CN101607731B - A kind of rear-earth-doped sodium aluminum fluoride and preparation method thereof - Google Patents
A kind of rear-earth-doped sodium aluminum fluoride and preparation method thereof Download PDFInfo
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- CN101607731B CN101607731B CN200810115199.7A CN200810115199A CN101607731B CN 101607731 B CN101607731 B CN 101607731B CN 200810115199 A CN200810115199 A CN 200810115199A CN 101607731 B CN101607731 B CN 101607731B
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Abstract
The present invention relates to a kind of rear-earth-doped sodium aluminum fluoride and preparation method thereof.Utilize and prepare a kind of rear-earth-doped sodium aluminum fluoride containing the fluorine aluminium complex solution of rare earth element or fluoride aqueous solution.The sodium aluminum fluoride utilizing the method to obtain contains at least one in rare-earth elements of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium, ree content with oxide basis for 0.01 ~ 5.0wt%.The present invention is relative to Process of Producing Cryolite in the past, and its feature is, (1) this sodium aluminum fluoride adulterates a small amount of rare earth, as the fusing assistant of aluminium metallurgy, decreases rare earth and adds step, cost-saving, reduces operation; (2) the method technique is simple, is easy to manipulation; (3) waste liquid utilizing extracting and separating rear earth, fluorine process to produce prepares sodium aluminum fluoride, solves the problem of fluoride waste contaminate environment, can turn waste into wealth, and has good economic benefit, environmental benefit and social benefit.
Description
Technical field
The present invention relates to a kind of rear-earth-doped sodium aluminum fluoride and preparation method thereof; the method discloses the method utilizing and prepare rear-earth-doped sodium aluminum fluoride containing the fluorine aluminium complex solution of rare earth element or fluoride aqueous solution; this solution can be the aluminium salt complex solution or fluoride aqueous solution that produce in rare-earth smelting sepn process, and this method belongs to environment protection and resource recycling field.
Technical background
The chemical name of sodium aluminum fluoride is sodium fluoroaluminate, and molecular formula is Na
3alF
6, the main fusing assistant being used as electrolysis of aluminum, the wear-resistant filler of rubber, emery wheel, the opacifier of enamel, the opalizer of glass and metal solvent etc.At present, aluminum smelting industry mainly uses cryolith in the world, and adds a small amount of rare earth element in aluminium metallurgy process.The traditional processing technology of cryolith is soda ash---hydrofluoaluminic acid method, this method is first reacted with hydrofluoric acid and aluminium hydroxide and is generated hydrofluoaluminic acid, then reacts with hydrofluoaluminic acid and soda ash and generate sodium aluminum fluoride.But this method exists, and investment is large, cost is high, complicated operation and the production of raw-material manufacture and product has the shortcomings such as serious environmental pollution.
The technical scheme preparing sodium aluminum fluoride disclosed in Chinese invention patent prospectus has: utilize the by product producing molecular sieve to prepare the method (publication number 1085523) of sodium aluminum fluoride, raffinate extracted from smelting columbite-tantalite ore is utilized to produce the technique (publication number 1686841) of sodium fluoroaluminate, the method (publication number 1522962) of manufacturing sodium aluminium fluoride by pickling aluminium slag, the method (publication number 1332118) of sodium aluminum fluoride is produced with fluoride waste, above patent is all that utilize some technique to produce liquid and waste slag produced prepares sodium aluminum fluoride, namely cost-saving, simple to operate, decreasing pollution, create economic worth again.
Summary of the invention
The object of the invention is to utilize and prepare a kind of rear-earth-doped sodium aluminum fluoride containing the fluorine aluminium complex solution of rare earth element or fluoride aqueous solution, and the production method providing a kind of technique simple, easy to operate, with low cost, low in the pollution of the environment.Containing rare-earth elements of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, at least one in yttrium in the sodium aluminum fluoride product utilizing the method to obtain, ree content with oxide basis for for 0.01 ~ 5.0wt%.Sodium aluminum fluoride Rare Earth Element Contents is with oxide basis preferably 0.05 ~ 1.0wt%.
For achieving the above object, sodium aluminum fluoride undertaken precipitating by original liquid and sodium salt or with aluminium salt, sodium salt and trace rare-earth with certain hybrid mode mixed precipitation.In order to keep feed acidity to be 0.0001 ~ 0.1mol/L, adding concentration is 0.1 ~ 6mol/L ammoniacal liquor, NaOH, NH
4hCO
3, NaHCO3, Na
2cO
3in at least one regulate feed acidity.Hybrid mode is for add fluorine-containing solution, earth solution, sodium salt solution and aluminum salt solution simultaneously, or add according to sodium salt solution, earth solution, fluorine-containing solution, aluminum salt solution order, or add according to sodium salt solution, aluminum salt solution, earth solution, fluorine-containing solution order.Precipitin reaction is carried out at the temperature of 20 ~ 150 DEG C, and standing filtration is precipitated product; Then dry at 60 ~ 200 DEG C of temperature, obtain rear-earth-doped sodium aluminum fluoride.
