CN1056092A - Producing V 2 O 5 from decomposing bone coal by hydrofluoric acid - Google Patents
Producing V 2 O 5 from decomposing bone coal by hydrofluoric acid Download PDFInfo
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- CN1056092A CN1056092A CN 91102560 CN91102560A CN1056092A CN 1056092 A CN1056092 A CN 1056092A CN 91102560 CN91102560 CN 91102560 CN 91102560 A CN91102560 A CN 91102560A CN 1056092 A CN1056092 A CN 1056092A
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Abstract
The present invention's " producing V 2 O 5 from decomposing bone coal by hydrofluoric acid " method is bone coal, fluorite to be mixed add sulfuric acid acidation decomposition, solid-liquid separation, the filtrate neutralization precipitation, the filter cake high temperature pyrolysis, oxidizer adds alkali, filter, filter cake makes red iron oxide, and the filtrate ammonium is separated, and filters, filter cake makes aluminium hydroxide, and filtrate is by 717
#Exchange column, the elutriant ammoniumization is separated, and the ignition of precipitate branch solves pure Vanadium Pentoxide in FLAKES, stone coal vanadium-containing 0.75%, total yield 〉=60%, benefit is obvious.
Description
The present invention relates to bone coal and produce the Vanadium Pentoxide in FLAKES technical field.
At present, bone coal is produced Vanadium Pentoxide in FLAKES and is all adopted the stone coal sodium roasting method both at home and abroad, Chinese patent literature retrieval is on the books: 1. stone coal ash sulfuric acid is mixed the acid slaking water logging of heating and is extracted Vanadium Pentoxide in FLAKES technical process (application number 90104669.8, document number 1049642A), 2. produce the sinter process (application number 89105480.4 of Vanadium Pentoxide in FLAKES, document number 1049141A), the stone coal sodium roasting method, process gas is seriously polluted, vanadium total yield low (being no more than 50%), associated element is difficult in the bone coal reclaims, the production cost height, 1. patent documentation is that 2. patent documentation is to be the raw material production Vanadium Pentoxide in FLAKES with the vanadium slag with bone coal fluidizing furnace lime-ash raw material production Vanadium Pentoxide in FLAKES, and above-mentioned technology does not all relate to hydrofluoric acid and decomposes bone coal.
" producing V 2 O 5 from decomposing bone coal by hydrofluoric acid " disclosed by the invention method, be to be raw material with the bone coal, be aided with the fluorite powder, sulfuric acid, a new operational path that uses general acid-resistant system and design, this technical process overcomes waste gas fully, waste water is to the pollution of environment, average acidleach rate of decomposition 〉=75% of vanadium, the total yield of vanadium 〉=60%, the iron of 50-60% and aluminium generate red iron oxide and two kinds of byproducts of aluminium hydroxide in the bone coal, other associated element is also recyclable in the bone coal, this method is produced comprehensive cost and is descended significantly, and the bone coal comprehensive utilization value improves, and benefit is obvious.
Below, technical solution of the present invention is illustrated it in detail.
The chemical principle of production technique of the present invention: vanadium is mainly composed in the illite that exists in the bone coal, titanium scherbinaite garnet, the chrome alum garnet, these three kinds of mineral belong to aluminum silicate mineral and silicates mineral, hydrofluoric acid is under normal temperature condition, but analysing silicon Barbiturates mineral, destroy its structure, make vanadium enter solution, for example:
In the production process, hydrofluoric acid is to be generated in same conversion unit by fluorite powder and sulfuric acid, bone coal, hydrofluoric acid reacts with bone coal after generating immediately, the vanadylic sulfate that generates enters solution, after the solid-liquid separation, adjusts solution PH 4～4.5, vanadium, aluminium, part iron produce co-precipitation at this moment, behind the suction strainer, filtrate cycle is used to decompose bone coal, the precipitation thermal degradation, under alkalescence (PH 〉=10) condition, oxidizer heated oxide and conversion, filtering separation, filter residue prepares red iron oxide, filtrate adds precipitation agent carbon ammonium, separate, filter residue is produced aluminium hydroxide, and filtrate is through 717
#The strongly basic anion exchange column, with sodium-chlor and ammonium chloride mixed solution wash-out, elutriant adds ammonium chloride to the ammonium meta-vanadate precipitation that generates white, is deposited in that calcination gets Vanadium Pentoxide in FLAKES under 550 ℃ of conditions.
The technological process of production of the present invention such as figure below.
