CN105565384A - Ammonium paratungstate preparation method - Google Patents
Ammonium paratungstate preparation method Download PDFInfo
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- CN105565384A CN105565384A CN201511016448.3A CN201511016448A CN105565384A CN 105565384 A CN105565384 A CN 105565384A CN 201511016448 A CN201511016448 A CN 201511016448A CN 105565384 A CN105565384 A CN 105565384A
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- diatomite
- tungstate solution
- hydrochloric acid
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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Abstract
The invention discloses an ammonium paratungstate preparation method. The method in the embodiment of the invention comprises the following steps: mixing a hydrochloric acid solution with diatomite, and heating the obtained mixture to obtain a diatomite-containing hydrochloric acid solution; adding a sodium tungstate solution to the diatomite-containing hydrochloric acid solution, and stirring the solutions to obtain a tungstic acid precipitate-containing mixed solution; carrying out primary filtering treatment on the tungstic acid precipitate-containing mixed solution to obtain a tungstic acid and diatomite mixture; mixing the tungstic acid and diatomite mixture with ammonia water to obtain a diatomite-containing ammonium tungstate solution; carrying out secondary filtering treatment on the diatomite-containing ammonium tungstate solution to obtain diatomite and an ammonium tungstate solution; and carrying out evaporating and crystallizing treatment on the ammonium tungstate solution to obtain ammonium paratungstate. The method effectively solves the problem of difficult filtration of viscous tungstic acid.
Description
Technical field
The present invention relates to tungsten ore smelting process field, particularly, relate to the method preparing ammonium paratungstate.
Background technology
The hydrometallurgy of tungsten is mainly divided into ion exchange process, extraction process, classical technique and acid technological process.Wherein prevailing technology is ion exchange process, extraction process, and these two kinds of techniques all need tungsten to be converted into ammonium tungstate system from sodium wolframate system, just by after being sintered into Tungsten oxide 99.999, and the tungsten powder needed for logical hydrogen reducing obtains.But the method technical process is complicated, need a large amount of water, cause wastewater discharge large and salt acid consumption is large, easily cause the problem of environmental pollution.
1958 ~ nineteen ninety of China once adopted classical technique to take wolframite as raw material production ammonium paratungstate.The technological process of the classical explained hereafter ammonium paratungstate of wolframite is: wolframite NaOH decomposes the thick Na of gained
2wO
4solution, through in HCl and after add MgCl
2removing P, As, Si; Na after purification
2wO
4solution adds CaCl
2precipitate white tungsten; Gained artificial scheelite adds industrial tungstic acid and carries out acid decomposition; Gained wolframic acid can produce WO by dinectly bruning
3, also can adding ammoniacal liquor, to carry out ammonia molten; The molten gained ammonium tungstate solution of ammonia produces ammonium paratungstate after evaporative crystallization; Crystalline mother solution adds a small amount of thick Na
2wO
4solution neutralizes, and adds HCl and Na
2s solution is except returning purification after molybdenum except P, As, Si operation; Acid decomposing wasting liquid adds Ca (OH)
2caCl is reclaimed in neutralization
2.
Before 2004, China's sheelite adopts acid technological process to produce APT substantially.Hydrochloric acid decompose tunstite process major part phosphorus, arsenic, silicon, molybdenum enter solution with the acid of solubility, exist in solution with assorted many wolframic acids form that solubleness is very large on a small quantity, cause the loss of tungsten and sour decomposing metal yield to decline, therefore should control the content of phosphorus in sheelite, arsenic, silicon, molybdenum.Ca in sheelite
5f (PO
4)
3generate the HF that corrodibility is very large, easy etching apparatus.Calcium, iron, aluminium major part enters solution with villaumite form and removes.
At present, the method producing wolframic acid is all by adding mineral acid to calcium wolframate, thus the wolframic acid needed for obtaining, ammoniacal liquor is then adopted to be dissolved by thick wolframic acid, tungsten enters solution with ammonium tungstate form, because pH value raises, can there is hydrolytic precipitation, with metasilicic acid H insoluble in weak alkaline medium in the soluble impurity such as iron, manganese of the non-washes clean of sour decomposition process
2siO
4enter slag phase and remove together with undecomposed ore particle.
