CN115874062A - Efficient acid-mixing curing leaching process for non-ferrous metal copper smelting slag - Google Patents
Efficient acid-mixing curing leaching process for non-ferrous metal copper smelting slag Download PDFInfo
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Abstract
The invention relates to a high-efficiency acid-mixing curing leaching process of nonferrous metal copper smelting slag, which comprises the following steps: s1: and (3) crushing and finely grinding the non-ferrous metal copper smelting slag. S2: and (3) mixing and stirring the concentrated acid and the crushed and finely ground nonferrous metal copper smelting slag in a mass ratio of 1. S3: and (5) placing the mixture obtained in the step (S2) into a reaction kettle, and curing to obtain clinker. S4: adding water into the clinker, stirring, and leaching for 0.5-5h to obtain a leaching solution and leaching residues. According to the method, the nonferrous metal copper smelting slag is cured by only a small amount of concentrated acid, and the valuable metal can be efficiently recovered by leaching after curing, so that the recovery rate of the valuable metal in the copper slag is improved, the acid consumption of the acid is greatly reduced, the raw materials such as hydrofluoric acid and the like which have toxicity and are difficult to recover and treat are not used, the process flow is greatly shortened, the method can be used for large-scale production, and the method has good economic benefits.
Description
Technical Field
The invention belongs to the technical field of wet metallurgy, and particularly relates to a high-efficiency acid-mixing curing leaching process for non-ferrous metal copper smelting slag.
Background
At present, valuable metal extraction resources are mainly various concentrates and the like, but the prior art for extracting valuable metals from concentrates is long in process flow, time-consuming and energy-consuming, serious in environmental pollution, high in cost and the like, and subsequent waste residues cannot be properly arranged, so that secondary pollution is easily caused, and the like. Therefore, compared with smelting from copper concentrate, the recycling of the copper smelting slag can greatly save energy consumption and reduce the stockpiling of solid wastes and the discharge of three wastes. The secondary pollution of the environment and the waste of resources can not be caused, the high-efficiency utilization of the copper smelting slag is promoted, the high-valued utilization level of the copper smelting slag is improved, the sustainable development of the resources is realized, and the economic effect is brought. The non-ferrous metal copper smelting slag is an industrial solid waste generated in the pyrometallurgical process, wherein valuable metals such as iron, silicon, magnesium, aluminum, nickel, copper, cobalt and the like are contained, and the non-ferrous metal copper smelting slag has a certain mineral utilization value. The iron and silicon contents in the non-ferrous metal copper smelting slag are higher, and SiO is used 2 The content is 25-40%, and the content of Fe is 25-45%.
The iron element in the non-ferrous metal copper smelting slag mostly exists in an iron olivine phase. Iron in the fayalite is easy to react with acid to decompose, and the decomposition of the iron can lead silicon in the fayalite to form a porous state, thereby providing convenience for the decomposition of the silicon. In addition, during the acid leaching process, elements such as nickel, copper, aluminum and the like contained in the nonferrous metal copper smelting slag can be leached together. In conclusion, the resource utilization of valuable elements in the non-ferrous metal copper smelting slag becomes possible. The resource utilization of the nonferrous metal copper smelting slag can reduce the accumulated land occupation, eliminate the environmental pollution, fully utilize valuable elements contained in the nonferrous metal copper smelting slag and have good economic, ecological and social benefits.
In the prior art, most of the processes for recycling metals from non-ferrous metal copper smelting slag are dilute acid leaching, wherein dilute acid is added into copper smelting slag to leach various metal ions contained in the copper smelting slag. However, copper smelting slag is generally in a glass state, and the glass state slag is difficult to dissolve in the dilute acid leaching process, so that the recovery rate of metals is low. For this reason, the prior art also adds hydrofluoric acid to increase the degree of dissolution of the glassy slag and improve the metal recovery rate. However, hydrofluoric acid is toxic and difficult to recover and dispose of, and can cause contamination.
The patent application with the application number of 201210587187.0 discloses a process for separating copper, zinc and iron in a leaching process of scrap copper smelting slag, wherein five selective leaching sections of the copper smelting slag are provided, the initial raw material copper smelting slag is leached respectively, then the leached slag is leached secondarily, valuable metals are extracted and separated, and then raffinate is extracted and extracted repeatedly. Although the method is simple to operate and high in valuable metal leaching rate, the method has the problems of long process section, large energy consumption, small treatment capacity and the like.
