CN104404243B - A kind of method of soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate - Google Patents

A kind of method of soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate Download PDF

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CN104404243B
CN104404243B CN201410758208.XA CN201410758208A CN104404243B CN 104404243 B CN104404243 B CN 104404243B CN 201410758208 A CN201410758208 A CN 201410758208A CN 104404243 B CN104404243 B CN 104404243B
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rare earth
ore concentrate
acid
low
weishan
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CN104404243A (en
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陈吉堂
程刚
张立全
郭军杰
胡德志
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钢研集团稀土科技有限公司
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Abstract

The method that the invention discloses a kind of soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate, including the step that rare earth ore concentrate carries out oxidizing roasting, for removing the moisture in rare earth ore concentrate, makes rare earth ore concentrate be changed into rare earth oxide and rare earth fluoride.The present invention adopts technique scheme, substantially increases the response rate of Weishan rare earth ore concentrate, and the response rate is up to more than 95%;Adopting soda acid fractional decomposition Weishan rare earth ore concentrate, the fired rear rare earth chemistry existence form of fine ore is by REFCO3It is changed into REOF and RE2O3, after dissolving with hydrochloric acid, fluorine element is changed into RE2F3, existing with slag state form, a small amount of fluorine and aluminum, quadrivalent cerium etc. form complex and enter in solution, it does not have fluorine overflows in a gaseous form, reduces environmental pollution.

Description

A kind of method of soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate

Technical field

The method that the present invention relates to a kind of soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate, belongs to technical field of rare-earth hydrometallurgy.

Background technology

Namely Weishan Rare Earth Mine tiny ore deposit fat, seamed deposit, and strolls all, within the scope of 0.85 square of axiom, it is known that big leader 60 is a plurality of, verifies rare earth oxide reserves more than 400 ten thousand tons, recoverable reserves 2,550,000 tons, mine life 100 years.Mining area belongs to single bastnaesite, light rare earth type, is characterized in that Ore and gangue mineral are simpler, rare-earth mineral is based on bastnaesite, mineral contain 17 kinds of rare earth elements, four kinds of elements of its kind of LaCePrNd account for rare-earth mineral more than 98% (lanthanum 34%, cerium is 49%, praseodymium 4%, neodymium 11%), oil in place is big, and harmful substance is from the superficial to the deep, washability is good, easily exploits.But, Weishan rare earth ore concentrate grade is relatively low, and concentrate content of rare earth is about 40%, and impurity content is high, and concentrate intractability is big, and the response rate is relatively low.

The main technique of current industrial processing rare earth ore concentrate has concentrated sulphuric acid high-temperature roasting method and soda processes.

The Weishan Rare Earth Mine smelting enterprise of more than 90% adopts concentrated sulphuric acid high temperature roast method, this flow process is to carry out in rotary kiln, rare earth ore concentrate reacts after mixing with concentrated sulphuric acid at 500 DEG C 600 DEG C, rare earth ore concentrate generates rare earth sulfate with sulfuric acid reaction, then leaching sulfuric acid rare earth with cold water makes rare earth enter infusion, the purer rare earth sulfate solution obtained after regulating solution PH, finally obtains mixed rare earth carbonate with carbon ammonium precipitation, or abstraction and type-reverting is rare earth chloride.

Said method is less demanding to the taste of concentrate, and industry is easy to control continuously, and chemical reagent consumption is few, and operating cost is relatively low, it is easy to large-scale production.But, said method carries out roasting after needing to mix rare earth ore concentrate with concentrated sulphuric acid, decomposition temperature is higher, the requirement of equipment is higher, in roasting process, fluorine overflows with HF, concentrated sulphuric acid decomposes to give off substantial amounts of containing S-acid waste gas, processes 1 ton of rare earth ore concentrate and produces 80kgHF and 360kg containing S-acid waste gas, and the response rate can only achieve 86%.

Soda processes is that concentrate is first through acid soak, by chemical mineral processing deliming, then decomposing with Caustic soda and make rare earth generate the water insoluble hydroxide being soluble in mineral acid, fluorine and phosphate radical then generate water-soluble sodium fluoride and sodium phosphate with alkali, make it separate with rare earth, be recycled.

Products in water washing after caustic digestion in said method, rare earth hydrate water insoluble and and magazins' layout, namely obtain re chloride after rare earth hydrate dissolving with hydrochloric acid after washing, remove impurity, reclaim Th simultaneously.Caustic soda decomposition technique produces without harmful gas, and waste residue amount is little and is easily handled, NaF, the Na in waste water3PO4Available causticizing process is recycled, and reduces the fluorine pollution to environment.

But this technique there is problems of, first, first Caustic soda must carry out deliming before decomposing Weishan rare earth ore concentrate, wastes substantial amounts of hydrochloric acid and causes rare earth to lose.Second, discontinuous in production process, operating process batch operation, and mineral decomposition temperature must reach more than 140 DEG C, the resolving time is long, and all ratios such as rare earth, Th, F are relatively decentralized, rare earth yield can only achieve 70%, and the response rate is relatively low, thus limiting its large-scale application.

In order to solve the pollution problem of mixed rare earth concentrates catabolic process, the researcher of China is made that a lot of effort.Such as: Chinese patent CN102251106A discloses a kind of method of alkaline process decomposing Baotou rare earth ore concentrate, this technique uses the HCL of 0.5-2mol/L, removes the most of calcium in concentrate at 80-95 DEG C.Concentrate after washing mixes by weight 1:1.2-1:1.6 with sodium hydroxide;Then heat this mixture to 120-200 DEG C, react 10-60min;Product is washed to neutrality, after the alkali cake dissolving with hydrochloric acid after washing, and is 4 5.5 with alkali cake readjustment pH value, obtains pure re chloride.

Chinese patent CN101392332A discloses a kind of sulfuric acid rare earth roasted ore and directly converts Extraction of rare earth process for cleanly preparing, for the sulfuric acid process roasting production technology that Baotou Iron Ore Concentrate is raw material, the technological process of the present invention is according to metathesis reaction conversion process in chemical process, according to the different mutual transforming principles of solubility product solid matter, what realize sulfate directly converts production.Rare earth compound etc. being carried out low cost entirely reclaim, water can realize complete alternation utilization simultaneously, takes the materials such as the intermediate impurity removal process non-rare earth Ca of recovering rare earth mineral.

Chinese patent CN101824531A discloses a kind of liquid alkali low-temperature roasting decomposition process of caustic soda liquid of mixed rare earth concentrates, relate to a kind of liquid alkali low-temperature roasting decomposition process of caustic soda liquid of mixed rare earth concentrates, including procedure below: (1), mixed by mixed rare earth concentrates with sodium hydroxide 1:0.5~1:1.5 by weight;(2) roasting, sintering temperature 150 DEG C~550 DEG C, roasting time 0.5~4 hour, by mixed Rare Earth Mine are carried out;(3), the roasted ore that roasting obtains is washed to neutrality;(4), washing after alkali cake dissolving with hydrochloric acid, control PH=4~5, obtain re chloride;(5), the thorium enriched thing washing rear enclosed after dissolving with hydrochloric acid is stored up or is dissolved further and extracts thorium and rare earth.

Above several method can only be suitable for high-grade baotite is carried out scale process, it is impossible to solves the problem that the Weishan low-grade rare earth ore concentrate response rate is low.

Summary of the invention

The technical problem to be solved in the present invention is for the deficiencies in the prior art, it is provided that one can reduce environmental pollution, energy efficient, the method decomposing low-grade Weishan rare earth ore concentrate that the response rate is high.

For solving the problems referred to above, the present invention is by the following technical solutions: the method for a kind of soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate, it is characterized in that: include carrying out rare earth ore concentrate the step of oxidizing roasting, for removing the moisture in rare earth ore concentrate, rare earth ore concentrate is made to be changed into rare earth oxide and rare earth fluoride.

The following is further improvement of the present invention:

In described oxidizing roasting step, sintering temperature is 400-600 DEG C, and roasting time is 1-2 hour.

Improve further:

Also including the rare earth ore concentrate after oxidizing roasting step is carried out acid-soluble step, the rare earth ore concentrate after oxidizing roasting is added dissolving with hydrochloric acid, make rare earth oxide and fluorine rare earth oxide dissolve, rare earth fluoride slag making, heat filtering obtains filtrate and acid dissolution slag.

Improve further:

Described concentration of hydrochloric acid is 9.5-10.0mol/L, and extraction temperature is 80 DEG C-95 DEG C, and liquid-solid mass ratio is 2:1.

Improve further:

Also include the step that the acid dissolution slag obtained in acid-soluble step is carried out caustic digestion, in described acid dissolution slag, add sodium hydroxide decompose, produce rare earth hydrate.

Improve further:

Decomposition temperature during caustic digestion step is 100-120 DEG C.

Improve further:

Also include the step that the rare earth hydrate obtained in caustic digestion step is carried out to be washed, native for the described hydroxide water through 60 DEG C-80 DEG C is repeatedly performed and is washed to PH < 9.

Improve further:

Also include the step that the filtrate obtained in acid-soluble step and the rare earth hydrate after water-washing step are carried out to be adjusted back, rare earth hydrate after adding water-washing step in described filtrate is adjusted back, filter, obtain rare earth chloride liquid and filtering residue, obtain final rare earth chloride product by after described rare earth chloride liquid remove impurity.

Improve further:

Readjustment temperature in described readjustment step is 85 DEG C-95 DEG C, and readjustment PH is 4-4.5.

Improve further:

Also include the filtering residue obtained in readjustment step is carried out the excellent molten step of hydrochloric acid, adopt the excellent molten recovery of hydrochloric acid to obtain rare earth chloride liquid and filtering residue described filtering residue.

The present invention adopts technique scheme, substantially increases the response rate of Weishan rare earth ore concentrate, and the response rate is up to more than 95%;Adopting soda acid fractional decomposition Weishan rare earth ore concentrate, the fired rear rare earth chemistry existence form of fine ore is by REFCO3It is changed into REOF and RE2O3, after dissolving with hydrochloric acid, fluorine element is changed into RE2F3, existing with slag state form, a small amount of fluorine and aluminum, quadrivalent cerium etc. form complex and enter in solution, it does not have fluorine overflows in a gaseous form, reduces environmental pollution;After two-step pretreatment fired, acid-soluble, the acid dissolution slag of generation accounts for the 1/3 of total concentrate, compared with directly adopting sodium hydroxide decomposition, what reduce sodium hydroxide makes consumption, save cost, wastewater discharge minimizing 2/3 compared with alkaline process decomposition, greatly reduce energy resource consumption.

Below in conjunction with accompanying drawing, the present invention is further illustrated.

Accompanying drawing explanation

Fig. 1 is the process chart of the low-grade rare earth ore concentrate in soda acid of the present invention associating low-temperature decomposition Weishan.

Detailed description of the invention

Embodiment 1, the method for a kind of soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate, step is as follows:

(1), by the Weishan rare earth ore concentrate of low taste carry out oxidizing roasting and remove moisture, make rare earth by REFCO simultaneously3It is changed into rare earth oxide RE2O3With rare earth fluoride REFO, sintering temperature is at 400-600 DEG C, and roasting time is 1-2 hour.The oxidation being all unfavorable for rare earth too high or too low for temperature during roasting, the time is too short, aoxidizes insufficient, long, there is crystalline transformation problem, therefore selects suitable time and temperature that rare earth ore concentrate can be made fully oxidized, improves the resolution ratio of concentrate.

During roasting, dominant response equation is as follows:

(2), the rare earth ore concentrate after oxidizing roasting being added dissolving with hydrochloric acid, make rare earth oxide and fluorine rare earth oxide dissolve, rare earth fluoride slag making, heat filtering obtains filtrate I and acid dissolution slag I;

Leaching condition is: concentration of hydrochloric acid is 9.5-10.0mol/L, and extraction temperature is 80 DEG C-95 DEG C, and liquid-solid mass ratio is 2:1, simultaneously at the uniform velocity filtered while hot after stirring 60min.Adopting concentration of hydrochloric acid is that 9.5-10.0mol/L can make after roasting RE in concentrate2O3Dissolving more abundant with REOF, dissolution rate is up to 75%.

