CN115124071A - Method for preparing thallium salt by selectively recovering thallium from thallium-containing sludge - Google Patents
Method for preparing thallium salt by selectively recovering thallium from thallium-containing sludge Download PDFInfo
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Abstract
The invention belongs to the technical field of solid waste treatment and thallium element recovery, and discloses a method for preparing thallium salt by selectively recovering thallium from thallium-containing sludge. The method comprises the following steps: (1) performing ball milling and crushing treatment on thallium-containing sludge, and then uniformly stirring and mixing the thallium-containing sludge and water to obtain a solid-liquid mixture; (2) carrying out hydro-thermal treatment on the solid-liquid mixture obtained in the step (1), and carrying out solid-liquid separation to obtain filter residue and a thallium extracting solution; (3) and (3) adding chloride or iodide into the thallium extracting solution obtained in the step (2), stirring for reaction until precipitation is separated out, and filtering and drying to obtain TlCl or TlI crystals. The method utilizes the difference between thallium sulfide in thallium-containing sludge and other heavy metal sulfides to realize thallium selective extraction, and promotes Tl through a hydrothermal treatment process 2 The release of S has the advantages of simple process, low cost and high thallium resource recovery efficiency.
Description
Technical Field
The invention belongs to the technical field of solid waste treatment and thallium element recovery, and particularly relates to a method for preparing thallium salt by selectively recovering thallium from thallium-containing sludge.
Background
Thallium is a rare and dispersed metal, the content of which in the earth crust is very low, and the dispersed thallium is gradually enriched after the smelting process as the exploitation amount of lead-zinc mineral resources increases. The recovery of thallium resources is neglected, resulting in great waste of resources. In addition, the smelting acidic sewage is usually subjected to deep removal of heavy metal ions by adding sulfides to generate sludge containing a large amount of heavy metal sulfides such as lead, zinc, cadmium, thallium and the like, wherein thallium mainly exists in monovalent ions and is easily dissolved in water, and serious thallium pollution can be caused by direct stacking.
Thallium chloride (thallium chloride) is a good semiconductor material and widely used in the fields of safety detection and imaging, and is also a raw material of other thallium reagents. Thallium iodide (thallium iodide) is often used as an additive in the preparation of luminescent materials such as scintillators and signal lamps, can significantly improve the photoelectric properties of the materials when doped with other halogen metals, and is an important raw material. Therefore, the thallium chloride or thallium iodide prepared by recycling the thallium resource has good economic value and environmental protection significance.
Patents CN 109850935 a and CN 109811128A disclose a method for preparing thallium chloride and thallium iodide by recovering thallium from acid smelting wastewater, respectively, wherein a trivalent thallium complex anion is obtained by oxidizing monovalent thallium ions in the wastewater; adsorbing trivalent thallium complex anions by anion exchange resin; and reducing trivalent thallium complex anion on the anion exchange resin, eluting to obtain eluent containing enriched monovalent thallium ions, and adding hydrochloric acid or iodide to react to obtain thallium chloride or thallium iodide. The patent CN 103818947A discloses a method for preparing thallium iodide by using lead-zinc ore smelting wastewater as a raw material; patent CN 109607595 a discloses a method for preparing thallium iodide by using thallium-containing waste acid water as a raw material. The above patent technologies all use smelting waste water as raw material, not smelting waste slag. Patent CN 108975386 a discloses a preparation method of thallium iodide based on interface effect; patent CN 108217716a discloses a method for preparing thallium iodide, which uses smelting waste residue as raw material to prepare thallium iodide, but does not utilize the property difference between different valence states of thallium and other heavy metal compounds, and needs to continuously adjust different valence states of thallium, so the process is complex.
Therefore, there is a need to propose a method for preparing thallium chloride or thallium iodide by selectively recovering thallium from thallium-containing sludge, so as to solve or at least alleviate the above technical drawbacks.
