CN103449486A - Method for preparing boehmite by liquid phase carbonating decomposition of sodium aluminate solution and sodium bicarbonate - Google Patents
Method for preparing boehmite by liquid phase carbonating decomposition of sodium aluminate solution and sodium bicarbonate Download PDFInfo
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- CN103449486A CN103449486A CN2013103829731A CN201310382973A CN103449486A CN 103449486 A CN103449486 A CN 103449486A CN 2013103829731 A CN2013103829731 A CN 2013103829731A CN 201310382973 A CN201310382973 A CN 201310382973A CN 103449486 A CN103449486 A CN 103449486A
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Abstract
The invention discloses a method for preparing boehmite by liquid phase carbonating decomposition of a sodium aluminate solution and sodium bicarbonate, which belongs to the field of industrial aluminum oxide. The method comprises the steps of: carrying out decomposition reaction between a NaHCO3 solution and a sodium aluminate solution, adding boehmite seed crystal to induce the sodium aluminate solution to crystallize and separate out boehmite; performing diaphragm electrolysis on a carbonate mother liquor obtained after decomposition of the sodium aluminate solution to dissociate carbon from alkali; preparing sodium bicarbonate in an anode region; and returning to the decomposition process, thereby recycling a carbon source. The method is suitable to a Bayer-process and a sintering-process decomposition of the sodium aluminate solution, the decomposition rate is high and the energy consumption of aluminum oxide roasting can be lowered.
Description
Technical field
The present invention relates to technical field of alumina production, particularly about utilizing sodium aluminate solution and sodium bicarbonate liquid phase method carbon to divide the novel method for preparing boehmite.
Technical background
As the basic raw material of producing metallic aluminium, alumina producing in aluminium industry in occupation of extremely important position.The method of alumina producing mainly contains Bayer process, sintering process and integrated process both at home and abroad at present.Integrated process is the combination of Bayer process and sintering process.The Bayer process energy consumption is low, but higher to the quality requirements of bauxite, and sintering process can be processed low-grade bauxite, and weak point is that power consumption is higher.
The kind that the Bayer process decomposition sodium aluminate liquid adopts is divided process, owing to being subject to solution Na
2o-Al
2o
3-H
2the restriction of O three-phase equilibrium, in actual production, the rate of decomposition of Bayer process decomposition of crystal seed can only be in 50% left and right, and plants minute time and reach 40～70 hours, and production efficiency is low.That the sintering process decomposition sodium aluminate liquid adopts is CO
2carbon method, rate of decomposition is high-about more than 90%, and carbon divide the time short-approximately about 4～5 hours, but have poor product quality, increased preparation CO
2operation, low, a large amount of CO of gas effciency
2enter the problems such as topsoil environment.Bayer process and the principal reaction of sintering process sodium aluminate solution decomposition course can use formula (1) and formula (2) to mean:
Al(OH)
- 4(aq)→βAl(OH)
3(s)+OH
- (aq) （1）
Al(OH)
- 4(aq)+CO
2→βAl(OH)
3(s)+CO
3 2- (aq) （2）
Al(OH)
- 4(aq)→γAlOOH
(s)+OH
- (aq)+H
2O （3）
Sodium aluminate solution can decomposite even alumina phase of various aluminium hydroxide, a water aluminum oxide in theory, as gibbsite β Al (OH)
3with boehmite γ AlOOH, or its mixture.No matter be that kind is divided or carbon divides at present, the decomposing sodium aluminate solution product is all gibbsite, 1 mole of aluminum oxide of every output, the heat of needs 170 kilojoules.If replace gibbsite at decomposition process with the separating out of boehmite (reacting 3), roasting energy consumption can reduce by 60%, because boehmite dewaters under 490 ℃, 1 mole of aluminum oxide of every output, only need the heat of 72 kilojoules.Therefore from the angle of production energy consumption, it is very useful directly separating out boehmite at decomposition process.
