CN115572814A - Sintering machine head ash multistage separation process - Google Patents
Sintering machine head ash multistage separation process Download PDFInfo
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- CN115572814A CN115572814A CN202211305157.6A CN202211305157A CN115572814A CN 115572814 A CN115572814 A CN 115572814A CN 202211305157 A CN202211305157 A CN 202211305157A CN 115572814 A CN115572814 A CN 115572814A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
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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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
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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
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/02—Working-up flue dust
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to the technical field of chemical industry, and provides S1 pulping: weighing sintering machine head ash by using a quantitative feeder, conveying the sintering machine head ash to a grinding and screening integrated machine, adding quantitative water or ore pulp water, mixing and stirring for 20min-40min to form mortar, wherein the weight ratio of the sintering machine head ash to the water is 1:1-1; s2, grinding: conveying the mortar in the step S1 to a tower mill for grinding, and grinding the mortar with uniform granularity; s3, low-intensity magnetic separation: magnetically separating the mortar in the step S2 by a low-intensity magnetic separator; s4, strong magnetic separation: carrying out magnetic separation again on the mortar subjected to the low-intensity magnetic separation by using a strong magnetic separator, and obtaining tail slurry after the magnetic separation; s5, alkali metal removal: carrying out solid-liquid separation on the tail slurry through a first thickening tank; the supernatant liquor passes through a second thickening tank again and then is evaporated and crystallized; s6, extracting copper and lead; s7, extracting gold and silver; through above-mentioned technical scheme, the metal recovery rate is low among the prior art has been solved, the great problem of waste that causes.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a sintering machine head ash multistage separation process.
Background
The steel production in China is mainly carried out in a long flow of a blast furnace and a converter, the sintered ore accounts for about 70-75% of the blast furnace burden, the dust generation amount in the sintering process accounts for about 1-2% of the total amount of the sintered ore, the annual sintering fly ash yield exceeds ten million tons, and the quantity is huge.
The dust removal of the sintering plant comprises two types of industrial dust removal ash and environmental dust removal ash, the process dust removal ash is divided into machine head dust removal ash and machine tail dust removal ash, and the sources of different dusts are as follows:
1. dust removal of a sintering machine head: because the sintering raw materials contain a large amount of fine materials, the materials enter the main pipeline through air draft to become powder tips, most of the powder tips are collected by the tip removing system, and a small amount of the powder tips are discharged along with smoke.
2. Dust removal at the tail of a sintering machine: dust generated in the processes of unloading, crushing and cooling of the sintered ore fired on the sintering machine is collected by a dust removal system.
3. Environmental dedusting ash: the method comprises dust generated during ore unloading at the tail part of a cooler, dust generated during the process that the sinter enters a screening system to screen, dust generated during the process of screening the sinter and dust generated during the process of transporting the sinter.
The dust removed by the sintering machine head refers to dust collected by an electric dust collector in a sintering process, and alkali metal enrichment can be caused if the dust is directly returned to sintering for use, and the dust is commonly called as 'grate bar pasting', so that the yield and the quality of sintered ore are reduced. In addition, the head ash contains iron, lead and a small amount of valuable elements such as gold, silver and the like. Iron powder is usually recovered through a magnetic separation process in the production process and recycled, but the recovery rate of the iron powder after magnetic separation is only 82.3%, and direct discharge can not only cause resource waste, but also pollute the environment.
Disclosure of Invention
The invention provides a sintering machine head ash multistage separation process, which solves the problems of low metal recovery rate and large waste in the related technology.
