CN115650196A - Synthesis method of zinc metaphosphate and application of zinc metaphosphate in thallium removal of zinc sulfate solution - Google Patents
Synthesis method of zinc metaphosphate and application of zinc metaphosphate in thallium removal of zinc sulfate solution Download PDFInfo
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- 229910052716 thallium Inorganic materials 0.000 title claims abstract description 104
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 title claims abstract description 101
- VUDJAFZYSMINQA-UHFFFAOYSA-L zinc metaphosphate Chemical compound [Zn+2].[O-]P(=O)=O.[O-]P(=O)=O VUDJAFZYSMINQA-UHFFFAOYSA-L 0.000 title claims abstract description 64
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 title claims abstract description 33
- 229960001763 zinc sulfate Drugs 0.000 title claims abstract description 33
- 229910000368 zinc sulfate Inorganic materials 0.000 title claims abstract description 33
- 238000001308 synthesis method Methods 0.000 title description 3
- 238000000034 method Methods 0.000 claims abstract description 59
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 49
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 22
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 21
- 239000011787 zinc oxide Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002893 slag Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000010189 synthetic method Methods 0.000 claims abstract description 5
- IPCXNCATNBAPKW-UHFFFAOYSA-N zinc;hydrate Chemical compound O.[Zn] IPCXNCATNBAPKW-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002002 slurry Substances 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 230000002194 synthesizing effect Effects 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 34
- 239000007787 solid Substances 0.000 description 13
- 238000003756 stirring Methods 0.000 description 13
- 238000001556 precipitation Methods 0.000 description 11
- 239000002351 wastewater Substances 0.000 description 10
- 239000011701 zinc Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 238000001914 filtration Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 239000010431 corundum Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000009388 chemical precipitation Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- -1 thallium ions Chemical class 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 231100000171 higher toxicity Toxicity 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 229940046892 lead acetate Drugs 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a synthetic method of zinc metaphosphate and application thereof in removing thallium in zinc sulfate solution. According to the method, phosphoric acid and zinc oxide are used as raw materials and are mixed according to a certain proportion, the mixture is roasted at the temperature of 100-500 ℃ for 2-10 h to obtain zinc metaphosphate agglomerates, the agglomerates are crushed and screened to obtain zinc metaphosphate powder, the zinc metaphosphate powder is added with zinc powder and water to be mixed into a zinc sulfate solution, the mixture is stirred at the temperature of 30-70 ℃ for 1-5 h, and then thallium-removing slag and qualified liquid are obtained through separation by a filter press. The method has the advantages of simple process, low cost, good thallium removal effect and easy connection with the existing production process.
Description
Technical Field
The invention relates to a synthetic method of zinc metaphosphate and application thereof in thallium removal of zinc sulfate solution, belonging to the technical field of chemical smelting and wastewater treatment.
Background
Thallium is a highly toxic element, has higher toxicity than heavy metals with strong toxicity such as cadmium, mercury, lead and the like, has stronger bioaccumulation, and has great threat to human bodies and ecological environment. The exploitation and utilization of mineral resources expose the minerals to the earth surface, and the Tl in the minerals is easily released and causes harm to the environment.
At present, scholars at home and abroad carry out a great deal of research on the removal process of the metal thallium, and the method mainly comprises a chemical precipitation method, an adsorption method, an ion exchange method, an extraction method and the like. The chemical precipitation method is the most studied method at present, and is divided into a sulfide precipitation method and a hydrolysis precipitation method according to the precipitation principle. Patents CN104445732A and CN104445733A adopt a sulfurization precipitation method to treat thallium-containing wastewater, the method has a good thallium removal effect, but two-stage treatment results in a longer process flow, more reagents are added, and the amount of slag is larger. In patent CN112981124a, a hydrolysis precipitation method is adopted, thallium in wastewater is oxidized first, and wastewater is adjusted to be alkaline, so that trivalent thallium is hydrolyzed and precipitated, thereby removing and enriching thallium. While CN106517587A combines two precipitation methods to remove thallium, firstly adjusts the pH value of the wastewater to hydrolyze and precipitate trivalent thallium, and then adds industrial sodium sulfate to sulfide and precipitate monovalent thallium, thereby reducing the use of oxidant, but not suitable for wastewater with high acidity.
