CN107661813B - Method for comprehensively recovering silver, lead and iron from electric precipitator dust - Google Patents
Method for comprehensively recovering silver, lead and iron from electric precipitator dust Download PDFInfo
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Abstract
The invention relates to a method for comprehensively recovering silver, lead and iron from electric precipitator dust, which comprises the following steps: I. water leaching and solid-liquid separation: firstly, leaching the electro-precipitator dust with water and carrying out solid-liquid separation treatment to obtain a solid 1 and a liquid 1 containing soluble salt; II. Flotation: and (3) pulping and mixed flotation are carried out on the solid 1 to obtain silver-lead concentrate and iron-containing tailings. The method mainly recovers silver and lead from the concentrate, enriches iron in the tailings and returns the iron to steel smelting, has simple process flow, low production cost and no environmental pollution, and is suitable for comprehensive resource utilization in steel smelting plants using iron ore with high silver and lead content as raw materials.
Description
Technical Field
The invention relates to a comprehensive utilization method of electric precipitator dust (also called sintering machine head dust), in particular to a method for comprehensively recovering silver, lead and iron from the electric precipitator dust.
Background
The electric precipitator dust is easy to cause environmental pollution and harm. For example, iron ore sintering or rotary hearth furnace cleaning operations in iron and steel plants are important processes for preparing charging materials for iron and steel production, and the electric precipitator dust is an inevitable product and also an important component of solid waste slag in iron and steel production. According to statistics, about 40 kg of electric precipitation dust is generated when 1 ton of sintered ore is produced. The iron and steel dust is rich in soluble salts and harmful elements such as copper, zinc, lead and the like, and can seriously affect the normal production of the original working procedure when being returned to a blast furnace for secondary utilization. And over time, the dust accumulation can cause environmental pollution. In addition, various valuable metal elements contained in the electric precipitator dust are not recycled, and the waste of resources is also caused. Therefore, the treatment and reasonable utilization of iron and steel dust such as electric dust removal ash are important contents for promoting environmental protection and developing circular economy.
Aiming at the valuable elements with high content in the electric dust removal ash, domestic steel enterprises develop related researches on resource utilization of other valuable elements aiming at the iron-containing dust and mud so as to achieve the aim of efficiently separating and recycling iron and other valuable elements. At present, three methods, namely a physical method, a fire method and a wet method, are mainly adopted for the comprehensive treatment of the electric precipitator dust, although the methods are still in the initial exploration stage at present.
Magnetic separation is mostly used in physical processes. The main metal element in the electric dedusting ash of the steel plant is iron element, iron concentrate is obtained by a mineral separation method mainly based on magnetic separation, and other valuable elements are enriched in tailings after magnetic separation, so that the purpose of comprehensive utilization is achieved, and more domestic steel enterprises have a precedent application.
The application of the fire method in the treatment of the dust and mud containing zinc is more, and the fire method is mainly divided into a cold-bonded pellet method, a circulating fluidized bed process (CBF process for short), a ring furnace process and a rotary kiln process (SPM process for short), and the latter two methods have the most representativeness.
The wet method is mainly used for treating dust and mud with high contents of zinc, potassium and the like, and is generally an alkali (acid) leaching method, a water dissolving method, a combined leaching method of ammonia and CO and the like.
In practice, more comprehensive research on methods is applied, for example, Liuxiong of Hunan puddle in China patent application CN200910227179.3 mentions a method for recovering lead from electric precipitator dust and preparing lead monoxide, and the method mainly adopts a flotation-magnetic separation-chloridizing leaching-precipitation roasting process to recover lead from electric precipitator dust.
At present, due to the influence of the economic downward pressure of mining industry, the comprehensive utilization of the electric precipitator dust by steel plants is more and more emphasized. The treatment process of the electric precipitator dust has stronger pertinence for recovering different valuable elements due to the complex chemical components of the electric precipitator dust. In combination with the actual steel plant, the research on the novel process for treating the electric precipitator dust has two basic conditions, and has significance for practical application. One is to have low cost, high recovery. The electric dedusting ash is used as an iron and steel smelting by-product, the output is limited, and the practical feasibility of the complex and difficult-to-control process is not high; meanwhile, the process also has to meet the requirement of higher recovery rate of the main elements of the process, so that the actual effect of comprehensive utilization can be achieved. And secondly, ensuring the environmental protection of the process. The electric precipitator dust is used as smelting waste slag, and the new process needs to avoid the problem of environmental pollution caused by the generation of new waste slag and waste materials as much as possible.
Disclosure of Invention
The invention aims to provide a method for comprehensively recovering silver, lead and iron from electric precipitator dust (hereinafter referred to as electric precipitator dust) in a steel plant. According to the method, the electric precipitation ash is firstly subjected to water leaching and solid-liquid separation treatment to obtain a solid part and a liquid part. The liquid is treated separately to recover the soluble salts. And (3) stirring and pulping the solid, and performing mixed flotation to obtain a mixed concentrate with a silver grade of more than 800g/t and a lead grade of more than 25%, and obtain tailings with an iron grade of 45-55%. The recovery rate of silver and lead in the concentrate is not lower than 85 percent. The method mainly recovers silver and lead from the concentrate, enriches iron in the tailings and returns the iron to steel smelting, has simple process flow, low production cost and no environmental pollution, and is suitable for comprehensive resource utilization in steel smelting plants using iron ore with high silver and lead content as raw materials.