The technique of directly separating out boehmite from supersaturated sodium aluminate solution early has report, Misra in 1986 and Siva.kumar propose a kind of " improvement Bayer process ", at the temperature of 115～145 ℃, add a large amount of boehmite crystal seeds, directly from sodium aluminate solution, separate out boehmite.Greece Filippou in 1993 and Paspaliaris have also proposed " decomposition of crystal seed " and have separated out the idea of boehmite.But at present research shows to separate out the boehmite problems such as (100～150 ℃) that has that rate of decomposition is slow, rate of decomposition is low, the product granularity is little, decomposition temperature is high from sodium aluminate solution.Rate of decomposition means decomposition process length and the raising of crystal seed internal circulating load in alumina producing slowly, and this production to aluminum oxide is fatal, and the bottleneck of Bayer process is just in decomposition of crystal seed.Little meaning of product granularity is difficult to meet the granularity requirements of electrolytic aluminum to sandy alumina, and the decomposition temperature height is energy-saving and cost-reducing unfavorable in alumina producing.
The patent that the Wang Zhi of Chinese Academy Of Sciences Process Engineering Research Institute etc. declares " sodium aluminate solution carbonation decomposes the method (patent No. 200710065214.7) for preparing boehmite " has proposed to add a large amount of boehmites in the sintering process carbonating is decomposed and has done crystal seed, at the inhibition gibbsite, separate out simultaneously, realize the controlled crystallization of boehmite, and be aided with crystal production promotor, this process is strengthened.Pass through to control CO in decomposition course
2draft speed is regulated the degree of supersaturation (decomposition gradient) of boehmite in sodium aluminate solution, thereby nucleation and the agglomeration of regulation and control crystal growing process make it carry out to the direction that is conducive to boehmite.The method have decomposing sodium aluminate solution speed fast, separate out boehmite content advantages of higher, can only be directed to but exist the method that the conventional sintering method is produced employing carbonating decomposition in aluminum oxide, and in producing for Bayer process, sodium aluminate solution adopts carbonating to decompose, after exist decomposing, a large amount of sodium carbonate solutions can't recycle in the Bayer process system and other production links are brought to the problems such as harm, and Sodium Aluminate Solution Carbonation Decomposition is difficult controls; Be subject to the control of gas-liquid interfacial mass transfer and local excessive decomposition can cause the generation of dawsonite, carbon divides quality product poor; Decomposition course CO
2utilization ratio low (usually<60%), and CO
2derive from the limestone kiln of high cost with low efficiency.Wan Pingyu, button are comprised of the molten operation of alkali, carbon operation break-down and film electrolytic regeneration circulating process because of " a kind of technique of producing aluminum oxide by alkali dissolving carbonation method " that (patent No.s 200710178670.2) such as keys proposes.The molten operation of alkali adopts high-concentration sodium hydroxide solution to dissolve the aluminum oxide in bauxite, obtains sodium aluminate solution; The carbon operation break-down adopts sodium bicarbonate or carbonic acid gas decomposition sodium aluminate dissolution fluid; Film electrolytic regeneration circulating process obtains sodium bicarbonate and sodium hydroxide solution by carbon operation break-down product sodium carbonate solution by the film electrolysis, and realizes the recycle of material.The method is mainly for the production of conventional gibbsite type aluminum hydroxide, lack innovation and break through aspect product crystal formation, hydroxide particle-size and intensity regulation and control, and this technique whether the production of applicable chemical aluminum oxide also require study.
Summary of the invention
The object of the invention is to, for existing deficiency in seed precipitation process in existing alumina-producing method Bayer process and sintering process, provide a kind of sodium aluminate solution and sodium bicarbonate liquid phase method carbon to divide the novel method for preparing boehmite, alumina producing efficiency can either be significantly improved and the sodium bicarbonate recycle can be realized again, prepare the boehmite granularity large, be suitable for commercial alumina production.
