CN104692429B - A kind of controllable method for preparing of bigger serface macropore volume boehmite - Google Patents
A kind of controllable method for preparing of bigger serface macropore volume boehmite Download PDFInfo
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- CN104692429B CN104692429B CN201510083641.2A CN201510083641A CN104692429B CN 104692429 B CN104692429 B CN 104692429B CN 201510083641 A CN201510083641 A CN 201510083641A CN 104692429 B CN104692429 B CN 104692429B
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- boehmite
- aluminum sulfate
- aluminum
- sulfate solution
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Abstract
The invention discloses a kind of controllable method for preparing of bigger serface macropore volume boehmite.The method, with aluminum sulfate, sodium metaaluminate as raw material, is first prepared, using titrimetry, the intermediate product aluminum hydrate forming boehmite, is then carried out hydrothermal treatment consists to the intermediate product obtaining, finally cool down, and washing is dried to obtain boehmite.With the increase of aluminum sulfate solution concentration in the method, the specific surface area of the bigger serface macropore volume boehmite obtaining is in 400 800m2It is incremented by in/g range, pore volume is in 1.4 2.4cm3It is incremented by in/g range.The method green simple it is easy to industrialization.
Description
Technical field
The invention belongs to boehmite preparing technical field, particularly to a kind of bigger serface macropore volume boehmite
Controllable method for preparing.
Background technology
Boehmite (boehmite), also referred to as boehmite, is the hydrate of aluminium oxide.Boehmite is as preparation
The important intermediate of aluminium oxide, itself can be used for being catalyzed with the advantage of bigger serface and certain heat stability
Agent and the carrier of adsorbent.
In prior art, report adopts aluminum nitrate as silicon source, and the Deca ammonia spirit in aluminum nitrate solution adjusts pH value
For 7-10, can be prepared into specific surface area is 383m2/g-475m2/ g, pore volume is 0.97-1.91cm3The boehmite of/g.This
Method production cost is higher, and environmental pollution is big.
Content of the invention
For above-mentioned deficiency of the prior art, the present invention provides a kind of thin water of bigger serface macropore volume of low cost
The preparation method of aluminum stone and the control method of boehmite specific surface area and pore volume.
The technical scheme is that：With aluminum sulfate, sodium metaaluminate as raw material, first the thin water of formation is prepared using titrimetry
The intermediate product of aluminum stone-aluminum hydrate, then carries out hydrothermal treatment consists to the intermediate product obtaining, finally cools down, washing, is dried
Obtain boehmite；The method controls specific surface area and the hole body of boehmite by the concentration controlling raw material sulphuric acid aluminum solutions
Long-pending.
The concrete steps of the controllable method for preparing of bigger serface macropore volume boehmite of the present invention include：
(1) prepare the aluminum sulfate solution of 0.1-0.7mol/L；The sodium hydroxide for 2-5 for the mol ratio and gibbsite are dissolved in
In water, at 100-120 DEG C, reaction 1-50h obtains the sodium aluminate solution that mass concentration is 5-55%；Sodium hydroxide and three water
The preferred 4-5 of mol ratio of aluminum stone；
(2) by sodium aluminate solution be added drop-wise in aluminum sulfate solution to pH value be 7-11, preferably pH be 9-10；
(3) it is simultaneously added dropwise sodium aluminate solution and aluminum sulfate solution in the suspension obtaining to step (2), Deca process is protected
Holding system pH is 7-11；Preferable ph is 9-10；
(4) suspension obtaining step (3) is transferred in autoclave, crystallization 5-50h at 70-150 DEG C；Temperature
Preferably 80-120 DEG C, the preferred 10-40h of crystallization time；
(5) after the completion of reacting, autoclave is cooled to room temperature, the white depositions obtaining are washed with deionized, in 60-
It is dried to obtain bigger serface macropore volume boehmite at 100 DEG C.
In above-mentioned preparation method, with the increase of aluminum sulfate solution concentration, the thin water of bigger serface macropore volume obtaining
The specific surface area of aluminum stone is in 400-800m2It is incremented by in/g range, pore volume is in 1.4-2.4cm3It is incremented by in/g range.
Beneficial effect：It is 400-800m that the present invention adopts hydrothermal synthesis method synthesis specific surface area2/ g, pore volume is 1.4-
2.4cm3The bigger serface macropore volume boehmite of/g, and can be by controlling the concentration of aluminum sulfate solution thin to gained
The specific surface area of diaspore and pore volume are regulated and controled.The method green simple it is easy to industrialization.
