss of zinc up to about 200t.Accordingly, it would be desirable to the more cost-effective technique of one, while the valuable metal in high efficiente callback solution, it is achieved waste water recycling, reach the purpose of zero-emission.
Summary of the invention
It is an object of the invention to provide a kind of high efficiency separation complicated containing the method for valuable metal ions in heavy metal solution, for respectively obtain be easily isolated the solution rich in zinc/cadmium, the solution rich in nickel cobalt, solution rich in the solution of copper and only calcic/magnesium.And only the solution of calcic/magnesium can directly return and produces workshop section containing heavy metal solution, it is achieved the high efficiente callback of valuable metal ions and wastewater zero discharge in solution.
For reaching the purpose of foregoing invention, the present invention by the following technical solutions:
A kind of high efficiency separation is complicated containing the method for valuable metal ions in heavy metal solution, comprises the following steps:
(1) first regulate pH=4.5～5.5 with alkali liquor containing heavy metal solution, remove bulky grain thing and insoluble matter then through the pretreatment process filtering, precipitating；
(2) pretreated continuous 1～4 grade of continuous extraction is carried out containing the synergic reagent after heavy metal solution saponification, make extraction equilibrium pH value=5.6～5.8, obtaining the raffinate of the extracted organic phase rich in heavy metal ion and only calcic/magnesium, raffinate returns production system；This synergic reagent is formed by Versatic10 and Mextral984H is composite, and its volume ratio is 2: 1～2: 4；Saponification rate is 30～60%；
(3) step (2) obtains extracted organic phase adopts and carries out continuous 1～2 grade of continuous washing containing zinc 40～100g/L, solution containing cadmium 4～10g/L, washes away the calcium/magnesium carried secretly, washes and be back to pretreatment process residual night；
(4) sulfuric acid solution that scrubbed extracted organic phase adopts concentration to be 4～6g/L carries out 1～4 grade of continuous back extraction, obtains liquid and back extraction organic facies 1 after the back extraction rich in zinc/cadmium；After this back extraction, liquid part returns the washing procedure of step (3) as wash solution；
(5) sulfuric acid solution that back extraction organic facies 1 adopts concentration to be 15～25g/L carries out continuous 1～4 grade of continuous back extraction, obtains rich in liquid after the back extraction of nickel cobalt and back extraction organic facies 2；
(6) sulfuric acid solution that back extraction organic facies 2 adopts concentration to be 160～200g/L carries out continuous 1～4 grade of continuous back extraction, obtaining rich in liquid after the back extraction of copper and back extraction organic facies 3, back extraction organic facies 3 continues on for the synergic solvent extraction operation of step (2) after saponification.
Method as above, preferably, described is that in solution, the content of copper is 1～5g/L containing heavy metal solution, the content of nickel is 0.1～1g/L, and the content of cobalt is 0.1～1g/L, and the content of zinc is 1～20g/L, the content of cadmium is 0.1～1g/L, the content of calcium is 0～1g/L, and the content of magnesium is 0～15g/L, and pH value of solution is 1～5.
Method as above, preferably, synergic solvent extraction condition in described step (2) is: temperature 20～40 DEG C, composite extractant concentration in organic facies is 0.5～2mol/L, the volume ratio of organic facies and aqueous phase is 1: 1～1: 2, extraction time 20～40min, extracts progression 1～4 grade, and extraction equilibrium pH is 5.6～5.8.
Method as above, it is preferable that the wash conditions in described step (3) is: temperature 20～40 DEG C, the volume ratio of organic facies and aqueous phase is 4: 1～2: 1, wash time 20～40min, washs progression 1～2 grade, adds NaOH solution and regulate pH value to 5.6～5.8 in backwash liquor.
The volume ratio of method as above, it is preferable that the back extraction condition in described step (4) is: back extraction acidity 4～6g/L, temperature 20～40 DEG C, organic facies and aqueous phase is 2: 1～1: 1, Stripping times 10～40min, back extraction progression 1～4 grade.
The volume ratio of method as above, it is preferable that the back extraction condition in described step (5) is: back extraction acidity 15～25g/L, temperature 20～40 DEG C, organic facies and aqueous phase is 2: 1～1: 1, Stripping times 20～40min, back extraction progression 1～4 grade.
The volume ratio of method as above, it is preferable that the back extraction condition in described step (6) is: back extraction acidity 160～200g/L, temperature 20～40 DEG C, organic facies and aqueous phase is 4: 1～1: 1, Stripping times 20～40min, back extraction progression 1～4 grade.
