CN1986409A - Preparing process of nano gamma-alumina powder with intraparticle mesoporous structure - Google Patents
Preparing process of nano gamma-alumina powder with intraparticle mesoporous structure Download PDFInfo
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- CN1986409A CN1986409A CN 200610125561 CN200610125561A CN1986409A CN 1986409 A CN1986409 A CN 1986409A CN 200610125561 CN200610125561 CN 200610125561 CN 200610125561 A CN200610125561 A CN 200610125561A CN 1986409 A CN1986409 A CN 1986409A
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Abstract
The process of preparing nanometer gamm-alumina powder with intraparticle mesoporous structure includes the following steps: dissolving ammonium aluminum sulfate, aluminum chloride and ammonium bicarbonate separately in double distilled water to compound solutions; adding surfactant to the solutions separately and regulating pH value of ammonium bicarbonate solution; dropping the aluminum salt solutions into ammonium bicarbonate solution while magnetically stirring to react; separating, washing, drying, azeotropic distillation to dewatering, and calcining to obtain nanometer gamm-alumina powder with intraparticle mesoporous structure. The nanometer gamm-alumina powder has homogeneously distributed particle size, average particle size of 20-63 nm, average intraparticle pore size of 2.8-7.4 nm, specific surface area of 95-212 sq m/g, and possesses wide application foreground.
Description
Technical field
The present invention relates to a kind of gama-alumina nanometer particle process method, belong to the mesoporous inorganic field of nanometer material technology with intraparticle mesoporous structure.
Background technology
Nano aluminium oxide (Al
2O
3) be meant the alumina product of particle size less than 100nm, because its particle is little, specific surface area is big, thereby higher chemically reactive is arranged, and is widely used in hard mass, reagent and catalyzer and carrier, luminescent material, electronic ceramic substrate and aerospace field.At present, the industrial preparation alumina powder mainly adopts methods such as Bel's method and the thermolysis of aluminium ammonium alum, needs special heating installation, has increased synthetic difficulty.And traditional wet chemical method is difficult to control effectively the size and the microtexture of particle, thereby traditional wet chemical method is difficult to truly nano alumina powder jointed of preparation.
The inorganic mesoporous material of M41S series silicon oxide that the seventies in last century, Mobile company utilized tensio-active agent self-assembly principle at first to synthesize to have meso-hole structure (pore size distribution in the 2-50nm scope be referred to as mesoporous material).At present, tensio-active agent successfully prepares the mesoporous or porous gama-alumina aspect of material.Mesoporous or porous gama-alumina has been widely used in aspects such as industrial adsorbents, chromatographic separation column material, catalyzer and carrier thereof.Yet, with the porous Al of surfactant templates method preparation
2O
3Be generally the relatively poor amorphous structure of thermostability, in its crystallization is the process of γ-phase alumina, can cause subsiding of vesicular structure, greatly reduced the specific surface area of material, thereby had a strong impact on its application aspect catalyzer and sorbent material.This shows that the gama-alumina mesoporous material that preparation has high thermal stability and specific surface area has important practical significance.At present, do not see both at home and abroad the document of the preparation of relevant nanometer gama-alumina nano-powder and application and use and report as yet with intraparticle mesoporous structure.
Summary of the invention
The object of the invention is to provide a kind of preparation method with gama-alumina nano-powder of intraparticle mesoporous structure, this method is easy and simple to handle, cost is low, and the aluminum oxide of preparation with nano-scale, γ-mutually nanocrystalline and mesoporous feature set has higher thermostability and specific surface area.
