CN101195858B - Method for extracting nickel with pressure leaching of non-metal high nickel sulfonium material - Google Patents
Method for extracting nickel with pressure leaching of non-metal high nickel sulfonium material Download PDFInfo
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Abstract
The invention relates to a nickel extracting method through the pressurized leaching of non metallization high content nickel matte material. The invention is characterized in that the two-stage atmospheric pressure leaching process and the two-stage pressurized leaching process are adopted to extract nickel through the pressurized leaching of the non metallization high content nickel matte material. By adopting the method of the invention, the leaching rate of nickel and cobalt is larger than 98 percent, the noble metal is completely concentrated in leached slag, the sulfur of the high content nickel matte is oxidized into sulfate radical to enter the solution, the pour solution of nickel sulphate and cobalt sulphate is obtained after the one stage pressurized leaching solution is processed through the one stage atmospheric pressure leaching and purifying. Copper is mainly delivered into the two-stage pressurized leaching solution. Iron and noble metal are concentrated in the two-stage pressurized leached slag. The process has the advantages that the process is simple, highly efficient and environment friendly, and the adaptability of the raw material is wide. The invention is suitable for the treatment of albata alloy, and through adjusting the relative technical parameter, the invention is suitable for selectively leaching and segregating nickel, copper and noble metal from non metallization high content nickel matte with various grades.
Description
Technical field
The pressurization of non-metallic high nickel matte material is leached and is extracted the nickel method, relates to the metallurgical method that extracts nickel and enriching noble metals with a kind of from non-metallic high nickel matte.
Background technology
Traditional nickel refining is to adopt nickel sulfide anode electrolysis technology, has following shortcoming: return slag is many 1), and return slag is handled complicated, and metal recovery rate is low; 2) energy, high material consumption, cost is higher; 3) product is relatively single, and share of market is low, is difficult to resist the market risk; 4) technical process bad adaptability, difficulty satisfies the processing of the raw material of different Ni/Cu ratio; 5) precious metal disperses seriously, and the rate of recovery is low.Deficiency at the traditional nickel refinery practice, in twentieth century second half, domestic and international many nickel refining factory all begins active research advanced person's nickel refining technology, more representational have high nickel matte sulfation to leach and two technologies of high nickel matte chlorination leaching, the common feature that they have is that technical process is short, the metal recovery rate height, tooling cost is low.But high nickel matte sulfation extract technology is relatively ripe, and the practical experience of success is arranged, and has following characteristics:
1) technical process is shortened significantly, the metal recovery rate height.The founding, liquid making, deironing, copper removal of soluble anode electrolysis production technical process, the round transport that removes operation such as cobalt and the dissolving of cobalt slag, P204 removal of impurities and intermediate material have been saved.
2) technology has been taken into account the requirement of advance, reliability, suitability and economical all many-sides simultaneously.Technology has adapted to the characteristics of raw material, has inherited reliability height such as copper nickel ore dressing separation, technology with low cost, has overcome some unfavorable defectives of former flow process.
3) technological transformation initial cost is little, reagent consumption, energy consumption are low; Simultaneously, the level of automation height of technology, labour intensity is low, and recruitment is few, is a technology-intensive technology.
4) nickel cobalt quality product height can be realized the requirement of many variety production simultaneously.
5) sulfate system corrodibility is little, the good relatively solution of material installation.
6) it is few not produce obnoxious flavour, waste residue, process waste liquor in the refining process, is free of contamination cleaning procedure.
Outokumpu company is one of more successful representational producer of high ice nickel sulfation extract technology practice, the nickel matte that the reactor of its employing Outokumpu development and Design carries out normal pressure and pressurization leaches, adopt three sections adverse currents to leach to flash stove nickel matte, electric furnace ice nickel is then adopted two sections leachings.Main leaching agent is sulfuric acid and oxygen, nickel matte composition: Ni
3S
2, cupric sulfide, corronel.Technology comprises: a, normal pressure copper removal; The normal pressure of b, nickel leaches; The pressurization of c, nickel is leached.Wherein, ferronickel enters solution, and copper is opened a way with CuS, not oxygenation or add sub-fraction oxygen and nickel is carried out selectivity leach.Alloy phase leaches in the normal pressure section, and iron is with pyrrhosiderite form precipitation during leaching, and sulfide leaches in pressurized segment, and iron precipitates with the rhombohedral iron ore form during leaching.Strict control pH value can improve the leaching yield of nickel cobalt.Pressurization is leached back liquid and is entered the normal pressure leaching.
