CN1074751C - Production method of rare earth nitrate - Google Patents
Production method of rare earth nitrate Download PDFInfo
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- CN1074751C CN1074751C CN97121934A CN97121934A CN1074751C CN 1074751 C CN1074751 C CN 1074751C CN 97121934 A CN97121934 A CN 97121934A CN 97121934 A CN97121934 A CN 97121934A CN 1074751 C CN1074751 C CN 1074751C
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- rare earth
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- earth nitrate
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 25
- -1 rare earth nitrate Chemical class 0.000 title claims abstract description 17
- 229910002651 NO3 Inorganic materials 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 239000013078 crystal Substances 0.000 claims abstract description 69
- 238000002425 crystallisation Methods 0.000 claims abstract description 25
- 230000008025 crystallization Effects 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 24
- 229910017604 nitric acid Inorganic materials 0.000 claims description 22
- 239000012141 concentrate Substances 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 10
- 239000006166 lysate Substances 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000012452 mother liquor Substances 0.000 claims description 3
- 238000009834 vaporization Methods 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 2
- 238000001640 fractional crystallisation Methods 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 12
- 230000008901 benefit Effects 0.000 abstract description 10
- 238000004090 dissolution Methods 0.000 abstract description 9
- 238000000746 purification Methods 0.000 abstract description 9
- 239000002253 acid Substances 0.000 abstract description 5
- 238000011978 dissolution method Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000002950 deficient Effects 0.000 abstract description 2
- 230000006698 induction Effects 0.000 abstract description 2
- 230000001939 inductive effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 25
- 239000000706 filtrate Substances 0.000 description 15
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 8
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 239000007790 solid phase Substances 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 239000012065 filter cake Substances 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000012535 impurity Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229920002978 Vinylon Polymers 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910018626 Al(OH) Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000011005 laboratory method Methods 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 208000031232 peroneal neuropathy Diseases 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical group 0.000 description 1
- 230000036186 satiety Effects 0.000 description 1
- 235000019627 satiety Nutrition 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention belongs to a preparation method of rare earth nitrate. The main characteristic is that the method of dominant dissolution and seed induction is adopted. The invention not only provides an advantageous dissolution method under the condition of acid-deficient dissolution, which has the advantages of high dissolution speed, high purification efficiency and high equipment production capacity, but also provides a seed crystal induced crystallization method which has the advantages of high crystallization speed, coarse crystal grains and good purification effect. The advantages dissolving and seed crystal inducing method is not only suitable for preparing rare earth nitrate in a laboratory, but also more suitable for producing the rare earth nitrate in an industrial scale.
Description
The invention belongs to inorganic salt of rare earth and make field, the in particular production method of rare earth nitrate.
The remarkable advantage of rare earth nitrate is a high-dissolvability, very easily participates in the modification and the doping of various materials with the solution form, its still not liquid-solid adulterated optimised form, and the adulterated best salt form of liquid-liquid especially.Compare with rare earth chloride, nitrate radical has and is washed easily or pyrolysis and the advantage removed.Therefore, they are subjected to the welcome of pottery, refractory metal, magneticsubstance and colored and optical material industry member just day by day.
With regard to present domestic industry present situation, both lacked economy and effective production method, lack the specifications of quality of product again, this has not only hindered applying of rare earth material, and has more restricted the special material industrial expansion.
People such as Tan Qinde (SCI, 7 (12): 1067,1986; Northwest University's journal, (4): 43,1984; Rare earth, (2): 6,1990; Rare earth, 12 (3): 30,1991) providing with rare earth oxide and the pure nitric acid of top grade is the prepared in laboratory method of the rare earth nitric acid aqueous solution compound of raw material research.What it provided all is the integration dissolution method, purpose is the method for preparation experiment with Yttrium trinitrate, its head end of this method be with rare earth oxide 800 ℃ of calcinations (＞2hr), remove volatile matter, add dissolving in (60-70 ℃) rare nitric acid (1: 1) then, control terminal point PH=3-4, the filtrate decompression behind the suction filtration is condensed into thick, slowly crystallization under the room temperature, recrystallization is placed on 45-50%H twice again
2SO
4Dewater in the atmosphere to constant weight and get crystal.In order to prevent the generation of mixed crystal, they are at preparation Y (NO
3)
36H
2O and Er (NO
3)
36H
2During O, propose to add the method for crystal seed.