Technical scheme provided by the invention is that a kind of preparation method with gama-alumina nano-powder of intraparticle mesoporous structure comprises following concrete steps:
(1), takes by weighing exsiccated ammonium alum, aluminum chloride and bicarbonate of ammonia as required, be dissolved in respectively in the secondary water, be made into the liquor alumini chloridi that the aluminum ion total concn is 0.3-0.5mol/L or the mixing solutions of exsiccated ammonium alum and aluminum chloride, the molar ratio range of exsiccated ammonium alum/aluminum chloride is 0-3 in the mixing solutions, and concentration is the ammonium bicarbonate soln of 0.3-0.6mol/L, with the impurity in the microporous membrane elimination solution;
(2), in the mixing solutions of liquor alumini chloridi or exsiccated ammonium alum and aluminum chloride, add poly(oxyethylene glycol) 400, be mixed with the Al that contains the 4-8wt% poly(oxyethylene glycol) 400
3+Concentration is the aluminium salt A solution of 0.3-0.5mol/L, adds Macrogol 2000 in ammonium bicarbonate soln, is made into the bicarbonate of ammonia B solution of the 0.3-0.6mol/L that contains the 1-8wt% Macrogol 2000, and adding ammoniacal liquor is regulated its pH value to 9-10;
(3), under magnetic agitation, in bicarbonate of ammonia B solution, drip 1/2 volume to isopyknic aluminium salt A solution, after titration is finished, continue to be stirred to and react completely, the centrifugation precipitation is washed to detecting no SO with secondary water washing
4 2-, the dry then dry powder that obtains;
(4), the dry powder that obtains is joined in the propyl carbinol of capacity, after the ultrasonic dispersing, fully reflux, distillation removes the azeotrope of 93-95 ℃ n-butanol-water, when the cut temperature rises to 115-120 ℃ of propyl carbinol boiling point, stop distillation, continue to reflux, propyl carbinol is reclaimed in underpressure distillation then, obtains loose γ-Al
2O
3Nano-powder;
(5), with the γ-Al that obtains
2O
3Nano-powder is at 850-900 ℃ of calcining, the γ-Al that obtains having the intraparticle mesoporous structure
2O
3Nanometer powder.
And, in step (1), the impurity in each solution that is disposed with the microporous membrane elimination at last.Dripping with 250-350 under the magnetic agitation of 1000-1300r/min in the step (3)/minute speed in bicarbonate of ammonia B solution, drip 1/2 volume to isopyknic aluminium salt A solution, and the precipitation of centrifugation washed with secondary water washing, detect to there not being SO with the 1-2% nitrate of baryta
4 2-, and then back for several times with washing with alcohol in 70-90 ℃ of dry 3-4 hour acquisition dry powder.Calcination time is 2-3 hour in the step (5), the γ-Al with intraparticle mesoporous structure that is obtained
2O
3The size distribution of nanometer powder is even, and median size is at 20-63nm in the particle, and the averaged particles internal orifice dimension is that specific surface area is at 95-212m at 2.8-7.4nm
2Local adjustable in the/g scope.
As shown from the above technical solution, the present invention by optimizing the precipitin reaction initiator kind, concentration and suitably add tensio-active agent and effectively regulated Al
2O
3Microtextures such as the particle size of product, aperture and specific surface area, thereby more stable γ-Al that acquisition has the intraparticle mesoporous structure
2O
3Nano-powder.Use the inventive method can prepare median size at 20-63nm, mean pore size is that specific surface area is at 95-212m at 2.8-7.4nm
2Local adjustable in the/g scope, as to have the stable and specific surface area of higher thermal gama-alumina nano-powder.And this with nano-scale, γ-mutually nanocrystalline and mesoporous feature set meso-porous nano gama-alumina will adsorb, separate, aspects such as catalyzer and carrier thereof, automobile three-effect catalysis conversion system, chromatographic separation column material show wide application prospect.
The present invention compared with prior art has the following advantages and effect:
1. starting material sources is wide, working condition is gentle, energy consumption and cost are low, is fit to suitability for industrialized production.
2. utilize the template action of tensio-active agent, realize nanometer Al by the concentration and the kind of regulating polyglycol surfactants and aluminium salt
2O
3The particle diameter of powder, particle internal orifice dimension size and the partial controllable that distributes thereof.
3.850-900 a ℃ calcining time can keep meso-hole structure when making mesoporous wall crystallization, thereby obtains high surface-area.And the mesoporous of usual method preparation subsided when 900 ℃ of calcinings fully.
This law preparation alumina powder jointed with nano-scale and mesoporous feature set, have broad application prospects at aspects such as catalyzer and carrier thereof, automobile three-effect catalysis conversion system, chromatographic separation column materials.
Description of drawings
Fig. 1 is the transmission electron microscope photo of embodiment 1 products obtained therefrom.
Fig. 2 is the transmission electron microscope photo of embodiment 2 products obtained therefroms.
