CN107777734A - A kind of method that nickel sulfate is prepared with nickel sulfide ore - Google Patents
A kind of method that nickel sulfate is prepared with nickel sulfide ore Download PDFInfo
- Publication number
- CN107777734A CN107777734A CN201710848285.8A CN201710848285A CN107777734A CN 107777734 A CN107777734 A CN 107777734A CN 201710848285 A CN201710848285 A CN 201710848285A CN 107777734 A CN107777734 A CN 107777734A
- Authority
- CN
- China
- Prior art keywords
- nickel
- sulfide ore
- prepared
- nickel sulfide
- nickel sulfate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of method that nickel sulfate is prepared with nickel sulfide ore, this method comprises the following steps：It is levigate to be firstly vulcanized nickel minerals, after addition diluted acid goes the removal of impurity, adds sulfuric acid, oxidant, sulfur cement, sulfuric acid calcium inhibitors, iron oxide crystal seed, after being well mixed, it is added in autoclave, and pressure-air is passed through, after reaction, separation of solid and liquid obtains nickel sulfate solution and leached mud.The present invention has the characteristics of flow is short, and leaching efficiency is high, and cost is low, green.
Description
Technical field
The present invention relates to nickel sulfide ore recycling field, and in particular to a kind of side that nickel sulfate is prepared with nickel sulfide ore
Method.
Background technology
The handling process of nickel sulfide ore generally can be divided into pyrogenic process and wet method.Pyrogenic attack technique is to use matte smelting, will
Ni-B alloy in nickel sulfide ore is into low nickel matte, then by low nickel matte with bessemerizing into high nickel matte, then produces through different method of refining
Go out different nickel products.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, puies forward 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 more than 1 atmospheric pressure in pressure, and ore or concentrate are handled with solution, is the complicated metalliferous mineral of processing
One of hydrometallurgy new process of resource.Have compared to normal pressure leaching, the characteristics of pressure leaching：(1) extraction temperature is improved, accelerates leaching
Go out speed, accelerate extraction time；(2) mineral that can make some can not be reacted at normal temperatures and pressures occur a certain degree of
Reaction；(3) pressurization causes oxygen or ammonia to have higher partial pressure in leaching process, Strengthen education process, improves the leaching of metal
Rate.(4), can the complicated material of processes composition for the strong adaptability of raw material.
But at present, there is impurity removal difficulty, extraction time length, the low problem of leaching efficiency in pressure leaching.
The content of the invention
To solve the problems, such as that prior art is present, the invention provides a kind of method that nickel sulfate is prepared with nickel sulfide ore.
This method has the characteristics of flow is short, and leaching efficiency is high, and cost is low, green.
To achieve the above objectives, this invention takes following technical scheme：
A kind of method that nickel sulfate is prepared with nickel sulfide ore, comprises the steps：
(1) pre-process
Parts by weight meter, 100 parts of nickel sulfide ore is levigate, and 100-300 part diluted acids are added, after stirring reaction, press filtration, obtain
To the nickel sulfide ore and the aqueous solution of pretreatment；
(2) oxygen leaching
In nickel sulfide ore after the pre-treatment, add 100-300 parts sulfuric acid, 10-20 parts oxidant, 1-5 parts sulfur cement,
1-5 part sulfuric acid calcium inhibitorses and 1-5 part iron oxide crystal seeds, after being well mixed, it is added in autoclave, and is passed through pressure-air,
After 140~200 DEG C fully 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 salpeter solution, and mass concentration is 5%.
In step (1), the obtained aqueous solution reclaims 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.
Described oxidant is copper sulphate, hydrogen peroxide, Peracetic acid, potassium permanganate or ammonium persulfate.
Described sulfur cement diethyldithiocarbamate, xanthate or TGA.
Described sulfuric acid calcium inhibitors is polyethylene diacid, polyacrylic acid or citric acid.
Relative to prior art, 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 addition diluted acid goes the removal of impurity,
Sulfuric acid, oxidant are added, sulfur cement, sulfuric acid calcium inhibitors, iron oxide crystal seed, after being well mixed, is added in autoclave, and
Pressure-air is passed through, 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 easily and acid reaction, generates magnesium sulfate, so as to realize the separation of magnesium and nickel sulfide concentrate.Wherein, oxygen
Agent can generate elemental sulfur, promote the dissolving of nickel sulfide ore with the reaction of Salmon-Saxl in nickel sulfide ore.Sulfur cement is combined with sulphur, is changed
Become the surface chemical property of sulphur, avoid sulphur from being advantageous to the dissolving of nickel sulfide ore in nickel sulfide ore adsorption.Iron oxide crystal seed,
Be advantageous to the ferric sulfate hydrolysis of nickel sulfide ore oxidation production, crystallize into iron oxide precipitation, be easy to separate with nickel sulfate solution；Vulcanization
The calcium impurities contained in nickel minerals, calcium sulfate precipitation is easily generated in still kettle wall or pipeline, fouling and line clogging is caused, adds
Sulfuric acid calcium inhibitors can avoid crystal of calcium sulfate from 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 that flow is short, leaching efficiency height, and cost is low, green
The characteristics of colour circle is protected, and the leaching rate of nickel is all higher than 95% in nickel sulfide ore.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment.
