CN112538568B - Method for removing fluorine and chlorine in zinc oxide powder by low-temperature roasting and water washing - Google Patents
Method for removing fluorine and chlorine in zinc oxide powder by low-temperature roasting and water washing Download PDFInfo
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
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Abstract
The invention provides a method for removing fluorine and chlorine in zinc oxide powder by low-temperature roasting and water washing, which comprises the following steps: respectively grinding zinc oxide powder and sodium carbonate, and mixing the obtained mixture according to the weight ratio of zinc oxide powder: carbonate =1: 0.1-1 mass ratio; uniformly mixing the ingredients, and roasting at 150-500 ℃ for 0.5-4 h; and (3) carrying out water solution agitation leaching on the roasted material at the temperature of 25-90 ℃, wherein the leaching time is 0.5-4 h, filtering to obtain zinc oxide powder without fluorine and chlorine and fluorine-containing chlorine filtrate, and recycling the fluorine-containing chlorine filtrate after fluorine and chlorine removal and purification. The method can realize the high-efficiency removal of fluorine and chlorine in the zinc oxide powder, has the fluorine removal rate of more than 95 percent and the chlorine removal rate of more than 95 percent, and has the advantages of high fluorine and chlorine removal rate, simple and convenient operation of the process, low energy consumption, low cost of raw materials, no pollution to the environment, cyclic utilization of aqueous solution and the like.
Description
Technical Field
The invention belongs to the field of non-ferrous metal smelting and secondary resource recovery, relates to a method for removing fluorine and chlorine, and particularly relates to a method for removing fluorine and chlorine in zinc oxide powder by low-temperature roasting and water washing.
Background
The zinc oxide powder is the smoke dust collected in the process of smelting lead and zinc by a pyrogenic process, is an important secondary resource and mainly comes from zinc concentrate boiling roasting smoke dust, zinc smelting slag rotary kiln volatilization smoke dust, lead pyrometallurgical smelting smoke dust, steel smelting waste galvanized sheet smoke dust and secondary resource pyrogenic process volatilization treatment smoke dust. The zinc oxide powder has higher zinc content and can be used as a main raw material for neutral leaching in zinc hydrometallurgy for zinc recovery. It is worth noting that although the valuable metal zinc in the zinc oxide powder has high recovery value, harmful elements such as fluorine and chlorine are accompanied, and the content of fluorine and chlorine is 0.2% -0.5% and 0.3% -3.5% respectively. If the zinc electrowinning process is not directly put into a leaching system for fluorine and chlorine removal, the concentration of fluorine and chlorine in the zinc electrowinning system exceeds the standard, and great adverse effect is generated on the subsequent zinc electrowinning process, which is mainly shown as follows: the fluorine ions destroy an aluminum oxide film on the surface of the cathode aluminum plate, so that the surface and the precipitated zinc form a zinc-aluminum alloy which is bonded, the zinc sheet is difficult to peel off, and the cathode aluminum plate is consumed; chloride ions are oxidized into chlorate at the anode and react with the anode lead plate, so that lead enters the solution and is separated out at the cathode part, and the product quality is reduced. In addition, when the concentration of fluorine and chlorine reaches a certain amount, toxic and harmful gases are generated in an acid environment, and the field operation environment is influenced. Therefore, it is necessary to remove fluorine and chlorine in the zinc oxide powder in a suitable manner.
In general, the removal method of fluorine and chlorine in zinc oxide powder is mainly divided into two methods:
1. a roasting method. The fire roasting is mainly to decompose the fluoride and chloride in the material at a certain high temperature and under a certain negative pressure and volatilize and remove the fluoride and chloride. The method has the advantages of simple flow, high removal rate, stable operation, large treatment capacity and suitability for materials containing simple chlorides and fluorides; the defects are that the roasting temperature is higher (500-800 ℃), and the zinc raw material with higher fluorine and chlorine content, especially the high-lead material, is easy to agglomerate in the roasting process and needs to be cleaned regularly; and the fluorine-chlorine-containing flue gas generated in the roasting process needs to be leached into the solution, and then fluorine and chlorine are removed.
2. And (4) wet processing. The wet method is mainly an alkali washing method, wherein, the fluorine and the chlorine can be eluted into the solution by the reaction of simple zinc fluoride, zinc chloride and the like in the solution by adopting sodium hydroxide or sodium carbonate, and then the solution is subjected to wastewater treatment by adopting purification and iron precipitation, cuprous dechlorination, lime defluorination and the like. The caustic washing operation is generally carried out industrially using sodium carbonate. The method has the advantages of simple process, easy operation and higher fluorine and chlorine removal rate of the zinc oxide powder containing simple fluoride and chloride; the defects are that the raw material applicability is not strong, the removal rate of the materials containing complex fluorochlorohydrin phases (such as basic zinc fluoride, basic zinc chloride and the like) is low, and the amount of waste water generated in alkali washing is large.
