CN105502451A - Method for producing aluminum fluoride and co-produced high-molecular ratio cryolite - Google Patents
Method for producing aluminum fluoride and co-produced high-molecular ratio cryolite Download PDFInfo
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- CN105502451A CN105502451A CN201511017661.6A CN201511017661A CN105502451A CN 105502451 A CN105502451 A CN 105502451A CN 201511017661 A CN201511017661 A CN 201511017661A CN 105502451 A CN105502451 A CN 105502451A
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- aluminum fluoride
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- 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
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- 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
- C01F7/54—Double compounds containing both aluminium and alkali metals or alkaline-earth metals
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Abstract
The invention discloses a method for producing aluminum fluoride and co-produced high-molecular ratio cryolite. The method comprises the following steps: (1) preparation of aluminum fluoride: heating fluosilicic acid of which the concentration is 13 to 14 percent to be 65 to 75 DEG C through a heat exchanger, and carrying out a stirring reaction on the fluosilicic acid and aluminum hydroxide under 70 to 80 DEG C for 12 to 16 minutes; then obtaining the aluminum fluoride through filtering and desiliconizing, crystallizing, drying, calcining and cooling; (2) preparation of the high-molecular ratio cryolite: carrying out the stirring reaction on a filtered aluminum fluoride mother solution and sodium fluoride under 80 to 90 DEG C for 50 to 60 minutes, filtering a reactant after the reaction is completed, feeding filtrate in a sewage pool for being treated, carrying out flash drying on a filter cake under 120 to 150 DEG C, and obtaining the high-molecular ratio cryolite. The aluminum fluoride prepared by the invention is low in concentration, is stable and is high in yield; the co-produced high-molecular ratio cryolite is high in quality and also high in yield; meanwhile, only the aluminum fluoride mother solution is brought in sewage during a production process, so compared with other production technologies, the method disclosed by the invention has the advantages of less sewage quantity and easiness in treatment.
Description
Technical field
The present invention relates to a kind of method of producing aluminum fluoride coproduction cryolite with high molecular ratio from, be specifically related to a kind of method utilizing low dose fluoride silicic acid to produce aluminum fluoride coproduction cryolite with high molecular ratio from.
Background technology
Aluminum fluoride is the important intermediate of the fluosilicic acid as byproduct direct synthesis technique ice making spar in fluorite and phophatic fertilizer production process, is mainly used in aluminium metallurgy and produces.Sodium aluminum fluoride, also claims sodium fluoroaluminate, and its molecular formula is Na
3alF
6, by the ratio of its Sodium Fluoride with the molecule of aluminum fluoride, cryolite with high molecular ratio from and lower molecular ratio sodium aluminum fluoride can be divided into.Wherein, cryolite with high molecular ratio from (nNaF.AlF
3, n:2.8 ~ 3.0) and be based on the mixture of positive sodium aluminum fluoride, can be used as the solubility promoter of aluminum smelting industry, there is volatilization loss few, Heat stability is good, the advantage that environmental pollution is little, in environment protection and economic benefit etc., be all better than low molecule sodium aluminum fluoride.But each electrolytic aluminium factory major part of Present Domestic uses molecular ratio to be the ionogen of the lower molecular ratio ice crystal masonry electrolysis of aluminum of 1.8 ~ 2.2.Therefore, investigation and application cryolite with high molecular ratio from makes the ionogen of electrolysis of aluminum, has been the task of top priority, and the meanwhile preparation of aluminum fluoride is the critical process of synthesis cryolite with high molecular ratio from.
At present, when tradition direct synthesis technique produces aluminum fluoride and cryolite with high molecular ratio from, silicofluoric acid is mainly derived from the by product in fluorite and phophatic fertilizer production process, concentration is between 18 ~ 20%, produce more intermediate product hydrogen fluoride gas or hydrogen-oxygen acid, all propose higher requirement to the selection of production unit material and environment protection; Meanwhile, original silicofluoric acid concentration is higher, and the aluminum fluoride concentration of generation is corresponding also high, more early crystallization, and aluminum fluoride yield reduces.And original silicofluoric acid concentration is lower, speed of response is slow, and the silica crystals particle of precipitation is thin, and slip is colloidal, and viscosity is large, hinders the reaction with aluminium hydroxide, and filtration velocity is slow simultaneously, and filter cake washing difficulty, in filter cake, liquid content is high, and aluminum fluoride yield reduces.Therefore, the aluminun fluoride solution of a kind of lower concentration of research preparation, high stability, to coproduction cryolite with high molecular ratio from, has important industrial value.
