CN104003429B - A kind of method utilizing Bayer-process seed-separating mother liquor to prepare boehmite - Google Patents
A kind of method utilizing Bayer-process seed-separating mother liquor to prepare boehmite Download PDFInfo
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- CN104003429B CN104003429B CN201410266128.2A CN201410266128A CN104003429B CN 104003429 B CN104003429 B CN 104003429B CN 201410266128 A CN201410266128 A CN 201410266128A CN 104003429 B CN104003429 B CN 104003429B
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Abstract
The invention discloses a kind of method utilizing Bayer-process seed-separating mother liquor to prepare boehmite, relate to the method that the intermediate solution of producing from aluminum oxide industry prepares boehmite.The present invention adopts NaHCO
3solution and Bayer-process seed-separating mother liquor generation neutralization reaction, bayer's process seed precipitation solution decomposition and crystallization separates out precipitation, agingly obtains product boehmite through for some time; The carbon mother liquid that Bayer-process seed-separating mother liquor obtains after decomposing, through diaphragm electrolysis, obtains sodium hydrogen carbonate solution in positive column, returns decomposition process, realize the recycle of sodium bicarbonate.The method is applicable to utilize Bayer-process seed-separating mother liquor to prepare the boehmite product of bigger serface, large pore volume, and rate of decomposition is fast and can reduce aluminium oxide calcining energy consumption.
Description
Technical field
The invention belongs to Chemicals preparation field, be specifically related to a kind of method utilizing Bayer-process seed-separating mother liquor to prepare boehmite, is the method that the intermediate solution of producing from aluminum oxide industry prepares boehmite furtherly.
Background technology
Aluminum oxide is the main raw material producing non-ferrous metal aluminium, the aluminum oxide of more than 90% is used for electrolysis aluminium metallurgy, this part aluminum oxide is called as metallurgical-grade aluminum oxide, and the aluminum oxide used beyond electrolysis aluminium metallurgy is called non-metallurgical-grade aluminum oxide or multiform alumina or chemical aluminum oxide.The production method of metallurgical-grade aluminum oxide mainly comprises Bayer process and sintering process, and wherein Bayer process is the prevailing technology of alumina producing, and at present, the aluminum oxide of produced worldwide and aluminium hydroxide, have more than 90% to be adopt Bayer process to produce.Namely two large processes of Bayer process decompose and stripping.
The decomposition of crystal seed process of sodium aluminate solution be molecular ratio lower (about about 1.6) sodium aluminate solution at normal temperatures, add aluminium hydroxide as crystal seed, constantly stir, the Al in solution
2o
3just slowly separate out with aluminium hydroxide form, the molecular ratio of solution constantly increases simultaneously.Process in leaching refers to separates out the solution (being referred to as decomposition nut liquid) after most of aluminium hydroxide, again can hydrated alumina in stripping bauxite when heating, and Here it is utilizes the process of seed precipitation solution stripping bauxite.Be used alternatingly above two processes and just can process bauxite many batches ofly, obtain pure aluminum hydroxide product, form the circulation of so-called Bayer process.The essence of Bayer process reacts (1) hocketing at different conditions exactly.
The feature of Bayer process is applicable high A/S ore, A/S > 7; This method flow process is simple, and cost is low; Good product quality, purity is high.Sodium aluminate solution crystal seed decomposition is the critical process of Bayer process production metallurgy grade aluminum oxide, it is characterized by resolving time long (40 ~ 70 hours), decomposition efficiency low (about 50%), make the consumption energy that about 50% aluminum oxide is meaningless in Recycling Mother Solution, take equipment capacity, be the major reason that in alumina producing, energy consumption is high, cost is high, decomposition of crystal seed becomes the bottleneck of alumina producing Bayer process industrial technology development.Therefore, point Focal point and difficult point being always China and the research of world's aluminum oxide industry is planted.If energy reasonable utilization Bayer-process seed-separating mother liquor, improves decomposing sodium aluminate solution rate, then can increase substantially alumina producing efficiency, significantly energy-saving and cost-reducing, significantly reduce costs, bring important and far-reaching impact will to China and world's aluminum oxide industry.
