CN102268545B - Intensified leaching method and device - Google Patents

Intensified leaching method and device Download PDF

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Publication number
CN102268545B
CN102268545B CN201110202765XA CN201110202765A CN102268545B CN 102268545 B CN102268545 B CN 102268545B CN 201110202765X A CN201110202765X A CN 201110202765XA CN 201110202765 A CN201110202765 A CN 201110202765A CN 102268545 B CN102268545 B CN 102268545B
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disk
leaching
stirring
sediment
transferpump
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CN102268545A (en
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伍耀明
黄强
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GUANGXI RESEARCH INSTITUTE OF METALLURGY
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GUANGXI RESEARCH INSTITUTE OF METALLURGY
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Abstract

The invention relates to an intensified leaching method and device. The method comprises the following steps of: carrying out intensified leaching on indissolvable materials containing high silicon and high ferrum by adopting sulphuric acid which has high acid content as much as 2-10 times of a theoretical amount and a high concentration of 750-1000 gram per liter, at a high temperature of 150-170 DEG C; then placing leached ore slurry under stirring into a sedimentation separating device, placing a crystallization mother solution into a heat-insulating intermediate tank, returning for cycle use, leaving crystallization substances and sediments in the sedimentation separating device, then adding water and stirring and dissolving the crystallization substances and filtering so as to obtain filtration residues and filtrate; and respectively carrying out neutralization de-ironing or non-ferrous metal neutralization precipitating on the filtrate in different sedimentation separating devices with the same structure by taking the processed minerals as a neutralization precipitation agent to obtain ferrum or nonferrous metal hydroxide products, and retuning sediments of undissolved substances to intensified leaching. According to the invention, the minerals are finally subjected to the intensified leaching and full recovery of resources is realized.