Summary of the invention
Technical problem to be solved by this invention is, what provide a kind of high yield utilizes lower concentration H
2siF
6produce the method for aluminum fluoride coproduction cryolite with high molecular ratio from.
The technical scheme that the present invention solves the employing of its technical problem is that a kind of method of producing aluminum fluoride coproduction cryolite with high molecular ratio from, comprises the following steps:
(1) react: be that 13 ~ 14% (preferred concentration is 13%) silicofluoric acid is heated to 65 DEG C ~ 75 DEG C by interchanger by concentration, then reactor is added after metering, then the aluminium hydroxide of metering is added, wherein, the metering of silicofluoric acid and aluminium hydroxide is than being 1:1.01 ~ 1:1.05 (preferably measure than be 1: 1.02), at 70 ~ 80 DEG C (preferably 80 DEG C), stirring reaction 12 ~ 16min (the preferred reaction time is 16min), after completion of the reaction, rinse resultant product in reactive tank with water, merge with reaction product;
(2) desiliconization, crystallization, cooling: the reaction product merged is filtered, filter cake washes with water, merging filtrate and washing lotion, holding temperature is at 90 ~ 100 DEG C (preferably 95 DEG C), crystallization 3 ~ 4h (preferred crystallization time is 4h), when slurry is discharged, stay a part of slurry to be used as bacterial classification, all the other slurries drain in crystallizer tank and cool;
(3) filtration, drying, calcining, cooling: by the filtration of the aluminum fluoride slurry of cooling, and with 50 ~ 90 DEG C of (preferably 60 ~ 70 DEG C) hot water, aluminum fluoride crystal is washed, filtrate and washing lotion flow into mother liquor tank, filter cake aluminum fluoride trihydrate carries out air stream drying, and 500 ~ 600 DEG C of calcinings, cooling, obtains aluminum fluoride;
(4) sodium aluminum fluoride synthesis: by the mother liquor of aluminum fluoride after filtering and Sodium Fluoride by measure than 1:2.8 ~ 1:3.2 (preferred measure than be 1: 3), under 80 ~ 90 DEG C (preferably 90 DEG C), stir lower reaction 50 ~ 60min (the preferred reaction time is 60min), react complete reactant is filtered, filtrate is sent into sewage lagoon and is processed, filter cake controls expansion drying at 120 DEG C ~ 150 DEG C, and the son that namely secures satisfactory grades compares sodium aluminum fluoride.
Further, described air stream drying divides three sections, and one section of temperature controls, at 180 DEG C ~ 250 DEG C, to deviate from all free-waters in aluminum fluoride trihydrate, deviates from 2.5 crystal water in aluminum fluoride trihydrate for two sections; Deviate from last half crystal water for 3rd section, whole drying and calcining process completes at above three sections.
The present invention is with warm therapy phosphoric acid production dilute phosphoric acid concentration process neutralization reaction and produces the low dose fluoride silicic acid obtained in calcium superphosphate neutralization reaction, direct method is adopted to produce aluminum fluoride, coproduction cryolite with high molecular ratio from, the aluminum fluoride concentration not only prepared is low, stable, yield is high; And coproduction cryolite with high molecular ratio from quality is high, yield is also high.Meanwhile, the present invention's sewage in process of production only has mother liquor of aluminum fluoride to bring into, and compared with other production technique, its sewage quantity is few, and easily processes.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
First adopt H
2siF
6with AL (OH)
3be prepared into ALF
3solution, and then add solid fluorinated sodium, prepare cryolite with high molecular ratio from, reaction formula is as follows:
2AL(OH)
3+H
2SiF
6＝2ALF
3+SiO
2+4H
2O(1)
ALF
3++3NaF＝Na
3ALF
6(2)
Embodiment 1: the method for producing aluminum fluoride coproduction cryolite with high molecular ratio from
1, the preparation of aluminum fluoride
(1) react: be that 13% silicofluoric acid is heated to 65 DEG C ~ 75 DEG C by graphite heat exchanger by concentration, then reactor is added after metering, then add the aluminium hydroxide of metering, wherein, silicofluoric acid is 1: 2 with the metering ratio of aluminium hydroxide, temperature of reaction controls at 80 DEG C, stirring reaction 16min, reactant gases suction washing tail gas is emptying, after completion of the reaction, rinse resultant product in reactive tank with water, be discharged into the Sio of next procedure in the lump with reactant
2filter filters.
(2) desiliconization: reaction product and flushing product are moved disk filter through vacuum and filters, then filter cake washes with water, send subsequent processing to carry out crystallization with filtrate.
