CN104692429A - Controllable preparation method of large-specific-area large-pore-volume boehmite - Google Patents

Controllable preparation method of large-specific-area large-pore-volume boehmite Download PDF

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CN104692429A
CN104692429A CN201510083641.2A CN201510083641A CN104692429A CN 104692429 A CN104692429 A CN 104692429A CN 201510083641 A CN201510083641 A CN 201510083641A CN 104692429 A CN104692429 A CN 104692429A
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boehmite
alum liquor
area
specific
aluminate solution
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CN104692429B (en
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宋家庆
孙建川
卢磊
徐向宇
吕志
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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Abstract

The invention discloses a controllable preparation method of large-specific-area large-pore-volume boehmite. The method comprises the following steps: preparing a medium product aluminum hydroxide of boehmite by using the titrimetry using aluminum sulfate and sodium metaaluminate as raw materials; performing hydro-thermal treatment on the obtained medium product; cooling; washing; and drying to obtain boehmite. According to the method, the specific area of the prepared large-specific-area large-pore-volume boehmite is gradually increased within the range of 400 to 800m<2>/g as the concentration of an aluminum sulfate solution increases, and the pore volume is gradually increased within the range of 1.4 to 2.4cm<3>/g. The method is green, simple and easy to be industrialized.

Description

A kind of controllable method for preparing of bigger serface macropore volume boehmite
Technical field
The invention belongs to boehmite preparing technical field, particularly a kind of controllable method for preparing of bigger serface macropore volume boehmite.
Background technology
Boehmite (boehmite), also referred to as boehmite, is the hydrate of aluminum oxide.Boehmite is as the important intermediate preparing aluminum oxide, and itself may be used for the carrier of catalyzer and sorbent material with the advantage of the certain thermostability of large specific surface sum.
In prior art, report adopts aluminum nitrate as aluminium source, and in aluminum nitrate solution, drip ammonia soln, adjust ph is 7-10, and can be prepared into specific surface area is 383m 2/ g-475m 2/ g, pore volume is 0.97-1.91cm 3the pseudo-boehmite of/g.This method production cost is higher, and environmental pollution is large.
Summary of the invention
For above-mentioned deficiency of the prior art, the invention provides the low preparation method of bigger serface macropore volume boehmite of a kind of cost and the control method of boehmite specific surface area and pore volume.
Technical scheme of the present invention is: with Tai-Ace S 150, sodium metaaluminate for raw material, first adopt volumetry to prepare the intermediate product-aluminium hydrate forming boehmite, then hydrothermal treatment consists is carried out to the intermediate product obtained, finally cool, washing, drying obtains boehmite; The method controls specific surface area and the pore volume of boehmite by the concentration controlling raw material sulphuric acid aluminum solutions.
The concrete steps of the controllable method for preparing of bigger serface macropore volume boehmite of the present invention comprise:
(1) alum liquor of 0.1-0.7mol/L is prepared; The sodium hydroxide and the gibbsite that by mol ratio are 2-5 are soluble in water, react 1-50h and obtain the sodium aluminate solution that mass concentration is 5-55% at 100-120 DEG C; The preferred 4-5 of mol ratio of sodium hydroxide and gibbsite;
(2) being added drop-wise to by sodium aluminate solution in alum liquor to pH value is 7-11, and preferred pH is 9-10;
(3) drip sodium aluminate solution and alum liquor in the suspension obtained to step (2), dropping process keeps system pH to be 7-11 simultaneously; Preferable ph is 9-10;
(4) suspension that step (3) obtains is transferred in autoclave, crystallization 5-50h at 70-150 DEG C; The preferred 80-120 DEG C of temperature, the preferred 10-40h of crystallization time;
(5) after having reacted, autoclave is cooled to room temperature, the white depositions deionized water wash obtained, at 60-100 DEG C, drying obtains bigger serface macropore volume boehmite.
In above-mentioned preparation method, along with the increase of alum liquor concentration, the specific surface area of the bigger serface macropore volume boehmite obtained is at 400-800m 2increase progressively within the scope of/g, pore volume is at 1.4-2.4cm 3increase progressively within the scope of/g.
Beneficial effect: the present invention adopts hydrothermal synthesis method synthesis ratio surface-area to be 400-800m 2/ g, pore volume is 1.4-2.4cm 3the bigger serface macropore volume boehmite of/g, and by the concentration controlling alum liquor, the specific surface area of gained boehmite and pore volume can be regulated and controled.This method is green simple, is easy to industrialization.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction figure of the bigger serface macropore volume boehmite obtained in embodiment 1.