Such as, although have scholar's research to cross to adopt in soluble tungstate salt, sodium wolframate, ammonium tungstate, add mineral acid precipitation wolframic acid, for wolframic acid filterableness how, there is no correlation report.How the wolframic acid be precipitated out is filtered, and obtain the wolframic acid of high-quality, need to be studied further.
Summary of the invention
The present invention is intended at least to solve one of technical problem existed in prior art.For this reason, one object of the present invention is to propose a kind of method preparing ammonium paratungstate, and the method, by adding diatomite in preparation process, makes the wolframic acid of generation be convenient to filter, significantly shorten the preparation time of ammonium paratungstate.
It should be noted that, the present invention completes based on the following work of contriver:
Contriver finds, in the process preparing ammonium paratungstate, contriver adds diatomite in reaction raw materials, significantly can shorten the filtration time of wolframic acid, and diatomite can not affect the purity that wolframic acid obtains ammonium tungstate solution after ammonia is molten, can not introduce impurity.In addition, diatomite has flourishing hole, can adsorb trickle wolframic acid particle, and in the molten process of ammonia, diatomite can be precipitated out, and after washing, can recycle.
Thus, according to an aspect of the present invention, the invention provides a kind of method preparing ammonium paratungstate.According to embodiments of the invention, the method comprises: hydrochloric acid soln and diatomite mixed and heat, to obtain containing diatomaceous hydrochloric acid soln; Sodium tungstate solution is added described containing in diatomaceous hydrochloric acid soln, and stir, to obtain the mixing solutions containing wolframic acid precipitation; The described mixing solutions containing wolframic acid precipitation is carried out the first filtration treatment, to obtain wolframic acid and diatomaceous mixture; Described wolframic acid and diatomaceous mixture are mixed with ammoniacal liquor, to obtain containing diatomaceous ammonium tungstate solution; The second filtration treatment is carried out, to obtain diatomite and ammonium tungstate solution containing diatomaceous ammonium tungstate solution by described; Described ammonium tungstate solution is carried out evaporative crystallization process, to obtain described ammonium paratungstate.
According to the method preparing ammonium paratungstate of the embodiment of the present invention, by adding diatomite in preparation process, the wolframic acid of generation is made to be convenient to filter, significantly shorten the preparation time of ammonium paratungstate, efficiently solve the problem that wolframic acid thickness is difficult to filter, and, the rate of recovery of W elements is high, and loss is few.
In addition, the method preparing ammonium paratungstate according to the above embodiment of the present invention, can also have following additional technical characteristic:
According to embodiments of the invention, the concentration of described hydrochloric acid soln is 1-10mol/L.According to a preferred embodiment of the invention, the concentration of described hydrochloric acid soln is 2-4mol/L.
According to embodiments of the invention, the volume ratio of described hydrochloric acid soln and described sodium tungstate solution is (1-3): 1.
According to embodiments of the invention, the concentration of described sodium tungstate solution is 100-300g/L.According to a preferred embodiment of the invention, the concentration of described sodium tungstate solution is 109-218g/L.
According to embodiments of the invention, the ratio of described diatomite and described sodium tungstate solution is (2-8) gram: 100 milliliters.According to a preferred embodiment of the invention, the ratio of described diatomite and described sodium tungstate solution is 8 grams: 100 milliliters.
According to embodiments of the invention, the temperature of described heating is 90-110 DEG C.
According to embodiments of the invention, it is 1-20ml/min that described sodium tungstate solution adds the described flow velocity containing diatomaceous hydrochloric acid soln.According to a preferred embodiment of the invention, described sodium tungstate solution adds the described flow velocity containing diatomaceous hydrochloric acid soln is 3.3ml/min.
According to embodiments of the invention, the speed of described stirring is 100-1000r/min.
According to embodiments of the invention, the time of described stirring is for being no less than 1 hour.
According to embodiments of the invention, the method comprises further: before described evaporative crystallization process, carry out purifying treatment to described ammonium tungstate solution.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 shows the schematic flow sheet of the method preparing ammonium paratungstate according to an embodiment of the invention.
Embodiment
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Being exemplary below by the embodiment be described with reference to the drawings, only for explaining the present invention, and can not limitation of the present invention being interpreted as.
In describing the invention, term " longitudinal direction ", " transverse direction ", " on ", D score, "front", "rear", "left", "right", " vertically ", " level ", " top ", the orientation of the instruction such as " end " or position relationship be based on orientation shown in the drawings or position relationship, be only the present invention for convenience of description instead of require that the present invention with specific azimuth configuration and operation, therefore must can not be interpreted as limitation of the present invention.
