CN111517348A - Production process for regenerating aluminum fluoride by using aluminum fluoride production tail gas washing liquid - Google Patents
Production process for regenerating aluminum fluoride by using aluminum fluoride production tail gas washing liquid Download PDFInfo
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- CN111517348A CN111517348A CN202010252227.0A CN202010252227A CN111517348A CN 111517348 A CN111517348 A CN 111517348A CN 202010252227 A CN202010252227 A CN 202010252227A CN 111517348 A CN111517348 A CN 111517348A
- Authority
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- China
- Prior art keywords
- aluminum fluoride
- production
- tail gas
- washing liquid
- regenerating
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 42
- 239000007788 liquid Substances 0.000 title claims abstract description 32
- 238000005406 washing Methods 0.000 title claims abstract description 26
- 230000001172 regenerating effect Effects 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002674 ointment Substances 0.000 claims abstract description 15
- 239000002351 wastewater Substances 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 13
- 239000012452 mother liquor Substances 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000001179 sorption measurement Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000004064 recycling Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000004806 packaging method and process Methods 0.000 claims abstract description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 23
- 238000006386 neutralization reaction Methods 0.000 claims description 11
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 10
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 4
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 4
- 239000004571 lime Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 3
- 239000010436 fluorite Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 3
- 239000013589 supplement Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 16
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052731 fluorine Inorganic materials 0.000 abstract description 10
- 239000011737 fluorine Substances 0.000 abstract description 10
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 16
- 229910001610 cryolite Inorganic materials 0.000 description 6
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/50—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/22—Fluorides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a production process for regenerating aluminum fluoride by utilizing tail gas washing liquid in aluminum fluoride production, which is to carry out solid-liquid adsorption reaction on the tail gas washing liquid in the aluminum fluoride production and aluminum oxide in a synthesis tank; filtering the solid-liquid mixture after the adsorption reaction to obtain solid aluminum fluoride ointment, drying the aluminum fluoride ointment, discharging, cooling and packaging to obtain an aluminum fluoride finished product; and discharging the filtered mother liquor into a waste water tank, and performing circulating cooling to replenish water for an aluminum fluoride production tail gas washing system so as to realize the recycling of water. The process effectively recovers the fluorine element in the tail gas washing liquid of the aluminum fluoride production system, is simple to operate, has no wastewater discharge in the process, realizes the economic recycling of water, reduces the production cost, and is beneficial to environmental protection.
Description
Technical Field
The invention relates to a process for regenerating fluoride salt in tail gas washing liquid, in particular to a process for regenerating aluminum fluoride by using tail gas washing liquid produced by aluminum fluoride.
Background
Aluminum fluoride is generally directly prepared by reacting hydrogen fluoride gas and aluminum hydroxide in a fluidized bed, and the method for preparing aluminum fluoride can obtain high-quality products and is rapidly developed in China in recent years. However, a large amount of tail gas containing hydrogen fluoride is generated after the hydrogen fluoride reacts with the aluminum hydroxide, the tail gas needs to be washed to ensure that the tail gas reaches the standard and is discharged, and a large amount of fluorine-containing wastewater with low concentration is generated in the tail gas washing process. At present, the treatment of the fluorine-containing wastewater mainly comprises the production of cryolite, although the production cost is low, the cryolite is gradually eliminated by the market and cannot meet the market demand, a large amount of cryolite stock can be caused by continuous production, a large amount of capital overstocks are caused, great economic benefit loss is caused, and great environmental protection pressure is caused due to the fact that the cryolite cannot be properly treated. Therefore, a new process and a new method are urgently needed to be found for transforming the original treatment mode of the tail gas washing liquid in the aluminum fluoride production into another product so as to achieve the purposes of wastewater treatment, fluorine recycling and cost reduction.
Disclosure of Invention
Aiming at the technical problems, the invention provides a process for regenerating aluminum fluoride by utilizing a tail gas washing liquid generated in the production of aluminum fluoride, the aluminum fluoride generated by the process effectively replaces cryolite, and the aim of treating fluorine-containing wastewater is fulfilled.