Fig. 3 is the transmission electron microscope photo of embodiment 3 products obtained therefroms.
Fig. 4 is the transmission electron microscope photo of embodiment 4 products obtained therefroms.
Fig. 5 is the transmission electron microscope photo of embodiment 5 products obtained therefroms.
Embodiment
Take by weighing exsiccated ammonium alum, aluminum chloride and bicarbonate of ammonia at first as required, be dissolved in respectively in the secondary water, be made into the liquor alumini chloridi that the aluminum ion total concn is 0.3-0.5mol/L or the mixing solutions of exsiccated ammonium alum and aluminum chloride, the molar ratio range of exsiccated ammonium alum/aluminum chloride is 0-1 in the mixing solutions, and concentration is the ammonium bicarbonate soln of 0.3-0.6mol/L, with the impurity in the microporous membrane elimination solution.
In the mixing solutions of liquor alumini chloridi or exsiccated ammonium alum and aluminum chloride, add poly(oxyethylene glycol) 400 then, be mixed with the Al that contains the 4-8wt% poly(oxyethylene glycol) 400
3+Concentration is 0.3-0.4mol/L's, adds Macrogol 2000 in ammonium bicarbonate soln, is made into the bicarbonate of ammonia B solution of the 0.3-0.6mol/L that contains the 1-8wt% Macrogol 2000, and adding ammoniacal liquor is regulated its pH value to 9-10.
Above-mentioned two steps are preparation storing solutions, all can repeat in the following embodiments, and are succinct for making embodiment, and this two step is listed separately, just no longer repeat among each embodiment.
The concentration that respectively contains 4.5wt% polyoxyethylene glycol (PEG) 400 under the magnetic agitation of embodiment 1:1300r/min is 0.3mol/LAlCl
3Solution be in the bicarbonate of ammonia B solution (pH is 9.3) of 0.6mol/L as aluminium salt A solution with the concentration that 300 droplets/minute speed adds the isopyknic 4.6wt% of containing polyoxyethylene glycol (PEG) 2000, after titration is finished, continue to stir 0.5h; Centrifugation is washed 3 times, washing with alcohol 3 times with secondary water washing, and 80 ℃ of dry 4h remove surface water, obtains dry powder.The dry powder that obtains is joined in the propyl carbinol of 80ml, after the ultrasonic dispersing, backflow 2h, distillation removes 93 ℃ the azeotrope of n-butanol-water, when the cut temperature rises to 117 ℃ of propyl carbinol boiling points, stops distillation, after continuing backflow 2h, propyl carbinol is reclaimed in underpressure distillation, obtains loose powder.
900 ℃ of calcinings obtained γ-Al in 2 hours
2O
3Product, its particle morphology is seen Fig. 1.Particle distribution is more even, and particle size range is 18-68nm, and median size is 38nm; Particle internal orifice dimension scope is 2-12nm, and mean pore size is 3.8nm in the particle.Specific surface area is 121m
2/ g, the crystallization degree of hole wall is higher.
The Al that will contain 4.5wt%PEG400 under the magnetic agitation of embodiment 2:1000r/min
3+Concentration is 0.30mol/L (AlCl
3: NH
4Al (SO
4)
2=1: 1 mol ratio) solution is in the bicarbonate of ammonia B solution (pH is 9.3) of 0.60mol/L as aluminium salt A solution with the concentration that 250 droplets/minute speed adds isopyknic 4.6wt%PEG2000 of containing, and after titration is finished, continues to stir 0.5h; Centrifugation is washed 3 times, washing with alcohol 3 times with secondary water washing, and 80 ℃ of dry 4h remove surface water, obtains dry powder.The dry powder that obtains is joined in the propyl carbinol of 80ml, after the ultrasonic dispersing, backflow 2h, distillation removes 93 ℃ the azeotrope of n-butanol-water, when the cut temperature rises to 117 ℃ of propyl carbinol boiling points, stops distillation, after continuing backflow 2h, propyl carbinol is reclaimed in underpressure distillation, obtains loose powder.
