CN115161492A - Method for preparing high-grade zinc oxide by treating secondary zinc oxide in rotary kiln - Google Patents
Method for preparing high-grade zinc oxide by treating secondary zinc oxide in rotary kiln Download PDFInfo
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- CN115161492A CN115161492A CN202210792346.4A CN202210792346A CN115161492A CN 115161492 A CN115161492 A CN 115161492A CN 202210792346 A CN202210792346 A CN 202210792346A CN 115161492 A CN115161492 A CN 115161492A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/34—Obtaining zinc oxide
- C22B19/38—Obtaining zinc oxide in rotary furnaces
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/24—Obtaining zinc otherwise than by distilling with leaching with alkaline solutions, e.g. ammonia
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/02—Working-up flue dust
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Abstract
The invention belongs to the technical field of material chemistry, and particularly relates to a method for preparing high-grade zinc oxide by treating secondary zinc oxide in a rotary kiln. The method for preparing high-grade zinc oxide by treating secondary zinc oxide in the rotary kiln comprises the following steps: (1) soaking in an alkali pool; (2) depositing zinc in an acetic acid tank; (3) soaking in a water tank; and (4) calcining in a rotary kiln. The method is established on the basis of the existing rotary kiln production line, not only can the investment cost of secondary treatment not be excessively increased, but also the existing production line resources can be fully utilized, so that the economic benefit is improved while the utilization rate of the production resources of enterprises is maximized, and high value-added products are obtained.
Description
Technical Field
The invention belongs to the technical field of material chemistry, and particularly relates to a method for preparing high-grade zinc oxide by treating secondary zinc oxide in a rotary kiln.
Background
The metal zinc is mainly widely applied to the fields of automobiles, metallurgy, machinery, medicine, household appliances, batteries, military and the like in the forms of zinc oxide, zinc plating and zinc-based alloy, and has an important strategic position in national economy and national defense construction. Although China is a large zinc resource country, with the rapid development of economy in recent years, the demand of zinc is greatly increased, zinc ore resources are continuously developed and utilized, and high-grade zinc-containing ores are gradually exhausted, so that the supply capacity of domestic zinc concentrate cannot meet the industrial production demand, the condition of shortage of metal zinc supply is increasingly severe, and the cost of metal zinc is sharply increased. However, various secondary materials containing zinc, such as zinc smelting slag, copper plant ash, steel plant ash, lead-zinc tailings, low-grade zinc oxide ore and the like, are huge in quantity and difficult to treat, the treatment mode of many smelting slags is not standard, and the smelting slags are abandoned, stacked or buried at will or even directly poured on cultivated lands and hillsides, so that serious environmental pollution is caused. In fact, if the treatment mode of the zinc-containing secondary material is proper, the problem of environmental pollution can be solved, and the zinc-containing secondary material can be converted into high-value resources, so that the resource problem of zinc concentrate shortage is relieved. Therefore, the method has great significance for saving resources, protecting environment and industrial production by enhancing the reutilization of various zinc-containing secondary resources.
At present, the pyrogenic process recycling of secondary materials containing zinc mostly adopts a rotary kiln volatilization method, namely, zinc is volatilized in a zinc vapor form and enters a flue gas treatment system by means of high-temperature reduction reaction and combining with the low boiling point characteristic of zinc, so that the aim of effectively separating zinc and various valuable metals from a solid phase main body is fulfilled. The principle is that the dried zinc-containing secondary material is mixed with a reducing agent and the like and then added into a rotary kiln, zinc oxide in the zinc-containing secondary material is reduced into gaseous zinc at high temperature and enters flue gas, the gaseous zinc is oxidized in the flue gas, and finally the gaseous zinc is collected in a cooling and dust collection system in the form of zinc oxide.
The zinc hypoxide obtained by primary rotary kiln calcination reduction-oxidation-evaporation-dust collection contains 60-65% of zinc, belongs to low-grade zinc oxide, and generally contains zinc oxide, iron oxide, lead oxide, nickel, cadmium, indium and other oxides due to different raw material sources and large chemical composition fluctuation, so that the impurity content is high, and the industrial production with high purity requirements is difficult to meet.
The zinc calcine is further purified by secondary high-temperature calcination of zinc hypoxide in a rotary kiln, although the secondary high-temperature calcination can effectively decompose sulfides and chlorides in the zinc hypoxide and evaporate lead-containing compounds to obtain the zinc calcine, many impurities cannot be completely removed, such as main impurities contained in the zinc hypoxide, such as Fe, ca, al and the like, so that the content of the zinc oxide cannot reach a high-purity grade and can only reach about 85%.
