CN105174293B - A kind of preparation method for the boehmite that pore-size distribution is concentrated - Google Patents
A kind of preparation method for the boehmite that pore-size distribution is concentrated Download PDFInfo
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- CN105174293B CN105174293B CN201510574331.0A CN201510574331A CN105174293B CN 105174293 B CN105174293 B CN 105174293B CN 201510574331 A CN201510574331 A CN 201510574331A CN 105174293 B CN105174293 B CN 105174293B
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Abstract
The present invention provides a kind of preparation method for the boehmite that pore-size distribution is concentrated, and its step includes：Neutralization plastic will be carried out under aluminum source compound normal pressure, gained slurry adds reactor and carries out 0.5~24h of hydro-thermal process in 100~200 DEG C；After reaction terminates, gained slurries are subjected to separation of solid and liquid, washing, obtain the product cake of imurity-removal；Dry, crush, obtain the boehmite powder of pore-size distribution concentration.This method preparation process is simple, and cost is cheap, is adapted to industrialized production；Control hydrothermal reaction condition can be prepared by the high-performance boehmite product that serial pore-size distribution is concentrated, and is suitable for use as polytype catalyst carrier, is with a wide range of applications.
Description
Technical field
The invention belongs to field of inorganic material preparing technology, is related to a kind of preparation method of boehmite, more particularly to a kind of
By the method for the boehmite for preparing pore-size distribution concentration in aluminum source compound with the laggard water-filling thermal response of plastic.
Background of invention
Alumina support is widely used in various chemical fields, particularly for the hydrogenation catalyst in petroleum refining process
Agent, hydrotreating application spans plurality of raw materials type and operating condition, but with one or more common targets, that is, removes
Heteroatom contaminants (sulphur, nitrogen, oxygen, metal), the H/C ratios in product are improved, so as to reduce aromatic compound, density and/or carbon
Residue, carbon key is cracked to reduce boiling range and mean molecule quantity.With petroleum resources increasingly in poor quality and heaviness, deposited in feedstock oil
In a large amount of organo-metallic compounds and asphalitine, it is desirable to which various petroleum refinement catalyst carriers have sufficiently large hole to be expanded
Dissipate, prevent or slow down poisoning or the inactivation of catalyst, while catalyst carrier will also keep big ratio surface, make active component more
Good is scattered so that it is guaranteed that catalyst has high catalytic activity.With increasingly becoming more meticulous for PETROLEUM PROCESSING, there is Large ratio surface
Alumina support with pore volume is not the requirement that can meet different fractions oil processing, therefore proposes the concept in effective hole.
For specific distillate, the hole with specific pore size distribution is considered as effective hole, can not be passed through for the too small reactant in aperture
Or the too big reactant in aperture is not enough to rest on the hole to react in hole and is referred to as invalid hole, this requires alumina support to exist
Simultaneously will also be with narrow pore size distribution with large surface and pore volume.
The primary raw material for producing alumina support is boehmite (A1OOHnH2O, n=0.08~0.62), also referred to as
False boehmite, it is that a kind of composition does not know, crystallizes a kind of aluminium hydroxide that is imperfect, having thin fold lamella, has
, pore volume big the features such as higher than surface.The performance of alumina support is mainly determined by the performance of boehmite, particularly intends thin water
The pore structure of aluminium stone determines the pore structure of alumina support substantially, therefore, to prepare high performance alumina support, first have to
High performance boehmite split is made.The preparation method of industrial boehmite mainly has：Neutralisation, kind point-score, alcohol
Aluminium method.Wherein neutralisation is current domestic widely used production method, can specifically be subdivided into aluminum nitrate method, aluminum sulfate method, carbon
Change method, double aluminium methods, pH value swing method etc..The major defect of the existing method for preparing boehmite is produced using single method
Product, aperture control scope is small, pore size distribution disperse, causes a set of technique productions kind of aluminum oxide producer very limited, can not
Adapt to the requirement of different catalysts.
