CN107777734B - A method of nickel sulfate is prepared with nickel sulfide ore - Google Patents
A method of nickel sulfate is prepared with nickel sulfide ore Download PDFInfo
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- CN107777734B CN107777734B CN201710848285.8A CN201710848285A CN107777734B CN 107777734 B CN107777734 B CN 107777734B CN 201710848285 A CN201710848285 A CN 201710848285A CN 107777734 B CN107777734 B CN 107777734B
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- nickel
- sulfide ore
- nickel sulfide
- acid
- nickel sulfate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
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- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of methods for preparing nickel sulfate with nickel sulfide ore, method includes the following steps: it is levigate to be firstly vulcanized nickel minerals, after diluted acid removal impurity is added, sulfuric acid, oxidant is added, sulfur cement, sulfuric acid calcium inhibitors, iron oxide crystal seed, after mixing, it is added in autoclave, and it is passed through pressure-air, after reaction, separation of solid and liquid obtains nickel sulfate solution and leached mud.The present invention has process short, and leaching efficiency is high, at low cost, environmentally protective feature.
Description
Technical field
The present invention relates to nickel sulfide ore resource utilization fields, and in particular to a kind of side that nickel sulfate is prepared with nickel sulfide ore
Method.
Background technique
The treatment process of nickel sulfide ore generally can be divided into pyrogenic process and wet process.Pyrogenic attack technique is to use matte smelting, will
Ni-B alloy in nickel sulfide ore is at low nickel matte, then by low nickel matte with bessemerizing into high nickel matte, then produces through different method of refining
Different nickel product out.Main technique has nickel sulfide ore shaft smelting, electro-smelting, flash smelting and bath smelting etc..
Wet processing process, which generally refers to leach into solution, proposes nickel process, and main technique has sulfating roasting lixiviation process, normal pressure
Ammonia leaching process, pressure ammonia leaching method, oxygen leaching method and chlorination leaching process etc..
Pressure leaching is to be greater than 1 atmospheric pressure in pressure, handles ore or concentrate with solution, is to handle complicated metalliferous mineral
One of hydrometallurgy new process of resource.Compared to normal pressure leaching, the characteristics of pressure leaching, has: (1) improving extraction temperature, accelerate leaching
Speed out accelerates extraction time；(2) some mineral that not can be carried out reaction at normal temperatures and pressures can be made to occur a degree of
Reaction；(3) so that oxygen or ammonia have higher partial pressure in leaching process, enhanced leaching process improves the leaching of metal for pressurization
Rate.(4) for the adaptable of raw material, can processes composition complexity material.
But difficult, extraction time is long, the low problem of leaching efficiency currently, pressure leaching is removed there are impurity.
Summary of the invention
In order to solve the problems existing in the prior art, the present invention provides a kind of methods for preparing nickel sulfate with nickel sulfide ore.
This method has process short, and leaching efficiency is high, at low cost, environmentally protective feature.
To achieve the above objectives, this invention takes following technical solutions:
A method of nickel sulfate being prepared with nickel sulfide ore, is included the following steps:
(1) it pre-processes
Parts by weight meter, 100 parts of nickel sulfide ore is levigate, and 100-300 parts of diluted acids are added, after being stirred to react, filters pressing is obtained
To pretreated nickel sulfide ore and aqueous solution；
(2) oxygen leaching
In nickel sulfide ore after the pre-treatment, be added 100-300 parts of sulfuric acid, 10-20 parts of oxidants, 1-5 parts of sulfur cements,
1-5 parts of sulfuric acid calcium inhibitors and 1-5 parts of iron oxide crystal seeds are added in autoclave after mixing, and are passed through pressure-air,
After 140~200 DEG C sufficiently reaction, separation of solid and liquid obtains nickel sulfate solution and leached mud.
In step (1), the fineness after nickel sulfide ore is levigate is 80 μm.