The technical scheme of the invention is as follows:
the sintering machine head ash multistage separation process comprises the following steps
S1, pulping: weighing sintering machine head ash by using a quantitative feeder, conveying the sintering machine head ash to a grinding and screening integrated machine, adding quantitative water or ore pulp water, mixing and stirring for 20min-40min to form mortar, wherein the weight ratio of the sintering machine head ash to the water is 1:1-1;
s2, grinding: conveying the mortar in the step S1 to a tower mill for grinding, and grinding the mortar with uniform granularity;
s3, low-intensity magnetic separation: magnetically separating the mortar in the step S2 by a low-intensity magnetic separator;
s4, strong magnetic separation: carrying out magnetic separation again on the mortar subjected to the low-intensity magnetic separation by using a strong magnetic separator, and obtaining tail slurry after the magnetic separation;
s5, alkali metal removal: carrying out solid-liquid separation on the tail slurry through a first thickening tank; the supernatant liquid passes through the second thickening tank again and then is evaporated and crystallized;
s6, extracting copper and lead: adding the bottom slurry of the lower layer after solid-liquid separation in the step S5 into a high-temperature reaction kettle, and synchronously adding hydrochloric acid and a sodium carbonate solution for reaction, wherein the reaction temperature is controlled to be 120-150 ℃, and the reaction time is 30-50 min; separating the reacted solution by a centrifugal machine to obtain filtrate and precipitate; conveying the separated filtrate into a cooling reaction kettle, adding excessive ammonium bicarbonate for reaction, then adding sodium sulfide, obtaining a precipitate of a copper compound after reaction, filtering out the precipitate of the copper compound, adding a mixed solution of hydrochloric acid and sodium chloride into the solution, stirring for 30-40 min at 85-90 ℃ to obtain a lead compound precipitate and a copper ion solution, adding excessive sodium hydroxide into the solution again to obtain a copper compound precipitate, and filtering again to obtain tailing slurry;
s7, extracting gold and silver: adding the tailing slurry obtained in the step S6 into a reaction kettle, simultaneously adding an environment-friendly gold extraction agent for reaction, keeping the pH value at 9-12, stirring for 25-35 min every 4.8-8 h, soaking zinc wires in the supernatant of the static mortar C after adding the environment-friendly gold extraction agent for 24h, and soaking for 2-4 h every time; stirring and soaking for 8-20 days, electrolyzing the replaced zinc wire, and smelting to obtain gold ingots and silver ingots.
As a further technical scheme, in the step S3, the dust and mud associated with the iron powder obtained by the low-intensity magnetic separation are separated by a cyclone, and the dust and mud are separated by the low-intensity magnetic separator again; in the step S4, the iron powder obtained by the strong magnetic separation is separated from dust and mud associated with the iron powder by a cyclone, and the dust and mud are separated by a strong magnetic separator again; and adding the obtained iron powder into a vacuum filter for dehydration.
As a further technical scheme, water is added into the reaction kettle in the step S7, and the water flows from the bottom to the top of the reaction kettle.
As a further technical scheme, two crystallization temperatures are set in the evaporation crystallization process in the step S5, and the two crystallization temperatures obtain the potassium salt and the sodium salt respectively.
As a further technical scheme, the environment-friendly gold extraction agent comprises one or more of five-membered cyclic imide, carbamide, sodium carbide cyanurate and sodium humate.
The working principle and the beneficial effects of the invention are as follows:
1. the whole process flow is closed, the materials are used, reasonable utilization can be realized after each element is extracted, waste is turned into wealth, and the utilization rate is extremely high.
2. The recovery rate of potassium and sodium reaches 98%, and the extraction rate of gold and silver can reach more than 90%, thus reducing resource waste.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a process flow diagram 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 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 be included within the scope of protection of the present invention.
Example 1
As shown in fig. 1, the present embodiment provides a multi-stage sorting process for sintering machine head ash, wherein firstly, sintering machine head ash is transported to a raw material storage tank through a suction and discharge tank car or a pipeline (pneumatic), a plurality of raw material storage tanks can be installed in parallel or in series, a quantitative kick-out device is installed at the lower part of the tank body, a screw conveyor is connected to a grinding and sieving all-in-one machine, production return circulating water is connected to the grinding and sieving all-in-one machine, and the weight ratio of the sintering machine head ash to water is 1:1-1; wherein the water can be slurry water, the weight ratio of the sintering machine head ash to the slurry water is 1:3-1, and then the mixture is subjected to screen milling and stirring for 30min, and the stirring temperature is 80-90 ℃, so that the sintering machine head ash and the water are uniformly mixed to form mortar.