Disclosure of Invention
In view of the above disadvantages and drawbacks of the prior art, an object of the present invention is to provide a method for preparing thallium salt from thallium-containing sludge by selective recovery of thallium.
The purpose of the invention is realized by the following technical scheme:
a process for the selective recovery of thallium to produce thallium salts from thallium containing sludge comprising the steps of:
(1) performing ball milling and crushing treatment on thallium-containing sludge, and then uniformly stirring and mixing the thallium-containing sludge and water to obtain a solid-liquid mixture;
(2) carrying out hydrothermal treatment on the solid-liquid mixture obtained in the step (1), and carrying out solid-liquid separation to obtain filter residue and a thallium extracting solution;
(3) and (3) adding chloride or iodide into the thallium extracting solution obtained in the step (2), stirring for reaction until precipitation is separated out, and filtering and drying to obtain TlCl or Tl I crystals.
Further, the thallium-containing sludge in the step (1) is heavy metal sulfide sludge precipitated by adding sulfide to the acid smelting wastewater.
Further, wet ball milling is adopted in the ball milling and crushing treatment in the step (1), the ball milling time of the wet ball milling is 1-6 hours, the rotating speed is 50-300 r/min, and the ball-to-material ratio is 1: 2-10.
Furthermore, the solid-to-liquid ratio of the thallium-containing sludge mixed with the water in the step (1) is 1kg: 2-10L.
Further, the temperature of the hydrothermal treatment in the step (2) is 60-140 ℃, and the time is 1-24 hours.
Further, in the hydrothermal treatment process in the step (2), the solid-liquid mixture is stirred.
Further, in the hydrothermal treatment process in the step (2), the pH value needs to be kept within a range of 7-8.
Further, the solid-liquid separation method in the step (2) comprises the following steps: after cooling the product after hydrothermal treatment, separating the supernatant from the precipitate by filtration and centrifugation.
And (3) further, returning the filter residue obtained in the step (2) to the lead-zinc ore smelting process for recycling.
Further, the chloride in the step (3) is at least one of potassium chloride and sodium chloride; the iodide is at least one of potassium iodide and sodium iodide, and the mass volume ratio of the added amount of the chloride and the iodide to the thallium extracting solution is 5-30 g/L.
Further, the stirring reaction time in the step (3) is 30-60 min.
The main principle of the invention comprises:
①Tl 2 S↓→2Tl + +S 2-
the method for producing the thallium-containing sludge main phase including CaSO by using sulfide to treat acid wastewater 4 ·2H 2 O，Tl 2 S, PbS, ZnS, CdS. Wherein Tl 2 S is wrapped in calcium sulfate and other heavy metal sulfides to be precipitated together. Due to Tl 2 S is a sparingly soluble substance (PbS, K) sp ＝10 -28 ；ZnS，K sp ＝10 -25 ；CdS，K sp ＝10 -28 ；Tl 2 S，K sp 0.02), the solubility increases with increasing temperature, gradually dissolving into an ionic state; and other heavy metal sulfides are insoluble substances and cannot be dissolved, so that thallium can be selectively extracted.
②CaSO 4 ·2H 2 O↓→CaSO 4 ·0.5H 2 O↓/CaSO 4 ↓ releasing entrained Tl 2 S
In the hydrothermal process, calcium sulfate dihydrate is gradually dehydrated into calcium sulfate hemihydrate/anhydrous calcium sulfate, which is a dissolution-recrystallization process, namely CaSO 4 ·2H 2 O will dissolve into Ca 2+ With SO 4 2- Re-nucleated to calcium sulfate hemihydrate or calcium sulfate anhydrite, and thus the Tl is encapsulated in the calcium sulfate in the process 2 S exposure to liquidThe environment gradually dissolves as the temperature increases. It should be noted that, in the technology, the selective extraction of thallium is realized through the difference between thallium sulfide and other heavy metal sulfides, and alkaline and acidic environments promote the dissolution of other heavy metal sulfides, so that the selective extraction cannot be realized, and therefore, the reaction condition needs to maintain the pH close to neutral.