The invention discloses a kind of method that nickel sulfate is prepared with nickel sulfide ore, comprise the steps：
(1) pre-process
Nickel sulfide ore is levigate, and diluted acid is added in levigate nickel sulfide ore, after stirring 1 hour, press filtration, obtains pre-processing sulphur
Change nickel minerals and the aqueous solution, the aqueous solution reclaims magnesium salts by condensing crystallizing.
Fineness after nickel sulfide ore is levigate is 80 μm；Diluted acid is sulfuric acid solution, hydrochloric acid solution, one kind of salpeter solution, dense
Degree is 5%, and addition 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 are added
Kind, after being well mixed, it is added in autoclave, and pressure-air is passed through, after reaction, separation of solid and liquid obtains nickel sulfate solution and leaching
Slag tap.Wherein oxidant is one kind in copper sulphate, hydrogen peroxide, Peracetic acid, potassium permanganate, ammonium persulfate, and addition is
The 10-20% of nickel sulfide ore quality；One kind in sulfur cement diethyldithiocarbamate, xanthate, TGA, addition are nickel sulfide mineral
The 1-5% of amount；Sulfuric acid calcium inhibitors is one kind in polyethylene diacid, polyacrylic acid, citric acid, and addition 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 addition of iron oxide crystal seed, it is nickel sulfide
The 1-5% of mineral amount.The concentration of sulfuric acid is 20%, and addition is the 100-300% of nickel sulfide ore quality.The pressure of pressure-air
For 2MPa.
Embodiment 1
(1) pre-process
Nickel sulfide ore is levigate, and 100g diluted acid (sulfuric acid, sulfuric acid, nitric acid) is added in levigate 100g nickel sulfide ores, is stirred
After mixing 1 hour, press filtration, obtain pre-processing nickel sulfide ore and the aqueous solution, the aqueous solution reclaims 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 oxidants, 1g sulphur are added
Bonding agent, 1g sulfuric acid calcium inhibitors and 1g iron oxide crystal seeds, after being well mixed, it is added in autoclave, and is passed through pressure-air,
After being reacted under conditions of 140 DEG C, separation of solid and liquid obtains nickel sulfate solution and leached mud.Wherein, the addition of iron oxide crystal seed,
For 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 embodiments of the invention, the leaching rate of nickel is all higher than 95% in nickel sulfide ore.
Claims (10)
- A kind of 1. method that nickel sulfate is prepared with nickel sulfide ore, it is characterised in that comprise the steps：(1) pre-processParts by weight meter, 100 parts of nickel sulfide ore is levigate, and 100-300 part diluted acids are added, after stirring reaction, press filtration, obtain pre- The nickel sulfide ore and the aqueous solution of processing；(2) oxygen leachingIn nickel sulfide ore after the pre-treatment, 100-300 parts sulfuric acid, 10-20 parts oxidant, 1-5 parts sulfur cement, 1-5 are added Part sulfuric acid calcium inhibitors and 1-5 part iron oxide crystal seeds, after being well mixed, it is added in autoclave, and is passed through pressure-air, After 140~200 DEG C are fully reacted, separation of solid and liquid obtains nickel sulfate solution and leached mud.
- A kind of 2. method that nickel sulfate is prepared with nickel sulfide ore as claimed in claim 1, it is characterised in that in step (1), sulphur Fineness after change nickel minerals is levigate is 80 μm.
- 3. a kind of method that nickel sulfate is prepared with nickel sulfide ore as claimed in claim 1, it is characterised in that dilute in step (1) Acid is sulfuric acid solution, hydrochloric acid solution or salpeter solution, and mass concentration is 5%.
- 4. a kind of method that nickel sulfate is prepared with nickel sulfide ore as claimed in claim 1, it is characterised in that in step (1), obtain The aqueous solution arrived reclaims magnesium salts by condensing crystallizing.
- 5. a kind of method that nickel sulfate is prepared with nickel sulfide ore as claimed in claim 1, it is characterised in that high in step (2) It is 6 hours to press the reaction time in kettle.
- A kind of 6. method that nickel sulfate is prepared with nickel sulfide ore as claimed in claim 1, it is characterised in that in step (2), sulphur The mass concentration of acid is 20%.
- 7. a kind of method that nickel sulfate is prepared with nickel sulfide ore as claimed in claim 1, it is characterised in that high in step (2) The pressure for pressing air is 2MPa.
- A kind of 8. method that nickel sulfate is prepared with nickel sulfide ore as claimed in claim 1, it is characterised in that described oxidant For copper sulphate, hydrogen peroxide, Peracetic acid, potassium permanganate or ammonium persulfate.
- 9. a kind of method that nickel sulfate is prepared with nickel sulfide ore as claimed in claim 1, it is characterised in that described sulphur combines Agent diethyldithiocarbamate, xanthate or TGA.