In addition to the chemical precipitation method, the adsorption method and the ion exchange method have been studied more. In patent CN107381926A, thallium is adsorbed by magnet powder, and wastewater is adjusted to be alkaline; CN109607599A and CN109850935A adopt an ion exchange method to purify thallium wastewater, firstly thallium ions in the wastewater are oxidized to obtain trivalent thallium ions, and then resin is used for adsorption.
In the zinc hydrometallurgy process, thallium has adverse effect on the zinc electrodeposition process, and the problem of plate burning is easily caused. In patent CN1780923A, zinc powder is used for replacing thallium ions in a zinc sulfate solution; CN109957668A and CN104894373A are disclosed in the patent, which are characterized in that 200-800 g/L lead acetate solution is added in the purification process of zinc sulfate solution to remove thallium, so that the cost is high. Therefore, the development of the process for economically and efficiently purifying and removing the thallium from the zinc sulfate solution has important significance for ensuring the stable operation of a zinc electrodeposition system.
Disclosure of Invention
Aiming at the problems in the background art, the invention provides a synthetic method of zinc metaphosphate and application thereof in removing thallium from a zinc sulfate solution. Has the advantages of strong adaptability of raw materials, simple process flow, good thallium removal effect and low cost.
The purpose of the invention is realized by the following technical scheme:
a synthetic method of zinc metaphosphate and application thereof in zinc sulfate solution thallium removal are disclosed, wherein zinc oxide and phosphoric acid are used as raw materials, zinc metaphosphate is firstly mixed, stirred and uniformly mixed, then the zinc metaphosphate is synthesized in a roasting furnace, the roasting temperature is 100-500 ℃, the roasting time is 2-10 h, a zinc metaphosphate block is obtained after roasting, zinc metaphosphate with the granularity smaller than 100 meshes is obtained after further crushing and screening, zinc powder and water are added into the zinc metaphosphate to be mixed and slurried to form zinc powder slurry, the zinc powder slurry is added into a thallium-containing sulfuric acid solution, thallium removal is stirred and replaced at 30-70 ℃, qualified thallium removal liquid and thallium removal slag are obtained after replacement and separation, the thallium removal liquid can be directly electrolyzed by electricity, the thallium removal slag can be further processed after washing, and heavy metals in the thallium removal liquid are recovered.
The method scientifically designs production steps, and has smooth connection of all procedures and good thallium removal effect. The method comprises the steps of preparing zinc metaphosphate at first, enabling zinc oxide to react with phosphoric acid to generate the zinc metaphosphate through roasting synthesis, mixing the zinc metaphosphate with zinc powder and water to obtain slurry, adding the slurry into a zinc sulfate solution to carry out displacement and thallium removal, and separating after displacement to obtain qualified liquid and thallium removal slag. The process has the advantages of no waste water and waste residue discharge, simple process flow, thorough thallium removal and low cost.
Preferably, the addition amount of the phosphoric acid is 3~5 times, the roasting temperature is 200 to 400 ℃, and the roasting time is 2 to 8 hours.
Preferably, the granularity of the zinc metaphosphate powder is less than 150 meshes.
Preferably, the content of the zinc powder in the size mixing liquid is 40-80%, and the adding amount of the zinc metaphosphate is 0.5-3% of the zinc powder. More preferably, the zinc powder content in the slurry is 50 to 70 percent, and the zinc metaphosphate is 1~2 percent of the zinc powder.
