CN101717857B - Method for rapidly and directly dipping nickel sulfide concentrate under action of ultrasonic wave - Google Patents
Method for rapidly and directly dipping nickel sulfide concentrate under action of ultrasonic wave Download PDFInfo
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- CN101717857B CN101717857B CN2009101842839A CN200910184283A CN101717857B CN 101717857 B CN101717857 B CN 101717857B CN 2009101842839 A CN2009101842839 A CN 2009101842839A CN 200910184283 A CN200910184283 A CN 200910184283A CN 101717857 B CN101717857 B CN 101717857B
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Abstract
The invention discloses a method for rapidly and directly dipping nickel sulfide concentrate under the action of ultrasonic wave, belonging to the field of heavy non-ferrous metal hydrometallurgy. The method comprises the following steps of: crushing nickel ore (or directly using commercially-sold ore fines) and ensuring that the granularity of over 90 percent of ore is 0.15-0.08 mm; evenly mixing the nickel ore and water and placing the mixture into a stainless steel reactor, wherein the weight ratio of the water to the nickel ore is 5-30:1; adding an oxidant which can be sodium nitrate or potassium nitrate, wherein the weight ratio of concentrated sulfuric acid to the nickel ore is 0.5-1.1:1; finally keeping the ultrasonic frequency at 20.02kHz and the power at 50-150W under the action of ultrasonic wave; and directly dipping at normal pressure and normal temperature for 40-60 min. The invention has the characteristics of operation at normal pressure, high reaction speed, high leaching rate up to 97-99 percent for only 40-60 min and relative safety and low cost by taking solid nitrate as the oxidant.
Description
Technical field
The invention belongs to heavy non-ferrous metal hydrometallurgy field, particularly under the ultrasonic wave effect, from nickel sulfide concentrate, directly leach the novel method of nickel through the oxidation acidolysis.
Background technology
Nickel sulfide concentrate is because itself and associated mineral character thereof, therefrom extracts metallic nickel and is not easy: the recovery of the low-concentration sulfur dioxide that pyrometallurgical processes produces is still a global difficult problem so far; Wet method is soaked the nickel process can not produce sulfurous gas, but leaching velocity is slow usually, and efficient is low, length consuming time, cost height.
Soak nickel process poor efficiency, consuming time, expensive problem for solving wet method, various wet methods are soaked the nickel new technological process and have been carried.For sake of convenience, by the basic parameter of its operation, with its be divided into two kinds of normal temperature and pressure method and high temperature and high pressure methods (Hydrometallurgy, 2008,91:35-55).According to the character of soaking nickel sulfide concentrate and concrete process characteristic, these two kinds of methods also replace sometimes or segmentation is used.
High temperature and high pressure method has higher leaching efficiency, leaching velocity and lower advantages such as leaching agent consumption faster.But also exist the energy consumption height, to the requirement height of equipment, the input and the high deficiency of maintenance cost of equipment.When purpose element leaching yield was improved, the leaching yield of various associated elements also improved simultaneously; And shortcoming such as operative technique complexity also seriously restricts its popularization.For example, the high pressure-temperature method leaches the method for nickel (Chinese patent CN1352308A) with sulfuric acid from nickel sulfide concentrate, require the stagnation pressure of leaching process to reach 1.0～1.3 * 10
6Pa, oxygen partial pressure reaches 2～3 * 105Pa, and extraction temperature reaches 100～180 ℃, and extraction time is 1～6 hour.And for example, United States Patent (USP) (US5855858) leaches nickel sulfide concentrate with sulfuric acid (40g/l)+hydrochloric acid (10-12g/l) under the high temperature of the high pressure of 0.2～2.0 * 106Pa and 90～160 ℃, and extraction time is 0.5～5.0 hour, and leaching yield is about 90～99%.