The Fukang, Xinjiang is the nickel manufacturing enterprise that China first hand adopts pressurized acid leaching technology, is mainly used in the metallize leaching of high nickel matte of shrend.Through updating of more than ten years, major equipment is stable at present, and running cost constantly descends, and economic and technical norms are more stable, has reached the index of design.The leaching yield of nickel: normal pressure extracting stage 25-35%, the pressurization extracting stage is 92-94%.High pressure leaches still useful volume 37m
3, inside lining anti-corrosive ceramic tile, operating pressure 0.8MPa, temperature 150-160 ℃.
December calendar year 2001, Jilin nickel industry company adopted the high ice of pressurized acid leaching art breading shrend nickel, and nickel cobalt leaching yield reaches 96.5%.It is 0.8MPa that its high pressure leaches the still operating pressure, Steel Lining 4mm titanium plate, working temperature 150-160 ℃, the maximum output pressure 2.0MPa of force (forcing) pump, the maximum ore pulp amount of squeezing into 4.0m
3/ hr.This technology is in order effectively to prevent the pollution of calcium in the nickel salt production process, magnesium ion, and total system adopts pure water production, and all equipment anticorrosions do not adopt lining ceramic tile (or earthenware brick) preservative coat, and all pumps have all adopted engineering plastics and fluorine alloy pump.Whole process using normal pressure leach one or two section pressurization and leach that (one section is soaked nickel, one section is soaked copper), effectively in leaching process, realized effectively separating of nickel cobalt and copper, iron, and in industrial production, used the pure oxygen leaching at home first, reduced processing charges significantly, shorten technical process, improved utilization efficiency of heat energy.
Above-mentioned technology is owing to all certain applicable elements being arranged, and is all undesirable for the processing of raw material that is rich in precious metal and non-metallic high nickel matte material.
Summary of the invention
The objective of the invention is limitation, provide a kind of and be suitable for being rich in the raw material of precious metal and the nickel method of extracting is leached in the pressurization of non-metallic high nickel matte material at the existence of above-mentioned prior art.
The pressurization of non-metallic high nickel matte material is leached and is extracted the nickel method, it is characterized in that it being to adopt two sections normal pressures, two sections pressure leaching process to leach from non-metallic high nickel matte pressurization and extract nickel, and its processing condition are:
A) non-metallic high nickel matte material is milled on the granularity accounts for more than 90% less than 50 μ m;
B) carry out one section normal pressure under the condition of the mineral liquid before adding acid, adding after will grinding and leach, the liquid-solid envelope-bulk to weight ratio of control pulp is 6-10: 1m
3/ ton, initial sulfuric acid concentration is 5g/l-15g/l, temperature of reaction is 65-85 ℃; Extraction time: 4-8 hour; The terminal point pH value is 5.0-6.5;
C) two sections normal pressures of control leach: the liquid-solid volume anharmonic ratio of pulp is 6-12: 1m
3/ ton, initial sulfuric acid concentration is 45g/l-75g/l, temperature of reaction is 60-80 ℃; Extraction time: 4-8 hour; The terminal point pH value is 1.0-3.0;
D) one section pressurization of control is leached: temperature of reaction is 160 ± 10 ℃, and leaching pressure is 0.60-0.80MPa, extraction time: 5-9 hour; Leaching the terminal point pH value is 1.0-3.0;
E) two sections pressurizations of control are leached: temperature of reaction is 160 ± 10 ℃, and leaching pressure is 0.60-0.80MPa, extraction time: 4-8 hour; Leaching the terminal point pH value is 1.0-3.0.
It is after raw material is measured by disk feeder and belted electronic balance that one section normal pressure of the present invention leaches pulp, be delivered in the pulp groove by two-way belt again, return uniformly continuously in the pulp groove into preceding liquid (one section pressurization leach liquor) and sulfuric acid and carry out pulp, the liquid-solid ratio during the control pulp reaches 6-10: 1m
3/ ton.