Therefore, how to economically and effectively further prepare the secondary zinc oxide into high-grade zinc oxide needs to be solved urgently.
Disclosure of Invention
The invention aims to provide a method for preparing high-grade zinc oxide by treating secondary zinc oxide in a rotary kiln aiming at the problem that the secondary treatment of the secondary zinc oxide still cannot meet the high-grade requirement at present.
The technical scheme of the invention is as follows: a method for preparing high-grade zinc oxide by treating secondary zinc oxide in a rotary kiln comprises the following steps:
(1) Soaking in an alkali pool: the method comprises the following steps of (1) immersing zinc hypoxide obtained by primary calcination reduction, oxidation, evaporation and dust collection in an additional alkali pool, wherein a sodium hydroxide solution with the concentration of 5-7 mol/L is contained in the alkali pool, and stirring and immersing for 1-2 hours; the zinc oxide in the zinc hypoxide reacts with sodium hydroxide to generate sodium metazincate solution, and alkali insoluble impurities contained in the zinc hypoxide are removed by precipitation.
The dust collected in the high-temperature reduction-evaporation-oxidation-dust collection process in the existing rotary kiln production line is extremely fine and uniform in particles, and the average particle size is about 500 nanometers.
The present inventors considered that if the acid leaching method is used to dissolve the secondary zinc oxide, although the speed is high and the dissolution rate is high, the acid leaching method is used to decompose the low-grade secondary zinc oxide, which is usually accompanied by dissolution of impurity metals such as iron, manganese, copper, etc., which may have a certain effect on the final product, and although these impurity metal ions may be removed by various methods such as substitution, precipitation, addition of ammonia water, etc., the difficulty and cost of purification are undoubtedly increased. Meanwhile, in the acid leaching process, silica gel is easily generated from silicon in the zinc oxide ore, and the liquid-solid separation is seriously influenced. And the leaching rate of an ammonia water-ammonium carbonate solution system commonly used in the existing alkaline leaching is low.
However, if sodium hydroxide is adopted, zinc element is dissolved in the sodium hydroxide solution to generate sodium metazincate solution:
ZnO + H 2 O + 2NaOH → Na 2 Zn(OH) 4 。
because the secondary zinc oxide has complex components and a plurality of impurity elements, compared with a sulfuric acid solution, the sodium hydroxide solution has strong selectivity. Except that a small number of elements such as Al, si, pb, zn and the like can be dissolved in sodium hydroxide, most elements can not be dissolved in the sodium hydroxide, and except that a small number of elements such as Ca, ba and the like can not be dissolved in sulfuric acid, most elements can be dissolved in the sulfuric acid, so that the selectivity of the sodium hydroxide is stronger than that of the sulfuric acid. Compared with an ammonia solution, the sodium hydroxide solution has the advantages of high leaching efficiency, high speed, easy volatilization of ammonia, large smell and difficult management. The sodium hydroxide solution is adopted for leaching, so that the leaching efficiency is high, the leaching selectivity is strong, and no pollution is caused.
(2) Depositing zinc in an acetic acid tank: enabling the supernatant containing the sodium metatitanate obtained in the alkali tank in the step (1) to flow into an added acetic acid tank through a grid arranged in the alkali tank, wherein glacial acetic acid is contained in the acetic acid tank, and the pH value in the acetic acid tank is kept between 8 and 12; stirring and reacting for 0.5-1 h at normal temperature to generate white zinc hydroxide precipitate.
The pH value of the sodium metazincate solution is adjusted to be between 8 and 12 by adopting acetic acid, so that zinc ions in the solution are converted into zinc hydroxide precipitate. The selected acetic acid is low-melting organic acid, and contains C, O and H, and no new impurities are introduced into the system, even if littleThe subsequent high-temperature calcination can be H 2 0 and CO 2 And (4) completely decomposing.
(3) Soaking in a water tank: and (3) carrying out suction filtration on the zinc hydroxide precipitate obtained in the step (2), placing the zinc hydroxide precipitate into a water tank, stirring, and soaking for 0.5-1 h to remove sodium hydroxide impurity ions.
(4) Calcining in a rotary kiln: drying and granulating the zinc hydroxide precipitate soaked in the water tank, placing the obtained pellets in a rotary kiln for secondary calcination at the calcination temperature of 1100-1200 ℃ for 2-3 h, wherein the chlorine removal rate is not less than 97.63 percent, and obtaining the high-grade zinc oxide with the zinc oxide content of 95-98 percent.
