CN103359765A - Preparation method of micron gamma aluminum oxide with controllable morphology and mesoporous structure - Google Patents
Preparation method of micron gamma aluminum oxide with controllable morphology and mesoporous structure Download PDFInfo
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- CN103359765A CN103359765A CN2013102901493A CN201310290149A CN103359765A CN 103359765 A CN103359765 A CN 103359765A CN 2013102901493 A CN2013102901493 A CN 2013102901493A CN 201310290149 A CN201310290149 A CN 201310290149A CN 103359765 A CN103359765 A CN 103359765A
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Abstract
The invention discloses a preparation method of micron gamma aluminum oxide with controllable morphology and a mesoporous structure. The method comprises the following steps of: uniformly stirring and mixing an aluminum source material, a dispersing agent, a precipitating agent, and deionized water at room temperature to obtain a mixed solution; sealing the obtained mixed solution, carrying out a hydrothermal reaction at 80-180 DEG C for 6-48 hours to obtain a mixed solution of white precipitate and a mother solution, centrifugally separating the white precipitate from the mother solution, washing the white precipitate, and drying the washed precipitate in a drying oven to obtain a dispersing agent compound gamma aluminum oxide precursor; and calcining the gamma aluminum oxide precursor to obtain one or more of zero-dimensional/one-dimensional/three-dimensional micron gamma aluminum oxide with the mesoporous structure. According to the micron gamma aluminum oxide with the controllable morphology and the mesoporous structure disclosed by the invention, the mesoporous structure enables the aluminum oxide to be widely applied to the fields of catalysis and adsorption. Simultaneously, the preparation method of the micron gamma aluminum oxide with the controllable morphology and the mesoporous structure disclosed by the invention is simple in process, safe to operate, and low in cost.
Description
Technical field
The present invention relates to gamma-alumina, particularly relate to a kind of pattern controlled and have meso-hole structure the micron gamma-alumina the preparation method; The micron gamma-alumina has zero dimension, one dimension, three-dimensional structure and with meso-hole structure.
Technical background
Activated alumina with meso-hole structure is one of most important support of the catalyst and sorbent material, is widely used at refining of petroleum catalyzer and sewage treatment area.Known aluminum oxide has 8 kinds of crystalline state, wherein γ-Al so far
2O
3Have higher pore volume, specific surface area and thermostability, therefore be widely used.One of critical nature of support of the catalyst and sorbent material is its meso-hole structure feature and specific surface area.Requirement to support of the catalyst and sorbent material at first provides large as far as possible reaction contact area, improve the dispersity of active ingredient, next is the aperture, the aperture is excessive, the specific surface area of carrier will reduce, the aperture is too small, brings adverse influence for the diffusion of reactant, thereby affects the activity of catalyzer and sorbent material.The potential application that has simultaneously the aluminum oxide of meso-hole structure not only depends on its porousness, more with its microscopic appearance very large relation is arranged.Present modal mesoporous γ-Al
2O
3The preparation method be template, adopt polyoxyethylene, P123, the various template such as glucose although the method is widely applicable, exist influence factor more, are difficult to effectively control for pattern, the properity of aluminum oxide.
Summary of the invention
The objective of the invention is to overcome the technical disadvantages of existing preparation gamma-alumina, provide a kind of technique simple, operational safety, and the low pattern of cost is controlled and have a preparation method of the micron gamma-alumina of meso-hole structure.
The present invention adopts hydrothermal method to prepare gamma-alumina forerunner product, by control hydrothermal temperature and the hydro-thermal time, can make zero dimension, the three-dimensional micron of peacekeeping gamma-alumina presoma, and it is identical and have a meso-hole structure micrometer alumina to obtain pattern through calcining and decomposing again.The mesoporous gamma-alumina of zero dimension, its pattern are the spheroid of rule, and independent or polymerization exists, and its diameter is 1～5 μ m, and mesoporous distribution concentrates on 10～15nm; One-dimensional mesoporous gamma-alumina, diameter are 200～500nm, and length is 10～20 μ m, and its length-to-diameter ratio is 40～50, and mesoporous distribution concentrates on 10～50nm; Three-dimensional gamma-alumina, the fiber cluster, the floweriness shape, staple length 1～3 μ m, integral diameter 3～5 μ m, mesoporous distribution concentrates on 30～50nm.