But, realize in commercial quantity producing, prior art is far from being enough.The problem that they exist is: (1) integration dissolution method.Because be that once foot drops into, acid consumption is big, the dissolving cycle is long.(2) crystal seed induced crystallization method is limited to suitable heavy rare earth element, as yttrium, erbium etc., and is not used for light rare earths, as lanthanum, cerium etc.But its to crystal seed structure and add-on without any regulation.(3) the sulfuric acid desiccating method is difficult to the industry use.
The object of the present invention is to provide a kind of advantage dissolving and crystal seed induction method, target is to obtain high dissolution rate and dissolution rate, and the solvating agent consumption is low, the purification efficiency height, and crystalline structure is simple, does not have mixed crystal substantially, produces high-purity rare-earth nitrate crystal.
Technical scheme of the present invention is: proposed differential expression advantage dissolving method, at the rare earth oxide of different-grain diameter, all kept maximum mass transfer force and maximum dissolution rate, used the dissolving power that keeps the acid deficient dissolving and increase equipment.Three advantage dissolvings that Here it is.Enter in the decompression evaporator after three times lysate merges, make it to concentrate and filter, crystal seed is dropped in last concentrated solution cooling back, to obtain the crystal solution of certain degree of supersaturation, filter crystal, then again through twice concentrated and crystallization, last mother liquor returns next circulation and concentrates and filter filtrate, concentrates at every turn and filter all to reach certain decontamination effect improving.
Technical characterictic of the present invention is: adopt dissolving, concentrate, crystallization, filtration process.
A. dissolving: the dilute nitric acid solution of heating theoretical amount, RE oxide powder differential ground after the immersion is added dissolving, treat solution colour become brown after, leach not molten thing, filtrate processing to be combined, the starting point concentration of each lysate keep more than the 7.5mol/l, temperature 70-80 ℃, continuously stirring, the dissolving release sequence is respectively 55%, 35% and 10% of total nitric acid amount;
B. concentrate: the lysate that three dissolvings are made merges, and evaporation under reduced pressure also removes moisture content, and to make supersaturated solution, between vaporization temperature 50-100 ℃, the density of final evaporated liquor surpasses 1.6g/cm
3
C. crystallization: adopt fractional crystallization, the cooling supersaturated solution is to room temperature, and to wherein dropping into crystal seed, each crystal seed amount of throwing in is the 1-3% of crystal amount in the supersaturated solution, stirs at a slow speed.
D. filter: filter the supersaturation rare earth nitrate solution, the white crystal that makes, i.e. rare earth nitrate, RE (NO
3)
36H
2O after mother liquor secondary concentration and the crystallization, concentrates and crystallization more for the third time.
Technical scheme of the present invention designs according to following principle: dissolving is respectively to liquid phase and by the mass transfer process of liquid phase to the solid phase transfer by solid phase with crystallization, they not only observe the diffusion mass transfer formula jointly, and crystallisation process is also obeyed nucleus generation and crystal growth rule.
The rate of mass transfer formula:
dm/dt=D·S·(C
2-C
1)/δ
In the formula: C
2, C
1-be respectively liquid phase and solid phase interface concentration of nitric acid
δ-thickness of diffusion layer
S-solid phase specific surface area
The D-spread coefficient
Formula shows that rare earth oxide solid granularity is more little, and its specific surface area is big more, and mass transfer is fast more; Concentration of nitric acid is high more, and dissolution rate is fast more.Therefore, adopting differential expression to add sour mode, is the thinnest part of granularity by dissolved rare earth oxide at first for the first time promptly, the thicker part of second and third time dissolving granularity, but still keeping concentrated nitric acid to react with it, this has not only guaranteed necessary dissolution rate, has also guaranteed dissolution rate completely.
