CN113106260A - Copper sludge treatment method, temperature control system and friction stir welding machine - Google Patents
Copper sludge treatment method, temperature control system and friction stir welding machine Download PDFInfo
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- CN113106260A CN113106260A CN202110541497.8A CN202110541497A CN113106260A CN 113106260 A CN113106260 A CN 113106260A CN 202110541497 A CN202110541497 A CN 202110541497A CN 113106260 A CN113106260 A CN 113106260A
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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
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0082—Leaching or slurrying with water
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0086—Treating solutions by physical methods
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
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Abstract
The invention provides a copper sludge treatment method, which comprises the following steps: introducing water vapor into the copper sludge for slurrying to obtain slurried copper sludge, and performing heat preservation leaching on the slurried copper sludge to obtain a copper sludge leachate and sludge residues; carrying out pressure filtration on the copper sludge leaching solution in a heat preservation environment to obtain a filtered copper sludge leaching solution; spraying the filtered copper sludge leachate in a first direction in a first reaction cavity, and simultaneously blowing a first reactant in a second direction; standing and stirring the first mixed reactant, and performing solid-liquid separation to obtain a first post-treatment liquid; spraying the first post-treatment liquid in a third direction in a second reaction cavity, and blowing a second reactant in a fourth direction to obtain a second mixed reactant; and stirring the second mixed reactant, and performing solid-liquid separation after standing to obtain a second post-treatment liquid. The invention can improve the reaction speed of the copper ions and the first reactant and reduce the usage amount of the reactant.
Description
Technical Field
The invention belongs to the technical field of welding, and particularly relates to a copper sludge treatment method, a temperature control system and a friction stir welding machine.
Background
The industrial copper-containing wastewater mainly comes from the industries of electroplating, electronics and circuit boards, and copper sludge obtained by chemical flocculation, neutralization and sedimentation often contains a large amount of copper and exists in an unstable state, so that the industrial copper-containing wastewater has heavy metal toxicity. According to the national records of dangerous wastes, the copper sludge belongs to dangerous wastes, but the dry-basis copper grade of the copper sludge is about 3-15 percent, is far higher than the exploitable grade of copper ore, and is a high-value metal resource. When the copper sludge is subjected to harmless treatment, the copper sludge can be treated by adopting a wet leaching technology or a biological metallurgy mode, in the wet leaching technology, leached copper ions exist in the form of sulfate, and the copper ions are displaced and separated from a leaching solution by adding substances having a displacement reaction with the copper ions, but the method usually directly adds the substances having the displacement reaction with the copper ions into the leaching solution, the displacement reaction is concentrated at one position in the leaching solution, the whole reaction needs longer waiting time and is uncontrollable, more substances having the displacement reaction with the copper ions need to be added, for example, in the case of taking iron simple substance as the displaced copper ions, the partial iron ion enrichment is caused, and more iron simple substance needs to be added.
Disclosure of Invention
The embodiment of the invention provides a copper sludge treatment method, aiming at solving the problems that in the existing wet leaching, replacement reaction is concentrated at a certain position in a leaching solution, the whole reaction needs longer waiting time, the reaction is uncontrollable, and more substances having replacement reaction with copper ions need to be added.
The embodiment of the invention provides a copper sludge treatment method, which comprises the following steps:
s1, introducing water vapor into copper sludge to perform slurrying to obtain slurried copper sludge, and performing heat preservation leaching on the slurried copper sludge to obtain a copper sludge leachate and sludge residues, wherein the initial water content of the copper sludge is 40-60%, the initial temperature of the copper sludge is 30-50 ℃, the water content of the slurried copper sludge is 80-90%, and the temperature of the slurried copper sludge is 80-90 ℃;
s2, carrying out pressure filtration on the copper sludge leachate in a heat preservation environment to obtain a filtered copper sludge leachate;
s3, spraying the filtered copper sludge leachate in a first direction in a first reaction chamber to form a sprayed leachate, and blowing a first reactant in a second direction, where the first direction and the second direction have a crossing point, so that the first reactant and the sprayed leachate are mixed in the first reaction chamber at a first relative speed to obtain a first mixed reactant;
s4, standing and stirring the first mixed reactant in the first reaction cavity, wherein the standing time is 30 minutes, the stirring time is 10 minutes, the standing frequency is N times, and the stirring frequency is N-1 times, and when the content of copper ions in the liquid is detected to be reduced to a preset value during the standing period, performing solid-liquid separation to obtain a first post-treatment liquid and solid copper, wherein the solid copper is used for refining copper;
s5, spraying the first post-treatment liquid in a third direction in a second reaction cavity to form a sprayed post-treatment liquid, and blowing a second reactant in a fourth direction, wherein the third direction and the fourth direction have a cross point, so that the second reactant and the sprayed post-treatment liquid are cross-mixed in the second reaction cavity at a second relative speed to obtain a second mixed reactant;
and S6, stirring the second mixed reactant in the second reaction cavity, continuously adding the second reactant into the second mixed reactant from a fifth direction, detecting the content of the second reactant in the second mixed reactant in real time, stopping adding the second reactant when the content of the second reactant in the second mixed reactant is larger than the first content value, standing, and performing solid-liquid separation to obtain a second post-treatment liquid and a solid reactant, wherein the second post-treatment liquid is used for evaporation and crystallization, and the solid reactant is used for preparing the first reactant or the second reactant.
