CN108910949A - The preparation method of high-purity potassium floutaramite - Google Patents
The preparation method of high-purity potassium floutaramite Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of high-purity potassium floutaramite.Its main feature is that including the following steps：(1) it decomposes：Tantalum niobium concentrate object is added into hydrofluoric acid and sulfuric acid and is decomposed；(2) sludge extraction：Counter-current extraction is carried out using MIBK solvent or sec-octyl alcohol solvent, fluorine niobic acid and fluorotantalic acid are extracted in solvent；(3) pickling：It is contacted using the solvent obtained after sulfuric acid solution adverse current and step (2) extraction；(4) anti-niobium mentions tantalum：Using sulfuric acid solution and obtained solvent in extraction tank counter-current extraction, fluorine niobic acid is extracted into water phase, forms fluorine niobic acid aqueous solution；(5) anti-tantalum：By remaining organic solution in another extraction tank, fluorotantalic acid organic solution is stripped into pure water using pure water, forms fluorotantalic acid aqueous solution；(6) it synthesizes：(7) crystallisation by cooling.The present invention provides a kind of methods that high-purity fluorine potassium tantalate is prepared in segmentation back extraction and fractional crystallizaton method, can effectively remove the impurity in potassium floutaramite.
Description
Technical field
The present invention relates to a kind of preparation methods of high-purity potassium floutaramite.
Background technique
In present tantalum niobium metallurgy, classical potassium floutaramite preparation process has been formd.It is exactly to be added using ore
Hydrofluoric acid, tantalum niobium is resolved into fluorotantalic acid, and perhaps fluorine niobic acid utilizes the fluorine niobium in MIBK or sec-octyl alcohol solution extraction aqueous solution
Acid or fluorotantalic acid, using Low acid sulfuric acid further remove load tantalum niobium it is organic in impurity, be using hydrogen ion concentration
The sulfuric acid solution back extraction load tantalum niobium organic solution of 1.2-1.6mol/L, fluorine niobic acid enter in acid solution.Reach with it is organic molten
The purpose that fluorotantalic acid separates in liquid.Organic solution containing fluorotantalic acid enters in anti-tantalum process, and it is molten to do back extraction using pure water
Fluorotantalic acid solution is stripped into pure water by liquid, forms fluorotantalic acid solution, then again by this fluorotantalic acid solution heating (92
Degree) it hydrofluoric acid and potassium chloride is added afterwards has obtained potassium floutaramite crystal by being cooled to 15 degree.
But the main problem of this technique is, the purity of the potassium floutaramite of preparation is limited.It is being used for the pure tantalum of sputtering target material
Metal needs purity height 99.9999%, and tungsten therein, molybdenum, the refractory metals such as niobium are main impurity elements, if
The change that cannot be removed during production potassium floutaramite, is difficult to remove in subsequent production process.Purity must be prepared thus
Very high potassium floutaramite, which just can guarantee, prepares high-purity tantalum metal.In prior art, the primary anti-tantalum operation generallyd use,
Trace niobium in solution, micro tungsten can enter in product.The single crystallization that technique also uses at present, part of impurity elements
The crystallization easy to form of the elements such as silicon, niobium crystallizes together with potassium floutaramite, the patent report that Chinese Patent Application No. is 02801094.9
A kind of high-purity fluorine potassium tantalate crystal in road or the manufacturing method of high-purity fluorine potassium niobate crystallization, but act the method used and only exist
Achieve the purpose that particle is uniform using different cooling rates in different sections, do not refer to how to remove it is miscellaneous in potassium floutaramite
Matter.Application number：The Chinese patent of 201110316023.X but this method main problem, imitate the extraction of the impurity such as niobium
Fruit is limited.Higher boiling metal such as tungsten in product containing part, molybdenum etc., content is generally all in 0.5-10.0ppm or so.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of high-purity potassium floutaramite, can obtain the very low height of impurity element
Pure potassium floutaramite.