3. A combined roasting-alkali washing method. The method mainly adopts a roasting method, firstly volatilizes most of fluorine-containing chlorine compounds, simultaneously decomposes a small amount of fluorine-containing chlorine compounds which are difficult to volatilize, and then elutes the fluorine-containing chlorine into a solution by combining with an alkali washing method. Compared with a roasting method or a wet method which is adopted independently, the method has the advantages of strong applicability to raw material treatment and high fluorine and chlorine removal rate; the disadvantages are longer flow and still higher energy consumption.
Of course, when zinc oxide powder materials are specifically treated, a corresponding recovery technical route needs to be established according to the phase properties of the materials and the current production situation of enterprises. Therefore, it is imperative to find a method for economically, reasonably and efficiently removing fluorine and chlorine from zinc oxide powder with different material properties.
Disclosure of Invention
Aiming at the technical defects in the existing process for removing fluorine and chlorine from zinc oxide powder, the invention aims to provide a method for removing fluorine and chlorine from zinc oxide powder by low-temperature roasting and water washing, which realizes the high-efficiency removal of fluorine and chlorine in zinc oxide powder, the removal rate of fluorine is more than 95%, the removal rate of chlorine is more than 95%, and the removal rate of fluorine and chlorine is greatly improved. The process is simple and convenient to operate, low in energy consumption, low in raw material cost and free of pollution to the environment, and meets the requirements of current green metallurgy on clean production.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for removing fluorine and chlorine in zinc oxide powder by low-temperature roasting and water washing, which comprises the following steps:
1) Respectively grinding the zinc oxide powder and the carbonate until the granularity is-200 to-400 meshes, and mixing the zinc oxide powder: carbonate =1: 0.1-1 mass ratio;
2) Uniformly mixing the ingredients in the step 1), and roasting at 150-500 ℃ for 0.5-4 h to obtain roasted sand;
3) Carrying out aqueous solution agitation leaching on the calcine in the step 2), wherein the leaching temperature is 25-90 ℃; the leaching time is 0.5-4 h, and the solid-to-liquid ratio (g/mL) is 1; filtering to obtain zinc oxide powder without fluorine and chlorine and fluorine-chlorine-containing water washing liquid; the fluorine-containing chlorine water washing liquid can be recycled after fluorine and chlorine removal and purification.
Preferably, the mass ratio of the zinc oxide powder to the carbonate in the step 1) is 1.
Preferably, the carbonate in step 1) is one or more of sodium carbonate, potassium carbonate and ammonium carbonate.
Preferably, the roasting in the step 2) is carried out at 200-400 ℃ for 2-4 h.
Preferably, the calcine in the step 3) is leached by stirring at 50-70 ℃, the leaching time is 0.5-2 h, and the solid-to-liquid ratio (g/mL) is 1.
The method can be applied to the zinc oxide powder containing simple fluoride and chloride, in particular to the zinc oxide powder containing complex fluorine-chlorine phases (such as basic zinc fluoride, basic zinc chloride and the like).
The principle involved therein mainly has the following aspects: taking basic zinc fluoro (chloro) fluoride as an example, the molecular formula is Zn 5 (OH) 8 (F,Cl) 2 ·H 2 O, which belongs to transition metal layered hydroxylate and is insoluble in water. According to the properties of the zinc oxide powder, fluorine and chlorine are difficult to enter the solution due to the reaction of the zinc oxide powder and the carbonate solution, and only a small amount of fluorine-containing chlorine compounds in the zinc oxide powder can be removed by a conventional alkali washing method, and basic zinc fluoro (chloro) chloride cannot be decomposed.
When the high-temperature roasting method is adopted, the high temperature (500-800 ℃) can promote the thermal decomposition to generate ZnO, HCl and HF. The production of HCl and HF can pollute the operating environment. The main reaction equation is shown in formula 1.
Zn 5 (OH) 8 (F,Cl) 2 ·H 2 O→5ZnO+2H(F,Cl)+4H 2 O (formula 1)
By adopting a low-temperature roasting method, the following reactions mainly occur, as shown in formula 2:
Zn 5 (OH) 8 (F,Cl) 2 ·H 2 O→4Zn(OH) 2 +Zn(F,Cl) 2 +H 2 o (formula 2)
By controlling the reaction temperature to be 200-400 ℃, on one hand, the addition of the carbonate promotes the decomposition of the basic zinc fluoride (chloride) and promotes the basic zinc fluoride (chloride) to be converted into zinc hydroxide and zinc fluoride (chloride); on the other hand, the generation of HCl and HF is inhibited by the carbonate, and the problem of volatilization pollution of HCl and HF in the high-temperature roasting process is solved; on the other hand, when the roasted material is washed by water, zinc fluoride (chloride) generated by low-temperature roasting can react with the residual carbonate, so that the fluorine (chloride) enters the solution, and the zinc is converted into zinc carbonate precipitate, thereby realizing the removal of fluorine and chlorine in the zinc oxide powder. The zinc hydroxide, the zinc carbonate and the zinc oxide can be jointly converted into zinc sulfate in the subsequent zinc smelting process and then enter an electrodeposition system, so that the zinc content is not lost while fluorine and chlorine are removed, and the whole zinc smelting process is not influenced.