Optionally, the step S1 further includes:
and adding the sludge residue into the original copper sludge, and preparing to obtain the hole sludge in the step S1.
Optionally, the first reactant includes a copper ion reactant, the copper ion reactant includes elemental iron powder, and the first post-treatment liquid includes ferrous ions generated by replacing copper ions with elemental iron.
Optionally, the spraying leachate is sprayed out through an atomizing nozzle, and the spraying leachate is in a discontinuous liquid drop state.
Optionally, the first relative speed includes a vector speed of the spraying leachate and a vector speed of the first reactant, the vector speed of the spraying leachate is a speed that ensures that the spraying leachate is in a discontinuous liquid drop state, and when a dosage ratio of the spraying leachate to the first reactant is 1: 1 to 1: 1.2, the spraying time of the spraying leachate is the same as the blowing time of the first reactant, and the vector velocity of the first reactant is determined to be 1 to 1.2 times of the vector velocity of the spraying leachate.
Optionally, the first direction and the second direction have an included angle of 120 degrees to 240 degrees in the horizontal direction.
Optionally, the second reactant includes elemental iron powder, and the second post-treatment liquid includes ferrous ions generated by reducing ferric iron with the elemental iron.
Optionally, the spraying post-treatment liquid is sprayed out through an atomizing nozzle, and the spraying post-treatment liquid is in a discontinuous liquid droplet state.
Optionally, the third relative velocity includes a vector velocity of the sprayed post-treatment liquid and a vector velocity of the second reactant, the vector velocity of the sprayed post-treatment liquid is a velocity that ensures that the sprayed post-treatment liquid is in a discontinuous liquid droplet state, and a ratio of usage amounts of the sprayed post-treatment liquid to the second reactant is 1: and 1, when the spraying time of the sprayed post-treatment fluid is the same as the blowing time of the second reactant, determining that the vector velocity of the second reactant is the same as the vector velocity of the sprayed leaching fluid.
Optionally, an included angle of 120 degrees to 240 degrees is formed between the third direction and the fourth direction in the horizontal direction, and the fifth direction is a direction perpendicular to a horizontal plane where a liquid level of the second mixed reactant is located when the second mixed reactant is standing.
In the embodiment of the invention, water vapor is introduced into copper sludge for slurrying to obtain slurried copper sludge, and the slurried copper sludge is subjected to heat preservation leaching to obtain a copper sludge leachate and sludge residue, wherein the initial water content of the copper sludge is 40-60%, the initial temperature of the copper sludge is 30-50 ℃, the water content of the slurried copper sludge is 80-90%, and the temperature of the slurried copper sludge is 80-90 ℃; carrying out pressure filtration on the copper sludge leachate under a heat preservation environment to obtain a filtered copper sludge leachate; spraying the filtered copper sludge leachate in a first direction in a first reaction cavity to form a sprayed leachate, and simultaneously blowing a first reactant in a second direction, wherein the first direction and the second direction have a cross point, so that the first reactant and the sprayed leachate are cross-mixed in the first reaction cavity at a first relative speed to obtain a first mixed reactant; standing and stirring the first mixed reactant in the first reaction cavity for 30 minutes, stirring for 10 minutes, standing for N times, and stirring for N-1 times, and performing solid-liquid separation to obtain a first post-treatment liquid and solid copper when the content of copper ions in the liquid is detected to be reduced to a preset value during standing, wherein the solid copper is used for refining copper; spraying the first post-treatment liquid in a third direction in a second reaction cavity to form sprayed post-treatment liquid, and blowing a second reactant in a fourth direction, wherein the third direction and the fourth direction have a cross point, so that the second reactant and the sprayed post-treatment liquid are mixed in the second reaction cavity at a second relative speed in a cross way to obtain a second mixed reactant; and stirring the second mixed reactant in the second reaction cavity, continuously adding the second reactant into the second mixed reactant from a fifth direction, detecting the content of the second reactant in the second mixed reactant in real time, stopping adding the second reactant when the content of the second reactant in the second mixed reactant is greater than a first content value, standing, and performing solid-liquid separation to obtain a second post-treatment liquid and a solid reactant, wherein the second post-treatment liquid is used for evaporative crystallization, and the solid reactant is used for preparing the first reactant or the second reactant. According to the invention, the filtered copper sludge leachate is sprayed in the first direction to form the sprayed leachate, and the first reactant is blown in the second direction, so that the first reactant can be fully contacted with the copper sludge leachate, the first reactant is more uniformly distributed in the copper sludge leachate, the contact area between the sprayed leachate and the first reactant is greatly increased, the reaction speed of copper ions and the first reactant is increased, the treatment speed of copper sludge treatment is further increased, the occurrence of local enrichment condition is reduced, and the usage amount of the first reactant can be reduced.