The advantage that the normal temperature and pressure method leaches nickel sulfide concentrate is tangible: at first saved energy consumption; The equipment that does not need special high temperature high voltage resistant; Lower equipment input and maintenance of equipment expense are arranged; The bigger security and the adaptability of broad are arranged; The leaching of associated element is also lower, thereby helps next step removal of impurities operation.But its shortcoming also is tangible: as slower leaching velocity; Lower leaching yield; Bigger equipment volume and long operating time; Lower output efficiency and more leaching agent consumption etc.But in order to accelerate leaching velocity, except that the dump leaching, real leaching process at normal temperatures and pressures is seldom.For example, United States Patent (USP) (US2008050294) soaks nickel in the lower nickel sulfide concentrate of nickel grade, with the sulfuric acid of 202～223g/l, leaches 3 hours leaching yield about 72% down at 80 ℃; And for example, Chinese invention patent (200710065624.1) soaks nickel with sulfuric acid from nickel sulfide concentrate, and vitriolic concentration is 100～120g/l, and temperature is 50～80 ℃, and extraction time is 1.5～2.0 hours, and leaching yield is 75～91%.
For overcoming the shortcoming that normal temperature and pressure leaches, discover that the reason that influences the nickel sulfide concentrate leaching velocity mainly contains two: the one, because there are the complicacy of form in nickelous sulfide and associated element thereof; The 2nd, because the reductive elementary sulfur causes its diffusion difficulty, sluggish in the absorption of nickel ore concentrate microparticle surfaces.For solving preceding problem, investigators have used various oxygenants, as pure oxygen, and ozone, chlorine, hydrogen peroxide, ferric ion wait the effective concentration that increases nickel ion, improve leaching velocity; For overcoming back one difficulty, except that adding strong mixing, what have has also improved temperature of reaction, reduces the speed of adsorbing, the thickness of minimizing adsorption layer with the turbulent flow of solution under churned mechanically fluctuation and the high temperature.But the former problem is that the gas oxygenant all is difficult for preserving, and the price that has is higher, and what have is dangerous to operator; And the latter is that mechanical stirring has individual limit: when rotating speed reaches certain limit, increase mixing speed in any case, and all like water off a duck's back to the attenuate of adsorption layer.And high-temperature operation can not be eliminated adsorption layer fully, and the problem of highly energy-consuming is arranged.
Summary of the invention
The present invention is in order to overcome the deficiency that above-mentioned prior art exists, seeks a kind of in the nickel sulfide concentrate novel method of extraction nickel.This method is the major advantage of above-mentioned two class methods of compatibility substantially: economize energy, consumption reduction and do not need special high pressure equipment thereby promptly can leach at normal temperatures and pressures substantially, have leaching velocity quickly simultaneously.
Technical scheme of the present invention: under the ultrasonic wave effect, the sulphur adsorption layer on nickel shot surface obtains removing to a certain degree, and the nickel shot surface exposure is come out.The cavitation effect of ultrasonic waves attenuate liquid-solid frictional belt, strengthened mass transfer, also reduced the resistance film that elementary sulfur absorption and reaction product cause when leaching, quickened to react and carried out.With the aqueous solution of a small amount of sulfuric acid and SODIUMNITRATE, nickel sulfide concentrate is leached in the oxidation acidolysis.This method has atmospheric operation, and speed of response is fast, the leaching yield height, and oxygenant is solid nitric acid salt, comparatively safe characteristics.
The present invention carries out according to the following steps: the granularity that guarantees the nickel ore concentrate fine ore is that 0.15～0.08mm accounts for more than 90%; Nickel minerals powder and water are mixed into ore pulp place in the stainless steel reactor, wherein water and nickel minerals weight ratio are 5～30: 1; Add oxygenant, wherein said oxygenant can be SODIUMNITRATE, saltpetre, pure oxygen, hydrogen peroxide or ozone, preferably adds solid oxidizing agent SODIUMNITRATE or saltpetre, and wherein solid oxidizing agent and nickel minerals weight ratio are 0.5～1.0: 1; Add 98% vitriol oil again, wherein the vitriol oil and nickel minerals weight ratio are 0.5～1.1: 1, and (frequency 20.02kHz, power are under 50～150W) effects, leach 40～60min under the normal temperature and pressure altogether at ultrasonic wave stainless steel probe at last.
