CN103449486B - 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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- CN103449486B CN103449486B CN201310382973.1A CN201310382973A CN103449486B CN 103449486 B CN103449486 B CN 103449486B CN 201310382973 A CN201310382973 A CN 201310382973A CN 103449486 B CN103449486 B CN 103449486B
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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 preparing boehmite.
Technical background
As producing the basic raw material of metallic aluminium, alumina producing in aluminum i ndustry 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.Bayer process energy consumption is low, but higher to the quality requirements of bauxite, and sintering process can process low-grade bauxite, and weak point is that power consumption is higher.
The kind that Bayer process decomposition sodium aluminate liquid adopts divides 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 about 50%, and plants point for up to 40 ~ 70 hours, and production efficiency is low.That sintering process decomposition sodium aluminate liquid adopts is CO
2carbon method, rate of decomposition is high-about more than 90%, and carbon divides time short-about 4 ~ 5 hours, but there is poor product quality, adds preparation CO
2low, a large amount of CO of operation, gas effciency
2enter the problems such as topsoil environment.Bayer process and the principal reaction of sintering process sodium aluminate solution decomposition course can represent by formula (1) and formula (2):
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 various aluminium hydroxide, a Water oxidize aluminium even alumina phase 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, decomposing sodium aluminate solution product is all gibbsite, and every output 1 moles aluminium, needs the heat of 170 kilojoules.If replace gibbsite at decomposition process with the precipitation of boehmite (reaction 3), then roasting energy consumption can reduce by 60%, because boehmite dewaters at 490 DEG C, every output 1 moles aluminium, only needs the heat of 72 kilojoules.Therefore from the angle of production energy consumption, directly separate out boehmite at decomposition process and be highly profitable.
The technique directly separating out boehmite from supersaturated sodium aluminate solution early has report, within 1986, Misra and Siva.kumar proposes a kind of " improvement Bayer process ", namely, at the temperature of 115 ~ 145 DEG C, add a large amount of boehmite crystal seed, directly from sodium aluminate solution, separate out boehmite.Within 1993, Greece Filippou and Paspaliaris it is also proposed the idea that " decomposition of crystal seed " separates out boehmite.But research shows that separating out boehmite from sodium aluminate solution exists the problems such as rate of decomposition is slow, rate of decomposition is low, product particle size is little, decomposition temperature high (100 ~ 150 DEG C) at present.Rate of decomposition means that in alumina producing, decomposition process length and crystal seed internal circulating load improve slowly, and this is fatal to the production of aluminum oxide, and the bottleneck of Bayer process is just in decomposition of crystal seed.Product particle size little meaning is difficult to meet the granularity requirements of electrolytic aluminum to sandy alumina, high energy-saving and cost-reducing unfavorable then in alumina producing of decomposition temperature.
Patent that Chinese Academy Of Sciences Process Engineering Research Institute Wang Zhi etc. declares " sodium aluminate solution carbonation decomposes the method (patent No. 200710065214.7) preparing boehmite " proposes adds a large amount of boehmite and does crystal seed in sintering process carbonation decomposition, separate out simultaneously at suppression gibbsite, realize the controlled crystallization of boehmite, and be aided with crystal production promotor, this process is strengthened.By control CO in decomposition course
2draft speed regulates the degree of supersaturation (decomposition gradient) of boehmite in sodium aluminate solution, thus the nucleation of regulation and control crystal growing process and agglomeration, make it carry out to the direction being conducive to boehmite.The method have decomposing sodium aluminate solution speed fast, separate out boehmite content advantages of higher, but there is the method that can only be directed to and adopt carbonation decomposition in conventional sintering method production aluminum oxide, and sodium aluminate solution adopts carbonation decomposition in producing for Bayer process, then depositing a large amount of sodium carbonate solution after disassembly cannot recycle and bring the problems such as harm to other production links in Bayer process system, and Sodium Aluminate Solution Carbonation Decomposition difficulty controls; Can cause the generation of dawsonite by the control of gas-liquid interfacial mass transfer and local excessive decomposition, carbon divides quality product poor; Decomposition course CO
2utilization ratio low (usual <60%), and CO
2derive from the limestone kiln of high cost with low efficiency." a kind of technique of producing aluminum oxide by alkali dissolving carbonation method " that Wan Pingyu, button propose because of (patent No.s 200710178670.2) such as keys is made up of the molten operation of alkali, carbon operation break-down and film electrolytic regeneration circulating process.The molten operation of alkali adopts the aluminum oxide in high-concentration sodium hydroxide solubilize bauxite, obtains sodium aluminate solution; Carbon operation break-down adopts sodium bicarbonate or carbon dioxide decomposition sodium aluminate solution fluid; Carbon operation break-down product sodium carbonate solution is obtained sodium bicarbonate and sodium hydroxide solution by film electrolysis by film electrolytic regeneration circulating process, and realizes the recycle of material.The method, mainly for the production of the gibbsite type aluminum hydroxide of routine, lacks strategic structural in product crystal formation, hydroxide particle-size and intensity modulation, and the production whether this technique is suitable for chemical aluminum oxide also requires study.