Purpose of the present invention is achieved through the following technical solutions:
A kind of pattern is controlled and have the preparation method of the micron gamma-alumina of meso-hole structure, comprises the steps and processing condition:
Step 1: aluminium source material, dispersion agent, precipitation agent and deionized water are mixed at ambient temperature, obtain mixing solutions; Aluminium source material and dispersion agent and the concentration in mixing solutions are respectively 0.2～1mol/L and 0.2～2mol/L; Precipitation agent and aluminium source material mol ratio are 3～20:1; Described dispersion agent is polyoxyethylene glycol, ammonium citrate, CTAB or polypyrrole alkane ketone; Described aluminium source material is one or both in six hydration aluminum chlorides, ANN aluminium nitrate nonahydrate and the Monoaluminum monoammonium disulfate Dodecahydrate; Precipitation agent is ammoniacal liquor or urea;
Step 2: the preparation of gamma-alumina presoma: with the mixing solutions sealing of gained, 80～180 ℃ of Water Under thermal responses 6～48 hours, obtain white precipitate and mother liquor mixing solutions, with white precipitate and mother liquor centrifugation, washing, then at the baking oven inner drying, obtain the compound gamma-alumina presoma of dispersion agent;
Step 3: with the calcining of the resulting gamma-alumina presoma of step 1, obtain one or more the micron gamma-alumina with meso-hole structure in zero dimension, the peacekeeping three-dimensional; Described calcining is to be warming up to 800～900 ℃ by room temperature with 5～20 ℃/min, and its insulation 2～10 hours after naturally cooling.
Preferably, described stirring is to realize that by magnetic agitation speed is 200～400rpm, churning time 1.5-2.5 hour.Described baking oven inner drying is 60～100 ℃ of dryings 6～12 hours in baking oven.Described washing is not for to wash and absolute ethanol washing white precipitation.The number of times of described washing and absolute ethanol washing is each 4～6 times.
With respect to prior art, the present invention has following advantage and beneficial effect:
Micron meso-porous alumina of the present invention adopts hydrothermal method, can make zero dimension, a peacekeeping is three-dimensional and has the micron gamma-alumina of meso-hole structure.Its distinctive meso-hole structure and high-specific surface area make it be widely used in the fields such as catalysis and absorption.Preparation pattern of the present invention is controlled and to have the micron gamma-alumina preparation technology of meso-hole structure simple to operate, and safety and cost are low.
Description of drawings
Fig. 1 is the SEM figure of the mesoporous micron of embodiment 1 gained zero dimension gamma-alumina;
Fig. 2 is the mesoporous distribution plan of the mesoporous micron of embodiment 1 gained zero dimension gamma-alumina;
Fig. 3 is the SEM figure of embodiment 2 gained zero dimensions and one-dimensional micron gamma-alumina;
Fig. 4 is the SEM figure of the one-dimensional mesoporous micron of embodiment 6 gained gamma-alumina;
Fig. 5 is the mesoporous distribution plan of the one-dimensional mesoporous micron of embodiment 6 gained gamma-alumina;
Fig. 6 is the SEM figure of embodiment 7 gained zero dimensions and three-dimensional meso-hole micron gamma-alumina;
Fig. 7 is the SEM figure of embodiment 8 gained three-dimensional meso-hole micron gamma-aluminas;
Fig. 8 is the mesoporous distribution plan of embodiment 8 gained three-dimensional meso-hole micron gamma-aluminas;
Fig. 9 is embodiment 8 gained three-dimensional meso-hole micron gamma-aluminas during as sorbent material, the Congo red ultra-violet absorption spectrum of absorption different time;
Figure 10 is embodiment 8 gained three-dimensional meso-hole micron gamma-aluminas during as sorbent material, the relative concentration curve of the Congo red solution of absorption different time.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but the scope of protection of present invention is not limited to the scope of embodiment statement.