(3) crystallization: the filtrate obtained during desiliconization and washing lotion are flowed into crystallizer tank, passes into steam heating during crystallization with coil pipe, maintains Tc at 95 DEG C, crystallization time 4h, charging and discharging time are about 2h in addition, stir in crystallisation process, to keep homogeneous temperature; When slurry is discharged, stay a part of slurry to be used as bacterial classification, slurry drains into cooling in crystallizer tank and enters next procedure.
(4) filter: filtered by the aluminum fluoride slip band filter cooled in geosyncline, and wash aluminum fluoride crystal with 65 DEG C of hot water, filtrate and washing lotion flow into ALF
3mother liquor tank, filter cake aluminum fluoride trihydrate enters subsequent processing through chute.
(5) dry, calcining: aluminum fluoride trihydrate is flowed into air stream drying from chute, and air stream drying divides three sections: a section to be all free-waters deviate from aluminum fluoride trihydrate; Two sections for deviating from 2.5 crystal water in aluminum fluoride trihydrate; Deviate from last half crystal water for 3rd section, whole drying and calcining process completes at above three sections, and one section of temperature controls at 180 DEG C ~ 250 DEG C, and the temperature of calcining controls 600 DEG C.
(6) cool: by drying with calcine aluminum fluoride completely and cool in cooling drum, feeding aluminum fluoride warehouse, packaging.
(7) vent gas washing system: it is made up of a Venturi scrubber and a scrubber sealing groove, and reaction end gas is emptying after Venturi scrubbing, after dry, calcined gas is then first through Venturi scrubbing, then enters after washing tower emptying through liquid seal trough.
The Al yield of obtained aluminum fluoride can reach more than 95%, F yield and can reach more than 90%, and can place for a long time in atmosphere and not absorb water.
2, the preparation of cryolite with high molecular ratio from
(1) sodium aluminum fluoride synthesis: the mother liquor of aluminum fluoride after filtering is squeezed into sodium aluminum fluoride scale tank from mother liquor of aluminum fluoride groove, sodium aluminum fluoride synthesis groove is sent into after metering, also synthesis groove is added after Sodium Fluoride metering, wherein, mother liquor of aluminum fluoride is 1: 3 with the metering ratio of Sodium Fluoride, under agitation react, temperature of reaction is at 90 DEG C, reaction times 60min, reactant gases sends into washing tail gas, emptying after washing, reacts complete and is filtered by reactant, filtrate is sent into sewage lagoon and is processed, and dehumidification system sent into by filter cake.
(2) sodium aluminum fluoride is dry: send in flash distillation dryer dry by sodium aluminum fluoride filter cake auger, material from bottom to top delivers to cyclone charging hole and cloth bag case feed opening through wind, sodium aluminum fluoride warehouse is sent into again through cooling auger, then metering packing sodium aluminum fluoride product, temperature controls 120 DEG C ~ 150 DEG C, dry emptying after cloth bag division.
Obtained sodium aluminum fluoride w (F) >=52%, w (Al) >=13%, w (Na)≤32% meets the technical requirements of GB/T4291-2007 sodium aluminum fluoride, and sodium aluminum fluoride molecular ratio can reach 2.8 to 3.0 between (fluorine 54.5%, aluminium 13%, sodium 31.6%), reach the requirement of cryolite with high molecular ratio from.
Claims (3)
1. produce a method for aluminum fluoride coproduction cryolite with high molecular ratio from, it is characterized in that, comprise the following steps,
(1) react: be that 13 ~ 14% silicofluoric acid are heated to 65 DEG C ~ 75 DEG C by interchanger by concentration, then reactor is added after metering, then the aluminium hydroxide through metering is added, wherein, silicofluoric acid is 1:1.01 ~ 1:1.05 with the metering ratio of aluminium hydroxide, at 70 ~ 80 DEG C, stirring reaction 12 ~ 16min, after completion of the reaction, rinse resultant product in reactive tank with water, merge with reaction product;
(2) desiliconization, crystallization, cooling: the reaction product merged filtered, filter cake washes with water, merging filtrate and washing lotion, holding temperature is at 90 ~ 100 DEG C, and crystallization 3 ~ 4h, when slurry is discharged, stay a part of slurry to be used as bacterial classification, all the other slurries drain in crystallizer tank and cool;
(3) filtration, drying, calcining, cooling: by the filtration of the aluminum fluoride slurry of cooling, and with 50 ~ 90 DEG C of hot water, aluminum fluoride crystal is washed, filtrate and washing lotion flow into mother liquor tank, filter cake aluminum fluoride trihydrate carries out air stream drying, and 500 ~ 600 DEG C of calcinings, cooling, obtains aluminum fluoride;
(4) sodium aluminum fluoride synthesis: the mother liquor of aluminum fluoride after filtration is pressed with Sodium Fluoride and measures than 1:2.8 ~ 1:3.2, at 80 ~ 90 DEG C, stir lower reaction 50 ~ 60min, react complete reactant is filtered, filtrate is sent into sewage lagoon and is processed, filter cake controls expansion drying at 120 DEG C ~ 150 DEG C, and the son that namely secures satisfactory grades compares sodium aluminum fluoride.
