CN213326765U - Device for producing low-silicon dry-process aluminum fluoride by using high-silicon fluorite powder - Google Patents
Device for producing low-silicon dry-process aluminum fluoride by using high-silicon fluorite powder Download PDFInfo
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- CN213326765U CN213326765U CN202021670990.7U CN202021670990U CN213326765U CN 213326765 U CN213326765 U CN 213326765U CN 202021670990 U CN202021670990 U CN 202021670990U CN 213326765 U CN213326765 U CN 213326765U
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Abstract
The utility model relates to an aluminium fluoride apparatus for producing technical field, concretely relates to utilize low silicon dry process aluminium fluoride device of high silicon fluorite powder production. The device for producing the low-silicon dry-method aluminum fluoride by using the high-silicon fluorite powder comprises an external heating type rotary reaction furnace, a pre-purification tower, a washing tower, an acid washing tower, a demister and a fluidized bed reactor which are sequentially connected; the external heating type rotary reaction furnace is connected with a fluorite storage tank and an acid mixing kettle; the top of the pre-purification tower is connected with the 1# emergency absorption spray tower and the 2# emergency absorption spray tower in sequence. The utility model discloses an utilize device of high silicon fluorite powder production low silicon dry process aluminium fluoride can adopt the fluorite production low silicon dry process aluminium fluoride of high impurity silicon content, has improved the purification degree of hydrogen fluoride gas, has avoided the waste of hydrogen fluoride gas, has reduced the manufacturing cost of aluminium fluoride, and the aluminium fluoride product index of production is qualified, has improved the market competition of product.
Description
Technical Field
The utility model relates to an aluminium fluoride apparatus for producing technical field, concretely relates to utilize low silicon dry process aluminium fluoride device of high silicon fluorite powder production.
Background
The dry-method aluminum fluoride production mainly comprises two parts of hydrogen fluoride preparation and aluminum fluoride synthesis. When fluorite is used for preparing hydrogen fluoride, the impurity silicon content in fluorite is high, which leads to high silicon content of hydrogen fluoride, so that the hydrogen fluoride needs to be subjected to desilication purification. The prior hydrogen fluoride desiliconization methods comprise a fluidized bed desiliconization method and a gas guide tube desiliconization method. Wherein, the fluidized bed desiliconization needs to use a large amount of nicotinic acid to generate free SO to achieve the ideal desiliconization effect3 2-A large amount of nicotinic acid is wasted, and Al formed by the reaction of sulfuric acid and alumina2(SO4)3Not only can lead to SO in the finished product sample4 2-Excessive standard, no temperature rise of the fluidized bed, Al2(SO4)3Too high a level may also lead to dead beds in the fluidized bed, resulting in SO in the finished sample4 2-The product is unqualified due to overhigh temperature; reaction of silicon dioxide with hydrogen fluoride gas and conversion of large amounts of HF gas to SiF4Enters tail gas absorption to cause a large amount of HF gas waste, and CaF in fluorite2The content is high, and the total yield is not increased; when SiF4After entering an atmospheric condensing tower, the reaction product reacts with water to obtain SiF4+2H2O←→SiO2+4HF, resulting in F in atmospheric condensation columns-Greatly improves the quality, needs a large amount of lime for neutralization, generates a large amount of sewage and increases the sewage treatment cost. Desiliconization of the gas-guide tube also causes a great deal of HF gas waste, and the waste degree is more serious than that of the fluidized bed desiliconization method; and the tail slag smoke is very large, which is contrary to the current safe environment protection situation.
In addition, the fluidized bed desiliconization method and the gas-guide tube desiliconization method require that the content of impurity silicon in fluorite is lower than 1.0 percent, so that a better desiliconization effect can be achieved during the desiliconization of hydrogen fluoride. Therefore, it is necessary to develop a device capable of producing low-silicon dry-process aluminum fluoride using high-silicon fluorite powder.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing an utilize low silicon dry process aluminium fluoride device of high silicon fluorite powder production, can adopt the low silicon dry process aluminium fluoride of fluorite production of high impurity silicon content, improved the purification degree of hydrogen fluoride gas, avoided the waste of hydrogen fluoride gas, reduced the manufacturing cost of aluminium fluoride, and the aluminium fluoride product index of production is qualified, has improved the market competition of product.
