CN106430312B - A kind of preparation method of monoclinic system tungstic acid - Google Patents
A kind of preparation method of monoclinic system tungstic acid Download PDFInfo
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Abstract
The present invention provides a kind of method preparing monoclinic system tungstic acid as raw material using copper-tungsten waste material, includes the steps that Ore Leaching, roasting, ammonification and acidolysis.The present invention is using copper-tungsten waste material as raw material, prepare have can photocatalytic degradation organic matter high-valued product monoclinic system tungstic acid, realize recycling for waste metal resource, energy conservation and environmental protection and resource reproducible utilization strategy of the product in terms of environment pollution control, meeting country will be recycled using regenerative resource (solar energy) again；The preparation method raw material of the present invention is easy to get, is at low cost, is simple for process, is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of preparation methods of tungstic acid, more particularly to prepare three oxidations using copper-tungsten waste material
Tungsten.
Background technology
Tungsten is widely used in because it has under high hardness, fusing point height, room temperature not by the good property such as air corrosion
Alloy process industry, shipping industry, anticorrosive paint, gas sensor, photocatalysis and display etc..Tungsten product prepares and gives up
During old product is eliminated, it can be formed and largely contain tungsten secondary resource, tungsten be recycled from secondary resource, not only the grade of tungsten carries
It is high and realize resources circulation.Currently, the recycling of tungsten slag is broadly divided into three parts：(1) valuable metal therein is recycled；
(2) wear-resistant material is produced using tungsten slag as raw mineral materials；(3) tungsten slag microcrystalline glass is produced.
Chinese patent CN201310002669.X is that raw material prepares tungstic acid using Disodium tungstate (Na2WO4) dihydrate and sodium chloride；
Chinese patent CN201310742106.4 is to be saturated ammonium tungstate solution and ammonium chloride, tartaric acid, ethylenediamine tetrapropionic acid etc. as raw material
Prepare tungsten trioxide powder.The above technology raw material are more expensive, and cost is larger, are not suitable for industrialized production；And not to product
Performance is studied.
The existing patent for preparing tungstic acid is substantially to analyze pure ammonium tungstate, sodium tungstate, ammonium paratungstate etc. as raw material,
Complex process, production cost is high, is unfavorable for industrialized production.
In view of the above shortcomings, the designer, is actively subject to research and innovation, to found a kind of oxidation of monoclinic system three
The preparation method of tungsten makes it with more the utility value in industry.
Invention content
In order to solve the above technical problems, the purpose of the present invention is provide a kind of monoclinic crystal using copper-tungsten waste material for raw material
It is the preparation method of tungstic acid, it is at low cost, simple for process, it is suitable for industrialized production.
The preparation method of a kind of monoclinic system tungstic acid of the present invention, which is characterized in that include the following steps：
(1) tungstic acid is dissolved in aqueous slkali, ammonium paratungstate or ammonium tungstate is obtained through ammonification；
(2) ammonium paratungstate in step (1) or ammonium tungstate obtain wolframic acid colloid through acidolysis；
(3) wolframic acid colloid is aged, washs, obtains the monoclinic system tungstic acid after drying.
Further, further include removing the copper in copper-tungsten using acid leaching process to obtain tungsten slag before step (1),
The step of tungsten slag roasts to obtain tungstic acid.
Further, the acid that acid leaching process uses is selected from one or more of nitric acid, hydrochloric acid and sulfuric acid.
Further, the tungsten slag roasts at 400-600 DEG C.
Further, the acidolysis is through reproducibility acid acidolysis.
Specifically,
(1) it uses nitric acid lixiviation process to remove the copper in copper-tungsten, obtains tungsten slag, the mass percentage of copper is extremely in tungsten slag
It is less than 0.5% less, roasting tungsten slag obtains tungstic acid at preferably shorter than 0.05%, 400-600 DEG C；
(2) tungstic acid is dissolved in aqueous slkali, and ammonium paratungstate or ammonium tungstate is obtained through ammonification；
(3) ammonium paratungstate or ammonium tungstate are configured to 1-2mol/L aqueous solutions, and are slowly added into the reduction of 3-4mol/L
Acidolysis in property acid, stirs to get yellow wolframic acid colloid；
(4) yellow wolframic acid colloid is aged 16-24h under 20-35 DEG C (room temperature), is dried at 100 DEG C after filtration washing
6h obtains monoclinic system tungstic acid, and yellow monoclinic system tungsten trioxide powder is obtained after grinding.
Further, the reproducibility acid is one or more of hydrochloric acid, sulfurous acid, hydrogen sulfide, HBr.