CN 101704538B disclose a kind of hydrothermal method for preparing series of special-shaped graded pseudo-boehmite, by aluminium salt, urine
Element, sulfate carry out hydro-thermal process jointly, prepare the production of the various shapes such as spindle, ellipsoid, three-dimensional flower-shaped, tiny balloon
Product, but product is smaller than surface made from the method, is distributed in 50~105m more2Between/g, such carrier, which is used to prepare, to be catalyzed
Agent, it is unfavorable for the high degree of dispersion of active component.
It is basic that CN 1045461C, which disclose one kind using aluminum salt solution or acid solution and aqueous slkali or composite alkali aluminum salting liquid,
Raw material, two kinds of solution are alternately added reactor, make the method for pH value alternatively swinging between acid and alkali that aluminium glue be made, are made and compare table
250~350m of face2/ g, 0.55~0.75ml/g of pore volume, 4~10nm of aperture collection mesopore account for the γ of cumulative volume 75~90%-
Al2O3Method.Between 5~7nm, aperture can not regulate and control carrier aperture made from the method.
CN 101357771B disclose it is a kind of can be in higher aluminium salt concentration range and relatively mild hydro-thermal reaction bar
The scale preparation method of high-ratio surface pseudo boehmite microsphere is realized under part.Product specific surface area reaches as high as made from the method
371.8m2/g, but pore volume is relatively low, maximum 0.44ml/g, while aperture can not equally obtain big in the range of 3.4~8.9nm
Aperture boehmite.
CN 103787388A disclose a kind of boehmite dry glue powder and aqueous solution of urea hydro-thermal process, further into
The method for concentrating pore size distribution and alumina supporter with high specific surface area is made in type, drying, roasting, and the method, which is made, has 10~20nm holes
Pore volume account for the alumina support of total pore volume 80% or so.
The content of the invention
In view of the shortcomings of the prior art, the boehmite concentrated it is an object of the invention to provide a kind of pore-size distribution
Preparation method.The present invention is by simply controlling hydrothermal conditions that a series of boehmite powder that pore-size distributions are concentrated is made
Body.This method preparation technology is simple, and cost is cheap, easily carries out industrialized production.
The present invention is neutralized the-hydro-thermal process method for preparing boehmite by aluminum source compound to be a kind of, it is characterised in that：
Comprise the following steps：
(1) aluminum source compound is subjected to neutralization plastic in atmospheric conditions；Wherein neutral temperature is 30~90 DEG C, and addition
Neutralization pH value is in 7~8 or anti-additions and endpoint pH is 7~8；
(2) slurry obtained by step (1) is added into reactor and carries out 0.5~24h of hydro-thermal process in 100~200 DEG C；
(3) after reaction terminates, slurries obtained by step (2) is subjected to separation of solid and liquid, washing, obtain the product filter of imurity-removal
Cake；
(4) dry, crush, obtain boehmite powder；
In aluminum source compound described in the method according to the invention, wherein step (1) and plastic includes acid silicon source and alkali
Property material in and plastic, either in alkaline silicon source and acidic materials and plastic or acid silicon source with alkaline silicon source and plastic.
The method according to the invention, wherein, the acid silicon source described in step (1) includes aluminum sulfate, aluminum nitrate, alum
Or aluminium chloride；Alkaline silicon source includes sodium metaaluminate or potassium metaaluminate；Alkaline matter includes sodium hydroxide, sodium carbonate, potassium hydroxide
Or ammoniacal liquor；Acidic materials include sulfuric acid, hydrochloric acid or nitric acid.
The method according to the invention, wherein, boehmite powder obtained by step (4) is most probable pore size in 6~20nm；
Wherein, most probable pore size is 6~12nm boehmite powder, and 80% hole integrated distribution is in most probable pore size ± 2nm scopes
It is interior；Most probable pore size is 12~20nm boehmite powder, and 80% hole integrated distribution is in most probable pore size ± 3nm scopes
It is interior.Described boehmite powder surface area per unit volume is 260~320m2/ g, pore volume are 0.7~1.2ml/g, most probable pore size ±
3nm endoporus accounts for total pore volume 80~90%.