The beneficial effects of the present invention is: the method for the present invention utilize isomeric acid kind of extractants Versatic10 and oximes chelate extraction agent Mextral984H composite after synergic solvent extraction effect and extraction back extraction nature difference under different pH condition, by controlling extraction and back extraction condition, it is separated and recovered from containing the copper in heavy metal solution, nickel cobalt, zinc/cadmium.The method implement after without waste water generation, finally give be easily isolated the solution rich in zinc/cadmium, the solution rich in nickel cobalt, solution rich in the solution of copper and only calcic/magnesium.And only the solution of calcic/magnesium can directly return and produces workshop section containing heavy metal solution, it is achieved the high efficiente callback of valuable metal ions and wastewater zero discharge in solution.The method is stable, reduced investment instant effect, non-environmental-pollution, is that high efficiente callback is containing the method for optimizing of valuable metal ions in heavy metal solution.
Accompanying drawing explanation
Fig. 1 is the process chart of a kind of preferred implementation of the present invention.
Detailed description of the invention
Embodiment
Below in conjunction with preferred embodiment example, the invention will be further described.
Embodiment 1 high efficiency separation is containing heavy metal solution
Zhejiang copper smelting plant heavy metal waste slag adopts sulfuric acid leaching, and in leachate, cupric is about 2g/L, nickel is about 0.9g/L, zinc is about 16g/L, and cadmium is about 0.3g/L, and calcium is about 0.7g/L, and magnesium is about 8g/L, and pH value is about 1.8.Employing present invention process processes, and flow process as it is shown in figure 1, unless otherwise indicated, compares the volume ratio being organic facies with aqueous phase herein, and concrete operation is as follows:
(1) in leachate, add lime cream and regulate pH to about 5.4.The requirement adding lime cream adjustment pH value in the method for the present invention is: in solution, heavy metal ion does not occur under the premise of hydrolysis, and the pH value of solution is height as far as possible.Adopt grid, inclined-plate clarifying basin pretreatment, remove the waste residue such as bulky grain thing and solid suspension.
(2) synergic reagent good for sedimentation tank supernatant saponification is carried out continuous 2 grades of extractions.Composite extractant is by Versatic10 and Mextral984H by volume 1∶1 composite forms, and composite extractant concentration in organic facies is 1mol/L, and diluent is DT100, and saponification rate is about 55%.Extraction conditions is: temperature 30 DEG C, is in a ratio of 1: 1.33, extraction time 30min, adds a small amount of NaOH solution and make extraction equilibrium pH about 5.6 in extraction process.After extraction, organic facies enters next stage backwash operation, and raffinate returns waste residue sulfuric acid leaching operation.
(3) by the organic facies after synergic solvent extraction with containing zinc 100g/L, solution (adopting zinc-rich/cadmium liquid that step (4) obtains to replace this solution after circulation) containing cadmium 10g/L carries out continuous 2 grades of washings, wash conditions is: temperature 20 DEG C, it is in a ratio of 3: 1, wash time 20min, adds a small amount of NaOH solution and makes pH about 5.6 in backwash liquor.After washing, backwash residual liquid returns step (2) synergic solvent extraction operation, and organic facies enters next stage operation.
(4) organic facies after washing is carried out 1 grade of selectivity back extraction.Back extraction condition is: temperature 20 DEG C, compares 1: 1, Stripping times 10min, back extraction acidity 5g/L sulfuric acid solution.After back extraction, liquid is zinc-rich/cadmium liquid, and part is for the washing procedure of step (3), and part is directly entered zinc cadmium centrifugal station；Back extraction organic facies 1 enters next stage operation.
(5) back extraction organic facies 1 is carried out continuous 2 grades of selectivity back extractions.Back extraction condition is: temperature 20 DEG C, compares 1: 1, Stripping times 30min, back extraction acidity 15g/L sulfuric acid solution.After back extraction, liquid is rich nickel cobalt liquid, is directly entered Separation of nickel and cobalt workshop section；Back extraction organic facies 2 enters next stage operation.
(6) back extraction organic facies 2 is carried out continuous 2 grades of selectivity back extractions.Back extraction condition is: temperature 20 DEG C, compares 3: 1, Stripping times 30min, back extraction acidity 180g/L sulfuric acid solution.After back extraction, liquid is copper-rich liquid, is directly entered cupric electrolysis operation；Back extraction organic facies 3 enters next stage operation.
(7) using NaOH solution that back extraction organic facies 3 is carried out saponification, saponification rate about 55%, after saponification, organic facies is used for step (2) synergic solvent extraction operation.