It should be noted that, term " first ", " second " only for describing object, and can not be interpreted as instruction or hint relative importance or imply the quantity indicating indicated technical characteristic.Thus, be limited with " first ", the feature of " second " can express or impliedly comprise one or more these features.Further, in describing the invention, except as otherwise noted, the implication of " multiple " is two or more.
According to an aspect of the present invention, the invention provides a kind of method preparing ammonium paratungstate.With reference to figure 1, according to embodiments of the invention, explain the method, the method comprises:
S100 heats
According to embodiments of the invention, hydrochloric acid soln and diatomite mixed and heats, obtaining containing diatomaceous hydrochloric acid soln.The guarantee of this process is follow-up to add sodium tungstate solution in excessive hydrochloric acid soln, makes sodium wolframate fully contact production wolframic acid with excessive hydrochloric acid.Meanwhile, hydrochloric acid soln and diatomaceous mixture heat, and are conducive to generating growing up of wolframic acid.
According to embodiments of the invention, the concentration of hydrochloric acid soln is not particularly limited, and generates wolframic acid as long as can react with sodium tungstate solution, and according to some embodiments of the present invention, the concentration of hydrochloric acid soln is 1-10mol/L.Thus, the filtration time of wolframic acid is short.According to a preferred embodiment of the invention, the concentration of hydrochloric acid soln is 2-4mol/L.Thus, the filtration time of wolframic acid significantly shortens.
According to embodiments of the invention, the temperature of heating is 90-110 DEG C.Thus, the filtration time of wolframic acid significantly shortens.
S200 stirs
Sodium tungstate solution is added containing in diatomaceous hydrochloric acid soln, and stir, obtain the mixing solutions containing wolframic acid precipitation.Thus, make sodium wolframate drop in hydrochloric acid, sodium wolframate is fully contacted with excessive hydrochloric acid, and sodium wolframate reacts completely, generates wolframic acid.
According to embodiments of the invention, the flow velocity that sodium tungstate solution adds containing diatomaceous hydrochloric acid soln is not special restriction, as long as sodium tungstate solution fully mixes with hydrochloric acid soln.According to embodiments of the invention, the sodium tungstate solution flow velocity added containing diatomaceous hydrochloric acid soln is 1-20ml/min.Thus, the filtration time of wolframic acid is short.According to a preferred embodiment of the invention, sodium tungstate solution adds the flow velocity containing diatomaceous hydrochloric acid soln is 3.3ml/min.Thus, the filtration time of wolframic acid significantly shortens.
According to embodiments of the invention, the volume ratio of hydrochloric acid soln and sodium tungstate solution is (1-3): 1.Thus, hydrochloric acid and sodium wolframate fully react generation wolframic acid.If the volume ratio of hydrochloric acid soln and sodium tungstate solution is lower than 1:1, then salt subacidity, sodium wolframate complete reaction cannot produce wolframic acid.If the volume ratio of hydrochloric acid soln and sodium tungstate solution is higher than 3:1, then salt excessive acid, not only causes the waste of reaction reagent, and introduces excessive chlorion in the product, for follow-up purification and impurity removal process adds obstacle.
According to embodiments of the invention, the concentration of sodium tungstate solution is not particularly limited, as long as can produce wolframic acid with hydrochloric acid reaction.According to some embodiments of the present invention, the concentration of sodium tungstate solution is 100-300g/L.Thus, the filtration time of wolframic acid is short.According to a preferred embodiment of the invention, the concentration of sodium tungstate solution is 109-218g/L.Thus, the filtration time of wolframic acid significantly shortens.
According to embodiments of the invention, the ratio of diatomite and sodium tungstate solution is not particularly limited, as long as diatomite can adsorb the wolframic acid of generation completely.According to some embodiments of the present invention, the ratio of diatomite and sodium tungstate solution is (2-8) gram: 100 milliliters.Thus, diatomite fully adsorbs the wolframic acid of generation, makes tungstic acid be easy to filter, efficiently solves the problem that wolframic acid thickness is difficult to filter.According to a preferred embodiment of the invention, the ratio of diatomite and sodium tungstate solution is 8 grams: 100 milliliters.Thus, the effect of diatomite adsorption wolframic acid is better, and tungstic acid is easier to filter.