Drawings
FIG. 1 is a flow chart of a method for treating copper sludge according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
According to the invention, the filtered copper sludge leachate is sprayed in the first direction to form the sprayed leachate, and the first reactant is blown in the second direction, so that the first reactant can be fully contacted with the copper sludge leachate, the first reactant is more uniformly distributed in the copper sludge leachate, the contact area between the sprayed leachate and the first reactant is greatly increased, the reaction speed of the first reactant and the first reactant is increased, the treatment speed of copper sludge treatment is further increased, the occurrence of local enrichment is reduced, and the use amount of the first reactant can be reduced.
Referring to fig. 1, fig. 1 is a flow chart of a copper sludge treatment method according to an embodiment of the present invention. By providing a copper sludge treatment method, the copper sludge treatment method comprises the following steps:
and S1, introducing water vapor into the copper sludge to perform slurrying to obtain slurried copper sludge, and performing heat preservation leaching on the slurried copper sludge to obtain copper sludge leachate and sludge residue.
In the embodiment of the invention, the initial water content of the copper sludge is 40-60%, the initial temperature of the copper sludge is 30-50 ℃, the water content of the slurried copper sludge is 80-90%, and the temperature of the slurried copper sludge is 80-90 ℃.
The copper sludge can be copper sludge obtained by treating copper-containing wastewater by a flocculation precipitation method, and the initial temperature of the copper sludge obtained by the flocculation precipitation method is controlled to be 30-50 ℃, and the water content is 80-90%.
Steam is introduced into the copper sludge to pulp, and the water vapor can be used for stirring, heating and humidifying the copper sludge simultaneously, so that the copper sludge can be pulped better, the fluidity of the copper sludge is increased, and the leaching time can be shortened.
The leaching may be performed by an acid leaching method, for example, sulfuric acid with a certain concentration is added to the slurried copper sludge, and specifically, the temperature of the slurried copper sludge in the leaching process is maintained at 80 ℃ to 90 ℃, the concentration of the sulfuric acid is 3mol/L to 3.5mol/L, and the leaching time is 60 minutes, so that a copper sludge leachate is obtained. The leaching result is copper sludge leachate and sludge residue, wherein the copper sludge leachate comprises a large amount of copper ions, the sludge residue is solid residue, the metal content of the sludge residue can be detected, when the metal content of the sludge residue exceeds a harmful standard, the sludge residue can be collected and then subjected to temperature and water content modulation to obtain new copper sludge, the new copper sludge is subjected to water vapor pulping to obtain pulped copper sludge, and the pulped copper sludge is subjected to heat preservation leaching to obtain new copper sludge leachate and new sludge residue until the metal content of the sludge residue does not exceed the harmful standard, so that the sludge residue is recycled.
And S2, carrying out pressure filtration on the copper sludge leachate in a heat preservation environment to obtain the filtered copper sludge leachate.
In an embodiment of the present invention, the heat preservation environment may be a pressure vessel environment at a temperature of 80 ℃ to 90 ℃, the pressure vessel includes a pressure filtering device, and the pressure filtering device may perform pressure filtering on the copper sludge leachate to obtain a filtered copper sludge leachate. The solid impurities with larger volume in the copper sludge leachate can be filtered through pressure filtration.
And S3, spraying the filtered copper sludge leachate in a first direction in the first reaction cavity to form a sprayed leachate, and simultaneously blowing a first reactant in a second direction.
In an embodiment of the present invention, the first direction and the second direction have a crossing point, so that the first reactant and the spray leachate are mixed in the first reaction chamber at a first relative speed to obtain a first mixed reactant.