Get 0.35g polyoxyethylene glycol, 3.4g six hydration aluminum chlorides, 2.52g urea and deionized water 70mL magnetic agitation and be dissolved to evenly, stirring velocity is 200rpm, and 1.5 hours time obtained mixing solutions, i.e. mother liquor.Then mixing solutions is transferred to and is sealed in the polytetrafluoroethyllining lining in the water heating kettle, with water heating kettle 80 ℃ microwave hydrothermal reaction 6 hours, behind the naturally cooling, obtain the mixing solutions of white precipitate and mother liquor, then separate by centrifugal solid-liquid, centrifugal speed is 4000rpm, 3 minutes time.Then pass through washing and absolute ethanol washing each 4 times, the washing white precipitate, and in baking oven 60 ℃ of dryings 12 hours, obtain the gamma-alumina presoma, at last with the gamma-alumina presoma, be warming up to 800 ℃ with 10 ℃/min from room temperature, simultaneously at 800 ℃ of insulations naturally cooling after 2 hours, obtain having the zero dimension micron gamma-alumina of meso-hole structure, zero dimension micron gamma-alumina diameter is 1～3 μ m, and mesoporous distribution of sizes concentrates on 13 and 50nm.Fig. 1 is the SEM picture of the mesoporous micron of gained zero dimension gamma-alumina, i.e. spherical mesoporous micron gamma-alumina.Fig. 1 is 3000 times SEM figure for the magnification that obtains when acceleration voltage is respectively 10KV and 5A with the acceleration electric current.As shown in the figure, the gamma-alumina globulate exists, and its diameter is for being 1～3 μ m, and Fig. 2 is its mesoporous distribution plan.As seen from the figure, mesoporous paper centering scale is at 13nm and 50nm place.Mesoporous formation is because in calcination process, because the decomposition of polyoxyethylene glycol so that stay hole between the particle, becomes mesoporous.The micron gamma-alumina makes it in adsorbing domain very large using value be arranged because of himself activity and its unique meso-hole structure.
Embodiment 2
Get 5g polyoxyethylene glycol, 19.3g six hydration aluminum chlorides, 50g urea and deionized water 80mL magnetic agitation and be dissolved to evenly, stirring velocity is 300rpm, and time 2 h obtains mixing solutions, i.e. mother liquor.Then mixing solutions is transferred to and is sealed in the polytetrafluoroethyllining lining in the water heating kettle, with water heating kettle 100 ℃ microwave hydrothermal reaction 10 hours, behind the naturally cooling, obtain the mixing solutions of white precipitate and mother liquor, then separate by centrifugal solid-liquid, centrifugal speed is 4000rpm, 3 minutes time.Then pass through washing and absolute ethanol washing each 5 times, the washing white precipitate, and in baking oven 80 ℃ of dryings 12 hours, obtain the gamma-alumina presoma, at last with the gamma-alumina presoma, be warming up to 820 ℃ with 10 ℃/min from room temperature, simultaneously at 820 ℃ of insulations naturally cooling after 4 hours, obtain having zero dimension and the one-dimensional micron gamma-alumina mixture of meso-hole structure, zero dimension micron gamma-alumina diameter is 2～5 μ m, staple length is 8～10 μ m, and diameter is 200～300nm.Fig. 3 is the zero dimension of present embodiment gained and the SEM image of one-dimensional micron gamma-alumina.Fig. 3 is 3000 times SEM figure for the magnification that obtains when acceleration voltage is respectively 10KV and 5A with the acceleration electric current.As seen from the figure, ball-aluminium oxide is independent or assemble existence, and its diameter is 2～5 μ m, and fibrous alumina length is 8～10 μ m, and diameter is 200～300nm.
Get 4.4g ammonium citrate, 10.5g six hydration aluminum chlorides, 55g urea and deionized water 90mL magnetic agitation and be dissolved to evenly, stirring velocity is 400rpm, and 2.5 hours time obtained mixing solutions, i.e. mother liquor.Then mixing solutions is transferred to and is sealed in the polytetrafluoroethyllining lining in the water heating kettle, with water heating kettle the microwave hydrothermal reaction of 120 ° of C 15 hours, behind the naturally cooling, obtain the mixing solutions of white precipitate and mother liquor, then separate by centrifugal solid-liquid, centrifugal speed is 4000rpm, 3 minutes time.Then pass through washing and absolute ethanol washing each 6 times, the washing white precipitate, and in baking oven 80 ℃ of dryings 12 hours, obtain the gamma-alumina presoma, at last with the gamma-alumina presoma, be warming up to 840 ℃ with 15 ℃/min from room temperature, simultaneously at 840 ℃ of insulations naturally cooling after 6 hours, obtain having zero dimension and the one-dimensional micron gamma-alumina mixture of meso-hole structure, one-dimensional micron gamma-alumina diameter is 200～300nm, length is 15～20 μ m, and mesoporous distribution of sizes concentrates on 13nm.