Boehmite, molecular formula Al
2o
3h
2o is preparation γ-Al
2o
3with α-Al
2o
3deng the important presoma of crystal formation aluminum oxide, can be used as non-metallurgical-grade aluminum oxide, to be widely used in support of the catalyst, fire retardant, refractory materials, coated material, sorbent material, binding agent etc. multi-field.Tradition alumina producing Bayer process adopts gibbsite decomposition of crystal seed supersaturated sodium aluminate solution, obtains aluminum oxide, as shown in (2) at 1000 ~ 1200 DEG C of Roasting Decomposition product gibbsites.
Al
2O
3·3H
2O
(s)→Al
2O
3(s)+3H
2O ΔH＝170KJ/mol (2)
The energy consumption of Roasting Decomposition product consumption is equivalent to 1/4th of current alumina producing total energy consumption, if directly separate out boehmite in seed precipitation process, then can save 60% of roasting energy consumption, i.e. (3)
Al
2O
3·H
2O
(s)→Al
2O
3(s)+H
2O ΔH＝72KJ/mol (3)
Decomposition course adopts boehmite to replace gibbsite, can reduce the energy consumption of producing aluminum oxide, reduces production cost, has unrivaled advantage and vast potential for future development.CN1186046A discloses one and first in sodium aluminate solution, passes into CO
2, reduce supersaturated sodium aluminate solution causticization coefficient, then add a crystal kind and make sodium aluminate solution crystal seed decompose the method preparing boehmite.The method is to 90 ~ 110g/l Al
2o
3, in the sodium aluminate solution of causticization coefficient 1.4 ~ 1.6, pass into CO
2gas, treats solution causticization factor alpha
kafter being down to 1.2 ~ 1.3, under 110 ~ 120 DEG C and seed ratio 2.0 ~ 2.5 condition, decomposition of crystal seed 30h, rate of decomposition can reach 48% ~ 52%, passes into CO
2consume the NaOH that utility value in subsequent technique is higher, and degradation production can only be used as the precursor of metallurgical-grade aluminum oxide, range of operating parameters is narrow is unfavorable for operation, is difficult to realize industrialization.Adopt sodium metaaluminate and Tai-Ace S 150 to be raw material in CN102653410, Hydrothermal Synthesis threadiness boehmite, the nanometer fibrous boehmite of Fibre diameter 5 ~ 20nm, its specific surface area is at 100m
2/ g ~ 249m
2/ g, its production cost is not high, environmental friendliness.Mention using aluminum nitrate as aluminium source in CN102153119A, by adding organic formwork agent (cetyl trimethylammonium bromide, Macrogol 2000, copolymer p 123 etc.) volatile salt as precipitation agent, preparing diameter is 7 ~ 500nm, length is 2 ~ 3 μm, and specific surface area is at 290 ~ 380m
2the boehmite of/g, but it adds a lot of expensive organic formwork agent, and production cost is too high, and environmental pollution is large.W. R. Grace & Co of the U.S. has reported the boehmite being prepared 2 ~ 20nm by the aluminium hydroxide after grinding and activated alumina under crystal growth inhibitor (silicate or phosphoric acid salt) exists through hydro-thermal reaction in CN1213800C, but the boehmite alumina content that this method obtains is low, containing a large amount of silicon oxide and phosphoric acid salt, the existence of these impurity is all disadvantageous in much reacting.Alumina producing flow process is alkali flow process, is afraid of the pollution of acidic substance most, as with Al
2(SO
4)
3alCl
3or HNO
3boehmite is produced with sodium aluminate solution, the SO after reaction in mother liquor Deng in acidic substance
4 2-, Cl
-, NO
3 -all can bring heavy corrosion to alumina producing flow process and equipment Deng acidic anionic, and mother liquor also cannot returning alumina Production Flow Chart recycle, thus produce and be subject to a definite limitation.Patent " a kind of sodium aluminate solution and sodium bicarbonate liquid phase method carbon divide the method preparing the boehmite " (patent No.: 201310382973.1) propose to adopt sodium bicarbonate liquid phase method carbon to divide sodium aluminate solution that Wang Zhi etc. declare, add boehmite crystal seed induction decomposing sodium aluminate solution and separate out boehmite, after decomposing, gained carbon mother liquid obtains sodium bicarbonate through diaphragm electrolysis, returns decomposition course stand-by.But the product that this method obtains is the metallurgical grade boehmite that added value is lower, and with a certain amount of gibbsite in product.Existing enterprise adopts and pass into CO in sodium aluminate solution
2method produce boehmite, affect by factor in many ways in production, product performance are stable not, and product is usually with the appearance of bayerite and gibbsite, and throughput is restricted, and facility investment is large, can not well meet consumers' demand.