The spraying can be carried out through the liquid spray nozzle, the filtered copper sludge leachate is dispersed in a spraying mode, the liquid surface area of the filtered copper sludge leachate can be increased, the sprayed leachate is fully contacted with the first reactant, the first reactant is prevented from being contacted and entering the filtered copper sludge leachate through the same liquid surface, the first reactant is prevented from being gathered at one position, and the reaction effect of the filtered copper sludge leachate and the first reactant is improved. The spraying angle is that the central spraying shaft is 15-30 degrees and is in a cone shape.
The first reactant is a solid reactant, specifically, the first reactant is a solid powdery reactant, for example, metal powder or metal scrap capable of reducing copper ions to copper simple substance, and the particle size of the metal powder is in the range of 15 μm to 50 μm. The first reactant can be blown by using a fan and a tuyere so as to be blown into the first reaction cavity. The blowing angle is the same as the spraying angle, and the blowing angle is conical.
In a possible embodiment, the first reaction chamber comprises an upper chamber and a lower chamber, the upper chamber is used for supporting the filtered copper sludge leachate to be sprayed in the first direction and the first reactant to be blown in the second direction, and the lower chamber is used for collecting the mixed first mixed reactant. The upper cavity can be a spherical cavity, the lower cavity can be a cylindrical cavity, and the upper cavity is smoothly connected with the lower cavity. Optionally, in the spraying process, the spraying speed is controlled, so that the parabola with the largest opening in the spraying leachate is in contact with the spherical inner cavity at an included angle smaller than 5 degrees, the spraying leachate is guaranteed to be in flexible contact with the spherical inner cavity, the spraying leachate is prevented from being splashed, meanwhile, the horizontal stress of the first reaction cavity can be reduced, and the service life of the first reaction cavity is prolonged.
The first direction is toward the vertical central axis of the first reaction chamber in the horizontal direction, and the second direction is also toward the vertical central axis of the first reaction chamber in the horizontal direction. The intersection of the first direction and the second direction is in the vicinity of the vertical mid-axis.
It will be appreciated that when powdered metal is added to a bath of water, the powdered metal will float on the surface of the liquid due to the surface tension of the liquid, and when the surface tension at a point in the surface of the liquid is unbalanced, the surface of the liquid will collapse, and a large amount of powdered metal will enter the liquid from the point where the surface of the liquid collapses, causing excessive accumulation of the powdered metal locally in the liquid and failure to disperse uniformly in the liquid. In the embodiment of the invention, as the spray leaching solution is a dispersed liquid, the first reactant is also a dispersed solid powder after being blown in, so that the spray leaching solution is well combined with the first reactant in the first reaction cavity through surface tension, and finally the bottom of the first reaction cavity is mixed to obtain the first mixed reactant.
Specifically, the first mixed reactant includes the filtered copper sludge leachate and the first reactant, and the first reactant is uniformly distributed in the filtered copper sludge leachate, so that the replacement reaction speed of copper ions in the first mixed reactant is increased.
S4, standing and stirring the first mixed reactant in the first reaction cavity, wherein the standing time is 30 minutes, the stirring time is 10 minutes, the standing frequency is N times, and the stirring frequency is N-1 times, and when the content of copper ions in the liquid is detected to be reduced to a preset value during the standing period, performing solid-liquid separation to obtain a first post-treatment liquid and solid copper.
In an embodiment of the present invention, the first mixed reactant includes a filtered copper sludge leachate and a first reactant, the filtered copper sludge leachate includes copper ions, the first reactant includes a metal capable of reducing the copper ions into a copper simple substance, for example, the copper ions may be replaced by a metal ordered before copper in a metal activity order table, and during a standing process, the copper ions are replaced to form the copper simple substance. In order to accelerate the process of the displacement reaction, after standing for 30 minutes, the first mixed reactant may be stirred, so that the precipitated first reactant may be stirred to maintain the uniform distribution of the first reactant in the first mixed reactant during the reaction, and the stirring may be performed by a rotary stirring with an angular speed of 30 r/m. And standing the mixture after stirring to enable the solid to be layered with liquid, wherein the solid is basically solid copper, the liquid is first post-treatment liquid, the first post-treatment liquid comprises metal ions obtained after copper ions are reduced into copper simple substances, and the reaction equation of iron and copper ions is as follows: fe + Cu2 +＝Cu+Fe2 +Therefore, the first post-treatment liquid includes ferrous ions.
The stirring mode can be a Boolmakin type stirring mode, can reduce the power consumption of stirring, and is suitable for the processes of mixing, dispersing, solid-liquid suspension, dissolving and the like.