In step (1), diluted acid is sulfuric acid solution, hydrochloric acid solution or nitric acid solution, and mass concentration is 5%.
In step (1), obtained aqueous solution recycles magnesium salts by condensing crystallizing.
In step (2), the reaction time is 6 hours in autoclave.
In step (2), the mass concentration of sulfuric acid is 20%.
In step (2), the pressure of pressure-air is 2MPa.
The oxidant is copper sulphate, hydrogen peroxide, Peracetic acid, potassium permanganate or ammonium persulfate.
Sulfur cement diethyldithiocarbamate, xanthate or the thioacetic acid.
The sulfuric acid calcium inhibitors are polyethylene diacid, polyacrylic acid or citric acid.
Compared with the existing technology, the present invention have it is following a little:
The method that the present invention prepares nickel sulfate with nickel sulfide ore, it is first that nickel sulfide ore is levigate, after diluted acid removal impurity is added,
Addition sulfuric acid, oxidant, sulfur cement, sulfuric acid calcium inhibitors, iron oxide crystal seed are added in autoclave after mixing, and
It is passed through pressure-air, after reaction, separation of solid and liquid obtains nickel sulfate solution and leached mud.This method is levigate by nickel sulfide concentrate, uses
Diluted acid is leached, and talcum is easy to react with acid, magnesium sulfate is generated, to realize the separation of magnesium and nickel sulfide concentrate.Wherein, oxygen
Agent can generate elemental sulfur, promote the dissolution of nickel sulfide ore with the reaction of Salmon-Saxl in nickel sulfide ore.Sulfur cement changes in conjunction with sulphur
The surface chemical property for becoming sulphur, avoids sulphur in nickel sulfide ore adsorption, is conducive to the dissolution of nickel sulfide ore.Iron oxide crystal seed,
The ferric sulfate hydrolysis for being conducive to nickel sulfide ore oxidation production, crystallizes into iron oxide precipitating, convenient for separating with nickel sulfate solution；Vulcanization
The calcium impurities contained in nickel minerals, calcium sulfate precipitation easily generated cause fouling and line clogging in still kettle wall or pipeline, are added
Sulfuric acid calcium inhibitors can avoid crystal of calcium sulfate precipitating.This method preparation process is simple, and raw material is easy to get, when plurality of raw materials is reacted,
Mutually collaboration can promote the progress of reaction and offers product to invade extracting rate, have process short, leaching efficiency height, at low cost, green
The characteristics of colour circle is protected, and the leaching rate of nickel is all larger than 95% in nickel sulfide ore.
Specific embodiment
Below in conjunction with specific embodiment, invention is further described in detail.
The invention discloses a kind of methods for preparing nickel sulfate with nickel sulfide ore, include the following steps:
(1) it pre-processes
Nickel sulfide ore is levigate, and diluted acid is added in levigate nickel sulfide ore, and after stirring 1 hour, filters pressing obtains pretreatment sulphur
Change nickel minerals and aqueous solution, aqueous solution recycles magnesium salts by condensing crystallizing.
Fineness after nickel sulfide ore is levigate is 80 μm；Diluted acid be sulfuric acid solution, hydrochloric acid solution, nitric acid solution one kind, it is dense
Degree is 5%, and additional amount is the 100-300% of nickel sulfide ore quality.
(2) oxygen leaching
In nickel sulfide ore after the pre-treatment, sulfuric acid, oxidant, sulfur cement, sulfuric acid calcium inhibitors, iron oxide crystalline substance is added
Kind, it after mixing, is added in autoclave, and be passed through pressure-air, after reaction, separation of solid and liquid obtains nickel sulfate solution and leaching
It slags tap.Wherein oxidant is one of copper sulphate, hydrogen peroxide, Peracetic acid, potassium permanganate, ammonium persulfate, and additional amount is
The 10-20% of nickel sulfide ore quality；One of sulfur cement diethyldithiocarbamate, xanthate, thioacetic acid, additional amount are nickel sulfide mineral
The 1-5% of amount；Sulfuric acid calcium inhibitors are one of polyethylene diacid, polyacrylic acid, citric acid, and additional amount is nickel sulfide mineral
The 1-5% of amount.