A kind of preparation method of high-purity potassium floutaramite, its special feature is that, include the following steps：
(1) it decomposes：Tantalum niobium concentrate object is added into hydrofluoric acid and sulfuric acid and is decomposed；
(2) sludge extraction：Counter-current extraction is carried out using MIBK solvent or sec-octyl alcohol solvent, fluorine niobic acid and fluorotantalic acid are extracted
It takes into solvent；
(3) pickling：It is contacted using the solvent obtained after sulfuric acid solution adverse current and step (2) extraction；
(4) anti-niobium mentions tantalum：Using sulfuric acid solution and obtained solvent in extraction tank counter-current extraction, fluorine niobic acid is extracted to water phase
In, form fluorine niobic acid aqueous solution；
(5) anti-tantalum：By remaining organic solution in another extraction tank, fluorotantalic acid organic solution is stripped using pure water
Into pure water, fluorotantalic acid aqueous solution is formed；
(6) it synthesizes：Potassium chloride and hydrofluoric acid will be added after the heating of obtained fluorotantalic acid aqueous solution；
(7) crystallisation by cooling：Potassium floutaramite crystal will be obtained after Synthesis liquid cooling, is centrifuged, drying obtains high-purity potassium floutaramite
Crystal.
Step (5) specifically uses two sections of anti-tantalums, and it is 0.05-0.6mol/ that the anti-tantalum liquid of the anti-tantalum of first segment, which is hydrogen ion concentration,
Sulfuric acid, hydrochloric acid or the hydrofluoric acid solution of L, the anti-tantalum liquid of the anti-tantalum of second segment are pure water, and using the anti-tantalum liquid of second segment as
The raw material of step (6) synthesis potassium floutaramite.
Step (7) specifically uses three-stage cooling, and the cooling temperature for controlling first segment is 70-80 DEG C, then that first segment is cold
But the liquid after is put into second segment cooling, and the crystallization obtained after first segment cooling is collected, and the cooling temperature for controlling second segment is
40 DEG C -70 DEG C, then the liquid that second segment obtains after cooling is put into three-stage cooling, is obtained after collection second segment is cooling
Crystallization, the cooling temperature of control third section are 10 DEG C -40 DEG C, collect the crystallization obtained after three-stage cooling, cold using second segment
But the potassium floutaramite obtained afterwards, which is carried out again one time recrystallization, be added pure water in, and be added high-pure hydrofluoric acid and
High purity potassium chloride finally obtains high-purity potassium floutaramite.
Anti- tantalum extraction in step (5) is to extract at 8 grades into 12 stage countercurrent extraction tanks.
The flow-rate ratio of control extraction organic solvent and strippant is 1 in step (5)：2 to 3：1.
Rotating speed of agitator is controlled in step (7) in cooling bath to turn for 30-90 per minute.
The anti-tantalum liquid acidity of control is 0.05-0.6mol/L in step (5).
The sulfuric acid, hydrochloric acid or hydrofluoric acid that the anti-tantalum liquid of second segment is hydrogen ion concentration 0.05-0.6mol/L in step (5) are molten
Liquid.
The anti-tantalum liquid of second segment controls filtering accuracy less than 0.1 micron by precision filtration equipment in step (5).
Further：
(1) tantalum niobium concentrate mountain flour is broken to no more than 200 mesh, is added into hydrofluoric acid, then add sulfuric acid, heat preservation is decomposed；
(2) extract in slot then into mine, using MIBK solvent or sec-octyl alcohol solvent extraction tantalum niobium, to make fluorotantalic acid
It is entered in solvent with fluorine niobic acid, recycles the sulfuric acid of 3.7-4.2mol/L counter-current extraction in descaling bath, make later containing tantalum
The organic solvent of niobium enters anti-niobium and mentions in tantalum slot, the sulfuric acid solution using 0.6-0.8mol/L and the organic solvent containing tantalum niobium
Counter-current extraction；
(3) obtained fluorine niobic acid solution is entered in sulfuric acid solution, and obtained fluorotantalic acid solution is stayed in organic molten
In agent；
(4) organic solvent containing fluorotantalic acid has been entered in anti-tantalum extraction tank, using 12 grades of anti-tantalum slots as
One section of back extraction groove body, using hydrogen ion concentration is the sulfuric acid of 0.05-0.6mol/L, hydrochloric acid or hydrofluoric acid solution as first
Then the anti-tantalum agent of section recycles the back extraction groove body of 12 grades of anti-tantalum slot as second segment, using pure water as strippant,
The fluorotantalic acid solution of second segment is obtained, for use；
(5) hydrofluoric acid and potassium chloride is added in obtained fluorotantalic acid solution, is heated to 92 DEG C or more and keeps the temperature half an hour,
It is put into first cooling bath, is cooled to 70 DEG C -80 DEG C, then solution is put into second cooling bath, is cooled to 40
DEG C -70 DEG C, finally solution is put into third cooling bath, is cooled to 10 DEG C -40 DEG C degrees Celsius；Collect second cooling bath
In potassium floutaramite crystallization, be then added into pure water, be warming up to 92 DEG C or more, hydrofluoric acid and potassium chloride is added, dissolve fluorine
It after potassium tantalate crystal, is put into cooling bath and crystallizes, collect potassium floutaramite crystal, centrifugation is dried to get the fluorotantalic acid of high-purity is arrived
Potassium solid.