Therefore, a simpler process for recycling metal from copper smelting slag as a raw material with less pollution is needed.
Disclosure of Invention
Technical problem to be solved
In order to solve the problems of long process flow and large pollution of a metal recovery process of copper smelting slag in the prior art, the invention provides an efficient acid-mixing curing leaching process of non-ferrous metal copper smelting slag.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
an efficient acid-mixing curing leaching process for non-ferrous metal copper smelting slag comprises the following steps:
s1: crushing and finely grinding the non-ferrous metal copper smelting slag;
s2: mixing and stirring concentrated acid and the crushed and finely ground nonferrous metal copper smelting slag according to the mass ratio of 1.9-1;
s3: putting the mixture obtained in the step S2 into a reaction kettle, and carrying out curing reaction to obtain clinker;
s4: adding water into the clinker, stirring, and leaching for 0.5-5h to obtain a leaching solution and leaching residues.
In the step S2, a small amount of concentrated acid liquid is used to form a thin film liquid on the surface of the non-ferrous metal copper smelting slag, the non-ferrous metal copper smelting slag particles are wrapped in the thin film liquid, and the concentrated acid liquid film permeates into the interior through the gaps on the surface of the non-ferrous metal copper smelting slag particles in the curing process and contacts with the copper smelting slag to generate a chemical reaction, so that the glassy copper smelting slag is gradually dissolved. Compared with dilute acid in the prior art, the concentrated acid has higher reaction activity, and can ensure that the glassy non-ferrous metal copper smelting slag is dissolved more thoroughly.
In the step S3, the mixture can be heated automatically to 130-220 ℃, so that the reaction activity of concentrated acid can be further improved, the glassy nonferrous metal copper smelting slag can be rapidly dissolved, and the leaching rate of valuable metals can be further improved. In the prior art, the curing heating temperature is generally 120-140 ℃, and is lower than the self-heating curing temperature of the invention, and the final curing degree, and the leaching rate and the recovery rate of valuable metals are relatively low.
In the efficient acid-mixing curing leaching process, preferably, in step S1, the nonferrous metal copper smelting slag is crushed and ground, and then screened by a 100-300-mesh sieve, so that the concentrated acid can completely dissolve the nonferrous metal copper smelting slag, and valuable metals in the nonferrous metal copper smelting slag can be fully recovered. If the granularity of the non-ferrous metal copper smelting slag after crushing and fine grinding is larger than 100 meshes, the leaching rate and the recovery rate of valuable metals can be influenced, and if the granularity is too small, the production cost can be increased.
In the efficient acid-mixing curing leaching process, preferably, in the step S3, water is added into the mixture, so that the mixture is subjected to self-heating curing and the temperature reaches 130-220 ℃.
In the efficient acid-mixed slaking and leaching process, the water is preferably added in an amount of 10-45% of the mass of the nonferrous copper smelting slag in the step S3.
In the prior art, the acid liquid is directly heated, and the temperature of the system is generally difficult to exceed 100 ℃ due to the limitation of liquid. Researchers in this application have found that when the slaking temperature is controlled to 130 ℃ to 220 ℃, the dissolution rate of the nonferrous metal copper smelting slag can be increased, and the leaching rate and recovery rate of valuable metals can be increased, and that the leaching rate and recovery rate of valuable metals can be reduced if the temperature is lower than the temperature, for example, 120 ℃. The invention realizes curing heating by adding water into the mixture, the concentrated acid can emit a large amount of heat after contacting with a small amount of water, and the mixture in the reaction kettle can quickly self-heat to 130-220 ℃ to provide the required temperature for curing. According to the invention, water is added into the mixture to enable the system temperature of the mixture to reach the required range, excessive or too little water can affect the dissolution degree of the nonferrous metal copper smelting slag, and when the mass of the water exceeds 45% of the mass of the nonferrous metal copper smelting slag, the acid liquor concentration is too low; when the amount of the slag is less than 10% by mass, the amount of heat released is insufficient to maintain the whole aging stage.
