CN104671264A - Preparation method of mesoporous alumina - Google Patents
Preparation method of mesoporous alumina Download PDFInfo
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- CN104671264A CN104671264A CN201510125165.6A CN201510125165A CN104671264A CN 104671264 A CN104671264 A CN 104671264A CN 201510125165 A CN201510125165 A CN 201510125165A CN 104671264 A CN104671264 A CN 104671264A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
The invention provides a preparation method of mesoporous alumina. The preparation method is characterized in that aluminum hydroxide and sodium hydroxide are adopted as raw materials, cetyl trimethyl ammonium bromide is adopted as a template agent, an ultrasonic assisting aging method, a program heating crystallization method and a high temperature roasting method are adopted to synthesize the mesoporous alumina, decomposed gas of the template agent is discharged into a waste gas treatment device. The method is safe to operate, simple in process, low in raw material cost, short in working period and environment-friendly in preparation process.
Description
Technical field
The present invention relates to a kind of preparation method of meso-porous alumina, more precisely about a kind of mesoporous alumina preparation method adopting the energy-conserving and environment-protective of the modes such as ultrasonic assistant is aging, temperature programming crystallization, waste gas recovery process in preparation process.
Background technology
Mesoporous material is a kind of novel nano structure material risen the nineties in 20th century.After Mobil company in 1992 has synthesized MCM-41, people successively have developed various non-silicon-based mesoporous material, comprise transition metal oxide, rare earth oxide and complex metal oxides.Mesoporous material refers to that specific surface area (is generally greater than 200m comparatively greatly
2/ g), pore size distribution is at the porous material of 2 ~ 50nm.If duct arranges according to the space group of geometry, narrow pore size distribution range, just belongs to ordered mesoporous material.This type material in catalysis, adsorb and the field such as to be separated and to be widely used.Aluminum oxide (Al
2o
3) crystal formation enrich, cheap and easy to get, there are good physicochemical property, be a kind of very important support of the catalyst and sorbent material, be industrially widely used.Meso-porous alumina is except having common Al
2o
3outside the excellent properties of material, also have mesoporous characteristic, its catalysis, absorption property are more superior, and therefore relevant Synthesis and applications research tool is of great significance, and causes the extensive concern of people in recent years.
Sol-gel method is modal mesoporous material preparation method, surfactant dissolves is formed vitreosol in a solvent, in succession add aluminium source and other reagent, fully agingly after stirring and dissolving change gel (i.e. presoma) into, aftertreatment is carried out to gel and namely obtains corresponding mesoporous material.Sun etc. are with AlCl
36H
2the ammonia soln of O is aluminium source, with polyoxyethylene glycol (PEG) for structure directing agent and dispersion agent, the presoma prepared through aging, washing and alcohol wash removing PEG and other impurity after at 110 DEG C of dry 2h, be placed in differing temps calcining obtain meso-porous alumina.Du etc. are with NaAlO
2for aluminium source, control its concentration of aqueous solution and form colloidal sol, drip HCl control ph, hot water bath temperature control is aging by gel, calcines after methanol wash and drying, and obtained aperture is at the boehmite-type meso-porous alumina of 2 ~ 20nm.Sol-gel method is applied widely, and safety is easy, but preparation cycle is long, poor repeatability.
Hydrothermal Synthesis technology is aluminum oxide synthesis one of major technique, refers in encloses container, using water as solvent, prepares under certain temperature, pressure, a kind of method of processing and evaluating material.Repair and fly to wait people to take sodium lauroyl glutamate as template, sodium metaaluminate is that aluminium source is in aqueous by sol-gel method aging for some time, generate pressure Crystallizing treatment by self after being promoted to comparatively high temps, then obtain meso-porous alumina through aftertreatments such as filtration, washing, roastings.
Ultrasonic wave is conducive to synthesizing the mesoporous material that pattern is homogeneous, degree of crystallinity is high, this promoter action is on the one hand because ultrasonic wave adds the solubleness of raw material, accelerate the balance of polycondensation-depolymerization, on the other hand because ultrasonic wave has impact to weathering process, cavitation bubble can play the effect of similar nucleus, promotes crystal growth, accelerates crystal seed dispersion, nucleus quantity in system is increased, effectively shortens preparation time.As Yin Wei etc. synthesizes mesopore molecular sieve under ul-trasonic irradiation, moisten bright great waves etc. with ultrasonic-assisted synthesis mesostructured material investigated ul-trasonic irradiation time and power to the impact of product.
Summary of the invention
The object of the present invention is to provide that a kind of operational safety, technique are simple, raw materials cost is low, the duration shorten, the mesoporous alumina preparation method of preparation process environmental protection.With aluminium hydroxide and sodium hydroxide for main raw material, take cetyl trimethylammonium bromide as template, ultrasonic assistant method that is aging, temperature programming crystallization is adopted effectively to shorten preparation time and reduce energy consumption, the decomposition gas that template is formed after high-temperature roasting enters the emission-control equipment that weakly alkaline absorption liquid is housed, and realizes environmental protection.
Preparation process is as follows:
Under stirring at room temperature state, quantitative analysis pure cerium hydroxide sodium is added in appropriate distilled water, after being heated to certain temperature, add quantitative analysis pure cerium hydroxide aluminium, keep boiling state to reflux for some time, be cooled to room temperature, obtain sodium aluminate solution.Taking the pure cetyl trimethylammonium bromide of quantitative analysis is dissolved in appropriate distilled water, be stirred well to whole dissolving, slowly add appropriate sodium aluminate solution, nitric acid regulator solution pH to 7 is dropwise dripped under whipped state, aging for some time under the room temperature ultrasonic agitation state of certain frequency, transfer them in autoclave, rise to 120 DEG C with certain temperature rise rate, crystallization for some time at 120 DEG C.Product through repeatedly wash, suction filtration, through 120 DEG C dry 2h.The solid obtained is placed in retort furnace in 600 DEG C of roasting 3h, the gas that in roasting process, cetyl trimethylammonium bromide decomposes enters the treatment unit that weakly alkaline (pH8 ~ 9) absorption liquid is housed through induced draft fan.