N may be an integer greater than or equal to 2, and in the embodiment of the present invention, since the sprayed leachate is mixed with the blown first reactant, it is possible to reduce the content of copper ions in the liquid to a preset value during the first standing process, in this case, N may also be 1, i.e., only one standing process is required, and no stirring is required. The solid copper can be used for copper refining. The preset value to which the content of the copper ions is reduced can be preset to be 0.08 mol/L.
And S5, spraying the first post-treatment liquid in the third direction in the second reaction cavity to form a sprayed post-treatment liquid, and simultaneously blowing the second reactant in the fourth direction.
In an embodiment of the present invention, the third direction and the fourth direction have a crossing point, so that the second reactant and the sprayed post-treatment liquid are mixed in the second reaction chamber at a second relative speed to obtain a second mixed reactant. The spraying angle is that the central spraying shaft is 15-30 degrees and is in a cone shape.
The second reactant is a solid reactant, specifically, the second reactant is a solid powdery reactant, and the particle size of the solid powder is in the range of 15 μm to 50 μm. The second reactant is used for oxidizing the metal ions generated by the first reactant or for enabling the metal ions generated by the first reactant to form metal salt, for example, when the first reactant is iron, ferrous ions and copper are generated after the iron and copper ions are converted, and the ferrous ions can be oxidized into ferric ions, so that ferric salt is obtained or a flocculating agent is added to precipitate iron, or the concentration of the ferrous ions is increased to crystallize to generate ferrous salt products. The second reactant can be blown by using a blower and a tuyere so as to be blown into the second reaction cavity. The blowing angle is the same as the spraying angle, and the blowing angle is conical.
In a possible embodiment, the second reaction chamber includes an upper chamber and a lower chamber, the upper chamber is used for supporting the first post-treatment liquid to be sprayed in the third direction and the second reactant to be blown in the fourth direction, and the lower chamber is used for collecting the mixed second reactant. The upper cavity can be a spherical cavity, the lower cavity can be a cylindrical cavity, and the upper cavity is smoothly connected with the lower cavity. Optionally, in the spraying process, the spraying speed is controlled, so that the parabola with the largest opening in the sprayed aftertreatment liquid is in contact with the spherical inner cavity at an included angle smaller than 5 degrees, the sprayed aftertreatment liquid is guaranteed to be in flexible contact with the spherical inner cavity, the phenomenon of splashing of the sprayed aftertreatment liquid is prevented, meanwhile, the horizontal stress of the second reaction cavity can be reduced, and the service life of the first reaction cavity is prolonged.
It should be noted that the third direction is toward the vertical central axis of the second reaction chamber in the horizontal direction, and the fourth direction is also toward the vertical central axis of the second reaction chamber in the horizontal direction. The intersection of the third and fourth directions is in the vicinity of the vertical mid-axis.
In the embodiment of the invention, the sprayed post-treatment liquid is a dispersed liquid, and the second reactant is also dispersed solid powder after being blown in, so that the sprayed post-treatment liquid is well combined with the second reactant in the second reaction chamber through surface tension, and finally the bottom of the second reaction chamber is mixed to obtain the second mixed reactant.
And S6, stirring the second mixed reactant in the second reaction cavity, continuously adding the second reactant into the second mixed reactant from the fifth direction, detecting the content of the second reactant in the second mixed reactant in real time, stopping adding the second reactant when the content of the second reactant in the second mixed reactant is larger than the first content value, and performing solid-liquid separation after standing to obtain a second post-treatment liquid and a solid reactant.
In an embodiment of the present invention, the second post-treatment liquid is used for evaporative crystallization, and the solid reactant is used for preparing the first reactant or the second reactant. It should be noted that, the substitution reaction of copper ions is to obtain electrons to form a copper simple substance, and the metal simple substance losing electrons will become a metal ion, will form a salt with an acid in the leaching solution, and can be evaporated and crystallized, for example, a ferrous ion will form ferrous sulfate with a sulfate ion in the leaching solution. The extra elementary metal can be used as a solid reactant, for example, the extra elementary iron can be used as a first reactant or a second reactant after being dried.
The stirring mode can be a Boolmakin type stirring mode, can reduce the power consumption of stirring, and is suitable for the processes of mixing, dispersing, solid-liquid suspension, dissolving and the like.
