CN103789561B - Weathering crust deposit type rare earth ore compound leaching agent - Google Patents
Weathering crust deposit type rare earth ore compound leaching agent Download PDFInfo
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- CN103789561B CN103789561B CN201410064086.4A CN201410064086A CN103789561B CN 103789561 B CN103789561 B CN 103789561B CN 201410064086 A CN201410064086 A CN 201410064086A CN 103789561 B CN103789561 B CN 103789561B
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- leaching agent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention belongs to the field of wet metallurgy and in particular discloses a compound leaching agent for preventing landslide in the process of leaching weathering crust deposit type rare earth ore in situ. The compound leaching agent consists of a mixed aqueous solution of an organic amine salt anti-swelling agent, a leaching agent and a pH regulator, wherein the concentration of the organic amine salt anti-swelling agent is 1-15g/L; the concentration of the leaching agent is 5-30g/L; the pH value of the mixed aqueous solution is regulated to be 4.0-6.0 by using the pH regulator. The compound leaching agent is preferably any one of dimethylamine hydrochloride, di-n-propylamine hydrochloride, diethylamine hydrochloride and triethylamine hydrochloride. Due to the addition of the anti-swelling agent, the compound leaching agent has the capacity of well preventing swelling of clay minerals, the rare earth leaching effect is not influenced, the leaching agent has the functions of leaching and preventing swelling, and landslide is effectively avoided in the process of leaching the weathering crust deposit type rare earth ore in situ.
Description
Technical field
The invention belongs to field of hydrometallurgy, when being specifically related to a kind of weathered superficial leaching rare-earth ore in-situ leaching, prevent the compound leaching agent of landslide.
Background technology
Weathered superficial leaching rare-earth ore (also known as ion adsorption type rare earth ore) is the distinctive rare-earth mineral of China, extensively be distributed in the areas such as the Jiangxi of south China, Fujian, Guangdong, Hunan, Guangxi, its ree distribution pattern is rich in middle heavy rare earth element, be the main source of heavy rare earths in China, there is huge commercial value.Weathered superficial leaching rare-earth ore is clay class mineral, primarily of compositions such as kaolinite, halloysite, montmorillonites, clay ore deposit is the load phase of rare earth, wherein the rare earth of about 85% is with hydration or hydroxyl hydration ionic adsorption on clay mineral, constitutes the uneven and baroque ion-exchange " resin " of a size.Thus conventional physical concentration method is adopted to make rare-earth enrichment, general employing Chemical Leaching technology recovering rare earth from the type rare-earth mineral.
The clay mineral of absorption rare earth ion can regard stationary phase as, and the solution containing leaching agent is moving phase, and the rare earth ion on clay mineral runs into the more active positively charged ion (as: Na of chemical property
+, K
+, H
+, NH
4 +deng) desorb can be exchanged by it, the leaching agent positively charged ion in solution is adsorbed up, and rare earth ion is desorbed.Reversible reaction during this ion exchange reaction is also inhomogeneous reaction, and the theoretical basis of weathered superficial leaching rare-earth ore extract technology has been established in this reaction.With NH
4 +for example, ion exchange reaction occurs in its chemical equation between clay mineral surface and solution and can be expressed as:
In formula, s represents solid phase; Aq represents aqueous phase.
Weathered leaching REO deposit adopts in-situ lixiviation processing recovering rare earth usually.In-situ lixiviation processing is that leaching agent solution is injected stope ore body incessantly from fluid injection shallow well, positively charged ion in ionogen and the rare earth ion in ore are exchanged, thus make rare earth ion enter generation leaching rare earth mother solution in leach liquor, mother liquor is after from intercepting gutter, side is oozed out, be collected to collecting tank, the mother liquor collected in pond precipitates the novel mining methods of one of recovering rare earth again after removal of impurities with oxalic acid or volatile salt.In-situ leaching mining does not destroy landform, landforms because of it, do not peel off vegetation, table soil, arrange outward without mine tailing, reduce labour intensity, little to environmental influence, can the ore that cannot exploit of the conventional reoovery method of back production, make full use of resource, save initial cost, reduce production cost, the advantages such as social benefit is obvious, are widely applied.But usually because fluid injection is improper in in-situ leaching process, landslide phenomenon is caused to occur, its major cause is that the clay mineral water suction in weathered superficial leaching rare-earth ore expands, when the component of massif gravity slide downward is greater than the friction resistance sum that the structural capacity of ore and ore slide, easy generation landslide, not only destroys farmland, contaminate environment, also have lost rare earth leaching amount and leaching agent, cause in-situ leaching technico-economical comparison to decline.