Embodiment 4
Get 6g ammonium citrate, 7.5g ANN aluminium nitrate nonahydrate, 15g urea and deionized water 100mL magnetic agitation and be dissolved to evenly, stirring velocity is 400rpm, and time 2 h obtains mixing solutions, i.e. mother liquor.Then mixing solutions is transferred to and is sealed in the polytetrafluoroethyllining lining in the water heating kettle, with water heating kettle the microwave hydrothermal reaction of 140 ° of C 18 hours, behind the naturally cooling, obtain the mixing solutions of white precipitate and mother liquor, then separate by centrifugal solid-liquid, centrifugal speed is 4000rpm, 3 minutes time.Then pass through washing and absolute ethanol washing each 5 times, the washing white precipitate, and in baking oven 100 ℃ of dryings 8 hours, obtain the gamma-alumina presoma, at last with the gamma-alumina presoma, be warming up to 860 ℃ with 20 ℃/min from room temperature, simultaneously at 860 ℃ of insulations naturally cooling after 8 hours, obtain having zero dimension and the one-dimensional micron gamma-alumina of meso-hole structure, one-dimensional micron gamma-alumina diameter is 200～300nm, length is 10～15 μ m, and mesoporous distribution of sizes concentrates on 15nm.
Embodiment 5
Get 3g CTAB, 12g ANN aluminium nitrate nonahydrate, 15g urea and deionized water 110mL magnetic agitation and be dissolved to evenly, stirring velocity is 200rpm, and time 2 h obtains mixing solutions, i.e. mother liquor.Then mixing solutions is transferred to and is sealed in the polytetrafluoroethyllining lining in the water heating kettle, with water heating kettle the microwave hydrothermal reaction of 130 ° of C 24 hours, behind the naturally cooling, obtain the mixing solutions of white precipitate and mother liquor, then separate by centrifugal solid-liquid, centrifugal speed is 4000rpm, 3 minutes time.Then pass through washing and absolute ethanol washing each 4 times, the washing white precipitate, and in baking oven 90 ℃ of dryings 12 hours, obtain the gamma-alumina presoma, at last with the gamma-alumina presoma, be warming up to 860 ℃ with 20 ℃/min from room temperature, simultaneously at 860 ℃ of insulations naturally cooling after 10 hours, obtain having zero dimension and the one-dimensional micron gamma-alumina of meso-hole structure, one-dimensional micron gamma-alumina diameter is 300～400nm, length is 10～20 μ m, and mesoporous distribution of sizes concentrates on 17nm.
Embodiment 6
Get 4g polypyrrole alkane ketone, 15g ANN aluminium nitrate nonahydrate, 35g urea and deionized water 120mL magnetic agitation and be dissolved to evenly, stirring velocity is 300rpm, and time 2 h obtains mixing solutions, i.e. mother liquor.Then mixing solutions is transferred to and is sealed in the polytetrafluoroethyllining lining in the water heating kettle, with water heating kettle the microwave hydrothermal reaction of 160 ° of C 30 hours, behind the naturally cooling, obtain the mixing solutions of white precipitate and mother liquor, then separate by centrifugal solid-liquid, centrifugal speed is 4000rpm, 3 minutes time.Then pass through washing and absolute ethanol washing each 5 times, the washing white precipitate, and in baking oven 80 ℃ of dryings 12 hours, obtain the gamma-alumina presoma, at last with the gamma-alumina presoma, be warming up to 880 ℃ with 150 ℃/min from room temperature, simultaneously at 880 ℃ of insulations naturally cooling after 4 hours, obtain having the one-dimensional micron gamma-alumina of meso-hole structure, one-dimensional micron gamma-alumina diameter is 400～500nm, length is 17～20 μ m, and mesoporous distribution of sizes concentrates on 13 and the 50nm place.Fig. 4 is the SEM picture of the one-dimensional mesoporous micron of present embodiment gained gamma-alumina, and Fig. 4 is 3000 times SEM figure for the magnification that obtains when acceleration voltage is respectively 10KV and 5A with the acceleration electric current.As shown in the figure, one dimension fibre shape micron gamma-alumina diameter is 400～500nm, and length is 17～20 μ m; Fig. 5 is its mesoporous distribution plan.As seen from the figure, mesoporous paper centering scale is at 13nm and 50nm place.Mesoporous formation is because in calcination process, because the decomposition of polyoxyethylene glycol so that stay hole between the particle, becomes mesoporous.The micron gamma-alumina makes it at catalytic field very large using value be arranged because of himself activity and its unique meso-hole structure.