The present invention provides a kind of methods that high-purity fluorine potassium tantalate is prepared in segmentation back extraction and fractional crystallizaton method, can
To effectively remove the impurity in potassium floutaramite.
Specific embodiment
The method of the present invention is specific as follows：
Tantalum niobium concentrate mountain flour is broken to 200 mesh first or hereinafter, sulfuric acid into hydrofluoric acid, is then added in addition, heat preservation is decomposed,
It enters in mine extraction slot, using MIBK, perhaps sec-octyl alcohol solution extraction tantalum niobium fluorotantalic acid and fluorine niobic acid enter MIBK or secondary
In octanol, the sulfuric acid of 3.7-4.2mol/L counter-current extraction in descaling bath is recycled, the organic solvent containing tantalum niobium is entered
Anti- niobium mentions in tantalum slot, uses acidity for the sulfuric acid solution of 0.6-0.8mol/L and the organic solvent counter-current extraction containing tantalum niobium.
Obtained fluorine niobic acid solution is entered in sulfuric acid solution, fluorotantalic acid then continues to stay in organic solvent, contains fluorine
The organic solvent of tantalic acid has entered in anti-tantalum extraction tank, using 12 grades of anti-tantalum slots as back extraction groove body for the first time, uses
The sulfuric acid or hydrochloric acid or hydrofluoric acid solution that hydrogen ion concentration is 0.05-0.6mol/L, as the anti-tantalum agent of first segment, then
It is anti-to obtain the second level using pure water as strippant as secondary back extraction groove body using 12 grades of anti-tantalum slot
The potassium floutaramite solution of tantalum, and use this solution as the raw material of high-purity potassium floutaramite.Then obtained fluorotantalic acid solution is added
Enter hydrofluoric acid and potassium chloride, is heated to 92 DEG C of heat preservation half an hours, is put into first cooling bath, is cooled to 70 DEG C, then
Solution is put into second cooling bath, is cooled to 40 DEG C, solution is put into third cooling bath, it is Celsius to be cooled to 15
Degree.The potassium floutaramite crystallization in second cooling bath is collected, is then added into pure water, is warming up to 92 DEG C or more, hydrogen fluorine is added
Acid and potassium chloride are put into cooling bath and crystallize after dissolving potassium floutaramite crystal, collect potassium floutaramite crystal, are centrifuged, and drying obtains
The potassium floutaramite solid of high-purity is arrived.
As a preferred solution of the present invention, anti-tantalum extraction is to extract at 8 grades into 12 stage countercurrent extraction tanks.
The anti-tantalum as a preferred solution of the present invention, extracting organic flow-rate ratio with strippant is 1：2 to 3：1.
The crystallisation by cooling as a preferred solution of the present invention, in cooling bath, rotating speed of agitator is 30-90 per minute
Turn.
The anti-tantalum liquid acidity is 0.05-0.6mol/L, preferably acidity 0.1- as a preferred solution of the present invention
Between 0.5mol/L.
It is 0.05-0.6mol/L's that the anti-tantalum liquid of second segment, which is hydrogen ion concentration, as a preferred solution of the present invention
Sulfuric acid or hydrochloric acid perhaps hydrofluoric acid solution selection be high-purity sulfuric acid or hydrochloric acid or hydrofluoric acid solution.
As a preferred solution of the present invention, the anti-tantalum liquid of second segment is by precision filtration equipment, and filtering accuracy is less than 0.1
Micron.