Summary of the invention
The object of the invention is to, for deficiency existing in seed precipitation process in existing alumina-producing method Bayer process and sintering process, a kind of sodium aluminate solution and sodium bicarbonate liquid phase method carbon is provided to divide the novel method preparing boehmite, alumina producing efficiency can either be significantly improved and can realize sodium bicarbonate recycle again, prepare boehmite granularity large, be suitable for commercial alumina and produce.
A kind of sodium aluminate solution that the present invention proposes and sodium bicarbonate liquid phase method carbon divide the method preparing boehmite, are achieved through the following technical solutions:
The present invention utilizes sodium aluminate solution and sodium bicarbonate generation liquid liquid neutralization reaction, with a kind of boehmite for crystal seed, makes decomposing sodium aluminate solution separate out boehmite, adopts 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 that stirred, by crystal seed coefficient be 0.1 ~ 2.0 boehmite crystal seed add in sodium aluminate solution, sodium hydrogen carbonate solution is driven in reactive tank by peristaltic pump and carries out decomposition reaction with sodium aluminate solution, boehmite is crystal growth under crystal seed induction, after decomposing 2 ~ 7h, obtain degradation production.
Degradation production is through liquid-solid filtering separation, and solid water is washed till neutrality, and dry obtained boehmite product at 80 DEG C, boehmite content modification scope is wide, and granularity is sand shape.Filtrate Na
2cO
3under certain current density after electrolysis certain hour, in anolyte compartment, sodium carbonate is sodium bicarbonate by converting and discharge sodium ion and oxygen, represents, the NaHCO that electrolysis obtains such as formula (4)
3solution is separating 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, decomposing solution temperature 85 ~ 100 DEG C, sodium bicarbonate concentration 60 ~ 120 grams per liter, adding rate 0.2 ~ 1.0gL
-1min
-1, addition manner comprise at a slow speed with quick two kinds, 2 ~ 7 hours resolving times.Diaphragm electrolysis carbon mother liquid temperature 40 ~ 80 DEG C, electrolysis time 4 ~ 20 hours, current density 0.01 ~ 0.1A/cm
2.Decompose boehmite granularity in after product large, sandy alumina requirement can have been reached.
In addition, the concentration of described sodium aluminate solution is preferably Al
2o
380 ~ 100 grams per liters, causticization coefficient is 1.3 ~ 1.5, and decomposing solution temperature is 85 ~ 95 DEG C.
Described sodium bicarbonate concentration is 80 ~ 100 grams per liters, and adding rate 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 decomposition mother solution temperature is 40 ~ 60 DEG C, 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 as having the following advantages:
(1) seed precipitation process of Bayer process and sintering process is applicable to, rate of decomposition is high, and separate out boehmite granularity large (median size 80 ~ 120 microns), boehmite content modification scope wide (60% ~ 98%), breaches the bottleneck of conventional decomposition course boehmite product particle size tiny (<40 micron), boehmite content low (about 50%).
(2) industrial sodium aluminate solution can be adopted to be raw material, to there is not the shortcomings such as traditional boehmite (mainly producing activated alumina) preparation process raw materials cost is high, complex process.
(3) carbon mother liquid (Na
2cO
3) obtain NaHCO through diaphragm electrolysis in positive column
3solution, can be directly used in seed precipitation process, and cost is low and can realize feedstock circulation comprehensive utilization.
Accompanying drawing explanation
Fig. 1 is flow chart making of the present invention.