The invention has the beneficial effects that:
the invention provides a method for removing fluorine and chlorine in zinc oxide powder by combining low-temperature roasting and water washing, which can realize the decomposition of complex fluorine-chlorine-containing phases (such as basic zinc fluoride, basic zinc chloride and the like) into simple fluorine-chlorine compounds by adding carbonate into the zinc oxide powder and roasting at a low temperature (200-400 ℃), simultaneously inhibit the volatilization of fluorine and chlorine into smoke, solve the problem of smoke pollution and save the leaching operation; moreover, the low temperature can inhibit the generation of zinc ferrite, thereby reducing the difficulty of recovering zinc from zinc oxide powder; the roasted product obtained after roasting is simply washed, so that most of fluorine and chlorine can be removed, the removal rate of fluorine is more than 95%, the removal rate of chlorine is more than 95%, and the removal effect of fluorine and chlorine is obvious; the method has the advantages of wide sources of the required raw material carbonate, low cost, easy operation of experiments, low requirement on equipment, environmental friendliness and capability of meeting the requirements of green metallurgy and solid waste recycling on clean production.
Drawings
FIG. 1 is a process flow diagram of the removal of fluorine and chlorine in zinc oxide powder by low-temperature roasting combined with water washing.
Detailed Description
The invention is described in detail below with reference to the figures and the embodiments. The following examples are only illustrative of the present invention, and the scope of the present invention shall include the full contents of the claims, not limited to the examples. Variations can be made within the knowledge of those skilled in the art without departing from the spirit of the invention.
Example 1
The process flow is shown in figure 1. The zinc oxide powder used in the experiment is from a lead-zinc smelting plant in Baoshan Yunnan, and is subjected to chemical element analysis and detection, wherein the zinc content is 51%, the fluorine content is 0.24%, and the chlorine content is 3.22%, and the detection result shows that the chlorine-containing phase is mainly basic zinc chloride (accounting for 90%), and the fluorine-containing phase is mainly basic zinc fluoride (accounting for about 70%). Respectively grinding 100g of zinc oxide powder and 10g of ammonium carbonate until the granularity is-200 meshes, uniformly mixing in a crucible, placing in a muffle furnace, and roasting at 200 ℃ for 3 hours to obtain roasted sand; placing the calcine into an aqueous solution for agitation leaching, wherein the leaching temperature is 50 ℃, the leaching time is 1h, and the solid-to-liquid ratio (g/mL) is 1; and after the stirring leaching is finished, carrying out solid-liquid separation to obtain the zinc oxide powder after the fluorine and chlorine removal and a filtrate. And weighing the zinc oxide powder after the fluorine and chlorine removal, detecting the fluorine and chlorine content in the zinc oxide powder, and calculating the fluorine and chlorine removal rate.
The removal rate of fluorine was calculated to be 95.12%, and the removal rate of chlorine was calculated to be 96.96%.
Example 2
The process flow is shown in figure 1. The zinc oxide powder used in the experiment is from a certain lead-zinc smelting plant in Baoshan Yunnan, and the lead-zinc smelting plant is subjected to chemical element analysis and detection, wherein the zinc content is 51%, the fluorine content is 0.24%, and the chlorine content is 3.22%, and the detection on the chlorine-containing phase shows that the chlorine-containing phase is mainly basic zinc chloride (accounting for 90%), and the fluorine-containing phase is mainly basic zinc fluoride (accounting for about 70%). Respectively grinding 100g of zinc oxide powder and 15g of potassium carbonate until the granularity is-200 meshes, uniformly mixing in a crucible, placing in a muffle furnace, and roasting at 300 ℃ for 3 hours to obtain roasted sand; placing the calcine in an aqueous solution for agitation leaching, wherein the leaching temperature is 60 ℃, the leaching time is 1.5h, and the solid-to-liquid ratio (g/mL) is 1; and after the agitation leaching is finished, carrying out solid-liquid separation to obtain the zinc oxide powder after the fluorine and chlorine removal and filtrate. And weighing the zinc oxide powder after the fluorine and chlorine removal, detecting the fluorine and chlorine content in the zinc oxide powder, and calculating the fluorine and chlorine removal rate.