In the efficient acid-mixing curing leaching process, the curing time in the step S3 is preferably 1-2 h.
The curing lasts for 1-2 h, preferably 1.5h, so that valuable metals in the nonferrous metal copper smelting slag can be leached, the required time is short, and the leaching effect is good.
In the efficient acid-mixed slaking and leaching process, the water is preferably added in an amount of 2.5 to 3.0 times the mass of the copper smelting slag in step S4.
In the efficient acid-mixing curing leaching process, preferably, in step S4, after water is added to the clinker, dilute acid is continuously added to adjust the pH value of the system to 0.5-4.5 so as to meet the acidity required for leaching, and if the pH value of the system is adjusted to be above 4.5, the leaching effect is poor and the recovery rate of valuable metals is low; if the pH of the system is adjusted to 0.5 or less, the amount of acid consumed is large and leaching of valuable metals is also affected.
In the efficient acid-mixed curing leaching process, the leaching time in the step S4 is preferably 2 hours.
In the efficient acid-mixing curing and leaching process, preferably, in the steps S2 and S4, the concentrated acid is concentrated sulfuric acid or concentrated hydrochloric acid, the mass fraction of the concentrated sulfuric acid is 90% -98%, and the mass fraction of the concentrated hydrochloric acid is 30% -38%.
(III) advantageous effects
The invention has the beneficial effects that:
the invention adopts an acid-mixing curing leaching process, adopts concentrated acid to replace dilute acid as a curing agent, uses a small amount of concentrated acid to be uniformly mixed with non-ferrous metal copper smelting slag, humidifies and infiltrates a small amount of concentrated acid liquid on the surface of the non-ferrous metal copper smelting slag, enables the concentrated acid to form a layer of film liquid on the surface of the non-ferrous metal copper smelting slag, wraps the non-ferrous metal copper smelting slag particles, permeates the interior through gaps on the surface of the non-ferrous metal copper smelting slag particles in the heating curing process, contacts with the copper smelting slag to generate chemical reaction, gradually dissolves the glassy state copper smelting slag, and combines with the leaching process to carry out high-efficiency leaching on metal ions contained in the glass state copper smelting slag. Therefore, the acid-mixing curing leaching process provided by the invention can be used for curing the nonferrous metal copper smelting slag by only adopting a small amount of concentrated acid, and can be used for efficiently recovering valuable metals after curing and leaching, so that the recovery rate of the valuable metals in the copper slag is improved, the acid consumption is greatly reduced, toxic and difficultly-recovered raw materials such as hydrofluoric acid are not used, the process flow is greatly shortened, the process flow can be used for large-scale production, good economic benefits are realized, and the environmental safety can be maintained.
Drawings
FIG. 1 is a process flow chart of the high-efficiency acid-mixing curing leaching process of the non-ferrous metal copper smelting slag of the invention.
Detailed Description
In order that the invention may be better understood, it is described in detail below with reference to specific embodiments.
Example 1
The embodiment provides a high-efficiency acid-mixing curing leaching process for non-ferrous metal copper smelting slag, which comprises the following steps:
s1: and crushing and finely grinding the non-ferrous metal copper smelting slag, and sieving with a 200-mesh sieve to obtain non-ferrous metal copper smelting slag powder.
S2: and (3) mixing and stirring 93% concentrated sulfuric acid and nonferrous copper smelting slag powder according to the mass ratio of 1:1 to obtain a mixture.
S3: and (3) putting the mixture obtained in the step (S2) into a reaction kettle, adding water into the mixture, wherein the addition amount of the water is 23% of the mass of the non-ferrous copper smelting slag, and curing for 1.5h to obtain clinker. In this step, after the water was added, the curing temperature in the reaction kettle was 174 ℃.
S4: adding water into the clinker, wherein the addition amount of the water is 3.0 times of the mass of the non-ferrous metal copper smelting slag, continuously adding dilute sulfuric acid after uniformly stirring, adjusting the pH value of the system to 3.0, and leaching for 2 hours to obtain a leaching solution and leaching slag.
And (3) carrying out post-treatment on the leaching solution, recovering valuable metals such as iron, copper, nickel, cobalt and the like in the leaching solution, and recovering silicon in the leaching slag.
