CN107746976A - The method that the positive carbonate of rare earth is prepared with high concentration precipitating reagent - Google Patents
The method that the positive carbonate of rare earth is prepared with high concentration precipitating reagent Download PDFInfo
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- CN107746976A CN107746976A CN201710827150.3A CN201710827150A CN107746976A CN 107746976 A CN107746976 A CN 107746976A CN 201710827150 A CN201710827150 A CN 201710827150A CN 107746976 A CN107746976 A CN 107746976A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
- C22B3/46—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
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Abstract
The invention discloses a kind of method that the positive carbonate of rare earth is prepared with high concentration precipitating reagent, including:In the case where being stirred continuously, by ammonium hydrogen carbonate and technical grade ammoniacal liquor in molar ratio 5.6:4.4~10:1 is mixed and added into 15~30 DEG C of water, and the concentration for making precipitating reagent is 3~6mol/L;Caused precipitation waste liquid and crystal seed containing ammonia nitrogen in rare earth raw material liquid, carbonated rare earth production process are inserted in reactive tank, crystal seed is the positive carbonate of rare earth of corresponding rare earths material production;The temperature of solution is between 20~40 DEG C in lower control reactive tank is stirred continuously, precipitating reagent is slowly added into reactive tank, the addition time is 3~9h, addition can obtain the positive carbonate products of rare earth and the precipitation waste liquid containing ammonia nitrogen so that untill pH=6.5~7 of solution after the precipitation directly progress filtration washing of generation.Present invention saves the energy and reduce the quantum of output of precipitation waste liquid, reach the purpose of energy-saving and emission-reduction.
Description
Technical field
The present invention relates to a kind of rare-earth wet method metallurgical technology, specifically, is related to one kind and prepares rare earth with high concentration precipitating reagent
The method of positive carbonate.
Background technology
At present, the method for the positive carbonate of industrialized production rare earth is that ammonium hydrogen carbonate solid is added into temperature for 45~55 DEG C
2.0~2.8mol/L ammonium bicarbonate soln is configured in water, ammonium bicarbonate soln reacts as precipitating reagent and earth solution.Instead
After the completion of answering, the positive carbonate of rare earth is can obtain after slurries filtering, washing.This technique because the solubility of ammonium hydrogen carbonate is smaller,
Not only need the ammonium bicarbonate soln concentration that consumes substantial amounts of heat energy but also make relatively low in course of dissolution, cause precipitating
During output precipitation waste liquid it is more.
Patent publication No. is that CN104891550A discloses a kind of method that ceria is prepared by mixed precipitant, is used
Ammonium hydrogen carbonate integral molar quantity and ammoniacal liquor integral molar quantity 55~25:The mixing that 45~75 ratio is configured to 2.0~5.5mol/L is sunk
Shallow lake agent solution, using solution of cerium chloride by oxidation as feed liquid, it is prepared under conditions of 50~70 DEG C based on basic carbonate cerium, cerous carbonate and hydrogen
Mixed sediment supplemented by cerium oxide.The method prepares that not only temperature is higher during sediment but also sediment is mixing
Thing.
Patent publication No. is that CN104017500A discloses a kind of preparation method of polishing powder from rare earth, and mischmetal is passed through
(ammonium hydrogen carbonate, the mass ratio of ammoniacal liquor are 1 to the mixed solution of ammonium hydrogen carbonate and ammoniacal liquor precipitation in mixed solution:1~2), during precipitation
Temperature be 45 DEG C~55 DEG C, digestion time be 12~18 hours, after ageing add fluoric-containing acid be fluorinated, the alkali being fluorinated
Formula carbonated rare earth.Although the method is precipitated using ammonium hydrogen carbonate and ammonia spirit, what is obtained is basic carbonate rare earth.
It is accordingly required in particular to a kind of method that the positive carbonate of rare earth is prepared with high concentration precipitating reagent, to solve above-mentioned technique
Present in problem.
The content of the invention
Technical problem solved by the invention is to provide a kind of method that the positive carbonate of rare earth is prepared with high concentration precipitating reagent,
The preparation temperature of precipitating reagent is reduced in preparation process and improves the concentration of precipitating reagent, so as to save the energy and reduce
The quantum of output of waste liquid is precipitated, has reached the purpose of energy-saving and emission-reduction.
Technical scheme is as follows:
A kind of method that the positive carbonate of rare earth is prepared with high concentration precipitating reagent, including:
In the case where being stirred continuously, by ammonium hydrogen carbonate and technical grade ammoniacal liquor in molar ratio 5.6:4.4~10:1 is mixed and added into 15
~30 DEG C of water, the concentration for making precipitating reagent are 3~6mol/L;
Caused precipitation waste liquid and crystal seed containing ammonia nitrogen in rare earth raw material liquid, carbonated rare earth production process are inserted into reactive tank
In, crystal seed is the positive carbonate of rare earth of corresponding rare earths material production;Amount of seed be required precipitating rare earth quality 20%~
100%, the concentration of reactive tank middle rare earth solution is allocated to 0.06~1.5mol/L with the precipitation waste liquid containing ammonia nitrogen;
Precipitating reagent is slowly added into instead by the temperature of solution between 20~40 DEG C in lower control reactive tank is stirred continuously
Answer in groove, the addition time is 3~9h, so that untill pH=6.5~7 of solution, the precipitation of generation is directly filtered addition
After washing, you can obtain the positive carbonate products of rare earth and the precipitation waste liquid containing ammonia nitrogen.
Further:Ammonium hydrogen carbonate used in precipitating reagent preparation uses solution or solid.
Further:Rare earth raw material liquid is single re chloride, mixed chlorinated rare earth solution, single rare earth nitrate solution
Or mixeding acid rare-earth solution.
Further:The positive carbonate of rare earth includes lanthanum carbonate normal salt, cerous carbonate normal salt or neodymium carbonate normal salt.
Further:In the case where being stirred continuously, by ammonium hydrogen carbonate solid and technical grade ammoniacal liquor in molar ratio 6:20 are added after 4 mixing
DEG C water, the concentration for making precipitating reagent is 4.5mol/L;By 3.5m3Rare earth concentration is that 1.7mol/L lanthanum chloride feed liquids are placed in reactive tank
In, it is 0.9mol/L to be allocated feed liquid to rare earth concentration with precipitation waste liquid, and adds 1t lanthanum carbonate normal salt as crystal seed;Continuous
It is 40 DEG C that solution temperature in reactive tank is controlled under stirring, precipitating reagent is slowly added into reactive tank, the addition time of precipitating reagent
For 7.2h, untill the addition of precipitating reagent makes the pH=6.7 of solution, after the precipitation of generation directly carries out filtration washing, you can
To lanthanum carbonate normal salt and precipitation waste liquid.
Further:In the case where being stirred continuously, by ammonium hydrogen carbonate solid and technical grade ammoniacal liquor in molar ratio 6:30 are added after 4 mixing
DEG C water, the concentration for making precipitating reagent is 4.8mol/L.By 3.5m3Rare earth concentration is that 1.66mol/L cerous nitrate feed liquids are placed in reaction
In groove, it is 0.6mol/L to be allocated feed liquid to rare earth concentration with precipitation waste liquid, and adds 1.5t cerous carbonate normal salt as crystal seed.
Be stirred continuously it is lower to control in reactive tank solution temperature be 35 DEG C, precipitating reagent is slowly added into reactive tank, the addition of precipitating reagent
Time is 8h, untill the addition of precipitating reagent makes the pH=6.7 of solution, after the precipitation of generation directly carries out filtration washing, you can
Obtain cerous carbonate normal salt and precipitation waste liquid.
Further:In the case where being stirred continuously, by ammonium hydrogen carbonate solid and technical grade ammoniacal liquor in molar ratio 6.2:Add after 3.8 mixing
Enter 25 DEG C of water, the concentration for making precipitating reagent is 4.5mol/L;By 1.5m3Rare earth concentration is that 1.42mol/L neodymium chloride feed liquids are inserted
In reactive tank, it is 0.18mol/L to be allocated feed liquid to rare earth concentration with precipitation waste liquid, and adds 0.6t neodymium carbonates normal salt as brilliant
Kind;Be stirred continuously it is lower to control solution temperature in reactive tank be 35 DEG C, precipitating reagent is slowly added into reactive tank, precipitating reagent
The addition time is 5h, untill the addition of precipitating reagent makes the pH=6.7 of solution, after the precipitation of generation directly carries out filtration washing,
It can obtain neodymium carbonate normal salt and precipitation waste liquid.
Compared with prior art, the technology of the present invention effect includes:
1st, this method has prepared the positive carbonate of rare earth by controlling the configuration proportion of mixed precipitant.
2nd, the preparation temperature of precipitating reagent is reduced in preparation process and improves the concentration of precipitating reagent, so as to save energy
Source and the quantum of output for reducing precipitation waste liquid, reduce the discharge capacity of waste water, while improve the concentration of ammonium chloride in waste water, real
Show the decrement enrichment of waste water, reach the purpose of energy-saving and emission-reduction.Due to reducing the usage amount of ammonium hydrogen carbonate, significantly reduce
The discharge of carbon dioxide, there is good environmental benefit.
3rd, the preparation of its product can be achieved in the present invention on the main equipment of existing production carbonated rare earth, it is not necessary to carries out
Large-scale transformation, is advantageous to large-scale promotion application.
4th, it is that raw material prepares mixed precipitant with ammonium hydrogen carbonate and ammoniacal liquor, has reached the purpose of ammoniacal liquor reuse, solved simultaneously
The problem of precipitating reagent in the winter time crystallizes.
5th, remarkable in economical benefits.
It is expected that performance evaluation:
(1) 20,000 tons of REO meters (lanthanum carbonate, cerous carbonate, lanthanum carbonate cerium) are produced per year:The expense of ammonium hydrogen carbonate reduction:0.61
* 713.7 yuan/ton * 20000 tons=870.71 ten thousand yuan of ton, the expense of wastewater treatment reduction:3.8m3*123.55 first * 20000 tons=
938.98 ten thousand yuan, heat reduced expense:0.25*252 yuan/ton of steam (steam cost measuring and calculating at this stage) * 20000 tons=126
Wan Yuan.1935.69 ten thousand yuan of the low expense of total co-falling.
(2) 0.5 ten thousand tons of REO meters (neodymium carbonate) are produced per year:The expense of ammonium hydrogen carbonate reduction:0.61 ton of * 713.7 yuan/ton of *
5000 tons=217.68 ten thousand yuan, the expense of wastewater treatment reduction:3.6m3*123.55 first * 5000 tons=222.39 ten thousand yuan, heating
The expense of reduction:0.25*252 yuan/ton of * 5000 tons=31.5 ten thousand yuan of steam (steam cost measuring and calculating at this stage), add up to co-falling low
471.57 ten thousand yuan of expense.
It is cost-saved altogether:2407.26 ten thousand yuan.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of the product of embodiment 1 in the present invention;
Fig. 2 is the X-ray diffractogram of the product of embodiment 2 in the present invention;
Fig. 3 is the X-ray diffractogram of the product of embodiment 3 in the present invention.
Embodiment
Technical solution of the present invention is elaborated below with reference to example embodiment.However, example embodiment can
Implement in a variety of forms, and be not understood as limited to embodiment set forth herein;On the contrary, these embodiments are provided so that
The design of example embodiment more comprehensively and completely, and is comprehensively communicated to those skilled in the art by the present invention.
A kind of method that the positive carbonate of rare earth is prepared with high concentration precipitating reagent proposed by the present invention, using following technical side
Case:
Step 1:In the case where being stirred continuously, by ammonium hydrogen carbonate and technical grade ammoniacal liquor in molar ratio 5.6:4.4~10:1 mixing is simultaneously
15~30 DEG C of water is added, the concentration for making precipitating reagent is 3~6mol/L;
Ammonium hydrogen carbonate used in precipitating reagent preparation can be solution or solid.
Step 2:By the caused precipitation waste liquid (or water) containing ammonia nitrogen in rare earth raw material liquid, carbonated rare earth production process and crystalline substance
Kind (the positive carbonate of rare earth of corresponding rare earths material production) is inserted in reactive tank;
Amount of seed is the 20%~100% of required precipitating rare earth (folding REO) quality, with containing ammonia nitrogen precipitation waste liquid (or
Water) concentration of reactive tank middle rare earth solution is allocated to 0.06~1.5mol/L.
Rare earth raw material liquid can be single re chloride, mixed chlorinated rare earth solution, single rare earth nitrate solution, mixed
Close rare earth nitrate solution etc..
Step 3:The temperature of solution slowly adds precipitating reagent between 20~40 DEG C in lower control reactive tank is stirred continuously
Enter into reactive tank, the addition time is 3~9h, and addition so that untill pH=6.5~7 of solution, directly enter by the precipitation of generation
After row filtration washing, you can obtain the positive carbonate products of rare earth and the precipitation waste liquid containing ammonia nitrogen.
Embodiment 1
In the case where being stirred continuously, by ammonium hydrogen carbonate solid and technical grade ammoniacal liquor in molar ratio 6:20 DEG C of water is added after 4 mixing,
The concentration for making precipitating reagent is 4.5mol/L.By 3.5m3Rare earth concentration is that 1.7mol/L lanthanum chloride feed liquids are placed in reactive tank, with heavy
It is 0.9mol/L that shallow lake waste liquid, which allocates feed liquid to rare earth concentration, and adds 1t lanthanum carbonate normal salt as crystal seed.In the case where being stirred continuously
It is 40 DEG C to control solution temperature in reactive tank, and precipitating reagent is slowly added into reactive tank, and the addition time of precipitating reagent is 7.2h,
Untill the addition of precipitating reagent makes the pH=6.7 of solution, after the precipitation of generation directly carries out filtration washing, you can obtain lanthanum carbonate
Normal salt and precipitation waste liquid.It is 7.2m to precipitate waste liquid quantum of output3/ tREO, the total amount of rare earth of product is 48.76%.
As shown in figure 1, it is the X-ray diffractogram of the product of embodiment 1 in the present invention, from figure 1 it appears that 2 θ exist
10.42 °, 18.54 °, 19.77 °, 27.20 °, 29.18 ° etc. nearby there is La2(CO3)3·8H2O characteristic diffraction peak, not
Detect the characteristic diffraction peak of basic carbonate lanthanum and lanthanum hydroxide.
Embodiment 2
In the case where being stirred continuously, by ammonium hydrogen carbonate solid and technical grade ammoniacal liquor in molar ratio 6:30 DEG C of water is added after 4 mixing,
The concentration for making precipitating reagent is 4.8mol/L.By 3.5m3Rare earth concentration is that 1.66mol/L cerous nitrate feed liquids are placed in reactive tank, is used
It is 0.6mol/L that precipitation waste liquid, which allocates feed liquid to rare earth concentration, and adds 1.5t cerous carbonate normal salt as crystal seed.Constantly stirring
Mix it is lower to control in reactive tank solution temperature be 35 DEG C, precipitating reagent is slowly added into reactive tank, the addition time of precipitating reagent is
8h, untill the addition of precipitating reagent makes the pH=6.7 of solution, after the precipitation of generation directly carries out filtration washing, you can obtain carbon
Sour cerium normal salt and precipitation waste liquid.It is 7.2m to precipitate waste liquid quantum of output3/ tREO, the total amount of rare earth of product is 49.52%.
As shown in Fig. 2 it is the X-ray diffractogram of the product of embodiment 2 in the present invention, from figure 2 it can be seen that 2 θ exist
10.45 °, 18.65 °, 19.86 °, 27.36 °, 29.34 ° etc. nearby there is Ce2(CO3)3·8H2O characteristic diffraction peak, not
Detect the characteristic diffraction peak of basic carbonate cerium and cerium hydroxide.
Embodiment 3
In the case where being stirred continuously, by ammonium hydrogen carbonate solid and technical grade ammoniacal liquor in molar ratio 6.2:25 DEG C are added after 3.8 mixing
Water, the concentration for making precipitating reagent is 4.5mol/L.By 1.5m3Rare earth concentration is that 1.42mol/L neodymium chloride feed liquids insert reactive tank
In, it is 0.18mol/L to be allocated feed liquid to rare earth concentration with precipitation waste liquid, and adds 0.6t neodymium carbonate normal salt as crystal seed.
Be stirred continuously it is lower to control in reactive tank solution temperature be 35 DEG C, precipitating reagent is slowly added into reactive tank, the addition of precipitating reagent
Time is 5h, untill the addition of precipitating reagent makes the pH=6.7 of solution, after the precipitation of generation directly carries out filtration washing, you can
Obtain neodymium carbonate normal salt and precipitation waste liquid.It is 8m to precipitate waste liquid quantum of output3/ tREO, the total amount of rare earth of product is 48.34%.
As shown in figure 3, it is the X-ray diffractogram of the product of embodiment 3 in the present invention, from figure 3, it can be seen that 2 θ exist
10.54 °, 18.82 °, 20.00 °, 27.57 °, 29.61 ° etc. nearby there is Nd2(CO3)3·8H2O characteristic diffraction peak, not
Detect the characteristic diffraction peak of neodymium hydroxyl-carbonate and neodymium hydroxide.
Term used herein is explanation and exemplary and nonrestrictive term.Because the present invention can be with a variety of
Form specific implementation without departing from the spiritual or substantive of invention, it should therefore be appreciated that above-described embodiment be not limited to it is any foregoing
Details, and should widely being explained in the spirit and scope that appended claims are limited, thus fall into claim or its etc.
Whole changes and remodeling in the range of effect all should be appended claims and covered.
Claims (7)
1. a kind of method that the positive carbonate of rare earth is prepared with high concentration precipitating reagent, including:
In the case where being stirred continuously, by ammonium hydrogen carbonate and technical grade ammoniacal liquor in molar ratio 5.6:4.4~10:1 is mixed and added into 15~30
DEG C water, the concentration for making precipitating reagent is 3~6mol/L;
Caused precipitation waste liquid and crystal seed containing ammonia nitrogen in rare earth raw material liquid, carbonated rare earth production process are inserted in reactive tank,
Crystal seed is the positive carbonate of rare earth of corresponding rare earths material production;Amount of seed is the 20%~100% of required precipitating rare earth quality,
The concentration of reactive tank middle rare earth solution is allocated to 0.06~1.5mol/L with the precipitation waste liquid containing ammonia nitrogen;
Precipitating reagent is slowly added into reactive tank by the temperature of solution between 20~40 DEG C in lower control reactive tank is stirred continuously
In, the addition time is 3~9h, and for addition so that untill pH=6.5~7 of solution, the precipitation of generation directly carries out filtration washing
Afterwards, you can obtain the positive carbonate products of rare earth and the precipitation waste liquid containing ammonia nitrogen.
2. the method for the positive carbonate of rare earth is prepared with high concentration precipitating reagent as claimed in claim 1, it is characterised in that:Precipitating reagent is matched somebody with somebody
Ammonium hydrogen carbonate used in system uses solution or solid.
