CN111377484A - Pyrite resource recovery processing method - Google Patents

Pyrite resource recovery processing method Download PDF

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Publication number
CN111377484A
CN111377484A CN202010198774.5A CN202010198774A CN111377484A CN 111377484 A CN111377484 A CN 111377484A CN 202010198774 A CN202010198774 A CN 202010198774A CN 111377484 A CN111377484 A CN 111377484A
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CN
China
Prior art keywords
recycling
pyrite
filter cake
acid
iron
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Pending
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CN202010198774.5A
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Chinese (zh)
Inventor
戴正亮
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Anqing Changhong Chemical Co ltd
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Anqing Changhong Chemical Co ltd
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Priority to CN202010198774.5A priority Critical patent/CN111377484A/en
Publication of CN111377484A publication Critical patent/CN111377484A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide (Fe2O3)
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/16Halides of ammonium
    • C01C1/164Ammonium chloride
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/18Nitrates of ammonium
    • C01C1/185Preparation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/08Ferroso-ferric oxide (Fe3O4)
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C3/00Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • C22B11/042Recovery of noble metals from waste materials
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/20Obtaining niobium, tantalum or vanadium
    • C22B34/24Obtaining niobium or tantalum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/04Working-up slag
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Fertilizers (AREA)

Abstract

The invention discloses a method for recycling and treating pyrite resources, which relates to the technical field of pyrite recycling and treatment, and specifically comprises the following steps: firstly, dissolving red powder with acid, and dissolving main substances such as iron and the like in the red powder into the acid; and then the filtrate is treated by an impurity removing agent to obtain an iron-containing solution with high purity, precious metals contained in the iron-containing solution are further treated by impurity removal, the obtained solid material contains metals such as gold, silver and copper, the pH of the acidic solution is adjusted, iron in the solid material can be settled to generate ferric hydroxide, pigments such as iron oxide red can be produced, and finally the solution after pH adjustment contains ammonium sulfate, ammonium chloride and the like, and the fertilizer can be produced by concentration and crystallization. The design realizes the resource recycling of the pyrite cinder, improves the comprehensive utilization rate of the pyrite cinder, has good environmental benefit, reduces environmental pollution, realizes the effect of changing waste into valuables, and can also generate economic benefit.