Wherein containing the fluorine aluminium complex solution of rare earth element, except containing except rare earth element, fluorine aluminium complex and aluminum ion, also containing SO
4 2-, NO
3 -, Cl
-in at least one.Fluorine aluminium complex is (AlFx)
3-x, more than one in 0 < x≤6, concentration is 0.05 ~ 1mol/L.And sodium salt is NaOH, Na
2cO
3, NaHCO
3, Na
2sO
4, NaCl, NaF, NaNO
3in at least one, concentration is 0.05 ~ 2.0mol/L.
Advantage of the present invention
Relative to Process of Producing Cryolite in the past, its feature is, (1) this sodium aluminum fluoride adulterates a small amount of rare earth, as the fusing assistant of aluminium metallurgy, decreases rare earth and adds step, cost-saving, reduces operation; (2) the method technique is simple, is easy to manipulation; (3) waste liquid utilizing extracting and separating rear earth, fluorine process to produce, solves the problem of fluoride waste exhaust emission environment, can turn waste into wealth, and has good economic benefit, environmental benefit and social benefit.
Embodiment
Embodiment 1:
Raw material: containing the fluorine aluminium complex solution 200ml of rare earth element, wherein aluminium ion concentration is 0.1mol/L, the existence form of fluorine aluminium complex is (AlF
6)
3-, rare earth element concentration is 10
-5mol/L, Na ion concentration is the NaCl solution 200ml of 0.3mol/L.
Fluorine aluminium complex solution containing rare earth element is heated to 70 DEG C, adds a small amount of sodium aluminum fluoride crystal seed, slowly add NaCl solution uniformly, and in 30min, be at the uniform velocity warming up to 92 DEG C ± 2 DEG C; Feed time is 60min; Continue to stir 30min after reinforced end; Leave standstill and filter, obtain precipitated product; Be placed on dry 2 ~ 4h in the baking oven of 105 DEG C, obtain rear-earth-doped sodium aluminum fluoride, content of rare earth is by REO about 0.01wt%.
Embodiment 2:
Raw material: containing the fluorine aluminium complex solution 200ml of rare earth element, wherein aluminium ion concentration is 0.1mol/L, the existence form of fluorine aluminium complex is (AlF
6)
3-, rare earth element concentration is 10
-3mol/L, Na ion concentration is the NaHCO of 0.3mol/L
3solution 200ml.
Fluorine aluminium complex solution containing rare earth element is heated to 70 DEG C, adds a small amount of sodium aluminum fluoride crystal seed, slowly add NaHCO uniformly
3solution, and in 30min, be at the uniform velocity warming up to 92 DEG C ± 2 DEG C; Feed time is 60min; Continue to stir 30min after reinforced end; Leave standstill and filter, obtain precipitation; Be placed on dry 2 ~ 4h in the baking oven of 105 DEG C, obtain rear-earth-doped sodium aluminum fluoride, content of rare earth is by REO about 0.8wt%.
Embodiment 3:
Raw material: containing the fluorine aluminium complex solution 200ml of rare earth element, wherein aluminium ion concentration is 0.05mol/L, the existence form of fluorine aluminium complex is (AlF
6)
3-, rare earth element concentration is 10
-4mol/L, Na ion concentration is the Na of 0.151mol/L
2sO
4solution 200ml.
Fluorine aluminium complex solution containing rare earth element is heated to 70 DEG C, adds a small amount of sodium aluminum fluoride crystal seed, slowly add Na uniformly
2sO
4solution, and in 30min, be at the uniform velocity warming up to 92 DEG C ± 2 DEG C; Feed time is 60min; Continue to stir 30min after reinforced end; Leave standstill and filter, obtain precipitation; Be placed on dry 2 ~ 4h in the baking oven of 105 DEG C, obtain rear-earth-doped sodium aluminum fluoride, content of rare earth is by REO about 0.15wt%.
Embodiment 4:
Raw material: containing the fluorine aluminium complex solution 200ml of rare earth element, wherein aluminium ion concentration is 0.5mol/L, the existence form of fluorine aluminium complex is (AlF
6)
3-, rare earth element concentration is 10
-2mol/L, Na ion concentration is the Na of 1.51mol/L
2cO
3solution 400ml.