According to embodiments of the invention, the speed of stirring is 100-1000r/min.Thus, ensure that the wolframic acid generated fully can contact with diatomite, diatomite is uniformly distributed in mixing solutions.
According to embodiments of the invention, the time of stirring is for being no less than 1 hour.Thus, ensure sodium wolframate and hydrochloric acid complete reaction, generate wolframic acid.
S300 first filtration treatment
According to embodiments of the invention, the mixing solutions precipitated containing wolframic acid is carried out the first filtration treatment, obtain wolframic acid and diatomaceous mixture.Thus, by the first filtration treatment, from mixing solutions by wolframic acid and diatomaceous mixture separation out.Because wolframic acid is thick, be difficult to filter, after wolframic acid mixes with diatomite by contriver, diatomite effectively adsorbs wolframic acid, forms the wolframic acid and diatomaceous mixture that are easy to filter.
S400 ammonia is molten
According to embodiments of the invention, wolframic acid and diatomaceous mixture are mixed with ammoniacal liquor, obtain containing diatomaceous ammonium tungstate solution.Utilize the wolframic acid in ammonia solvent wolframic acid and diatomaceous mixture, generate the ammonium tungstate solution of high economic worth, and achieve wolframic acid and be separated with diatomaceous.
S500 second filtration treatment
According to embodiments of the invention, the second filtration treatment will be carried out containing diatomaceous ammonium tungstate solution, obtain diatomite and ammonium tungstate solution.Thus, by the second filtration treatment, by solid-state diatomite separating treatment from the ammonium tungstate solution of liquid state, and being separated the diatomite obtained can reuse, and effectively reduces production cost.
The process of S600 evaporative crystallization
According to embodiments of the invention, ammonium tungstate solution is carried out evaporative crystallization process, obtain ammonium paratungstate.Thus, by evaporative crystallization process, obtain the ammonium paratungstate of high economic worth.
According to embodiments of the invention, the method comprises further: before evaporative crystallization process, carries out purifying treatment to ammonium tungstate solution.Thus, the ammonium paratungstate impurity of production is few, and purity is high.
According to the method preparing ammonium paratungstate of the embodiment of the present invention, by adding diatomite in preparation process, the wolframic acid of generation is made to be convenient to filter, significantly shorten the preparation time of ammonium paratungstate, efficiently solve the problem that wolframic acid thickness is difficult to filter, and, the rate of recovery of W elements is high, and loss is few.Further, this technical process preparing the method for ammonium paratungstate is simple, and in preparation process, soda acid consumption is few, and the amount of industrial wastewater of generation significantly reduces, and environmental pollution is little.
Below with reference to specific embodiment, the present invention will be described, it should be noted that, these embodiments are only illustrative, and can not be interpreted as limitation of the present invention.
Embodiment 1
The hydrochloric acid reaction of diatomite, sodium wolframate and different concns is prepared wolframic acid, compares the filtration procedure of concentration of hydrochloric acid to wolframic acid, specific as follows:
(1) measure 50ml concentrated hydrochloric acid, be made into respectively acidity be 2,4,6, the hydrochloric acid of 8mol/l, then eachly add 2g diatomite, water-bath adds 90 DEG C;
(2) by 4 parts be the dense material of sodium wolframate (tungstic oxide concentration is 195g/l) of 100ml, be numbered: A, B, C, D, wherein A joins in the hydrochloric acid of the 2mol/l heated in advance, B joins in the hydrochloric acid of the 4mol/l heated in advance, C joins in the hydrochloric acid of the 6mol/l heated in advance, D joins in the hydrochloric acid of the 8mol/l heated in advance, stir, the reaction times is 1h;
(3) after reaction terminates, add cold pure water, constant volume respectively in 4 groups of mixtures that step (2) obtains, filter, and record filtering time and filtrate volume.Result is as follows:
Experimental result shows, sodium wolframate and acidity are 2, the hydrochloric acid reaction of 4mol/l, and the wolframic acid of generation more easily filters.