3. the method for the positive carbonate of rare earth is prepared with high concentration precipitating reagent as claimed in claim 1, it is characterised in that:Rare earths material
Liquid is single re chloride, mixed chlorinated rare earth solution, single rare earth nitrate solution or mixeding acid rare-earth solution.
4. the method for the positive carbonate of rare earth is prepared with high concentration precipitating reagent as claimed in claim 1, it is characterised in that:The positive carbon of rare earth
Hydrochlorate includes lanthanum carbonate normal salt, cerous carbonate normal salt or neodymium carbonate normal salt.
5. the method for the positive carbonate of rare earth is prepared with high concentration precipitating reagent as claimed in claim 1, it is characterised in that:Constantly stirring
Mix down, by ammonium hydrogen carbonate solid and technical grade ammoniacal liquor in molar ratio 6:20 DEG C of water is added after 4 mixing, the concentration for making precipitating reagent is
4.5mol/L;By 3.5m3Rare earth concentration is that 1.7mol/L lanthanum chloride feed liquids are placed in reactive tank, is allocated feed liquid with precipitation waste liquid
It is 0.9mol/L to rare earth concentration, and adds 1t lanthanum carbonate normal salt as crystal seed;The solution in lower control reactive tank is stirred continuously
Temperature is 40 DEG C, precipitating reagent is slowly added into reactive tank, the addition time of precipitating reagent is 7.2h, and the addition of precipitating reagent makes
Untill the pH=6.7 of solution, after the precipitation of generation directly carries out filtration washing, lanthanum carbonate normal salt and precipitation waste liquid are obtained.
6. the method for the positive carbonate of rare earth is prepared with high concentration precipitating reagent as claimed in claim 1, it is characterised in that:Constantly stirring
Mix down, by ammonium hydrogen carbonate solid and technical grade ammoniacal liquor in molar ratio 6:30 DEG C of water is added after 4 mixing, the concentration for making precipitating reagent is
4.8mol/L.By 3.5m3Rare earth concentration is that 1.66mol/L cerous nitrate feed liquids are placed in reactive tank, is adjusted feed liquid with precipitation waste liquid
It is 0.6mol/L to be assigned to rare earth concentration, and adds 1.5t cerous carbonate normal salt as crystal seed;In lower control reactive tank is stirred continuously
Solution temperature is 35 DEG C, and precipitating reagent is slowly added into reactive tank, and addition time of precipitating reagent is 8h, the addition of precipitating reagent
Untill the pH=6.7 for making solution, after the precipitation of generation directly carries out filtration washing, cerous carbonate normal salt and precipitation waste liquid are obtained.
7. the method for the positive carbonate of rare earth is prepared with high concentration precipitating reagent as claimed in claim 1, it is characterised in that:Constantly stirring
Mix down, by ammonium hydrogen carbonate solid and technical grade ammoniacal liquor in molar ratio 6.2:25 DEG C of water is added after 3.8 mixing, makes the dense of precipitating reagent
Spend for 4.5mol/L;By 1.5m3Rare earth concentration is that 1.42mol/L neodymium chloride feed liquids are inserted in reactive tank, will be expected with precipitation waste liquid
It is 0.18mol/L that liquid, which is allocated to rare earth concentration, and adds 0.6t neodymium carbonate normal salt as crystal seed;It is being stirred continuously lower control reaction
Solution temperature is 35 DEG C in groove, and precipitating reagent is slowly added into reactive tank, and the addition time of precipitating reagent is 5h, and precipitating reagent adds
Untill entering the pH=6.7 that amount makes solution, after the precipitation of generation directly carries out filtration washing, obtain neodymium carbonate normal salt and precipitation is useless
Liquid.
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RU2608033C1 (en) * | 2015-12-08 | 2017-01-12 | Открытое акционерное общество "Научно-исследовательский, проектный и конструкторский институт горного дела и металлургии цветных металлов" (ОАО "Гипроцветмет") | Method of producing scandium oxide |
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Application publication date: 20180302 |