Embodiment 1：
1000kg tantalum niobium concentrate stone (tantalum oxide 30%, niobium oxide 20%) is crushed to 200 mesh, is added to 1700L matter
In the hydrofluoric acid for measuring percent concentration 55%, the sulfuric acid of 400L mass percent concentration 92% is then added, heat preservation is decomposed.
It enters in mine extraction slot, extracts tantalum niobium using MIBK solution, enter fluorotantalic acid and fluorine niobic acid in MIBK, then benefit
With the sulfuric acid of 3.7mol/L in descaling bath counter-current extraction, the organic solvent containing tantalum niobium is entered into anti-niobium after extraction and mentions tantalum slot
In, use acidity for the sulfuric acid solution of 0.75mol/L with containing tantalum niobium organic solvent carry out counter-current extraction, fluorine niobic acid solution into
Enter into sulfuric acid solution, fluorotantalic acid then continues to stay in organic solvent.
Organic solvent containing fluorotantalic acid is entered in anti-tantalum extraction tank, using 12 grades of anti-tantalum slots as the first time
It is stripped groove body, uses hydrogen ion concentration for the sulfuric acid solution of 0.1mol/L, as the anti-tantalum agent of first segment, then recycles 12
The anti-tantalum slot of grade has obtained the solution of the anti-tantalum in the second level using pure water as strippant as secondary back extraction groove body,
Take this solution 1000L as the raw material of high-purity potassium floutaramite.
Then solution is warming up to 92 DEG C, is added beyond (specially 30%) excellent pure grade quality of chemical dosage ratio 20%
Concentration is 40% hydrofluoric acid and excellent pure grade potassium chloride, is heated to 92 DEG C of heat preservation half an hours, is put into first cooling bath, cold
But to 70 DEG C, then solution is put into second cooling bath, is cooled to 40 DEG C, be finally put into solution cooling to third
In slot, it is cooled to 15 degrees Celsius.
The potassium floutaramite crystallization 20kg in second cooling bath is collected, is then added into 200L pure water, is warming up to 92 DEG C
More than, it is added beyond (specially 30%) the excellent pure grade hydrofluoric acid and excellent pure grade potassium chloride of chemical dosage ratio 20%, dissolves fluorine tantalum
It after sour potassium crystal, is put into cooling bath and crystallizes, collect potassium floutaramite crystal, be centrifuged, drying has obtained the 17kg fluorine tantalum of high-purity
Sour potassium solid.
Potassium floutaramite is analyzed, the results are shown in Table 1, purity reaches 99.9999% or more, main impurity niobium, tungsten and molybdenum element
Both less than 0.01ppm.
Table 1：
Embodiment 2：
1000kg tantalum niobium concentrate stone (tantalum oxide 30%, niobium oxide 20%) is crushed to 200 mesh hereinafter, being added extremely
In the hydrofluoric acid that 1700L mass concentration is 55%, the sulfuric acid that 400L mass concentration is 92% is then added, heat preservation is decomposed.
It enters in mine extraction slot, extracts tantalum niobium using sec-octyl alcohol solution, fluorotantalic acid and fluorine niobic acid enter in sec-octyl alcohol, benefit
With the sulfuric acid of 4.2mol/L, counter-current extraction, the organic solvent containing tantalum niobium enter anti-niobium and mention in tantalum slot in descaling bath, use
The sulfuric acid solution and the organic solvent counter-current extraction containing tantalum niobium that acidity is 0.7mol/L.
Fluorine niobic acid solution is entered in sulfuric acid solution, fluorotantalic acid then continues to stay in organic solvent, contains fluorotantalic acid
Organic solvent has entered in anti-tantalum extraction tank, using 12 grades of anti-tantalum slots as back extraction groove body for the first time, using hydrogen ion
Concentration is the sulfuric acid solution of 0.3mol/L, as the anti-tantalum agent of first segment, then recycles 12 grades of anti-tantalum slot as second
Back extraction groove body, using pure water as strippant, organic ratio with water phase is 1：1, rotating speed of agitator is 100 revolutions per minute
Clock.The solution of the anti-tantalum in the second level has been obtained, has been filtered using the filter membrane that filtering accuracy is 0.1 micron, this solution 1000L is taken to make
For the raw material of high-purity potassium floutaramite.