Description

A kind of method and device of strengthening leaching
One, technical field
The present invention relates to a kind of non-ferrous metal technical field of wet metallurgy, particularly a kind of method and device of strengthening leaching.
Two, background technology
In non-ferrous metal metallurgy, run into through regular meeting and to be difficult to sour dissolved material, especially high silicon materials, not only hard to tolerate, but also sad filter.The treating method that tackles the indissoluble material adopts high pressure to leach often.Yet the autoclave ME is complicated, and cost is high, and support equipment is many, and complex operation has brought inconvenience to the user, and autoclave is handled when containing the magnesium material and scabbed seriously in addition, and range of application is restricted.
Three, summary of the invention
The purpose of this invention is to provide a kind of method and device of strengthening leaching, this method and device can effectively be handled the material hard to manage of high silicon high iron and other non-ferrous metal elements.
The method that said reinforcement is leached is with excessive high-concentration sulfuric acid, at high temperature material hard to manage is leached, and makes by molten first procatarxis common-ion effcet and crystallization is separated out.
Said device is a settling separation device.Be to obtain settlement separate to strengthening the crystalline mother solution, crystallisate, the leached mud that leach generation.The hydroxide product that produces when also the breeze that adopts the ore deposit of handling being done the neutralization precipitation agent, give over to the mixture of crystal seed, molten breeze sediment obtains settlement separate.
Content of the present invention achieves the above object through following technical scheme: a kind of method and device of strengthening leaching comprises the steps:
(1) adopt 2～10 times the indissoluble material that contains high silicon high iron to be strengthened leaching, obtain leaching ore pulp to the big acid amount sulfuric acid of theoretical amount, the high density of 750～1000g/L, 150～170 ℃ high-temperature,
(2) said leaching ore pulp is under agitation put into settling separation device, the crystalline mother solution that obtains after the sedimentation is put into the insulation storage tank, returns to recycle; Crystallisate and sediment are stayed in the settling separation device, add water stirring and dissolving crystallisate then, filter; Obtain filter residue and filtrating
(3) said filtrating is done the neutralization precipitation agent with the processing mineral, respectively in the different settling separation devices of same structure carry out with deironing or neutralization precipitation non-ferrous metal, obtain iron or non-ferrous metal hydroxide product, dissolve the thing sediment and turn back to strengthen and leach.
Said indissoluble material is meant silicate, wustite with common sulfuric acid indissoluble, contains 10～30% the difficult filtering material of high silicon.
A kind of device that is suitable for the method for said reinforcement leaching; Assembly said settling separation device by stirring rake, sensitometer, big cone, upper strata stirring rake, large cylinder, U trap, phonomoter, light source, valve and stir shaft on sediment transferpump, product transferpump, little conic tube, disk lower stirring paddle, stirring disk, the disk; Said sediment transferpump is connected with the conelet cylindrical shell; The product transferpump is connected with large cylinder, stirring rake on the disk, disk lower stirring paddle and stir disk and all be welded on the stir shaft, and stirring rake and disk lower stirring paddle are welded on the upper surface and the lower surface of stirring disk respectively on the disk; Sensitometer is installed on the wire between big cone base and the conelet cylindrical shell upper edge; Light source is installed on the wire between big cone base and the conelet cylindrical shell upper edge, and light source is corresponding with sensitometer, and big cone upper end is connected with large cylinder; The lower end is connected with the conelet cylindrical shell; The upper strata stirring rake is positioned at the top of the wire of big cone and large cylinder, and U trap is connected on the valve of inlet pipe of product transferpump, and phonomoter is connected with stir shaft.
Outstanding advantage of the present invention is:
1, compares with the high pressure leaching; Adopt to strengthen leach can handle silicate, wustite and formed the glass slag water granulated slag the general sulfuric acid dissolution of solution not material hard to tolerate; Especially be prone to form the difficult filtering high silicon materials of silica gel; Filtration is become be easy to, help the comprehensive reutilization of resource.
2, leach relatively with vitriol oil slaking, the present invention strengthens leaching with the sulfuric acid of 2～10 times of theoretical amount to material, and leaching velocity is fast; The time brief; The dissolved substance crystallization is separated out, and obtains sulfuric acid concentration height, crystalline mother solution that metal ion content is low, and crystalline mother solution can return circulation continuously and leach.
Four, description of drawings
Fig. 1 is the structural representation of the settling separation device of the method that is suitable for strengthening leaching of the present invention.
Embodiment
Below through accompanying drawing and embodiment technical scheme of the present invention is further described.
A kind of method and device of strengthening leaching comprises the steps:
(1) adopt 2～10 times the indissoluble material that contains high silicon high iron to be strengthened leaching, obtain leaching ore pulp to the big acid amount sulfuric acid of theoretical amount, the high density of 750～1000g/L, 150～170 ℃ high-temperature,
(2) said leaching ore pulp is under agitation put into settling separation device, the crystalline mother solution that obtains after the sedimentation is put into the insulation storage tank, returns to recycle; Crystallisate and sediment are stayed in the settling separation device, add water stirring and dissolving crystallisate then, filter; Obtain filter residue and filtrating
(3) said filtrating is done the neutralization precipitation agent with the processing mineral, respectively in the different settling separation devices of same structure carry out with deironing or neutralization precipitation non-ferrous metal, obtain iron or non-ferrous metal hydroxide product, dissolve the thing sediment and turn back to strengthen and leach.