Present invention also offers a kind of boehmite powder, the most probable pore size of the boehmite powder 6~
20nm；Wherein, most probable pore size is 6~12nm boehmite powder, and 80% hole integrated distribution is in most probable pore size ± 2nm
In the range of；Most probable pore size is 12~20nm boehmite powder, and 80% hole integrated distribution is in most probable pore size ± 3nm models
In enclosing.
The present invention uses neutralization-hydro-thermal method, and emphasis neutralizes the condition and hydrothermal condition of plastic by adjusting, and controls product
The growth of grain, the crystal formation change such as perfect, and then the size, crystalline phase, pattern of crystal grain are controlled, so as to form the plan of pore-size distribution concentration
Boehmite.Boehmite prepared by the present invention has narrow pore-size distribution so that has using it as catalyst prepared by carrier
There is high effective hole, the selectivity of catalyst can be effectively improved.
Embodiment：
Embodiment 1
Bottom water 5L is added in 20L stirred tanks, after being heated to 70~75 DEG C, cocurrent adds aluminum sulfate under conditions of quick stirring
Solution (concentration is calculated as 95g/L with aluminum oxide) and sodium aluminate solution (concentration is calculated as 300g/L with aluminum oxide), control system pH
It is worth for 7.0~7.5, stops charging after adding 8.0kg aluminum sulfate solutions and 5.2kg sodium aluminate solutions altogether, by gained slurry
Be transferred to after adding 20L autoclaves, in 200 DEG C of hydro-thermal process 1h, processing terminate after by gained slurries separation of solid and liquid, go from
Sub- water washing, the product cake of imurity-removal is obtained, dry, pulverize to obtain boehmite powder in 120 DEG C, its physico-chemical property
It is shown in Table 1.
Embodiment 2
Bottom water 5L is added in 20L stirred tanks, after being heated to 80~85 DEG C, cocurrent adds aluminum sulfate under conditions of quick stirring
Solution (concentration is calculated as 95g/L with aluminum oxide) and sodium aluminate solution (concentration is calculated as 300g/L with aluminum oxide), control system pH
It is worth for 7.0~7.5, stops charging after adding 8.0kg aluminum sulfate solutions and 5.0kg sodium aluminate solutions altogether, by gained slurry
Be transferred to after adding 20L autoclaves, in 200 DEG C of hydro-thermal process 4h, processing terminate after by gained slurries separation of solid and liquid, go from
Sub- water washing, the product cake of imurity-removal is obtained, dry, pulverize to obtain boehmite powder in 120 DEG C, its physico-chemical property
It is shown in Table 1.
Embodiment 3
Bottom water 5L is added in 20L stirred tanks, after being heated to 70~75 DEG C, cocurrent adds aluminum sulfate under conditions of quick stirring
Solution (concentration is calculated as 95g/L with aluminum oxide) and sodium aluminate solution (concentration is calculated as 300g/L with aluminum oxide), control system pH
It is worth for 7.5~8.0, stops charging after adding 8.0kg aluminum sulfate solutions and 5.3kg sodium aluminate solutions altogether, by gained slurry
Be transferred to after adding 20L autoclaves, in 200 DEG C of hydro-thermal process 12h, processing terminate after by gained slurries separation of solid and liquid, go
Ion water washing, the product cake of imurity-removal is obtained, dry, pulverize to obtain boehmite powder in 120 DEG C, its materialization
Matter is shown in Table 1.
Embodiment 4
Bottom water 8L is added in 20L stirred tanks, after being heated to 40~45 DEG C, adding 8kg sodium aluminate solutions, (concentration is to aoxidize
Aluminium is calculated as 300g/L), it is subsequently passed CO2Gas, it is 7.5 to control endpoint pH, and it is anti-that gained slurry is transferred into addition 20L high pressures
After answering kettle, in 100 DEG C of hydro-thermal process 24h, gained slurries separation of solid and liquid, deionized water are washed, removed after terminating by processing
The product cake of impurity, it dry, pulverize to obtain boehmite powder in 120 DEG C, its physico-chemical property is shown in Table 1.
Embodiment 5
Bottom water 5L is added in 20L stirred tanks, after being heated to 80~85 DEG C, adding 8.0kg aluminum sulfate solutions, (concentration is to aoxidize
Aluminium is calculated as 95g/L), ammoniacal liquor is then slowly added to, it is 7.5 to control endpoint pH, and it is anti-that gained slurry is transferred into addition 20L high pressures
After answering kettle, in 180 DEG C of hydro-thermal process 8h, processing terminate after by gained slurries separation of solid and liquid, deionized water washing, obtain removing miscellaneous
The product cake of matter, it dry, pulverize to obtain boehmite powder in 120 DEG C, its physico-chemical property is shown in Table 1.
Embodiment 6
Bottom water 5L is added in 20L stirred tanks, after being heated to 80~85 DEG C, adding 8.0kg aluminum sulfate solutions, (concentration is to aoxidize
Aluminium is calculated as 95g/L), ammoniacal liquor is then slowly added to, it is 7.5 to control endpoint pH, and it is anti-that gained slurry is transferred into addition 20L high pressures
After answering kettle, in 150 DEG C of hydro-thermal process 1h, processing terminate after by gained slurries separation of solid and liquid, deionized water washing, obtain removing miscellaneous
The product cake of matter, it dry, pulverize to obtain boehmite powder in 120 DEG C, its physico-chemical property is shown in Table 1.
Comparative example 1
Bottom water 5L is added in 20L stirred tanks, after being heated to 70~75 DEG C, cocurrent adds aluminum sulfate under conditions of quick stirring
Solution (concentration is calculated as 95g/L with aluminum oxide) and sodium aluminate solution (concentration is calculated as 300g/L with aluminum oxide), control system pH
It is worth for 7.0~7.5, stops charging after adding 8.0kg aluminum sulfate solutions and 5.2kg sodium aluminate solutions altogether, then raise temperature to
85~90 DEG C of burin-in process 2h, aging wash gained slurries separation of solid and liquid, deionized water after terminating, and obtain the production of imurity-removal
Thing filter cake, it dry, pulverize to obtain boehmite powder in 120 DEG C, its physico-chemical property is shown in Table 1.
Comparative example 2
Bottom water 8L is added in 20L stirred tanks, after being heated to 40~45 DEG C, adding 8kg sodium aluminate solutions, (concentration is to aoxidize
Aluminium is calculated as 300g/L), it is subsequently passed CO2Gas, it is 7.5 to control endpoint pH, then raises temperature to 85~90 DEG C of burin-in process 2h,
Aging terminate after by gained slurries separation of solid and liquid, deionized water washing, obtain the product cake of imurity-removal, in 120 DEG C of dryings,
Crushing obtains boehmite powder, and its physico-chemical property is shown in Table 1.
Comparative example 3
Bottom water 5L is added in 20L stirred tanks, after being heated to 80~85 DEG C, adding 8.0kg aluminum sulfate solutions, (concentration is to aoxidize
Aluminium is calculated as 95g/L), ammoniacal liquor is then slowly added to, it is 7.5 to control endpoint pH, then raises temperature to 85~90 DEG C of burin-in process 2h,
By gained slurries separation of solid and liquid after end, deionized water washing, the product cake of imurity-removal is obtained, dry, pulverize in 120 DEG C
Boehmite powder is obtained, its physico-chemical property is shown in Table 1.
1 each embodiment of table and the physico-chemical property of comparative example product
Claims (4)
1. a kind of method that neutralization-hydro-thermal method prepares boehmite, it is characterised in that：
Comprise the following steps：
1) aluminum source compound is subjected to neutralization plastic in atmospheric conditions, it is 30 ~ 90 DEG C to control neutral temperature, and in addition and pH
Be worth in 7 ~ 7.5 or anti-additions and endpoint pH be 7 ~ 7.5；
2) by step 1）Gained slurry adds reactor and carries out 0.5 ~ 24h of hydro-thermal process in 150~200 DEG C；
3) after reaction terminates, by step 2）Gained slurries carry out separation of solid and liquid, washing, obtain the product cake of imurity-removal；
4) dry, crush, obtain boehmite powder；
Step 1）In described aluminum source compound and plastic includes in acid silicon source and alkaline matter and plastic, or alkaline silicon source
With in acidic materials and plastic, or acid silicon source with alkaline silicon source and plastic；
Acid silicon source includes aluminum sulfate, aluminum nitrate, alum or aluminium chloride；Alkaline silicon source includes sodium metaaluminate or meta-aluminic acid
Potassium；
Step 4）Gained boehmite powder is most probable pore size in 6~20nm；Wherein, most probable pore size is 6 ~ 12nm plan
Boehmite powder, 80% hole integrated distribution is in the range of most probable pore size ± 2nm；Most probable pore size is the 12 ~ 20nm thin water of plan
Aluminium stone flour body, 80% hole integrated distribution is in the range of most probable pore size ± 3nm.