Temperature in autoclave is 140-200 DEG C, and the reaction time is 6 hours；The additional amount of iron oxide crystal seed is nickel sulfide
The 1-5% of mineral amount.The concentration of sulfuric acid is 20%, and additional amount is the 100-300% of nickel sulfide ore quality.The pressure of pressure-air
For 2MPa.
Embodiment 1
(1) it pre-processes
Nickel sulfide ore is levigate, and the diluted acid (sulfuric acid, sulfuric acid, nitric acid) of 100g is added in levigate 100g nickel sulfide ore, stirs
After mixing 1 hour, filters pressing obtains pretreatment nickel sulfide ore and aqueous solution, and aqueous solution recycles magnesium salts by condensing crystallizing.Wherein, sulphur
Fineness after change nickel minerals is levigate is 80 μm.
(2) oxygen leaching
In nickel sulfide ore after the pre-treatment, 100g sulfuric acid (concentration of sulfuric acid is 20%), 10g oxidant, 1g sulphur is added
Bonding agent, 1g sulfuric acid calcium inhibitors and 1g iron oxide crystal seed are added in autoclave after mixing, and are passed through pressure-air,
After reacting under conditions of 140 DEG C, separation of solid and liquid obtains nickel sulfate solution and leached mud.Wherein, the additional amount of iron oxide crystal seed,
It is the 5% of pretreated nickel sulfide ore quality, the pressure of pressure-air is 2MPa, and the reaction time is 6 hours.
Table 1 lists the pretreatment of nickel sulfide ore and oxygen leaching formula in embodiment 1~16.
Table 1
In the embodiment of the present invention, the leaching rate of nickel is all larger than 95% in nickel sulfide ore.
Claims (8)
1. a kind of method for preparing nickel sulfate with nickel sulfide ore, which is characterized in that include the following steps:
(1) it pre-processes
Parts by weight meter, 100 parts of nickel sulfide ore is levigate, and 100-300 parts of diluted acids are added, after being stirred to react, filters pressing is obtained pre-
The nickel sulfide ore and aqueous solution of processing；
(2) oxygen leaching
In nickel sulfide ore after the pre-treatment, 100-300 parts of sulfuric acid, 10-20 parts of oxidants, 1-5 parts of sulfur cements, 1-5 are added
Part sulfuric acid calcium inhibitors and 1-5 parts of iron oxide crystal seeds are added in autoclave after mixing, and are passed through pressure-air,
After 140~200 DEG C are sufficiently reacted, separation of solid and liquid obtains nickel sulfate solution and leached mud；
Sulfur cement diethyldithiocarbamate, xanthate or the thioacetic acid；
The sulfuric acid calcium inhibitors are polyethylene diacid, polyacrylic acid or citric acid.
2. a kind of method for preparing nickel sulfate with nickel sulfide ore as described in claim 1, which is characterized in that in step (1), sulphur
Fineness after change nickel minerals is levigate is 80 μm.
3. a kind of method for preparing nickel sulfate with nickel sulfide ore as described in claim 1, which is characterized in that dilute in step (1)
Acid is sulfuric acid solution, hydrochloric acid solution or nitric acid solution, and mass concentration is 5%.
4. a kind of method for preparing nickel sulfate with nickel sulfide ore as described in claim 1, which is characterized in that in step (1), obtain
The aqueous solution arrived recycles magnesium salts by condensing crystallizing.
5. a kind of method for preparing nickel sulfate with nickel sulfide ore as described in claim 1, which is characterized in that high in step (2)
Pressing the reaction time in kettle is 6 hours.
6. a kind of method for preparing nickel sulfate with nickel sulfide ore as described in claim 1, which is characterized in that in step (2), sulphur
The mass concentration of acid is 20%.