Clay mineral water-swellable in weathered superficial leaching rare-earth ore successively experience surface hydration expands and infiltration hydration swelling two processes.It is because the siloxane bond on clay crystal face top layer and hydrogen-oxygen key all have polarity that surface hydration expands, and they can the water molecules of adsorb polar, the multiple-level surface water of formation; Surface of clay aquation makes distance between crystal layer more than after 10A, surface hydration can weaken greatly to the effect of aquation, surface hydration terminates, infiltration aquation expands the beginning, and namely between clay crystal layer, cation concn is greater than the cation concn in environment, produces osmotic pressure effect, water molecules is caused to enter, thus formation diffusion double layer, under double electrode layer repulsion effect, support Large space makes more water enter between crystal layer.Therefore, prevent weathered superficial leaching rare-earth ore from when in-situ leaching, landslide occurring, just should select to add suitable leaching agent, this leaching agent can keep high rare earth leaching yield on the one hand, need prevent clay ore deposit from expanding on the other hand, thus reach the object preventing landslide.
The people such as Cui Guiling take polyacrylamide as hyle, by methylolation and hydroxyl cationization synthesis polyhydroxy cation polymkeric substance, it can be combined well with clay surface, and effectively in and the electronegativity on clay surface, thus preventive effect of expansion is better, but can not be used as rare earth leaching agent.The people such as Tong Wei close, have synthesized quaternary ammonium salt cationic surfactant (4C
12aC), the electrostatic attraction between the tensio-active agent of positively charged and electronegative clay makes tensio-active agent easily be adsorbed by clay ore deposit, reaches good anti-swollen performance.But because quaternary ammonium salt cationic surfactant tends to reduce clay ore deposit to the absorption of water, the wetting ability of clay mineral can be changed, hinder the leaching process of rare earth.Opening to attain to please waits people to have rated the hydration swelling feature of clay mineral under different Fluid Contacting condition, finds NH
4cl and (NH
4)
2sO
4, NH
4nO
3anti-swollen ability after composite is better than single conventional rare leaching agent.
Summary of the invention
The object of the invention is to provide a kind of compound leaching agent for weathered superficial leaching rare-earth ore, wherein add the existing ability preventing more by force clay mineral from expanding of expansion-resisting agent, do not affect rare earth leaching effect again, have leaching and anti-swollen function concurrently, landslide when effectively preventing weathered superficial leaching rare-earth ore in-situ leaching.
For achieving the above object, the technical scheme of employing is as follows:
A kind of weathered superficial leaching rare-earth ore compound leaching agent, it consists of the mixed aqueous solution of organic amine salt expansion-resisting agent, leaching agent and pH adjusting agent; Organic amine salt expansion-resisting agent concentration is 1-15g/L, and leaching agent concentration is 5-30g/L, and pH adjusting agent regulates mixed aqueous solution pH value between 4.0-6.0;
Described organic amine salt expansion-resisting agent general formula is: R
1r
2r
3n
+r
4b
-;
Wherein, R
1, R
2, R
3, R
4for-C
nh
2n+1, n=0,1,2,3 or 4;
B
-for-OH, Cl
-, Br
-, I
-, NO
3 -, SO
4 2-, CH
3cOO
-any one.
By such scheme, described organic ammonium salt expansion-resisting agent be preferably in dimethylamine hydrochloride, di-n-propylamine hydrochloride, diethylamine vitriol, triethylamine hydrochloride any one.
By such scheme, described leaching agent is the mixture of any one or they in ammonium chloride and ammonium sulfate.
By such scheme, described pH adjusting agent is hydrochloric acid or sulfuric acid.
In in-situ leaching process, in leaching agent, add organic amine salt expansion-resisting agent, on the one hand expansion-resisting agent can with NH in leaching agent
4 +form good compatibility, do not affect the leaching of rare earth ion; On the other hand, positively charged ion amine salt can be ionized out, to embed in the hexagonal loop of clay aspect and water molecules is wherein squeezed out, and due to polarized action, presenting positive polarity, comparing NH
4 +there is more lasting clay stabilization.
Organic amine salt expansion-resisting agent can ionize out positively charged ion amine salt in water, and chemical equation can be expressed as:
The R ionized out
1r
2r
3r
4n
+can to embed in the hexagonal loop of clay aspect and water molecules is wherein squeezed out, the water molecules of Coating combination is reduced, the polarized action of organic amine salt ion simultaneously, present positive polarity, make it more easily to be adsorbed on electronegative clay mineral surface, and its size is less, interlayer can provide enough spaces to make organic chain lie low in interlayer, form relatively more unified orderly arrangement at interlayer, reduce clay mineral interlamellar spacing.