According to one aspect of the invention, a method for comprehensively recovering silver, lead and iron from electric precipitator dust is provided, which comprises the following steps:
I. water leaching and solid-liquid separation: firstly, leaching the electro-precipitator dust by water, and carrying out solid-liquid separation treatment to obtain a solid 1 and a liquid 1 containing soluble salt;
II. Flotation: and (3) pulping and mixed flotation are carried out on the solid 1 to obtain silver-lead concentrate and iron-containing tailings.
The silver-lead concentrate can be used for silver-lead smelting, so that silver and lead are recovered. The iron-containing tailings can be used for iron and steel smelting, so that iron is recovered. The liquid 1 containing soluble salts may be treated to recover the soluble salts therein.
Thus, the method according to the invention may further comprise the step of performing silver-lead smelting to recover silver and lead.
The method according to the invention may further comprise the step of performing iron and steel smelting to recover iron.
The process according to the invention may further comprise the step of recovering the soluble salts in the soluble salt containing liquid 1.
FIG. 1 shows a schematic of a process scheme for the integrated recovery of silver, lead, iron and soluble salts from an electro-precipitator ash in accordance with the present invention.
The relevant contents are respectively described as follows.
I. Water leaching and solid-liquid separation.
Considering that the electric precipitator dust contains a large amount of soluble salt, if the electric precipitator dust is directly floated, the soluble salt is dissolved in the ore pulp, so that the flotation effect is influenced, and the aim of comprehensive utilization cannot be achieved, therefore, the electric precipitator dust is firstly treated by two steps of water leaching and solid-liquid separation.
When the water leaching treatment is performed, the solid-to-liquid ratio of the electro-precipitator ash to water may be about 1:0.5 to 1:10, preferably about 1:1 to 1:5, more preferably about 1:1.5 to 1:3, and most preferably about 1: 2. The time of the water leaching treatment (hereinafter referred to as "water leaching time") is not particularly limited as long as soluble salts can be leached out. For example, the water immersion time may be 20 minutes or more, 30 minutes or more, 40 minutes or more, or the like. The water immersion for an excessively long time does not increase the amount of the soluble salt leached, and therefore, the water immersion time may be 10 hours or less, 5 hours or less, 3 hours or less, 2 hours or less, or 1 hour or less, in view of the process efficiency.
And (3) carrying out solid-liquid separation treatment on the mixture subjected to water leaching to obtain wet solid 1 and liquid 1. The method for performing solid-liquid separation is not limited as long as the solid and the soluble salt-containing liquid can be separated. For example, solid-liquid separation can be carried out by filtration or sedimentation separation, for example, by a method such as atmospheric filtration, pressure filtration, vacuum filtration, centrifugal filtration, and centrifugal sedimentation. The solid-liquid separation may be performed using a settling tank, a vacuum filtration device, a plate-and-frame filtration device, a centrifugal sedimentation device, or the like.
After water leaching and solid-liquid separation treatment, the metal grade in the solid 1 can be generally improved by 20-25% compared with the original electric precipitator dust due to the dissolution of soluble salts in the electric precipitator dust.
II. Flotation
And pulping and mixed flotation are carried out on the solid 1 to obtain silver-lead concentrate and iron-containing tailings.
The flotation method for treating the electric precipitator dust requires that the proportion of solid dust with the granularity of less than 74 micrometers (less than 200 meshes) is more than 60 percent. Under the condition that the particle size of the electric precipitator dust does not meet the requirement, the ore grinding process can be carried out before stirring and pulping, so that the particle size of the electric precipitator dust meets the particle size requirement.
1. Pulping
Adding water into the solid 1, adding a flotation activating agent and a regulator, preferably stirring, and preparing into ore pulp for flotation.
In the step, the mass concentration of the ore pulp is preferably controlled to be 30-50%. Within the above mass concentration range, good flotation results can be obtained.
In this step, the adjusting agent is used for adjusting the pH value of the ore pulp and can be selected from sodium carbonate, sodium hydroxide and lime, and sodium carbonate is preferred. The conditioning agent may be used in an amount of about 0.8 to 2.8 kilograms per ton (kg/t), preferably 1.5kg/t, based on the mass of solids in the pulp. The pH value of the pulp is controlled to be in a range of about 6 to 12, preferably about 8 to 12, more preferably about 9 to 11, and especially about 9.5 to 10.5. Within the above pH range, a good flotation effect can be obtained.
In this step, the activator, which is used to improve the floatability of the useful mineral, may be selected from sodium sulphide and soda, preferably sodium sulphide. Based on the mass of the solid in the ore pulp, the dosage of the activating agent can be 2-10 kg/t, and is preferably 4 kg/t. Within the above range, a good activating effect can be obtained. In the case of too low or too high an activator, a reduction in the recovery rate may result.