The device for producing the low-silicon dry-method aluminum fluoride by using the high-silicon fluorite powder comprises an external heating type rotary reaction furnace, a pre-purification tower, a washing tower, an acid washing tower, a demister and a fluidized bed reactor which are sequentially connected; the external heating type rotary reaction furnace is connected with a fluorite storage tank and an acid mixing kettle; the top of the pre-purification tower is connected with the 1# emergency absorption spray tower and the 2# emergency absorption spray tower in sequence.
The acid mixing kettle is connected with the high-position acid tank, and the pre-purification tower and the acid washing tower are connected with the high-position acid tank.
The 1# emergency absorption spray tower is connected with the 1# emergency absorption spray tank; and the 2# emergency absorption spray tower is connected with the 2# emergency absorption spray tank.
The top of the 2# emergency absorption spray tower is connected with a central absorption pipeline.
The washing tower is connected with the liquid collection kettle, and the liquid collection kettle is also connected with a recovery kettle.
A tail gas outlet of the fluidized bed reactor is connected with an inlet of the cyclone dust collector; and a dust outlet of the cyclone dust collector is connected with a feed inlet of the fluidized bed reactor, and a gas outlet of the cyclone dust collector is connected with a tail gas treatment pipeline.
The fluidized bed reactor is also connected with a product collecting pipeline.
The working process of the device for producing the low-silicon dry-process aluminum fluoride by using the high-silicon fluorite powder is as follows:
(1) preparing hydrogen fluoride: adding high-silicon fluorite powder in a fluorite storage tank and mixed sulfuric acid in an acid mixing kettle into an external heating type rotary reaction furnace for reaction to prepare crude hydrogen fluoride gas;
(2) hydrogen fluoride purification: turning an external heating typeCrude hydrogen fluoride gas generated in the furnace enters the pre-purification tower from the lower part of the pre-purification tower, fully contacts with pre-purification acid flowing reversely to wash off dust, sulfuric acid mist, water and partial impurities in the gas, enters from the bottom of a water washing tower and contacts with alkali wash flowing reversely to remove H in the hydrogen fluoride gas2SiF6And SiO2Spraying and washing until the bottom of the water washing tower forms colloidal crystals, placing the crystals outside after precipitation, and maintaining the liquid level of the water washing tower at 40 percent, wherein the liquid level is not too high so as to ensure that the hydrogen fluoride gas is discharged out of the tower after being fully contacted with water; the gas out of the tower enters an acid washing tower from the bottom to contact with acid washing liquid flowing reversely, redundant water is dried, evaporated and heated, and the purified hydrogen fluoride gas is separated from acid mist carried by the hydrogen fluoride gas through a demister to obtain pure hydrogen fluoride gas; wherein, the acid liquor flowing out of the pre-purification tower and the acid washing tower is introduced into a high-position acid tank for dehydration and is recycled as the raw material of the mixed sulfuric acid; the top of the pre-purification tower is connected with a No. 1 emergency absorption spray tower and a No. 2 emergency absorption spray tower in series, and the hydrogen fluoride gas is absorbed under emergency conditions to prevent environmental pollution;
(3) aluminum fluoride synthesis: introducing the purified hydrogen fluoride gas into the bottom of the fluidized bed reactor as fluidized gas, reacting with aluminum hydroxide added at the upper part of the fluidized bed reactor to obtain dry-process aluminum fluoride, treating tail gas by using a cyclone dust collector, introducing dust into the fluidized bed reactor for continuous reaction, and introducing the residual tail gas into a tail gas treatment pipeline for further treatment.