Beneficial effect of the present invention is:
1) in the present invention, compound leaching agent possesses the stronger ability preventing clay mineral hydration swelling, and not by temperature, local water mineralization degree affects, and effectively can prevent the landslide caused because of the expansion of clay mineral during weathered superficial leaching rare-earth ore in-situ leaching;
2) selected expansion-resisting agent and weathered superficial leaching rare-earth ore leaching agent have good coordinative role, use at low concentrations and not only have good preventive effect of expansion, and can also improve the leaching of rare earth;
3) needed for this compound leaching agent, reagent is easy to get, with low cost.
Embodiment
Following embodiment explains technical scheme of the present invention further, not as limiting the scope of the invention.
Embodiment 1
The weathered superficial leaching rare-earth ore 250.0g taking oven dry loads in glass column, by following component preparation compound leaching agent (mass concentration): di-n-propylamine hydrochloride 4g/L, ammonium chloride 6g/L, and with 2.0mol/L hydrochloric acid conditioning solution pH4.5, this compound leaching agent is adopted to add in post in the ratio of solid-to-liquid ratio 1:2 (g:mL), regulate flow rate control at 0.52mL/min, post leaching is carried out to weathered superficial leaching rare-earth ore, content of rare earth in leach liquor makes indicator with xylenol orange under the condition of pH=5.5, detect by EDTA volumetry, calculating rare earth leaching yield is 93.66%,
Measure clay mineral linear expansivity:
Take the weathered superficial leaching rare-earth ore 2.0g after vacuum-drying, maintenance pressure is 8.0MPa, compressing tablet 5.0min on tabletting machine, use vernier caliper measurement sample length, and sample is arranged on intelligent clay swelling instrument, above-mentioned compound leaching agent is injected measuring cylinder, and under 30 DEG C of normal pressures, measure the linear expansivity in this ore deposit after 8.0 hours, its result is 1.134%.
Comparative example 1:
Implementation method is with embodiment 1, and preparation ammonium chloride mass concentration is the leaching agent of 6g/L, and hydrochloric acid conditioning solution pH4.5, adopts this composite solution to carry out post leaching to weathered superficial leaching rare-earth ore, and detect leach liquor content of rare earth, rare earth leaching yield is 85.06%; Linear expansivity is 1.934%.Leaching effect is pretty good, but preventive effect of expansion is undesirable.
Comparative example 2
Implementation method is with embodiment 1, by following component preparation compound leaching agent (mass concentration): polyhydroxy cation polymkeric substance 4g/L, ammonium chloride 6g/L, hydrochloric acid conditioning solution pH4.5, this composite solution is adopted to carry out post leaching to weathered superficial leaching rare-earth ore, detect leach liquor content of rare earth, rare earth leaching yield is 24.45%; Linear expansivity is 1.441%.Although there is good preventive effect of expansion, the expansion-resisting agent added have impact on the leaching of rare earth greatly.
Comparative example 3
Implementation method, with embodiment 1, prepares compound leaching agent (mass concentration) by following component: quaternary ammonium salt cationic surfactant (4C
12aC) 4g/L, ammonium chloride 6g/L, hydrochloric acid conditioning solution pH4.5, adopts this composite solution to carry out post leaching to weathered superficial leaching rare-earth ore, and detect leach liquor content of rare earth, rare earth leaching yield is 20.35%; Linear expansivity is 1.369%.Although there is good preventive effect of expansion, the expansion-resisting agent added have impact on the leaching of rare earth greatly.
Known by the comparative analysis of embodiment 1 and comparative example thereof, be surprised to find that expansion-resisting agent in the present invention in compound leaching agent and leaching agent achieve synergistic effect, there is better leaching effect and preventive effect of expansion.
Embodiment 2
Implementation method is with embodiment 1, by following component preparation compound leaching agent: 1g/L di-n-propylamine hydrochloride, 5g/L ammonium chloride, hydrochloric acid conditioning solution pH4.0, this compound leaching liquid is adopted to carry out post leaching to weathered superficial leaching rare-earth ore, detect leach liquor content of rare earth, rare earth leaching yield is 68.76%, and rate of expansion is 1.879%.
Di-n-propylamine hydrochloride adds as expansion-resisting agent, and leaching agent achieves synergistic effect, has good leaching effect and preventive effect of expansion.
Embodiment 3
Implementation method is with embodiment 1, by following component preparation compound leaching agent: 15g/L di-n-propylamine hydrochloride, 30g/L ammonium chloride, hydrochloric acid conditioning solution pH6.0, this compound leaching liquid is adopted to carry out post leaching to weathered superficial leaching rare-earth ore, detect leach liquor content of rare earth, rare earth leaching yield is 95.41%, and rate of expansion is 2.010%.
Di-n-propylamine hydrochloride adds as expansion-resisting agent, and leaching agent achieves synergistic effect, has good leaching effect and preventive effect of expansion.