The former employing chemical precipitation method of this factory progressively reclaims valuable metal in solution, and year loss zinc is about 200t, and year about 1～20,000 tons of waste residues store up, environmental pollution is serious.After adopting this technique, not only production cost decreases about 30%, and valuable metal is fully reclaimed, Qi Zhongtong, zinc, the response rate about 90% of cadmium, nickel the response rate about 80%.While solving environmental pollution, save a large amount of production cost for enterprise, bring considerable economic benefit.
Embodiment 2 high efficiency separation is containing heavy metal solution
In Zhejiang zinc abstraction factory purification slag leachate, cupric is about 5g/L, nickel is about 0.3g/L, cobalt is about 0.8g/L, and zinc is about 20g/L, and cadmium is about 0.7g/L, and calcium is about 0.5g/L, and magnesium is about 10g/L, and pH value is about 1.0.Employing present invention process processes, and flow process as it is shown in figure 1, unless otherwise indicated, compares the volume ratio being organic facies with aqueous phase herein, and concrete operation is as follows:
(1) in leachate, add lime cream and regulate pH to about 5.4.The requirement adding lime cream adjustment pH value in the method for the present invention is: in solution, heavy metal ion does not occur under the premise of hydrolysis, and the pH value of solution is height as far as possible.Adopt grid, inclined-plate clarifying basin pretreatment, remove the waste residue such as bulky grain thing and solid suspension.
(2) synergic reagent good for sedimentation tank supernatant saponification is carried out continuous 3 grades of extractions.Composite extractant composite is formed by volume by Versatic10 and Mextral984H at 1: 1, and composite extractant concentration in organic facies is 1M, and diluent is DT100, and saponification rate is about 35%.Extraction conditions is: temperature 30 DEG C, and the volume ratio of organic facies and aqueous phase is 1: 2, and extraction time 30min adds a small amount of NaOH solution and makes extraction equilibrium pH about 5.6 in extraction process.After extraction, organic facies enters next stage backwash operation, and raffinate returns and leaches operation.
(3) by the organic facies after synergic solvent extraction with containing zinc 100g/L, solution (adopting zinc-rich/cadmium liquid that step (4) obtains to replace this solution after circulation) containing cadmium 10g/L carries out continuous 2 grades of washings, wash conditions is: temperature 20 DEG C, it is in a ratio of 3: 1, wash time 20min, adds a small amount of NaOH solution and makes pH about 5.6 in backwash liquor.After washing, backwash residual liquid returns step (2) synergic solvent extraction operation, and organic facies enters next stage operation.
(4) organic facies after washing is carried out 1 grade of selectivity back extraction.Back extraction condition is: temperature 20 DEG C, compares 1: 1, Stripping times 10min, back extraction acidity 5g/L sulfuric acid solution.After back extraction, liquid is zinc-rich/cadmium liquid, and part is for the washing procedure of step (3), and part is directly entered zinc cadmium centrifugal station；Back extraction organic facies 1 enters next stage operation.
(5) back extraction organic facies 1 is carried out continuous 3 grades of selectivity back extractions.Back extraction condition is: temperature 20 DEG C, compares 1: 1, Stripping times 30min, back extraction acidity 20g/L sulfuric acid solution.After back extraction, liquid is rich nickel cobalt liquid, is directly entered Separation of nickel and cobalt workshop section；Back extraction organic facies 2 enters next stage operation.
(6) back extraction organic facies 2 is carried out continuous 2 grades of selectivity back extractions.Back extraction condition is: temperature 20 DEG C, compares 3: 1, Stripping times 30min, back extraction acidity 180g/L sulfuric acid solution.After back extraction, liquid is copper-rich liquid, is directly entered cupric electrolysis operation；Back extraction organic facies 3 enters next stage operation.
(7) using NaOH solution that back extraction organic facies 3 is carried out saponification, saponification rate about 35%, after saponification, organic facies is used for step (2) synergic solvent extraction operation.
Adopt this technique reclaim valuable metal, the response rate of its copper about 90%, the response rate of zinc about 85%, nickel, cobalt, cadmium the response rate about 80%.