Summary of the invention
The present invention is directed to the Bayer-process seed-separating mother liquor meaningless circulation in systems in which that prior art exists, increase the problems such as production energy consumption, object is that providing a kind of is raw material with Bayer-process seed-separating mother liquor, uses NaHCO
3decompose Bayer-process seed-separating mother liquor, does liquid phase method carbon divide the higher non-metallurgical grade of preparation added value to use from Bayer-process seed-separating mother liquor? the method of boehmite product, and the sodium carbonate solution that seed precipitation solution obtains after decomposing can generate sodium bicarbonate through diaphragm electrolysis, returns decomposition course and recycles.
The present invention is the above-mentioned purpose that is achieved by the following technical programs:
A kind of method utilizing Bayer-process seed-separating mother liquor to prepare boehmite, employing Bayer-process seed-separating mother liquor is raw material, Bayer-process seed-separating mother liquor is decomposed with sodium hydrogen carbonate solution, boehmite is as crystal seed, organic additive is as dispersion agent, under agitation condition there is neutralization reaction in sodium bicarbonate and Bayer-process seed-separating mother liquor fast, crystallization precipitates, aging through for some time, slurries realize solid-liquor separation after filtration, solid part washing is dry obtains product boehmite, liquid portion is the diaphragm electrolysis carbon mother liquid sodium hydrogen carbonate solution obtained in positive column, for liquid phase method carbon step by step, realize sodium hydrogen carbonate solution recycling, the condition that described sodium bicarbonate decomposes Bayer-process seed-separating mother liquor is: the concentration of Bayer-process seed-separating mother liquor is Al
2o
330 ~ 80 grams per liters, causticization coefficient is 2.1 ~ 3.2, and stirring velocity is 100 ~ 500rmin
-1neutral temperature is 30 ~ 90 DEG C, aging temperature is 70 ~ 100 DEG C, crystal seed coefficient is 0 ~ 1.5, sodium bicarbonate concentration is 70 ~ 150 grams per liters, namely reaction times neutralize with digestion time is 0.5 hour ~ 8 hours, and dispersion agent is one or both in organic additive polyhydroxy-alcohol, many carboxylic acids, and addition is 0% ~ 5%.
Bayer-process seed-separating mother liquor is utilized to prepare boehmite method by described one, under wherein said agitation condition there is neutralization reaction and comprise sodium hydrogen carbonate solution and add in Bayer-process seed-separating mother liquor in sodium bicarbonate and Bayer-process seed-separating mother liquor fast, or Bayer-process seed-separating mother liquor adds in sodium hydrogen carbonate solution, or both simultaneously and stream join in reactive tank and react.
Utilize Bayer-process seed-separating mother liquor to prepare boehmite method by described one, wherein said Bayer-process seed-separating mother liquor concentration is Al
2o
330 ~ 80 grams per liters, Al
2o
350 ~ 70g/l, causticization coefficient is 2.4 ~ 3.0, and neutralization reaction temperature is 50 ~ 80 DEG C, and aging temperature is 85 ~ 100 DEG C.
Utilize Bayer-process seed-separating mother liquor to prepare boehmite method by described one, wherein said crystal seed coefficient 0 ~ 1.5, sodium bicarbonate concentration is 90 ~ 120 grams per liters.
Utilize Bayer-process seed-separating mother liquor to prepare boehmite method by described one, namely the wherein said sodium hydrogen carbonate solution decomposition Bayer-process seed-separating mother liquor reaction times neutralize with digestion time is 0.5 ~ 4 hour, and stirring velocity is 100 ~ 500rmin
-1.
Utilize Bayer-process seed-separating mother liquor to prepare boehmite method by described one, wherein said dispersion agent addition is 0.05% ~ 3%.
Utilize Bayer-process seed-separating mother liquor preparative chemistry product boehmite method by described one, wherein said Bayer-process seed-separating mother liquor rate of decomposition is 60% ~ 95%.