Brief description
Fig. 1 is the X-ray powder diffraction figure of the bigger serface macropore volume boehmite obtaining in embodiment 1.
Fig. 2 is the transmission electron microscope photo of the bigger serface macropore volume boehmite obtaining in embodiment 1.
Specific embodiment
Embodiment 1
Weigh 22.56g sodium hydroxide (Beijing Chemical Plant's product, analysis is pure, similarly hereinafter), gibbsite 9.78g (Shanxi Aluminium Plant
Industrial products, alumina content 65%, similarly hereinafter), the 67.66g deionized water rear 120 DEG C of reaction 5h that stir prepare Na/Al
=4.5 sodium aluminate solutions；Weigh 33.32g Patent alum (Xi Long chemical industry Co., Ltd., Factory produce, analysis pure, under
With), plus deionized water dissolving, prepared concentration is the aluminum sulfate solution of 0.1mol/L；Weigh 25g aluminum sulfate solution, in room temperature and
Under stirring condition, and it is added dropwise over sodium aluminate solution, drops to pH=10.5, carry out double dripping as bottom liquid；To in the liquid of bottom
Be simultaneously added dropwise sodium aluminate solution and aluminum sulfate solution, should during keep system pH=10.5, finally Deca 75g aluminum sulfate altogether
Solution, obtains white suspension after being added dropwise to complete.
The uniform white suspension obtaining is encapsulated in autoclave, puts into 100 DEG C of baking oven crystallization 20 hours；Institute
Obtain product to filter, after being washed with deionized, in 60 DEG C of dryings 24 hours, obtain product S1.
The product obtaining is characterized by XRD, by XRD spectra, the product being obtained is pure phase boehmite.Than
Surface area 410.6m2/ g, pore volume is 1.48cm3/g.
Embodiment 2
Accurately weigh 22.56g sodium hydroxide, gibbsite 9.78g, 67.66g deionized water stirs latter 120 DEG C instead
5h is answered to prepare Na/Al=4.5 sodium aluminate solution.Weigh 99.96g Patent alum, plus deionized water dissolving, it is obtained
Concentration is the aluminum sulfate solution of 0.3mol/L.Weigh 25g aluminum sulfate solution, under room temperature and stirring condition, and be added dropwise over partially
Sodium aluminate solution, drops to pH=9.5, carries out double dripping as bottom liquid；It is simultaneously added dropwise sodium aluminate solution and sulfur in the liquid of bottom
Sour aluminum solutions, should during keep system pH=9.5, finally Deca 75g aluminum sulfate solution altogether, obtain white after being added dropwise to complete outstanding
Supernatant liquid.
The uniform white suspension obtaining is encapsulated in autoclave, puts into 100 DEG C of baking oven crystallization 20 hours.Institute
Obtain product to filter, after being washed with deionized, in 60 DEG C of dryings 24 hours, obtain product S2.
The product obtaining is characterized by XRD, by XRD spectra, the product being obtained is pure phase boehmite.Than
Surface area 524.6m2/ g, pore volume is 1.67cm3/g.
Embodiment 3
Accurately weigh 22.56g sodium hydroxide, gibbsite 9.78g, 67.66g deionized water stirs latter 120 DEG C instead
5h is answered to prepare Na/Al=4.5 sodium aluminate solution.Weigh 166.6g Patent alum, plus deionized water dissolving, it is obtained
Concentration is the aluminum sulfate solution of 0.5mol/L.Weigh 25g aluminum sulfate solution, under room temperature and stirring condition, and be added dropwise over partially
Sodium aluminate solution, drops to pH=9.0, carries out double dripping as bottom liquid；It is simultaneously added dropwise sodium aluminate solution and sulfur in the liquid of bottom
Sour aluminum solutions, should during keep system pH=9.0, finally Deca 75g aluminum sulfate solution altogether, obtain white after being added dropwise to complete outstanding
Supernatant liquid.
The uniform white suspension obtaining is encapsulated in autoclave, puts into 100 DEG C of baking oven crystallization 20 hours.Institute
Obtain product to filter, after being washed with deionized, in 60 DEG C of dryings 24 hours, obtain product S3.
The product obtaining is characterized by XRD, by XRD spectra, the product being obtained is pure phase boehmite.Than
Surface area 674.8m2/ g, pore volume is 1.85cm3/g.