Compared with the prior art, the utility model discloses there is following beneficial effect:
(1) the utility model utilizes the water washing tower and the acid washing tower to purify and dry crude hydrogen fluoride gas, thereby not only avoiding the burden on the pre-purification tower and the acid cooling discharge, but also avoiding the waste of HF gas and being beneficial to improving the yield;
(2) the utility model leads the acid liquor flowing out from the pre-purification tower and the acid washing tower to the high-position acid tank for dehydration, and the acid liquor is recycled as the raw material of the mixed sulfuric acid, thereby effectively utilizing the acid liquor and reducing the cost;
(3) the top of the pre-purification tower is connected with the 1# emergency absorption spray tower and the 2# emergency absorption spray tower in series, so that the hydrogen fluoride gas is absorbed under emergency, the hydrogen fluoride gas is prevented from leaking, and the environmental pollution risk is reduced;
(4) the utility model discloses a device reforms transform, can adopt the fluorite production low silicon dry process aluminium fluoride of high impurity silicon content, not only ensures that the aluminium fluoride product index of production is qualified, reaches national standard AF-1 grade in the national standard GB/T4292-2007, has reduced the manufacturing cost of aluminium fluoride moreover, has improved the market competition of product.
Drawings
FIG. 1 is a schematic structural diagram of a device for producing low-silicon dry-process aluminum fluoride by using high-silicon fluorite powder;
in the figure: 1. a fluorite storage tank; 2. mixing an acid kettle; 3. a liquid collection kettle; 4. washing the tower with water; 5. a recovery kettle; 6. an acid washing tower; 7. a demister; 8. an aluminum hydroxide storage tank; 9. a fluidized bed reactor; 10. a cyclone dust collector; 11. a tail gas treatment pipeline; 12. a high acid tank; 13. an external heating type rotary reaction furnace; 14. a pre-purification tower; 15. 1# emergency absorption spray tank; 16. 1# emergency absorption spray tower; 17. 2# emergency absorption spray tank; 18. 2# emergency absorption spray tower; 19. a central absorption line; 20. a product collection line.
Detailed Description
The present invention will be further described with reference to the following examples, but the scope of the present invention is not limited thereto.
Example 1
As shown in fig. 1, a device for producing low-silicon dry-process aluminum fluoride by using high-silicon fluorite powder comprises an external heating type rotary reaction furnace 13, a pre-purification tower 14, a water washing tower 4, an acid washing tower 6, a demister 7 and a fluidized bed reactor 9 which are connected in sequence; the external heating type rotary reaction furnace 13 is connected with the fluorite storage tank 1 and the acid mixing kettle 2; the fluidized bed reactor 9 is connected with an aluminum hydroxide storage tank 8; the top of the pre-purification tower 14 is connected with a # 1 emergency absorption spray tower 16 and a # 2 emergency absorption spray tower 18 in sequence.
The acid mixing kettle 2 is connected with a high-position acid tank 12, and the pre-purification tower 14 and the acid washing tower 6 are connected with the high-position acid tank 12.
The 1# emergency absorption spray tower 16 is connected with the 1# emergency absorption spray tank 15; the 2# emergency absorption spray tower 18 is connected to the 2# emergency absorption spray tank 17.
The top of the 2# emergency absorption spray tower 18 is connected with a central absorption pipeline 19.
The washing tower 4 is connected with the liquid collection kettle 3, and the liquid collection kettle 3 is also connected with a recovery kettle 5.
A tail gas outlet of the fluidized bed reactor 9 is connected with an inlet of a cyclone dust collector 10; a dust outlet of the cyclone 10 is connected with a feed inlet of the fluidized bed reactor 9, and a gas outlet of the cyclone 10 is connected with a tail gas treatment pipeline 11.
The fluidized-bed reactor 9 is also connected to a product take-up line 20.