- A kind of 10. method that nickel sulfate is prepared with nickel sulfide ore as claimed in claim 1, it is characterised in that described sulfuric acid Calcium inhibitors is polyethylene diacid, polyacrylic acid or citric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710848285.8A CN107777734B (en) | 2017-09-19 | 2017-09-19 | A method of nickel sulfate is prepared with nickel sulfide ore |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710848285.8A CN107777734B (en) | 2017-09-19 | 2017-09-19 | A method of nickel sulfate is prepared with nickel sulfide ore |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107777734A true CN107777734A (en) | 2018-03-09 |
| CN107777734B CN107777734B (en) | 2019-06-07 |
Family
ID=61438088
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710848285.8A Expired - Fee Related CN107777734B (en) | 2017-09-19 | 2017-09-19 | A method of nickel sulfate is prepared with nickel sulfide ore |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107777734B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110826A (en) * | 2018-09-05 | 2019-01-01 | 广西银亿新材料有限公司 | A kind of production method of LITHIUM BATTERY nickel sulfate |
| CN111411222A (en) * | 2020-03-30 | 2020-07-14 | 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 |
| CN113215398A (en) * | 2021-05-06 | 2021-08-06 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method of nickel sulfide concentrate |
| CN114058850A (en) * | 2021-11-04 | 2022-02-18 | 中南大学 | Process for leaching nickel from sintered nickel alloy body |
| CN114477319A (en) * | 2022-03-03 | 2022-05-13 | 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 |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060067874A1 (en) * | 2003-12-04 | 2006-03-30 | Chevrontexaco Technology Ventures Llc | Method of producing a nickel salt solution |
| 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 |
-
2017
- 2017-09-19 CN CN201710848285.8A patent/CN107777734B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060067874A1 (en) * | 2003-12-04 | 2006-03-30 | Chevrontexaco Technology Ventures Llc | Method of producing a nickel salt solution |
| 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 |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110826A (en) * | 2018-09-05 | 2019-01-01 | 广西银亿新材料有限公司 | A kind of production method of LITHIUM BATTERY nickel sulfate |
| CN111411222A (en) * | 2020-03-30 | 2020-07-14 | 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 |
| 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 |
| CN113215398A (en) * | 2021-05-06 | 2021-08-06 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method of nickel sulfide concentrate |
| CN114058850A (en) * | 2021-11-04 | 2022-02-18 | 中南大学 | Process for leaching nickel from sintered nickel alloy body |
| CN114477319A (en) * | 2022-03-03 | 2022-05-13 | 湖南中先智能科技有限公司 | Nickel sulfate preparation process and equipment |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107777734B (en) | 2019-06-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107777734A (en) | A kind of method that nickel sulfate is prepared with nickel sulfide ore | |
| US20060191377A1 (en) | Method for processing elemental sulfur-bearing materials using high temperature pressure leaching | |
| CN1800422A (en) | Method for processing cobalt copper alloy | |
| CN106460089A (en) | Process for recovery of copper from arsenic-bearing and/or antimony-bearing copper sulphide concentrates | |
| WO2015129385A1 (en) | Method for producing hematite for iron production | |
| CN107034359A (en) | A kind of utilization cyanide wastewater reclaims the method for neutralizing valuable metal in waste residue | |
| CN103088206A (en) | Chemical metallurgy method for extracting beryllium oxide from chrysoberyl | |
| CN103484694A (en) | Method for extracting bismuth from copper-bismuth concentrate | |
| CN104204246A (en) | Method for producing hematite for iron production | |
| CN111235404A (en) | Impurity removal method for producing cobalt hydroxide from copper raffinate | |
| JP2022514634A (en) | Process for metal recovery from multi-metal nodules | |
| JP2010090420A (en) | Method for removing arsenic in concentrate for non-ferrous metal smelting and concentrate for non-ferrous metal smelting obtained by the method | |
| CN103993170A (en) | Method for recycling metals from copper-lead-zinc-arsenic-antimony bulk concentrate | |
| AU2009259277B2 (en) | Method for leaching nickel matte in the presence of added copper | |
| CA2931118C (en) | Process for producing refined nickel and other products from a mixed hydroxide intermediate | |
| CN107777735B (en) | A method of ammonium nickel sulfate is prepared with nickel sulfide ore normal pressure | |
| CN102021332A (en) | Technology for recycling Ni, Co, Fe, and Mg from nickel oxide mineral | |
| US3817743A (en) | Treatment of copper iron sulfides to form x-bornite | |
| CN103589880B (en) | Method for preparing crude bismuth by reducing bismuth oxychloride | |
| CN108467054B (en) | Method for recycling feed-grade basic copper chloride from waste circuit boards and application of method | |
| AU2013220926B2 (en) | Process for zinc oxide production from ore | |
| JP2011032149A (en) | Method for producing crude nickel sulfate solution | |
| CN105013615A (en) | Technology for extracting scheelite from low-grade scheelite floatation tailing | |
| CN114182094B (en) | Comprehensive recycling method for valuable metals in hard alloy grinding material | |
| CN108048671A (en) | A kind of heterogenite leaching method of low cost |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190607 Termination date: 20200919 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |