CN101323461B - Method for synthesizing cryolite by using waste from aluminum fluoride and trihydrate alumina production - Google Patents
Method for synthesizing cryolite by using waste from aluminum fluoride and trihydrate alumina production Download PDFInfo
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- CN101323461B CN101323461B CN2008101407749A CN200810140774A CN101323461B CN 101323461 B CN101323461 B CN 101323461B CN 2008101407749 A CN2008101407749 A CN 2008101407749A CN 200810140774 A CN200810140774 A CN 200810140774A CN 101323461 B CN101323461 B CN 101323461B
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- aluminum fluoride
- cryolite
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- synthetic
- sodium aluminum
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Abstract
The invention relates to a method for utilizing wastes generated in the manufacturing process of aluminum fluoride and aluminum hydroxide to synthesize cryolite. The method mainly includes the following steps: (1) the condensed fluid is collected and processed; (2) the carbon alkali solution is blended; (3) the condensed fluid and carbon alkali solution are injected into a cryolite synthesizing tank under the normal temperature and pressure and are stirred for synthesis; (4) the cryolite material slurry is obtained through final aging. The invention utilizes the carbon alkali generated in themanufacturing process of aluminum hydroxide to be reacted with the atmosphere condensed fluid generated in the manufacturing process of dry aluminum fluoride under the normal temperature and pressureto synthesize cryolite as a new product, which breaks the limit of a single manufacturing system so as to convert the atmosphere condensed fluid and carbon alkali which are once wasted into useful things and opens up a recyclable new economical way of disposing waste solid and waste water.
Description
Technical field
The present invention relates to the synthetic field of sodium aluminum fluoride, relate in particular to a kind of method of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide.
Background technology
In market competition fierce day by day today, energy-saving and cost-reducing, form low input, low consumption, low emission and high efficiency saving type production technique, realize that three big principles of recycling economy " minimizing, utilize again, resource utilization " have become the theme of world industry production.In aluminum fluoride by dry process is produced, aluminium hydroxide and hydrogen fluoride are at the fluidized-bed internal reaction, the water vapour that is produced is discharged with condensed gas, carry out the atmosphere condensation process through after at different levels the gathering dust, hydrogen fluoride gas that water vapour, silicon tetrafluoride gas, part have not been reacted and dust-precipitator are handled remaining aluminum fluoride, the aluminum hydroxide particle cooling forms the atmosphere phlegma, directly efflux (conventional atmosphere phlegma precipitation process flow process is seen Fig. 1) more after treatment, and effectively fluorine, aluminium component are failed to be utilized effectively, and have been polluted environment in the atmosphere phlegma.Disclose a kind of " two-stage type reclaiming of aluminum fluoride from tail gas condensate of aluminum fluoride production system system and technology " among the Chinese patent literature CN1962450A, but its recycling to fluorine, aluminium still not very abundant.
In the production of aluminum hydroxide process, have a large amount of carbanions in bauxite and the lime, enter system through the stripping reaction, separated out in the mother liquid evaporation operation, form carbon alkali, a large amount of carbon alkali causticizations need drop into a large amount of lime and carry out causticization processing (solid carbon alkaline purification flow process as shown in Figure 2), and technology is loaded down with trivial details, economic benefit not significantly (selling price is very low, have only pure carbon alkali 5%).And also contain a large amount of sodium aluminates and sodium hydroxide inside the carbon alkali of separating out, and be not fully utilized yet, very unfortunate.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
Utilize the Al in the useless carbon alkali in the production of aluminum hydroxide
2O
3, Na
2HF, AlF in the discarded atmosphere phlegma during O and aluminum fluoride are produced
3, synthetic cryolite at normal temperatures and pressures, main chemical equation is as follows:
Na
2OAl
2O
3+ 2Na
2CO
3+ 12HF → 2Na
3AlF
6↓ (sodium aluminum fluoride)+6H
2O+CO
2↑
Na
2OAl
2O
3+ 4NaOH+12HF → 2Na
3AlF
6↓ (sodium aluminum fluoride)+6H
2O
Al (OH)
3+ 3NaOH+6HF → Na
3AlF
6↓ (sodium aluminum fluoride)+6H
2O
AlF
3+ 3NaOH+3HF → Na
3AlF
6↓ (sodium aluminum fluoride)+3H
2O
2AlF
3+ 3Na
2CO
3+ 6HF → 2Na
3AlF
6↓ (sodium aluminum fluoride)+3H
2O+3CO
2↑
A kind of method of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide may further comprise the steps:
(1) the phlegma collection and treatment collect produced in the aluminum fluoride by dry process production process contain HF, AlF
3The atmosphere phlegma, it is caused subsider carries out sedimentation and handle, underflow is delivered to Waste Water Treatment, overflow causes the synthetic groove of sodium aluminum fluoride;
(2) formed solid carbon alkali in the production of aluminum hydroxide process is collected in the allotment of carbon alkaline solution, it is dissolved in 60～80 ℃ the hot water, be deployed into basicity and be the carbon alkaline solution of 110～140g/L, settlement separate through subsider again, overflow causes the synthetic groove of sodium aluminum fluoride, and underflow is delivered to Waste Water Treatment;
(3) reaction is synthetic at normal temperatures and pressures, with above-mentioned gained phlegma, carbon alkaline solution with 7.0～9.0: 1 volume ratio is introduced the synthetic groove of sodium aluminum fluoride, stirs building-up reactions and carries out 20～40 minutes;
(4) during terminal point ageing reaction end the HF acidity control of solution at 1.5～4g/L, and ageing 20～40 minutes, cryolite slurry;
(5) filter cryolite slurry and get the sodium aluminum fluoride filter cake, filtrate causes Waste Water Treatment.
In the described step (5) gained sodium aluminum fluoride filter cake deliver to the sodium aluminum fluoride production system do seed or under 150～300 ℃, dry the sodium aluminum fluoride finished product.
In described step (2), the basicity of carbon alkaline solution is adjusted to 115～125g/L.
In described step (3), phlegma, carbon alkaline solution are with 7.5～8.5: 1 volume ratio is introduced the synthetic groove of sodium aluminum fluoride.
In described step (4), the HF acidity control of solution is at 2～3g/L during reaction end.
The present invention has actively useful effect:
Break through the limitation of single production system, utilize the carbon alkali that is produced in the production of aluminum hydroxide process, with the atmosphere phlegma reaction synthetic cryolite of handling generation in the aluminum fluoride by dry process production at normal temperatures and pressures, form a kind of product innovation, thereby atmosphere phlegma and carbon alkali turned waste into wealth, opened up the recycling economy new way of waste residue, wastewater treatment.
Atmosphere phlegma and hydrogen aluminium carbon alkali reaction synthetic sodium aluminum fluoride molecular ratio are stabilized in about 2.4, can reach the requirement of medium molecule ratio ice spar, and sodium aluminum fluoride granularity D50 belongs to the medium particle diameter of powdery at 12～16 μ m; Impurity component content such as the iron in the sodium aluminum fluoride, sulfate radical and phosphorus all meet the relevant requirements in the sodium aluminum fluoride national standard (GB/T4291-2007).
Description of drawings
Fig. 1 is conventional atmosphere phlegma precipitation process schema;
Fig. 2 is the conventional processing schema of solid carbon alkali;
Fig. 3 is the process flow sheet that utilizes atmosphere phlegma and carbon alkali synthetic cryolite.
Embodiment
1 one kinds of methods of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide of embodiment may further comprise the steps:
(1) the phlegma collection and treatment collect produced in the aluminum fluoride by dry process production process contain HF, AlF
3The atmosphere phlegma, it is caused subsider carries out sedimentation and handle, underflow is delivered to Waste Water Treatment, overflow causes the synthetic groove of sodium aluminum fluoride;
(2) formed solid carbon alkali in the production of aluminum hydroxide process is collected in the allotment of carbon alkaline solution, it is dissolved in 70 ℃ the hot water, be deployed into basicity and be the carbon alkaline solution of 120g/L, settlement separate through subsider again, overflow causes the synthetic groove of sodium aluminum fluoride, and underflow is delivered to Waste Water Treatment;
(3) reaction is synthetic at normal temperatures and pressures, and phlegma, carbon alkaline solution are introduced the synthetic groove of sodium aluminum fluoride with 8: 1 volume ratio, stir building-up reactions and carry out 30 minutes;
(4) during terminal point ageing reaction end the HF acidity control of solution at 2.5g/L, and ageing 30 minutes, cryolite slurry;
(5) filter cryolite slurry and get the sodium aluminum fluoride filter cake, filtrate (the main component result of laboratory test sees Table 2) causes Waste Water Treatment.
(6) gained sodium aluminum fluoride filter cake in the step (5) is delivered to the sodium aluminum fluoride production system do seed or under 200 ℃, dry sodium aluminum fluoride finished product (quality index sees Table 1).
2 one kinds of methods of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide of embodiment may further comprise the steps:
(1) the phlegma collection and treatment collect produced in the aluminum fluoride by dry process production process contain HF, AlF
3The atmosphere phlegma, it is caused subsider carries out sedimentation and handle, underflow is delivered to Waste Water Treatment, overflow causes the synthetic groove of sodium aluminum fluoride;
(2) formed solid carbon alkali in the production of aluminum hydroxide process is collected in the allotment of carbon alkaline solution, it is dissolved in 80 ℃ the hot water, be deployed into basicity and be the carbon alkaline solution of 128g/L, settlement separate through subsider again, overflow causes the synthetic groove of sodium aluminum fluoride, and underflow is delivered to Waste Water Treatment;
(3) reaction is synthetic at normal temperatures and pressures, and phlegma, carbon alkaline solution are introduced the synthetic groove of sodium aluminum fluoride with 7.6: 1 volume ratio, stir building-up reactions and carry out 40 minutes;
(4) during terminal point ageing reaction end the HF acidity control of solution at 2.8g/L, and ageing 25 minutes, cryolite slurry;
(5) filter cryolite slurry and get the sodium aluminum fluoride filter cake, filtrate (the main component result of laboratory test sees Table 2) causes Waste Water Treatment.