The working process of the device for producing the low-silicon dry-process aluminum fluoride by using the high-silicon fluorite powder is as follows:
(1) preparing hydrogen fluoride: adding high-silicon fluorite powder in a fluorite storage tank 1 and mixed sulfuric acid in an acid mixing kettle 2 into an external heating type rotary reaction furnace 13 for reaction to prepare crude hydrogen fluoride gas;
(2) hydrogen fluoride purification: crude hydrogen fluoride gas generated in the external heating type rotary furnace 13 enters the pre-purification tower 14 from the lower part thereof, fully contacts with pre-purification acid flowing reversely to wash off dust, sulfuric acid mist, water and partial impurities in the gas, enters from the bottom of the water washing tower 4, contacts with alkaline washing liquid flowing reversely to remove H in the hydrogen fluoride gas2SiF6And SiO2Spraying and washing until colloidal crystals are formed at the bottom of the water washing tower 4, externally discharging after precipitation, and maintaining the liquid level of the water washing tower 4 at 40 percent, wherein the liquid level is not too high so as to ensure that the hydrogen fluoride gas is fully contacted with water and then is discharged out of the tower; the gas out of the tower enters an acid washing tower 6 from the bottom to contact with acid washing liquid flowing reversely, redundant water is dried, evaporated and heated, and the purified hydrogen fluoride gas is separated from acid mist carried by the hydrogen fluoride gas through a demister 7 to obtain pure hydrogen fluoride gas; wherein, the acid liquor flowing out of the pre-purification tower 14 and the acid washing tower 6 is introduced into the high-position acid tank 12 for dehydration and is recycled as the raw material of the mixed sulfuric acid; the top of the pre-purification tower 14 is connected with a 1# emergency absorption spray tower 16 and a 2# emergency absorption spray tower 18 in series, and the hydrogen fluoride gas is absorbed under emergency conditions, so that the environment is prevented from being polluted;
(3) aluminum fluoride synthesis: purified hydrogen fluoride gas is introduced into the bottom of the fluidized bed reactor 9 to be used as fluidized gas and reacts with aluminum hydroxide added to the upper part of the fluidized bed reactor 9 to obtain dry-process aluminum fluoride, tail gas is treated by the cyclone dust collector 10, dust is introduced into the fluidized bed reactor 9 to continue to react, and the rest tail gas is introduced into the tail gas treatment pipeline 11 to be further treated.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The utility model provides an utilize low silicon dry process aluminium fluoride device of high silica fluorite powder production which characterized in that: comprises an external heating type rotary reaction furnace (13), a pre-purification tower (14), a water washing tower (4), an acid washing tower (6), a demister (7) and a fluidized bed reactor (9) which are connected in sequence; the external heating type rotary reaction furnace (13) is connected with the fluorite storage tank (1) and the acid mixing kettle (2); the fluidized bed reactor (9) is connected with an aluminum hydroxide storage tank (8); the top of the pre-purification tower (14) is connected with a 1# emergency absorption spray tower (16) and a 2# emergency absorption spray tower (18) in sequence.
2. The apparatus for producing low-silicon dry aluminum fluoride by using high-silicon fluorite powder according to claim 1, which is characterized in that: the acid mixing kettle (2) is connected with the high-position acid tank (12), and the pre-purification tower (14) and the acid washing tower (6) are connected with the high-position acid tank (12).
3. The apparatus for producing low-silicon dry aluminum fluoride by using high-silicon fluorite powder according to claim 1, which is characterized in that: the 1# emergency absorption spray tower (16) is connected with the 1# emergency absorption spray tank (15); the 2# emergency absorption spray tower (18) is connected with the 2# emergency absorption spray tank (17).
4. The apparatus for producing low-silicon dry aluminum fluoride by using high-silicon fluorite powder according to claim 1, which is characterized in that: the top of the 2# emergency absorption spray tower (18) is connected with a central absorption pipeline (19).
5. The apparatus for producing low-silicon dry aluminum fluoride by using high-silicon fluorite powder according to claim 1, which is characterized in that: the water washing tower (4) is connected with the liquid collection kettle (3), and the liquid collection kettle (3) is also connected with a recovery kettle (5).
6. The apparatus for producing low-silicon dry aluminum fluoride by using high-silicon fluorite powder according to claim 1, which is characterized in that: a tail gas outlet of the fluidized bed reactor (9) is connected with an inlet of the cyclone dust collector (10); a dust outlet of the cyclone dust collector (10) is connected with a feed inlet of the fluidized bed reactor (9), and a gas outlet of the cyclone dust collector (10) is connected with a tail gas treatment pipeline (11).
7. The apparatus for producing low-silicon dry aluminum fluoride by using high-silicon fluorite powder according to claim 1, which is characterized in that: the fluidized bed reactor (9) is also connected with a product collecting pipeline (20).
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| CN202021670990.7U CN213326765U (en) | 2020-08-12 | 2020-08-12 | Device for producing low-silicon dry-process aluminum fluoride by using high-silicon fluorite powder |
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| CN202021670990.7U CN213326765U (en) | 2020-08-12 | 2020-08-12 | Device for producing low-silicon dry-process aluminum fluoride by using high-silicon fluorite powder |
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