Through calculation, the leaching rate of Fe, cu, ni and Co in the embodiment is 93.7%, and the recovery rate of Si is 85%.
Example 2
The embodiment provides a high-efficiency acid-mixing curing leaching process for non-ferrous metal copper smelting slag, which comprises the following steps:
s1: crushing and finely grinding the non-ferrous metal copper smelting slag, and sieving with a 200-mesh sieve to obtain non-ferrous metal copper smelting slag powder.
S2: mixing and stirring concentrated sulfuric acid with the mass fraction of 98% and non-ferrous metal copper smelting slag powder according to the mass ratio of 1.
S3: and (3) putting the mixture obtained in the step (S2) into a reaction kettle, adding water into the mixture, wherein the addition amount of the water is 30% of the mass of the non-ferrous copper smelting slag, and curing for 1.5h to obtain clinker. In the step, after detection, the curing temperature in the reaction kettle after adding water is 220 ℃.
S4: adding water into the clinker, wherein the addition amount of the water is 2.5 times of the mass of the nonferrous metal copper smelting slag, continuously adding dilute sulfuric acid after uniformly stirring, adjusting the pH value of the system to 2.5, and leaching for 2 hours to obtain a leaching solution and leaching slag.
And (3) carrying out post-treatment on the leaching solution, recovering valuable metals such as iron, copper, nickel, cobalt and the like in the leaching solution, and recovering silicon in the leaching slag.
Through calculation, the leaching rate of Fe, cu, ni and Co in the embodiment is 91.9%, and the recovery rate of Si is 84.1%.
Example 3
The embodiment provides a high-efficiency acid-mixing curing leaching process for non-ferrous metal copper smelting slag, which comprises the following steps:
s1: and crushing and finely grinding the non-ferrous metal copper smelting slag, and sieving with a 100-mesh sieve to obtain non-ferrous metal copper smelting slag powder.
S2: mixing and stirring concentrated sulfuric acid with the mass fraction of 90% and non-ferrous metal copper smelting slag powder according to the mass ratio of 1.6 to obtain a mixture.
S3: and (3) putting the mixture obtained in the step (S2) into a reaction kettle, adding water into the mixture, wherein the addition amount of the water is 26% of the mass of the non-ferrous copper smelting slag, and curing for 1.5h to obtain clinker. In this step, after the water was added, the curing temperature in the reaction vessel was 154 ℃.
S4: adding water into the clinker, wherein the addition amount of the water is 2.5 times of the mass of the non-ferrous metal copper smelting slag, continuously adding dilute sulfuric acid after uniformly stirring, adjusting the pH value of the system to 2.5, and leaching for 2 hours to obtain a leaching solution and leaching slag.
And (3) carrying out post-treatment on the leaching solution, recovering valuable metals such as iron, copper, nickel, cobalt and the like in the leaching solution, and recovering silicon in the leaching slag.
Through calculation, the leaching rate of iron, copper, nickel and cobalt in the embodiment is 90.9%, and the recovery rate of silicon element is 83.2%.
Example 4
The embodiment provides a high-efficiency acid-mixing curing and leaching process of non-ferrous metal copper smelting slag, which is different from the embodiment 1 in that in the step S3, the addition amount of water is 20% of the mass of the non-ferrous metal copper smelting slag, and the curing time is 2 hours. In the step S4, the addition amount of water is 2.5 times of the mass of the non-ferrous metal copper smelting slag, the dilute sulfuric acid is continuously added after the uniform stirring, the pH value of the system is adjusted to 3.0, and the leaching is carried out for 4 hours.
Through calculation, the leaching rate of Fe, cu, ni and Co in the embodiment is 92.1%, and the recovery rate of Si is 81.7%.
Example 5
The embodiment provides a high-efficiency acid-mixing curing leaching process for non-ferrous metal copper smelting slag, which is different from the embodiment 1 in that in the step S4, the addition amount of water is 3.0 times of the mass of non-ferrous metal copper smelting slag, dilute sulfuric acid is continuously added after the water is uniformly stirred, the pH value of a system is adjusted to 4.5, and leaching is carried out for 5 hours.