The manner and time of stirring are not particularly limited as long as the electric fly ash can be uniformly mixed with the activator and the modifier. The stirring time is generally 5 to 30 minutes, preferably 15 minutes.
2. Mixed flotation
And performing mixed flotation operation on the pulp obtained by pulping to obtain silver-lead bulk concentrate and iron-containing tailings.
The hybrid flotation operation includes rougher flotation, scavenger flotation and optionally cleaner flotation.
The roughing is performed as follows: adding a collecting agent into the ore pulp obtained by stirring and pulping, and then carrying out flotation separation to obtain roughed concentrate and roughed tailings. The amount of collector used for roughing can be about 100-1000 grams per ton (g/t), preferably about 100-800 g/t, based on the mass of solids in the pulp. The number of roughing is not particularly limited, but may be performed 1 to 2 times, preferably 2 times, in view of time and cost. The foam product obtained after the roughing is roughed concentrate, and the product in the flotation tank is roughed tailings.
When the rough concentration is carried out for multiple times, tailings obtained by the previous rough concentration are used as raw materials in the subsequent rough concentration. And combining the rougher concentrates obtained by the first rougher flotation and the second rougher flotation to obtain final silver-lead bulk concentrates or further performing concentration. The type and amount of collector used in each rougher can be the same or different. Preferably, the same collector is used for each rougher and the amount is progressively reduced. In a preferred embodiment, the collector dosage for the first rougher flotation may be about 200 to 1000 grams per ton (g/t), preferably about 250 to 800g/t, especially about 250g/t, based on the mass of solids in the pulp. The amount of collector used for the second rougher flotation may be about 100-500 g/t, preferably about 100-300 g/t, especially about 150g/t, based on the mass of solids in the pulp. Within the above dosage range, a better flotation effect can be obtained.
The scavenging is performed as follows: and adding a collecting agent into the roughed tailings left in the flotation tank after roughing, and then performing flotation separation to obtain scavenged middlings and scavenged tailings. Based on the mass of the solids in the ore pulp, the amount of the scavenging collector can be about 50-300 g/t, preferably about 50-200 g/t, and more preferably about 50-150 g/t. The number of times of scavenging is not particularly limited, but may be 1 to 2 times, preferably 1 time, in view of time and cost. And obtaining a foam product after scavenging, namely scavenging middlings, and obtaining a product in the flotation tank, namely scavenging tailings.
When the scavenging is carried out for a plurality of times, the tailings obtained by the previous scavenging are used as raw materials in the later scavenging. Returning the middlings in the 1 st scavenging to the previous-stage roughing; and (4) returning the middlings in the 2 nd and later scavenging to the last scavenging in sequence. And the product in the flotation tank after the last scavenging is the iron-containing tailings. The type and amount of collector used in each sweep may be the same or different. Preferably, the same collector is used for each sweep and the amount is progressively reduced. In a preferred embodiment, the amount of collector used for the first sweep may be about 50-300 g/t, preferably about 50-200 g/t, and more preferably about 50-150 g/t, based on the mass of solids in the slurry. Based on the mass of the solids in the ore pulp, the amount of the collector used for the second scavenging can be about 50-150 g/t, preferably about 50-100 g/t. Within the above dosage range, a better flotation effect can be obtained.
The concentration refers to a process of adding a collecting agent into rough concentrate obtained after rough concentration and then carrying out flotation separation. The concentration times can be determined according to the actual requirement on the concentrate grade, and can be carried out for 0-2 times. The concentration times can be increased appropriately to obtain a higher grade concentrate. The foam product obtained after the concentration is the concentrated concentrate, and the product in the flotation tank is the concentrated tailings.
When concentration is performed multiple times, the tailings of the previous concentration are used as raw materials in the subsequent concentration. Returning the 1 st fine concentration tailings to rough concentration; and returning the tailings of the 2 nd and later concentration to the last concentration in sequence. And finally, the concentrated concentrate obtained by concentration for the last time is the silver-lead bulk concentrate. The type and amount of collector used in each concentration can be the same or different. Preferably, the same collector is used for each concentration and the amount is progressively reduced. In a preferred embodiment, the collector dosage for the first concentration may be about 0-100 g/t, preferably about 10-80 g/t, based on the mass of solids in the slurry. The amount of collector used for the second concentration can be about 0-50 g/t, preferably about 0-25 g/t, based on the mass of solids in the pulp. Within the above dosage range, a better flotation effect can be obtained.
In the flotation, a collecting agent is required to be used for collecting useful minerals, and the collecting agent can be one or more selected from ethionam, butyl sodium xanthate, butylamine black powder and the like, and is preferably a mixture of ethionam and butylamine black powder. In the mixture of ethionamide and butylamine black, the weight ratio of ethionamide to butylamine black is preferably from about 0.5 to about 2:1, more preferably from about 0.5 to about 1.5:1, especially about 1:1.
The types of collectors used in the roughing, scavenging and polishing may be the same or different, and preferably the same collector is used.
There is no particular limitation on the time required for the collective flotation. Generally speaking, the roughing operation time is about 14 to 20 minutes, the scavenging operation time is about 5 to 8 minutes, and the concentration operation time can be about 0 to 7 minutes according to actual needs.