Then solution is warming up to 92 DEG C, is added beyond top grade hydrofluoric acid and the excellent pure grade chlorination of chemical dosage ratio 20%
Potassium is heated to 92 DEG C of heat preservation half an hours, is put into first cooling bath, is cooled to 70 DEG C, and then solution is put into
In two cooling baths, 40 DEG C are cooled to, solution is put into third cooling bath, is cooled to 15 degrees Celsius.
The potassium floutaramite crystallization 150kg in second cooling bath is collected, is then added into 200L pure water, is warming up to 92 DEG C
More than, it is added beyond the excellent pure grade hydrofluoric acid and excellent pure grade potassium chloride of chemical dose 20%, after dissolving potassium floutaramite crystal, is put into
It is crystallized in cooling bath, collects potassium floutaramite crystal, be centrifuged, drying has obtained the 143kg potassium floutaramite solid of high-purity.Analysis
Potassium floutaramite the results are shown in Table 2, and purity reaches 99.9999% or more, and main impurity niobium, tungsten and molybdenum element are both less than
0.01ppm。
Table 2：
Comparative example 1：
1000kg tantalum niobium concentrate stone (tantalum oxide 30%, niobium oxide 20%) is crushed to 200 mesh hereinafter, being added extremely
In the hydrofluoric acid of 1700L mass fraction 55%, the sulfuric acid of 400L mass fraction 92% is then added, heat preservation is decomposed.
It enters in mine extraction slot, extracts tantalum niobium using MIBK or sec-octyl alcohol solution, fluorotantalic acid and fluorine niobic acid enter
In MIBK or sec-octyl alcohol, using the sulfuric acid of 4.0mol/L, counter-current extraction, the organic solvent containing tantalum niobium enter in descaling bath
It is mentioned in tantalum slot to anti-niobium, uses acidity for the sulfuric acid solution of 0.80mol/L and the organic solvent counter-current extraction containing tantalum niobium, fluorine niobium
Acid solution enters in sulfuric acid solution, and fluorotantalic acid then continues to stay in organic solvent, and the organic solvent containing fluorotantalic acid enters
In anti-tantalum extraction tank, uses 10 grades of anti-tantalum slot rotating speed of agitator to transfer to for per minute 90 to be stripped groove body, utilize pure water
As strippant.
The solution of anti-tantalum is obtained, takes this solution 1000L as the raw material of potassium floutaramite.Then solution is warming up to 92
DEG C, excellent pure grade hydrofluoric acid and excellent pure grade potassium chloride that stoichiometric ratio is more than 20% is added, is heated to 92 DEG C of heat preservation half an hours,
It is cooled to 15 degrees Celsius.The potassium floutaramite crystallization 60kg in second cooling bath is collected, is then added into 200L pure water, heats up
To 92 DEG C or more, 40% hydrofluoric acid of excellent pure grade and 20kg excellent pure grade potassium chloride that stoichiometric ratio is more than 20% is added, dissolves fluorine
It after potassium tantalate crystal, is put into cooling bath and crystallizes, collect potassium floutaramite crystal, be centrifuged, drying has obtained the 56kg fluorine of high-purity
Potassium tantalate solid.The purity of analysis potassium floutaramite reaches 99.99% or more.
Table 3：
The present invention mainly uses multistage extraction and multistage extraction, can further drop the impurity in potassium floutaramite, according to
The behavior that impurity crystallizes under the Extraction behavior of impurity and different cooling temperatures under different acidity, is prepared for the fluorotantalic acid of high-purity
Potassium.
Claims (10)
1. a kind of preparation method of high-purity potassium floutaramite, which is characterized in that include the following steps：
(1) it decomposes：Tantalum niobium concentrate object is added into hydrofluoric acid and sulfuric acid and is decomposed；
(2) sludge extraction：Counter-current extraction is carried out using MIBK solvent or sec-octyl alcohol solvent, fluorine niobic acid and fluorotantalic acid are extracted to
In solvent；
(3) pickling：It is contacted using the solvent obtained after sulfuric acid solution adverse current and step (2) extraction；
(4) anti-niobium mentions tantalum：Using sulfuric acid solution and obtained solvent in extraction tank counter-current extraction, fluorine niobic acid is extracted into water phase,
Form fluorine niobic acid aqueous solution；
(5) anti-tantalum：By remaining organic solution in another extraction tank, fluorotantalic acid organic solution is stripped to pure using pure water
In water, fluorotantalic acid aqueous solution is formed；
(6) it synthesizes：Potassium chloride and hydrofluoric acid will be added after the heating of obtained fluorotantalic acid aqueous solution；
(7) crystallisation by cooling：Potassium floutaramite crystal will be obtained after Synthesis liquid cooling, is centrifuged, it is brilliant to obtain high-purity potassium floutaramite for drying
Body.