Through calculation, in the embodiment, the leaching rate of the iron, copper, nickel and cobalt is 92.6%, and the recovery rate of the silicon element is 84.1%.
Example 6
The embodiment provides a high-efficiency acid-mixing curing leaching process of nonferrous metal copper smelting slag, which is different from the embodiment 1 in that in the step S2, the mass fraction of concentrated sulfuric acid is 98%. In the step S3, the addition amount of water is 20% of the mass of the nonferrous copper smelting slag, and the aging is carried out for 1h. In the step S4, the addition amount of water is 2.5 times of the mass of the non-ferrous metal copper smelting slag, dilute sulfuric acid is continuously added after uniform stirring, the pH value of the system is adjusted to 2.5, and leaching is carried out for 5 hours.
Through calculation, the leaching rate of iron, copper, nickel and cobalt in the embodiment is 93.1%, and the recovery rate of silicon element is 83.8%.
Comparative example 1
The comparative example differs from example 1 in that in step S3 no water is added, the reactor is heated and the temperature of the mixture is measured to be 120 ℃. The final leaching rate of Fe, cu, ni and Co is 71.7%, and the recovery rate of Si element is 67.1%.
Comparative example 2
The present comparative example differs from example 1 in that in step S2, dilute sulfuric acid is added, the mass ratio of dilute sulfuric acid to nonferrous copper smelting slag being 3:1. In the step S3, the reaction kettle is heated, and the temperature of the mixture can only reach 120 ℃ after detection. Finally, the leaching rate of the iron, the copper and the nickel and the cobalt is 67.8 percent, and the recovery rate of the silicon element is 63.5 percent.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art can change or modify the technical content disclosed above into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (9)
1. An efficient acid-mixing curing leaching process for nonferrous metal copper smelting slag is characterized by comprising the following steps:
s1: crushing and finely grinding the non-ferrous metal copper smelting slag;
s2: mixing and stirring concentrated acid and the crushed and finely ground nonferrous metal copper smelting slag according to the mass ratio of 1.9-1;
s3: putting the mixture obtained in the step S2 into a reaction kettle, and carrying out curing reaction to obtain clinker;
s4: adding water into the clinker, stirring, and leaching for 0.5-5h to obtain a leaching solution and leaching residues.
2. The high-efficiency acid-mixing curing leaching process as claimed in claim 1, wherein in step S1, the non-ferrous metal copper smelting slag is crushed, finely ground and then sieved by a 100-300-mesh sieve.
3. The efficient acid-mixing curing leaching process as claimed in claim 1, wherein in the step S3, water is added into the mixture to perform self-heating curing on the mixture, and the self-heating temperature reaches 130-220 ℃.
4. The high-efficiency acid-mixing curing leaching process as claimed in claim 3, wherein in the step S3, the addition amount of water is 10-45% of the mass of the nonferrous copper smelting slag.
5. The high-efficiency acid-mixing curing and leaching process as claimed in claim 1, wherein in the step S3, the curing time is 1-2 h.
6. The high-efficiency acid-mixing slaking and leaching process according to claim 1, wherein in the step S4, the addition amount of water is 2.5-3.0 times of the mass of the copper smelting slag.
7. The high-efficiency acid-mixing curing leaching process as claimed in claim 1, wherein in the step S4, after water is added into the clinker, dilute acid is continuously added to adjust the pH value of the system to 0.5-4.5.
8. The high-efficiency acid-mixing curing leaching process as claimed in claim 1, wherein in the step S4, the leaching time is 2h.
9. The high-efficiency acid-mixing curing and leaching process as claimed in any one of claims 1 or 7, wherein in steps S2 and S4, the concentrated acid is concentrated sulfuric acid or concentrated hydrochloric acid, the mass fraction of the concentrated sulfuric acid is 90% -98%, and the mass fraction of the concentrated hydrochloric acid is 30% -38%.
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2022
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1510151A (en) * | 2002-12-26 | 2004-07-07 | 中国科学院过程工程研究所 | Cobalt slag containing treating method |
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| CN114149031A (en) * | 2021-12-07 | 2022-03-08 | 紫金矿业集团股份有限公司 | Method for preparing ferrous sulfate from copper smelting slag |
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