Preferably, the adding amount of the zinc powder slurry is 0.5 to 3g/L, the stirring temperature is 30 to 60 ℃, and the time is 1 to 3 hours.
Preferably, the synthesis method of the zinc metaphosphate and the application thereof in thallium removal comprise the following main steps:
s1, synthesis and preparation: zinc oxide and phosphoric acid are used as raw materials, the raw materials are mixed and uniformly mixed to obtain mixed slurry, the adding amount of the phosphoric acid is 3~6 times of the amount of the zinc oxide, the slurry is roasted in a roasting furnace to synthesize zinc metaphosphate, the roasting temperature is 100-500 ℃ in the roasting process, and the roasting time is 2-10 hours.
S2, crushing and size mixing: pouring the zinc metaphosphate agglomerate out of the roasting furnace, crushing the zinc metaphosphate agglomerate in a crusher, sieving the crushed powder to obtain zinc metaphosphate with the granularity of less than 100 meshes, mixing the zinc metaphosphate agglomerate with zinc powder, pouring the mixture into a size mixing tank, adding water or a thallium-containing solution into the size mixing tank, and obtaining zinc powder slurry with the solid content of 30-80 percent.
S3, stirring and sinking thallium: pouring zinc powder slurry with solid content of 40-80% into a thallium-containing zinc sulfate solution, adding the slurried zinc powder at 0.5-5 g/L, stirring the solution at 30-60 ℃ for 1-5 h, precipitating and filtering after the reaction is finished, and directly sending the solution to zinc electrodeposition.
The technical scheme of the invention takes zinc oxide and phosphoric acid as raw materials to prepare the zinc metaphosphate, and has the advantages of high production efficiency, low-temperature operation, simple process and the like. The following reactions mainly occur in the process:
ZnO+2H 3 PO 4 = Zn(PO 3 ) 2 +3H 2 O(g) (1)
in the thallium removal process, a zinc thallium replacement reaction mainly occurs, the zinc powder dispersion effect is enhanced by introducing zinc phosphate, and meanwhile, new impurities are not introduced, so that the purity of the system is controlled, and the occurrence reaction is as follows:
Zn + 2Tl + = Zn 2+ + 2Tl (2)
Zn + Tl 3+ = Zn 2+ + Tl + (3)
3Zn + 2Tl 3+ = 3Zn 2+ + 2Tl (4)
preferably, the adding amount of the phosphoric acid in the step S1 is 3~5 times of zinc oxide, the baking temperature is 200-400 ℃, and the baking time is 2-8 hours.
Preferably, the granularity of the zinc metaphosphate powder in the step S2 is less than 150 meshes, and the addition amount of the zinc metaphosphate powder is 0.5-2% of the zinc powder.
Preferably, the solid content of the slurry in the step S2 is 50-80%.
Preferably, the adding amount of the zinc powder in the step S3 is 0.5 to 5 g/L, the replacement temperature is 30 to 60 ℃, and the time is 1 to 3 hours.
The invention has the beneficial effects that:
(1) The zinc metaphosphate is obtained by roasting synthesis, the synthesis temperature is low, no waste slag and waste gas are generated, and the zinc metaphosphate is clean and environment-friendly.
(2) The zinc powder and the zinc metaphosphate are mixed and size-mixed, so that powder agglomeration is reduced, powder dispersion is facilitated, and the thallium removal efficiency of the zinc powder is improved.
(3) The zinc metaphosphate is used as a dispersing agent, the dispersing effect is good, and the zinc metaphosphate is mixed with zinc powder to remove thallium, so that secondary pollution of impurity ions to a zinc sulfate solution is eliminated.
(4) The method uses zinc powder to replace and remove thallium, is suitable for acidic solutions, and can reduce the concentration of partial heavy metal impurity ions in the thallium removal process.
(5) The method scientifically designs production steps, has smooth connection of all procedures and stable thallium removal effect, and does not introduce new impurity ions into the solution. No waste water and waste residue are discharged, and the method has the advantages of strong raw material adaptability, simple process flow, good thallium removal effect, cleanness and environmental protection.