A kind of sodium aluminate solution and sodium bicarbonate liquid phase method carbon that the present invention proposes divide the method for preparing boehmite, are achieved through the following technical solutions:
The present invention utilizes sodium aluminate solution and sodium bicarbonate generation liquid liquid neutralization reaction, take a kind of boehmite as crystal seed, makes decomposing sodium aluminate solution separate out boehmite, adopts the diaphragm electrolysis carbon mother liquid to make sodium carbonate be converted into sodium hydrogen carbonate solution.Mainly as shown in Figure 1, comprise the following steps:
Deployed sodium aluminate solution is joined in the reactive tank stirred, the boehmite crystal seed that is 0.1～2.0 by the crystal seed coefficient adds in sodium aluminate solution, sodium hydrogen carbonate solution is driven in reactive tank and is carried out decomposition reaction with sodium aluminate solution by peristaltic pump, boehmite is induced lower crystal growth at crystal seed, after decomposing 2～7h, obtain degradation production.
Degradation production is through liquid-solid filtering separation, and solid water is washed till neutrality, and under 80 ℃, drying makes the boehmite product, and boehmite content modification scope is wide, and granularity is the sand shape.Filtrate Na
2cO
3under certain current density, after the electrolysis certain hour, in anolyte compartment, sodium carbonate is converted into sodium bicarbonate and discharges sodium ion and oxygen by electrolysis, means the NaHCO that electrolysis obtains suc as formula (4)
3solution is being separated out boehmite for decomposing sodium aluminate solution.
2NaCO
3+H
2O-2e→2NaHCO
3+1/2O
2+Na
+ （4）
The feature of aforesaid method is, the concentration Al of sodium aluminate solution
2o
360～160 grams per liters, causticization coefficient 1.3～1.7, stirring velocity 100～300rmin
-1, boehmite crystal seed coefficient 0.1～2.0,85～100 ℃ of decomposing solution temperature, sodium bicarbonate concentration 60～120 grams per liters, add speed 0.2～1.0gL
-1min
-1, addition manner comprises at a slow speed and quick two kinds, 2～7 hours resolving times.40～80 ℃ of diaphragm electrolysis carbon mother liquid temperature, electrolysis time 4～20 hours, current density 0.01～0.1A/cm
2.Decompose in after product the boehmite granularity large, can reach the sandy alumina requirement.
In addition, the concentration of described sodium aluminate solution is preferably Al
2o
380～100 grams per liters, the causticization coefficient is 1.3～1.5, the decomposing solution temperature is 85～95 ℃.
Described sodium bicarbonate concentration is 80～100 grams per liters, and interpolation speed is 0.2～0.5gL
-1min
-1.
The described decomposing sodium aluminate solution time is 2～4 hours, and stirring velocity is 100～150rmin
-1.
Described electrolytic carbon denominator liquid temp is 40～60 ℃, and electrolysis time is 5～10 hours, and current density is 0.01～0.05A/cm
2.
The present invention is compared with prior art if any following advantage:
(1) be applicable to the seed precipitation process of Bayer process and sintering process, rate of decomposition is high, and separate out boehmite granularity large (80～120 microns of median sizes), boehmite content modification scope wide (60%～98%), broken through the bottleneck of conventional decomposition course boehmite product granularity tiny (<40 microns), boehmite content low (50% left and right).
(2) can adopt industrial sodium aluminate solution is raw material, does not have the shortcomings such as traditional boehmite (mainly producing activated alumina) the preparation process raw materials cost is high, complex process.
(3) carbon mother liquid (Na
2cO
3) make NaHCO through diaphragm electrolysis in positive column
3solution, can be directly used in seed precipitation process, and cost is low and can realize the utilization of raw material circulation comprehensive.
The accompanying drawing explanation
Fig. 1 is flow chart making of the present invention.