Embodiment 7
Get 3g polypyrrole alkane ketone, 8g Monoaluminum monoammonium disulfate Dodecahydrate, 30g urea and deionized water 120mL magnetic agitation and be dissolved to evenly, stirring velocity is 200rpm, and time 2 h obtains mixing solutions, i.e. mother liquor.Then mixing solutions is transferred to and is sealed in the polytetrafluoroethyllining lining in the water heating kettle, with water heating kettle the microwave hydrothermal reaction of 180 ° of C 36 hours, behind the naturally cooling, obtain the mixing solutions of white precipitate and mother liquor, then separate by centrifugal solid-liquid, centrifugal speed is 4000rpm, 3 minutes time.Then pass through washing and absolute ethanol washing each 6 times, the washing white precipitate, and in baking oven 100 ℃ of dryings 12 hours, obtain the gamma-alumina presoma, at last with the gamma-alumina presoma, be warming up to 900 ℃ with 15 ℃/min from room temperature, simultaneously at 900 ℃ of insulations naturally cooling after 2 hours, obtain having zero dimension and the three-dimensional micron gamma-alumina of meso-hole structure, three-dimensional micron gamma-alumina is that the fiber of 1～2 μ m consists of the three-dimensional structure that integral diameter is 2～4 μ m by length, and mesoporous distribution of sizes concentrates on 30nm.Fig. 6 is the SEM picture of present embodiment gained zero dimension and three-dimensional meso-hole micron gamma-alumina, in calcination process, because the decomposition of polyoxyethylene glycol so that stay hole between the particle, becomes mesoporous.Fig. 6 is 3000 times SEM figure for the magnification that obtains when acceleration voltage is respectively 10KV and 5A with the acceleration electric current.As shown in the figure, the spherical in shape and clustered fiber of aluminum oxide exists, and the ball-aluminium oxide diameter is 2～4 μ m, and clustered fiber shape aluminum oxide is that the fiber of 1～2 μ m consists of the three-dimensional structure that integral diameter is 2～4 μ m by length.Mesoporous formation is because in calcination process, because the decomposition of polyoxyethylene glycol so that stay hole between the particle, becomes mesoporous.
Get 7g polypyrrole alkane ketone, 10g Monoaluminum monoammonium disulfate Dodecahydrate, 30g urea and deionized water 120mL magnetic agitation and be dissolved to evenly, stirring velocity is 400rpm, and time 2 h obtains mixing solutions, i.e. mother liquor.Then mixing solutions is transferred to and is sealed in the polytetrafluoroethyllining lining in the water heating kettle, with water heating kettle the microwave hydrothermal reaction of 200 ° of C 48 hours, behind the naturally cooling, obtain the mixing solutions of white precipitate and mother liquor, then separate by centrifugal solid-liquid, centrifugal speed is 4000rpm, 3 minutes time.Then pass through washing and absolute ethanol washing each 6 times, the washing white precipitate, and in baking oven 80 ℃ of dryings 12 hours, obtain the gamma-alumina presoma, at last with the gamma-alumina presoma, be warming up to 900 ℃ with 20 ℃/min from room temperature, simultaneously at 900 ℃ of insulations naturally cooling after 10 hours, obtain having the three-dimensional micron gamma-alumina of meso-hole structure, three-dimensional micron gamma-alumina is that the fiber of 2-3 μ m consists of the three-dimensional structure that integral diameter is 3-5 μ m by length, and mesoporous distribution of sizes concentrates on 13 and 50nm.Fig. 7 is three-dimensional meso-hole micron gamma-alumina at acceleration voltage and the magnification of accelerating to obtain when electric current is respectively 10KV and 5A is 3000 times SEM figure, i.e. fiber cluster shape shape three-dimensional arrangement as shown in Figure 7, gamma-alumina are that the fiber of 2-3 μ m consists of the three-dimensional structure that integral diameter is 3-5 μ m by length.Fig. 8 is its mesoporous distribution plan.As seen from the figure, mesoporous paper centering scale is at 13nm and 250nm place.Mesoporous formation is because in calcination process, because the decomposition of polyoxyethylene glycol so that stay hole between the particle, becomes mesoporous.Thus obtained three-dimensional meso-hole micron gamma-alumina has very large using value in the sorbent material field.Fig. 9 is three-dimensional meso-hole micron gamma-alumina during as sorbent material, its adsorption effect phenogram, and it is Congo red in what leave standstill namely to put into three-dimensional meso-hole micron gamma-alumina, the ultra-violet absorption spectrum of absorption different time.Figure 10 is three-dimensional meso-hole micron gamma-alumina during as sorbent material, the Congo red relative concentration curve of absorption different time, and as seen from the figure, after 10 minutes, Congo red in the solution almost completely is adsorbed.The gamma-alumina surface exists L acid sites and basic center, and a large amount of hydroxyl groups is arranged, and therefore, gamma-alumina has extraordinary activity.And mesoporous gamma-alumina makes its L acid sites, and basic center and hydroxyl group quantity increase, thereby have increased activity, and then shows excellent adsorption property.
Claims (5)
1. a pattern is controlled and have the preparation method of the micron gamma-alumina of meso-hole structure, it is characterized in that comprising the steps and processing condition:
Step 1: aluminium source material, dispersion agent, precipitation agent and deionized water are mixed at ambient temperature, obtain mixing solutions; Aluminium source material and dispersion agent and the concentration in mixing solutions are respectively 0.2～1mol/L and 0.2～2mol/L; Precipitation agent and aluminium source material mol ratio are 3～20:1; Described dispersion agent is polyoxyethylene glycol, ammonium citrate, CTAB or polypyrrole alkane ketone; Described aluminium source material is one or both in six hydration aluminum chlorides, ANN aluminium nitrate nonahydrate and the Monoaluminum monoammonium disulfate Dodecahydrate; Precipitation agent is ammoniacal liquor or urea;
Step 2: the preparation of gamma-alumina presoma: with the mixing solutions sealing of gained, 80～180 ℃ of Water Under thermal responses 6～48 hours, obtain white precipitate and mother liquor mixing solutions, with white precipitate and mother liquor centrifugation, washing, then at the baking oven inner drying, obtain the compound gamma-alumina presoma of dispersion agent;
Step 3: with the calcining of the resulting gamma-alumina presoma of step 1, obtain one or more the micron gamma-alumina with meso-hole structure in zero dimension, the peacekeeping three-dimensional; Described calcining is to be warming up to 800～900 ℃ by room temperature with 5～20 ℃/min, and its insulation 2～10 hours after naturally cooling.
2. controlled according to claims 1 described pattern and have the preparation method of the micron gamma-alumina of meso-hole structure, it is characterized in that: described stirring is for realizing that by magnetic agitation speed is 200～400rpm, churning time 1.5-2.5 hour.
3. controlled according to claims 1 described pattern and have the preparation method of the micron gamma-alumina of meso-hole structure, it is characterized in that: described baking oven inner drying is 60～100 ℃ of dryings in baking oven 6～12 hours.
Controlled according to claims 1 described pattern and have meso-hole structure the micron gamma-alumina the preparation method, it is characterized in that: described washing is not for to wash and absolute ethanol washing white precipitation.
Controlled according to claims 4 described a kind of patterns and have meso-hole structure the micron gamma-alumina the preparation method, it is characterized in that: the number of times of described washing and absolute ethanol washing is each 4～6 times.
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