Dominant response equation is as follows:

(3), in acid dissolution slag I, add sodium hydroxide decomposition, produce rare earth hydrate II;

Decomposition temperature is 100-120 DEG C, and this step makes rare earth generate the water insoluble rare earth hydrate being soluble in mineral acid, and fluorine therein and carbonate then generate water-soluble sodium fluoride and sodium carbonate with alkali so that it is separate with rare earth, be recycled.The decomposition being added to rare earth fluoride of sodium hydroxide, makes rare earth fluoride be converted into rare earth hydrate, it is simple to dissolving with hydrochloric acid.

Dominant response equation is as follows:

(4), rare for hydroxide II soil is repeatedly performed through the water of 60 DEG C-80 DEG C it is washed to PH < 9, when rare earth hydrate washes with water, owing to rare earth hydrate II is water insoluble and separate with soluble impurity, namely the rare earth hydrate II after washing obtains re chloride after being used as readjustment agent dissolving, remove impurity.

Rare earth hydrate is washed repeatedly, can effectively remove F and CO3 2-, fluorine enters waste water with free state, and waste water processes through effluent treatment plant, and discharge water fluoride content is up to standard, does not pollute the environment;Meanwhile, can prevent from when adjusting back, regenerating rare earth fluoride precipitation, reduce the response rate, the aqueous alkali produced after washing can Reusability effectively reduce water make consumption, the hot wash simultaneously using 60 DEG C more than-80 DEG C is raising Na3CO3Dissolubility with NaF, it is simple to separate.

(5), add in filtrate I and wash qualified rare earth hydrate II and carry out readjustment and be filtrated to get rare earth chloride liquid II and filtering residue III, after rare earth chloride liquid II is added akali sulphide remove impurity, obtain final rare earth chloride product.

Described readjustment temperature is 85 DEG C-95 DEG C, and readjustment PH is 4-4.5, owing to the filtrate I after dissolving with hydrochloric acid is containing substantial amounts of non-rare earth impurity, adopts rare earth hydrate II to adjust back pH value, can effectively lower the amount of bringing into of non-rare earth impurity.

(6), the filtering residue III obtained in upper step adopt the excellent row that dissolves into of hydrochloric acid recycle, obtain rare earth chloride liquid IV and filtering residue IV, can rare earth chloride liquid IV be mixed in filtrate I and be uniformly carried out readjustment step, it is also possible to individually adjust back, fill storehouse after being washed by filtering residue IV and seal up for safekeeping.

(7), the water lotion that upper step washing filtering residue IV obtains is squeezed into making beating recycling in rare earth hydrate II.

The method that above-mentioned soda acid is combined low-temperature decomposition low-grade Weishan rare earth ore concentrate carries out experimental verification, carries out lab scale, pilot scale respectively and tries greatly the response rate to determine Weishan Rare Earth Mine.

Embodiment 2, carries out small scale experiments to Weishan Lake Rare Earth Mine.

Experimental facilities: Muffle furnace, iron pan, balance, beaker, graduated cylinder, filter, iron crucible, electric furnace, Glass rod, motor stirrer etc..

Experimental raw: 40% rare earth ore concentrate, concentrated hydrochloric acid, sodium hydroxide etc..