Further, the aqueous slkali is ammonium hydroxide, and tungstic acid obtains ammonium paratungstate through ammonification, crystallization, specifically, by three
Tungsten oxide is dissolved in the ammonia spirit that mass percent is 25-28%, wherein the solid-liquid mass ratio of tungstic acid and ammonia spirit
It is 1:5-10, slow mechanism dissolved 12-24h take supernatant, evaporative crystallization to obtain white crystal ammonium paratungstate.
Further, or by tungstic acid it is dissolved in NaOH or KOH solution, crystallization obtains sodium tungstate or potassium tungstate, wolframic acid
Sodium or potassium tungstate obtain ammonium tungstate after ammonification, specifically, tungstic acid is dissolved in 5-10mol/LNaOH or KOH solution,
Middle tungstic acid and NaOH or the solid-liquid mass ratio 1 of KOH solution:5-10, stirring and dissolving 5-10h, obtains wolframic acid at 40-80 DEG C
Sodium or wolframic acid potassium solution, filtering, evaporative crystallization obtain sodium tungstate or potassium tungstate crystal.
Further, the sodium tungstate or potassium tungstate crystallized is added to before ammonification in nitric acid, obtains yellow wolframic acid
Yellow wolframic acid precipitation is dissolved in ammonia spirit, ammonium tungstate is obtained after ammonification, specifically, obtained wolframic acid sodium crystal is added by precipitation
Enter into 1-3mol/L nitric acid, wherein the solid-to-liquid ratio 1 of wolframic acid sodium crystal and nitric acid:2-4, filtering solution obtain yellow wolframic acid precipitation,
Yellow wolframic acid is added in 25-28% ammonia spirits, wherein the solid-to-liquid ratio of yellow wolframic acid and ammonia spirit is 1:5-10, slow mechanism dissolved
After 12-24h, supernatant is filtered to take, then the ammonia still process 30-60min at 60-100 DEG C, until solution ph is 6-7 or so, obtains wolframic acid
Ammonium salt solution.
According to the above aspect of the present invention, the present invention at least has the advantages that：
The present invention using copper-tungsten waste material as raw material, prepare have can photocatalytic degradation organic matter high-valued product monocline
Crystallographic system tungstic acid realizes the resource circulation utilization of waste metal, and will recycle product using renewable energy solar energy
Energy conservation and environmental protection strategy in terms of environment pollution control, meeting country；The present invention preparation method raw material be easy to get, be at low cost,
It is simple for process, it is suitable for industrialized production.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, with presently preferred embodiments of the present invention and coordinate attached drawing below, is described in detail such as
Under.
Description of the drawings
Fig. 1 is rhombic system tungstic acid XRD diagram；
Fig. 2 is the monoclinic system tungstic acid XRD diagram that in the present invention prepared by embodiment 1；
Fig. 3 is the monoclinic system tungstic acid XRD diagram that in the present invention prepared by embodiment 2；
Fig. 4 is the monoclinic system tungstic acid XRD diagram that in the present invention prepared by embodiment 3；
Fig. 5 is the monoclinic system tungstic acid XRD diagram that in the present invention prepared by embodiment 4；
Fig. 6 is the characterization for the monoclinic system tungstic acid degradation of methylene blue solution that in the present invention prepared by embodiment 1 to 4
Figure.
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is described in further detail.Implement below
Example is not limited to the scope of the present invention for illustrating the present invention.
Embodiment 1
12g copper-tungsten waste materials are first detached copper tungsten by two nitroxylic acid lixiviation process, obtained 8.3g tungsten slags, wherein
Cupric is less than 0.05%, and tungsten slag is roasted at 400 DEG C, obtains 10g or so yellow green tungsten trioxide powders, which is rhombic system
Tungstic acid, XRD schematic diagrames as shown in Figure 1；It is 25-28% ammonium hydroxide that mass percent, which is added, in rhombic system tungstic acid
In, solid-to-liquid ratio 1:5, slow mechanism dissolved 18h, dissolution rate are 90% or so, take supernatant, evaporative crystallization that it is brilliant to obtain 9.71g whites
Body ammonium paratungstate；1mol/L aqueous solutions are made in ammonium paratungstate, are slowly added into the hydrochloric acid of 3mol/L, 1h is stirred, obtains Huang
Color wolframic acid colloid, is aged 16h at room temperature, and 6h is dried at 100 DEG C after filtration washing, solid tungstic acid is obtained, after grinding
Obtain 8.5g yellow tungsten trioxide powders.Through XRD analysis, product is monoclinic system tungstic acid, as shown in Figure 2；It is ground through experiment
Study carefully, irradiates 3h in 500W xenon lamps, 0.10g monoclinic systems tungsten trioxide powder can be such that 10mg/L/ methylene blue solutions drop
Solution rate reaches 98.74%, as shown in Figure 6.