Claims (8)
1. a high efficiency separation is complicated containing the method for valuable metal ions in heavy metal solution, it is characterised in that: it comprises the following steps:
(1) first regulate pH=4.5～5.5 with alkali liquor containing heavy metal solution, remove bulky grain thing and insoluble matter then through the pretreatment process filtering, precipitating；
(2) pretreated continuous 1～4 grade of continuous extraction is carried out containing the synergic reagent after heavy metal solution saponification, make extraction equilibrium pH value=5.6～5.8, obtaining the raffinate of the extracted organic phase rich in heavy metal ion and only calcic/magnesium, raffinate returns production system；This synergic reagent is formed by Versatic10 and Mextral984H is composite, and its volume ratio is 2: 1～2: 4；Saponification rate is 30～60%；
(3) step (2) obtains extracted organic phase adopts and carries out continuous 1～2 grade of continuous washing containing zinc 40～100g/L, solution containing cadmium 4～10g/L, washes away the calcium/magnesium carried secretly, washes and be back to pretreatment process residual night；
(4) sulfuric acid solution that scrubbed extracted organic phase adopts concentration to be 4～6g/L carries out 1～4 grade of continuous back extraction, obtains liquid and back extraction organic facies 1 after the back extraction rich in zinc/cadmium；After this back extraction, liquid part returns the washing procedure of step (3) as wash solution；
(5) sulfuric acid solution that back extraction organic facies 1 adopts concentration to be 15～25g/L carries out continuous 1～4 grade of continuous back extraction, obtains rich in liquid after the back extraction of nickel cobalt and back extraction organic facies 2；
(6) sulfuric acid solution that back extraction organic facies 2 adopts concentration to be 160～200g/L carries out continuous 1～4 grade of continuous back extraction, obtaining rich in liquid after the back extraction of copper and back extraction organic facies 3, back extraction organic facies 3 continues on for the synergic solvent extraction operation of step (2) after saponification.
2. the method for claim 1, it is characterized in that: described is that in solution, the content of copper is 1～5g/L containing heavy metal solution, the content of nickel is 0.1～1g/L, the content of cobalt is 0.1～1g/L, the content of zinc is 1～20g/L, and the content of cadmium is 0.1～1g/L, and the content of calcium is 0～1g/L, the content of magnesium is 0～15g/L, and pH value of solution is 1～5.
3. the method for claim 1, it is characterized in that: the synergic solvent extraction condition in described step (2) is: temperature 20～40 DEG C, composite extractant concentration in organic facies is 0.5～2mol/L, the volume ratio of organic facies and aqueous phase is 1: 1～1: 2, extraction time 20～40min, extracting progression 1～4 grade, extraction equilibrium pH is 5.6～5.8.
4. the method for claim 1, it is characterized in that: the wash conditions in described step (3) is: temperature 20～40 DEG C, the volume ratio of organic facies and aqueous phase is 4: 1～2: 1, wash time 20～40min, washing progression 1～2 grade, adds NaOH solution and regulates pH value to 5.6～5.8 in backwash liquor.
5. the method for claim 1, it is characterized in that: the back extraction condition in described step (4) is: back extraction acidity 4～6g/L, temperature 20～40 DEG C, the volume ratio of organic facies and aqueous phase is 2: 1～1: 1, Stripping times 10～40min, back extraction progression 1～4 grade.
6. the method for claim 1, it is characterized in that: the back extraction condition in described step (5) is: back extraction acidity 15～25g/L, temperature 20～40 DEG C, the volume ratio of organic facies and aqueous phase is 2: 1～1: 1, Stripping times 20～40min, back extraction progression 1～4 grade.
7. the method for claim 1, it is characterized in that: the back extraction condition in described step (6) is: back extraction acidity 160～200g/L, temperature 20～40 DEG C, the volume ratio of organic facies and aqueous phase is 4: 1～1: 1, Stripping times 20～40min, back extraction progression 1～4 grade.