Description

Pyrite resource recovery processing method
Technical Field
The invention relates to the technical field of recovery and treatment of pyrite cinder, in particular to a method for recovering and treating pyrite resources.
Background
Pyrite is the main raw material for producing sulfuric acid in China, the sulfuric acid produced by pyrite currently accounts for more than 80% of the total amount of sulfuric acid in China, and meanwhile, 0.8-0.9 ton of sulfuric acid cinder is produced when one ton of sulfuric acid is produced. Every year, millions of tons of cinder are removed in China, the main components are ferric oxide and ferroferric oxide, and most of the cinder is stacked except a small amount of the cinder is used for iron making, chemical engineering and building materials, so that great environmental risk exists. And the cinder contains 40-60% of iron and valuable metals such as gold, silver, copper and the like.
The pyrite cinder contains other valuable metal elements such as gold, silver, copper and the like besides rich iron, but the existing resource recycling technology for the pyrite cinder is not perfect enough, so that the pyrite cinder can not be recycled better, a large amount of precious metal substances in the pyrite cinder are lost and wasted, and most of the cinder is stacked, so that the environment is seriously influenced. Therefore, the person skilled in the art provides a pyrite resource recovery process to solve the problems set forth in the above background art.
Disclosure of Invention
The invention aims to provide a pyrite resource recovery processing method to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a pyrite resource recovery processing method specifically comprises the following steps:
s1, adding the adjusted acid into the reaction kettle, adding red powder according to a certain material ratio, and then heating the reaction kettle for reaction;
s2, after the heating reaction of the S1, filtering the reaction liquid in the reaction kettle while the reaction liquid is hot to obtain a first-stage filter cake and a first-stage filtrate, and respectively collecting the first-stage filter cake and the first-stage filtrate for later use;
s3, adding an impurity removing agent into the primary filtrate obtained in the step S2, removing impurities, filtering, obtaining a secondary filter cake and a secondary filtrate after removing impurities, and mixing the secondary filter cake and the primary filter cake obtained in the step S2;
s4, adjusting the pH value of the secondary filtrate obtained by removing impurities in the S3 with alkali liquor to be neutral, and then filtering and separating;
s5, washing, drying, calcining and crushing the filter cake mixed in the S3 to obtain the pigment;
s6, concentrating and crystallizing the filtrate obtained by filtering and separating S4 to obtain the fertilizer.
As a further scheme of the invention: the red powder in the S1 is pyrite cinder, and the acid in the S1 can be one or a mixture of sulfuric acid, hydrochloric acid and nitric acid, wherein the concentration of the acid is 20-40%.
As a still further scheme of the invention: the impurity removing agent in the S3 can be one or more compounds of sodium hydroxide, potassium hydroxide, sodium sulfide and ferrous sulfate.
As a still further scheme of the invention: the first-stage filter cake and the second-stage filter cake are both slag containing precious metals, the gold content of the slag is 10-12%, the silver content of the slag is 5-10%, and other precious metals such as palladium, niobium, rhodium and the like are contained.
As a still further scheme of the invention: the alkali liquor used in S4 can be one or a mixture of ammonia water, sodium hydroxide and potassium hydroxide.
As a still further scheme of the invention: the pigment prepared by the S5 can be iron oxide red, iron oxide yellow, iron oxide black and the like.
As a still further scheme of the invention: the fertilizer prepared by the S6 can be ammonium chloride, ammonium nitrate and the like.
Compared with the prior art, the invention has the beneficial effects that: the invention relates to a pyrite resource recycling method, which comprises the steps of reacting pyrite cinder with acid, adding alkali liquor to adjust the pH value to obtain filtered slag (namely filter cake), calcining, drying, crushing and grinding the slag to obtain iron pigments, wherein the obtained iron pigments such as iron oxide red, iron oxide yellow, iron oxide black and the like have the advantages of multiple colors, wide color spectrum, no toxicity, low price and the like, are widely used and used in large amount, the solution after pH adjustment contains ammonium sulfate, ammonium chloride and the like, chemical fertilizers can be produced through concentration and crystallization, the obtained chemical fertilizers can be suitable for agricultural planting, the recycling of pyrite cinder resources is realized, the maximum utilization rate of the pyrite cinder is also realized, the comprehensive recycling utilization rate of the pyrite cinder is high, the environmental benefit is good, and the environmental pollution is reduced, the effect of changing waste into valuable is realized, and economic benefit can be generated.
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 fall within the protection scope of the present invention.
Example 1
Firstly, adding 30% hydrochloric acid into a reaction kettle, adding red powder according to the material ratio of the slag acid molar ratio of 1:3, heating to 80 ℃, and stirring for reaction for about 2 hours; then, after the heating reaction, filtering the reaction liquid in the reaction kettle while the reaction liquid is hot to obtain a first-stage filter cake and a first-stage filtrate, and respectively collecting the first-stage filter cake and the first-stage filtrate for later use; secondly, adding an impurity removing agent into the obtained primary filtrate, removing impurities and filtering, obtaining a secondary filter cake and a secondary filtrate after removing impurities, and mixing the secondary filter cake and the primary filter cake; further, adjusting the pH value of the secondary filtrate (the main component is ferric chloride) obtained by impurity removal by using ammonia water to be neutral, and then filtering and separating; further washing, drying, calcining and crushing the mixed filter cake (the main component is ferric hydroxide) to obtain the pigment; and finally, concentrating and crystallizing the filtrate obtained by filtering and separating to obtain the ammonium chloride fertilizer.
Example 2
Firstly, adding 25% sulfuric acid into a reaction kettle, adding red powder according to the material ratio of the molar ratio of slag acid to the material ratio of 1:3, heating to 80 ℃, and stirring for reaction for about 2.5 hours; then, after the heating reaction, filtering the reaction liquid in the reaction kettle while the reaction liquid is hot to obtain a first-stage filter cake and a first-stage filtrate, and respectively collecting the first-stage filter cake and the first-stage filtrate for later use; secondly, adding an impurity removing agent into the obtained primary filtrate, removing impurities and filtering, obtaining a secondary filter cake and a secondary filtrate after removing impurities, and mixing the secondary filter cake and the primary filter cake; further, adjusting the pH value of the secondary filtrate (the main component is ammonium sulfate) obtained by impurity removal to be neutral by using sodium hydroxide, and then filtering and separating; further washing, drying, calcining and crushing the mixed filter cake (the main component is ferric hydroxide) to obtain the pigment; and finally, concentrating and crystallizing the filtrate obtained by filtering and separating to obtain the ammonium sulfate fertilizer.
The heavy metal components and contents of the pyrite cinder (namely red powder) adopted by the invention are shown in the table:
composition (I) Fe S As SiO2 Cu Zn Co Au Ag
Content (wt.) 53.04 1.08 0.08 11.31 0.36 0.44 0.03 0.98 32.69
Note: the measurement units of Au and Ag in the above tables are g/t.
The working principle of the invention is as follows: the invention designs a method for recycling and treating pyrite resources, which mainly aims at recycling and treating pyrite cinder (namely red powder), and the main principle is as follows: firstly, dissolving red powder with acid, dissolving main substances such as iron in the red powder into the acid, and separating to obtain a filter cake containing precious metals such as gold, silver and copper; and then the filtrate is treated by an impurity removing agent to obtain an iron-containing solution with high purity, precious metals contained in the iron-containing solution are further treated by impurity removal, the obtained solid material contains metals such as gold, silver and copper, the pH of the acidic solution is further adjusted, iron in the acidic solution can be settled to generate ferric hydroxide, pigments such as iron oxide red can be further produced, and finally the solution after the pH is adjusted contains ammonium sulfate, ammonium chloride and the like.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.