Experimentation:

1, take the low-grade rare earth ore concentrate in 1000g Weishan, heat 2 hours at 600 DEG C of temperature with Muffle furnace, after taking-up, weigh to obtain 884g;

2, putting in 1.2L hydrochloric acid by the Rare Earth Mine after roasting, be simultaneously heated to 95 DEG C what stir, be incubated 30 minutes, filter, obtain filtrate 1.14L after reaction, acid dissolution slag is 405g;

3, acid dissolution slag is put in iron crucible, add 180g sodium hydroxide, and add suitable quantity of water and be adjusted to atherosclerotic, with about heating by electric cooker to 110 DEG C, be stirred continuously lower insulation 2 hours, obtain rare earth hydrate;

4, the water of 80 DEG C is adopted to wash rare earth hydrate obtained for previous step, it is about 9 to pH, obtains rare earth hydrate, by adjustment pH value in the rare earth hydrate addition filtrate after washing to 4-4.5, obtaining rare earth chloride liquid and filtering residue, rare earth chloride liquid concentration is 1.702mol/l;

5, the filtering residue obtained in step 4 carrying out the excellent molten process of hydrochloric acid, concentration of hydrochloric acid is 1.0mol/l, temperature > 90 DEG C, excellent solution adds soda readjustment, readjustment liquid is mixed in the filtrate obtained in step 2, and final that rare earth chloride liquid volume is 1.71L, concentration is 1.25mol/L.

Mass balance:

In Rare Earth Mine used, rare earth oxide quality is:

1000 × 40% × (1-7%)=372g

In final gained rare earth chloride liquid, rare earth oxide quality is:

1.25mol/L×1.71L×169g/L=361g

The last response rate is:

361g÷372g=97.0%

Embodiment 3, in order to further determine that the response rate in Weishan Lake Rare Earth Mine small scale experiments, the popularization that will feed intake carries out pilot scale.

Experimental facilities: platform balance, large beaker, filter, iron crucible, electric furnace, Glass rod etc..

Experimental raw: Rare Earth Mine grade (46.5%), concentrated hydrochloric acid, sodium hydroxide etc. after rotary kiln baking.

Experimentation:

1, taking Rare Earth Mine after 10kg rotary kiln baking, put in 16L concentrated hydrochloric acid, be simultaneously heated to 95 DEG C in stirring, be incubated 30 minutes, after reaction, filtration, obtains filtrate 15.4L, and rare earth concentration is 1.21mol/L, and acid dissolution slag is 4.3kg;

2, filtering residue is put in rustless steel metal bucket, add 1.5kg sodium hydroxide, and add suitable quantity of water and be adjusted to atherosclerotic, with about heating by electric cooker to 110 DEG C, be stirred continuously lower insulation 2 hours, obtain rare earth hydrate;

3, adopting the water of 80 DEG C to carry out being washed to pH rare earth hydrate obtained for previous step is about 9;

4, the rare earth hydrate after washing is added readjustment pH to 4-4.5 in filtrate, after filtration, obtain rare earth chloride liquid and filtering residue;

5, the filtering residue in step 4 carrying out the excellent molten process of hydrochloric acid, readjustment, filtration, mixed that rare earth chloride liquid volume is 23.0L with former rare earth chloride liquid, concentration is 1.15mol/L.

Mass balance:

In Rare Earth Mine used, rare earth oxide quality is:

10000×46.5%=4650g

In final gained rare earth chloride liquid, rare earth oxide quality is:

1.15mol/L×23.0L×169g/L=4473g

The last response rate is:

4473g÷4650g=96.2%

Embodiment 4, from lab scale and pilot-scale experiment, is smelted Weishan Lake Rare Earth Mine by this technique, and total rare earth recovery rate is significantly high, and gained solution concentration is also significantly high, very applicable, in order to better investigate technological effect, carries out the big examination of production line.

Experimental facilities: rotary kiln, graphite retort, filter press, adjust back tank, alkali turns tank etc.

Experimental raw: Weishan Lake Rare Earth Mine (grade 40%), concentrated hydrochloric acid, sodium hydroxide etc.