Embodiment
Introduce outstanding advantages of the present invention and innovative point further below by embodiment, but the present invention is in no way limited to embodiment.Embodiment 1:
Configure sodium aluminate solution 200ml with industrial aluminium hydroxide and sodium hydroxide, chemical composition is Al
2o
360 grams per liters, causticization coefficient is 1.3, decomposing solution temperature 85 DEG C, stirring velocity 100rmin
-1under condition, add the boehmite crystal seed that crystal seed coefficient is 0.1, and to add concentration with peristaltic pump be 60 grams per liter NaHCO
3solution, adding rate 0.2gL
-1min
-1, resolving time 2h, is separated the boehmite of precipitation with carbon mother liquid, obtains product boehmite.Gained carbon mother liquid is through diaphragm electrolysis, and electrolytic solution temperature 40 DEG C, electrolysis time 4h, current density is 0.01A/cm
2, obtain NaHCO in positive column
3solution, is adjusted to 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/μm | Anode hydrogen-carbonate na concn/g/L |
| 75% | 120 | 40 |
Embodiment 2:
Configure sodium aluminate solution 200ml with industrial aluminium hydroxide and sodium hydroxide, chemical composition is Al
2o
3120 grams per liters, causticization coefficient is 1.7, decomposing solution temperature 95 DEG C, stirring velocity 200rmin
-1under condition, add the boehmite crystal seed that crystal seed coefficient is 1.0, and to add concentration with peristaltic pump be 80 grams per liter NaHCO
3solution, adding rate 0.8gL
-1min
-1, resolving time 4h, is separated the boehmite of precipitation with carbon mother liquid, obtains product boehmite.Gained carbon mother liquid is through diaphragm electrolysis, and electrolytic solution temperature 50 C, electrolysis time 8h, current density is 0.1A/cm
2, obtain NaHCO in positive column
3solution, is adjusted to 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/μm | Anode hydrogen-carbonate na concn/g/L |
| 80% | 85 | 60 |
Embodiment 3:
Configure sodium aluminate solution 200ml with industrial aluminium hydroxide and sodium hydroxide, chemical composition is Al
2o
3140 grams per liters, causticization coefficient is 1.5, decomposing solution temperature 85 DEG C, stirring velocity 300rmin
-1under condition, add the boehmite crystal seed that crystal seed coefficient is 2.0, and to add concentration with peristaltic pump be 100 grams per liter NaHCO
3solution, adding rate 0.4gL
-1min
-1, resolving time 7h, is separated the boehmite of precipitation with carbon mother liquid, obtains product boehmite.Gained carbon mother liquid is through diaphragm electrolysis, and electrolytic solution temperature 60 C, electrolysis time 16h, current density is 0.02A/cm
2, obtain NaHCO in positive column
3solution, is adjusted to 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/μm | Anode hydrogen-carbonate na concn g/L |
| 95 | 110 | 75 |
Embodiment 4:
Configure sodium aluminate solution 200ml with industrial aluminium hydroxide and sodium hydroxide, chemical composition is Al
2o
3160 grams per liters, causticization coefficient is 1.6, decomposing solution temperature 95 DEG C, stirring velocity 200rmin
-1under condition, add the boehmite crystal seed that crystal seed coefficient is 1.0, and to add concentration with peristaltic pump be 120 grams per liter NaHCO
3solution, adding rate 0.4
gl
-1min
-1, resolving time 6h, the boehmite of precipitation is separated with carbon mother liquid, obtains product boehmite.Gained carbon mother liquid is through diaphragm electrolysis, and electrolytic solution temperature 80 DEG C, electrolysis time 18h, current density is 0.08A/cm
2, obtain NaHCO in positive column
3solution, is adjusted to 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/μm | Anode hydrogen-carbonate na concn g/L |
| 88 | 95 | 100 |
Embodiment 5:
Configure sodium aluminate solution 200ml with industrial aluminium hydroxide and sodium hydroxide, chemical composition is Al
2o
3120 grams per liters, causticization coefficient is 1.5, decomposing solution temperature 90 DEG C, stirring velocity 100rmin
-1under condition, add the boehmite crystal seed that crystal seed coefficient is 0.6, and to add in-degree with peristaltic pump be 80 grams per liter NaHCO
3solution 300ml, adding rate increases gradually, resolving time 5h, is separated by the boehmite of precipitation with carbon mother liquid, obtains product boehmite.Gained carbon mother liquid is through diaphragm electrolysis, and electrolytic solution temperature 50 C, electrolysis time 20h, current density is 0.01A/cm
2, obtain NaHCO in positive column
3solution, is adjusted to 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/μm | Anode hydrogen-carbonate na concn g/L |
| 90 | 106 | 83 |
Embodiment 6:
Configure sodium aluminate solution 200ml with industrial aluminium hydroxide and sodium hydroxide, chemical composition is Al
2o
3100 grams per liters, causticization coefficient is 1.7, decomposing solution temperature 100 DEG C, stirring velocity 300rmin
-1under condition, add the boehmite crystal seed that crystal seed coefficient is 1.5, and to add in-degree with peristaltic pump be 100 grams per liter NaHCO