It is in order to reach higher leaching yield, to prevent that simultaneously a large amount of evaporations of moisture from causing valuable metal to run off and environmental pollution that one section normal pressure extraction temperature of method of the present invention is controlled at 65-85 ℃.
One section normal pressure of method of the present invention leaches the terminal point pH value and is controlled between the 5.0-6.5, is the content that enough subsalt to be arranged in one section normal pressure slag and reduce foreign ion in the solution in order to guarantee.
After one section normal pressure of method of the present invention leaches and finishes, ore pulp returned carry out gravity settling in the thickener, supernatant is as finished fluid, and underflow enters two sections normal pressures by rubber pipe pump and leaches.
It is one section normal pressure to be leached thickener underflow squeeze in the pulp groove that method two section normal pressure of the present invention leaches pulp, and continous-stable preceding liquid and sulfuric acid are squeezed into carried out pulp in the pulp groove simultaneously, and the liquid-solid ratio during the control pulp reaches 6-12: 1.
It is to create conditions in order to leach for one section pressurization that method two section normal pressure extraction temperature of the present invention is controlled at 60-80 ℃, prevents that simultaneously a large amount of evaporations of moisture from causing valuable metal to run off and environmental pollution.
It is that 1.0-3.0 creates conditions in order to leach for one section pressurization that method two section normal pressure of the present invention leaches the terminal point pH value.
After method two section normal pressure of the present invention leached and finishes, ore pulp flowed in the surge tank by the overanxious back of screen cloth, squeezed into by force (forcing) pump to enter autoclave in the ore pulp well heater after the heating and carry out one section pressurization and leach reaction again.
Temperature of reaction when one section pressurization of method of the present invention is leached is 160 ± 10 ℃, is in order to reach higher nickel cobalt leaching yield, the safety in production that can not influence autoclave to be arranged simultaneously.
Leaching pressure when the pressurization of one section of method of the present invention is leached is 0.60-0.80MPa, is in order to control oxygen partial pressure, thus the leaching yield of control ambrose alloy, and realize that the selectivity of ambrose alloy leaches.
Temperature of reaction when method two section pressurization of the present invention is leached is 160 ± 10 ℃, is in order to reach higher copper, nickel leaching yield, can not to influence the safety in production of autoclave simultaneously again.
Leaching pressure when method two section pressurization of the present invention is leached is 0.60-0.80MPa, is in order to control oxygen partial pressure, to improve the leaching yield of nickel, copper.
The preceding liquid that method of the present invention leaches as one section normal pressure with one section pressurization leach liquor, the copper in the solution, acid and alloy phase and Ni
3S
2React, copper is suppressed in the slag, thereby can access purified rich cobalt nickel sulfate solution.
One section normal pressure leach liquor of method output of the present invention is used for the soluble anode electrolytic nickel is produced replenishing of nickel ion, also can be directly used in the preparation of nickel sulfate hexahydrate crystal, also further is used for the production of electro deposited nickel behind the abstraction impurity removal.
Method copper of the present invention stays in one section pressurization leached mud with the form of cupric sulfide, and iron is deposited in the slag with the form of rhombohedral iron ore or pyrrhosiderite, and precious metal is not participated in reaction and stayed in the slag, thereby has realized that selectivity leaches the purpose of nickel cobalt.
Method of the present invention is in two sections pressurizations are leached, and copper, nickel enter leach liquor, and iron is deposited in the slag with the form of rhombohedral iron ore or pyrrhosiderite, and precious metal is not participated in reaction and stayed in the slag, realizes the enrichment of precious metal, and can be used for the raw material of electrosmelting enriching noble metals.
Arsenic in the method solution of the present invention, tellurium, bismuth, lead etc. mainly get off with the form co-precipitation that is similar to indissoluble iron cpds such as ferric arsenate, plumbojarosite, can not cause the enrichment of trace element in process of production.
