CN86106797A

CN86106797A - Pressure elution process of ion type RE crude ore and device

Info

Publication number: CN86106797A
Application number: CN198686106797A
Authority: CN
Inventors: 陈启仁; 邓星中; 李芝
Original assignee: GANZHOU NONFERROUS METALLURGICAL INSTITUTE
Current assignee: GANZHOU NONFERROUS METALLURGICAL INSTITUTE
Priority date: 1986-09-23
Filing date: 1986-09-23
Publication date: 1988-04-06

Abstract

The present invention is a kind of to ion type rareearth raw ore the pressurize technology and the device of elution.The thick rare-earth original ore bed of material in the elution groove, the NH under pressurized conditions in the scrub solution ₄ ⁺Or Na ⁺With the rare earth ion generation permutoid reaction that is adsorbed on the clay mineral such as kaolinite, reach and quicken the elution process purpose.The elution groove is made of withstand voltage cell body, cone seal lid and more than ten component such as removable bottom with holes.The present invention can make be shortened to about 4 hours by 24～72 hours of diafiltration elution elution period, and the rare earth yield can improve 10～25%.The present invention especially is adapted to the elution of the rare-earth original ore of filtration characteristic difference.

Description

The invention belongs to the hydrometallurgy field.

Before the present invention, from the ion adsorption type re raw ore, directly extract the technology of rare earth compound, be that rare-earth original ore is poured in the stripping cell, Xiang Chizhong adds the ammonium sulfate or the sodium-chlor scrub solution of proper concn, under the effect of scrub solution, be adsorbed in the rare earth ion on the clay minerals such as kaolinite, white mica, with the NH in the scrub solution ⁺ ₄Or Na ⁺Permutoid reaction takes place, and rare earth ion is sulfuric acid rare earth or rare earth chloride changes in the solution, and the natural filtration effect by ore bed can obtain rare earth mother solution, through operations such as oxalic acid precipitation, filtration, calcinations, can obtain the rare earth oxide product again.This explained hereafter cycle reaches 24 to 72 hours; The stripping cell area is big, and cloth is inhomogeneous, so that the scrub solution infiltrate bed of material, often the infiltrate bed of material on request; For devoting exclusive attention to output, the elution operation can not be carried out under optimized conditions, causes the rare earth yield must be low, to the raw ore of filtration characteristic difference more very; By artificial open work, labor condition is poor entirely for input and output material, and labour intensity is big; Stripping cell ties up to ground and constructs and form, and consumes steel, and the leak resistance in pond is relatively poor, and rare-earth mineral has been adopted nearby, and stripping cell is also promptly scrapped.The present invention is directed to the subject matter that above-mentioned technology exists,, improve the rare earth yield, reduce labor intensity, rare earth elution technology and device are studied, make rare earth elution technology that new breakthrough be arranged for shortening the production cycle.

Technology content of the present invention is: (1) at the good filter cloth in removable bottom (3) upper berth in elution troughed belt hole, and makes it in running order (seeing accompanying drawing one solid line part); (2), make the cone seal lid open (seeing accompanying drawing one dotted line position) by the handwheel (12) on rotation conic sealing cover (2) governor lever (16); (3) start feeding belt, cover (rotating speed: 10～15 rev/mins) for cone seal rare-earth original ore in rotation, rare-earth original ore is fed in the elution groove cell body (1) equably, make the rare-earth original ore bed of material in cell body, reach specified altitude (being complementary) by the period with rare earth elution device; (4) clean the cone seal lid.And make it to be in sealed state (seeing accompanying drawing one solid line position); (5) in cell body, inject specific concentrations scrub solution (as ammonium sulfate 2～3% or sodium-chlor 6～8%), its liquid: admittedly be 0.6～1: 1; (6) in cell body, send into pressurized air, make the intravital pressure of groove remain on 1～5 kilograms per centimeter ²At this moment, scrub solution passes the bed of material evenly, apace under pressure and gravity combined action, the rare earth ion generation permutoid reaction in ammonium ion wherein or sodium ion and the rare-earth original ore and enter solution.And be collected in the rare earth mother solution groove; (7) treat that the big portion of scrub solution passes a certain amount of top water that reinjects behind the bed of material, its liquid: admittedly be 0.1～0.2: 1, so that further reclaim rare earth and scrub solution remaining in the cell body; (8) after all passing the bed of material, then blocks in top water the source of the gas that enters cell body; (9) start the removable bottom lifting mechanism, make removable bottom progressively be opened to accompanying drawing one dotted line position, with the intravital rare earth tailings of removal slot.So far promptly finish the whole process of pressurization elution.The rare earth mother solution of elution can require to adopt different art breading according to difference.As wish to get mishmetal then with after the rare earth mother solution clarification, and under the condition of PH1.5～2, adding oxalic acid precipitation, the consumption of oxalic acid is relevant with the partition of rare earth, is generally H ₂C ₂O ₄: TR ₂O ₃=1.6～2.2: 1, the gained rare earth oxalate promptly gets mixed rare-earth oxide after calcination is handled, gained oxalic acid liquid adjust PH to 5～6 and scrub solution to specific concentrations (as ammonium sulfate about 2%, about sodium-chlor 7%), promptly can be recycled after making residue oxalate denominationby and calcium ion effect generation caoxalate; As wish to get grouping products, then, use extraction agent (as P with after the rare earth mother solution clarification ₂₀₄Deng) extract, hydrochloric acid back extraction grouping can be returned use after the concentration of the surplus liquid adjustment of extraction agent scrub solution.