Embodiment 4
Accurately weigh 22.56g sodium hydroxide, gibbsite 9.78g, 67.66g deionized water stirs latter 120 DEG C instead
5h is answered to prepare Na/Al=4.5 sodium aluminate solution.Weigh 233.24g Patent alum, plus deionized water dissolving, system
Obtain the aluminum sulfate solution that concentration is 0.7mol/L.Weigh 25g aluminum sulfate solution, under room temperature and stirring condition, and be added dropwise over
Sodium aluminate solution, drops to pH=8.5, carries out double dripping as bottom liquid；Be simultaneously added dropwise in the liquid of bottom sodium aluminate solution and
Aluminum sulfate solution, should during keep system pH=8.6, finally Deca 75g aluminum sulfate solution altogether, obtain white after being added dropwise to complete
Suspension.
The uniform white suspension obtaining is encapsulated in autoclave, puts into 100 DEG C of baking oven crystallization 20 hours.Institute
Obtain product to filter, after being washed with deionized, in 60 DEG C of dryings 24 hours, obtain product S4.
The product obtaining is characterized by XRD, by XRD spectra, the product being obtained is pure phase boehmite.Than
Surface area 786.8m2/ g, pore volume is 2.37cm3/g.
Claims (1)
1. a kind of controllable method for preparing of bigger serface macropore volume boehmite is it is characterised in that the concrete step of the method
Rapid inclusion：
Accurately weigh 22.56g sodium hydroxide, gibbsite 9.78g, 67.66g deionized water stirs latter 120 DEG C and reacts 5h
Prepare Na/Al=4.5 sodium aluminate solution；Weigh 233.24g Patent alum, plus deionized water dissolving, it is obtained dense
Spend the aluminum sulfate solution for 0.7mol/L；Weigh 25g aluminum sulfate solution, under room temperature and stirring condition, and be added dropwise over inclined aluminum
Acid sodium solution, drops to pH=8.5, carries out double dripping as bottom liquid；It is simultaneously added dropwise sodium aluminate solution and sulphuric acid in the liquid of bottom
Aluminum solutions, should during keep system pH=8.6, finally Deca 75g aluminum sulfate solution altogether, obtain white suspension after being added dropwise to complete
Liquid；
The uniform white suspension obtaining is encapsulated in autoclave, puts into 100 DEG C of baking oven crystallization 20 hours, gained produces
Thing filters, and after being washed with deionized, in 60 DEG C of dryings 24 hours, obtains pure phase boehmite, its specific surface area is
786.8m2/ g, pore volume is 2.37cm3/g.
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| CN105883871B (en) * | 2016-04-17 | 2017-12-29 | 北京化工大学 | A kind of preparation method of boehmite |
| CN106966417B (en) * | 2017-04-01 | 2018-07-31 | 廖志龙 | A method of preparing soilless sticking high specific area boehmite |
| CN108212224B (en) * | 2017-12-06 | 2020-10-02 | 北京化工大学 | Boehmite catalyst carrier and preparation method thereof |
| CN110015673A (en) * | 2018-01-10 | 2019-07-16 | 北京化工大学 | Boehmite and preparation method thereof |
| CN110102250A (en) * | 2019-05-16 | 2019-08-09 | 安庆北化大科技园有限公司 | A kind of preparation method of modified aluminas adsorbent, adsorbent obtained and its application |
| CN112794350B (en) * | 2020-12-31 | 2022-10-04 | 烟台恒辉化工有限公司 | Preparation method of small-pore active alumina powder |
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| CN1128761C (en) * | 2000-12-05 | 2003-11-26 | 中国石油化工股份有限公司 | Process for preparing hydrated aluminium oxide |
| CN101450812A (en) * | 2007-12-07 | 2009-06-10 | 中国科学院大连化学物理研究所 | Method for preparing nano pseudo boehmite and microchannel reactor |
| CN101643228A (en) * | 2008-08-08 | 2010-02-10 | 中国科学院大连化学物理研究所 | Method for preparing alumina having mesoporous structure |
| CN102173442B (en) * | 2011-02-25 | 2013-01-16 | 中国海洋石油总公司 | Preparation method for aperture-adjustable alumina oxide |
| CN102653410A (en) * | 2011-03-03 | 2012-09-05 | 中国石油天然气股份有限公司 | Method for preparing fibriform boehmite |
| CN102910654B (en) * | 2012-11-08 | 2014-07-30 | 北京化工大学 | Preparation method of fibrous boehmite with large specific surface area and large pore area |
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