In the embodiment of the invention, water vapor is introduced into copper sludge for slurrying to obtain slurried copper sludge, and the slurried copper sludge is subjected to heat preservation leaching to obtain a copper sludge leachate and sludge residue, wherein the initial water content of the copper sludge is 40-60%, the initial temperature of the copper sludge is 30-50 ℃, the water content of the slurried copper sludge is 80-90%, and the temperature of the slurried copper sludge is 80-90 ℃; carrying out pressure filtration on the copper sludge leachate under a heat preservation environment to obtain a filtered copper sludge leachate; spraying the filtered copper sludge leachate in a first direction in a first reaction cavity to form a sprayed leachate, and simultaneously blowing a first reactant in a second direction, wherein the first direction and the second direction have a cross point, so that the first reactant and the sprayed leachate are cross-mixed in the first reaction cavity at a first relative speed to obtain a first mixed reactant; standing and stirring the first mixed reactant in the first reaction cavity for 30 minutes, stirring for 10 minutes, standing for N times, and stirring for N-1 times, and performing solid-liquid separation to obtain a first post-treatment liquid and solid copper when the content of copper ions in the liquid is detected to be reduced to a preset value during standing, wherein the solid copper is used for refining copper; spraying the first post-treatment liquid in a third direction in a second reaction cavity to form sprayed post-treatment liquid, and blowing a second reactant in a fourth direction, wherein the third direction and the fourth direction have a cross point, so that the second reactant and the sprayed post-treatment liquid are mixed in the second reaction cavity at a second relative speed in a cross way to obtain a second mixed reactant; and stirring the second mixed reactant in the second reaction cavity, continuously adding the second reactant into the second mixed reactant from a fifth direction, detecting the content of the second reactant in the second mixed reactant in real time, stopping adding the second reactant when the content of the second reactant in the second mixed reactant is greater than a first content value, standing, and performing solid-liquid separation to obtain a second post-treatment liquid and a solid reactant, wherein the second post-treatment liquid is used for evaporative crystallization, and the solid reactant is used for preparing the first reactant or the second reactant. According to the invention, the filtered copper sludge leachate is sprayed in the first direction to form the sprayed leachate, and the first reactant is blown in the second direction, so that the first reactant can be fully contacted with the copper sludge leachate, the first reactant is more uniformly distributed in the copper sludge leachate, the contact area between the sprayed leachate and the first reactant is greatly increased, the reaction speed of copper ions and the first reactant is increased, the treatment speed of copper sludge treatment is further increased, the occurrence of local enrichment condition is reduced, and the usage amount of the first reactant can be reduced.
Optionally, step S1 further includes:
the sludge residue is added to the original copper sludge to prepare the hole sludge in the step S1. Specifically, the metal content of the sludge residue may be detected, and when the metal content of the sludge residue exceeds a harmful standard, the sludge residue may be collected and then added to the original copper sludge, and the temperature and the water content are adjusted to obtain the hole sludge in step S1, so as to recycle the sludge residue.
Optionally, the first reactant includes a copper ion reactant, the copper ion reactant includes elemental iron powder, and the first post-treatment liquid includes ferrous ions generated by replacing copper ions with elemental iron. The iron elementary substance powder can be obtained by processing iron-containing solid wastes such as waste steel, cutting leftover materials, stamping wastes and the like. The granularity of the iron simple substance powder is in the range of 15-50 mu m.
Optionally, the spraying leachate is sprayed out through an atomizing nozzle, and the spraying leachate is in a discontinuous liquid drop state. The filtered copper sludge leachate can be sprayed out through the atomizing nozzle, so that liquid beads are formed after the filtered copper sludge leachate is sprayed out, the surface area of liquid is increased, the filtered copper sludge leachate can be better contacted with the first reactant, and the reaction speed of copper ion replacement reaction is improved. The diameter of the spray hole of the atomizing spray head is in the range of 60-90 μm.
Optionally, the first relative velocity includes a vector velocity of the spray leachate and a vector velocity of the first reactant, the vector velocity of the spray leachate is a velocity that ensures that the spray leachate is in a discontinuous liquid droplet state, and a ratio of usage amounts of the spray leachate to the first reactant is 1: 1 to 1: 1.2, the time for spraying the leachate is the same as the time for blowing the first reactant, and the vector velocity of the first reactant is 1 to 1.2 times the vector velocity of the leachate.
Specifically, the vector velocity of the leachate to be sprayed is determined by the spraying velocity of the atomizing nozzle and the first direction, the droplet state is a state in which the droplet can be dropped by the influence of gravity, and the first reactant may be blown into the first reaction chamber by using a blower and a tuyere. The vector velocity of the first reactant is determined by the blowing velocity of the air nozzle and the second direction, and the blowing velocity of the air nozzle is correlated with the ejection velocity of the atomizing head. It can be understood that, for a certain amount of filtered copper sludge leachate, the amount of the first reactant is prepared according to a proportion, and the spraying time of the filtered copper sludge leachate is the same as the blowing time of the first reactant, namely, the spraying time and the blowing time begin and end simultaneously. The dosage ratio of the spraying leaching solution to the first reactant is 1: 1 to 1: 1.2, the spraying time of the spraying leachate is the same as the blowing time of the first reactant, and the blowing speed of the air nozzle is determined to be 1 to 1.2 times of the spraying speed of the atomizing nozzle.
Optionally, the first direction and the second direction have a projection angle of 120 degrees to 240 degrees on a horizontal plane. By setting the projection included angle of the first direction and the second direction on the same horizontal plane to be 120 degrees to 240 degrees, the spraying leaching liquid can be contacted with the first reactant at a higher relative speed, and the mixing effect of the spraying leaching liquid and the first reactant is improved.
Optionally, the second reactant includes elemental iron powder, and the second post-treatment liquid includes ferrous ions generated by reducing ferric iron with the elemental iron.
In an embodiment of the present invention, the first post-treatment liquid comprises ferrihydriteHowever, because the content of ferrous ions is not much different from the content of copper ions in the filtered leaching solution, the content of ferrous ions in the second post-treatment solution can be increased by considering the process cost and the output. The ferrous ions can be used for crystallization to obtain ferrous salt, so that the content of the ferrous ions is increased, and more ferrous salt can be produced. In an acid environment, a simple substance of iron is oxidized into ferric iron, excessive ferric iron can reduce the ferric iron into ferrous ions, and the reaction formula is as follows: 2Fe3 ++Fe＝3Fe2 +。
Optionally, the spraying post-treatment liquid is sprayed out through an atomizing nozzle, and the spraying post-treatment liquid is in a discontinuous liquid droplet state. The spraying post-treatment liquid comprises ferrous ions, and the first post-treatment liquid can be sprayed out through the atomizing nozzle, so that the first post-treatment liquid forms liquid beads after being sprayed out, the surface area of the liquid is increased, and the first post-treatment liquid can be better contacted with a second reactant.
Optionally, the third relative velocity includes a vector velocity of the spray post-treatment liquid and a vector velocity of the second reactant, the vector velocity of the spray post-treatment liquid is a velocity that ensures that the spray post-treatment liquid is in a discontinuous droplet state, and a ratio of usage amounts of the spray post-treatment liquid and the second reactant is 1: and (1) when the spraying time of the sprayed post-treatment solution is the same as the blowing time of the second reactant, the vector velocity of the second reactant is determined to be the same as the vector velocity of the sprayed leachate. Specifically, the method comprises the following steps.
Optionally, the third direction and the fourth direction have a projection angle of 120 degrees to 240 degrees on a horizontal plane, and the fifth direction is a direction perpendicular to the horizontal plane where the liquid level of the second mixed reactant is located when the second mixed reactant is standing. By setting the projection included angle of the third direction and the fourth direction on the same horizontal plane to be 120 degrees to 240 degrees, the sprayed post-treatment liquid can be contacted with the second reactant at a higher relative speed, and the mixing effect of the sprayed post-treatment liquid and the second reactant is improved.
It is noted that the terms "comprises" and "comprising," and any variations thereof, in the description and claims of this application and the description of the drawings are intended to cover non-exclusive inclusions. The terms "first," "second," and the like in the description and claims of this application or the accompanying drawings are used for distinguishing between different objects and not for describing a particular order. Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the application. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Reference herein to "further" means that the particular feature, structure, or characteristic may be further included in an embodiment, and may be combined with the embodiment as a single preferred embodiment, or multiple preferred embodiments. It is explicitly and implicitly understood by a person skilled in the art that the embodiments described herein or further embodiments may be combined with other embodiments.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The copper sludge treatment method is characterized by comprising the following steps:
s1, introducing water vapor into copper sludge to perform slurrying to obtain slurried copper sludge, and performing heat preservation leaching on the slurried copper sludge to obtain a copper sludge leachate and sludge residues, wherein the initial water content of the copper sludge is 40-60%, the initial temperature of the copper sludge is 30-50 ℃, the water content of the slurried copper sludge is 80-90%, and the temperature of the slurried copper sludge is 80-90 ℃;
s2, carrying out pressure filtration on the copper sludge leachate in a heat preservation environment to obtain a filtered copper sludge leachate;
s3, spraying the filtered copper sludge leachate in a first direction in a first reaction chamber to form a sprayed leachate, and blowing a first reactant in a second direction, where the first direction and the second direction have a crossing point, so that the first reactant and the sprayed leachate are mixed in the first reaction chamber at a first relative speed to obtain a first mixed reactant;
s4, standing and stirring the first mixed reactant in the first reaction cavity, wherein the standing time is 30 minutes, the stirring time is 10 minutes, the standing frequency is N times, and the stirring frequency is N-1 times, and when the content of copper ions in the liquid is detected to be reduced to a preset value during the standing period, performing solid-liquid separation to obtain a first post-treatment liquid and solid copper, wherein the solid copper is used for refining copper;
s5, spraying the first post-treatment liquid in a third direction in a second reaction cavity to form a sprayed post-treatment liquid, and blowing a second reactant in a fourth direction, wherein the third direction and the fourth direction have a cross point, so that the second reactant and the sprayed post-treatment liquid are cross-mixed in the second reaction cavity at a second relative speed to obtain a second mixed reactant;
and S6, stirring the second mixed reactant in the second reaction cavity, continuously adding the second reactant into the second mixed reactant from a fifth direction, detecting the content of the second reactant in the second mixed reactant in real time, stopping adding the second reactant when the content of the second reactant in the second mixed reactant is larger than the first content value, standing, and performing solid-liquid separation to obtain a second post-treatment liquid and a solid reactant, wherein the second post-treatment liquid is used for evaporation and crystallization, and the solid reactant is used for preparing the first reactant or the second reactant.
2. The copper sludge treatment method according to claim 1, further comprising, in step S1:
and adding the sludge residue into the original copper sludge, and preparing to obtain the hole sludge in the step S1.
3. The copper sludge treatment method according to claim 1, wherein the first reactant comprises a copper ion reactant, the copper ion reactant comprises elemental iron powder, and the first post-treatment liquid comprises ferrous ions generated by replacement of copper ions by elemental iron.
4. The copper sludge treatment method according to claim 3, wherein the spray leachate is sprayed through an atomizing nozzle, and the spray leachate is in a discontinuous liquid droplet state.
5. The copper sludge treatment process of claim 4 wherein the first relative velocity comprises a vector velocity of the spray leach solution and a vector velocity of the first reactant, the vector velocity of the spray leach solution being such that the spray leach solution is in a discrete droplet state, the ratio of the amount of the spray leach solution to the amount of the first reactant being 1: 1 to 1: 1.2, the spraying time of the spraying leachate is the same as the blowing time of the first reactant, and the vector velocity of the first reactant is determined to be 1 to 1.2 times of the vector velocity of the spraying leachate.
6. The copper sludge treatment method of claim 5, wherein the first direction and the second direction have an angle of 120 degrees to 240 degrees in a horizontal direction.
7. The copper sludge treatment method according to claim 3, wherein the second reactant comprises elemental iron powder, and the second post-treatment liquid comprises ferrous ions generated by reduction of ferric iron by the elemental iron.
8. The copper sludge treatment method according to claim 7, wherein the post-treatment liquid is sprayed through an atomizing nozzle, and the post-treatment liquid is in a discontinuous liquid droplet state.
9. The copper sludge treatment method according to claim 8, wherein the third relative velocity includes a vector velocity of the spray post-treatment liquid and a vector velocity of the second reactant, the vector velocity of the spray post-treatment liquid is a velocity that ensures that the spray post-treatment liquid is in a discontinuous droplet state, and the ratio of the amount of the spray post-treatment liquid to the amount of the second reactant is 1: and 1, when the spraying time of the sprayed post-treatment fluid is the same as the blowing time of the second reactant, determining that the vector velocity of the second reactant is the same as the vector velocity of the sprayed leaching fluid.
10. The copper sludge treatment method according to claim 8, wherein the third direction and the fourth direction have an angle of 120 degrees to 240 degrees in a horizontal direction, and the fifth direction is a direction perpendicular to a horizontal plane of a liquid surface of the second mixed reactant when the second mixed reactant is left standing.
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| CN106521166A (en) * | 2016-11-29 | 2017-03-22 | 湖南埃格环保科技有限公司 | Method for preparing copper powder and ferrous sulfate by using solution leached through sludge containing copper wet method |
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| JPS529623A (en) * | 1975-07-15 | 1977-01-25 | Hideo Koshimura | Process and apparatus for extracting and separating cu |
| CN103397190A (en) * | 2013-07-29 | 2013-11-20 | 紫金矿业集团股份有限公司 | Method for producing high-purity gold and copper sulphate from gold-bearing copper sludge |
| CN106521166A (en) * | 2016-11-29 | 2017-03-22 | 湖南埃格环保科技有限公司 | Method for preparing copper powder and ferrous sulfate by using solution leached through sludge containing copper wet method |
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