CN105347373B - Preparation method of pseudo-boehmite - Google Patents
Preparation method of pseudo-boehmite Download PDFInfo
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- CN105347373B CN105347373B CN201510809736.8A CN201510809736A CN105347373B CN 105347373 B CN105347373 B CN 105347373B CN 201510809736 A CN201510809736 A CN 201510809736A CN 105347373 B CN105347373 B CN 105347373B
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Abstract
The invention discloses a preparation method of pseudo-boehmite. The preparation method comprises the following steps: the step of gel-forming, the step of aging, the step of separation and washing and the step of drying. During the step of gel-forming, a meta-aluminate solution and carbon dioxide gas are contacted with each other in an inorganic membrane reactor so as to form a reaction product, wherein pressure of the carbon dioxide gas is greater than or equal to 0.1 MPa. By the method of the invention, pseudo-boehmite of stable quality can be produced.
Description
Technical field
The side of boehmite is produced the present invention relates to a kind of preparation method of boehmite, especially a kind of carbonizatin method
Method.
Background technology
Alumina powder is often used in as drier, adsorbent, catalyst and catalyst carrier in chemical field.But
It is that naturally or manually a water aluminum oxide of production and the specific surface area of gibbsite are low, pore volume is small, activity is low, thus can not
For doing drier, adsorbent, catalyst and catalyst carrier.Boehmite has high-specific surface area, big pore volume, macropore
The features such as footpath, high activity, it is suitable for making the catalyst in field such as drier, adsorbent and petrochemical industry, chemical fertilizer and tail gas and urges
Agent carrier etc..Accordingly, it would be desirable to a water aluminum oxide or gibbsite are converted into boehmite.
Crystallization degree of pseudo-boehmite is low, and water content is higher than boehmite, is often existed with colloidal state.At present, boehmite
Preparation method mainly includes aluminium alcoholates Hydrolyze method, acid system and alkaline process (carbonizatin method).
Having main steps that for aluminium alcoholates Hydrolyze method production boehmite is anti-with higher alcohol in the presence of a catalyst by metallic aluminium
Aluminium alcoholates should be generated.The product purity of aluminium alcoholates Hydrolyze method is high, but a large amount of waste water, Organic Alcohol recovery cost can be formed in production process
Greatly, boehmite selling at exorbitant prices is caused.
Acid system be with aluminium salts such as aluminum sulfate, aluminum nitrate, aluminium chloride as raw material, it is solvable with NaOH, sodium carbonate, ammoniacal liquor etc.
Property alkali carry out neutralization reaction and prepare boehmite, preparation process includes that plastic, aging, washing are dried etc..The main of acid system lacks
Point is the relatively costly of production boehmite.
China mainly produces boehmite using carbonizatin method.Department of chemistry of Tongji University, Shanghai Petroleum Chemical Engineering Institute, temperature
The units such as Zhou Jing crystal aluminas Co., Ltd have carried out deep development to alkaline process boehmite.The basic process steps of alkaline process
Including gel, aging, separation and washing, dry etc..During carbonizatin method plastic, there is NaOH and CO2Quick neutralization reaction,
NaAlO2With CO2Neutralization reaction, NaAlO2Spontaneous hydrolysis reaction, CO2With the aluminium hydroxide (hydrated alumina) and Na of generation2CO3
Recombination reaction, specific reaction equation is as follows：
2NaOH+CO2=Na2CO3+H2O (1)
2NaAlO2+CO2+3H2O=2Al (OH)3+Na2CO3 (2)
NaAlO2+2H2O=Al (OH)3+NaOH (3)
Na2CO3+CO2+2Al(OH)3=2NaAl (CO3)(OH)2+H2O (4)
The aluminium hydroxide of reaction (2) generation is converted into boehmite under optimum conditions, and reacts the hydrogen-oxygen of (3) generation
Change aluminium and be then converted into gibbsite, and reaction (2) and reaction (3) they are parallel reaction.Therefore, thin water aluminium is intended in the product of carbonizatin method
Stone or gibbsite content depend on the speed and the extent of reaction of reaction (2) and reaction (3).
Carbonizatin method prepares boehmite can rely on sintering process to produce alumina technology, using intermediate product NaAlO2It is molten
Liquid and CO2Used as reaction raw materials, process is simple is the minimum process route of cost.Formation waste liquid in production can return to oxidation
Aluminium production procedure is recycled, and basic no waste mine discharge, environmental pollution is small, is a kind of compared with competitive superiority and the method for future.