In one embodiment, as shown in figure 2, the bulk flotation according to the invention comprises two roughers and one scavenger, in particular as follows:
(1) roughly selecting one: adding a collecting agent into the pulp obtained by pulping according to the proportion of about 200-1000 g/t based on the mass of solids in the pulp, and performing flotation separation to obtain rougher concentrate 1 and rougher tailings 1;
(2) and (4) rough selection of two: adding a collecting agent into the rougher tailings 1 according to the proportion of about 100-500 g/t based on the mass of solids in the ore pulp, and performing flotation separation to obtain rougher concentrates 2 and rougher tailings 2;
(3) sweeping: adding a collecting agent into the rougher tailings 2 according to the proportion of about 50-300 g/t based on the mass of solids in the ore pulp to obtain middlings 1 and iron-containing tailings, and returning the middlings 1 to the step (2) to be mixed with the tailings 1;
(4) and combining the roughing concentrate 1 and the roughing concentrate 2 to obtain the silver-lead concentrate.
In another embodiment, as shown in fig. 3, the bulk flotation according to the invention comprises two roughers, one scavenger and one cleaner, in particular as follows:
(1) roughly selecting one: adding a collecting agent into the pulp obtained by pulping according to the proportion of about 200-1000 g/t based on the mass of solids in the pulp, and performing flotation separation to obtain rougher concentrate 1 and rougher tailings 1;
(2) and (4) rough selection of two: adding a collecting agent into the rougher tailings 1 according to the proportion of about 100-500 g/t based on the mass of solids in the ore pulp, and performing flotation separation to obtain rougher concentrates 2 and rougher tailings 2;
(3) sweeping: adding a collecting agent into the rougher tailings 2 according to the proportion of about 50-300 g/t based on the mass of solids in the ore pulp to obtain middlings 1 and iron-containing tailings, and returning the middlings 1 to the step (2) to be mixed with the rougher tailings 1;
(4) selecting: and (3) merging the roughing concentrate 1 and the roughing concentrate 2, adding a collecting agent according to the proportion of about 0-100 g/t based on the mass of solids in the ore pulp, performing flotation separation to obtain silver-lead concentrate and concentration tailings 1, and returning the concentration tailings 1 to the step (1) to be mixed with the ore pulp obtained by pulping.
In yet another embodiment, as shown in fig. 4, the bulk flotation according to the invention comprises two roughenings, one sweep and two beneficiations, in particular as follows:
(1) roughly selecting one: adding a collecting agent into the pulp obtained by pulping according to the proportion of about 200-1000 g/t based on the mass of solids in the pulp, and performing flotation separation to obtain rougher concentrate 1 and rougher tailings 1;
(2) and (4) rough selection of two: adding a collecting agent into the rougher tailings 1 according to the proportion of about 100-500 g/t based on the mass of solids in the ore pulp, and performing flotation separation to obtain rougher concentrates 2 and rougher tailings 2;
(3) sweeping: adding a collecting agent into the rougher tailings 2 according to the proportion of about 50-300 g/t tailings 2 based on the mass of solids in the ore pulp to obtain middlings 1 and iron-containing tailings, and returning the middlings 1 to the step (2) to be mixed with the rougher tailings 1;
(4) selecting one: combining the roughing concentrate 1 and the roughing concentrate 2, adding a collecting agent according to the proportion of about 0-100 g/t based on the mass of solids in the ore pulp, performing flotation separation to obtain a concentrating concentrate 1 and a concentrating tailing 1, and returning the concentrating tailing 1 to the step (1) to be mixed with the ore pulp obtained by pulping
(5) Selecting two: and (3) adding a collecting agent into the concentrated concentrate 1 according to the proportion of about 0-50 g/t based on the mass of the solids in the ore pulp, performing flotation separation to obtain silver-lead concentrate and concentrated tailings 2, and returning the concentrated tailings 2 to the step (4) to mix with the rough concentrate 1 and the rough concentrate 2.
III, silver, lead, iron and soluble salt recovery
The silver-lead concentrate can be used for silver-lead smelting, so that silver and lead are recovered. The iron-containing tailings can be used for iron and steel smelting, so that iron is recovered. The liquid 1 containing soluble salts may be treated to recover the soluble salts therein.
The method of silver-lead smelting and steel smelting is not particularly limited and may be performed using techniques and equipment well known in the related art, and thus, will not be described in detail.
The soluble salt-containing liquid 1 can be treated by chemical means to recover the soluble salt product. The recovered soluble salt product may be prepared into a potassium fertilizer, or may be a potassium salt product such as potassium chloride, potassium sulfate, potassium nitrate, potassium dihydrogen phosphate, or the like. The chemical treatment method is not particularly limited as long as the desired product can be obtained. For example, there may be a method of preparing a potassium fertilizer or a potassium salt product as disclosed in, for example, CN104609443A, CN101723713A, CN101519218A, CN101234766A and the like.