Drawings
FIG. 1 is a process flow diagram of the method of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
This example is a method for synthesizing zinc metaphosphate and its application in removing thallium from zinc sulfate solution, and the process flow diagram is shown in fig. 1.
The components of the thallium-containing zinc sulfate solution used as the test raw materials are as follows: zn 154.8g/L, tl 3.6mg/L, pH =4.5.
The specific steps of the embodiment are as follows:
s1, synthesis and preparation: weighing 5g of zinc oxide and 15g of phosphoric acid, pouring the zinc oxide and the phosphoric acid into a corundum crucible, stirring and mixing uniformly, putting the crucible into a muffle furnace for roasting, setting the temperature at 200 ℃, cooling to room temperature after roasting for 8 hours, and pouring out the solid in the crucible to obtain the compound with the weight of 16.28 g.
S2, crushing and size mixing: putting the zinc metaphosphate lumps into a crusher for crushing, and sieving all crushed powder through a 150-mesh sieve; 15g of zinc powder and 0.375g of zinc metaphosphate powder are weighed and poured into an agate mortar to be mixed evenly, and 4ml of distilled water is poured to be mixed to obtain zinc powder slurry with the solid content of 77.42 percent.
S3, stirring and sinking thallium: 1000ml and 3g/L of zinc powder slurry are added into the thallium-containing zinc sulfate solution raw material, the mixture is stirred for 2 hours in a water bath kettle with the constant temperature of 60 ℃, after the reaction is finished, filtration and separation are carried out, 2.31g of thallium precipitation slag is obtained, a thallium removal liquid 983 ml is obtained, the thallium content is analyzed to be 0.33 mg/L, and the thallium removal rate is calculated to be 90.83%.
Example 2
This example is a method for synthesizing zinc metaphosphate and its application in removing thallium from zinc sulfate solution, and the process flow diagram is shown in fig. 1.
The components of the thallium-containing solution as the test raw material were: zn 154.8g/L, tl 3.0.0 mg/L, pH =4.5.
The specific steps of the embodiment are as follows:
s1, synthesis and preparation: weighing 5g of zinc oxide and 25g of phosphoric acid, pouring the zinc oxide and the phosphoric acid into a corundum crucible, stirring and mixing uniformly, putting the crucible into a muffle furnace for roasting, setting the temperature at 500 ℃, cooling to room temperature after roasting for 2 hours, and pouring out the solid in the crucible to obtain 25.11g of the composite.
S2, crushing and size mixing: putting the zinc metaphosphate cake into a crusher for crushing, and sieving all crushed powder by a 100-mesh sieve; 15g of zinc powder and 0.25g of zinc metaphosphate powder are weighed and poured into an agate mortar to be mixed evenly, and 8ml of distilled water is poured to be mixed to obtain zinc powder slurry with the solid content of 64.51 percent.
S3, stirring and sinking thallium: 1000ml of the thallium-containing zinc sulfate solution raw material is taken, 3g/L zinc powder slurry is added into the thallium-containing zinc sulfate solution raw material, 2h is stirred in a water bath kettle with the constant temperature of 50 ℃, after the reaction is finished, filtration and separation are carried out, thallium precipitation slag 1.96 g is obtained, thallium removal liquid 984 ml is obtained, the thallium content is analyzed to be 0.29 mg/L, and the thallium removal rate is calculated to be 91.94%.
Example 3
This example is a method for synthesizing zinc metaphosphate and its application in removing thallium from zinc sulfate solution, and the process flow diagram is shown in fig. 1.
The thallium-containing solution used as the test raw material comprises the following components: zn 154.8g/L, tl 3.0.0 mg/L, pH =4.5.