2. the preparation method of high-purity potassium floutaramite as described in claim 1, it is characterised in that：Step (5) specifically uses two sections
Anti- tantalum, the anti-tantalum liquid of the anti-tantalum of first segment are sulfuric acid, hydrochloric acid or hydrofluoric acid solution that hydrogen ion concentration is 0.05-0.6mol/L,
The anti-tantalum liquid of the anti-tantalum of second segment is pure water, and using the anti-tantalum liquid of second segment as the raw material of step (6) synthesis potassium floutaramite.
3. the preparation method of high-purity potassium floutaramite as described in claim 1, it is characterised in that：Step (7) specifically uses three sections
Cooling, the cooling temperature for controlling first segment is 70-80 DEG C, then puts first segment liquid after cooling into second segment cooling,
Collect first segment it is cooling after obtained crystallization, the cooling temperature for controlling second segment is 40 DEG C -70 DEG C, then will second segment it is cooling after
Obtained liquid is put into three-stage cooling, and the crystallization obtained after second segment cooling is collected, and the cooling temperature of control third section is
10 DEG C -40 DEG C, the crystallization obtained after three-stage cooling is collected, the potassium floutaramite obtained after cooling using second segment, by the fluorine tantalum
Sour potassium carries out a recrystallization again, is added in pure water, and high-pure hydrofluoric acid and high purity potassium chloride is added, finally obtains high-purity fluorine tantalum
Sour potassium.
4. the preparation method of high-purity potassium floutaramite as described in claim 1, it is characterised in that：Anti- tantalum extraction in step (5)
It is to be extracted at 8 grades into 12 stage countercurrent extraction tanks.
5. the preparation method of high-purity potassium floutaramite as described in claim 1, it is characterised in that：There is control extraction in step (5)
Solvent and the flow-rate ratio of strippant are 1：2 to 3：1.
6. the preparation method of high-purity potassium floutaramite as described in claim 1, it is characterised in that：In step (7) in cooling bath
Rotating speed of agitator is controlled to turn for 30-90 per minute.
7. the preparation method of high-purity potassium floutaramite as described in claim 1, it is characterised in that：The anti-tantalum liquid of control in step (5)
Acidity is 0.05-0.6mol/L.
8. the preparation method of high-purity potassium floutaramite as described in claim 1, it is characterised in that：The anti-tantalum of second segment in step (5)
Liquid is sulfuric acid, hydrochloric acid or the hydrofluoric acid solution of hydrogen ion concentration 0.05-0.6mol/L.
9. the preparation method of high-purity potassium floutaramite as described in claim 1, it is characterised in that：Second segment is anti-in step (5)
Tantalum liquid controls filtering accuracy less than 0.1 micron by precision filtration equipment.
10. the preparation method of high-purity potassium floutaramite as described in claim 1, it is characterised in that：
(1) tantalum niobium concentrate mountain flour is broken to no more than 200 mesh, is added into hydrofluoric acid, then add sulfuric acid, heat preservation is decomposed；
(2) extract in slot then into mine, using MIBK solvent or sec-octyl alcohol solvent extraction tantalum niobium, to make fluorotantalic acid and fluorine
Niobic acid enters in solvent, recycles the sulfuric acid of 3.7-4.2mol/L counter-current extraction in descaling bath, makes later containing tantalum niobium
Organic solvent enters anti-niobium and mentions in tantalum slot, using sulfuric acid solution and the organic solvent adverse current containing tantalum niobium of 0.6-0.8mol/L
Extraction；
(3) obtained fluorine niobic acid solution is entered in sulfuric acid solution, and obtained fluorotantalic acid solution is stayed in organic solvent；
(4) organic solvent containing fluorotantalic acid has been entered in anti-tantalum extraction tank, using 12 grades of anti-tantalum slot as first segment
It is stripped groove body, using hydrogen ion concentration is the sulfuric acid of 0.05-0.6mol/L, hydrochloric acid or hydrofluoric acid solution as first segment
Then anti-tantalum agent recycles 12 grades of anti-tantalum slot to obtain as the back extraction groove body of second segment using pure water as strippant
The fluorotantalic acid solution of second segment, for use；
(5) hydrofluoric acid and potassium chloride is added in obtained fluorotantalic acid solution, is heated to 92 DEG C or more and keeps the temperature half an hour, is put into
Into first cooling bath, 70 DEG C -80 DEG C are cooled to, then solution is put into second cooling bath, is cooled to 40 DEG C -70
DEG C, finally solution is put into third cooling bath, is cooled to 10 DEG C -40 DEG C degrees Celsius；It collects in second cooling bath
Potassium floutaramite crystallization, is then added into pure water, is warming up to 92 DEG C or more, and hydrofluoric acid and potassium chloride is added, and dissolves fluorotantalic acid
It after potassium crystal, is put into cooling bath and crystallizes, collect potassium floutaramite crystal, centrifugation is dried to get solid to the potassium floutaramite of high-purity
Body.