Know that crystal seed has very important effect to crystallisation process.This be because, generating the solid phase crystal by the liquid phase solute is to be finished by two processes of mutual linking, be that nucleus generates and two stages of seeded growth, their speed not only depends on the degree of supersaturation of solute, and the growth rate of crystal seed depends on the specific surface area of crystal seed.If crystal seed is meticulous, specific surface area is excessive, and then growth velocity is fast; Otherwise if crystal seed is thick excessively, specific surface area is little, and then growth velocity is slow.Therefore, making crystal seed also is a crucial step.Crystal seed generating rate and growth velocity are expressed as following formula:
W
1=K·(C
s-C
1)/C
1
In the formula: W
1The generating rate of-crystal seed
K-formation temperature coefficient
C
s-solid phase solute concentration
C
1-liquid phase solute concentration
W
2=D/r·S(C
s-C
1)
In the formula: W
2The generating rate of-crystal seed
The D-spread coefficient
R-crystal seed particle diameter
S-seed ratio table is long-pending
Formula shows that the degree of supersaturation of solute is high more, and the generation of crystal seed and growth velocity are all high more.The crystal seed particle diameter is more little, and its growth velocity is high more.Therefore, the generation of crystal seed should be finished than under the high saturation.The size of crystal seed all should be controlled with distribution.
Description of drawings:
Accompanying drawing 1 is a process flow sheet of producing rare earth nitric acid aqueous solution compound with advantage dissolving and crystal seed revulsion.
Accompanying drawing 2 is an equipment flowsheet of the present invention.
[1] distilled water storage tank, [2] concentrated nitric acid storage tank, [3], [4], [5] dissolving vessel, [6]
[8] strainer, [7] vaporizer, [9] condenser, [10] crystallizer, [11] centrifugal mistake
Filter
Describe by reference to the accompanying drawings the present invention in detail:
The differential expression advantage dissolving that the present invention proposes, namely the nitric acid allocation order of chemical quantity is according to dissolving Order is respectively 55%, 35% and 10% of total amount. Solution temperature is 70-80 ℃. Dissolving Time is followed successively by 30 fens, 45 minutes and 60 minutes.
The thickening filtration operation that the present invention proposes is in order to generate flocculent deposit, such as Fe (OH)3,
Al(OH)
3Deng flocculation, should add the neutral flocculant of 10g/T (quality) in the concentrate, as West uncle youth, then filtering and impurity removing. The addition of its flocculant is the impurity levels such as iron, aluminium, silicon 0.1%. Filtrate is filtered with the vinylon more than 300 orders and felt cloth behind flocculation again, with Remove impurity in the lysate, obtain the primary purification effect. The evaporation concentrate is in 40-50 ℃ of lower warp The above vinylon of 300 orders and felt cloth filter, and obtain the double purification effect.
The crystal seed revulsion that the present invention proposes, the formation condition of its crystal seed is that degree of supersaturation is higher, The injected volume of crystal seed is 1% (quality) of total crystal amount. The growth conditions of crystal is to concentrate satiety Lower with degree, in order to the generation of bigger regular crystal. Crystal seed concentrate for three times and crystallization in all rise Important inducing action.
Three sections differential dissolvings that the present invention proposes and flocculation-filtration method ([3] .[4 in the accompanying drawing 2] .[5] Dissolving tank and [6] filter), guarantee that not only content is 55% particulate footpath rare earth oxide, and really Directly rare earth oxide can both be at theoretical acid consumption bar to protect content and be 35% and 10% middle grain and coarse grain Obtain rapidly and fully dissolving under the part. This low acid dissoluting liquid (PH=3-4) is in flocculant group Poly-effect is lower can to obtain important primary purification effect (filter, [6]). For example, purity is 99% rare earth oxide and the reaction of technical grade red fuming nitric acid (RFNA), lysate is through concentrating and filtration, purification (filtration Device, [8]) the rear rare earth nitrate that obtains, its concentration can improve a magnitude, and namely purity is 99.9% More than.