The main technical advantages of the invention are as follows:
1. simple technological process, low production cost and high metal recovery rate. Because the particle size of the electric precipitator dust is fine, crushing and ore grinding are not needed, the ore dressing process is directly completed through mixed flotation after stirring, the recovery rate of the silver and the lead in the concentrate is not lower than 85 percent, and the recovery rate of the main element iron in the tailings is not lower than 90 percent.
2. Environmental protection and high efficiency. The process flow only forms two products of the silver-lead concentrate and the iron-containing tailings, and for an iron and steel plant, the iron-containing tailings can return to the iron and steel smelting flow while the silver-lead product is sorted out. In addition, when the method is put into practical application, wastewater generated by dehydration of concentrate and tailings can be collected and recycled by water leaching and flotation of the returned electro-precipitator dust, and discharge and pollution are avoided.
Drawings
FIG. 1 is a schematic diagram of a process for the integrated recovery of silver, lead and iron from an electro-precipitator ash according to an embodiment of the present invention.
Figure 2 is a flow diagram of a hybrid flotation process including two roughenings and one sweep according to one embodiment of the present invention.
Figure 3 is a flow diagram of a hybrid flotation process including two roughenings, one sweep and one concentration according to one embodiment of the present invention.
Figure 4 is a flow diagram of a hybrid flotation process including two roughenings, one sweep and two beneficiating according to one embodiment of the present invention.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Reagent:
the raw material electro-precipitator dust is sintering machine head dust of a steel plant, wherein particles with the particle size of less than 74 mu m account for 62.5 percent; wherein the grades of three main metal elements of silver, lead and iron are respectively 208g/t, 6.2 percent and 27.2 percent.
The flotation activating agent is sodium sulfide;
the regulator is sodium carbonate.
Collecting agents are butylamine black powder and ethion nitrogen in a weight ratio of 1:1
Example one
The experiment for the comprehensive recovery of silver, lead and iron was carried out according to the mixed flotation process comprising two roughenings and one scavenging as shown in figure 2.
Firstly, carrying out water immersion treatment on sintering machine head ash according to a solid-liquid ratio of 1:2, wherein the water immersion time is 30min, filtering to obtain wet solid 1 and liquid 1, the water content in the wet solid 1 is about 10-12%, and the liquid 1 is remained.
Adding water into the wet solid 1, stirring to prepare ore pulp with the mass concentration of about 33.3%, adding a flotation activating agent and a 1kg/t regulator according to the mass of solids in the ore pulp, and adjusting the pH value of the ore pulp to about 11, wherein the stirring time is 15 min.
And adding a collecting agent into the pulp obtained by pulping according to the proportion of about 250g/t based on the mass of the solid in the pulp, and performing flotation separation to obtain rougher concentrate 1 and rougher tailings 1.
And adding a collecting agent into the rougher tailings 1 according to the proportion of about 150g/t based on the mass of the solids in the ore pulp, and performing flotation separation to obtain rougher concentrates 2 and rougher tailings 2.
Based on the mass of the solid in the ore pulp, collecting agent is added into the rougher tailings 2 according to the proportion of about 100g/t to obtain middlings 1 and iron-containing tailings, and the middlings 1 are returned to the step to be mixed with the rougher tailings 1.
And combining the roughing concentrate 1 and the roughing concentrate 2 to obtain the silver-lead concentrate.
The finally obtained silver-lead concentrate and the iron-containing tailings are considered as test samples, and the test results are shown in table 1.
TABLE 1 example flotation results
Example two:
the experiment for the comprehensive recovery of silver, lead and iron was carried out according to the mixed flotation process comprising two roughenings, one scavenging and one concentrating as shown in figure 3.
Firstly, carrying out water immersion treatment on sintering machine head ash according to a solid-liquid ratio of 1:2, wherein the water immersion time is 30min, filtering to obtain wet solid 1 and liquid 1, the water content in the wet solid 1 is about 10-12%, and the liquid 1 is remained.
Adding water into the wet solid 1, stirring to prepare ore pulp with the mass concentration of about 33.3%, adding a flotation activating agent and a 1kg/t regulator according to the mass of solids in the ore pulp, and adjusting the pH value of the ore pulp to about 11, wherein the stirring time is 15 min.
And adding a collecting agent into the pulp obtained by pulping according to the proportion of about 250g/t based on the mass of the solid in the pulp, and performing flotation separation to obtain rougher concentrate 1 and rougher tailings 1.
And adding a collecting agent into the rougher tailings 1 according to the proportion of about 150g/t based on the mass of the solids in the ore pulp, and performing flotation separation to obtain rougher concentrates 2 and rougher tailings 2.
Based on the mass of the solid in the ore pulp, collecting agent is added into the rougher tailings 2 according to the proportion of about 100g/t to obtain middlings 1 and iron-containing tailings, and the middlings 1 are returned to be mixed with the rougher tailings 1.
And combining the roughing concentrate 1 and the roughing concentrate 2, adding a collecting agent according to the proportion of about 50g/t based on the mass of solids in the ore pulp, performing flotation separation to obtain silver-lead concentrate and concentration tailings 1, and returning the concentration tailings 1 to be mixed with the ore pulp obtained by pulping.