Chinese patent literature CN1091428C discloses a kind of preparation method of boehmite：By sodium metaaluminate or aluminic acid
Sodium solution and carbonated gas are contacted, and the plastic in the way of intermittently or serially, the aging aluminium hydroxide for obtaining is isolated
Solid product, washs and dries；The endpoint pH or process pH value of the plastic are controlled in the range of 6~9.5, plastic reaction
Time or the residence time be less than 40 minutes, plastic reaction 10~100 DEG C of temperature, plastic reaction terminate after be rapidly added alkalescence
Material, makes the pH value of slurries rise to more than 9.5 or carry out separation of solid and liquid and wash rapidly.
Chinese patent literature CN103449484A discloses a kind of method of continuous production boehmite：By sodium metaaluminate
Solution is continuously added in reaction unit, while being passed through the mixed gas of air and carbon dioxide, makes sodium aluminate solution shape
It is sufficiently mixed with carbon dioxide into powerful liquid stream；The flow of control mixed gas and sodium aluminate solution, makes anti-
The slurry temperature that should be generated is 25~55 DEG C, and pH value is 9.5~11；Slurry is carried out always after with the curved pipeline of multiple u-shapeds
Change, filter, wash and dried process, obtain boehmite.
The above method is used to being passed directly into CO in reaction unit2Decomposition plastic is carried out, thus is had the disadvantage that：Technique
Equipment falls behind, and automatization level is low, and efficiency is low；Conventional decomposition groove is to CO2Absorptivity is low, and production capacity is small；Reaction time
Long, product quality fluctuation is big；Production equipment easily scabs, and the cycle of operation is short；Continuous prodution relatively difficult to achieve.
Therefore, in the urgent need to a kind of preparation method of boehmite, its product quality stabilization, it is possible to achieve continuous metaplasia
Produce.
The content of the invention
It is an object of the invention to provide a kind of preparation method of boehmite, its plan that can produce steady quality
Boehmite.Further aim of the present invention is to provide a kind of preparation method of boehmite, and it can realize serialization
Production.
Present inventor is studied with keen determination, it is found that following technical scheme can realize above-mentioned purpose.
A kind of preparation method of boehmite, described preparation method includes plastic step：By meta-aluminate solution with
Carbon dioxide is contacted to form product in inorganic film reactor；The pressure of described carbon dioxide >=
0.1MPa。
According to preparation method of the present invention, it is preferable that described inorganic film reactor includes housing and inoranic membrane group
Part, described inorganic membrane assembly is arranged on enclosure interior；Described inorganic membrane assembly includes inoranic membrane；The shape of described inoranic membrane
Shape is tubulose, hollow fiber, web-like or helical form；Described inoranic membrane includes matrix and the functional layer being carried on matrix,
The material of described functional layer includes metal, alloy, glass or ceramics, and the material of described matrix includes cellular glass, burns
Knot metal or ceramics.
According to preparation method of the present invention, it is preferable that the reaction temperature of described plastic step is 20~100 DEG C,
The pH value of product is 9~10.5.
According to preparation method of the present invention, it is preferable that in described plastic step, meta-aluminate solution it is average
Flow is 150~200 ml/mins, and the average discharge of carbon dioxide is 10~30 liters/min.
According to preparation method of the present invention, it is preferable that described meta-aluminate is soluble alkali metal meta-aluminic acid
Salt；It it is 20~50 g/l with the meta-aluminate concentration that aluminum oxide is counted in meta-aluminate solution.
According to preparation method of the present invention, it is preferable that described preparation method also includes：
Aging Step：Described product heat ageing is obtained into ageing products；
Separating, washing step：The ageing products are carried out into separation of solid and liquid to obtain solid matter, then using water to institute
The solid matter stated wash obtaining washed product；With
Drying steps：The washed product is dried to obtain boehmite.
According to preparation method of the present invention, it is preferable that in described Aging Step, aging temperature is 40~70
DEG C, ageing time is 50~200 minutes.
According to preparation method of the present invention, it is preferable that in described separating, washing step, wash temperature be 20~
100 DEG C, washing times are 5~15 times；The pH value of final washes is 6.8~7.
According to preparation method of the present invention, it is preferable that in described drying steps, drying temperature is 105~130
DEG C, drying time is 1~24 hour.