Accompanying drawing explanation
Fig. 1 is the meso-porous alumina sample XRD diffractogram prepared according to embodiment one;
Fig. 2 a is the meso-porous alumina sample pore size distribution curve prepared according to embodiment one;
Fig. 2 b is the meso-porous alumina sample pore size distribution curve prepared according to embodiment two;
Fig. 2 c is the meso-porous alumina sample pore size distribution curve prepared according to embodiment three.
Embodiment
Following embodiment is to make those skilled in the art understand the present invention in more detail, but lift embodiment the present invention do not imposed any restrictions.
embodiment one
Under stirring at room temperature state, 500g analytical pure sodium hydroxide is added in 800g distilled water, after being heated to 80 DEG C, add 650g analytical pure aluminium hydroxide, keep boiling state backflow 2h, be cooled to room temperature, obtain sodium aluminate solution; Taking 36.5g analytical pure cetyl trimethylammonium bromide is dissolved in 500ml distilled water, be stirred well to whole dissolving, slowly add the sodium aluminate solution that 30g is obtained, nitric acid regulator solution pH to 7 is dropwise dripped under whipped state, aging 2h under the room temperature ultrasonic agitation state that ultrasonic frequency is 40KHz, transfer them in autoclave, rise to 120 DEG C with the temperature rise rate of 2 DEG C/min, crystallization 4h at 120 DEG C; Product through repeatedly wash, suction filtration, through 120 DEG C dry 2h; The solid obtained is placed in retort furnace in 600 DEG C of roasting 3h, the gas that in roasting process, cetyl trimethylammonium bromide decomposes enters the treatment unit that pH8 ~ 9 weakly alkaline absorption liquid is housed through induced draft fan.XRD diffraction characterizes proves that the aluminum oxide obtained is mesoporous material.Meso-porous alumina specific surface area: 277m
2/ g; Pore volume: 0.49m
3/ g; Mean pore size: 7.2nm.
embodiment two
Operation steps is identical with embodiment one, and only changing weathering process is not having to stir in ultrasonic wave situation to carry out 2h, and other conditions are constant.The meso-porous alumina specific surface area obtained: 236m
2/ g; Pore volume: 0.32m
3/ g; Mean pore size: 5.4nm.
embodiment three
Operate identical with embodiment one, only change crystallization process and do not adopt temperature-programmed mode, 120 DEG C of crystallization 6h, other conditions are constant.The meso-porous alumina specific surface area obtained: 256m
2/ g; Pore volume: 0.47m
3/ g; Mean pore size: 7.4nm.
Claims (1)
1. the preparation method of a meso-porous alumina, it is characterized in that comprising the following steps: under stirring at room temperature state, 500g analytical pure sodium hydroxide is added in 800g distilled water, 650g analytical pure aluminium hydroxide is added after being heated to 80 DEG C, keep boiling state backflow 2h, be cooled to room temperature, obtain sodium aluminate solution; Taking 36.5g analytical pure cetyl trimethylammonium bromide is dissolved in 500ml distilled water, be stirred well to whole dissolving, slowly add the sodium aluminate solution that 30g is obtained, nitric acid regulator solution pH to 7 is dropwise dripped under whipped state, aging 2h under the room temperature ultrasonic agitation state that ultrasonic frequency is 40KHz, transfer them in autoclave, rise to 120 DEG C with the temperature rise rate of 2 DEG C/min, crystallization 4h at 120 DEG C; Product through repeatedly wash, suction filtration, through 120 DEG C dry 2h; The solid obtained is placed in retort furnace in 600 DEG C of roasting 3h, the gas that in roasting process, cetyl trimethylammonium bromide decomposes enters the treatment unit that pH8 ~ 9 weakly alkaline absorption liquid is housed through induced draft fan.
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| CN201510125165.6A CN104671264A (en) | 2015-03-23 | 2015-03-23 | Preparation method of mesoporous alumina |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105056876A (en) * | 2015-08-14 | 2015-11-18 | 黄志强 | Preparation method and application of rare earth yttrium-doped alumina nano-material |
| CN108622921A (en) * | 2018-08-16 | 2018-10-09 | 青岛科技大学 | A kind of high temperature resistant low-sodium aluminum hydroxide novel preparation method |
| CN111807393A (en) * | 2020-07-17 | 2020-10-23 | 青岛科技大学 | Method for improving compatibility of aluminum hydroxide |
| CN113620836A (en) * | 2021-08-13 | 2021-11-09 | 山东达民化工股份有限公司 | Preparation method of acetonitrile |
-
2015
- 2015-03-23 CN CN201510125165.6A patent/CN104671264A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105056876A (en) * | 2015-08-14 | 2015-11-18 | 黄志强 | Preparation method and application of rare earth yttrium-doped alumina nano-material |
| CN108622921A (en) * | 2018-08-16 | 2018-10-09 | 青岛科技大学 | A kind of high temperature resistant low-sodium aluminum hydroxide novel preparation method |
| CN111807393A (en) * | 2020-07-17 | 2020-10-23 | 青岛科技大学 | Method for improving compatibility of aluminum hydroxide |
| CN113620836A (en) * | 2021-08-13 | 2021-11-09 | 山东达民化工股份有限公司 | Preparation method of acetonitrile |
| CN113620836B (en) * | 2021-08-13 | 2022-08-05 | 山东达民化工股份有限公司 | Preparation method of acetonitrile |
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