Pumping the uniformly mixed mortar into a tower mill by a diaphragm pump for grinding, dispersing and dissociating to ensure that the granularity of the mortar is uniform; the method comprises the steps of firstly introducing mortar into a weak magnetic secondary separator to separate iron powder with high magnetism, then introducing the mortar into a super strong magnetic separator to recover and salvage weak magnetic iron powder, removing superfine dust mud attached to the iron powder from the iron powder separated by the weak magnetic separator and the strong magnetic separator through a desliming cyclone, then introducing the iron powder into the weak magnetic separator and the strong magnetic separator, returning tailings to a grinding and screening integrated machine for pulping, and returning the qualified iron powder into an iron powder storage bin for sintering after dehydration.
And (3) sequentially feeding the tail pulp subjected to magnetic separation into a first thickening tank (or a first leaching tank) and a second thickening tank (or a second leaching tank) for overflow separation, wherein alkali metals such as calcium, magnesium, potassium, sodium and the like are dissolved in water in the process, and the thickening tank or the leaching tank is made of corrosion-resistant materials such as glass fiber reinforced plastics, PP or PE and the like due to high chloride ion content in the water. The lower part of a cone of the dense pool or the leaching tank is provided with a vertically upward lifting spiral auger and a high-pressure low-flow clear water washing pump, the spiral auger is used for preventing mortar at the bottom of the tank body from hardening, clear water (supplied by the high-pressure pump) conveniently penetrates tail slurry, alkali metal is washed and replaced from bottom to top in a high-concentration mode, sodium carbonate is added into clear liquid at the upper layer of the washed clear liquid, calcium and magnesium ions and the sodium carbonate generate calcium and magnesium carbonate mixed precipitate and sodium chloride, the calcium and magnesium carbonate mixed precipitate and the sodium chloride enter a precision filter to remove impurities (returned for sintering) such as a calcium and magnesium carbonate mixture, concentrated brine after the impurities are removed enters an evaporator for concentration and crystallization, and potassium chloride and sodium chloride are separated by utilizing the crystallization temperature difference of the potassium chloride and the sodium chloride. Potassium chloride is sold as a potash fertilizer, and sodium chloride is returned to a steel mill for use; and the washed mortar at the lower part enters the next copper and lead extraction process.
Introducing the washed mortar at the lower part into a high-temperature reaction kettle, adding ammonium bicarbonate, and dissolving the ammonium bicarbonate into a large amount of NH 3 ·H 2 O
The reaction equation is as follows: NH (NH) 4 HCO 3 +H 2 O＝H 2 CO 3 +NH 4 OH，
The copper element in the ore pulp can follow NH 3 ·H 2 The O reacts to generate basic copper carbonate,
the reaction equation is as follows: cuO + nh3.H2o = [ Cu (NH) 3 ) 4 〕(OH) 2 +3H 2 O)，
The copper-containing solution is replaced by the principle of potassium-sodium washing, and then sodium sulfide is added to become copper sulfide precipitate.
The reaction equation is as follows: cu 2+ +Na 2 S＝2Na + +CuS↓，
Can be used as a smelting raw material of copper after dehydration.