According to preparation method of the present invention, it is preferable that the pore volume of described boehmite be 0.3~0.5 milliliter/
Gram, specific surface area is 260~500m2/g。
The present invention is reacted meta-aluminate solution and carbon dioxide in inorganic film reactor, anti-in inoranic membrane
Gas concentration lwevel can be effectively controlled in answering device, so as to promote the neutralization reaction of meta-aluminate and carbon dioxide and press down
Meta-aluminate spontaneous hydrolysis reaction processed, so as to obtain the boehmite of steady quality.The present invention is reacted at ambient pressure, can
To ensure that plastic reaction safety is carried out, be conducive to industrial applications.It is inorganic using tubular type according to currently preferred technical scheme
Membrane reactor, hollow fiber form inorganic film reactor can realize continuous prodution.
Brief description of the drawings
Fig. 1 is of the invention into adhesive dispenser.
Fig. 2 is the XRD of boehmite prepared by the embodiment of the present invention 1.
Description of reference numerals is as follows：
1- meta-aluminate feed units；2- carbon dioxide feed units；3- inorganic film reactors；The storage of 4- product is single
Unit；5- measures supply unit；6- flow controlling units.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to
This.
" boehmite " chemical formula of the invention is (A12O3·xH2O, 2>x>1), also referred to as " false boehmite ",
With boehmite ((A1 in its structure2O3·H2O) it is similar to, but its crystallinity is very low, and close to gelinite, its crystallization water is high
In boehmite (referring to " chemical encyclopedia, Beijing：Chemical Industry Press, 1998, volume 10, page 938 ").
" 1atm " of the invention is a standard atmospheric pressure, due to the difference of height above sea level, is fluctuated in 1atm and 10% belonged to
In the scope of the present invention." 1atm " of the invention is intended to indicate that normal pressure, i.e., gas pressure is not controlled especially.
" wt% " of the invention represents percetage by weight.
The preparation method of boehmite of the invention includes plastic step.Optionally, boehmite of the invention
Preparation method can also include Aging Step, separating, washing step and drying steps.
<Plastic step>
Plastic step of the invention is that meta-aluminate solution and carbon dioxide are connect in inorganic film reactor
Touch to form product.
In the present invention, described inorganic film reactor can be inorganic selected from tubular type inorganic film reactor or hollow fiber form
Membrane reactor.Tubular type described here, hollow fiber form each mean the shape of inoranic membrane.Preferably, inoranic membrane of the invention
Reactor is tubular type inorganic film reactor or hollow fiber form inorganic film reactor.
In the present invention, described inorganic film reactor includes housing and inorganic membrane assembly, and described inorganic membrane assembly sets
Put in enclosure interior.In the present invention, the housing is tightly connected with inorganic membrane assembly, can be using the conventional method in this area
Sealed, repeated no more here.The structure of inorganic film reactor of the invention can be known in the art those, here not
Repeat again.
Inorganic membrane assembly of the invention includes inoranic membrane.Inoranic membrane of the invention include metal film, alloy film, ceramic membrane or
Glass-film；Preferably ceramic membrane or glass-film；More preferably ceramic membrane.The shape of inoranic membrane of the invention can for tubulose, in
Hollow fiber shape, web-like or helical form.Inoranic membrane of the invention can be the ceramic membrane of tubulose or hollow fiber, tubulose or hollow
Fibrous glass-film, web-like or spiral helicine metal film, or be web-like or spiral helicine alloy film.Preferably, this hair
Bright inoranic membrane can be the ceramic membrane of tubulose or hollow fiber.Generally, it is considered that tubulose, hollow fiber, web-like or spiral
The inoranic membrane of shape is not suitable for the continuous production of boehmite；Inoranic membrane that is of the invention then finding above-mentioned shape, especially
The ceramic membrane of tubulose or hollow fiber, can be used for the continuous production of boehmite.
Inoranic membrane of the invention includes matrix and the functional layer being carried on matrix, and the material of described functional layer includes gold
Category, alloy, glass or ceramics, the material of described matrix include cellular glass, sintering metal or ceramics.Function of the invention
Layer is preferably glass material or ceramic material, more preferably ceramic material；Matrix of the invention is preferably glass material or ceramics
Material, more preferably ceramic material.Metal membrane material of the invention can be 304,304L, 316,316L, Ni-Cu alloy, Kazakhstan
Family name's alloy, nickel alloy, titanium etc..The instantiation of metal film of the invention includes but is not limited to Nanjing University of Technology laboratory
The product of production.Metal film membrane aperture of the invention can be 0.1~200 μm, preferably 1~100 μm.Ceramic membrane of the invention
Material can be α-Al2O3, ZrO2Or TiO2, preferably α-Al2O3.Ceramic membrane membrane aperture of the invention is 0.004~3 μm, excellent
Elect 0.01~2 μm, more preferably 0.1~0.5 μm as.The instantiation of ceramic membrane of the invention includes but is not limited to Nanjing Ai Yu
The product of Qi Mo Science and Technology Ltd.s production.
