CN102061387A - Two-stage type nickel precipitation method - Google Patents
Two-stage type nickel precipitation method Download PDFInfo
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- CN102061387A CN102061387A CN2011100015272A CN201110001527A CN102061387A CN 102061387 A CN102061387 A CN 102061387A CN 2011100015272 A CN2011100015272 A CN 2011100015272A CN 201110001527 A CN201110001527 A CN 201110001527A CN 102061387 A CN102061387 A CN 102061387A
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Abstract
The invention discloses a two-stage type nickel precipitation method. The method comprises the following steps of: (1) primary nickel precipitation: adding a NaOH solution to a nickel sulfate solution containing magnesium, regulating a pH value to be 7.5-8.5 and reacting at a temperature of 20-80 DEG C for 0.5-3 h; (2) separating precipitates obtained in the step (1) from a nickel precipitation mother liquid; (3) secondary nickel precipitation: adding a NaOH solution to the nickel precipitation mother liquid obtained in the step (2), regulating the pH value to 9-10 and reacting at a temperature of 20-80 DEG C for 0.5-3 h; (4) separating precipitates obtained in the step (3) from the nickel precipitation mother liquid and returning precipitates obtained in the step (4) by separation to a system of an agitation and leaching procedure to be cycled. Nickel hydroxide products containing more than 45% of nickel can be precipitated with the two-stage type nickel precipitation method, and the nickel precipitation rate can reach more than 99%.
Description
Technical field
The present invention relates to a kind of sulfuric acid leaching and produce the method for metallic nickel and nickel salt, relate in particular to a kind of from nickel sulfate solution the method for heavy nickel separating nickel magnesium.
Background technology
The normal pressure acid leaching process of red soil nickel ore is the comparatively popular direction of present red soil nickel ore treatment process research.The technology that existing normal pressure pickling process is handled red soil nickel ore is: red soil nickel ore is carried out fragmentation and ore grinding earlier handle, ore pulp after levigate and sulfuric acid are reacted under the condition of heating according to a certain percentage, nickel metal in the ore leached enters solution, simultaneously some for example metal such as magnesium, manganese also can be leached simultaneously and be entered in the solution.Leach liquor carries out liquid-solid separation with filter.Filtrate is sunk nickel with precipitation agent and is obtained the nickel throw out, and magnesium is stayed in the solution, obtains the high nickel salt of purity thereby nickel magnesium separated.Precipitation agent commonly used has sulfide, sodium hydroxide, yellow soda ash etc.
But there are following some shortcomings in tradition when adopting metallic sulfide as the sulfide precipitation agent: as precipitation agent, often need pressurized, heated with hydrogen sulfide, sodium sulphite etc., and the operational condition harshness, the facility investment height is unfavorable for producing; Sulfide precipitation is subjected to the influence of acidity very big, precipitation agent Na
2S9H
2O has following ionization reaction: Na in the aqueous solution
2S 2Na
++ S
2-, S in acidic solution
2-Also can react and generate H
2S gas: S
2-+ H
+HS
-, HS
-+ H
+H
2S so not only can cause the precipitation agent loss, makes precipitation not exclusively, and environment is polluted.
At the deficiency of the heavy nickel of sulfuration, the someone proposes sodium hydroxide with economic environmental protection and sinks the method for nickel.It is low that this method has a cost, and less investment does not produce obnoxious flavoures such as hydrogen sulfide, good operational environment, advantages such as safety and environmental protection.But nickel ion has the part magnesium ion when precipitating fully precipitates simultaneously, thus higher with containing magnesium in the heavy nickel postprecipitation of sodium hydroxide, the subsequent disposal trouble.
Summary of the invention
In view of this, the purpose of this invention is to provide the heavy nickel method of a kind of two-section type, it can improve nickel content in the nickel hydroxide, reduces the content of magnesium, improves the direct yield of nickel.