(6) gained sodium aluminum fluoride filter cake in the step (5) is delivered to the sodium aluminum fluoride production system do seed or under 250 ℃, dry sodium aluminum fluoride finished product (quality index sees Table 1).
As can be seen from Table 1, atmosphere phlegma and hydrogen aluminium carbon alkali reaction synthetic sodium aluminum fluoride molecular ratio are stabilized in about 2.4, can reach the requirement of medium molecule ratio ice spar; Sodium aluminum fluoride granularity D50 belongs to the medium particle diameter of powdery at 12～16 μ m; Iron, sulfate radical and phosphorus content all are lower than sodium aluminum fluoride national standard (GB/T4291-2007) requirement.
The emission standard of the fluoride waste of national requirements for environmental protection is 10mg/L F
-, the fluorine content of the filtrate after the processing is 30～60 times of discharging standards, so the further processing of the fluoride waste of discharging, but F-content is more directly handled reduction more than 80%, and the expense cost of processing then significantly descends.
3 one kinds of methods of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide of embodiment, substantially the same manner as Example 1, difference is: in step (2), the solid carbon alkali of collecting dissolved in 75 ℃ the hot water, making it becomes the carbon alkaline solution that basicity is 135g/L, delivers to that subsider is settlement separate to go out solid impurity again; Phlegma, carbon alkaline solution are introduced the synthetic groove of sodium aluminum fluoride with 8.6: 1 volume ratio in step (3), stir building-up reactions at normal temperatures and pressures and carry out 35 minutes; In step (4), during with reaction end the HF acidity control of solution at 2.2g/L, and ageing 25 minutes, cryolite slurry.
4 one kinds of methods of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide of embodiment, substantially the same manner as Example 2, difference is: in step (2), the solid carbon alkali of collecting dissolved in 65 ℃ the hot water, making it becomes the carbon alkaline solution that basicity is 125g/L, delivers to subsider again; Phlegma, carbon alkaline solution are introduced the synthetic groove of sodium aluminum fluoride with 7.2: 1 volume ratio in step (3), stir building-up reactions at normal temperatures and pressures and carry out 40 minutes; In step (4), during with reaction end the HF acidity control of solution at 2.6g/L, and ageing 35 minutes, cryolite slurry.
5 one kinds of methods of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide of embodiment, substantially the same manner as Example 1, difference is: in step (2), the solid carbon alkali of collecting dissolved in 78 ℃ the hot water, making it becomes the carbon alkaline solution that basicity is 115g/L, delivers to that subsider is settlement separate to go out solid impurity again; Phlegma, carbon alkaline solution are introduced the synthetic groove of sodium aluminum fluoride with 7.1: 1 volume ratio in step (3), stir building-up reactions at normal temperatures and pressures and carry out 30 minutes; In step (4), during with reaction end the HF acidity control of solution at 2.9g/L, and ageing 35 minutes, cryolite slurry; With gained sodium aluminum fluoride filter cake in the step (5) under 250 ℃, dry the sodium aluminum fluoride finished product.
6 one kinds of methods of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide of embodiment, substantially the same manner as Example 2, difference is: in step (2), the solid carbon alkali of collecting dissolved in 65 ℃ the hot water, making it becomes the carbon alkaline solution that basicity is 135g/L, delivers to subsider again; Phlegma, carbon alkaline solution are introduced the synthetic groove of sodium aluminum fluoride with 8.5: 1 volume ratio in step (3), stir building-up reactions at normal temperatures and pressures and carry out 35 minutes; In step (4), during with reaction end the HF acidity control of solution at 2.1g/L, and ageing 25 minutes, cryolite slurry; Gained sodium aluminum fluoride filter cake in the step (5) is delivered to the sodium aluminum fluoride production system do seed.
7 one kinds of methods of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide of embodiment, substantially the same manner as Example 1, difference is: in step (2), the solid carbon alkali of collecting dissolved in 76 ℃ the hot water, making it becomes the carbon alkaline solution that basicity is 128g/L, delivers to that subsider is settlement separate to go out solid impurity again; Phlegma, carbon alkaline solution are introduced the synthetic groove of sodium aluminum fluoride with 7.9: 1 volume ratio in step (3), stir building-up reactions at normal temperatures and pressures and carry out 36 minutes; In step (4), during with reaction end the HF acidity control of solution at 1.8g/L, and ageing 32 minutes, cryolite slurry; With gained sodium aluminum fluoride filter cake in the step (5) under 260 ℃, dry the sodium aluminum fluoride finished product.