Utilize Bayer-process seed-separating mother liquor to prepare boehmite method by described one, wherein said boehmite product specific surface area scope is at 100 ~ 400m
2/ g, pore volume scope are at 0.5 ~ 2.0ml/g.
Compared with prior art, excellent benefit of the present invention is:
1. adopt Bayer-process seed-separating mother liquor to be raw material, NaHCO
3liquid phase method carbon divides Bayer-process seed-separating mother liquor to prepare the boehmite of high added value, for producing aluminum oxide energy efficient, realizing Bayer-process seed-separating mother liquor recycling, having economic interests and application potential.
2. adopt NaHCO
3as neutralizing agent, the fast and Bayer-process seed-separating mother liquor rate of decomposition high (more than 80%) of speed of response, and other acid ions that can not induce one in the circulation of aluminum oxide alkalescence, can not cause corrosion to flow process and equipment.
3. Bayer-process seed-separating mother liquor decomposes rear gained carbon mother liquid through diaphragm electrolysis renewable one-tenth NaHCO
3, liquid phase method carbon operation break-down can be returned and use, achieve the recycle of material.
4. this invention produces boehmite preparation technology simply, and easy to operate, parameter is controlled, and production cost is lower, excellent product performance, without gibbsite or other dephasigns of bayerite.Control certain preparation condition and can obtain high-specific surface area (100 ~ 4000m
2/ g), the boehmite product of large pore volume (0.5 ~ 2.0ml/g), be with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the process flow sheet preparing boehmite with Bayer-process seed-separating mother liquor;
Fig. 2 is the XRD spectra of the boehmite product prepared under not adding crystal seed condition with Bayer-process seed-separating mother liquor;
Fig. 3 is the SEM photo of the boehmite product prepared under not adding crystal seed condition with Bayer-process seed-separating mother liquor;
Fig. 4 is the XRD spectra of the boehmite product prepared under adding boehmite crystal seed condition with Bayer-process seed-separating mother liquor;
Fig. 5 is the SEM photo of the boehmite product prepared under adding boehmite crystal seed condition with Bayer-process seed-separating mother liquor.
Embodiment
Below in conjunction with accompanying drawing, with embodiments of the invention, the invention will be further described, but do not limit the present invention with this.
The present invention is a kind of method utilizing Bayer-process seed-separating mother liquor to prepare boehmite, and the technical process of the method as shown in Figure 1, can be summarized as following steps:
1. there is neutralization reaction under stirring action in Bayer-process seed-separating mother liquor and sodium hydrogen carbonate solution in isothermal reaction groove, non-metallurgical grade boehmite is crystal seed, be added with organic additive as dispersion agent, Bayer-process seed-separating mother liquor decomposes gained and is deposited in and carries out aging in carbon mother liquid, obtains slurries.
2. the slurries after aging, through isolated by vacuum filtration, obtain filter cake and carbon mother liquid (Na
2cO
3), extremely neutral with the deionized water wash filter cake of heat, filter cake is at 120 DEG C of baking oven inner drying 24h subsequently, and solid product obtains boehmite powder after depolymerization.Carbon mother liquid is converted into sodium bicarbonate through diaphragm electrolysis in anolyte compartment, represents, the NaHCO that electrolysis obtains such as formula (4)
3solution is separating out boehmite for Bayer-process seed-separating mother liquor.
The feature of aforesaid method is: Bayer-process seed-separating mother liquor concentration Al
2o
330 ~ 80g/l, causticization coefficient 2.1 ~ 3.2, stirring velocity 100 ~ 500rmin
-1, neutral temperature 30 ~ 90 DEG C, aging temperature 70 ~ 100 DEG C, crystal seed coefficient 0 ~ 1.5, NaHCO
3concentration 70 ~ 150g/l, addition manner is short mix, comprises Bayer-process seed-separating mother liquor and adds NaHCO to
3in solution, NaHCO
3solution to add in Bayer-process seed-separating mother liquor and both simultaneously and stream joins in reactive tank, 0.5 hour ~ 8 hours reaction times (neutralization and digestion time).Dispersion agent is one or more in the organic additive such as polyhydroxy-alcohol, many carboxylic acids, and addition is 0% ~ 5%.Electrolytic carbon decomposition mother solution obtains sodium hydrogen carbonate solution in positive column, and concentration can reach 40 ~ 100g/l, returns to carbon operation break-down, realizes sodium bicarbonate cyclic regeneration.