Above-mentioned purpose realizes by following proposal:
A kind of two-section type is sunk the nickel method, it is characterized in that, said method comprising the steps of:
1) one section heavy nickel: in the nickel sulfate solution that contains magnesium, add NaOH solution, adjust the pH value 7.5
-8.5 temperature of reaction is 20-80 ℃, the reaction times is 0.5-3 hour;
2) precipitation that step 1) is obtained is separated with heavy nickel mother liquor;
3) add NaOH solution in the heavy nickel mother liquor that obtains two sections heavy nickel: to step 2), adjust the pH value at 9-10, temperature of reaction is 20-80 ℃, and the reaction times is 0.5-3 hour;
4) precipitation that step 3) is obtained is separated with heavy nickel mother liquor, and will separate system's internal recycle that the precipitation that obtains is back to the agitation leach operation in this step 4).
According to aforesaid method, it is characterized in that in step 1), the nickel concentration in the single nickel salt is 3.42g/l, magnesium density is 30.28g/l, and the NaOH strength of solution is 40g/l, and adjusting the pH value is 7.5, and temperature of reaction is 80 ℃, the reaction times is 3 hours; In step 3), the NaOH strength of solution is 40g/l, and adjusting the pH value is 9, and temperature of reaction is 80 ℃, and the reaction times is 3 hours.
According to aforesaid method, it is characterized in that in step 1), the nickel concentration in the single nickel salt is 2.9g/l, magnesium density is 25.09g/l, and the NaOH strength of solution is 45g/l, and adjusting the pH value is 8.15, and temperature of reaction is 50 ℃, the reaction times is 1.5 hours; In step 3), the NaOH strength of solution is 40g/l, and the pH value is 10, and temperature of reaction is 50 ℃, and the reaction times is 0.5 hour.
According to aforesaid method, it is characterized in that in step 1), the nickel concentration in the single nickel salt is 1.95g/l, magnesium density is 19.74g/l, and the NaOH strength of solution is 50g/l, and adjusting the pH value is 8.5, and temperature of reaction is 20 ℃, the reaction times is 0.5 hour; In step 3), the NaOH strength of solution is 40g/l, and the pH value is 9.3, and temperature of reaction is 20 ℃, and the reaction times is 2 hours.
Beneficial effect of the present invention: (1) nickel hydroxide nickel content height.Adopt such scheme, precipitablely go out nickeliferously greater than 45% nickel hydroxide product, and the nickel deposition rate reaches more than 99%; (2) to contain moisture low for nickel hydroxide.Adopt such scheme, the nickel hydroxide that is settled out contains moisture less than 55%.(3) to contain magnesium low for precipitation, and Mg content can drop to below 1%.(4) to have sedimentation speed fast for processing method of the present invention, and strainability is good, process characteristics such as nickel, cobalt yield height.It is simple that the present invention also has technical process in addition, less investment, and energy consumption is low, and production cost is low, and is free from environmental pollution, the more high advantage of social benefit and economic benefit.
Description of drawings
Fig. 1 is the schema of the heavy nickel method of two-section type of the present invention.
Embodiment
Referring to Fig. 1, leach the nickel sulfate solution that contains magnesium that obtains after the also removal of impurities from red soil nickel ore by sulfuric acid, carry out following processing:
1) one section heavy nickel: add NaOH solution in the nickel sulfate solution that contains magnesium, adjust the pH value at 7.5-8.5, temperature of reaction is 20-80 ℃, and the reaction times is 0.5-3 hour;
2) precipitation that step 1) is obtained is separated with heavy nickel mother liquor, and the precipitation that obtains enters refining procedure;
3) add NaOH solution in the heavy nickel mother liquor that obtains two sections heavy nickel: to step 2), adjust the pH value at 9-10, temperature of reaction is 20-80 ℃, and the reaction times is 0.5-3 hour;
4) precipitation that step 3) is obtained is separated with heavy nickel mother liquor, and will separate system's internal recycle that the precipitation that obtains is back to the agitation leach operation in this step 4).
Embodiment 1
The red soil nickel ore leach liquor contains nickel concentration 3.43g/l, contains magnesium 30.28 g/l.The aqueous sodium hydroxide solution that adds 40g/l, adjusting pH value is 7.5,80 degrees centigrade of temperature were reacted 3 hours, carried out liquid-solid separation.Obtain precipitation and contain magnesium 0.12%, nickeliferous 50%, separate the nickeliferous 0.343g/l of solution that obtains, contain magnesium 30.26g/l.The solution that separation obtains is 9.0 with the aqueous sodium hydroxide solution continuation rising pH value of 40g/l, and 80 degrees centigrade of temperature were reacted 3 hours, carry out liquid-solid separation, obtain precipitating nickeliferous 35.91%, contain magnesium 6.92%, separate obtaining the nickeliferous 0.0099g/l of solution, contain magnesium 30.20g/l.