Embodiment 2
Wolframic acid is prepared in the reaction of the diatomite of hydrochloric acid, sodium wolframate and Different Weight, and more diatomaceous weight ratio is on the impact of the filtration procedure of wolframic acid, specific as follows:
(1) measure the hydrochloric acid that 150ml acidity is 4mol/l, add respectively weight be 2,4,6, the diatomite of 8g, water-bath adds 90 DEG C;
(2) by 4 parts be the dense material of sodium wolframate (tungstic oxide concentration is 195g/l) of 100ml, be numbered: A, B, C, D, E, wherein A joins in the hydrochloric acid soln heated in advance, do not add diatomite in this solution, B join added in the diatomaceous hydrochloric acid soln of 2g in advance, C join added in the diatomaceous hydrochloric acid soln of 4g in advance, D join added in the diatomaceous hydrochloric acid soln of 6g in advance, E joins and added in the diatomaceous hydrochloric acid soln of 8g in advance, stir, the reaction times is 1h;
(3), after reaction terminates, cold pure water is added, constant volume, record filtering time and filtrate volume respectively in 4 groups of mixtures that step (2) obtains.Result is as follows:
Result shows, in reactant, after adding diatomite, filtration time significantly shortens, and A group does not add diatomite, and filtration time needs 180 minutes, B group only adds 2g diatomite, and filtration time just significantly shortens to the half less than A group, and, along with the ratio of diatomite and sodium tungstate solution raises, the filtration time of wolframic acid obviously shortens, and in 4 groups, the filtration time of D group is the shortest, be only 27 minutes, be only about 1/6 of A group filtration time.
Embodiment 3
Wolframic acid is prepared in the reaction of the sodium tungstate solution of hydrochloric acid, diatomite and different concns, compares the concentration of sodium tungstate solution to the impact of the filtration procedure of wolframic acid, specific as follows:
(1) measuring four groups of 150ml acidity is the hydrochloric acid of 4mol/l, adds 6g diatomite, and water-bath adds 90 DEG C;
(2) be 312g/l by the tungstic oxide concentration of sodium tungstate solution, by this concentration configuration tungstic oxide concentration be 109,218,265, the sodium tungstate solution of 312g/l.Be 109 by tungstic oxide concentration, 218,265, the sodium tungstate solution of 312g/l, be numbered: A, B, C, D, join in the hydrochloric acid soln of the 4mol/l heated in advance respectively, stir, the reaction times is 1h;
(3), after reaction terminates, cold pure water is added, constant volume, record filtering time and filtrate volume respectively in 4 groups of mixtures that step (2) obtains.Result is as follows:
Result shows, when the concentration of sodium tungstate solution is 109g/L and 218g/L, the filtration time of wolframic acid obviously shortens.
Embodiment 4
The hydrochloric acid of differing temps and diatomite mixed solution and sodium tungstate solution reaction are prepared wolframic acid, compares the temperature of hydrochloric acid and diatomite mixed solution to the impact of the filtration procedure of wolframic acid, specific as follows:
(1) hydrochloric acid that 150ml concentration is 4mol/l is measured, be numbered A, B, C, D, often organize and all add 6g diatomite, wherein A bath temperature is 80 DEG C, B bath temperature is 90 DEG C, C bath temperature is 100 DEG C, D bath temperature is 110 DEG C, obtains 4 groups of hydrochloric acid and diatomite mixed solution;
(2) measure 4 parts of dense material of sodium wolframate (tungstic oxide concentration is 195g/l) for 100ml, add in A, B, C, D4 group hydrochloric acid and diatomite mixed solution that step (1) obtains successively, adjoint stir process, the reaction times is 1h;
(3) after reaction terminates, respectively to the pure water adding heat in 4 groups of mixtures that step (2) obtains, constant volume, record filtering time and filtrate volume.Result is as follows:
Result shows, when the temperature of hydrochloric acid and diatomite mixed solution is 90-110 degree Celsius, the filtration time of wolframic acid obviously shortens.
Embodiment 5
Hydrochloric acid and diatomite mixed solution and sodium tungstate solution reaction are prepared wolframic acid, compares the flow velocity of sodium tungstate solution to the impact of the filtration procedure of wolframic acid, specific as follows:
Measure the hydrochloric acid that 150ml concentration is 4mol/l, be numbered A, B, C, D, often organize and all add 6g diatomite, wherein No. A speed adding sodium wolframate is 3.3ml/min, No. B speed adding sodium wolframate is 6.7ml/min, No. C speed adding sodium wolframate is 16.7ml/min; No. D speed adding sodium wolframate is 33ml/min.Temperature of reaction is 95 DEG C, and the time is 1h, after reaction terminates, adds the pure water of heat, constant volume in 4 groups of mixtures, record filtering time and filtrate volume and.Result is as follows:
Result shows, when the flow velocity of sodium tungstate solution is 3.3ml/min, 6.7ml/min and 16.7ml/min, the filtration time of wolframic acid obviously shortens, and wherein, when the flow velocity of sodium tungstate solution is 3.3ml/min, the filtration time of wolframic acid obviously shortens more remarkable.