The invention relates to a process for regenerating aluminum fluoride by using a washing liquid of tail gas in aluminum fluoride production, which comprises the following steps:
(1) the aluminum fluoride production tail gas washing liquid in the washing tank and the aluminum oxide are subjected to solid-liquid adsorption reaction in the synthesis tank, wherein the reaction formula is Al2O3+6HF=2AlF3+3H2O；
(2) Filtering the solid-liquid mixture after the adsorption reaction in the step (1) to obtain solid aluminum fluoride ointment, drying the aluminum fluoride ointment, discharging, cooling and packaging to obtain an aluminum fluoride finished product;
(3) discharging the filtered mother liquor obtained in the step (2) into a waste water tank, and performing circulating cooling to supplement water for an aluminum fluoride production tail gas washing system so as to realize the recycling of water;
(4) discharging redundant mother liquor in the waste water tank into a neutralization tank, and adding lime for neutralization reaction;
(5) and (4) filtering the solid-liquid mixture obtained after the neutralization reaction in the step (4) to obtain solid calcium fluoride ointment, mixing the calcium fluoride ointment into wet fluorite, and drying to obtain the anhydrous hydrofluoric acid production raw material.
Further, in the step (1), the concentration of hydrofluoric acid in the cleaning solution is 2.5-3.0 g/L, the mass-to-volume ratio of the alumina to the cleaning solution is 2.6-3.2 g/L, the reaction temperature is 70-85 ℃, and the pH of the reaction end point is = 4-5.
Further, in the step (2), the drying temperature is 550-650 ℃.
Further, in the step (3), the temperature of the mother liquor is 20-25 ℃ after being cooled.
Furthermore, in the step (4), the concentration of hydrofluoric acid in the mother liquor is 0.5-1 g/L.
Further, in the step (4), the neutralization reaction temperature is 20-25 ℃, the reaction time is 0.5-1.0 h, and the pH value of the reaction end point is 6-7.
And further, in the step (5), the filtered filtrate is discharged into a water storage tank and is used for supplementing water to a cooling system, so that the primary water consumption is reduced, and the economic recycling of water is realized.
The invention has the beneficial effects that:
1. the process effectively recovers the fluorine element in the tail gas washing liquid of the aluminum fluoride production system, converts the fluorine element into the aluminum fluoride, realizes the purpose that the aluminum fluoride replaces cryolite and achieves the treatment of the fluorine-containing wastewater, and reduces the environmental pollution caused by the discharge of fluorine.
2. According to the process, the redundant mother liquor in the wastewater tank is added with lime, so that the fluorine element is further recovered, the generated calcium fluoride can be used as a raw material for anhydrous hydrofluoric acid production, and the production cost is saved.
3. The process is simple to operate, no wastewater is discharged in the process, the economic recycling of water is realized, the production cost is reduced, and the process is beneficial to environmental protection.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The present invention is further illustrated by the following specific embodiments.
(1) Discharging the cleaning solution of tail gas generated in the production of aluminum fluoride in the cleaning tank into a No. 1 tank of a synthesis tank, wherein the concentration of hydrofluoric acid in the cleaning solution is 2.5-3.0 g/L, uniformly adding aluminum oxide into the No. 1 tank of the synthesis tank for adsorption reaction, wherein the reaction formula is Al2O3+6HF=2AlF3+3H2And O, the adding amount of the alumina is 2.6-3.2 g/L, stirring is carried out at the stirring speed of 220r/min, then solid and liquid overflows from the No. 1 synthesis tank enter the No. 2, No. 3 and No. 4 synthesis tanks to realize full reaction, the reaction temperature is controlled to be 70 ℃, and the pH of the reaction end point is = 4-5.
(2) Filtering the solid-liquid mixture after the adsorption reaction by a plate-and-frame filter to realize solid-liquid separation to obtain solid aluminum fluoride ointment, discharging the aluminum fluoride ointment into an aluminum fluoride ointment box, drying by a flash evaporation dryer at the drying temperature of 550 ℃ and the discharging temperature of 180 ℃, conveying the materials into a finished product bin through a secondary conveying process, naturally cooling and packaging to obtain the finished product of aluminum fluoride.
(3) Mother liquor obtained by filtering after adsorption reaction is discharged into a waste water tank, and is used for replenishing water for an aluminum fluoride production tail gas washing system after being cooled to 25 ℃ through circulating cooling, so that the cyclic utilization of water is realized.
(4) And (3) allowing redundant mother liquor in the waste water tank to enter a neutralization tank, wherein the concentration of hydrofluoric acid in the mother liquor is 0.5-1 g/L, adding lime for neutralization reaction, and arranging 2 neutralization tanks in series to ensure full reaction, wherein the pH value at the end point of the reaction is 6-7, the reaction temperature is 25 ℃, and the reaction time is 1.0 h.