2. the method for production aluminum fluoride coproduction cryolite with high molecular ratio from according to claim 1, is characterized in that, comprise the following steps,
(1) react: be that 13% silicofluoric acid is heated to 65 DEG C ~ 75 DEG C by graphite heat exchanger by concentration, then reactor is added after metering, then the hydrofluorination aluminium of metering is added, wherein, silicofluoric acid is 1: 1.02 with the metering ratio of aluminium hydroxide, at 80 DEG C, stirring reaction 16min, after completion of the reaction, rinse resultant product in reactive tank with water, merge with reaction product;
(2) desiliconization, crystallization, cooling: the reaction product of merging is moved disk filter through vacuum and filters, filter cake washes with water, merging filtrate and washing lotion, holding temperature is at 95 DEG C, crystallization 4h, when slurry is discharged, stay a part of slurry to be used as bacterial classification, all the other slurries drain in crystallizer tank and cool;
(3) filtration, drying, calcining, cooling: the aluminum fluoride slurry band filter of cooling is filtered, and with 60 ~ 70 DEG C of hot water, aluminum fluoride crystal is washed, filtrate and washing lotion flow into mother liquor tank, filter cake aluminum fluoride trihydrate carries out air stream drying, and 500 ~ 600 DEG C of calcinings, cooling, obtains aluminum fluoride;
(4) sodium aluminum fluoride synthesis: by mother liquor of aluminum fluoride and the Sodium Fluoride after filtering by measuring than being 1: 3, at 90 DEG C, 60min is reacted under stirring, react complete reactant is filtered, filtrate is sent into sewage lagoon and is processed, filter cake controls expansion drying at 120 DEG C ~ 150 DEG C, and the son that namely secures satisfactory grades compares sodium aluminum fluoride.
3. the method for production aluminum fluoride coproduction cryolite with high molecular ratio from according to claim 1 and 2, it is characterized in that, described air stream drying divides three sections, and one section of temperature controls at 180 DEG C ~ 250 DEG C, deviate from all free-waters in aluminum fluoride trihydrate, deviate from 2.5 crystal water in aluminum fluoride trihydrate for two sections; Deviate from last half crystal water for 3rd section, whole drying and calcining process completes at above three sections.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106477610A (en) * | 2016-09-21 | 2017-03-08 | 广西大学 | A kind of preparation method of technical grade cryolite with high molecular ratio |
| CN108017077A (en) * | 2017-12-11 | 2018-05-11 | 达州励志环保科技有限公司 | A kind of method for producing aluminum fluoride coproduction cryolite with high molecular ratio |
| CN109231247A (en) * | 2018-11-28 | 2019-01-18 | 达州励志环保科技有限公司 | A kind of method that the by-product of fluosilicic acid legal system aluminum fluoride prepares ice crystal |
| CN113697835A (en) * | 2021-01-05 | 2021-11-26 | 蔡从美 | Method for extracting aluminum fluoride from silicon dioxide slag |
| CN115010157A (en) * | 2022-06-22 | 2022-09-06 | 中石化南京工程有限公司 | System and method for producing anhydrous aluminum fluoride by using fluosilicic acid |
| CN115196660A (en) * | 2022-06-22 | 2022-10-18 | 中石化南京工程有限公司 | Method and system for producing cryolite from fluosilicic acid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106477610A (en) * | 2016-09-21 | 2017-03-08 | 广西大学 | A kind of preparation method of technical grade cryolite with high molecular ratio |
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| CN113697835A (en) * | 2021-01-05 | 2021-11-26 | 蔡从美 | Method for extracting aluminum fluoride from silicon dioxide slag |
| CN115010157A (en) * | 2022-06-22 | 2022-09-06 | 中石化南京工程有限公司 | System and method for producing anhydrous aluminum fluoride by using fluosilicic acid |
| CN115196660A (en) * | 2022-06-22 | 2022-10-18 | 中石化南京工程有限公司 | Method and system for producing cryolite from fluosilicic acid |
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