The inventor finds that in the process design process, in the process steps of preparing the high-grade zinc oxide from the secondary zinc oxide based on the existing rotary kiln production line, the process route is simple, the process is suitable for large-scale production, and the dechlorination problem also exists. The inventor repeatedly studies to obtain: the two factors of the calcination temperature and the calcination time are mutually cooperated and have important influence on the zinc oxide content and the chlorine removal rate.
First, the inventors found that the tendency of the influence of the calcination temperature on the zinc oxide content and the chlorine removal rate was consistent, as can be seen in fig. 4. The factors of energy consumption and production cost are comprehensively considered, the calcination temperature is designed to be 1100-1200 ℃, the zinc oxide content is more than or equal to 95 percent and the chlorine removal rate is more than or equal to 97 percent in the temperature range; and at the temperature, lead element is completely removed, and a large amount of alkali insoluble substances in the zinc hypoxide are soaked and removed in an alkali pool, so that the kiln caking problem cannot occur in the calcining process at the temperature.
Then, based on the process route and the calcination temperature conditions, the inventor researches that the influence of the calcination time on the zinc oxide content and the influence on the chlorine removal rate are obviously different: when the calcination time reaches 1.5 h, the zinc oxide content still keeps growing trend along with the increase of the calcination time, and the chlorine removal rate is basically kept at a stable level along with the increase of the calcination time, as can be seen in figure 5. The inventor prefers the calcination time to be 2-3 h by integrating the production cost factor and the calcination temperature and process design.
And (2) the concentration of the sodium hydroxide solution in the alkali pool in the step (1) is 6 mol/L.
The solid-to-liquid ratio of the zinc hypoxide to the sodium hydroxide solution in the alkali pool in the step (1) is 1:20 to 25.
The water content of the pellets obtained by drying and granulating in the step (4) is 10-14%.
The grain diameter of the material ball obtained by drying and granulating in the step (4) is 8-15 mm.
The calcination temperature in the step (4) is 1150 ℃, and the calcination time is 2 h.
The invention has the beneficial effects that: compared with the existing direct secondary calcining method of the rotary kiln, the recovery rate of the zinc oxide is improved by at least 10 percent, and the purity of the zinc oxide is improved by about 18 to 25 percent. The recovery rate of zinc oxide is above 97%.
Drawings
FIG. 1 is an external view of a raw material, zinc hypoxide, in an example of the present invention.
FIG. 2 is an XRD spectrum of a raw material zinc hypoxide in an example of the present invention.
Figure 3 is an SEM topography of zinc hypoxide in an embodiment of the invention.
FIG. 4 is a graph showing the relationship between the chlorine removal rate of secondary zinc oxide, the zinc oxide content of the product and the calcination temperature.
Figure 5 is a graph of the relationship between the chlorine removal rate of secondary zinc oxide, the zinc oxide content of the product and the calcination time.
FIG. 6 is an XRD pattern of high grade zinc oxide obtained in the examples of the present invention.
FIG. 7 is an SEM image of high-grade zinc oxide obtained in the example of the invention.
FIG. 8 is an external view of high-grade zinc oxide obtained in the example of the present invention.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
The composition of the zinc oxide dust before treatment used in this example is shown in Table 1.
TABLE 1 composition of the Secondary Zinc oxide
| ZnO | Fe 2 O 3 | PbO | SiO 2 | Al 2 O 3 | CaO | Cl - | K 2 O | S 6+ |
| 76.14 | 5.43 | 3.76 | 1.15 | 0.39 | 1.01 | 4.83 | 3.15 | 1.66 |
The method for preparing high-grade zinc oxide by treating secondary zinc oxide in the rotary kiln comprises the following steps:
(1) Soaking in an alkali pool: and (2) immersing secondary zinc oxide obtained by primary calcining reduction, oxidation, evaporation and dust collection of a rotary kiln into an added alkali pool, wherein the solid-to-liquid ratio of the secondary zinc oxide to a sodium hydroxide solution in the alkali pool is 1:20. and (3) a sodium hydroxide solution with the concentration of 6 mol/L is filled in the alkali pool, the sodium hydroxide solution is stirred and soaked for 1h, zinc oxide in the secondary zinc oxide reacts with the sodium hydroxide to generate a sodium metatitanate solution, the leaching rate of the zinc reaches 96.36%, and alkali insoluble impurities contained in the secondary zinc oxide are removed by precipitation.
(2) Depositing zinc in an acetic acid tank: enabling the supernatant containing the sodium metatitanate obtained in the alkali tank in the step (1) to flow into an added acetic acid tank through a grid arranged in the alkali tank, wherein glacial acetic acid is contained in the acetic acid tank, and the pH value in the acetic acid tank is kept between 8 and 12; stirring and reacting for 0.5-1 h at normal temperature to generate zinc hydroxide white precipitate.