The finally obtained silver-lead concentrate and the iron-containing tailings are considered as test samples, and the test results are shown in table 2.
TABLE 2 flotation results of example two
Example three:
the experiments for the comprehensive recovery of silver, lead and iron were carried out according to the mixed flotation process of figure 4 including two roughenings, one scavenging and two beneficiating.
Firstly, carrying out water immersion treatment on sintering machine head ash according to a solid-liquid ratio of 1:2, wherein the water immersion time is 30min, filtering to obtain wet solid 1 and liquid 1, the water content in the wet solid 1 is about 10-12%, and the liquid 1 is remained.
Adding water into the wet solid 1, stirring to prepare ore pulp with the mass concentration of about 33.3%, adding a flotation activating agent and a 1kg/t regulator according to the mass of solids in the ore pulp, and adjusting the pH value of the ore pulp to about 11, wherein the stirring time is 15 min.
And adding a collecting agent into the pulp obtained by pulping according to the proportion of about 250g/t based on the mass of the solid in the pulp, and performing flotation separation to obtain rougher concentrate 1 and rougher tailings 1.
And adding a collecting agent into the rougher tailings 1 according to the proportion of about 150g/t based on the mass of the solids in the ore pulp, and performing flotation separation to obtain rougher concentrates 2 and rougher tailings 2.
Based on the mass of the solids in the ore pulp, collecting agents are added into the rougher tailings 2 according to the proportion of about 100g/t, middlings 1 and iron-containing tailings are obtained through flotation separation, and the middlings 1 are returned to be mixed with the rougher tailings 1.
Combining the roughing concentrate 1 and the roughing concentrate 2, adding a collecting agent according to the proportion of about 50g/t based on the mass of solids in the ore pulp, performing flotation separation to obtain a concentrating concentrate 1 and a concentrating tailing 1, and returning the concentrating tailing 1 to the step (1) to be mixed with the ore pulp obtained by pulping;
and (3) performing flotation operation on the concentrated concentrate 1 again without adding any collecting agent to obtain silver-lead concentrate and concentrated tailings 2, and returning the concentrated tailings 2 to be mixed with the rough concentrate 1 and the rough concentrate 2.
The finally obtained silver-lead concentrate and the iron-containing tailings are considered as test samples, and the test results are shown in table 3.
TABLE 3 results of flotation in example III
Example four:
experiments were carried out in the same manner as in the example two, except that no collector was added during the flotation operation after the rougher concentrate 1 and the rougher concentrate 2 were combined.
The finally obtained silver-lead concentrate and the iron-containing tailings are considered as test samples, and the test results are shown in table 4.
TABLE 4 flotation results of example IV
Example five:
the experiment was carried out in the same way as in the example, except that when the concentrate 1 was again subjected to flotation, a collector was added at a rate of about 25g/t, based on the mass of solids in the pulp.
The finally obtained silver-lead concentrate and the iron-containing tailings are considered as test samples, and the test results are shown in table 5.
TABLE 5 flotation results of example V
Claims (51)
1. A method for comprehensively recovering silver, lead and iron from electric precipitator dust comprises the following steps:
I. water leaching and solid-liquid separation: firstly, leaching the electro-precipitator dust with water and carrying out solid-liquid separation treatment to obtain a solid 1 and a liquid 1 containing soluble salt;
wherein, when the water leaching treatment is carried out, the solid-to-liquid ratio of the electro-precipitator dust to the water is 1:0.5 to 1: 10; the time of water leaching treatment is more than 20 minutes;
II. Flotation: the solid 1 is pulped and mixed floated to obtain silver-lead concentrate and iron-containing tailings,
wherein the pulping is carried out as follows: adding water into the solid 1, adding a flotation activating agent and a regulator into the mixture to prepare ore pulp for flotation, controlling the mass concentration of the ore pulp to be 30-50%, wherein the regulator is selected from sodium carbonate, sodium hydroxide and lime, the activating agent is selected from sodium sulfide and soda, the dosage of the regulator is 0.8-2.8 kg/t and the dosage of the activating agent is 2-10 kg/t based on the mass of the solid in the ore pulp,
the mixed flotation comprises 1-2 times of roughing, 1-2 times of scavenging and 0-2 times of fine separation;
the roughing is performed as follows: adding a collecting agent into the ore pulp obtained by stirring and pulping, and then carrying out flotation separation to obtain roughed concentrate and roughed tailings; based on the mass of solids in the ore pulp, the using amount of a collecting agent for rough separation is 100-1000 g/t;
the scavenging is performed as follows: adding a collecting agent into the roughed tailings left in the flotation tank after roughing, and then performing flotation separation to obtain scavenged middlings and scavenged tailings; based on the mass of solids in the ore pulp, the using amount of the scavenging collector is 50-300 g/t,
the concentration is carried out as follows: adding a collecting agent into the rough concentration obtained after rough concentration, then carrying out flotation separation to obtain concentrated concentrate and concentrated tailings,
the collecting agent is one or more selected from ethidium nitrate, butyl sodium xanthate and butylamine black powder.
2. The method of claim 1, wherein the solid to liquid ratio of the electro-precipitator ash to water is from 1:1 to 1: 5.