850 ℃ of calcinings obtained γ-Al in 3 hours
2O
3Product, its particle morphology is seen Fig. 2.Particle distribution is more even, and particle size range is 56-87nm, and median size is 63nm; Particle internal orifice dimension scope is 2-9nm, and mean pore size is 4.7nm in the particle, and specific surface area is 153m
2/ g, the crystallization degree of hole wall is higher.
The Al that will contain 8wt%PEG400 under the magnetic agitation of embodiment 3:1300r/min
3+Concentration is 0.4mol/L (AlCl
3: NH
4Al (SO
4)
2=1: solution 1) is in the bicarbonate of ammonia B solution (pH is 9.3) of 0.40mol/L as aluminium salt A solution with the concentration that contains 8wt%PEG2000 that 350 droplets/minute speed adds 2 times of volumes, after titration is finished, continues to stir 0.5h; Centrifugation, wash 3 times with secondary water washing, the precipitation that obtains is joined in the propyl carbinol of 80ml, after the ultrasonic dispersing, backflow 2h, distillation removes the azeotrope of 93 ℃ n-butanol-water, when the cut temperature rises to 117 ℃ of propyl carbinol boiling points, stop distillation, continue backflow 2h after, propyl carbinol is reclaimed in underpressure distillation, obtains loose powder.
880 ℃ of calcinings obtained γ-Al in 2.5 hours
2O
3Product, its particle morphology is seen Fig. 3.Particle surface is more coarse, is connected to form filamentary structure between medium hole nano particles, and particle size range is 25-75nm, and median size is 51nm; Particle internal orifice dimension scope is 2.2-9nm, and mean pore size is 5.2nm, and specific surface area is 212m
2/ g, the crystallization degree of hole wall is higher.
The Al that will contain 8wt%PEG400 under the magnetic agitation of embodiment 4:1300r/min
3+Concentration is 0.3mol/L (AlCl
3: NH
4Al (SO
4)
2=1: solution 1) is in the bicarbonate of ammonia B solution (pH is 9.3) of 0.30mol/L as aluminium salt A solution with the concentration that contains 1.4wt%PEG2000 that 300 droplets/minute speed adds 2 times of volumes, after titration is finished, continues to stir 0.5h; Centrifugation is washed 3 times, washing with alcohol 3 times with secondary water washing, and 80 ℃ of dry 4h remove surface water, obtains dry powder.The dry powder that obtains is joined in the propyl carbinol of 80ml, after the ultrasonic dispersing, backflow 2h, distillation removes 93 ℃ the azeotrope of n-butanol-water, when the cut temperature rises to 117 ℃ of propyl carbinol boiling points, stops distillation, after continuing backflow 2h, propyl carbinol is reclaimed in underpressure distillation, obtains loose powder.
900 ℃ of calcinings obtained γ-Al in 2 hours
2O
3Product, its particle morphology is seen Fig. 4, and particle distribution is more even, and particle size range is 10-50nm, and median size is 20nm; Particle internal orifice dimension scope is 2-7nm, and mean pore size is 2.8nm, and specific surface area is 132m
2/ g, the crystallization degree of hole wall is higher.。
The Al that will contain 7wt%PEG400 under the magnetic agitation of embodiment 5:1300r/min
3+Concentration is 0.4mol/L (AlCl
3: NH
4Al (SO
4)
2=1: 3) solution is in the bicarbonate of ammonia B solution (pH is 9.3) of 0.30mol/L as aluminium salt A solution with the concentration that 300 droplets/minute speed adds isopyknic 5.2wt%PEG2000 of containing, and after titration is finished, continues to stir 0.5h; Centrifugation, wash 3 times with secondary water washing, the precipitation that obtains is joined in the propyl carbinol of 80ml, after the ultrasonic dispersing, backflow 2h, distillation removes the azeotrope of 93 ℃ n-butanol-water, when the cut temperature rises to 117 ℃ of propyl carbinol boiling points, stop distillation, continue backflow 2h after, propyl carbinol is reclaimed in underpressure distillation, obtains loose powder.
900 ℃ of calcinings obtained γ-Al in 2 hours
2O
3Product, its particle morphology is seen Fig. 5.Particle surface is more coarse, and particle size range is 10-75nm, and median size is 25nm; Particle internal orifice dimension scope is 2-18nm, and mean pore size is 7.4nm, and specific surface area is 96m
2/ g, the crystallization degree of hole wall is higher.