Experimentation:

1, take 1t Weishan Lake Rare Earth Mine and put in rotary kiln, roasting 2 hours under 600 DEG C of temperature;

2, putting in 1.6 cubes of concentrated hydrochloric acid by the ore deposit after roasting, logical steam, heating, to 95 DEG C, is incubated 60 minutes, filters, obtain filtrate 1.65 cubes after reaction, and rare earth concentration is 1.12mol/L, and acid dissolution slag is 418kg;

3, acid dissolution slag is put into alkali and turn in tank, add 150kg sodium hydroxide, and add suitable quantity of water stirring to atherosclerotic, with about eddy heating for heating to 110 DEG C, it is stirred continuously lower insulation 4 hours, obtains rare earth hydrate, will the rare earth hydrate that obtain adopt > washing of 70 degrees Celsius, be about 9 to pH;

4, the rare earth hydrate after washing is added readjustment pH to 4-4.5 in filtrate, after filtration, obtain rare earth chloride liquid and filtering residue;

What 5, the filtering residue in step 4 carried out the excellent molten process of hydrochloric acid arrives rare earth chloride liquid, and mixed that rare earth chloride liquid volume is 2.15 cubes with former rare earth chloride liquid, concentration is 1.05mol/L.

Mass balance:

In Rare Earth Mine used, rare earth oxide quality is:

1t×40%=4.0×105g

In final gained rare earth chloride liquid, rare earth oxide quality is:

1.05mol/L×2.15×103L×169g/L=3.81×105g

The last response rate is:

3.81×105g÷4.0×105g=95.4%

By above-mentioned experiment it can be seen that adopt the rare earth resolution ratio of the method for the soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate of the present invention can reach more than 95%, resolution ratio significantly improves.

Last it is noted that obvious, above-described embodiment is only for clearly demonstrating example of the present invention, and is not the restriction to embodiment.For those of ordinary skill in the field, other multi-form change or variations can also be made on the basis of the above description.Here without also cannot all of embodiment be given exhaustive;And the apparent change thus amplified out or variation are still among protection scope of the present invention.

Claims (3)

1. the method for a soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate, it is characterised in that: include the step that rare earth ore concentrate is carried out oxidizing roasting, for removing the moisture in rare earth ore concentrate, make rare earth ore concentrate be changed into rare earth oxide and rare earth fluoride;In described oxidizing roasting step, sintering temperature is 400-600 DEG C, and roasting time is 1-2 hour;Also including the rare earth ore concentrate after oxidizing roasting step is carried out acid-soluble step, the rare earth ore concentrate after oxidizing roasting is added dissolving with hydrochloric acid, make rare earth oxide and fluorine rare earth oxide dissolve, rare earth fluoride slag making, heat filtering obtains filtrate and acid dissolution slag;Described concentration of hydrochloric acid is 9.5-10.0mol/L, and extraction temperature is 80 DEG C-95 DEG C, and liquid-solid mass ratio is 2:1;Also include the step that the acid dissolution slag obtained in acid-soluble step is carried out caustic digestion, in described acid dissolution slag, add sodium hydroxide decompose, produce rare earth hydrate;Decomposition temperature during caustic digestion step is 100-120 DEG C;Also include the step that the rare earth hydrate obtained in caustic digestion step is carried out to be washed, described rare earth hydrate is repeatedly performed through the water of 60 DEG C-80 DEG C and is washed to pH < 9;
Described method, also include the step that the filtrate obtained in acid-soluble step and the rare earth hydrate after water-washing step are carried out to be adjusted back, rare earth hydrate after adding water-washing step in described filtrate is adjusted back, filter, obtain rare earth chloride liquid and filtering residue, obtain final rare earth chloride product by after described rare earth chloride liquid remove impurity.
2. the method for a kind of soda acid according to claim 1 associating low-temperature decomposition low-grade Weishan rare earth ore concentrate, it is characterised in that: the readjustment temperature in described readjustment step is 85 DEG C-95 DEG C, and readjustment pH is 4-4.5.
3. the method for a kind of soda acid according to claim 2 associating low-temperature decomposition low-grade Weishan rare earth ore concentrate, it is characterized in that: also include the filtering residue obtained in readjustment step is carried out the excellent molten step of hydrochloric acid, adopt the excellent molten recovery of hydrochloric acid to obtain rare earth chloride liquid and filtering residue described filtering residue.
CN201410758208.XA 2014-12-12 2014-12-12 A kind of method of soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate CN104404243B (en)

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