Pressurization elution device among the present invention is shown in figure one, by cell body (1), cone seal lid (2), sealing cover transmission rig (13), removable bottom (3) and removable bottom lifting mechanism formations such as (7) .Cell body (1) is welded with general steel plate, and its volume is decided according to the ore handling capacity size.Apparatus of the present invention cell body size, length * wide * height is 2200 * 2000 * 2600 millimeters, and the cell body bottom is welded with angle steel flange and groove seat (15) is connected and fixed, and groove seat available metal spare or cement preform are made.The removable bottom (3) that is drilled with aperture is an ironcasting, be fastened on the elution groove lower angle steel flange by hinges (17), realize the closure or openness of removable bottom by the removable bottom lifting mechanism of forming by pulley (18), wireline (11) self-locking worm gear worm screw (7) .Driving motor power 1 kilowatt of of cone seal lid transmission rig (13), 10～15 rev/mins of cone seal lid rotating speeds.Cone seal lid and cell body contact site inlay a wear-resisting soft sealing-ring of garden ring-type (14) (as rubber etc.), and the sealing circle can freely be changed.The scrub solution injection tube (4) of band reverse checkvalve is equipped with on the cell body top.For guaranteeing to be convenient to safely check, pressure safety valve (9) and tensimeter (8) are housed on elution groove cell body top.

The schedule of operation of elution groove: (1) must complete filter cloth earlier before the cell body feed, after by lifting mechanism (7) it is closed removable bottom; (2) with handwheel (12) cone seal lid (2) is put down (dotted line position that is in accompanying drawing one), back actuating motor makes cone seal lid (2) rotation; (3) raw ore is fed on the cone seal lid (2), treat that cell body fills with specified altitude after, close the electric motor of cone seal lid transmission rig; (4) it is airtight with the cell body top that artificial rotation hand wheel (12) makes the cone seal lid; (5) injection tube (4) of scrub solution by the band reverse checkvalve injected in the cell body; (6) inlet pipe (5) by the band reverse checkvalve adds pressurized air in cell body; (7) elution finishes, and adds water by injection tube (4) in groove, treats promptly to close water valve after top water all passes the bed of material in the groove; (8) start removable bottom transmission rig (7) removable bottom is opened, the rare earth tailings in the removal slot.

Advantage of the present invention is: (1) is because the elution operation is to carry out under pressurized conditions, can strengthen the permutoid reaction and the solid-liquid separation process of ammonium ion or the sodium ion and the rare earth ion of scrub solution solution, thereby the cycle of elution operation was shortened to about 4 hours by 24～72 hours that have technology now, improve 6～18 times of work efficiency; (2) rare-earth original ore falls in the elution groove by the cone seal lid that rotates, and makes the interior cloth of groove even, abundant, the uniform contact of rare-earth mineral in scrub solution energy and the groove; (3) pressurization elution technology can make the yield of rare earth improve 10～25% than existing technology; (4) owing to adopt rotary conveyor feed and elution trough washery to carry rare earth, can reduce labor intensity greatly, improve working conditions.

The present invention is applicable to ion adsorption type rare earth ore elution rare earth, is adapted to especially that clay mineral contents such as rare-earth original ore fine size, kaolinite are many, the elution of the rare-earth original ore of strainability difference.

Claims

1, a kind of from the ion adsorption type re raw ore the direct technology of elution rare earth oxide, it is characterized in that rare-earth original ore packs in the elution groove cell body [1], the back adds scrub solution by the injection tube that has reverse checkvalve [4], imports the pressurized air elution of pressurizeing again to cell body [1] in.

2, technology according to claim 1 is characterized in that said elution is at liquid: Gu=carry out under 0.6～1: 1 condition.

3, technology according to claim 1 is characterized in that said pressurization, is to keep 1～5 kilograms per centimeter in cell body ²Carry out elution under the pressure condition.

4, a kind of for realizing that aforesaid right requires the device of technology, it is characterized in that this device is by cell body (1), cone seal lid (2), removable bottom with holes (3), cone seal lid transmission rig (13), garden annular seal ring (14), the scrub solution injection tube (4) of removable bottom lifting mechanism (7) band reverse checkvalve and the inlet pipe compositions such as (5) of band reverse checkvalve.

5, device according to claim 4 is characterized in that it is to regulate by handwheel (12) that said cone seal covers down motion, and its rotation is by transmission rig (13) control, and cone seal covers 10～15 rev/mins of rotating speeds.

6, device according to claim 4 is characterized in that said cone seal covers at itself and contact site, cell body top to be lined with a garden annular seal ring (14).

7, device according to claim 4, it is characterized in that said removable bottom (3) one ends are connected by hinge (17) is fixed on the elution groove lower angle iron flange, the other end is by pulley (18), wireline (11), self-locking worm gear worm gearing (13) are opened and are closed.