(5) And filtering the solid-liquid mixture after the reaction is finished by a plate and frame filter to obtain solid calcium fluoride ointment, mixing the calcium fluoride ointment into wet fluorite, drying the mixture to be used as a production raw material of anhydrous hydrofluoric acid, discharging the filtrate filtered by the plate and frame filter into a water storage tank for supplementing water to a cooling system, reducing the consumption of primary water and realizing the economic recycling of the water.
Claims (7)
1. A production process for regenerating aluminum fluoride by utilizing a washing liquid of tail gas generated in the production of aluminum fluoride is characterized by comprising the following steps of:
(1) carrying out solid-liquid adsorption reaction on the aluminum fluoride production tail gas washing liquid and aluminum oxide in a synthesis tank;
(2) filtering the solid-liquid mixture after the adsorption reaction in the step (1) to obtain solid aluminum fluoride ointment, drying the aluminum fluoride ointment, discharging, cooling and packaging to obtain an aluminum fluoride finished product;
(3) discharging the filtered mother liquor obtained in the step (2) into a waste water tank, and performing circulating cooling to supplement water for an aluminum fluoride production tail gas washing system so as to realize the recycling of water;
(4) discharging redundant mother liquor in the waste water tank into a neutralization tank, and adding lime for neutralization reaction;
(5) and (4) filtering the solid-liquid mixture obtained after the neutralization reaction in the step (4) to obtain solid calcium fluoride ointment, mixing the calcium fluoride ointment into wet fluorite, and drying to obtain the anhydrous hydrofluoric acid production raw material.
2. The production process for regenerating aluminum fluoride by using the washing liquid of the tail gas from the production of aluminum fluoride according to claim 1, which is characterized in that: in the step (1), the concentration of hydrofluoric acid in the cleaning solution is 2.5-3.0 g/L, the mass-to-volume ratio of the alumina to the cleaning solution is 2.6-3.2 g/L, the reaction temperature is 70-85 ℃, and the pH of the reaction end point is = 4-5.
3. The production process for regenerating aluminum fluoride by using the washing liquid of the tail gas from the production of aluminum fluoride according to claim 1, which is characterized in that: in the step (2), the drying temperature is 550-650 ℃.
4. The production process for regenerating aluminum fluoride by using the washing liquid of the tail gas from the production of aluminum fluoride according to claim 1, which is characterized in that: in the step (3), the temperature of the mother liquor is 20-25 ℃ after being cooled.
5. The production process for regenerating aluminum fluoride by using the washing liquid of the tail gas from the production of aluminum fluoride according to claim 1, which is characterized in that: in the step (4), the concentration of hydrofluoric acid in the mother liquor is 0.5-1 g/L.
6. The production process for regenerating aluminum fluoride by using the washing liquid of the tail gas from the production of aluminum fluoride according to claim 1, which is characterized in that: in the step (4), the neutralization reaction temperature is 20-25 ℃, the reaction time is 0.5-1.0 h, and the pH value of the reaction end point is 6-7.
7. The production process for regenerating aluminum fluoride by using the washing liquid of the tail gas from the production of aluminum fluoride according to claim 1, which is characterized in that: and (5) discharging the filtered filtrate into a water storage tank for supplementing water to a cooling system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010252227.0A CN111517348A (en) | 2020-04-01 | 2020-04-01 | Production process for regenerating aluminum fluoride by using aluminum fluoride production tail gas washing liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010252227.0A CN111517348A (en) | 2020-04-01 | 2020-04-01 | Production process for regenerating aluminum fluoride by using aluminum fluoride production tail gas washing liquid |
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| CN111517348A true CN111517348A (en) | 2020-08-11 |
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| CN202010252227.0A Pending CN111517348A (en) | 2020-04-01 | 2020-04-01 | Production process for regenerating aluminum fluoride by using aluminum fluoride production tail gas washing liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112520770A (en) * | 2020-12-17 | 2021-03-19 | 河南中色东方韶星实业有限公司 | Comprehensive utilization method of atmospheric condensate |
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2020
- 2020-04-01 CN CN202010252227.0A patent/CN111517348A/en active Pending
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| JPH10137744A (en) * | 1996-11-11 | 1998-05-26 | Nec Corp | Treatment of waste water containing fluorine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112520770A (en) * | 2020-12-17 | 2021-03-19 | 河南中色东方韶星实业有限公司 | Comprehensive utilization method of atmospheric condensate |
| CN112520770B (en) * | 2020-12-17 | 2023-04-07 | 河南东方韶星实业有限公司 | Comprehensive utilization method of atmospheric condensate |
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Application publication date: 20200811 |