The removal rate of fluorine was calculated to be 96.01% and the removal rate of chlorine was calculated to be 97.22%.
Example 3
The process flow is shown in figure 1. The zinc oxide powder used in the experiment is from a certain lead-zinc smelter in Baoshan Yunnan, and the lead-zinc smelter is subjected to chemical element analysis and detection, wherein the zinc content is 51%, the fluorine content is 0.24%, and the chlorine content is 3.22%, and the detection on the chlorine-containing phase shows that the chlorine-containing phase is mainly basic zinc chloride (about 90%), and the fluorine-containing phase is mainly basic zinc fluoride (about 70%). Respectively grinding 100g of zinc oxide powder and 20g of sodium carbonate until the granularity is-200 meshes, uniformly mixing in a crucible, placing in a muffle furnace, and roasting at 400 ℃ for 2h to obtain roasted sand; placing the calcine into an aqueous solution for agitation leaching, wherein the leaching temperature is 70 ℃, the leaching time is 2 hours, and the solid-to-liquid ratio (g/mL) is 1; and after the stirring leaching is finished, carrying out solid-liquid separation to obtain the zinc oxide powder after the fluorine and chlorine removal and a filtrate. And weighing the zinc oxide powder after the fluorine and chlorine removal, detecting the fluorine and chlorine content in the zinc oxide powder, and calculating the fluorine and chlorine removal rate.
The removal rate of fluorine was calculated to be 96.77% and the removal rate of chlorine was calculated to be 97.63%.
From the above examples, it can be seen that the method for removing fluorine and chlorine from zinc oxide powder by low-temperature roasting combined with water washing provided by the invention realizes high-efficiency removal of fluorine and chlorine in zinc oxide powder, the removal rate of fluorine and chlorine is above 95%, and the removal rate of fluorine and chlorine is greatly improved. The process is simple and convenient to operate, low in energy consumption, low in raw material cost and free of environmental pollution, and meets the requirements of current green metallurgy on clean production.
The invention has not been described in detail and is part of the common general knowledge of a person skilled in the art.
Claims (5)
1. A method for removing fluorine and chlorine in zinc oxide powder by low-temperature roasting and water washing is characterized by comprising the following steps:
1) Respectively grinding the zinc oxide powder and the carbonate until the granularity is-200 to-400 meshes, and mixing the zinc oxide powder: carbonate =1: 0.1-1 mass ratio;
2) Uniformly mixing the ingredients in the step 1), and roasting at 150-500 ℃ for 0.5-4 h to obtain roasted sand;
3) Carrying out aqueous solution stirring leaching on the calcine in the step 2), wherein the leaching temperature is 25-90 ℃; the leaching time is 0.5-4 h, and the solid-to-liquid ratio g/mL is 1; filtering to obtain zinc oxide powder without fluorine and chlorine and fluorine-chlorine-containing water washing liquid; the fluorine-chlorine-containing washing liquid can be recycled after being subjected to fluorine-chlorine removal and purification;
wherein, the phases of fluorine and chlorine in the zinc oxide powder are basic zinc fluoride (chloride).
2. The method for removing fluorine and chlorine in zinc oxide powder by low-temperature roasting and water washing as claimed in claim 1, wherein the mass ratio of the zinc oxide powder to the carbonate in the step 1) is 1.
3. The method for removing fluorine and chlorine in zinc oxide powder by low-temperature roasting and water washing combined as claimed in claim 1, wherein the carbonate in step 1) is one or more of sodium carbonate, potassium carbonate and ammonium carbonate.
4. The method for removing fluorine and chlorine in zinc oxide powder by low-temperature roasting and water washing combined as claimed in claim 1, wherein the roasting in step 2) is carried out at 200-400 ℃ for 2-4 h.
5. The method for removing fluorine and chlorine in zinc oxide powder by low-temperature roasting and water washing combined according to claim 1, wherein the roasted product in the step 3) is subjected to agitation leaching at 50-70 ℃, the leaching time is 0.5-2 h, and the solid-to-liquid ratio g/mL is 1.
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| DE19640869B4 (en) * | 1996-10-04 | 2010-08-12 | Ruhr-Zink Gmbh | Process for the recovery of valuable metals, in particular zinc, from raw materials containing chlorine or fluorine |
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| CN103924091A (en) * | 2014-04-29 | 2014-07-16 | 何宇波 | Smelting method for removing fluorine and chlorine out of fluorine-and-chlorine-containing inferior zinc oxide and enriching valuable metals |
| CN104593586B (en) * | 2014-12-19 | 2017-11-10 | 昆明理工大学 | A kind of method that microwave low-temperature bake takes off fluorine and chlorine removal with alkali wash processing zinc oxide fumes |
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