Embodiment
Further introduce outstanding advantages of the present invention and innovative point below by embodiment, but the present invention is in no way limited to embodiment.Embodiment 1:
With industrial aluminium hydroxide and sodium hydroxide configuration sodium aluminate solution 200ml, chemical composition is Al
2o
360 grams per liters, the causticization coefficient is 1.3,85 ℃ of decomposing solution temperature, stirring velocity 100rmin
-1under condition, add the boehmite crystal seed that the crystal seed coefficient is 0.1, and to add concentration with peristaltic pump be 60 grams per liter NaHCO
3solution, add speed 0.2gL
-1min
-1, resolving time 2h, separate the boehmite of separating out with carbon mother liquid, obtain the product boehmite.The gained carbon mother liquid is through diaphragm electrolysis, 40 ℃ of electrolytic solution temperature, and electrolysis time 4h, current density is 0.01A/cm
2, in positive column, obtain NaHCO
3solution, be adjusted into suitable concentration stand-by.
Decomposing sodium aluminate solution product and carbon mother liquid electrolysis the results are shown in Table 1
Table 1 decomposing sodium aluminate solution product and carbon mother liquid electrolysis result
| Boehmite content/% | Boehmite granularity/μ m | Anode hydrogen-carbonate na concn/g/L |
| 75% | 120 | 40 |
Embodiment 2:
With industrial aluminium hydroxide and sodium hydroxide configuration sodium aluminate solution 200ml, chemical composition is Al
2o
3120 grams per liters, the causticization coefficient is 1.7,95 ℃ of decomposing solution temperature, stirring velocity 200rmin
-1under condition, add the boehmite crystal seed that the crystal seed coefficient is 1.0, and to add concentration with peristaltic pump be 80 grams per liter NaHCO
3solution, add speed 0.8gL
-1min
-1, resolving time 4h, separate the boehmite of separating out with carbon mother liquid, obtain the product boehmite.The gained carbon mother liquid is through diaphragm electrolysis, the electrolytic solution temperature 50 C, and electrolysis time 8h, current density is 0.1A/cm
2, in positive column, obtain NaHCO
3solution, be adjusted into suitable concentration stand-by.
The results are shown in Table 2
Table 2 decomposing sodium aluminate solution product and carbon mother liquid electrolysis result
| Boehmite content/% | Boehmite granularity/μ m | Anode hydrogen-carbonate na concn/g/L |
| 80% | 85 | 60 |
Embodiment 3:
With industrial aluminium hydroxide and sodium hydroxide configuration sodium aluminate solution 200ml, chemical composition is Al
2o
3140 grams per liters, the causticization coefficient is 1.5,85 ℃ of decomposing solution temperature, stirring velocity 300rmin
-1under condition, add the boehmite crystal seed that the crystal seed coefficient is 2.0, and to add concentration with peristaltic pump be 100 grams per liter NaHCO
3solution, add speed 0.4gL
-1min
-1, resolving time 7h, separate the boehmite of separating out with carbon mother liquid, obtain the product boehmite.The gained carbon mother liquid is through diaphragm electrolysis, the electrolytic solution temperature 60 C, and electrolysis time 16h, current density is 0.02A/cm
2, in positive column, obtain NaHCO
3solution, be adjusted into suitable concentration stand-by.
The results are shown in Table 3
Table 3 decomposing sodium aluminate solution product and carbon mother liquid electrolysis result
| Boehmite content/% | Boehmite granularity/μ m | Anode hydrogen-carbonate na concn g/L |
| 95 | 110 | 75 |
Embodiment 4:
With industrial aluminium hydroxide and sodium hydroxide configuration sodium aluminate solution 200ml, chemical composition is Al
2o
3160 grams per liters, the causticization coefficient is 1.6,95 ℃ of decomposing solution temperature, stirring velocity 200rmin
-1under condition, add the boehmite crystal seed that the crystal seed coefficient is 1.0, and to add concentration with peristaltic pump be 120 grams per liter NaHCO
3solution, add speed 0.4
gl
-1min
-1, resolving time 6h, the boehmite of separating out separates with carbon mother liquid, obtains the product boehmite.The gained carbon mother liquid is through diaphragm electrolysis, 80 ℃ of electrolytic solution temperature, and electrolysis time 18h, current density is 0.08A/cm
2, in positive column, obtain NaHCO
3solution, be adjusted into suitable concentration stand-by.