2. according to the method for claim 1, it is characterised in that alkaline matter includes sodium hydroxide, sodium carbonate, potassium hydroxide
Or ammoniacal liquor；Acidic materials include sulfuric acid, hydrochloric acid or nitric acid.
3. according to the method for claim 1, it is characterised in that described boehmite powder surface area per unit volume be 260 ~
320m2/ g, pore volume are 0.7 ~ 1.2ml/g, and most probable pore size ± 3nm endoporus accounts for total pore volume 80 ~ 90%.
A kind of 4. boehmite powder made from claim 1 methods described, it is characterised in that the boehmite powder
Most probable pore size in 6~20nm；Wherein, most probable pore size is 6 ~ 12nm boehmite powder, and 80% hole integrated distribution exists
In the range of most probable pore size ± 2nm；Most probable pore size is 12 ~ 20nm boehmite powder, and 80% hole integrated distribution most may be used
In the range of a few aperture ± 3nm.
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| CN105645446B (en) * | 2016-03-24 | 2017-07-28 | 中国铝业股份有限公司 | Carbonation method prepares the aging method of boehmite |
| CN110015673A (en) * | 2018-01-10 | 2019-07-16 | 北京化工大学 | Boehmite and preparation method thereof |
| CN110240187B (en) * | 2018-08-24 | 2021-09-03 | 广州凌玮科技股份有限公司 | Preparation method of easily-dispersible nano boehmite for ink-jet printing adsorption medium |
| CN112452316A (en) * | 2020-11-02 | 2021-03-09 | 青岛惠城环保科技股份有限公司 | Preparation method of easily peptized pseudo-boehmite |
| CN112479240A (en) * | 2020-11-30 | 2021-03-12 | 上海簇睿低碳能源技术有限公司 | Preparation method of high-viscosity pseudo-boehmite |
| CN115124056B (en) * | 2022-06-29 | 2024-01-23 | 中国铝业股份有限公司 | Pseudo-boehmite and preparation method and application thereof |
| WO2024046421A1 (en) * | 2022-08-31 | 2024-03-07 | 中国石油化工股份有限公司 | Mesoporous pseudo-boehmite having hydroxyl-rich surface, catalytic cracking catalyst containing pseudo-boehmite, and preparation and use thereof |
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| CN103172097A (en) * | 2013-04-11 | 2013-06-26 | 北京化工大学 | Pseudo-boehmite with large specific surface area and preparation method and application thereof |
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| CN1285509C (en) * | 2003-12-10 | 2006-11-22 | 山东师范大学 | Method for preparing unidimensional Al00H and gamma-Al2O3 nano materials |
| CN1868885B (en) * | 2006-05-12 | 2010-07-21 | 广西民族大学 | Self-dispersion type nanometer gamma A100H and its preparation method and use |
| CN101318677A (en) * | 2008-07-10 | 2008-12-10 | 上海交通大学 | Method for preparing aluminum oxide nano-stick |
| JP5530672B2 (en) * | 2008-08-18 | 2014-06-25 | 株式会社フジミインコーポレーテッド | Method for producing boehmite particles and method for producing alumina particles |
| CN101503206A (en) * | 2009-03-19 | 2009-08-12 | 上海交通大学 | Preparation of one-dimensional nano gamma-AlOOH |
| CN102807240A (en) * | 2012-07-27 | 2012-12-05 | 上海度朔磨料磨具有限公司 | Method for preparing pseudo-boehmite and method for preparing microcrystalline fused alumina abrasive |
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