The specific steps of this example are as follows:
s1, synthesis and preparation: weighing 5g of zinc oxide and 30g of phosphoric acid, pouring the zinc oxide and the phosphoric acid into a corundum crucible, stirring and mixing uniformly, putting the crucible into a muffle furnace for roasting, setting the temperature at 400 ℃, cooling to room temperature after roasting for 5 hours, and pouring out the solid in the crucible to obtain the compound with the weight of 16.17g.
S2, crushing and size mixing: putting the zinc metaphosphate cake into a crusher for crushing, and sieving all crushed powder through a 200-mesh sieve; 15g of zinc powder and 0.1g of zinc metaphosphate powder are weighed and poured into an agate mortar to be mixed evenly, and 10ml of distilled water is poured to be mixed to obtain the zinc powder slurry with the solid content of 59.76 percent.
S3, stirring and sinking thallium: 1000ml and 1g/L of zinc powder slurry are added into the raw material of the thallium-containing zinc sulfate solution, the raw material is stirred for 4 h in a water bath kettle with the constant temperature of 40 ℃, after the reaction is finished, filtration and separation are carried out, thallium precipitation slag 0.58 g and thallium removal liquid 993 ml are obtained, the thallium content is analyzed to be 0.82 mg/L, and the thallium removal rate is calculated to be 77.22%.
Example 4
This example is a method for synthesizing zinc metaphosphate and its application in removing thallium from zinc sulfate solution, and the process flow diagram is shown in fig. 1.
The components of the thallium-containing solution as the test raw material were: zn 154.8g/L, tl 3.0.0 mg/L, pH =4.5.
The specific steps of the embodiment are as follows:
s1, synthesis preparation: weighing 5g of zinc oxide and 20g of phosphoric acid, pouring the zinc oxide and the phosphoric acid into a corundum crucible, stirring and mixing uniformly, putting the crucible into a muffle furnace for roasting, setting the temperature at 300 ℃, cooling to room temperature after roasting for 5 hours, and pouring out the solid in the crucible to obtain the compound with the weight of 16.17g.
S2, crushing and size mixing: putting the zinc metaphosphate cake into a crusher for crushing, and sieving all crushed powder by a 100-mesh sieve; 15g of zinc powder and 0.15g of zinc metaphosphate powder are weighed and poured into an agate mortar to be mixed evenly, and 15ml of distilled water is poured to be mixed to obtain zinc powder slurry with the solid content of 49.75 percent.
S3, stirring and sinking thallium: 1000ml of the thallium-containing zinc sulfate solution raw material is taken, 3g/L zinc powder slurry is added into the thallium-containing zinc sulfate solution raw material, the mixture is stirred in a water bath kettle with the constant temperature of 50 ℃ for 3 hours, filtration and separation are carried out after the reaction is finished, 1.48g of thallium precipitation slag is obtained, 995ml of solution after thallium removal is analyzed, the thallium content is 0.47mg/L, and the thallium removal rate is calculated to be 86.94%.
Example 5
This example is a method for removing thallium from zinc metaphosphate, and the process flow chart is shown in fig. 1.
The components of the thallium-containing solution as the test raw material were: zn 154.8g/L, tl 3.0.0 mg/L, pH =4.5.
The specific steps of the embodiment are as follows:
s1, synthesis and preparation: weighing 5g of zinc oxide and 15g of phosphoric acid, pouring the zinc oxide and the phosphoric acid into a corundum crucible, stirring and mixing uniformly, putting the crucible into a muffle furnace for roasting, setting the temperature at 150 ℃, cooling to room temperature after roasting for 8 hours, and pouring out the solid in the crucible to obtain 16.02g of the composite.
S2, crushing and size mixing: putting the zinc metaphosphate lumps into a crusher for crushing, and sieving all crushed powder through a 150-mesh sieve; 15g of zinc powder and 0.40g of zinc metaphosphate powder are weighed and poured into an agate mortar to be uniformly mixed, and 25ml of distilled water is poured to be mixed to obtain zinc powder slurry with the solid content of 42.37 percent.