Adopt method of the present invention, the leaching yield of nickel, cobalt is greater than 98%, precious metal is enriched in the leached mud fully, and the sulphur in the high nickel matte all is oxidized to sulfate radical and enters solution, obtains the solution of purified single nickel salt, rose vitriol after one section pressurization leach liquor purifies through one section normal pressure leaching.Copper mainly enters in two sections pressurization immersion liquid.Iron and concentration of precious metal are in two sections pressurization leached muds.Method of the present invention, simply efficient, eco-friendly flow process has the wide advantage of adaptability to raw material, and by adjusting the correlation technique parameter, the non-metallic high nickel matte selective leaching that can be suitable for various grades goes out separating nickel, copper and precious metal.
Description of drawings
Fig. 1 is the principle process flow sheet of method of the present invention.
Embodiment
The nickel method of extracting is leached in the pressurization of non-metallic high nickel matte material, be to adopt two sections normal pressures, two sections pressure leaching process to leach from non-metallic high nickel matte pressurization and extract nickel, its processing condition are: a) non-metallic high nickel matte material is milled on the granularity and accounts for more than 90% less than 50 μ m; B) carry out one section normal pressure under the condition of the mineral liquid before adding acid, adding after will grinding and leach, control pulp liquid-solid ratio 6-10: 1m
3/ ton, initial sulfuric acid concentration is 5g/l-15g/l, temperature of reaction is 70-85 ℃; C) two sections normal pressures of control leach: pulp liquid-solid ratio 6-12: 1m
3/ ton, initial sulfuric acid concentration is 45-75g/l, initial soln cupric 3-10g/l, temperature of reaction is 60-80 ℃; D) one section pressurization of control is leached: temperature of reaction is 160 ± 10 ℃, and leaching pressure is 0.60-0.80MPa; E) two sections pressurizations of control are leached: temperature of reaction is 150 ± 15 ℃, and leaching pressure is 0.40-0.70MPa;
Embodiment 1
Concrete steps: with non-metallic high nickel matte material (Ni65.6%, Co1.0%, Cu3.0%, Fe3.5%, S23.5%), granularity accounts for more than 90% less than 50 μ m, after the metering, to the pulp groove, in the pulp groove, to return uniformly continuously into preceding liquid (one section pressurized fluid) and sulfuric acid and carry out pulp, the liquid-solid ratio during the control pulp reaches 7: 1m
3/ ton, ore pulp send one section normal pressure to leach after the pulp, and controlling one section normal pressure leaching temperature of reaction is 75 ℃, and the terminal point pH value is controlled at 5.5; After one section normal pressure leaches and finishes, ore pulp returned carry out gravity settling in the thickener, supernatant is as finished fluid, and underflow enters two sections normal pressure pulps by rubber pipe pump, two sections normal pressure pulp time control slurrying liquid-solid ratio 7: 1m
3/ ton, initial sulfuric acid concentration is 60g/l, initial soln cupric 7.5g/l, ore pulp send two sections normal pressures to leach after the pulp, and controlling two sections normal pressures leaching temperature of reaction is 70 ℃, and leaching the terminal point pH value is 1.5; After two sections normal pressures leached and finish, ore pulp flowed in the surge tank by the overanxious back of screen cloth, squeezed into by force (forcing) pump to enter autoclave in the ore pulp well heater after the heating and carry out one section pressurization and leach reaction again; Controlling one section pressurization leaching temperature of reaction is 160 ℃, and leaching pressure is 0.65MPa; Carry out dense separation after one section pressurization is leached, liquid is provided and delivered and is made the preceding liquid of one section normal pressure, and slag carries out two sections pressurizations and leaches, and control reaction temperature is 155 ℃ during two sections pressurization leachings, and leaching pressure is 0.60MPa; Finally make whole process nickel leaching yield greater than 95%, precious metal, copper, iron are stayed in the leached mud.