Claims (7)

1. A pyrite resource recovery processing method is characterized by comprising the following steps:
s1, adding the adjusted acid into the reaction kettle, adding red powder according to a certain material ratio, and then heating the reaction kettle for reaction;
s2, after the heating reaction of the S1, filtering the reaction liquid in the reaction kettle while the reaction liquid is hot to obtain a first-stage filter cake and a first-stage filtrate, and respectively collecting the first-stage filter cake and the first-stage filtrate for later use;
s3, adding an impurity removing agent into the primary filtrate obtained in the step S2, removing impurities, filtering, obtaining a secondary filter cake and a secondary filtrate after removing impurities, and mixing the secondary filter cake and the primary filter cake obtained in the step S2;
s4, adjusting the pH value of the secondary filtrate obtained by removing impurities in the S3 with alkali liquor to be neutral, and then filtering and separating;
s5, washing, drying, calcining and crushing the filter cake mixed in the S3 to obtain the pigment;
s6, concentrating and crystallizing the filtrate obtained by filtering and separating S4 to obtain the fertilizer.
2. The method for recycling and treating pyrite resource according to claim 1, wherein said red powder in S1 is pyrite cinder, and the acid in S1 is selected from one or more of sulfuric acid, hydrochloric acid, and nitric acid, wherein the concentration of the acid is 20-40%.
3. The method for recycling and treating pyrite resource according to claim 1, wherein the removal agent in S3 can be one or more compounds selected from sodium hydroxide, potassium hydroxide, sodium sulfide, and ferrous sulfate.
4. The method for recycling and treating pyrite resource according to claim 1, wherein said first and second filter cakes are slag containing precious metals, gold content is 10-12%, silver content is 5-10%, and other precious metals such as palladium, niobium, rhodium, etc.
5. The method for recycling and treating pyrite resource according to claim 1, wherein the lye used in S4 is selected from one or a mixture of ammonia, sodium hydroxide and potassium hydroxide.
6. The method for recycling and treating pyrite resource according to claim 1, wherein the pigment produced in S5 is selected from red iron oxide, yellow iron oxide, black iron oxide, etc.
7. The method for recycling and treating pyrite resource of claim 1, wherein said fertilizer produced by S6 is selected from ammonium chloride, ammonium nitrate, etc.
CN202010198774.5A 2020-03-20 2020-03-20 Pyrite resource recovery processing method Pending CN111377484A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114906830A (en) * 2022-07-19 2022-08-16 昆明川金诺化工股份有限公司 Method for controllably preparing battery-grade iron phosphate from pyrite cinder

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1491997A (en) * 2003-09-04 2004-04-28 复旦大学 Process for preparing ferric oxide red powder
CN101157985A (en) * 2007-09-25 2008-04-09 池煊庆 Comprehensive reclaiming method for pyrite slag
CN102115212A (en) * 2010-12-31 2011-07-06 张胜勇 Method for preparing industrial ferrous sulfate and zinc sulfate by using pyrite cinders
WO2013108478A1 (en) * 2012-01-17 2013-07-25 Jx日鉱日石金属株式会社 Gold recovery method, and gold production method using same
CN104445431A (en) * 2014-11-14 2015-03-25 贵州大学 Method for preparing high-purity iron oxide red from pyrites slag
CN106868307A (en) * 2017-02-13 2017-06-20 中国科学院过程工程研究所 A kind of pyrite cinder arsenic removal is enriched with the comprehensive utilization process of gold and silver

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1491997A (en) * 2003-09-04 2004-04-28 复旦大学 Process for preparing ferric oxide red powder
CN101157985A (en) * 2007-09-25 2008-04-09 池煊庆 Comprehensive reclaiming method for pyrite slag
CN102115212A (en) * 2010-12-31 2011-07-06 张胜勇 Method for preparing industrial ferrous sulfate and zinc sulfate by using pyrite cinders
WO2013108478A1 (en) * 2012-01-17 2013-07-25 Jx日鉱日石金属株式会社 Gold recovery method, and gold production method using same
CN104445431A (en) * 2014-11-14 2015-03-25 贵州大学 Method for preparing high-purity iron oxide red from pyrites slag
CN106868307A (en) * 2017-02-13 2017-06-20 中国科学院过程工程研究所 A kind of pyrite cinder arsenic removal is enriched with the comprehensive utilization process of gold and silver

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王为振等: "含金滤液中金、银及其他有价金属回收的试验研究", 《矿冶》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114906830A (en) * 2022-07-19 2022-08-16 昆明川金诺化工股份有限公司 Method for controllably preparing battery-grade iron phosphate from pyrite cinder
CN114906830B (en) * 2022-07-19 2022-10-14 昆明川金诺化工股份有限公司 Method for controllably preparing battery-grade iron phosphate from pyrite cinder

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Application publication date: 20200707