S3, stirring and sinking thallium: 1000ml of the raw material of the thallium-containing zinc sulfate solution is taken, 4g/L zinc powder slurry is added into the raw material, the raw material is stirred in a water bath kettle with the constant temperature of 30 ℃ for 5 hours, after the reaction is finished, filtration and separation are carried out to obtain 1.33g of thallium precipitation slag, 994ml of solution after thallium removal is obtained, the thallium content is analyzed to be 0.28 mg/L, and the calculated thallium removal rate is 92.22%.
Claims (7)
1. A synthetic method of zinc metaphosphate and application thereof in removing thallium in zinc sulfate solution are characterized by comprising the following steps:
mixing phosphoric acid and zinc oxide serving as raw materials according to a certain proportion, roasting at 100-500 ℃, obtaining zinc metaphosphate lumps after roasting, crushing and sieving to obtain zinc metaphosphate powder, adding the zinc metaphosphate powder into zinc powder and water, then mixing to form zinc powder slurry, adding the zinc powder slurry into a thallium-containing zinc sulfate solution to perform thallium removal reaction, and then separating by a filter press to obtain thallium removal slag and a liquid after thallium removal.
2. The method for synthesizing zinc metaphosphate according to claim 1 and its application in removing thallium from zinc sulfate solution are characterized in that: the raw materials for synthesizing the zinc metaphosphate comprise phosphoric acid and zinc oxide, and the addition amount of the phosphoric acid is 3~6 times of the mass of the zinc oxide.
3. The method for synthesizing zinc metaphosphate according to claim 1 and its application in removing thallium from zinc sulfate solution are characterized in that: the baking time is 2 to 10 hours.
4. The method for synthesizing zinc metaphosphate and its application in removing thallium from zinc sulfate solution according to claim 1, characterized by that: the granularity of the zinc metaphosphate powder is less than 100 meshes.
5. The method for synthesizing zinc metaphosphate according to claim 1 and its application in removing thallium from zinc sulfate solution are characterized in that: the zinc powder slurry contains 40-80% of zinc powder, and the addition amount of zinc metaphosphate is 0.5-3% of the mass of the zinc powder.
6. The method for synthesizing zinc metaphosphate according to claim 1 and its application in removing thallium from zinc sulfate solution are characterized in that: the adding amount of the zinc powder slurry is 0.5-5 g/L.
7. The method for synthesizing zinc metaphosphate and its application in removing thallium from zinc sulfate solution according to claim 1, characterized by that: the reaction temperature of the thallium removal reaction is 30 to 70 ℃, and the reaction time of the thallium removal reaction is 1 to 5 hours.
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| CN1761616A (en) * | 2003-03-14 | 2006-04-19 | 日本化学工业株式会社 | High purity metaphosphate and method for production thereof |
| WO2013045905A1 (en) * | 2011-09-30 | 2013-04-04 | Faradion Ltd | Condensed polyanion electrode |
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| CN114042920A (en) * | 2021-11-16 | 2022-02-15 | 苏州铂韬新材料科技有限公司 | Superfine flaky zinc powder and preparation process thereof |
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| CN1761616A (en) * | 2003-03-14 | 2006-04-19 | 日本化学工业株式会社 | High purity metaphosphate and method for production thereof |
| WO2013045905A1 (en) * | 2011-09-30 | 2013-04-04 | Faradion Ltd | Condensed polyanion electrode |
| CN105504384A (en) * | 2016-01-27 | 2016-04-20 | 江苏爱特恩东台新材料科技有限公司 | Zinc oxide special for natural rubber and preparation method of zinc oxide |
| CN114042920A (en) * | 2021-11-16 | 2022-02-15 | 苏州铂韬新材料科技有限公司 | Superfine flaky zinc powder and preparation process thereof |
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