Embodiment 2
Concrete steps: with non-metallic high nickel matte material (Ni65.6%, Co1.0%, Cu3.0%, Fe3.5%, S23.5%), granularity accounts for more than 90% less than 50 μ m, after the metering, to the pulp groove, in the pulp groove, to return uniformly continuously into preceding liquid (one section pressurized fluid) and sulfuric acid and carry out pulp, the liquid-solid ratio during the control pulp reaches 8: 1m
3/ ton, ore pulp send one section normal pressure to leach after the pulp, and controlling one section normal pressure leaching temperature of reaction is 80 ℃, and the terminal point pH value is controlled at 5.3; After one section normal pressure leaches and finishes, ore pulp returned carry out gravity settling in the thickener, supernatant is as finished fluid, and underflow enters two sections normal pressure pulps by rubber pipe pump, two sections normal pressure pulp time control slurrying liquid-solid ratio 8: 1m
3/ ton, initial sulfuric acid concentration is 55g/l, initial soln cupric 6g/l, ore pulp send two sections normal pressures to leach after the pulp, and controlling two sections normal pressures leaching temperature of reaction is 75 ℃, and leaching the terminal point pH value is 1.8; After two sections normal pressures leached and finish, ore pulp flowed in the surge tank by the overanxious back of screen cloth, squeezed into by force (forcing) pump to enter autoclave in the ore pulp well heater after the heating and carry out one section pressurization and leach reaction again; Controlling one section pressurization leaching temperature of reaction is 155 ℃, and leaching pressure is 0.62MPa; Carry out dense separation after one section pressurization is leached, liquid is provided and delivered and is made the preceding liquid of one section normal pressure, and slag carries out two sections pressurizations and leaches, and control reaction temperature is 150 ℃ during two sections pressurization leachings, and leaching pressure is 0.54MPa; Finally make whole process nickel leaching yield greater than 95%, precious metal, copper, iron are stayed in the leached mud.
Embodiment 3
Concrete steps: with non-metallic high nickel matte material (Ni65.6%, Co1.0%, Cu3.0%, Fe3.5%, S23.5%), granularity accounts for more than 90% less than 50 μ m, after the metering, to the pulp groove, in the pulp groove, to return uniformly continuously into preceding liquid (one section pressurized fluid) and sulfuric acid and carry out pulp, the liquid-solid ratio during the control pulp reaches 9: 1m
3/ ton, ore pulp send one section normal pressure to leach after the pulp, and controlling one section normal pressure leaching temperature of reaction is 85 ℃, and the terminal point pH value is controlled at 5.8; After one section normal pressure leaches and finishes, ore pulp returned carry out gravity settling in the thickener, supernatant is as finished fluid, and underflow enters two sections normal pressure pulps by rubber pipe pump, two sections normal pressure pulp time control slurrying liquid-solid ratio 6: 1m
3/ ton, initial sulfuric acid concentration is 65g/l, initial soln cupric 8g/l, ore pulp send two sections normal pressures to leach after the pulp, and controlling two sections normal pressures leaching temperature of reaction is 70 ℃, and leaching the terminal point pH value is 2.0; After two sections normal pressures leached and finish, ore pulp flowed in the surge tank by the overanxious back of screen cloth, squeezed into by force (forcing) pump to enter autoclave in the ore pulp well heater after the heating and carry out one section pressurization and leach reaction again; Controlling one section pressurization leaching temperature of reaction is 165 ℃, and leaching pressure is 0.75MPa; Carry out dense separation after one section pressurization is leached, liquid is provided and delivered and is made the preceding liquid of one section normal pressure, and slag carries out two sections pressurizations and leaches, and control reaction temperature is 140 ℃ during two sections pressurization leachings, and leaching pressure is 0.48MPa; Finally make whole process nickel leaching yield greater than 95%, precious metal, copper, iron are stayed in the leached mud.