③Tl + +Cl - →TlCl↓；Tl + +I - →TlI↓
In the precipitation process, the ionic Tl is precipitated by chloride or iodide + Converting into TlCl or Tl I products.
Compared with the prior art, the invention has the beneficial effects that:
the method utilizes the difference between thallium sulfide in thallium-containing sludge and other heavy metal sulfides to realize thallium selective extraction, and promotes Tl through a hydrothermal treatment process 2 And S is released, so that the method has the advantages of simple process, low cost and high thallium resource recovery efficiency.
Drawings
FIG. 1 is a graph showing the effect of hydrothermal temperature (80 deg.C, 95 deg.C, 120 deg.C, 140 deg.C) on the extraction of different heavy metal elements in example 1;
FIG. 2 is a graph showing phase changes of the residue after extraction at different hydrothermal temperatures (80 deg.C, 95 deg.C, 120 deg.C, 140 deg.C) in example 1.
Fig. 3 is a graph showing the change of extraction efficiency of different heavy metal elements after hydrothermal extraction at different pH (3.2, 4.0, 5.0, 6.3, 7.5, 10.0, 11.0) in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
(1) 50g of thallium-containing sludge (heavy metal sulfide sludge precipitated by adding sulfide into smelting acidic wastewater, the thallium content is 3.5%, lead content is 6.9%, cadmium content is 5.4%, zinc content is 1.7%, and water content is 22%) is subjected to ball milling and crushing treatment (ball milling time is 1h, rotating speed is 100r/min, ball-to-material ratio is 1:2), and then the thallium-containing sludge is fully mixed and stirred with 300ml of deionized water to obtain a solid-liquid mixture.
(2) And (3) putting the solid-liquid mixture into a hydrothermal kettle, keeping the pH value of the solution at 7.5, heating to 120 ℃, stirring for reaction for 6 hours, standing and cooling to room temperature after the reaction is finished. And opening the hydrothermal kettle, separating the supernatant from the precipitate in a filtering and centrifuging mode to obtain a thallium extracting solution and a certain amount of filter residue, and returning the obtained filter residue to the lead-zinc ore smelting process for recycling.
(3) And adding 2g of potassium chloride into the thallium extracting solution, stirring and reacting for 40min until a precipitate is separated out, filtering and drying to obtain 1.4g of thallium chloride solid.
Through ICP-MS detection, the relative content of thallium, lead, zinc and cadmium in the thallium extracting solution obtained in the step (2) accounts for 99.78%, 0.17%, 0% and 0.05%, the extraction efficiency is calculated by comparing the content in the filter residue, and the selective extraction efficiency of thallium is 63%. The obtained solid thallium chloride is subjected to digestion test, and the purity can reach 99.7%.
The effect of different hydrothermal temperatures (80 ℃, 95 ℃, 120 ℃, 140 ℃) on the extraction of different heavy metal elements is experimentally studied, and the result is shown in figure 1. It was found that the thallium concentration in the thallium extract increases with increasing temperature, and the leaching of other heavy metals is very low.
Phase change of the residue after extraction at different hydrothermal temperatures (80 deg.C, 95 deg.C, 120 deg.C, 140 deg.C) was experimentally investigated, and the results are shown in FIG. 2. It was found that as the temperature increased, the calcium sulphate dihydrate was gradually converted to calcium sulphate hemihydrate/anhydrite and the thallium leaching concentration increased during the conversion.
The experimental study on the change of extraction efficiency of different heavy metal elements after hydrothermal extraction under different pH conditions (3.2, 4.0, 5.0, 6.3, 7.5, 10.0 and 11.0) shows that the results are shown in FIG. 3. As can be seen from the results in FIG. 3, the hydrothermal extraction process maintains pH close to neutral, thallium selective extraction can be realized, and alkaline and acidic environments promote dissolution of other heavy metal sulfides, so that selective extraction cannot be realized.