Map 1; A kind of settling separation device that is suitable for strengthening the method for leaching; Assembly said settling separation device by stirring rake 6, sensitometer 7, big cone 8, upper strata stirring rake 9, large cylinder 10, U trap 11, phonomoter 12, light source 13, valve 14 and stir shaft 15 on sediment transferpump 1, product transferpump 2, conelet cylindrical shell 3, disk lower stirring paddle 4, stirring disk 5, the disk; Said sediment transferpump 1 is connected with conelet cylindrical shell 3; Product transferpump 2 is connected with large cylinder 10, and stirring rake 6, disk lower stirring paddle 4 and stirring disk 5 all are welded on the stir shaft 15 on the disk, and stirring rake 6 is welded on upper surface and the lower surface that stirs disk 5 respectively with disk lower stirring paddle 4 on the disk; Sensitometer 7 is installed on the wire between big cone 8 bottoms and conelet cylindrical shell 3 upper edges; Light source 13 is installed on the wire between big cone 8 bottoms and conelet cylindrical shell 3 upper edges, and light source 13 is corresponding with sensitometer 7, and big cone 8 upper ends are connected with large cylinder 10; The lower end is connected with conelet cylindrical shell 3; Upper strata stirring rake 9 is positioned at the top of the wire of big cone 8 and large cylinder 10, and U trap 11 is connected on the valve 14 of inlet pipe of product transferpump 2, and phonomoter 12 is connected with stir shaft 15.
A kind of principle of work and process of settling separation device of the method that is suitable for strengthening leaching are:
When settling separation device separates the time spent as leaching settling ore pulp, the limit adds leaches the ore pulp limit and stirs, and after adding, promptly stops to stir, and sediment is deposited in the conelet cylindrical shell 3, and crystallisate is in big cone 8, and large cylinder 10 tops are high acidity crystalline mother solutions.
When settling separation device as in during with deironing or neutralization precipitation non-ferrous metal; Do in the neutralization precipitation agent and deironing or neutralization precipitation non-ferrous metal with the processing mineral; Do not dissolve mineral precipitation in conelet cylindrical shell 3; Iron or non-ferrous metal oxyhydroxide are in large cylinder 10, and the intermediates that are mingled with sediment and oxyhydroxide are stored in the big cone 8.
In when reclaiming non-ferrous metal with deironing or deposition; The iron or the oxyhydroxide of non-ferrous metal that at first pump in the large cylinder 10 with product transferpump 2 filter; Obtain the product filter cake; In little cylindrical shell 3, pump sediment with sediment transferpump 1 then, can make the intermediates that are mingled with sediment and oxyhydroxide big cone 8 in can from big cone 8 in the middle of short circuit directly not descend owing to stir the effect of disk 5 this moment; But evenly drop in the conelet cylindrical shell 3 temporary through the periphery that stirs disk 5; When the intermediates that are mingled with sediment and oxyhydroxide dropped between the wire of big cone 8 bottoms and conelet cylindrical shell 3, the light of light source 13 can shine on the sensitometer 7 on opposite, because the optoelectronic induction effect of sensitometer 7 and light source 13; Control sediment transferpump 1 stops immediately, can the intermediates that are mingled with sediment and oxyhydroxide in the big cone 8 be kept in the conelet cylindrical shell 3.
Embodiment 1
This embodiment adopts high acidity sulfuric acid to strengthen the instance that leaches cobalt nickel slag.
Get cobalt nickel slag 155 grams of moisture 25wt%, composition (wt%): Mn 0.42, and Fe 2.53, and Ni 7.21, and Co 5.40.Add water 275ml and size mixing, add the 275ml vitriol oil again, stir down at 160 ℃ and strengthen leaching after 30 minutes; Cool to 95 ℃, filter the drip washing of spraying at last at B; Then crystallisate and slag are added water stirring and dissolving crystallisate, cross to filter and leach dried slag 35 grams, slag contains Co 0.025wt%; Contain Ni 0.034wt%, the leaching yield of Co, Ni all is 99.86wt%.
Embodiment 2
This embodiment adopts the crystalline mother solution that returns to add the vitriol oil to strengthen the instance that leaches cobalt nickel slag.
Get cobalt nickel slag 247 grams of moisture 25wt%, material composition is got the crystalline mother solution 500ml of embodiment 1 with embodiment 1, adds 247 gram cobalt nickel slags stirrings and sizes mixing; Add the 300ml vitriol oil, stir to strengthen at 170 ℃ and leached 30 minutes, cool to 95 ℃, filter at B; The drip washing of spraying at last adds water stirring and dissolving crystallisate with crystallisate and slag then, crosses to filter leached mud 65 grams; Slag contains Co 0.007wt%, contains Ni 0.011wt%, and the leaching yield of Co, Ni all reaches 99.95wt%.The leaching mother liquor 780ml of this moment analyzes crystalline mother solution and contains (g/L): Co 0.96, and Ni 6.41, and Mn 3.24, H 2SO 4820.7.
Embodiment 3
This embodiment adopts high acidity crystalline mother solution to strengthen the instance of leaching roasting cobalt nickel slag.
Be taken at 800 ℃ of baked cobalt nickel slag 50 grams, composition (wt%): Mn 0.71, and Fe 2.49, and Co 5.18, and Ni 7.34.Get the crystalline mother solution 250ml of embodiment 2, add the 50ml vitriol oil, under 155 ℃, strengthen and leached 30 minutes; Cool to 95 ℃, filter the drip washing of spraying at last at B; Then crystallisate and slag are added water stirring and dissolving crystallisate, cross and filter leached mud 16 grams, the composition of leached mud (wt%): Ni 0.056; Co 0.034, SiO 252.50 CaO 6.26, cobalt leaching yield 99.79wt%, nickel leaching yield 99.76wt%; Get 300ml leaching concentrated mother liquor and contain (g/L): Fe 0.41, Mn 0.21, and Co 1.37, and Ni 8.31, H 2SO 4748.2.
Embodiment 4
This embodiment is the instance that the method that adopt to strengthen leaches leaches the residue behind the molybdenum nickel minerals volatile smelting.
The molybdenum nickel minerals contains SiO 2, Fe, CaO and Mo, Ni, the molybdenum nickel minerals residue behind 1150 ℃ of volatile smeltings contains Ni2.97wt%, gets the molybdenum nickel minerals residue behind the said volatile smelting of 30 grams; Add 200ml water and size mixing, add the 150ml vitriol oil again, strengthening leaching under 160 ℃ after 30 minutes; Cross to filter and do the quantity of slag 12 grams; Leached mud rate 40wt%, leached mud contains Ni 0.12wt%, then the leaching yield 98.38wt% of nickel.