3solution 300ml, adding rate reduces gradually, resolving time 6h, is separated by the boehmite of precipitation with carbon mother liquid, obtains product boehmite.Gained carbon mother liquid is through diaphragm electrolysis, and electrolytic solution temperature 80 DEG C, electrolysis time 12h, current density is 0.06A/cm
2, obtain NaHCO in positive column
3solution, is adjusted to 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/μm | Anode hydrogen-carbonate na concn g/L |
| 92 | 92 | 80 |
Embodiment 7:
Configure sodium aluminate solution 200ml with industrial aluminium hydroxide and sodium hydroxide, chemical composition is Al
2o
380 grams per liters, causticization coefficient is 1.4, decomposing solution temperature 80 DEG C, stirring velocity 200rmin
-1under condition, add the boehmite crystal seed that crystal seed coefficient is 1.5, and to add in-degree with peristaltic pump be 80 grams per liter NaHCO
3solution 300ml, adding rate reduces gradually, resolving time 5h, is separated by the boehmite of precipitation with carbon mother liquid, obtains product boehmite.Gained carbon mother liquid is through diaphragm electrolysis, and electrolytic solution temperature 85 DEG C, electrolysis time 14h, current density is 0.05A/cm
2, obtain NaHCO in positive column
3solution, is adjusted to 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/μm | Anode hydrogen-carbonate na concn g/L |
| 86 | 83 | 90 |
In a word, the present invention adopts sodium bicarbonate reinforcing sodium aluminate solution to divide and parses boehmite, novel NaHCO
3liquid phase method carbon divides and changes solution-air two-step reaction into liquid-liquid single step reaction, eliminate gas film mass transfer to control to cause local undue, reactive liquid solution make system degree of supersaturation evenly and easily regulation and control, be beneficial to the control of boehmite nucleation and crystallization, and sodium bicarbonate comes from electrolytic carbon decomposition mother solution positive column product, the circulation comprehensive achieving sodium carbonate utilizes, and has to plant to divide and CO
2the advantage that carbon divides, also overcomes their disadvantage simultaneously, 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 completely, implementation procedure and the same the various embodiments described above of method; 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 thereto, any those skilled in the art are in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
Claims (5)
1. a sodium aluminate solution and sodium bicarbonate liquid phase method carbon divide the method preparing boehmite, it is characterized in that: adopt sodium hydrogen carbonate solution liquid phase method decomposition sodium aluminate liquid, add boehmite crystal seed in sodium aluminate solution, and add sodium bicarbonate and sodium aluminate solution generation decomposition reaction, boehmite is crystal growth under crystal seed induction, through solid-liquid separation after decomposition, obtain 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, achieves 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, causticization coefficient is 1.3 ~ 1.7, and stirring velocity is 100 ~ 300rmin
-1, boehmite crystal seed coefficient is 0.1 ~ 2.0, and decomposing solution temperature is 85 ~ 100 DEG C; Sodium bicarbonate concentration is 60 ~ 120 grams per liters, and sodium bicarbonate adding rate is 0.2 ~ 1.0gL
-1min
-1, addition manner comprise at a slow speed with quick two kinds of patterns, the decomposition reaction time is 2 ~ 7 hours; Electrolytic carbon decomposition mother solution temperature is 40 ~ 80 DEG C, and electrolysis time is 4 ~ 20 hours, and current density is 0.01 ~ 0.1A/cm
2.
2. in accordance with the method for claim 1, it is characterized in that: the concentration of described sodium aluminate solution is Al
2o
380 ~ 100 grams per liters, decomposing solution temperature is 85 ~ 95 DEG C.
3. in accordance with the method for claim 1, it is characterized in that: described sodium bicarbonate concentration is 80 ~ 100 grams per liters, adding rate 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, stirring velocity is 150 ~ 200rmin
-1.
5. in accordance with the method for claim 1, it is characterized in that: described electrolytic carbon decomposition mother solution temperature is 40 ~ 60 DEG C, and electrolysis time is 5 ~ 10 hours, and current density is 0.01 ~ 0.05A/cm
2.
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| IT202000016093A1 (en) * | 2020-07-03 | 2022-01-03 | Giacomo Mencarini | PROCEDURE FOR THE RECYCLING OF ALUMINUM-BASED MATERIALS FOR FOOD USE |
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| CN104003429B (en) * | 2014-06-14 | 2015-09-30 | 中国科学院过程工程研究所 | A kind of method utilizing Bayer-process seed-separating mother liquor to prepare boehmite |
| 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 |
| CN111392753B (en) * | 2020-03-31 | 2022-03-15 | 中国铝业股份有限公司 | Method for separating out sodium bicarbonate from deep carbonation mother liquor |
| 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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