Embodiment 4
Implementation method is with embodiment 1, by following component preparation compound leaching agent: dimethylamine hydrochloride 4g/L, ammonium chloride 6g/L, hydrochloric acid conditioning solution pH4.5, this composite solution is adopted to carry out post leaching to weathered superficial leaching rare-earth ore, detect leach liquor content of rare earth, calculate rare earth leaching yield, rare earth leaching yield is 97.46%, and rate of expansion is 1.590%.
Dimethylamine hydrochloride adds as expansion-resisting agent, and leaching agent achieves synergistic effect, has good leaching effect and preventive effect of expansion.
Embodiment 5
Implementation method is with embodiment 1, by following component preparation compound leaching agent: the mixture 6g/L of the mass ratio 1:1 of diethylamine vitriol 4g/L, ammonium chloride and ammonium sulfate, hydrochloric acid conditioning solution pH4.5, this composite solution is adopted to carry out post leaching to weathered superficial leaching rare-earth ore, detect leach liquor content of rare earth, calculating rare earth leaching yield is 91.35%, and rate of expansion is 1.235%.
Diethylamine vitriol adds as expansion-resisting agent, and leaching agent achieves synergistic effect, has good leaching effect and preventive effect of expansion.
Embodiment 6
Implementation method is with comparative example 1, by following component preparation compound leaching agent: triethylamine hydrochloride 4g/L, ammonium sulfate 6g/L, sulfuric acid regulation solution pH4.5, this composite solution is adopted to carry out post leaching to weathered superficial leaching rare-earth ore, detect leach liquor content of rare earth, rare earth leaching yield is 88.65%, and rate of expansion is 1.390%.
Triethylamine hydrochloride adds as expansion-resisting agent, and leaching agent achieves synergistic effect, has good leaching effect and preventive effect of expansion.
Claims (3)
1. a weathered superficial leaching rare-earth ore compound leaching agent, is characterized in that the mixed aqueous solution consisting of organic amine salt expansion-resisting agent, leaching agent and pH adjusting agent; Organic amine salt expansion-resisting agent concentration is 1-15g/L, and leaching agent concentration is 5-30g/L, and pH adjusting agent regulates mixed aqueous solution pH value between 4.0-6.0;
Described organic amine salt expansion-resisting agent is any one in dimethylamine hydrochloride, di-n-propylamine hydrochloride, diethylamine vitriol, triethylamine hydrochloride.
2. weathered superficial leaching rare-earth ore compound leaching agent as claimed in claim 1, is characterized in that described leaching agent is the mixture of any one or they in ammonium chloride and ammonium sulfate.
3. weathered superficial leaching rare-earth ore compound leaching agent as claimed in claim 1, is characterized in that described pH adjusting agent is hydrochloric acid or sulfuric acid.
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| CN103789561B true CN103789561B (en) | 2015-06-24 |
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Families Citing this family (11)
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| CN104498738B (en) * | 2014-11-28 | 2017-05-03 | 武汉工程大学 | Method for leaching rare earth from weathering crust leaching type rare-earth ore heap |
| CN105331835B (en) * | 2015-10-11 | 2017-07-28 | 江西理工大学 | A kind of leaching agent and its leaching ore deposit method that ore deposit process is soaked applied to ion type rareearth ore |
| CN105112692B (en) * | 2015-10-11 | 2017-09-15 | 江西理工大学 | A kind of leaching ore deposit method of ion adsorption type rare earth ore |
| CN106498188B (en) * | 2016-10-14 | 2019-01-01 | 赣州弘茂稀土工程有限公司 | The rare earth original place of ion type rareearth ore controls extract technology |
| WO2018162951A1 (en) * | 2017-03-07 | 2018-09-13 | Ree Uno Spa | System and method for processing of minerals containing the lanthanide series and production of rare earth oxides |
| CN107217141B (en) * | 2017-05-24 | 2018-09-28 | 江西理工大学 | In-situ ionic rare earth leaching mine adsorbs the computational methods of ammonium ion critical concentration again |
| CN107190144B (en) * | 2017-05-24 | 2018-09-04 | 江西理工大学 | In-situ ionic rare earth soaks the computational methods of mine ammonium sulfate dosage |
| CN108823436A (en) * | 2018-07-05 | 2018-11-16 | 武汉工程大学 | A kind of compound leaching agent of the formates of weathered superficial leaching rare-earth ore |
| CN109082543B (en) * | 2018-09-17 | 2020-12-22 | 中南民族大学 | Composite leaching agent for enhanced leaching of weathering crust leaching type rare earth ore |
| CN109735708B (en) * | 2019-03-21 | 2019-10-08 | 江西理工大学 | A kind of weathered superficial leaching rare-earth ore leaching agent and leaching method |
| US11512005B2 (en) * | 2019-09-05 | 2022-11-29 | Ree Uno Spa | System and method for processing of minerals containing the lanthanide series and production of rare earth oxides |
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