The main chemical reactions equation that the present invention may relate to is as follows:
Ni
3S
2+2NO
3 -+8H
+→3Ni
2++2S+2NO+4H
2O
Or Ni
3S
2+ 2NO
3 -+ 8H
+→ 3Ni
2++ 2S+NO
2+ 4H
2O
The technico-economical comparison that the present invention reaches: nickel leaching yield 95%～99%.
Soak the nickel technology with existing other and compare the advantage that has:
1. use solid nitric acid sodium or saltpetre as oxygenant.Avoided gaseous oxidant to be difficult for the hidden danger of preservation and secure context;
2. use the leaching process of intensified by ultrasonic wave nickel sulfide concentrate, not only on molecular level, improved the mass transfer velocity of reactant and resultant, and reduced the activation energy of reaction, ultrasonic wave acts on the heat energy of leaching process degeneration and has also strengthened reaction process to a certain extent, and energy is fully used;
3. speed of reaction is fast, the leaching yield height.Reach 97%～99% leaching yield and only use 40～60min, avoided lower leaching yield under extraction time long in the general similar leaching and the most of situation;
4. low to the nickel ore concentrate granularity requirements.The nickel ore concentrate granularity is 0.15～0.08mm more than 90%, and this just in time is equivalent to commercially available industrial fine ore 100 orders～200 orders, can be connected with existing processes.Avoided the higher shortcoming of nickel minerals fine grinding degree requirement in the similar leaching; Leaching process is a normal pressure, does not have extra heat supply.Avoided in a lot of similar leachings up to the extraction temperature of hundreds of degree and some leaching process up to 1.3 * 10
6The pressure of handkerchief.
Embodiment
Further describe the present invention's (used nickel sulfide concentrate is all from the fine ore of Jinchuan Nickel company in the example) below in conjunction with embodiment:
Embodiment 1
Nickel sulfide concentrate is formed (%)
| Ni | Cu | Mg | Fe | S |
| 9.35 | 4.25 | 3.01 | 27.09 | 25.41 |
Nickel sulfide concentrate is levigate to the 0.15mm, accurately taking by weighing 2g becomes ore pulp in the 100ml stainless steel reactor with the water stirring and evenly mixing, water and nickel sulfide concentrate weight ratio are 30: 1, add the solid oxidizing agent SODIUMNITRATE, SODIUMNITRATE and nickel sulfide concentrate weight ratio are 0.825: 1, after stirring 10min, add 98% vitriol oil again, the vitriol oil and nickel sulfide concentrate weight ratio are 1.1: 1, simultaneously under the ultrasonic wave effect, normal pressure leaches 40min altogether, need not heat specially fully (but the degeneration heat of ultrasonic wave and solution molecule effect can make temperature raise to some extent, down together), ultrasonic frequency 20.02kHz, power is 90W, and the nickel leaching yield is 98.22%.
Embodiment 2
Nickel sulfide concentrate is formed with embodiment 1,
Nickel sulfide concentrate is levigate to the 0.08mm, accurately taking by weighing 10g becomes ore pulp in the 500ml stainless steel reactor with the water stirring and evenly mixing, water and nickel minerals weight ratio are 20: 1, add the solid oxidizing agent SODIUMNITRATE, SODIUMNITRATE and nickel sulfide concentrate weight ratio are 1: 1, after stirring 10min, add 98% vitriol oil again, the vitriol oil and nickel sulfide concentrate weight ratio are 1.33: 1, and under the ultrasonic wave effect, normal pressure leaches 50min altogether at last, need not heat specially fully, ultrasonic frequency 20.02kHz, power are 120W, and the nickel leaching yield is 98.31%.