The reduction vaporization that the present invention proposes and concentrated-filtration method have not only reduced evaporating temperature, by Normal pressure is lower more than 100 ℃, is reduced to 61-76 ℃, and the double purification that can obtain to replenish effect Really.
The crystal seed induced crystallization method that the present invention proposes, its crystal seed is high degree of supersaturation (crystal solution ratio Heavily be more than 1.8) micro crystal that generates under the condition, its addition is rare earth nitrate to be crystallized 1% of amount.
Important characteristic of the present invention and effect are: the dissolving of (1) differential rather than prior art-integration Dissolving; (2) important primary purification effect has been received in flocculation-filter; (3) concentrate-filter, receive The secondary supplement clean-up effect. Twice clean-up effect not only is better than the effect that repeatedly is recrystallized, and Solved the routine techniques difficult problem of special processing crystalline mother solution. (4) crystal seed induced crystallization adopts little Thin crystal seed is not only accelerated the brilliant speed of burl, and is conducive to improve the purity of product.
Embodiment 1
Take by weighing Y
2O
3(.99%) 100 grams after water-wet, drop in the rare nitric acid of heat (80 ℃) (by the dense HNO of 92.3ml in the differential mode
3(23mol/l) and 92.3mlH
2Rare nitric acid that O forms) dissolving, (the pale brown look of solution) filters when treating PH=3-4, filter cake dropped into hot rare HNO again
3In (58.1ml HNO
3/ 58.1mlH
2O, 80 ℃), filter when treating PH=3-4, when treating PH=3-4, dissolving finishes again filter cake to be dropped in the hot dilute nitric acid solution (16.6ml/16.6ml) in the differential mode.The concentrated nitric acid gross weight that three dissolvings are consumed is 179ml.
Merge three times filtrate, be evaporated to 163ml, filter and be cooled to room temperature (＜20 ℃), drop into 1% crystal seed (crystallite), filter 255.3 gram crystal, be evaporated to 22ml more successively, 10ml, respectively crystal 42 grams, 20 grams add up to make crystal 3 17.3 grams.
Embodiment 2
Take by weighing La
2O
3(99.9%) 500 gram, behind water infiltration, drop into hot rare nitric acid (676ml, 7.44mol/l successively in the differential mode, 70 ℃) in, when treating that solution acidity is reduced to PH=3-4, solution is filtered, filtrate gives over to concentrated, filter cake drops into (360ml in second part of hot dilute nitric acid solution in the differential mode, 7.44mol/l, 80 ℃), when treating that solution acidity is reduced to PH=3-4, solution is filtered, filtrate gives over to concentrated, and filter cake drops into (120ml, 7.44mol/l in the 3rd part of hot dilute nitric acid solution in the differential mode again, 78 ℃), after treating to dissolve fully, solution is filtered, filtrate gives over to concentrated.
The cumulative volume of three filtrates is 1450ml.Evaporation--be concentrated into the 765ml postcooling to room temperature (＜20 ℃), add crystal seed, slowly mix and stir after-filtration and get crystal 8225 gram, filtrate continuation is concentrated into the 436ml postcooling to room temperature, adds crystal seed 2% and leads and lure crystallization, and crystal solution is filtered, and obtains crystal 2 75.4 grams; Filtrate is continued evaporation concentration to 54ml, is cooled to room temperature, adds crystal seed 2% induced crystallization, and crystal solution is filtered, and obtains crystal 6 6.1 grams.Three crystal gross weights are 1164 grams.By the crystallization re-computation, meet chemical formula: La (NO
3)
33H
2O.