Embodiment 2
The red soil nickel ore leach liquor contains nickel concentration 2.9g/l, contains magnesium 25.09g/l.The aqueous sodium hydroxide solution that adds 45g/l, adjusting pH value is 8.15,50 degrees centigrade of temperature were reacted 1.5 hours, carried out liquid-solid separation.Obtain precipitation and contain magnesium 0.43%, nickeliferous 47.45%, separate the nickeliferous 0.29g/l of solution that obtains, contain magnesium 25.07g/l.The solution that separation obtains is 10 with the aqueous sodium hydroxide solution continuation rising pH value of 40g/l, and 50 degrees centigrade of temperature were reacted 0.5 hour, carry out liquid-solid separation, obtain precipitating nickeliferous 36.5%, contain magnesium 7.48%, separate obtaining the nickeliferous 0.0082g/l of solution, contain magnesium 24.65g/l.
Embodiment 3
The red soil nickel ore leach liquor contains nickel concentration 1.95g/l, contains magnesium 19.74 g/l.The aqueous sodium hydroxide solution that adds 50g/l, adjusting pH value is 8.5,20 degrees centigrade of temperature were reacted 0.5 hour, carried out liquid-solid separation.Obtain precipitation and contain magnesium 0.95%, nickeliferous 45.88%, separate the nickeliferous 0.195g/l of solution that obtains, contain magnesium 19.73g/l.The solution that separation obtains is 9.3 with the aqueous sodium hydroxide solution continuation rising pH value of 40g/l, and 20 degrees centigrade of temperature were reacted 2 hours, carry out liquid-solid separation, obtain precipitating nickeliferous 38. 1%, contain magnesium 7.62%, separate obtaining the nickeliferous 0.0076g/l of solution, contain magnesium 19.70g/l.
Embodiment 4
The red soil nickel ore leach liquor contains nickel concentration 2.35g/l, contains magnesium 21.34 g/l.The aqueous sodium hydroxide solution that adds 50g/l, adjusting pH value is 8.3,20 degrees centigrade of temperature were reacted 1.3 hours, carried out liquid-solid separation.Obtain precipitation and contain magnesium 0.60%, nickeliferous 46.42%, separate the nickeliferous 0.21g/l of solution that obtains, contain magnesium 23.73g/l.The solution that separation obtains is 9.5 with the aqueous sodium hydroxide solution continuation rising pH value of 40g/l, and 20 degrees centigrade of temperature were reacted 3 hours, carry out liquid-solid separation, obtain precipitating nickeliferous 37. 1%, contain magnesium 7.81%, separate obtaining the nickeliferous 0.0079g/l of solution, contain magnesium 22.41g/l.
Claims (4)
1. the heavy nickel method of two-section type is characterized in that, said method comprising the steps of:
1) one section heavy nickel: add NaOH solution in the nickel sulfate solution that contains magnesium, adjust the pH value at 7.5-8.5, temperature of reaction is 20-80 ℃, and the reaction times is 0.5-3 hour;
2) precipitation that step 1) is obtained is separated with heavy nickel mother liquor;
3) add NaOH solution in the heavy nickel mother liquor that obtains two sections heavy nickel: to step 2), adjust the pH value at 9-10, temperature of reaction is 20-80 ℃, and the reaction times is 0.5-3 hour;
4) precipitation that step 3) is obtained is separated with heavy nickel mother liquor, and will separate system's internal recycle that the precipitation that obtains is back to the agitation leach operation in this step 4).
2. method according to claim 1 is characterized in that, in step 1), the nickel concentration in the single nickel salt is 3.42g/l, and magnesium density is 30.28g/l, and the NaOH strength of solution is 40g/l, and adjusting the pH value is 7.5, and temperature of reaction is 80 ℃, and the reaction times is 3 hours; In step 3), the NaOH strength of solution is 40g/l, and adjusting the pH value is 9, and temperature of reaction is 80 ℃, and the reaction times is 3 hours.