Claims (2)

1. a method of strengthening leaching is characterized in that, this method comprises the following steps:
(1) adopt 2～10 times the indissoluble material that contains high silicon high iron to be strengthened leaching, obtain leaching ore pulp to the big acid amount sulfuric acid of theoretical amount, the high density of 750～1000g/L, 150～170 ℃ high-temperature,
(2) said leaching ore pulp is under agitation put into settling separation device, the crystalline mother solution that obtains after the sedimentation is put into the insulation storage tank, returns to recycle; Crystallisate and sediment are stayed in the settling separation device, add water stirring and dissolving crystallisate then, filter; Obtain filter residue and filtrating
(3) said filtrating is done the neutralization precipitation agent with the processing mineral, respectively in the different settling separation devices of same structure carry out with deironing or neutralization precipitation non-ferrous metal, obtain iron or non-ferrous metal hydroxide product, dissolve the thing sediment and turn back to strengthen and leach,
Said indissoluble material is meant silicate, wustite with common sulfuric acid indissoluble, contains 10～30% the difficult filtering material of high silicon.
2. device that is applicable to the method that the said reinforcement of claim 1 is leached; It is characterized in that; This device assemblies said settling separation device by stirring rake, sensitometer, big cone, upper strata stirring rake, large cylinder, U trap, phonomoter, light source, valve and stir shaft on sediment transferpump, product transferpump, little conic tube, disk lower stirring paddle, stirring disk, the disk, and said sediment transferpump is connected with the conelet cylindrical shell, and the product transferpump is connected with large cylinder; Stirring rake, disk lower stirring paddle and stirring disk all are welded on the stir shaft on the disk; And stirring rake and disk lower stirring paddle are welded on upper surface and the lower surface that stirs disk respectively on the disk, and sensitometer is installed on the wire between big cone base and the conelet cylindrical shell upper edge, and light source is installed on the wire between big cone base and the conelet cylindrical shell upper edge; Light source is corresponding with sensitometer; Big cone upper end is connected with large cylinder, and the lower end is connected with the conelet cylindrical shell, and the upper strata stirring rake is positioned at the top of the wire of big cone and large cylinder; U trap is connected on the valve of inlet pipe of product transferpump, and phonomoter is connected with stir shaft.
CN201110202765XA 2011-07-20 2011-07-20 Intensified leaching method and device Expired - Fee Related CN102268545B (en)

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CN104152684B (en) * 2014-08-29 2016-05-04 伍耀明 A kind of cylinder Horizontal normal pressure strengthening leaching tanks
CN112143900A (en) * 2020-10-10 2020-12-29 何耀 Red mud leaching slag washing tank and use method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101323908A (en) * 2008-07-31 2008-12-17 广西冶金研究院 Method for reclaiming cobalt from manganese cobalt slag
CN101583728A (en) * 2006-11-15 2009-11-18 开普敦大学 Sulfidisation process and apparatus for enhanced recovery of oxidised and surface oxidised base and precious metal minerals
CN101979679A (en) * 2010-10-19 2011-02-23 东北大学 Method for treating chromite by sulfuric acid leaching

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101583728A (en) * 2006-11-15 2009-11-18 开普敦大学 Sulfidisation process and apparatus for enhanced recovery of oxidised and surface oxidised base and precious metal minerals
CN101323908A (en) * 2008-07-31 2008-12-17 广西冶金研究院 Method for reclaiming cobalt from manganese cobalt slag
CN101979679A (en) * 2010-10-19 2011-02-23 东北大学 Method for treating chromite by sulfuric acid leaching

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