Example 2
(1) 100g of thallium-containing sludge (thallium content of 1.2%, lead content of 11%, cadmium content of 5.6%, zinc content of 2.4%, water content of 6%) is subjected to ball milling and crushing treatment (ball milling time is 2h, rotating speed is 70r/min, ball-to-material ratio is 1:6), and then the sludge is fully mixed and stirred with 250ml of deionized water to obtain a solid-liquid mixture.
(2) And (3) putting the solid-liquid mixture into a hydrothermal kettle, keeping the pH value of the solution at 7.8, heating to 90 ℃, stirring for reacting for 18 hours, standing and cooling to room temperature after the reaction is finished. And opening the hydrothermal kettle, separating the supernatant from the precipitate in a filtering and centrifuging mode to obtain a thallium extracting solution and a certain amount of filter residue, and returning the obtained filter residue to the lead-zinc ore smelting process for recycling.
(3) And adding 3g of potassium chloride into the thallium extracting solution, stirring and reacting for 30min until precipitates are separated out, filtering and drying to obtain 0.8g of solid thallium chloride.
By ICP-MS detection, the relative content of thallium, lead, zinc and cadmium in the thallium extract is respectively 99.84%, 0.14%, 0% and 0.02%, the extraction efficiency is calculated by comparing the content of the filter residue, and the selective extraction efficiency of thallium is 65%. The obtained solid thallium chloride is subjected to digestion test, and the purity can reach 99.8%.
Example 3
(1) 100g of thallium-containing sludge (thallium content of 3.5%, lead of 6.9%, cadmium of 5.4%, zinc of 1.7%, water content of 22%) is subjected to ball milling and crushing treatment (ball milling time is 1h, rotating speed is 70r/min, ball-to-material ratio is 1:2), and then is fully mixed and stirred with 600ml of deionized water to obtain a solid-liquid mixture.
(2) And (3) putting the solid-liquid mixture into a hydrothermal kettle, keeping the pH value of the solution at 7.2, heating to 80 ℃, reacting for 6 hours, standing and cooling to room temperature after the reaction is finished. And opening the hydrothermal kettle, separating the supernatant from the precipitate in a filtering and centrifuging mode to obtain a thallium extracting solution and a certain amount of filter residue, and returning the obtained filter residue to the lead-zinc ore smelting process for recycling.
(3) And adding 4g of potassium chloride into the thallium extracting solution, stirring and reacting for 40min until a precipitate is separated out, filtering and drying to obtain 1.3g of thallium chloride solid.
By ICP-MS detection, the relative content of thallium, lead, zinc and cadmium in the thallium extract is respectively 99.88%, 0.1%, 0% and 0.02%, the extraction efficiency is calculated by comparing the content of the filter residue, and the selective extraction efficiency of thallium is 46.64%. The obtained solid thallium chloride is subjected to digestion test, and the purity can reach 99.8%.
Example 4
(1) 60g of thallium-containing sludge (thallium content of 1.2%, lead content of 11%, cadmium content of 5.6%, zinc content of 2.4%, water content of 6%) is subjected to ball milling and crushing treatment (ball milling time is 2h, rotating speed is 250r/min, ball-to-material ratio is 1:10), and then the sludge is fully mixed and stirred with 400ml of deionized water to obtain a solid-liquid mixture.
(2) And (3) putting the solid-liquid mixture into a hydrothermal kettle, keeping the pH of the solution at 7.6, heating to 140 ℃, reacting for 24 hours, standing and cooling to room temperature after the reaction is finished. And opening the hydrothermal kettle, separating the supernatant from the precipitate in a filtering and centrifuging mode to obtain a thallium extracting solution and a certain amount of filter residue, and returning the obtained filter residue to the lead-zinc ore smelting process for recycling.