Embodiment 3
Take by weighing cerous carbonate and (contain CeO
2, 48%) and 100 grams, behind water infiltration, add (98ml, 7.44mol/l, 80 ℃) in the hot dilute nitric acid solution in the differential mode, when treating that solution acidity is reduced to PH=3-4, solution to be filtered, filtrate reservation, wait to concentrate; Filter cake adds (22ml, 7.44mol/l, 80 ℃) in hot rare nitric acid in the differential mode again, treats to dissolve fully after-filtration.
Merge twice filtrate and carry out evaporation concentration, after treating that liquor capacity arrives 50ml, be cooled to room temperature (＜20 ℃), drop into 1% crystal seed, slowly stir, after the growth crystallization, filter to such an extent that crystal 6 5.9 restrains, crystal keeps makes product, the filtrate revaporization, arrive the 15ml postcooling to room temperature to liquor capacity, drop into seeded crystallization and filter, crystal 15.5 grams; Filtrate continuation is evaporated to volume 8ml, and crystallisation by cooling also filters to such an extent that crystal 13.5 restrains, and three crystallizations are totally 94.9 grams.
Claims (1)
1, a kind of method for preparing rare earth nitrate, wherein rare earth element comprises yttrium, lanthanum and cerium, its operation comprises:
A, dissolving: the rare earth compound material powder after will soaking adds in the dilute nitric acid solution of theoretical amount in batches and dissolves, filter, the starting point concentration of each lysate keeps more than the 7.5mol/l, temperature 70-80 ℃, continuously stirring, the dissolving release sequence is respectively 55%, 35% and 10% of total nitric acid amount;
B, concentrated: the lysate that three dissolvings are made merges, evaporation under reduced pressure, and to make supersaturated solution, between vaporization temperature 50-100 ℃, the density of final evaporated liquor surpasses 1.6g/cm
3
C, crystallization: adopt fractional crystallization, the cooling supersaturated solution is to room temperature, and to wherein dropping into crystal seed, each crystal seed amount of throwing in is the 1-3% of crystal amount in the supersaturated solution body, stirs at a slow speed;
D, filtration: filter the supersaturation rare earth nitrate solution, the white crystal that makes, promptly rare earth nitrate after mother liquor secondary concentration and the crystallization, concentrates and crystallization more for the third time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121934A CN1074751C (en) | 1997-11-21 | 1997-11-21 | Production method of rare earth nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121934A CN1074751C (en) | 1997-11-21 | 1997-11-21 | Production method of rare earth nitrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1218007A CN1218007A (en) | 1999-06-02 |
| CN1074751C true CN1074751C (en) | 2001-11-14 |
Family
ID=5176553
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97121934A Expired - Fee Related CN1074751C (en) | 1997-11-21 | 1997-11-21 | Production method of rare earth nitrate |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976388A (en) * | 2011-09-07 | 2013-03-20 | 中国石油大学(华东) | Method for hydrothermal preparation of rare earth nitrates |
| US20140356259A1 (en) * | 2013-05-30 | 2014-12-04 | Nano And Advanced Materials Institute Limited | Selective Separation of Rare Earth Metals by Integrated Extraction and Crystallization |
| CN104030330B (en) * | 2014-06-14 | 2017-01-18 | 中国科学院过程工程研究所 | Method for preparing high-purity aluminum hydroxide through induced crystallization |
| CN105776307B (en) * | 2016-02-05 | 2018-05-01 | 四川省新材料研究中心 | The pre-treating method that a kind of rare earth oxide isolates and purifies |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4231997A (en) * | 1979-04-05 | 1980-11-04 | Engelhard Minerals & Chemicals Corporation | Preparation of rare earth nitrates |
-
1997
- 1997-11-21 CN CN97121934A patent/CN1074751C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4231997A (en) * | 1979-04-05 | 1980-11-04 | Engelhard Minerals & Chemicals Corporation | Preparation of rare earth nitrates |
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| Publication number | Publication date |
|---|---|
| CN1218007A (en) | 1999-06-02 |
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