Introducing the washed copper-removed ore pulp into a high-temperature steam reaction kettle according to a certain amount, simultaneously adding a prepared mixed solution of hydrochloric acid and sodium chloride, stirring for half an hour at 89 ℃, reacting residual copper and a large amount of lead (PbO, pbCl and PbOHCl) in the ore pulp with hydrochloric acid to generate copper chloride and lead chloride,
the reaction equation is as follows: cuO +2hcl = cucl 2 +H 2 O，
PbO+2HCl＝PbCl 2 +H 2 O，
PbOHCl+HCl＝PbCl 2 +H 2 O，
PbCl 2 +2NaCl＝Na 2 PbCl 4 ，
Dehydrating the mortar to obtain filtrate, cooling the filtrate to separate out lead chloride,
the reaction equation is as follows: na (Na) 2 PbCl 4 ＝PbCl 2 +2NaCl, and drying to obtain lead chloride; dissolving lead chloride into sodium chloride solution, adding sodium carbonate, reacting to generate lead carbonate precipitate,
the reaction equation is as follows: pbCl 2 +Na 2 CO 3 ＝PbCO 3 ↓+2NaCl。
Dehydrating and drying the lead carbonate precipitate, heating to obtain a lead monoxide product,
the reaction equation is as follows: pbCO 3 ＝PbO+CO 2 ↑。
The mother liquor after lead removal contains copper chloride, sodium hydroxide is added to generate copper hydroxide precipitate,
the reaction equation is as follows: cuCl 2 +2NaOH＝Cu(OH) 2 ↓+2NaCl，
The mother liquor is recycled or sent to an evaporator to extract sodium chloride.
And (3) extracting gold and silver from the residual mortar in a leaching tank by a wet method, adjusting the pH value of the mortar to be kept between 9 and 12, adding an environment-friendly medicament after the alkalinity is adjusted, starting a water pump for half an hour every day for 3 to 5 times, stirring to mix precipitates in the mortar C with liquid, and enabling the precipitates in the mortar C to be fully contacted when a zinc wire is replaced by the precipitates in the mortar C, so that the reaction efficiency is improved, the rest time is static soaking time, and the whole leaching process is different from 8 to 20 days. Beginning the next day after alkalinity adjustment and medicine addition, during the period of static soaking, a water permeable container filled with zinc wires is placed into the clarified upper precious liquid for replacement for 2-4 hours, the zinc wires are taken out and then a water pump is started for stirring, during the period, the alkalinity and the medicament loss are detected every day to supplement the required numerical value, and the circulation operation is analogized until the alkalinity, the medicament and the zinc wires are not changed, then mortar is taken out, dehydrated, dried, sample preparation and clarified upper precious liquid water in the tank body for assay, so that the recovery rate of the gold and silver can be clearly seen to be more than 90 percent and is far greater than 50 percent of the recovery rate in the prior art, and the great improvement is achieved.
The replaced gold and silver are separated by smelting, and the mortar after valuable elements are extracted is dried after dehydration, so that the gold and silver can be used as a good raw material of a cement plant, the harm and indirect adverse effect caused by direct recycling of sintering machine head ash can be thoroughly eliminated by adopting the treatment process because the gold and silver are not contained with harmful elements and contain a certain iron element, and the valuable elements can be recovered and utilized. The whole treatment process has reasonable process flow design and obvious economic benefit, the leaching agent used in the extraction process can realize closed cycle, the method is an effective way for recycling the sintering machine head ash solid waste, the dust is changed into gold, and the waste is changed into valuable.