8. the method for claim 1, it is characterised in that: described method includes following operation:
Operation 1, adding alkali liquor containing heavy metal solution pH regulator to 4.5～5.5, and will be filtered, precipitates pretreatment, removes bulky grain insoluble matter therein and solid suspension；
Operation 2, operation 1 pretreatment supernatant is carried out continuous 1～4 grade of synergic solvent extraction, extraction conditions is: synergic reagent is Versatic10 and the Mextral984H through saponification, and both volume ratios are 2: 1～2: 4, and saponification rate is 30～60%, composite extractant concentration in organic facies is 0.5～2mol/L, the volume ratio of temperature 20～40 DEG C, organic facies and aqueous phase is 1: 1～1: 2, extraction time 20～40min, add NaOH solution and regulate pH, maintain extraction equilibrium pH about 5.6～5.8；Extracting end raffinate and be the solution of only calcic/magnesium, organic facies enters operation 3；
Operation 3, organic facies operation 2 obtained liquid after the part back extraction containing zinc 40～100g/L, solution containing cadmium 4～10g/L or operation 4 carries out continuous 1～2 grade of washing, wash conditions is: temperature 20～40 DEG C, the volume ratio of organic facies and aqueous phase is 4: 1～2: 1, extraction time 20～40min, adds NaOH solution and regulates pH to 5.6～5.8 in backwash liquor；Backwash after washing returns operation 2 residual night, and after washing, organic facies enters operation 4；
Operation 4, carries out selectivity back extraction by the organic facies of operation 3, and back extraction condition is: temperature 20～40 DEG C, and the volume ratio of organic facies and aqueous phase is 2: 1～1: 1, Stripping times 10～40min, back extraction acidity 4～6g/L sulfuric acid solution, back extraction progression 1～4 rank；After back extraction gained back extraction, liquid is zinc-rich/cadmium liquid, and part is washed for operation 3, is partially into zinc cadmium centrifugal station；Back extraction organic facies enters operation 5；
Operation 5, carries out selectivity back extraction by the organic facies of operation 4, and back extraction condition is: temperature 20～40 DEG C, and the volume ratio of organic facies and aqueous phase is 2: 1～1: 1, Stripping times 20～40min, back extraction acidity 15～25g/L sulfuric acid solution, back extraction progression 1～4 rank；After back extraction gained back extraction, liquid is rich nickel cobalt liquid, enters NI-G centrifugal station；Back extraction organic facies enters operation 6；
Operation 6, carries out selectivity back extraction by the organic facies of operation 5, and back extraction condition is: temperature 20～40 DEG C, and the volume ratio of organic facies and aqueous phase is 4: 1～1: 1, Stripping times 20～40min, back extraction acidity 160～200g/L sulfuric acid solution, back extraction progression 1～4 rank；After back extraction gained back extraction, liquid is copper-rich liquid, can directly reclaim；Back extraction organic facies enters operation 7；
Operation 7, adds NaOH solution in the back extraction organic facies of operation 6 and carries out saponification, and saponification rate about 30～60%, after saponification, organic facies entrance operation 2 carries out synergic solvent extraction.
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| CN109534580A (en) * | 2018-12-29 | 2019-03-29 | 宜宾北方川安化工有限公司 | Trimethylolethane trimethacrylate nitrate wastewater industrializes stable treatment method |
| CN109797294A (en) * | 2019-02-02 | 2019-05-24 | 广东芳源环保股份有限公司 | The method of nickel, cobalt is recycled in a kind of magnesium water |
| CN111206154A (en) * | 2020-02-25 | 2020-05-29 | 中国科学院过程工程研究所 | Method for separating and recovering valuable metal ions in waste ternary battery material |
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| CN108118155A (en) * | 2017-12-26 | 2018-06-05 | 广东工业大学 | A kind of method of discarded ickel-cadmium cell recycling |
| CN108179275A (en) * | 2017-12-26 | 2018-06-19 | 广东工业大学 | The recovery method of cadmium nickel in a kind of waste Ni Cd battery |
| CN108118155B (en) * | 2017-12-26 | 2019-10-11 | 广东工业大学 | A kind of method of discarded ickel-cadmium cell resource utilization |
| CN108179275B (en) * | 2017-12-26 | 2019-11-08 | 广东工业大学 | The recovery method of cadmium nickel in a kind of waste Ni Cd battery |
| CN109534580A (en) * | 2018-12-29 | 2019-03-29 | 宜宾北方川安化工有限公司 | Trimethylolethane trimethacrylate nitrate wastewater industrializes stable treatment method |
| CN109797294A (en) * | 2019-02-02 | 2019-05-24 | 广东芳源环保股份有限公司 | The method of nickel, cobalt is recycled in a kind of magnesium water |
| CN109797294B (en) * | 2019-02-02 | 2021-11-09 | 广东芳源环保股份有限公司 | Method for recovering nickel and cobalt from magnesium water |
| CN111206154A (en) * | 2020-02-25 | 2020-05-29 | 中国科学院过程工程研究所 | Method for separating and recovering valuable metal ions in waste ternary battery material |
| CN111549242A (en) * | 2020-04-24 | 2020-08-18 | 核工业北京化工冶金研究院 | Uranium purification method for alkaline residue leachate |
| CN112250207A (en) * | 2020-08-21 | 2021-01-22 | 广东臻鼎环境科技有限公司 | Method for extracting copper ion extractant from waste liquid |
| CN114317961A (en) * | 2021-12-30 | 2022-04-12 | 重庆康普化学工业股份有限公司 | Co-extraction system for nickel-cobalt co-extraction and co-extraction method thereof |
| CN114717415A (en) * | 2022-03-30 | 2022-07-08 | 有研资源环境技术研究院(北京)有限公司 | Method for separating multi-metal mixed solution |
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