Embodiment 2
50g copper-tungsten waste materials are first detached copper tungsten by two nitroxylic acid lixiviation process, obtained 34.1g tungsten slags, wherein
Cupric is less than 0.05%, and tungsten slag is roasted at 600 DEG C, obtains 41g or so yellow green tungsten trioxide powders, which is rhombic system
Tungstic acid；It is added into 25-28% ammonium hydroxide, solid-to-liquid ratio 1:10, for 24 hours, dissolution rate is 90% or so to slow mechanism dissolved, is taken
Clear liquid, evaporative crystallization obtain 40.12g white crystal ammonium paratungstates；2mol/L aqueous solutions are made in ammonium paratungstate, are slowly added to
Into the hydrochloric acid of 4mol/L, 2h is stirred, yellow wolframic acid colloid is obtained, is aged at room temperature for 24 hours, after filtration washing at 100 DEG C
6h is dried, solid tungstic acid is obtained, 34.05g yellow tungsten trioxide powders is obtained after grinding.Through XRD analysis, product is monocline
Crystallographic system tungstic acid, as shown in Figure 3；Through experimental study, 3h is irradiated in 500W xenon lamps, 0.25g monoclinic systems three aoxidize
Tungsten powder can make 50mg/L/ methylene blue solution degradation rates reach 96.51%, as shown in Figure 6.
Embodiment 3
12g copper-tungsten waste materials are first detached copper tungsten by two nitroxylic acid lixiviation process, obtained 8.3g tungsten slags, wherein
Cupric is less than 0.5%, and tungsten slag is roasted at 400 DEG C, obtains 10g or so yellow green tungsten trioxide powders, which is rhombic system
Tungstic acid；It adds it in the sodium hydroxide solution of 50ml5mol/L, 5h is stirred at 40 DEG C, tungstic acid dissolution rate is
90% or so, supernatant is filtered to take, evaporative crystallization obtains 12.80g wolframic acid sodium crystals；Wolframic acid sodium crystal is added to 23ml
In the salpeter solution of 1mol/L, after stirring 0.5h, 9.68g Huang wolframic acids precipitation is obtained by filtration；Yellow wolframic acid is added to the dense ammonia of 50ml
In water (25-28%) solution, after slow mechanism dissolved 12h, it is 7 or so to take supernatant, 60 DEG C of ammonia still processs to solution ph, and it is molten to obtain ammonium tungstate
Liquid；This ammonium tungstate solution is added in 50ml 3mol/L hydrochloric acid solutions, after stirring 1h, is aged 16h at room temperature, through filtering
6h is dried at 100 DEG C after washing, obtains solid tungstic acid, 8.5g yellow tungsten trioxide powders are obtained after grinding.Through XRD points
Analysis, product are monoclinic system tungstic acid, as shown in Figure 4；Through experimental study, 3h, 0.10g tri- are irradiated in 500W xenon lamps
Tungsten oxide powder can make 10mg/L/ methylene blue solution degradation rates reach 98.74%, as shown in Figure 6.
Embodiment 4
50g copper-tungsten waste materials are first detached copper tungsten by two nitroxylic acid lixiviation process, obtained 34.1g tungsten slags, wherein
Cupric is less than 0.5%, and tungsten slag is roasted at 600 DEG C, obtains 41g or so yellow green tungsten trioxide powders, which is rhombic system
Tungstic acid；It adds it in the sodium hydroxide solution of 100ml 10mol/L, 10h, tungstic acid dissolution rate is stirred at 80 DEG C
It is 90% or so, filters to take supernatant, evaporative crystallization obtains 52.48g wolframic acid sodium crystals；Add it to 200ml 3mol/L's
In salpeter solution, after stirring 0.5h, 39.68g Huang wolframic acids precipitation is obtained by filtration；Yellow wolframic acid is added to 400ml mass percents
For in the ammonium hydroxide of 25%-28%, slow mechanism dissolved for 24 hours after, it is 7 or so to take supernatant, 100 DEG C of ammonia still processs to pH value of solution, obtains wolframic acid
Ammonium salt solution；This ammonium tungstate solution is added in 280ml 4mol/L hydrochloric acid solutions, after stirring 2h, is aged 16h at room temperature, is passed through
6h is dried at 100 DEG C after filtration washing, obtains solid tungstic acid, 34.84g yellow tungsten trioxide powders are obtained after grinding.
Through XRD analysis, product is monoclinic system tungstic acid, as shown in Figure 5；Through experimental study, 3h is irradiated in 500W xenon lamps,
0.25g tungsten trioxide powders can make 50mg/L/ methylene blue solution degradation rates reach 92.18%, as shown in Figure 6.