In addition, described Bayer-process seed-separating mother liquor concentration is preferably Al
2o
350 ~ 70g/l, causticization coefficient is 2.4 ~ 3.0.
Described neutralization reaction temperature is 50 ~ 80 DEG C, and aging temperature is 85 ~ 100 DEG C
Described sodium bicarbonate concentration is 90 ~ 120g/l, and crystal seed coefficient is 0 ~ 1.5.
Described dispersion agent addition is 0.05% ~ 3%.
The described reaction times is 0.5 ~ 4 hour, and stirring velocity is 100 ~ 500rmin
-1.
Here is several concrete concrete instances.
Embodiment 1
Adjustment Bayer-process seed-separating mother liquor concentration is Al
2o
330g/l, causticization coefficient is 2.1, and sodium bicarbonate concentration is 70g/l, 100ml Bayer-process seed-separating mother liquor is joined in reactive tank, reactive tank is placed in water bath with thermostatic control, is added fast in Bayer-process seed-separating mother liquor by 200ml sodium hydrogen carbonate solution and carries out neutralization reaction, stirring velocity 300rmin
-1, control neutral temperature 30 DEG C, gained slurries are aging at 70 DEG C, and the reaction times is 3 hours, and rapid filtration wash, realizes solid-liquor separation, and the grinding of solid drying obtains boehmite product.Gained carbon mother liquid, through diaphragm electrolysis, obtains the NaHCO of 45g/l in positive column
3solution, is adjusted to suitable concentration stand-by.
Bayer-process seed-separating mother liquor liquid phase method carbon divides and the results are shown in Table 1.
Table 1 Bayer-process seed-separating mother liquor liquid phase method carbon divides result
| Rate of decomposition/% | Boehmite specific surface area/m 2/g | Boehmite pore volume/ml/g |
| 70％ | 120 | 0.55 |
Embodiment 2
Adjustment Bayer-process seed-separating mother liquor concentration is Al
2o
350g/l, causticization coefficient is 2.4, sodium bicarbonate concentration is 90g/l, join in reactive tank by 100ml Bayer-process seed-separating mother liquor, reactive tank is placed in water bath with thermostatic control, is poured into fast in Bayer-process seed-separating mother liquor by 200ml sodium hydrogen carbonate solution and carries out neutralization reaction, add boehmite crystal seed, crystal seed coefficient 0.5, adds dispersion agent Macrogol 2000 addition 0.5%, stirring velocity 500rmin
-1, control neutral temperature 60 DEG C, gained slurries are aging at 100 DEG C, and the reaction times is 0.5 hour, and rapid filtration wash, realizes solid-liquor separation, and the grinding of solid drying obtains boehmite product.Gained carbon mother liquid, through diaphragm electrolysis, obtains the NaHCO of 65g/l in positive column
3solution, is adjusted to suitable concentration stand-by.
Bayer-process seed-separating mother liquor liquid phase method carbon divides and the results are shown in Table 2.
Table 2 Bayer-process seed-separating mother liquor liquid phase method carbon divides result
| Rate of decomposition/% | Boehmite specific surface area/m 2/g | Boehmite pore volume/ml/g |
| 75％ | 160 | 0.70 |
Embodiment 3
Adjustment Bayer-process seed-separating mother liquor concentration is Al
2o
380g/l, causticization coefficient is 2.8, sodium bicarbonate concentration is 120g/l, join in reactive tank by 200ml sodium hydrogen carbonate solution, reactive tank is placed in water bath with thermostatic control, pours 100ml Bayer-process seed-separating mother liquor into sodium hydrogen carbonate solution fast and carries out neutralization reaction, add boehmite crystal seed, crystal seed coefficient 1.5, adds dispersion agent Macrogol 4000 addition 1%, stirring velocity 200rmin
-1, control neutral temperature 80 DEG C, gained slurries are aging at 80 DEG C, and the reaction times is 5 hours, and rapid filtration wash, realizes solid-liquor separation, and the grinding of solid drying obtains boehmite product.Gained carbon mother liquid, through diaphragm electrolysis, obtains the NaHCO of 80g/l in positive column
3solution, is adjusted to suitable concentration stand-by.
Bayer-process seed-separating mother liquor liquid phase method carbon divides and the results are shown in Table 3.