7. a kind of method for preparing nickel sulfate with nickel sulfide ore as described in claim 1, which is characterized in that high in step (2)
The pressure for pressing air is 2MPa.
8. a kind of method for preparing nickel sulfate with nickel sulfide ore as described in claim 1, which is characterized in that the oxidant
For copper sulphate, hydrogen peroxide, Peracetic acid, potassium permanganate or ammonium persulfate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710848285.8A CN107777734B (en) | 2017-09-19 | 2017-09-19 | A method of nickel sulfate is prepared with nickel sulfide ore |
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| CN201710848285.8A CN107777734B (en) | 2017-09-19 | 2017-09-19 | A method of nickel sulfate is prepared with nickel sulfide ore |
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| CN107777734A CN107777734A (en) | 2018-03-09 |
| CN107777734B true CN107777734B (en) | 2019-06-07 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110826B (en) * | 2018-09-05 | 2020-11-06 | 广西银亿新材料有限公司 | Production method of battery-grade nickel sulfate |
| CN111411222B (en) * | 2020-03-30 | 2022-02-01 | 东北大学秦皇岛分校 | Method for extracting valuable metal from copper-nickel sulfide ammonium persulfate-sulfuric acid through oxidation leaching |
| CN112680602A (en) * | 2020-12-18 | 2021-04-20 | 衢州华友钴新材料有限公司 | Treatment method for improving leaching efficiency of copper-containing sulfide ore |
| CN113215398B (en) * | 2021-05-06 | 2022-03-29 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method of nickel sulfide concentrate |
| CN114058850B (en) * | 2021-11-04 | 2022-09-16 | 中南大学 | Process for leaching nickel from sintered nickel alloy body |
| CN114477319B (en) * | 2022-03-03 | 2024-06-11 | 湖南中先智能科技有限公司 | Nickel sulfate preparation process and equipment |
| CN115747489A (en) * | 2022-12-06 | 2023-03-07 | 金川集团镍盐有限公司 | Method for leaching high-magnesium low-nickel sulfide ore under normal pressure |
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| CN1786225A (en) * | 2005-07-09 | 2006-06-14 | 云南锡业集团有限责任公司 | Wet treatment method of iron containing nickel sulfide material |
| AU2008100563B4 (en) * | 2008-06-13 | 2008-09-04 | Murrin Murrin Operations Pty Ltd | Method for the Recovery of Nickel from Ores |
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| CN105363564A (en) * | 2015-12-10 | 2016-03-02 | 内蒙古科技大学 | Desulfurization reagent for removing pyrrhotite in iron concentrate containing high sulphur by flotation method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US7799296B2 (en) * | 2003-12-04 | 2010-09-21 | Ovonic Battery Company, Inc. | Method of producing a nickel salt solution |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1786225A (en) * | 2005-07-09 | 2006-06-14 | 云南锡业集团有限责任公司 | Wet treatment method of iron containing nickel sulfide material |
| AU2008100563B4 (en) * | 2008-06-13 | 2008-09-04 | Murrin Murrin Operations Pty Ltd | Method for the Recovery of Nickel from Ores |
| CN101760617A (en) * | 2008-12-24 | 2010-06-30 | 中国恩菲工程技术有限公司 | Improved method for leaching magnesium-containing ore |
| CN101805828A (en) * | 2010-04-19 | 2010-08-18 | 中南大学 | Low-cost method for disposing red soil nickel ore |
| CN102994746A (en) * | 2012-11-21 | 2013-03-27 | 广西藤县雅照钛白有限公司 | Method for producing nickel sulfide ore concentrate by use of industrial waste acid |
| CN105363564A (en) * | 2015-12-10 | 2016-03-02 | 内蒙古科技大学 | Desulfurization reagent for removing pyrrhotite in iron concentrate containing high sulphur by flotation method |
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Granted publication date: 20190607 Termination date: 20200919 |