Claims (1)
1. the pressurization of non-metallic high nickel matte material is leached and is extracted the nickel method, it is characterized in that it being to adopt two sections normal pressures, two sections pressure leaching process to leach from non-metallic high nickel matte pressurization and extract nickel, and its processing condition are:
A) non-metallic high nickel matte material is milled on the granularity accounts for more than 90% less than 50 μ m;
B) material after will grinding is adding acid, is adding one section pressurization leach liquor and carry out one section normal pressure under as the condition of preceding liquid and leach, and the liquid-solid envelope-bulk to weight ratio of control pulp is 6-10: 1m
3/ ton, initial sulfuric acid concentration is 5g/l-15g/l, temperature of reaction is 65-85 ℃; Extraction time: 4-8 hour; Endpoint pH is 5.0-6.5;
C) two sections normal pressures of control leach: the liquid-solid envelope-bulk to weight ratio of pulp is 6-12: 1m
3/ ton, initial sulfuric acid concentration is 45g/l-75g/l, temperature of reaction is 60-80 ℃; Extraction time: 4-8 hour; Endpoint pH is 1.0-3.0;
D) one section pressurization of control is leached: temperature of reaction is 160 ± 10 ℃, and leaching pressure is 0.60-0.80MPa, extraction time: 5-9 hour; The leaching endpoint pH is 1.0-3.0;
E) two sections pressurizations of control are leached: temperature of reaction is 160 ± 10 ℃, and leaching pressure is 0.60-0.80MPa, extraction time: 4-8 hour; The leaching endpoint pH is 1.0-3.0.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007103036185A CN101195858B (en) | 2007-12-20 | 2007-12-20 | Method for extracting nickel with pressure leaching of non-metal high nickel sulfonium material |
Applications Claiming Priority (1)
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|---|---|---|---|
| CN2007103036185A CN101195858B (en) | 2007-12-20 | 2007-12-20 | Method for extracting nickel with pressure leaching of non-metal high nickel sulfonium material |
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| CN101195858A CN101195858A (en) | 2008-06-11 |
| CN101195858B true CN101195858B (en) | 2010-08-25 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FI20110279A0 (en) * | 2011-08-29 | 2011-08-29 | Outotec Oyj | A method for recovering metals from material containing them |
| CN105296755B (en) * | 2015-11-20 | 2018-06-08 | 金川集团股份有限公司 | A kind of method that non-metallic high nickel matte pressureleaching solution removes iron |
| CN105400960A (en) * | 2015-11-20 | 2016-03-16 | 金川集团股份有限公司 | Method for pressurizing cobalt-rich copper matte to leach out nickel and cobalt and remove iron |
| CN105838882B (en) * | 2016-06-21 | 2017-11-17 | 昆明冶金研究院 | Separating molybdenum from nickel recovery process in a kind of nickel-molybdenum symbiotic ore oxygen pressure acid steep |
| CN107630146B (en) * | 2017-08-07 | 2019-12-20 | 中国恩菲工程技术有限公司 | Nickel recovery process |
| JP7277084B2 (en) * | 2018-06-27 | 2023-05-18 | 住友金属鉱山株式会社 | Method for separating copper from nickel and cobalt |
| CN112280978A (en) * | 2020-11-19 | 2021-01-29 | 金川集团股份有限公司 | Method for pressure leaching of high-sulfur low-copper-nickel material |
| CN113526576B (en) * | 2021-05-31 | 2022-06-03 | 金川集团股份有限公司 | Preparation method of high-nickel low-acid low-sodium nickel sulfate solution |
| CN113957264A (en) * | 2021-09-13 | 2022-01-21 | 广东邦普循环科技有限公司 | Method for preparing nickel sulfate from low grade nickel matte |
| CN113957243B (en) * | 2021-10-22 | 2023-10-17 | 金川镍钴研究设计院有限责任公司 | Method for realizing open circuit of nickel, copper and iron in high-nickel matte and enriching noble metals |
| WO2023092480A1 (en) * | 2021-11-26 | 2023-06-01 | 深圳市坤鹏冶金工程技术有限公司 | Method for extracting nickel sulfate from nickel matte |
| CN114908257A (en) * | 2022-05-07 | 2022-08-16 | 金川集团股份有限公司 | Method for producing high-quality nickel sulfate solution |
| CN115323189A (en) * | 2022-08-24 | 2022-11-11 | 中国恩菲工程技术有限公司 | Treatment method of nickel and sulfur with high copper content |
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Owner name: JINCHUAN GROUP CO., LTD. Free format text: FORMER NAME: JINCHUAN GROUP CORP., LTD. |
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| CP01 | Change in the name or title of a patent holder |
Address after: 737103 Jinchuan Road, Gansu, China, No. 98, No. Patentee after: Jinchuan Group Co., Ltd. Address before: 737103 Jinchuan Road, Gansu, China, No. 98, No. Patentee before: Jinchuan Group Corp., Ltd. |