8 one kinds of methods of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide of embodiment, substantially the same manner as Example 2, difference is: in step (2), the solid carbon alkali of collecting dissolved in 79 ℃ the hot water, making it becomes the carbon alkaline solution that basicity is 118g/L, delivers to subsider again; Phlegma, carbon alkaline solution are introduced the synthetic groove of sodium aluminum fluoride with 8.3: 1 volume ratio in step (3), stir building-up reactions at normal temperatures and pressures and carry out 33 minutes; In step (4), during with reaction end the HF acidity control of solution at 3.6g/L, and ageing 28 minutes, cryolite slurry; Gained sodium aluminum fluoride filter cake in the step (5) is delivered to the sodium aluminum fluoride production system do seed.
9 one kinds of methods of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide of embodiment, substantially the same manner as Example 1, difference is: in step (2), the solid carbon alkali of collecting dissolved in 60 ℃ the hot water, making it becomes the carbon alkaline solution that basicity is 110g/L, delivers to that subsider is settlement separate to go out solid impurity again; Phlegma, carbon alkaline solution are introduced the synthetic groove of sodium aluminum fluoride with 7.0: 1 volume ratio in step (3), stir building-up reactions at normal temperatures and pressures and carry out 40 minutes; In step (4), during with reaction end the HF acidity control of solution at 1.6g/L, and ageing 40 minutes, cryolite slurry; With gained sodium aluminum fluoride filter cake in the step (5) under 150 ℃, dry the sodium aluminum fluoride finished product.
10 1 kinds of methods of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide of embodiment, substantially the same manner as Example 2, difference is: in step (2), the solid carbon alkali of collecting dissolved in 80 ℃ the hot water, making it becomes the carbon alkaline solution that basicity is 140g/L, delivers to subsider again; Phlegma, carbon alkaline solution are introduced the synthetic groove of sodium aluminum fluoride with 9.0: 1 volume ratio in step (3), stir building-up reactions at normal temperatures and pressures and carry out 40 minutes; In step (4), during with reaction end the HF acidity control of solution at 4.0g/L, and ageing 20 minutes, cryolite slurry; With gained sodium aluminum fluoride filter cake in the step (5) deliver to the sodium aluminum fluoride production system do seed or under 300 ℃, dry the sodium aluminum fluoride finished product.
Table 1 synthetic cryolite quality index
Table 2 filtrate result of laboratory test
Claims (5)
1. method of utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide may further comprise the steps:
(1) the phlegma collection and treatment collect produced in the aluminum fluoride by dry process production process contain HF, A1F
3The atmosphere phlegma, it is caused subsider carries out sedimentation and handle, underflow is delivered to Waste Water Treatment, overflow causes the synthetic groove of sodium aluminum fluoride;
(2) formed solid carbon alkali in the production of aluminum hydroxide process is collected in the allotment of carbon alkaline solution, it is dissolved in 60～80 ℃ the hot water, be deployed into basicity and be the carbon alkaline solution of 110～140g/L, settlement separate through subsider again, overflow causes the synthetic groove of sodium aluminum fluoride, and underflow is delivered to Waste Water Treatment;
(3) reaction is synthetic at normal temperatures and pressures, and step (1) gained phlegma, step (3) gained carbon alkaline solution are with 7.0～9.0: 1 volume ratio is introduced the synthetic groove of sodium aluminum fluoride, stirs building-up reactions and carries out 20～40 minutes;
(4) during terminal point ageing reaction end the HF acidity control of solution at 1.5～4.0g/L, and ageing 20～40 minutes, cryolite slurry;
(5) filter cryolite slurry and get the sodium aluminum fluoride filter cake, filtrate causes Waste Water Treatment.
2. the method for utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide according to claim 1, it is characterized in that, with gained sodium aluminum fluoride filter cake in the step (5) deliver to the sodium aluminum fluoride production system do seed or under 150～300 ℃, dry the sodium aluminum fluoride finished product.
3. the method for utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide according to claim 1 and 2 is characterized in that in described step (2), the basicity of described carbon alkaline solution is adjusted to 115～125g/L.
4. the method for utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide according to claim 3 is characterized in that, in step (3), described phlegma, carbon alkaline solution are with 7.5～8.5: 1 volume ratio is introduced the synthetic groove of sodium aluminum fluoride.
5. the method for utilizing the waste synthetic cryolite in aluminum fluoride, the production of aluminum hydroxide according to claim 4 is characterized in that, in step (4), the HF acidity control of solution is at 2～3g/L during reaction end.
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