Find by embodiment and a large amount of experiment, particle size and pore size and distribution thereof and surfactant concentrations and the polymerization degree and relevant with the composition and the concentration of inorganic salt can be selected polyglycol surfactants and aluminium salt or its mixture of the different ratios and the polymerization degree as required for use.In certain scope (as: poly(oxyethylene glycol) 400 concentration 4-8wt%, the concentration 1-8wt% of Macrogol 2000), the concentration of PEG is big more, and particle size is more little, aperture and specific surface area are big more.900 ℃ of calcinings obtain γ-Al
2O
3The main diffraction peak of X-ray powder diffraction pattern of nano-powder is: 46.0 ° (100), 67.1 ° (90), 37.0 ° 60), 49.0 ° (58), 39.7 ° (53) are γ-Al
2O
3Characteristic peak, and do not find the characteristic diffraction peak of any other type body, specific surface area is along with aluminium salt and PEG concentration, the kind 95-212m that do not coexist
2Change in/g the scope.Specific surface area, crystallization degree, particle size are relevant with the setting of warm area, along with the rising of calcining temperature, can obtain specific surface area and reduce gradually, the nano-powder that crystallization degree, crystal grain and particle size increase gradually.1000 ℃ of calcinings are after 2 hours, and principal crystalline phase still is γ-Al
2O
3
Claims (4)
1, a kind of preparation method with gama-alumina nano-powder of intraparticle mesoporous structure is characterized in that comprising following concrete steps:
(1), takes by weighing exsiccated ammonium alum, aluminum chloride and bicarbonate of ammonia as required, be dissolved in respectively in the secondary water, be made into the liquor alumini chloridi that the aluminum ion total concn is 0.3-0.5mol/L or the mixing solutions of exsiccated ammonium alum and aluminum chloride, the molar ratio range of exsiccated ammonium alum/aluminum chloride is 0-3 in the mixing solutions, and concentration is the ammonium bicarbonate soln of 0.3-0.6mol/L, with the impurity in the microporous membrane elimination solution;
(2), in the mixing solutions of liquor alumini chloridi or exsiccated ammonium alum and aluminum chloride, add poly(oxyethylene glycol) 400, be mixed with the Al that contains the 4-8wt% poly(oxyethylene glycol) 400
3+Concentration is the aluminium salt A solution of 0.3-0.5mol/L, adds Macrogol 2000 in ammonium bicarbonate soln, is made into the bicarbonate of ammonia B solution of the 0.3-0.6mol/L that contains the 1-8wt% Macrogol 2000, and adding ammoniacal liquor is regulated its pH value to 9-10;
(3), under magnetic agitation, in bicarbonate of ammonia B solution, drip 1/2 volume to isopyknic aluminium salt A solution, after titration is finished, continue to be stirred to and react completely, the centrifugation precipitation is washed to detecting no SO with secondary water washing
4 2-, the dry then dry powder that obtains;
(4), the dry powder that obtains is joined in the propyl carbinol of capacity, after the ultrasonic dispersing, fully reflux, distillation removes the azeotrope of 93-95 ℃ n-butanol-water, when the cut temperature rises to 115-120 ℃ of propyl carbinol boiling point, stop distillation, continue to reflux, propyl carbinol is reclaimed in underpressure distillation then, obtains loose γ-Al
2O
3Nano-powder;
(5), with the γ-Al that obtains
2O
3Nano-powder is at 850-900 ℃ of calcining, the γ-Al that obtains having the intraparticle mesoporous structure
2O
3Nanometer powder.
2, the preparation method with gama-alumina nano-powder of intraparticle mesoporous structure according to claim 1 is characterized in that: in step (1), and the impurity in each solution that is disposed with the microporous membrane elimination at last.
3, the preparation method with gama-alumina nano-powder of intraparticle mesoporous structure according to claim 1, it is characterized in that: dripping with 250-350 under the magnetic agitation of 1000-1300r/min in the step (3)/minute speed in bicarbonate of ammonia B solution, drip 1/2 volume to isopyknic aluminium salt A solution, and the precipitation of centrifugation washed with secondary water washing, detect to there not being SO with the 1-2% nitrate of baryta
4 2-, and then back for several times with washing with alcohol in 70-90 ℃ of dry 3-4 hour acquisition dry powder.