3. The method of claim 1, wherein the solid to liquid ratio of the electro-precipitator ash to water is from 1:1.5 to 1: 3.
4. The method of claim 1, wherein the solids to liquid ratio of the electro-precipitator ash to water is 1: 2.
5. The method according to claim 1, wherein the water leaching treatment is carried out for 30 minutes or more.
6. The method according to claim 1, wherein the water leaching treatment is carried out for 40 minutes or more.
7. The method according to claim 1, wherein the proportion of solid dust having a particle size of the electric precipitator dust of less than 74 μm is 60% or more.
8. The method according to claim 1, further comprising the step of performing a grinding process prior to the agitated pulping.
9. The method of claim 1, wherein the modifying agent is sodium carbonate.
10. The method of claim 1, wherein the pH value of the ore pulp is controlled to be in a range of 6-12 by using the regulator.
11. The method of claim 1, wherein the pH value of the ore pulp is controlled to be in a range of 8-12 by using the regulator.
12. The method of claim 1, wherein the pH value of the ore pulp is controlled to be in a range of 9-11 by using the regulator.
13. The method of claim 1, wherein the pH value of the ore pulp is controlled to be in a range of 9.5-10.5 by using the regulator.
14. The method of claim 1, wherein the activator is sodium sulfide.
15. The method according to claim 1, wherein the rougher collector is used in an amount of 100-800 g/t based on the mass of solids in the pulp.
16. The method of claim 1, wherein the number of roughers is 2.
17. The process according to claim 16, wherein when the rougher flotation is performed a plurality of times, the tailings obtained from the previous rougher flotation are used as raw materials in the later rougher flotation; and combining the rougher concentrates obtained by the first rougher flotation and the second rougher flotation to obtain final silver-lead bulk concentrates or further performing concentration.
18. A method according to claim 16 wherein the same collector is used for each rougher pass and the amount is progressively reduced.
19. A method according to claim 16 wherein the first rougher is used in an amount of 200 to 1000g/t of collector based on the mass of solids in the pulp.
20. A method according to claim 16 wherein the first rougher is used in an amount of 250 to 800g/t of collector based on the mass of solids in the pulp.
21. A method according to claim 16 wherein the second rougher application is from 100 to 500g/t of collector based on the mass of solids in the pulp.
22. A method according to claim 16 wherein the second rougher pick has a collector dosage of 100 to 300g/t based on the mass of solids in the pulp.
23. The method according to claim 1, wherein the scavenger is used in an amount of 50 to 200g/t based on the mass of solids in the pulp.
24. The method according to claim 1, wherein the scavenger is used in an amount of 50 to 150g/t based on the mass of solids in the pulp.
25. The method of claim 1, wherein the number of sweeps is 1.
26. The method of claim 1, wherein when a plurality of scavenging is carried out, the tailings obtained from the previous scavenging are used as raw materials in the later scavenging, and the middlings in the 1 st scavenging are returned to the previous-stage roughing; returning the middlings in the 2 nd scavenging to the last scavenging; and the product in the flotation tank after the last scavenging is the iron-containing tailings.
27. A method according to claim 26 wherein the same collector is used for each sweep and the dose is progressively reduced.
28. The method according to claim 26, wherein the collector dosage for the 1 st sweep is 50-300 g/t based on the mass of solids in the pulp.
29. The method according to claim 26, wherein the collector dosage for the 1 st sweep is 50-200 g/t based on the mass of solids in the pulp.
30. The method according to claim 26, wherein the collector dosage for the 1 st sweep is 50-150 g/t based on the mass of solids in the pulp.
31. The method according to claim 26, wherein the 2 nd sweep uses 50-150 g/t of collector based on the mass of solids in the pulp.
32. The method according to claim 26, wherein the 2 nd sweep uses 50-100 g/t of collector based on the mass of solids in the pulp.
33. The method of claim 1, wherein when performing a plurality of beneficiations, a post-beneficiation uses tailings of a previous beneficiation as a feedstock; returning the 1 st fine concentration tailings to rough concentration; returning the tailings of the 2 nd concentration to the last concentration; and finally, the concentrated concentrate obtained by concentration for the last time is the silver-lead bulk concentrate.
34. A method according to claim 33 wherein the same collector is used for each concentration and the amount is progressively reduced.
35. The method according to claim 33, wherein the collector dosage for 1 st beneficiating is 0-100 g/t based on the mass of solids in the pulp.
36. The method according to claim 33, wherein the collector dosage for 1 st beneficiating is 10-80 g/t based on the mass of solids in the pulp.
37. The method according to claim 33, wherein the collector dosage for the 2 nd concentrating is 0-50 g/t based on the mass of solids in the pulp.
38. The method according to claim 33, wherein the collector dosage for the 2 nd concentrating is 0-25 g/t based on the mass of solids in the pulp.
39. A method according to claim 1 wherein the same collector is used in roughing, scavenging and concentrating.
40. The method according to claim 1, wherein the roughing operation time is 14 to 20 minutes in total, the scavenging operation time is 5 to 8 minutes in total, and the concentrating operation time is 0 to 7 minutes.