Fluorine aluminium complex solution containing rare earth element is heated to 70 DEG C, adds a small amount of sodium aluminum fluoride crystal seed, slowly add Na uniformly
2cO
3solution, and in 30min, be at the uniform velocity warming up to 92 DEG C ± 2 DEG C; Feed time is 60min; Continue to stir 30min after reinforced end; Leave standstill and filter, obtain precipitation; Be placed on dry 2 ~ 4h in the baking oven of 105 DEG C, obtain rear-earth-doped sodium aluminum fluoride, content of rare earth is by REO about 1.5wt%.
Embodiment 5:
Raw material: containing the fluorine aluminium complex solution 200ml of rare earth La Ce enriched substance, wherein aluminium ion concentration is 0.1mol/L, the existence form of fluorine aluminium complex is AlF
3, rare earth element concentration is 10
-3mol/L, 0.302mol/L NaF solution 200ml.
Fluorine aluminium complex solution containing rare earth element is heated to 70 DEG C, adds a small amount of sodium aluminum fluoride crystal seed, slowly add NaF solution uniformly, and in 30min, be at the uniform velocity warming up to 92 DEG C ± 2 DEG C; Feed time is 60min; Continue to stir 30min after reinforced end; Leave standstill and filter, obtain precipitation; Be placed on dry 2 ~ 4h in the baking oven of 105 DEG C, obtain rear-earth-doped sodium aluminum fluoride, content of rare earth is by REO about 0.8wt%.
Embodiment 6:
0.6mol/L Fluorinse is added a small amount of LaCl
3, obtaining rare earth element concentration is 10
-3the solution 200ml of mol/L, Al
3+concentration is the Al of 0.2mol/L
2(SO
4)
3solution 200ml, concentration is the HF solution 60ml of 2mol/L.Slowly add above several solns simultaneously, and in 30min, be at the uniform velocity warming up to 92 DEG C ± 2 DEG C, add a small amount of sodium aluminum fluoride crystal seed; Feed time is 60min; Continue to stir 30min after reinforced end; Leave standstill and filter, obtain precipitation; Be placed on dry 2 ~ 4h in the baking oven of 105 DEG C, obtain rear-earth-doped sodium aluminum fluoride, content of rare earth is by REO about 0.4wt%.
Embodiment 7:
Raw material: containing the fluorine aluminium complex solution 200ml of rare earth La Ce enriched substance, wherein aluminium ion concentration is 0.1mol/L, the existence form of fluorine aluminium complex is 50%AlF
3with 50% (AlF
2)
+, rare earth element concentration is 10
-3mol/L, 0.302mol/L NaF solution 200ml, 2mol/L HF solution 4.8ml.
Fluorine aluminium complex solution containing rare earth element is heated to 70 DEG C, adds a small amount of sodium aluminum fluoride crystal seed, slowly add HF solution, NaF solution uniformly, and in 30min, be at the uniform velocity warming up to 92 DEG C ± 2 DEG C; Feed time is 60min; Continue to stir 30min after reinforced end; Leave standstill and filter, obtain precipitation; Be placed on dry 2 ~ 4h in the baking oven of 105 DEG C, obtain rare earth doped sodium aluminum fluoride, content of rare earth is by REO about 0.8wt%.
Embodiment 8:
Add ammonium hydroxide by containing in the fluorine aluminium complex solution of rare earth element, make 0.6mol/L ammonium fluoride solutions, Al
3+concentration is the Al of 0.1mol/L
2(SO
4)
3solution 200ml, Na
+concentration is the Na of 0.3mol/L
2sO
4solution 200ml and 10
-2the rare earth element 200ml of mol/L.Above several solns is slowly added simultaneously, and in 30min, is at the uniform velocity warming up to 92 DEG C ± 2 DEG C, add a small amount of sodium aluminum fluoride crystal seed; Feed time is 60min; Continue to stir 30min after reinforced end; Leave standstill and filter, obtain precipitation; Be placed on dry 2 ~ 4h in the baking oven of 105 DEG C, obtain rear-earth-doped sodium aluminum fluoride, content of rare earth is by REO about 5.0wt%.
Embodiment 9:
Raw material: containing the fluorine aluminium complex solution 200ml of rare earth element, wherein aluminium ion concentration is 0.1mol/L, the existence form of fluorine aluminium complex is (AlF
6)
3-, rare earth element concentration is 10
-3mol/L, acidity are 0.3mol/L, and Na ion concentration is the NaOH solution 200ml of 0.3mol/L.
By the NaOH solution of 6mol/L, the acidity of the fluorine aluminium complex solution containing rare earth element is adjusted to 0.1mol/L, is heated to 70 DEG C, adds a small amount of sodium aluminum fluoride crystal seed, slowly add NaOH solution uniformly, and in 30min, be at the uniform velocity warming up to 92 DEG C ± 2 DEG C; Feed time is 60min; Continue to stir 30min after reinforced end; Leave standstill and filter, obtain precipitation; Be placed on dry 2 ~ 4h in the baking oven of 105 DEG C, obtain rear-earth-doped sodium aluminum fluoride, content of rare earth is by REO about 0.80wt%.