The recovery rate of potassium element and sodium element reaches 98% after the whole process is finished, and the extraction rate of gold and silver can reach more than 90%, so that the resource waste is reduced, and the metal elements in the sintering machine head ash are effectively recovered and utilized.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The sintering machine head ash multistage separation process is characterized by comprising the following steps
S1, pulping: weighing sintering machine head ash by using a quantitative feeder, conveying the sintering machine head ash to a grinding and screening integrated machine, adding quantitative water or ore pulp water, mixing and stirring for 20min-40min to form mortar, wherein the weight ratio of the sintering machine head ash to the water is 1:1-1;
s2, grinding: conveying the mortar in the step S1 to a tower mill for grinding, and grinding the mortar with uniform granularity;
s3, low-intensity magnetic separation: magnetically separating the mortar in the step S2 by a low-intensity magnetic separator;
s4, strong magnetic separation: carrying out magnetic separation again on the mortar subjected to the low-intensity magnetic separation by using a strong magnetic separator, and obtaining tail slurry after the magnetic separation;
s5, alkali metal removal: carrying out solid-liquid separation on the tail slurry through a first thickening tank; the supernatant liquid passes through the second thickening tank again and then is evaporated and crystallized;
s6, extracting copper and lead: adding the bottom slurry of the lower layer after solid-liquid separation in the step S5 into a high-temperature reaction kettle, and synchronously adding hydrochloric acid and a sodium carbonate solution for reaction, wherein the reaction temperature is controlled to be 120-150 ℃, and the reaction time is 30-50 min; separating the reacted solution by a centrifugal machine to obtain filtrate and precipitate; conveying the separated filtrate into a cooling reaction kettle, adding excessive ammonium bicarbonate for reaction, then adding sodium sulfide, obtaining a precipitate of a copper compound after reaction, filtering out the precipitate of the copper compound, adding a mixed solution of hydrochloric acid and sodium chloride into the solution, stirring for 30-40 min at 85-90 ℃ to obtain a lead compound precipitate and a copper ion solution, adding excessive sodium hydroxide into the solution again to obtain a copper compound precipitate, and filtering again to obtain tailing slurry;
s7, extracting gold and silver: adding the tailing slurry obtained in the step S6 into a reaction kettle, simultaneously adding an environment-friendly gold extraction agent for reaction, keeping the pH value at 9-12, stirring for 25-35 min every 4.8-8 h, soaking zinc wires in the supernatant of the static mortar C after adding the environment-friendly gold extraction agent for 24h, and soaking for 2-4 h every time; stirring and soaking for 8-20 days, electrolyzing the replaced zinc wire, and smelting to obtain gold ingots and silver ingots.
2. The multi-stage sorting process of sintering machine head ash according to claim 1, characterized in that in the step S3, the dust and mud associated with the iron powder obtained by low-intensity magnetic separation are separated by a cyclone, and the dust and mud are sorted again by the low-intensity magnetic separator; in the step S4, the iron powder obtained by the strong magnetic separation is separated from dust and mud associated with the iron powder by a cyclone, and the dust and mud are separated by a strong magnetic separator again; and adding the obtained iron powder into a vacuum filter for dehydration.
3. The sintering machine head ash multistage separation process according to claim 1, characterized in that water is added into the reaction kettle in step S7, and the water flows from the bottom to the top of the reaction kettle.
4. The multi-stage sorting process of sintering machine head ash according to claim 1, characterized in that two crystallization temperatures are set in the evaporative crystallization process in step S5, and the two crystallization temperatures obtain potassium salt and sodium salt, respectively.
5. The multi-stage sorting process of sintering machine head ash according to claim 1, characterized in that the environment-friendly gold extraction agent comprises one or more of five-membered cyclic imide, carbamide, sodium carbide cyanurate and sodium humate.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723713A (en) * | 2009-12-10 | 2010-06-09 | 湖南华菱湘潭钢铁有限公司 | Overall treatment method of steel works sintering dust |
| CN101723439A (en) * | 2009-12-10 | 2010-06-09 | 湖南华菱湘潭钢铁有限公司 | Method for recovering lead chloride from sintered ashes and preparing lead monoxide |
| CN103773967A (en) * | 2014-02-12 | 2014-05-07 | 湘潭大学 | Method for recycling silver, copper and zinc from sintered ash in iron and steel plant |
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- 2022-10-24 CN CN202211305157.6A patent/CN115572814A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723713A (en) * | 2009-12-10 | 2010-06-09 | 湖南华菱湘潭钢铁有限公司 | Overall treatment method of steel works sintering dust |
| CN101723439A (en) * | 2009-12-10 | 2010-06-09 | 湖南华菱湘潭钢铁有限公司 | Method for recovering lead chloride from sintered ashes and preparing lead monoxide |
| CN103773967A (en) * | 2014-02-12 | 2014-05-07 | 湘潭大学 | Method for recycling silver, copper and zinc from sintered ash in iron and steel plant |
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| Title |
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| 王笑 等: "烧结机头电除尘灰的资源化应用现状" * |
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