The results are shown in Table 4
Table 4 decomposing sodium aluminate solution product and carbon mother liquid electrolysis result
| Boehmite content/% | Boehmite granularity/μ m | Anode hydrogen-carbonate na concn g/L |
| 88 | 95 | 100 |
Embodiment 5:
With industrial aluminium hydroxide and sodium hydroxide configuration sodium aluminate solution 200ml, chemical composition is Al
2o
3120 grams per liters, the causticization coefficient is 1.5,90 ℃ of decomposing solution temperature, stirring velocity 100rmin
-1under condition, add the boehmite crystal seed that the crystal seed coefficient is 0.6, and to add in-degree with peristaltic pump be 80 grams per liter NaHCO
3solution 300ml, adding speed increases gradually, and resolving time 5h, separate the boehmite of separating out with carbon mother liquid, obtain the product boehmite.The gained carbon mother liquid is through diaphragm electrolysis, the electrolytic solution temperature 50 C, and electrolysis time 20h, current density is 0.01A/cm
2, in positive column, obtain NaHCO
3solution, be adjusted into suitable concentration stand-by.
The results are shown in Table 5
Table 5 decomposing sodium aluminate solution product and carbon mother liquid electrolysis result
| Boehmite content/% | Boehmite granularity/μ m | Anode hydrogen-carbonate na concn g/L |
| 90 | 106 | 83 |
Embodiment 6:
With industrial aluminium hydroxide and sodium hydroxide configuration sodium aluminate solution 200ml, chemical composition is Al
2o
3100 grams per liters, the causticization coefficient is 1.7,100 ℃ of decomposing solution temperature, stirring velocity 300rmin
-1under condition, add the boehmite crystal seed that the crystal seed coefficient is 1.5, and to add in-degree with peristaltic pump be 100 grams per liter NaHCO
3solution 300ml, add speed and reduce gradually, and resolving time 6h, separate the boehmite of separating out with carbon mother liquid, obtain the product boehmite.The gained carbon mother liquid is through diaphragm electrolysis, 80 ℃ of electrolytic solution temperature, and electrolysis time 12h, current density is 0.06A/cm
2, in positive column, obtain NaHCO
3solution, be adjusted into suitable concentration stand-by.
The results are shown in Table 6
Table 6 decomposing sodium aluminate solution product and carbon mother liquid electrolysis result
| Boehmite content/% | Boehmite granularity/μ m | Anode hydrogen-carbonate na concn g/L |
| 92 | 92 | 80 |
Embodiment 7:
With industrial aluminium hydroxide and sodium hydroxide configuration sodium aluminate solution 200ml, chemical composition is Al
2o
380 grams per liters, the causticization coefficient is 1.4,80 ℃ of decomposing solution temperature, stirring velocity 200rmin
-1under condition, add the boehmite crystal seed that the crystal seed coefficient is 1.5, and to add in-degree with peristaltic pump be 80 grams per liter NaHCO
3solution 300ml, add speed and reduce gradually, and resolving time 5h, separate the boehmite of separating out with carbon mother liquid, obtain the product boehmite.The gained carbon mother liquid is through diaphragm electrolysis, 85 ℃ of electrolytic solution temperature, and electrolysis time 14h, current density is 0.05A/cm
2, in positive column, obtain NaHCO
3solution, be adjusted into suitable concentration stand-by.