One embodiment of the present of invention: get stone coal powder 100 grams (granularity 100%-60 order), 200 milliliters of fluorite powder 20-25 gram (or 20-25 milliliter 40% hydrofluoric acid) 5% sulphuric acid solns, 100 milliliters in water (solid-to-liquid ratio=1: 2.5～3.0 this moment), place 1000 milliliters beaker, be heated on the electric furnace about 80 ℃, react after 30 minutes, cooling, vacuum filtration, filter residue washes with water 3 times, filtrate and washing lotion are merged into blue look and are contained vanadium solution, under continuous stirring condition, in blue look solution, add the carbon ammonium and be neutralized to PH4～4.5, at this moment vanadium, aluminium and part iron produce co-precipitation, the vacuum suction filter precipitation, and washing precipitation 2 times, washing lotion and filtrate merge (fluoride) circulation and are used for the bone coal decomposition, be deposited in the box-type furnace under 550 ℃ of conditions thermal degradation 60～80 minutes, pulverize the cooling back, oxidizer, under alkalescence (PH 〉=10) condition, heated oxide and conversion, vacuum suction filter, the washing filter residue is (with the filter residue oven dry and be crushed to the 100%-200 order, make red iron oxide) for several times, and washing lotion and filtrate merge, add a spot of precipitation agent carbon ammonium, stir, make the aluminum hydroxide precipitation of even white, vacuum suction filter, washing (will precipitate oven dry and pulverizing for several times, make aluminium hydroxide), washing lotion and filtrate merge, through 717
#The strong basicity cationic exchange coloum, the absorption back goes out the vanadium that adsorbs on the post with sodium-chlor and ammonium chloride mixing elutriant wash-out, add a spot of ammonium chloride, stir, obtain the ammonium meta-vanadate precipitation of white, the vacuum suction filter precipitation, and wash 2 times, drain calcination a few hours under 550 ℃ of conditions, make 〉=98% pure Vanadium Pentoxide in FLAKES the total yield of vanadium 〉=60%.
It is as follows to implement record:
| Numbering | Bone coal 100 grams contain vanadium % | Sulfuric acid (5%) milliliter | Hydrofluoric acid (40%) milliliter | Fluorite powder gram | Water-soluble vanadium gram | Acidleach rate % | Tailings contains the vanadium gram |
| 1 | 0.71 | 200 | 25 | 0.58 | 81.70 | 0.11 | |
| 2 | 0.71 | 200 | 25 | 0.50 | 70.42 | ||
| 3 | 0.77 | 100 | 25 | 0.60 | 77.92 | 0.15 | |
| 4 | 0.77 | 200 | 25 | 0.52 | 67.53 | ||
| 5 | 0.77 | 200 | 30 | 0.58 | 75.32 | ||
| 6 | 0.73 | 150 | 25 | 0.67 | 91.78 |
The total yield P=P of vanadium
1* P
2* P
3* P
4* P
5-5% process loss=75% * 97% * 97% * 97% * 97%-5%=61.4%
In the formula: P
1Average acidleach rate 〉=75% of=vanadium
P
2=tetravalence vanadium solubility rate 〉=97%
P
3=tetravalence vanadium deposition rate 〉=97%
P
4=exchange adsorption rate 〉=97%
P
5=elution efficiency 〉=97%
Utilize above-mentioned technical process, utilize general acidproof production unit, feed intake at bone coal and implement 100 kilograms for tens times, obtain the result and be: average acidleach rate of decomposition 〉=75% of vanadium;
The total yield of vanadium 〉=60%.
The iron of 50-60% and aluminium obtain reclaiming in the bone coal.217 tons of bone coals (containing vanadium 0.75%) can be produced 1 ton of Vanadium Pentoxide in FLAKES, 14 tons of red iron oxides, 5 tons in aluminium hydroxide.
Claims (3)
1, a kind ofly produces the production technique of the method, particularly producing V 2 O 5 from decomposing bone coal by hydrofluoric acid of Vanadium Pentoxide in FLAKES, it is characterized in that bone coal, fluorite are added sulfuric acid acidation to be decomposed with bone coal, the filtrate neutralization precipitation, alkali is molten behind the precipitation high temperature pyrolysis, filters the filtrate ammonium and separates, filter then, filtrate is by 717
#Exchange column, centrifugation gets inclined to one side ammonium after the elutriant ammoniumization, and the inclined to one side ammonium of calcination gets pure Vanadium Pentoxide in FLAKES.
2, the method for claim 1 is characterized in that the filter cake of the molten after-filtration of alkali can make red iron oxide.
3, production method as claimed in claim 1 is characterized in that ammonium separates the filter cake of after-filtration and can make aluminium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91102560 CN1056092A (en) | 1991-04-18 | 1991-04-18 | Producing V 2 O 5 from decomposing bone coal by hydrofluoric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91102560 CN1056092A (en) | 1991-04-18 | 1991-04-18 | Producing V 2 O 5 from decomposing bone coal by hydrofluoric acid |
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| Publication Number | Publication Date |
|---|---|
| CN1056092A true CN1056092A (en) | 1991-11-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91102560 Pending CN1056092A (en) | 1991-04-18 | 1991-04-18 | Producing V 2 O 5 from decomposing bone coal by hydrofluoric acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099484A (en) * | 2014-07-31 | 2014-10-15 | 武汉科技大学 | Method for extracting vanadium by roasting vanadium-containing stone coal in size fraction grading and fluidization manner |
| CN107354303A (en) * | 2017-07-18 | 2017-11-17 | 东北大学 | A kind of water logging vanadium extraction waste removing sodium technology |
| CN107573516A (en) * | 2017-09-11 | 2018-01-12 | 东北石油大学 | A kind of preparation method of vanadium modified metal organic framework material |
-
1991
- 1991-04-18 CN CN 91102560 patent/CN1056092A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099484A (en) * | 2014-07-31 | 2014-10-15 | 武汉科技大学 | Method for extracting vanadium by roasting vanadium-containing stone coal in size fraction grading and fluidization manner |
| CN107354303A (en) * | 2017-07-18 | 2017-11-17 | 东北大学 | A kind of water logging vanadium extraction waste removing sodium technology |
| CN107573516A (en) * | 2017-09-11 | 2018-01-12 | 东北石油大学 | A kind of preparation method of vanadium modified metal organic framework material |
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