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| CN110563038A (en) * | 2019-09-25 | 2019-12-13 | 九江有色金属冶炼有限公司 | method for preparing low-antimony low-iron high-purity niobium oxide from niobium tantalite |
| CN110923740A (en) * | 2019-10-17 | 2020-03-27 | 东北大学 | Method for electrochemically deeply removing water-soluble extractant in tantalum liquid in preparation process of potassium fluotantalate |
| CN111690827A (en) * | 2020-07-01 | 2020-09-22 | 江西拓泓新材料有限公司 | Method for recovering tantalum resource from potassium fluotantalate crystallization mother liquor |
| CN112010348A (en) * | 2020-09-14 | 2020-12-01 | 宁夏东方钽业股份有限公司 | Preparation method of high-purity niobium oxide for high-purity niobium sheet for irradiation monitoring tube |
| CN116358253A (en) * | 2023-02-14 | 2023-06-30 | 宁夏东方钽业股份有限公司 | Potassium fluorotantalate drying and preserving equipment and method |
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| CN104480304A (en) * | 2014-04-15 | 2015-04-01 | 宁夏东方钽业股份有限公司 | Method for reducing usage amount of ammonia gas during process of tantalum-niobium hydrometallurgical extraction |
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| CN1460088A (en) * | 2001-04-06 | 2003-12-03 | 三井金属鉱业株式会社 | Method for producing high purity potassium fluorotantalate crystal or high purity potassium fluoroniobate crystal and recrystallization vessel for use in method for production, and potassium |
| CN104480304A (en) * | 2014-04-15 | 2015-04-01 | 宁夏东方钽业股份有限公司 | Method for reducing usage amount of ammonia gas during process of tantalum-niobium hydrometallurgical extraction |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563038A (en) * | 2019-09-25 | 2019-12-13 | 九江有色金属冶炼有限公司 | method for preparing low-antimony low-iron high-purity niobium oxide from niobium tantalite |
| CN110923740A (en) * | 2019-10-17 | 2020-03-27 | 东北大学 | Method for electrochemically deeply removing water-soluble extractant in tantalum liquid in preparation process of potassium fluotantalate |
| CN110923740B (en) * | 2019-10-17 | 2021-02-19 | 东北大学 | Method for electrochemically deeply removing water-soluble extractant in tantalum liquid in preparation process of potassium fluotantalate |
| CN111690827A (en) * | 2020-07-01 | 2020-09-22 | 江西拓泓新材料有限公司 | Method for recovering tantalum resource from potassium fluotantalate crystallization mother liquor |
| CN112010348A (en) * | 2020-09-14 | 2020-12-01 | 宁夏东方钽业股份有限公司 | Preparation method of high-purity niobium oxide for high-purity niobium sheet for irradiation monitoring tube |
| CN112010348B (en) * | 2020-09-14 | 2022-08-19 | 宁夏东方钽业股份有限公司 | Preparation method of high-purity niobium oxide for high-purity niobium sheet for irradiation monitoring tube |
| CN116358253A (en) * | 2023-02-14 | 2023-06-30 | 宁夏东方钽业股份有限公司 | Potassium fluorotantalate drying and preserving equipment and method |
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