The results are shown in Table 7
Table 7 decomposing sodium aluminate solution product and carbon mother liquid electrolysis result
| Boehmite content/% | Boehmite granularity/μ m | Anode hydrogen-carbonate na concn g/L |
| 86 | 83 | 90 |
In a word, the present invention adopts the sodium bicarbonate reinforcing sodium aluminate solution to divide and parses boehmite, novel NaHCO
3liquid phase method carbon divides and changes the solution-air two-step reaction into liquid-liquid single step reaction, having eliminated the air film mass transport limitation causes too local, reactive liquid solution makes the more all even easy regulation and control of system degree of supersaturation, be beneficial to the control of boehmite nucleation and crystallization, and sodium bicarbonate comes from electrolysis carbon mother liquid positive column product, realized the circulation comprehensive utilization of sodium carbonate, had to plant and divide and CO
2the advantage that carbon divides, the while has also overcome their disadvantage, has high-level efficiency, less energy-consumption, low cost and advantages of environment protection.
It should be noted that, according to the various embodiments described above of the present invention, those skilled in the art are the four corners that can realize independent claim of the present invention and appurtenance fully, implementation procedure and method same the various embodiments described above; And non-elaborated part of the present invention belongs to techniques well known.
The above; be only part embodiment of the present invention, but protection scope of the present invention is not limited to this, in the technical scope that any those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.
Claims (5)
1. a sodium aluminate solution and sodium bicarbonate liquid phase method carbon divide the method for preparing boehmite, it is characterized in that: adopt sodium hydrogen carbonate solution liquid phase method decomposition sodium aluminate liquid, add the boehmite crystal seed in sodium aluminate solution, and interpolation sodium bicarbonate and sodium aluminate solution generation decomposition reaction, boehmite is induced lower crystal growth at crystal seed, decomposition, by solid-liquid separation, obtains the degradation production boehmite; The carbon mother liquid obtained after decomposing sodium aluminate solution, through diaphragm electrolysis, obtains sodium hydrogen carbonate solution in positive column, turns back to decomposition course, has realized the recycle of sodium bicarbonate; Described decomposition sodium aluminate liquid condition comprises: the concentration of sodium aluminate solution is Al
2o
360～160 grams per liters, the causticization coefficient is 1.3～1.7, stirring velocity is 100～300rmin
-1, boehmite crystal seed coefficient is 0.1～2.0, the decomposing solution temperature is 85～100 ℃; Sodium bicarbonate concentration is 60～120 grams per liters, and it is 0.2～1.0gL that sodium bicarbonate adds speed
-1min
-1, addition manner comprises at a slow speed and quick two kinds of patterns, the decomposition reaction time is 2～7 hours; Electrolytic carbon denominator liquid temp is 40～80 ℃, and electrolysis time is 4～20 hours, and current density is 0.01～0.1A/cm
2.
2. it is characterized in that in accordance with the method for claim 1: the concentration of described sodium aluminate solution is Al
2o
380～100 grams per liters, the decomposing solution temperature is 85～95 ℃.
3. in accordance with the method for claim 1, it is characterized in that: described sodium bicarbonate concentration is 80～100 grams per liters, and interpolation speed is 0.2～0.5gL
-1min
-1.
4. in accordance with the method for claim 1, it is characterized in that: the described decomposing sodium aluminate solution time is 3～5 hours, and stirring velocity is 150～200rmin
-1.
5. in accordance with the method for claim 1, it is characterized in that: described electrolytic carbon denominator liquid temp is 40～60 ℃, and electrolysis time is 5～10 hours, and current density is 0.01～0.05A/cm
2.
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| CN110451541A (en) * | 2019-08-05 | 2019-11-15 | 中海油天津化工研究设计院有限公司 | A kind of preparation method mixing aluminium hydroxide |
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| CN114130382B (en) * | 2021-12-14 | 2023-11-21 | 河南能源化工集团研究总院有限公司 | Aluminum hydroxide powder and preparation method thereof |
| CN115231596A (en) * | 2022-08-05 | 2022-10-25 | 洛阳中超新材料股份有限公司 | Industrial preparation method of bayer stone |
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