41. The method of claim 1, wherein the bulk flotation is carried out according to one of the following routes:
route one: the method comprises two times of rough concentration and one time of scavenging, and specifically comprises the following steps:
(1) roughly selecting one: adding a collecting agent into the pulp obtained by pulping according to the proportion of 200-1000 g/t based on the mass of solids in the pulp, and performing flotation separation to obtain roughed concentrate 1 and roughed tailings 1;
(2) and (4) rough selection of two: adding a collecting agent into the rougher tailings 1 according to the proportion of 100-500 g/t based on the mass of solids in the ore pulp, and performing flotation separation to obtain rougher concentrates 2 and rougher tailings 2;
(3) sweeping: adding a collecting agent into the rougher tailings 2 according to the proportion of 50-300 g/t based on the mass of solids in the ore pulp to obtain middlings 1 and iron-containing tailings, and returning the middlings 1 to the step (2) to be mixed with the tailings 1;
(4) combining the roughing concentrate 1 and the roughing concentrate 2 to obtain silver-lead concentrate;
and a second route: the method comprises two times of rough concentration, one time of scavenging and one time of fine concentration, and specifically comprises the following steps:
(1) roughly selecting one: adding a collecting agent into the pulp obtained by pulping according to the proportion of 200-1000 g/t based on the mass of solids in the pulp, and performing flotation separation to obtain roughed concentrate 1 and roughed tailings 1;
(2) and (4) rough selection of two: adding a collecting agent into the rougher tailings 1 according to the proportion of 100-500 g/t based on the mass of solids in the ore pulp, and performing flotation separation to obtain rougher concentrates 2 and rougher tailings 2;
(3) sweeping: adding a collecting agent into the rougher tailings 2 according to the proportion of 50-300 g/t based on the mass of solids in the ore pulp to obtain middlings 1 and iron-containing tailings, and returning the middlings 1 to the step (2) to be mixed with the rougher tailings 1;
(4) selecting: combining the roughing concentrate 1 and the roughing concentrate 2, adding a collecting agent according to the proportion of 0-100 g/t based on the mass of solids in the ore pulp, performing flotation separation to obtain silver-lead concentrate and concentration tailings 1, and returning the concentration tailings 1 to the step (1) to be mixed with the ore pulp obtained by pulping;
and a third route: the method comprises two times of rough concentration, one time of scavenging and two times of fine concentration, and specifically comprises the following steps:
(1) roughly selecting one: adding a collecting agent into the pulp obtained by pulping according to the proportion of 200-1000 g/t based on the mass of solids in the pulp, and performing flotation separation to obtain roughed concentrate 1 and roughed tailings 1;
(2) and (4) rough selection of two: adding a collecting agent into the rougher tailings 1 according to the proportion of 100-500 g/t based on the mass of solids in the ore pulp, and performing flotation separation to obtain rougher concentrates 2 and rougher tailings 2;
(3) sweeping: adding a collecting agent into the rougher tailings 2 according to the proportion of 50-300 g/t tailings 2 based on the mass of solids in the ore pulp to obtain middlings 1 and iron-containing tailings, and returning the middlings 1 to the step (2) to be mixed with the rougher tailings 1;
(4) selecting one: combining the roughing concentrate 1 and the roughing concentrate 2, adding a collecting agent according to the proportion of 0-100 g/t based on the mass of solids in the ore pulp, performing flotation separation to obtain a concentrating concentrate 1 and a concentrating tailing 1, and returning the concentrating tailing 1 to the step (1) to be mixed with the ore pulp obtained by pulping
(5) Selecting two: and (3) adding a collecting agent into the concentrated concentrate 1 according to the proportion of 0-50 g/t based on the mass of the solids in the ore pulp, performing flotation separation to obtain silver-lead concentrate and concentrated tailings 2, and returning the concentrated tailings 2 to the step (4) to mix with the rough concentrate 1 and the rough concentrate 2.
42. A method according to claim 1 or 41 wherein the collector is a mixture of ethidium and butylamine black.
43. The method of claim 42, wherein the weight ratio of ethionamide to butylamine as black drug is 0.5-2: 1.
44. The method of claim 43, wherein the weight ratio of ethionamide to butylamine as black drug is 0.5-1.5: 1.
45. A method according to claim 42 wherein the collector is a 1:1 mixture of ethidium and butylamine black.
46. The method of claim 1, further comprising:
a step of performing silver-lead smelting to recover silver and lead; and/or
And (3) performing iron and steel smelting to recover iron.
47. The method of claim 1, further comprising the step of recovering the soluble salts in the soluble salt-containing liquid 1.
48. The method of claim 47, wherein the soluble salt-containing liquid 1 is treated by chemical means to recover a soluble salt product.
49. The method of claim 48, wherein the recovered soluble salt product is made into a potassium fertilizer.
50. The method of claim 48, wherein the recovered soluble salt product is formed into a potassium salt product.
51. The method of claim 50, wherein the potassium salt is selected from the group consisting of potassium chloride, potassium sulfate, potassium nitrate, potassium dihydrogen phosphate.
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