The above is only a preferred embodiment of the present invention, it is not intended to restrict the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and
Modification, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of monoclinic system tungstic acid, which is characterized in that include the following steps：
(1) it uses nitric acid lixiviation process to remove the copper in copper-tungsten, obtains tungsten slag, the mass percentage of copper is at least low in tungsten slag
Tungsten slag is roasted at 0.5%, 400-600 DEG C obtains tungstic acid；
(2) tungstic acid is dissolved in aqueous slkali, and ammonium paratungstate or ammonium tungstate is obtained through ammonification；
(3) ammonium paratungstate or ammonium tungstate are configured to 1-2mol/L aqueous solutions, and are slowly added into the reproducibility acid of 3-4mol/L
Middle acidolysis stirs to get yellow wolframic acid colloid；
(4) yellow wolframic acid colloid is aged 16-24h at 20-35 DEG C, dries 6h at 100 DEG C after filtration washing, obtains monocline
Crystallographic system tungstic acid.
2. preparation method according to claim 1, it is characterised in that：The reproducibility acid is hydrochloric acid, sulfurous acid, vulcanization
One or more of hydrogen, HBr.
3. preparation method according to claim 1, it is characterised in that：In step (2), the aqueous slkali is ammonium hydroxide, three oxygen
Change tungsten and obtains ammonium paratungstate through ammonification, crystallization.
4. preparation method according to claim 1, it is characterised in that：In step (2), tungstic acid is dissolved in quality percentage
Than in the ammonia spirit for 25-28%, wherein the solid-liquid mass ratio of tungstic acid and ammonia spirit is 1:5-10, slow mechanism dissolved
12-24h takes supernatant, evaporative crystallization to obtain white crystal ammonium paratungstate.
5. preparation method according to claim 1, it is characterised in that：In step (2), by tungstic acid be dissolved in NaOH or
In KOH solution, crystallization obtains sodium tungstate or potassium tungstate, and sodium tungstate or potassium tungstate obtain ammonium tungstate after ammonification.
6. preparation method according to claim 1, it is characterised in that：In step (2), tungstic acid is dissolved in 5-10mol/
In L NaOH or KOH solution, wherein tungstic acid and NaOH or the solid-liquid mass ratio 1 of KOH solution:5-10 is stirred at 40-80 DEG C
Dissolving 5-10h is mixed, sodium tungstate or wolframic acid potassium solution are obtained, filtering, evaporative crystallization obtain sodium tungstate or potassium tungstate crystal.
7. preparation method according to claim 5, it is characterised in that：It crystallizes the obtained sodium tungstate or potassium tungstate is added
Into nitric acid, yellow wolframic acid precipitation is obtained, yellow wolframic acid precipitation is dissolved in ammonia spirit, ammonium tungstate is obtained after ammonification.
8. preparation method according to claim 7, it is characterised in that：Obtained wolframic acid sodium crystal is added to 1-3mol/L
In nitric acid, the wherein solid-to-liquid ratio 1 of wolframic acid sodium crystal and nitric acid:2-4, filtering solution obtain yellow wolframic acid precipitation, yellow wolframic acid are added
In 25-28% ammonia spirits, wherein the solid-to-liquid ratio of yellow wolframic acid and ammonia spirit is 1:After 5-10, slow mechanism dissolved 12-24h, filtering
Supernatant is taken, then the ammonia still process 30-60min at 60-100 DEG C, until pH value of solution is 6-7, obtains ammonium tungstate solution.
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| CN107115859A (en) * | 2017-04-05 | 2017-09-01 | 新疆师范高等专科学校 | The preparation method of tungsten trioxide nano crystalline substance photochemical catalyst |
| JP7125513B2 (en) * | 2018-05-11 | 2022-08-24 | エルジー エレクトロニクス インコーポレイティド | Method for producing transition metal oxide fine particles |
| CN108745341B (en) * | 2018-06-14 | 2021-01-15 | 深圳技术大学 | Preparation method of tungsten trioxide for catalyzing photodegradation of organic matters |
| CN109019691B (en) * | 2018-10-10 | 2021-04-06 | 江西省修水赣北钨业有限公司 | Preparation process of ammonium paratungstate |
| CN109647378B (en) * | 2018-12-17 | 2021-08-31 | 福州大学 | Preparation method of nanosheet self-assembled microsphere photocatalytic material for removing peculiar smell hydrogen sulfide |
| CN113861468B (en) * | 2021-10-11 | 2024-01-23 | 中国科学技术大学先进技术研究院 | Preparation method of photochromic tungsten oxide film and photochromic product |
| CN115784311A (en) * | 2022-11-24 | 2023-03-14 | 赣州市光华有色金属有限公司 | Method for recycling tungsten oxide through tungsten oxide waste |
| CN116639732A (en) * | 2023-06-05 | 2023-08-25 | 崇义章源钨业股份有限公司 | Method for preparing high-purity nano yellow-tungstic acid |
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| CN104118911B (en) * | 2014-07-11 | 2015-09-23 | 沈阳远大科技园有限公司 | A kind of method reclaiming tungstic oxide in discarded SCR catalyst completely |
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