Embodiment 10:
Raw material: containing the fluorine aluminium complex solution 200ml of rare earth element ce, wherein aluminium ion concentration is 0.1mol/L, the existence form of fluorine aluminium complex is (AlF
6)
3-, rare earth element concentration is 10
-3mol/L, acidity are the solution of 0.2mol/L, and Na ion concentration is the NaNO of 0.3mol/L
3solution 200ml.
With the ammoniacal liquor of 6mol/L, the acidity of the fluorine aluminium complex solution containing rare earth element is adjusted to 0.001mol/L, is heated to 70 DEG C, adds a small amount of sodium aluminum fluoride crystal seed, slowly add NaNO uniformly
3solution, and in 30min, be at the uniform velocity warming up to 92 DEG C ± 2 DEG C; Feed time is 60min; Continue to stir 30min after reinforced end; Leave standstill and filter, obtain precipitation; Be placed on dry 2 ~ 4h in the baking oven of 105 DEG C, obtain rear-earth-doped sodium aluminum fluoride, content of rare earth is by REO about 0.80wt%.
Claims (8)
1. a rear-earth-doped sodium aluminum fluoride, it is characterized in that, described sodium aluminum fluoride contains at least one in rare-earth elements of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium, ree content with oxide basis for 0.01 ~ 5.0wt%.
2. a kind of rear-earth-doped sodium aluminum fluoride according to claim 1, is characterized in that, sodium aluminum fluoride Rare Earth Element Contents is with oxide basis preferably 0.05 ~ 1.0wt%.
3. a preparation method for rear-earth-doped sodium aluminum fluoride according to claim 1, is characterized in that, preparation process comprises following key step:
(1) fluorine aluminium complex solution and sodium salt carry out precipitating or fluoride aqueous solution and sodium salt, aluminium salt and trace rare-earth with certain feed way mixed precipitation, described fluorine aluminium complex solution contains trace rare-earth element, fluorine aluminium complex, aluminum ion and acid ion;
(2) leave standstill filtration, be precipitated product;
(3) aftertreatment obtains rear-earth-doped sodium aluminum fluoride.
4. the preparation method of a kind of rear-earth-doped sodium aluminum fluoride according to claim 3, is characterized in that, in original liquid, fluorine aluminium complex is (AlF
x)
3-x, more than one in 0 < x≤6, fluorine aluminium complex concentration is 0.05-1mol/L.
5. the preparation method of a kind of rear-earth-doped sodium aluminum fluoride according to claim 3, is characterized in that, before step (1), adding concentration is 0.1-6mol/L ammoniacal liquor, NaOH, NH
4hCO
3, NaHCO
3, Na
2cO
3in at least one regulate feed acidity, feed acidity is 0.0001-0.1mol/L.
6. the preparation method of a kind of rear-earth-doped sodium aluminum fluoride according to claim 3, it is characterized in that, feed way is for add fluorine-containing solution, earth solution, sodium salt solution and aluminum salt solution simultaneously, or add according to sodium salt solution, earth solution, fluorine-containing solution, aluminum salt solution order, or add according to sodium salt solution, aluminum salt solution, earth solution, fluorine-containing solution order.
7. the preparation method of a kind of rear-earth-doped sodium aluminum fluoride according to claim 3, it is characterized in that, sodium salt is Na
2cO
3, NaHCO
3, Na
2sO
4, NaCl, NaF, NaNO
3in at least one, the concentration of sodium ion is 0.05-2.0mol/L.
8. the preparation method of a kind of rear-earth-doped sodium aluminum fluoride according to claim 3, it is characterized in that, precipitin reaction is carried out at 20-150 DEG C of temperature, dry under being deposited in 60-200 DEG C of temperature.
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| CN101177309A (en) * | 2007-11-16 | 2008-05-14 | 北大方正集团有限公司 | Method for comprehensive recovery and utilization of fluorine-containing alkali waste water and saponification of extracting agent |
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| 于旭光 等.熔盐电解制备稀土铝合金的研究.《稀土》.2006,第27卷(第6期),33-36. * |
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Effective date of registration: 20181107 Address after: 614300 No. 13, Yang Zhu Ba Road, Ebian Yi Autonomous County, Leshan City, Sichuan Patentee after: Leshan research rare earth new material Co Ltd Address before: 100088, 2, Xinjie street, Beijing Patentee before: Grirem Advanced Materials Co., Ltd. |
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