In the present invention, the reaction temperature of described plastic step can be 20~100 DEG C, preferably 20~70 DEG C, more
Preferably 25~50 DEG C.In the present invention, the pH value of the product of described plastic step can be 9~10.5, preferably
9.2~10.2, more preferably 9.5~10.
In the present invention, the pH value of described meta-aluminate solution is 10~14, preferably 12~14.Inclined aluminium of the invention
Acid salt solution includes meta-aluminate, water and pH adjusting agent.Meta-aluminate of the invention can be soluble alkali metal meta-aluminic acid
Salt, such as sodium metaaluminate or potassium metaaluminate etc., preferably sodium metaaluminate.PH adjusting agent of the invention can be NaOH, hydrogen
Potassium oxide or ammoniacal liquor etc., preferably NaOH.In meta-aluminate solution of the invention, the meta-aluminate in terms of aluminum oxide is dense
It is 20~50 g/l to spend, preferably 30~40 g/l, more preferably 33~35 g/l.In the present invention, in described plastic
The average discharge of the meta-aluminate solution in step be 150~200 ml/mins, preferably 160~180 ml/mins, more
Preferably 165~175 ml/mins.
In the present invention, the average discharge of the carbon dioxide in described plastic step can for 10~30 liters/
Minute, preferably 15~25 liters/min, more preferably 20~23 liters/min.Carbon dioxide gas in described plastic step
Pressure >=the 0.1MPa of body, can be 1~1.3atm, preferably normal pressure.
<Aging Step>
Aging Step of the invention is that above-mentioned product heat ageing is obtained into ageing products.In the present invention, it is aging
Temperature can be 40~70 DEG C, more preferably preferably 45~65 DEG C, 50~60 DEG C；Ageing time can be 50~200 minutes,
Preferably 55~180 minutes, more preferably 60~90 minutes.
<Separating, washing step>
Separating, washing step of the invention is that the ageing products are carried out into separation of solid and liquid to obtain solid matter, is then adopted
Described solid matter wash with water to obtain washed product.In the present invention, the method for separation of solid and liquid can include
Filter, centrifugation etc., preferably filter.The operating condition of separation of solid and liquid of the invention can using it is known in the art those, here
Repeat no more.In the present invention, wash temperature can be 20~100 DEG C, more preferably preferably 25~80 DEG C, 30~50 DEG C；
Washing times can be 5~15 times, preferably 8~10 times.In the present invention, the total amount of slurry is 10~30 liters, preferably
It is 13~20 liters；Each water consumption can be the same or different, preferably identical water consumption.In the present invention, it is final
The pH value of washes is 6.8~7, preferably 7.
<Drying steps>
Drying steps of the invention are that the washed product is dried to obtain into boehmite.In the present invention, temperature is dried
Degree can be 105~130 DEG C, more preferably preferably 108~120 DEG C, 110~118 DEG C；Drying time can be 1~24 small
When, preferably 2~15 hours, more preferably 3~10 hours.
<Boehmite>
The pore volume V of boehmite of the invention is 0.3~0.5 ml/g, preferably 0.35~0.45 ml/g；Than
Surface area S is 260~500m2/ g, preferably 280~450m2/g。
Boehmite of the invention can be used for producing activated alumina, and then as drier, adsorbent, catalyst
And catalyst carrier.
<Method of testing>
Specific surface area, pore volume using nitrogen absorption under low temperature BET method determine (- 196 DEG C, Kang Ta instrument companies of the U.S.
NOVA4000e types specific surface and lacunarity analysis instrument).
(CuK α, λ=0.154nm, sweep the X'pert-MPD types X-ray diffractometer of the Dutch PHILIPS Co. of XRD spectrum use
Retouch 5-80 ° of scope, 4 °/min of sweep speed) determine.
The ceramic membrane used in following examples is：Ceramic membrane materials α-Al2O3, membrane aperture is 0.3 μm, Nanjing Ai Yu fine jades
Film Science and Technology Ltd. product.