Embodiment 3
Nickel sulfide concentrate is formed with embodiment 1,
Nickel sulfide concentrate is levigate to the 0.1mm, accurately taking by weighing 10g becomes ore pulp in the 500ml stainless steel reactor with the water stirring and evenly mixing, water and nickel sulfide concentrate weight ratio are 20: 1, add solid oxidizing agent saltpetre, saltpetre and nickel sulfide concentrate weight ratio are 0.8: 1, after stirring 10min, add 98% vitriol oil again, sulfuric acid and nickel sulfide concentrate weight ratio are 1.4: 1, and under the ultrasonic wave effect, normal pressure leaches 50min altogether simultaneously, need not heat specially fully, ultrasonic frequency 20.02kHz, power are 120W, and the nickel leaching yield is 97.79%.
Claims (1)
1. the method for rapidly and directly dipping of nickel sulfide concentrate under action of ultrasonic wave is characterized in that carrying out according to following step: nickel minerals is pulverized, and making its ore particle degree is that 0.15～0.08mm accounts for more than 90%; Nickel minerals and water are mixed into ore pulp to be placed in the stainless steel reactor; Add oxygenant; Add 98% vitriol oil again, wherein the vitriol oil and nickel minerals weight ratio are 0.5～1.1: 1, and under the ultrasonic wave effect, normal temperature and pressure is leaching 40～60min down at last; Wherein said water and nickel minerals weight ratio are 5～30: 1; Wherein said ultrasonic frequency 20.02kHz, power are 50～150W; Wherein said oxygenant is SODIUMNITRATE, saltpetre, pure oxygen, hydrogen peroxide or ozone; Wherein solid oxidizing agent and nickel minerals weight ratio are 0.5～1.0: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101842839A CN101717857B (en) | 2009-08-18 | 2009-08-18 | Method for rapidly and directly dipping nickel sulfide concentrate under action of ultrasonic wave |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101842839A CN101717857B (en) | 2009-08-18 | 2009-08-18 | Method for rapidly and directly dipping nickel sulfide concentrate under action of ultrasonic wave |
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| Publication Number | Publication Date |
|---|---|
| CN101717857A CN101717857A (en) | 2010-06-02 |
| CN101717857B true CN101717857B (en) | 2011-07-06 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899568B (en) * | 2010-07-23 | 2012-06-20 | 陕西华泽镍钴金属有限公司 | Method for producing electrolytic nickel by leaching chemically precipitated nickel sulfide with pure oxygen |
| JP5445777B2 (en) * | 2010-07-28 | 2014-03-19 | 住友金属鉱山株式会社 | Method for producing ferronickel smelting raw material from low-grade nickel oxide ore |
| CN102732719B (en) * | 2012-07-10 | 2013-10-16 | 金堆城钼业股份有限公司 | Method for purifying molybdenum disulfide by ultrasonic-assisted acid leaching of molybdenite |
| KR20150051691A (en) * | 2013-11-05 | 2015-05-13 | 한국지질자원연구원 | Leaching method of molybdenum from sulfide mineral contained molybdenum and copper using electrolytic oxidation |
| CN106947877B (en) * | 2016-12-27 | 2018-09-28 | 核工业北京化工冶金研究院 | A method of improving ground-dipping uranium extraction leaching rate using ultrasonic wave |
| CN107043853A (en) * | 2016-12-30 | 2017-08-15 | 四川师范大学 | The dezincification method of copper solution |
| CN113584314B (en) * | 2021-07-29 | 2023-03-14 | 湖南中伟新能源科技有限公司 | High nickel matte normal pressure leaching method and nickel sulfate |
| RU2768928C1 (en) * | 2021-08-03 | 2022-03-25 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | Method for dissolving metal sulfides using ozone and hydrogen peroxide |
| CN114934193A (en) * | 2022-05-24 | 2022-08-23 | 浙江伽能环境工程有限责任公司 | Method for enhancing normal-pressure acid leaching efficiency of nickel anode mud desulfurization slag |
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Granted publication date: 20110706 Termination date: 20120818 |