Fig. 2 is the transmission electron microscope photo of the bigger serface macropore volume boehmite obtained in embodiment 1.
Embodiment
Embodiment 1
Take 22.56g sodium hydroxide (Beijing Chemical Plant's product, analytical pure, lower same), gibbsite 9.78g (Shanxi Aluminium Plant Industrial products, alumina content 65%, lower same), 67.66g deionized water and stirring evenly rear 120 DEG C of reaction 5h prepares Na/Al=4.5 sodium aluminate solution; Take 33.32g Patent alum (Xi Long chemical plant company limited produces, analytical pure, lower same), add deionized water dissolving, obtained concentration is the alum liquor of 0.1mol/L; Take 25g alum liquor, under room temperature and agitation condition, and dropwise add sodium aluminate solution, drop to pH=10.5, carry out two dripping as end liquid; In end liquid, drip sodium aluminate solution and alum liquor simultaneously, in this process, keep system pH=10.5, finally drip 75g alum liquor altogether, after being added dropwise to complete, obtain white suspension.
The uniform white suspension obtained is encapsulated in autoclave, puts into 100 DEG C of baking oven crystallization 20 hours; Products therefrom filters, and after deionized water wash, in 60 DEG C of dryings 24 hours, obtains product S 1.
Characterized by XRD by the product obtained, known by XRD spectra, the product obtained is pure phase boehmite.Specific surface area 410.6m 2/ g, pore volume is 1.48cm 3/ g.
Embodiment 2
Accurately take 22.56g sodium hydroxide, gibbsite 9.78g, 67.66g deionized water and stirring evenly rear 120 DEG C of reaction 5h prepares Na/Al=4.5 sodium aluminate solution.Take 99.96g Patent alum, add deionized water dissolving, obtained concentration is the alum liquor of 0.3mol/L.Take 25g alum liquor, under room temperature and agitation condition, and dropwise add sodium aluminate solution, drop to pH=9.5, carry out two dripping as end liquid; In end liquid, drip sodium aluminate solution and alum liquor simultaneously, in this process, keep system pH=9.5, finally drip 75g alum liquor altogether, after being added dropwise to complete, obtain white suspension.
The uniform white suspension obtained is encapsulated in autoclave, puts into 100 DEG C of baking oven crystallization 20 hours.Products therefrom filters, and after deionized water wash, in 60 DEG C of dryings 24 hours, obtains product S 2.
Characterized by XRD by the product obtained, known by XRD spectra, the product obtained is pure phase boehmite.Specific surface area 524.6m 2/ g, pore volume is 1.67cm 3/ g.
Embodiment 3
Accurately take 22.56g sodium hydroxide, gibbsite 9.78g, 67.66g deionized water and stirring evenly rear 120 DEG C of reaction 5h prepares Na/Al=4.5 sodium aluminate solution.Take 166.6g Patent alum, add deionized water dissolving, obtained concentration is the alum liquor of 0.5mol/L.Take 25g alum liquor, under room temperature and agitation condition, and dropwise add sodium aluminate solution, drop to pH=9.0, carry out two dripping as end liquid; In end liquid, drip sodium aluminate solution and alum liquor simultaneously, in this process, keep system pH=9.0, finally drip 75g alum liquor altogether, after being added dropwise to complete, obtain white suspension.
The uniform white suspension obtained is encapsulated in autoclave, puts into 100 DEG C of baking oven crystallization 20 hours.Products therefrom filters, and after deionized water wash, in 60 DEG C of dryings 24 hours, obtains product S 3.
Characterized by XRD by the product obtained, known by XRD spectra, the product obtained is pure phase boehmite.Specific surface area 674.8m 2/ g, pore volume is 1.85cm 3/ g.
Embodiment 4
Accurately take 22.56g sodium hydroxide, gibbsite 9.78g, 67.66g deionized water and stirring evenly rear 120 DEG C of reaction 5h prepares Na/Al=4.5 sodium aluminate solution.Take 233.24g Patent alum, add deionized water dissolving, obtained concentration is the alum liquor of 0.7mol/L.Take 25g alum liquor, under room temperature and agitation condition, and dropwise add sodium aluminate solution, drop to pH=8.5, carry out two dripping as end liquid; In end liquid, drip sodium aluminate solution and alum liquor simultaneously, in this process, keep system pH=8.6, finally drip 75g alum liquor altogether, after being added dropwise to complete, obtain white suspension.
The uniform white suspension obtained is encapsulated in autoclave, puts into 100 DEG C of baking oven crystallization 20 hours.Products therefrom filters, and after deionized water wash, in 60 DEG C of dryings 24 hours, obtains product S 4.
Characterized by XRD by the product obtained, known by XRD spectra, the product obtained is pure phase boehmite.Specific surface area 786.8m 2/ g, pore volume is 2.37cm 3/ g.