(3) And adding 2g of sodium chloride into the thallium extracting solution, stirring and reacting for 60min until a precipitate is separated out, filtering and drying to obtain 0.4g of thallium chloride solid.
By ICP-MS detection, the relative content of thallium, lead, zinc and cadmium in the thallium extract is respectively 99.91%, 0.07%, 0% and 0.02%, the extraction efficiency is calculated by comparing the content of the filter residue, and the selective extraction efficiency of thallium is 73.45%. The obtained solid thallium chloride is subjected to digestion test, and the purity can reach 99.8%.
Example 5
(1) 100g of thallium-containing sludge (thallium content of 3.5%, lead of 6.9%, cadmium of 5.4%, zinc of 1.7%, water content of 22%) is subjected to ball milling and crushing treatment (ball milling time is 2h, rotation speed is 200r/min, ball-to-material ratio is 1:5), and then is fully mixed and stirred with 300ml of deionized water to obtain a solid-liquid mixture.
(2) And (3) putting the solid-liquid mixture into a hydrothermal kettle, keeping the pH of the solution at 7.5, heating to 140 ℃, reacting for 12 hours, standing and cooling to room temperature after the reaction is finished. And opening the hydrothermal kettle, separating the supernatant from the precipitate in a filtering and centrifuging mode to obtain a thallium extracting solution and a certain amount of filter residue, and returning the obtained filter residue to the lead-zinc ore smelting process for recycling.
(3) And adding a potassium iodide solid into the thallium extracting solution, stirring and reacting for 40min until a precipitate is separated out, filtering and drying to obtain 2.4g of thallium iodide solid.
By ICP-MS detection, the relative contents of thallium, lead, zinc and cadmium in the thallium extract are respectively 99.85%, 0.12%, 0% and 0.03%, the extraction efficiency is calculated by comparing the contents of the filter residue, and the thallium selective extraction efficiency is 74%. The obtained thallium iodide solid is subjected to digestion test, and the purity can reach 99.8%.
Example 6
(1) 40g of thallium-containing sludge (thallium content of 1.2%, lead content of 11%, cadmium content of 5.6%, zinc content of 2.4%, water content of 6%) is subjected to ball milling and crushing treatment (ball milling time of 0.5h, rotation speed of 200r/min, ball-to-material ratio of 1:10), and then is fully mixed and stirred with 280ml of deionized water to obtain a solid-liquid mixture.
(2) And (3) putting the solid-liquid mixture into a hydrothermal kettle, keeping the pH of the solution at 7.5, heating to 95 ℃, reacting for 24 hours, standing and cooling to room temperature after the reaction is finished. And opening the hydrothermal kettle, separating the supernatant from the precipitate in a filtering and centrifuging mode to obtain a thallium extracting solution and a certain amount of filter residue, and returning the obtained filter residue to the lead-zinc ore smelting process for recycling.
(3) And adding sodium iodide solid into the thallium extracting solution, stirring and reacting for 45min until precipitate is separated out, filtering and drying to obtain 0.2g of thallium iodide solid.
By ICP-MS detection, the relative content of thallium, lead, zinc and cadmium in the thallium extract is respectively 99.88%, 0.08%, 0% and 0.04%, the extraction efficiency is calculated by comparing the content in the filter residue, and the selective extraction efficiency of thallium is 48.85%. The obtained thallium iodide solid is subjected to digestion test, and the purity can reach 99.8%.
Comparative example 1
Compared with the embodiment 1, the comparative example adopts normal temperature water immersion to replace the hydrothermal treatment process, and comprises the following specific steps:
(1) 50g of thallium-containing sludge (thallium content of 3.5%, lead of 6.9%, cadmium of 5.4%, zinc of 1.7%, water content of 22%) is subjected to ball milling and crushing treatment (ball milling time is 1h, rotating speed is 100r/min, ball-to-material ratio is 1:2), and then the sludge is fully mixed and stirred with 300ml of deionized water to obtain a solid-liquid mixture.