Embodiment 6
Hydrochloric acid and diatomite mixed solution and sodium tungstate solution reaction are prepared wolframic acid, compares the impact of differential responses time on the filtration procedure of wolframic acid, specific as follows:
(1) measure the hydrochloric acid that 150ml concentration is 4mol/l, be numbered A, B, C, D, wherein A, B, C, D group all adds 2g diatomite, and temperature of reaction is 95 DEG C;
(2) the dense material of sodium wolframate that 4 parts is 100ml is measured; Add respectively in A, B, C, D4 group mixed solution that step (1) obtains, the reaction times is 0.5h, 1h, 2h, 3h;
(3) after reaction terminates, respectively to the pure water adding heat in 4 groups of mixtures that step (2) obtains, constant volume, record filtering time.Result is as follows:
| Numbering | A | B | C | D |
| Reaction times h | 0.5 | 1 | 2 | 3 |
| Filtration time min | 1 | 0.5 | 0.5 | 0.5 |
Result shows, be 0.5 constantly little when reacted, the filtration time of wolframic acid is long, and be greater than 1 constantly little when reacted, the filtration time of wolframic acid is without considerable change, and the prolongation of time has no significant effect reaction.
In the description of this specification sheets, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present invention or example.In this manual, identical embodiment or example are not necessarily referred to the schematic representation of above-mentioned term.And the specific features of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although illustrate and describe embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple change, amendment, replacement and modification to these embodiments when not departing from principle of the present invention and aim, scope of the present invention is by claim and equivalents thereof.
Claims (10)
1. prepare a method for ammonium paratungstate, it is characterized in that, comprising:
Hydrochloric acid soln and diatomite are mixed and heats, to obtain containing diatomaceous hydrochloric acid soln;
Sodium tungstate solution is added described containing in diatomaceous hydrochloric acid soln, and stir, to obtain the mixing solutions containing wolframic acid precipitation;
The described mixing solutions containing wolframic acid precipitation is carried out the first filtration treatment, to obtain wolframic acid and diatomaceous mixture;
Described wolframic acid and diatomaceous mixture are mixed with ammoniacal liquor, to obtain containing diatomaceous ammonium tungstate solution;
The second filtration treatment is carried out, to obtain diatomite and ammonium tungstate solution containing diatomaceous ammonium tungstate solution by described;
Described ammonium tungstate solution is carried out evaporative crystallization process, to obtain described ammonium paratungstate.
2. method according to claim 1, is characterized in that, the concentration of described hydrochloric acid soln is 1-10mol/L, preferably, is 2-4mol/L.
3. method according to claim 2, is characterized in that, the volume ratio of described hydrochloric acid soln and described sodium tungstate solution is (1-3): 1.
4. method according to claim 1, is characterized in that, the concentration of described sodium tungstate solution is 100-300g/L, preferably, is 109-218g/L.
5. method according to claim 4, is characterized in that, the ratio of described diatomite and described sodium tungstate solution is (2-8) gram: 100 milliliters, preferably, is 8 grams: 100 milliliters.
6. method according to claim 1, is characterized in that, the temperature of described heating is 90-110 DEG C.
7. method according to claim 1, is characterized in that, it is 1-20ml/min that described sodium tungstate solution adds the described flow velocity containing diatomaceous hydrochloric acid soln, preferably, is 3.3ml/min.
8. method according to claim 1, is characterized in that, the speed of described stirring is 100-1000r/min.
9. method according to claim 1, is characterized in that, the time of described stirring is for being no less than 1 hour.
10. method according to claim 1, is characterized in that, comprises further:
Before described evaporative crystallization process, purifying treatment is carried out to described ammonium tungstate solution.
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| CN117566799B (en) * | 2024-01-15 | 2024-03-15 | 崇义章源钨业股份有限公司 | Method for preparing ammonium paratungstate |
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