Claims (6)

1. a controllable method for preparing for bigger serface macropore volume boehmite, is characterized in that, the concrete steps of the method comprise:
(1) alum liquor of 0.1-0.7mol/L is prepared; The sodium hydroxide and the gibbsite that by mol ratio are 2-5 are soluble in water, react 1-50h and obtain the sodium aluminate solution that mass concentration is 5-55% at 100-120 DEG C;
(2) sodium aluminate solution is added drop-wise in alum liquor to pH value be 7-11,
(3) drip sodium aluminate solution and alum liquor in the suspension obtained to step (2), dropping process keeps system pH to be 7-11 simultaneously;
(4) suspension that step (3) obtains is transferred in autoclave, crystallization 5-50h at 70-150 DEG C;
(5) after having reacted, autoclave is cooled to room temperature, the white depositions deionized water wash obtained, at 60-100 DEG C, drying obtains bigger serface macropore volume boehmite.
2. according to the preparation method described in claim 1, it is characterized in that, in step (1), the mol ratio of sodium hydroxide and gibbsite is 4-5.
3. according to the preparation method described in claim 1, it is characterized in that, in step (2), pH value controls at 9-10.
4. according to the preparation method described in claim 1, it is characterized in that, in step (3), pH value controls at 9-10.
5. according to the preparation method described in claim 1, it is characterized in that, in step (4), temperature is 80-120 DEG C, and crystallization time is 10-40h.
6. according to the preparation method described in claim 1, it is characterized in that, along with the increase of alum liquor concentration, the specific surface area of the bigger serface macropore volume boehmite obtained is at 400-800m 2increase progressively within the scope of/g, pore volume is at 1.4-2.4cm 3increase progressively within the scope of/g.
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CN105883871A (en) * 2016-04-17 2016-08-24 北京化工大学 Preparation method of bohemite
CN106966417A (en) * 2017-04-01 2017-07-21 廖志龙 A kind of method for preparing soilless sticking specific area boehmite
CN108212224A (en) * 2017-12-06 2018-06-29 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

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CN105883871A (en) * 2016-04-17 2016-08-24 北京化工大学 Preparation method of bohemite
CN105883871B (en) * 2016-04-17 2017-12-29 北京化工大学 A kind of preparation method of boehmite
CN106966417A (en) * 2017-04-01 2017-07-21 廖志龙 A kind of method for preparing soilless sticking specific area boehmite
CN108212224A (en) * 2017-12-06 2018-06-29 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

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