Table 3 Bayer-process seed-separating mother liquor liquid phase method carbon divides result
| Rate of decomposition/% | Boehmite specific surface area/m 2/g | Boehmite pore volume/ml/g |
| 80％ | 200 | 0.83 |
Embodiment 4
Adjustment Bayer-process seed-separating mother liquor concentration is Al
2o
340g/l, causticization coefficient is 3.2, sodium bicarbonate concentration is 150g/l, join in reactive tank by 200ml sodium hydrogen carbonate solution, reactive tank is placed in water bath with thermostatic control, pours 100ml Bayer-process seed-separating mother liquor into sodium hydrogen carbonate solution fast and carries out neutralization reaction, add boehmite crystal seed, crystal seed coefficient 0.2, adds dispersion agent sodium lauryl sulphate addition 3%, stirring velocity 100rmin
-, control neutral temperature 50 DEG C, gained slurries are aging at 95 DEG C, and the reaction times is 6 hours, and rapid filtration wash, realizes solid-liquor separation, and the grinding of solid drying obtains boehmite product.Gained carbon mother liquid, through diaphragm electrolysis, obtains the NaHCO of 100g/l in positive column
3solution, is adjusted to suitable concentration stand-by.
Bayer-process seed-separating mother liquor liquid phase method carbon divides and the results are shown in Table 4.
Table 4 Bayer-process seed-separating mother liquor liquid phase method carbon divides result
| Rate of decomposition/% | Boehmite specific surface area/m 2/g | Boehmite pore volume/ml/g |
| 88％ | 255 | 0.62 |
Embodiment 5
Adjustment Bayer-process seed-separating mother liquor concentration is Al
2o
360g/l, causticization coefficient is 2.5, sodium bicarbonate concentration is 110g/l, 200ml sodium hydrogen carbonate solution and 100ml Bayer-process seed-separating mother liquor are also flowed to join fast in reactive tank and carries out neutralization reaction, reactive tank is placed in water bath with thermostatic control, add dispersion agent sodium lauryl sulphate addition 1%, stirring velocity 400rmin
-1, control neutral temperature 90 DEG C, gained slurries are aging at 90 DEG C, and the reaction times is 2 hours, and rapid filtration wash, realizes solid-liquor separation, and the grinding of solid drying obtains boehmite product.Gained carbon mother liquid, through diaphragm electrolysis, obtains the NaHCO of 75g/l in positive column
3solution, is adjusted to suitable concentration stand-by.
Bayer-process seed-separating mother liquor liquid phase method carbon divides and the results are shown in Table 5.
Table 5 Bayer-process seed-separating mother liquor liquid phase method carbon divides result
| Rate of decomposition/% | Boehmite specific surface area/m 2/g | Boehmite pore volume/ml/g |
| 76％ | 285 | 1.13 |
Embodiment 6
Adjustment Bayer-process seed-separating mother liquor concentration is Al
2o
350g/l, causticization coefficient is 2.2, sodium bicarbonate concentration is 100g/l, 100ml Bayer-process seed-separating mother liquor is joined in reactive tank, reactive tank is placed in water bath with thermostatic control, is poured into fast in Bayer-process seed-separating mother liquor by 200ml sodium hydrogen carbonate solution and carries out neutralization reaction, adds dispersion agent Macrogol 2000 and coordinates by 1:1 with Macrogol 4000, addition 4%, stirring velocity 150rmin
-1, control neutral temperature 70 DEG C, gained slurries are aging at 100 DEG C, and the reaction times is 8 hours, and rapid filtration wash, realizes solid-liquor separation, and the grinding of solid drying obtains boehmite product.Gained carbon mother liquid, through diaphragm electrolysis, obtains 60g/l NaHCO in positive column
3solution, is adjusted to suitable concentration stand-by.
Bayer-process seed-separating mother liquor liquid phase method carbon divides and the results are shown in Table 6.