(3) Soaking in a water tank: and (3) carrying out suction filtration on the zinc hydroxide precipitate obtained in the step (2), placing the zinc hydroxide precipitate into a water tank, stirring, and soaking for 0.5-1 h to remove sodium hydroxide impurity ions.
(4) Calcining in a rotary kiln: drying and granulating the zinc hydroxide precipitate soaked in the water tank, wherein the water content of the obtained material ball is 10-14%, and the particle size of the material ball is 8-15 mm. And placing the obtained pellets in a rotary kiln for secondary calcination at 1150 ℃ for 2 h, wherein the chlorine removal rate is more than or equal to 97.63 percent, and obtaining high-grade zinc oxide with the zinc oxide content of 98 percent.
As can be seen from FIG. 6, the obtained high grade zinc oxide has a single pure phase and no impurity peak.
Claims (6)
1. A method for preparing high-grade zinc oxide by treating secondary zinc oxide in a rotary kiln comprises the following steps:
soaking in an alkali pool: the method comprises the following steps of (1) immersing zinc hypoxide obtained by primary calcination reduction, oxidation, evaporation and dust collection in an additional alkali pool, wherein a sodium hydroxide solution with the concentration of 5-7 mol/L is contained in the alkali pool, and stirring and immersing for 1-2 hours; reacting zinc oxide in the secondary zinc oxide with sodium hydroxide to generate a sodium metazincate solution, and removing alkali insoluble impurities contained in the secondary zinc oxide by precipitation;
(2) Depositing zinc in an acetic acid tank: enabling the supernatant containing the sodium metatitanate obtained in the alkali tank in the step (1) to flow into an added acetic acid tank through a grid arranged in the alkali tank, wherein glacial acetic acid is contained in the acetic acid tank, and the pH value in the acetic acid tank is kept between 8 and 12; stirring and reacting for 0.5-1 h at normal temperature to generate white zinc hydroxide precipitate;
(3) Soaking in a water tank: filtering the zinc hydroxide precipitate obtained in the step (2), placing the zinc hydroxide precipitate in a water tank, stirring, and soaking for 0.5-1 h to remove sodium hydroxide impurity ions;
(4) Calcining in a rotary kiln: drying and granulating the zinc hydroxide precipitate soaked in the water tank, placing the obtained pellets into a rotary kiln for secondary calcination at the calcination temperature of 1100-1200 ℃ for 2-3 h, wherein the chlorine removal rate is not less than 97.63 percent, and obtaining high-grade zinc oxide with the zinc oxide content of 95-98 percent.
2. The method for preparing high-grade zinc oxide by treating zinc hypoxide in a rotary kiln as claimed in claim 1, wherein the concentration of the sodium hydroxide solution in the alkali pool in the step (1) is 6 mol/L.
3. The method for preparing high-grade zinc oxide by treating zinc hypoxide in a rotary kiln as claimed in claim 1, wherein the solid-to-liquid ratio of the zinc hypoxide to the sodium hydroxide solution in the alkali pool in the step (1) is 1:20 to 25.
4. The method for preparing high-grade zinc oxide by treating secondary zinc oxide in a rotary kiln as claimed in claim 1, wherein the water content of the pellets obtained by drying and granulating in the step (4) is 10-14%.
5. The method for preparing high-grade zinc oxide by treating zinc hypoxide in the rotary kiln as claimed in claim 1, wherein the grain size of the pellets obtained by drying and granulating in the step (4) is 8-15 mm.
6. The method for preparing high-grade zinc oxide by treating zinc hypoxide in a rotary kiln as claimed in claim 1, wherein the calcination temperature in the step (4) is 1150 ℃ and the calcination time is 2 hours.
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| CN102092687A (en) * | 2010-09-06 | 2011-06-15 | 王嘉兴 | Method for producing zinc hydrosulfite by using sodium hydrosulfite filtration residues |
| CN102627313A (en) * | 2012-04-12 | 2012-08-08 | 广汉隆达饲料有限公司 | Wet production process for feed-grade active zinc oxide |
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| CN112744856A (en) * | 2021-01-12 | 2021-05-04 | 李发武 | Method for producing zinc oxide for ceramic glaze by using hot-dip galvanizing ash |
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2022
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| CN112744856A (en) * | 2021-01-12 | 2021-05-04 | 李发武 | Method for producing zinc oxide for ceramic glaze by using hot-dip galvanizing ash |
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