3. method according to claim 1 is characterized in that, in step 1), the nickel concentration in the single nickel salt is 2.9g/l, and magnesium density is 25.09g/l, and the NaOH strength of solution is 45g/l, and adjusting the pH value is 8.15, and temperature of reaction is 50 ℃, and the reaction times is 1.5 hours; In step 3), the NaOH strength of solution is 40g/l, and the pH value is 10, and temperature of reaction is 50 ℃, and the reaction times is 0.5 hour.
4. method according to claim 1 is characterized in that, in step 1), the nickel concentration in the single nickel salt is 1.95g/l, and magnesium density is 19.74g/l, and the NaOH strength of solution is 50g/l, and adjusting the pH value is 8.5, and temperature of reaction is 20 ℃, and the reaction times is 0.5 hour; In step 3), the NaOH strength of solution is 40g/l, and the pH value is 9.3, and temperature of reaction is 20 ℃, and the reaction times is 2 hours.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874852A (en) * | 2012-09-28 | 2013-01-16 | 广西银亿科技矿冶有限公司 | High-activity magnesite powder and manufacturing method thereof and method for reclaiming nickel cobalt from laterite nickel ores |
| CN103468972A (en) * | 2013-08-15 | 2013-12-25 | 中国恩菲工程技术有限公司 | Treatment method for comprehensive recycling of scandium and nickel cobalt from lateritic nickel ore |
| CN103993174A (en) * | 2014-05-23 | 2014-08-20 | 中国恩菲工程技术有限公司 | Method of precipitating nickel by using mixed base |
| WO2015027888A1 (en) * | 2013-08-26 | 2015-03-05 | 中国恩菲工程技术有限公司 | Nickel hydroxide product and preparation method thereof |
| CN111471863A (en) * | 2019-01-24 | 2020-07-31 | 河北中科同创道格赛尔新材料科技有限公司 | Method for step-by-step alkaline precipitation of nickel |
| CN115212891A (en) * | 2021-04-21 | 2022-10-21 | 浙江微通催化新材料有限公司 | Preparation method of carbon-supported Pd-Ni bimetallic catalyst and application of carbon-supported Pd-Ni bimetallic catalyst in Suzuki coupling reaction |
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| CN1995414A (en) * | 2006-12-20 | 2007-07-11 | 潘继红 | Vitriol intensified leach extraction method for nickel oxide ore |
| CN101230422A (en) * | 2008-02-02 | 2008-07-30 | 贵研铂业股份有限公司 | Method for enriching nickel from lateritic nickel with co-production of iron-oxide red |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874852A (en) * | 2012-09-28 | 2013-01-16 | 广西银亿科技矿冶有限公司 | High-activity magnesite powder and manufacturing method thereof and method for reclaiming nickel cobalt from laterite nickel ores |
| CN103468972A (en) * | 2013-08-15 | 2013-12-25 | 中国恩菲工程技术有限公司 | Treatment method for comprehensive recycling of scandium and nickel cobalt from lateritic nickel ore |
| CN103468972B (en) * | 2013-08-15 | 2016-02-24 | 中国恩菲工程技术有限公司 | The treatment process of red soil nickel ore synthetical recovery scandium and nickel cobalt |
| WO2015027888A1 (en) * | 2013-08-26 | 2015-03-05 | 中国恩菲工程技术有限公司 | Nickel hydroxide product and preparation method thereof |
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| CN103993174A (en) * | 2014-05-23 | 2014-08-20 | 中国恩菲工程技术有限公司 | Method of precipitating nickel by using mixed base |
| CN103993174B (en) * | 2014-05-23 | 2016-06-29 | 中国恩菲工程技术有限公司 | The method of mixed base coprecipitated nickel hydroxide |
| CN111471863A (en) * | 2019-01-24 | 2020-07-31 | 河北中科同创道格赛尔新材料科技有限公司 | Method for step-by-step alkaline precipitation of nickel |
| CN115212891A (en) * | 2021-04-21 | 2022-10-21 | 浙江微通催化新材料有限公司 | Preparation method of carbon-supported Pd-Ni bimetallic catalyst and application of carbon-supported Pd-Ni bimetallic catalyst in Suzuki coupling reaction |
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Application publication date: 20110518 |