(2) Keeping the pH value of the solid-liquid mixture at 7.5, carrying out water leaching treatment for 6h at normal temperature, separating the supernatant from the precipitate in a filtering and centrifuging manner to obtain a thallium extracting solution and a certain amount of filter residue, and returning the obtained filter residue to the lead-zinc ore smelting process for recycling.
(3) And adding 2g of potassium chloride into the thallium extracting solution, stirring and reacting for 40min until precipitates are separated out, filtering and drying to obtain 0.32g of solid thallium chloride.
Through ICP-MS detection, the relative content of thallium, lead, zinc and cadmium in the thallium extracting solution obtained in the step (2) accounts for 0.98%, 0.01%, 0.00% and 0.011% respectively, the extraction efficiency is calculated by comparing the content in the filter residue, and the selective extraction efficiency of thallium is 14.4%. The obtained solid thallium chloride is subjected to digestion test, and the purity is 99.7%.
As can be seen from the comparison of this comparative example with example 1, the selective extraction efficiency of thallium can be significantly improved by the high-temperature hydrothermal reaction.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for preparing thallium salts from thallium containing sludge by selective recovery of thallium comprising the steps of:
(1) performing ball milling and crushing treatment on thallium-containing sludge, and then uniformly stirring and mixing the thallium-containing sludge and water to obtain a solid-liquid mixture;
(2) carrying out hydrothermal treatment on the solid-liquid mixture obtained in the step (1), and carrying out solid-liquid separation to obtain filter residue and a thallium extracting solution;
(3) and (3) adding chloride or iodide into the thallium extracting solution obtained in the step (2), stirring for reaction until precipitation is separated out, and filtering and drying to obtain TlCl or TlI crystals.
2. The method for selectively recovering thallium to prepare thallium salt from thallium containing sludge as claimed in claim 1, wherein the thallium containing sludge in step (1) is heavy metal sulfide sludge precipitated by adding sulfide for treating smelting acidic wastewater.
3. The method for preparing thallium salt from thallium-containing sludge according to claim 1, wherein wet ball milling is adopted in the ball milling and pulverization treatment in step (1), the ball milling time of the wet ball milling is 1-6 h, the rotation speed is 50-300 r/min, and the ball-to-material ratio is 1: 2-10.
4. The method for preparing thallium salt from thallium-containing sludge according to claim 1, wherein the solid-to-liquid ratio of the thallium-containing sludge mixed with water in step (1) is 1kg: 2-10L.
5. The method for preparing thallium salt from thallium-containing sludge according to claim 1, wherein the temperature of the hydrothermal treatment in step (2) is 60-140 ℃ for 1-24 h.
6. The method for selectively recovering thallium to produce thallium salts from thallium containing sludge as claimed in claim 1, wherein the solid-liquid mixture is subjected to agitation during the hydrothermal treatment in step (2).
7. The method for preparing thallium salt from thallium-containing sludge according to claim 1, wherein during the hydrothermal treatment in step (2), it is necessary to maintain the pH in the range of 7 to 8.
8. The method for selectively recovering thallium to produce thallium salts from thallium containing sludge as claimed in claim 1, wherein the solid-liquid separation in step (2) is: cooling the product after the hydrothermal treatment, and separating the supernatant from the precipitate in a filtration and centrifugation mode; the obtained filter residue is returned to the lead-zinc ore smelting process for recycling.
9. The method for preparing thallium salt selective recovery from thallium containing sludge according to claim 1, wherein the chloride in step (3) is at least one of potassium chloride and sodium chloride; the iodide is at least one of potassium iodide and sodium iodide, and the mass volume ratio of the added amount of the chloride and the iodide to the thallium extracting solution is 5-30 g/L.
10. The method for selectively recovering thallium to produce thallium salts from thallium containing sludge as claimed in claim 1, wherein the stirring reaction time in step (3) is 30-60 min.
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