Table 6 Bayer-process seed-separating mother liquor liquid phase method carbon divides result
| Rate of decomposition/% | Boehmite specific surface area/m 2/g | Boehmite pore volume/ml/g |
| 93％ | 350 | 1.50 |
Claims (8)
1. the method utilizing Bayer-process seed-separating mother liquor to prepare boehmite, it is characterized in that: employing Bayer-process seed-separating mother liquor is raw material, Bayer-process seed-separating mother liquor is decomposed with sodium hydrogen carbonate solution, boehmite is as crystal seed, organic additive is as dispersion agent, under agitation condition there is neutralization reaction in sodium bicarbonate and Bayer-process seed-separating mother liquor fast, crystallization precipitates, aging through for some time, slurries realize solid-liquor separation after filtration, solid part washing is dry obtains product boehmite, liquid portion is carbon mother liquid, this carbon mother liquid obtains sodium hydrogen carbonate solution in positive column after diaphragm electrolysis, for liquid phase method carbon step by step, realize sodium hydrogen carbonate solution recycling, the condition that described sodium bicarbonate decomposes Bayer-process seed-separating mother liquor is: the concentration of Bayer-process seed-separating mother liquor is Al
2o
330 ~ 80 grams per liters, causticization coefficient is 2.1 ~ 3.2, and stirring velocity is 100 ~ 500rmin
-1neutral temperature is 30 ~ 90 DEG C, aging temperature is 70 ~ 100 DEG C, crystal seed coefficient is 0 ~ 1.5, sodium bicarbonate concentration is 70 ~ 150 grams per liters, namely reaction times neutralize with digestion time is 0.5 hour ~ 8 hours, and dispersion agent is one or both in organic additive polyhydroxy-alcohol, many carboxylic acids, and addition is 0% ~ 5%.
2. utilize Bayer-process seed-separating mother liquor to prepare boehmite method according to one according to claim 1, it is characterized in that: under described agitation condition, sodium bicarbonate and Bayer-process seed-separating mother liquor neutralization reaction occurs fast comprise sodium hydrogen carbonate solution and add in Bayer-process seed-separating mother liquor, or Bayer-process seed-separating mother liquor adds in sodium hydrogen carbonate solution, or both simultaneously and stream join in reactive tank and react.
3. utilize Bayer-process seed-separating mother liquor to prepare boehmite method according to one according to claim 1, it is characterized in that: described Bayer-process seed-separating mother liquor concentration is Al
2o
350 ~ 70g/l, causticization coefficient is 2.4 ~ 3.0, and neutralization reaction temperature is 50 ~ 80 DEG C, and aging temperature is 85 ~ 100 DEG C.
4. utilize Bayer-process seed-separating mother liquor to prepare boehmite method according to one according to claim 1, it is characterized in that: described crystal seed coefficient 0 ~ 1.5, sodium bicarbonate concentration is 90 ~ 120 grams per liters.
5. utilize Bayer-process seed-separating mother liquor to prepare boehmite method according to one according to claim 1, it is characterized in that: namely the described sodium hydrogen carbonate solution decomposition Bayer-process seed-separating mother liquor reaction times neutralize with digestion time is 0.5 ~ 4 hour, and stirring velocity is 100 ~ 500rmin
-1.
6. utilize Bayer-process seed-separating mother liquor to prepare boehmite method according to one according to claim 1, it is characterized in that: described dispersion agent addition is 0.05% ~ 3%.
7. utilize Bayer-process seed-separating mother liquor to prepare boehmite method according to one according to claim 1, it is characterized in that: described Bayer-process seed-separating mother liquor rate of decomposition is 60% ~ 95%.
8. utilize Bayer-process seed-separating mother liquor to prepare boehmite method according to one according to claim 1, it is characterized in that: described boehmite product specific surface area scope is at 100 ~ 400m
2/ g, pore volume scope are at 0.5 ~ 2.0ml/g.
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| CN101665262B (en) * | 2009-10-21 | 2011-07-06 | 中国铝业股份有限公司 | Preparation method for pseudo-boehmite |
| CN101920978B (en) * | 2010-06-25 | 2012-12-12 | 山西铝厂科技化工公司 | Method for producing boehmite by using washing liquor |
| CN102942199B (en) * | 2012-10-17 | 2014-04-09 | 河南科技大学 | Preparation method of boehmite nanocrystallines or nanowhiskers |
| CN103449486B (en) * | 2013-08-29 | 2015-05-06 | 中国科学院过程工程研究所 | Method for preparing boehmite by liquid phase carbonating decomposition of sodium aluminate solution and sodium bicarbonate |
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2014
- 2014-06-14 CN CN201410266128.2A patent/CN104003429B/en not_active Expired - Fee Related
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