Embodiment
Below with reference to accompanying drawing, the present invention will be described in more detail.Fig. 1 includes inclined aluminium for of the invention into adhesive dispenser
Hydrochlorate feed unit 1, carbon dioxide feed unit 2, inorganic film reactor 3, product memory cell 4 measure supply unit 5
With flow controlling unit 6.Meta-aluminate feed unit 1 (liquid phase feed unit) is by metering supply unit 5 and inorganic film reaction
Device 3 is connected, for quantitatively supplying meta-aluminate solution to inorganic film reactor 3；Carbon dioxide feed unit 2 passes through flow control
Unit processed 6 is connected with inorganic film reactor 3, for quantitatively supplying carbon dioxide to inorganic film reactor 3.Product is stored
Unit 4 is connected by pipeline with inorganic film reactor 3, for accommodating product.
In meta-aluminate feed unit 1, by sodium metaaluminate stoste (alumina content：200 g/l) it is diluted with water to be formed
Sodium aluminate solution.The sodium aluminate solution (liquid phase) of meta-aluminate feed unit 1 is delivered to through metering supply unit 5 inorganic
Membrane reactor 3.Carbon dioxide in carbon dioxide feed unit 2 is delivered to inorganic film reaction through flow controlling unit 6
Device 3.In inorganic film reactor 3, carbon dioxide (gas phase) diffuses to meta-aluminic acid through inorganic membrane assembly (ceramic film component)
Sodium solution, the two is contacted and plastic of decomposing reacts to form product, wherein comprising aluminium hydroxide.The product is defeated
Deliver to product memory cell 4.Boehmite is obtained through aging, filtering and washing, dry (device is not shown).
, referring to table 1, the performance parameter of gained boehmite is referring to table 2 for other process conditions of embodiment 1~5.Implement
The XRD of boehmite prepared by example 1 is referring to Fig. 2.
Table 1
Table 2
| Performance parameter | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Pore volume V (ml/g) | 0.35 | 0.40 | 0.41 | 0.42 | 0.45 |
| Specific surface area (m2/g) | 440.50.33 | 387.80 | 347.56 | 303.33 | 280.87 |
The performance parameter variations very little of the gained boehmite of embodiment 1~5, this shows that the method for the present invention can be obtained
The boehmite product of steady quality.
Additionally, embodiment 1~5 is repeated 5 times respectively, the performance parameter variations scope of gained boehmite is less than 3%,
This shows that the method for the present invention is reproducible.
The present invention is not limited to above-mentioned implementation method, in the case of without departing substantially from substance of the invention, this area skill
Any deformation that art personnel are contemplated that, improvement, replacement each fall within the scope of the present invention.
Claims (8)
1. a kind of preparation method of boehmite, it is characterised in that described preparation method includes plastic step：By meta-aluminic acid
Salting liquid is contacted to form product with carbon dioxide in inorganic film reactor；Described carbon dioxide
Pressure be 1~1.3atm；
Wherein, described inorganic film reactor is tubular type inorganic film reactor；Described inorganic film reactor includes housing and nothing
Machine membrane module, described inorganic membrane assembly is arranged on enclosure interior；Described inorganic membrane assembly includes inoranic membrane；Described is inorganic
Film is the ceramic membrane of tubulose；
In described plastic step, the average discharge of meta-aluminate solution is 150~200 ml/mins；Carbon dioxide
Average discharge be 10~30 liters/min.
2. preparation method according to claim 1, it is characterised in that：The reaction temperature of described plastic step be 20~
100 DEG C, the pH value of product is 9~10.5.
3. preparation method according to claim 1, it is characterised in that：Described meta-aluminate is that soluble alkali metal is inclined
Aluminate；It it is 20~50 g/l with the meta-aluminate concentration that aluminum oxide is counted in meta-aluminate solution.
4. preparation method according to claim 1, it is characterised in that described preparation method also includes：
Aging Step：Described product heat ageing is obtained into ageing products；
Separating, washing step：The ageing products are carried out into separation of solid and liquid to obtain solid matter, then using water to described
Solid matter wash obtaining washed product；With
Drying steps：The washed product is dried to obtain boehmite.
5. preparation method according to claim 4, it is characterised in that：In described Aging Step, aging temperature is 40
~70 DEG C, ageing time is 50~200 minutes.
6. preparation method according to claim 4, it is characterised in that：In described separating, washing step, wash temperature
It it is 20~100 DEG C, washing times are 5~15 times；The pH value of final washes is 6.8~7.
7. preparation method according to claim 6, it is characterised in that：In described drying steps, drying temperature is 105
~130 DEG C, drying time is 1~24 hour.
8. preparation method according to claim 4, it is characterised in that：The pore volume of described boehmite is 0.3~0.5
Ml/g, specific surface area is 260~500m2/g。
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