4, the preparation method with gama-alumina nano-powder of intraparticle mesoporous structure according to claim 1 is characterized in that: calcination time is 2-3 hour in the step (5), the γ-Al with intraparticle mesoporous structure that is obtained
2O
3The size distribution of nanometer powder is even, and median size is at 20-63nm in the particle, and the averaged particles internal orifice dimension is that specific surface area is at 95-212m at 2.8-7.4nm
2Local adjustable in the/g scope.
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| CN101412527B (en) * | 2008-05-19 | 2011-03-23 | 中国计量学院 | Preparation of pore diameter adjustable mesoporous powdered alumina |
| CN102616820A (en) * | 2012-04-24 | 2012-08-01 | 上海大学 | Method for preparing mesoporous gamma-Al2O3 nano material with high specific surface area at low temperature |
| CN101774534B (en) * | 2009-11-04 | 2012-10-31 | 中国科学院上海硅酸盐研究所 | B2O3/Al2O3 composite powder with double-pore-canal nano-pore structure and preparation method thereof |
| CN103395809A (en) * | 2013-07-23 | 2013-11-20 | 浙江万里学院 | Method for synthesizing nanometer gama-Al2O3 by adopting solvent replacement/azeotropic distillation drying method and applications thereof |
| EP2550235A4 (en) * | 2010-03-22 | 2015-06-17 | Univ Brigham Young | Method for making highly porous, stable metal oxide with a controlled pore structure |
| CN104843753A (en) * | 2015-05-22 | 2015-08-19 | 鸿福晶体科技(安徽)有限公司 | Method for preparing porous spherical high-purity alumina powder |
| US9114378B2 (en) | 2012-03-26 | 2015-08-25 | Brigham Young University | Iron and cobalt based fischer-tropsch pre-catalysts and catalysts |
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| CN107155324A (en) * | 2014-06-13 | 2017-09-12 | Ifp 新能源公司 | Amorphous mesoporous aluminas of distribution of pores with optimization and preparation method thereof |
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| CN101412527B (en) * | 2008-05-19 | 2011-03-23 | 中国计量学院 | Preparation of pore diameter adjustable mesoporous powdered alumina |
| CN101774534B (en) * | 2009-11-04 | 2012-10-31 | 中国科学院上海硅酸盐研究所 | B2O3/Al2O3 composite powder with double-pore-canal nano-pore structure and preparation method thereof |
| EP2550235A4 (en) * | 2010-03-22 | 2015-06-17 | Univ Brigham Young | Method for making highly porous, stable metal oxide with a controlled pore structure |
| US9334173B2 (en) | 2010-03-22 | 2016-05-10 | Brigham Young University | Method for making highly porous, stable metal oxides with a controlled pore structure |
| US9114378B2 (en) | 2012-03-26 | 2015-08-25 | Brigham Young University | Iron and cobalt based fischer-tropsch pre-catalysts and catalysts |
| CN102616820A (en) * | 2012-04-24 | 2012-08-01 | 上海大学 | Method for preparing mesoporous gamma-Al2O3 nano material with high specific surface area at low temperature |
| US9289750B2 (en) | 2013-03-09 | 2016-03-22 | Brigham Young University | Method of making highly porous, stable aluminum oxides doped with silicon |
| CN103395809A (en) * | 2013-07-23 | 2013-11-20 | 浙江万里学院 | Method for synthesizing nanometer gama-Al2O3 by adopting solvent replacement/azeotropic distillation drying method and applications thereof |
| CN103395809B (en) * | 2013-07-23 | 2017-03-01 | 宁波江东晟创工业产品设计有限公司 | One kind is using solvent displacement/azeotropic point distillation seasoning synthesis nanometer γ Al2O3Method and its application |
| CN107155324A (en) * | 2014-06-13 | 2017-09-12 | Ifp 新能源公司 | Amorphous mesoporous aluminas of distribution of pores with optimization and preparation method thereof |
| CN104843753A (en) * | 2015-05-22 | 2015-08-19 | 鸿福晶体科技(安徽)有限公司 | Method for preparing porous spherical high-purity alumina powder |
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