CN104477998B - A kind of preparation method of order mesoporous Cu-Mn complex oxide - Google Patents
A kind of preparation method of order mesoporous Cu-Mn complex oxide Download PDFInfo
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Abstract
The preparation method that the present invention relates to a kind of order mesoporous Cu-Mn complex oxide, is dissolved in alcoholic solution by copper nitrate and manganese nitrate, and metal total mol concentration is 1～2.3mol/L, and copper manganese mol ratio is 0～3, stirs；With ordered mesoporous silica dioxide for template, metal total mole number: template mole=1:1～25:16, it is placed in the bottle,suction of evacuation, upper end uses separatory funnel to seal；The solution of preparation is placed in separatory funnel, is slowly dropped in template under vacuum state, after dripping off, keep vacuum state 0.5～1 hour；Roasting in vacuum impregnation, vacuum drying, Muffle furnace is adopted namely to obtain the national standard method of ordered mesopore structure。It is low, simple to operate that the inventive method has cost, the advantage such as prepared Cu-Mn complex oxide pore structure high-sequential, pore-size distribution are narrow。
Description
Technical field
The invention belongs to solid mesoporous material preparing technical field, be specifically related to a kind of method preparing order mesoporous Cu-Mn complex oxide for hard template method with ordered mesoporous silicon。
Background technology
Cu-Mn complex oxide is the material that a class has significant application value, because it has the crystal structure of uniqueness, electromagnetic property and higher oxidation, reducing power, it is widely used in above canister, filter type self-rescuer, fire mask, life saving mask, oxidation tank etc.。Compared to non-hole Cu-Mn complex oxide, it is big that the violent oxide of mesoporous copper has pore passage structure prosperity, specific surface area and pore volume, and therefore performance is more superior, and purposes is more extensive。
But, the preparation traditional preparation method of many employings of current Cu-Mn complex oxide includes the methods such as coprecipitation, step-by-step precipitation method, infusion process and sol-gal process and prepares, and prepared Cu-Mn complex oxide is non-pore structure, and specific surface area is less。Only having the synthesis of mesoporous national standard method of little bibliographical information, it adopts oxide-reduction method, prepares the violent composite oxides structure of copper for without ordered meso-porous structure。Although above-mentioned preparation method is fairly simple, but the performance such as catalytic stability of the violent composite oxides of prepared copper etc. are poor, and performance can not get a promotion further。
Summary of the invention
Present invention aim to address the problems of the prior art, it is provided that the synthetic method of the order mesoporous Cu-Mn complex oxide that a kind of pore passage structure is flourishing。
The preparation method of a kind of order mesoporous Cu-Mn complex oxide, it is characterised in that comprise the steps:
(1) being dissolved in alcoholic solution by copper nitrate and manganese nitrate, metal total mol concentration is 1～2.3mol/L, and copper manganese mol ratio is 0～3, stirs standby；
(2) with ordered mesoporous silica dioxide for template, metal total mole number: template mole=1:1～25:16, it is placed in the bottle,suction of evacuation, continues evacuation 1 hour, upper end uses separatory funnel to seal；
(3) solution that step (1) is prepared is placed in separatory funnel, is slowly dropped in the template in step (2) under vacuum state, after dripping off, keep vacuum state 0.5～1 hour；
(4) solution of bottle,suction in step (3) is transferred in crystallizing dish, is placed in 50 DEG C of vacuum drying ovens dry；
(5) product that step (4) obtained grinds, and is placed in Muffle furnace roasting, is warming up to 300 DEG C with 1 DEG C/min, and keeps 2 hours；
(6) product that step (5) obtains is placed in the beaker of the sodium hydroxide filling 2moL/L, repeatedly stirs in a water bath, sucking filtration, through oven drying after, obtain the national standard method of ordered mesopore structure。
Step (4) described drying time is 2 days。
The described bath temperature of step (6) 40 DEG C, oven drying temperature is 100 DEG C。
Ordered mesopore structure has that porosity is big, pore passage structure in order and the advantage such as high-specific surface area and pore volume, therefore, the violent composite oxides of copper preparing ordered mesopore structure can be widened further and improve its performance, have very important significance。It is low, simple to operate that the inventive method has cost, the advantage such as prepared Cu-Mn complex oxide pore structure high-sequential, pore-size distribution are narrow。
The present invention discloses the preparation of ordered mesopore structure Cu-Mn complex oxide first, up to now, without the synthesis of pertinent literature and patent report ordered mesopore structure Cu-Mn complex oxide。
Accompanying drawing explanation
Fig. 1 is the XRD figure of embodiment 1～3。
Fig. 2 is TEM figure, Fig. 3 of embodiment 1 is the TEM figure of embodiment 2。
Detailed description of the invention
Embodiment 1:
Reference literature [R.Ryooetal., ChemCommun., (2003) 2136] synthesis KIT-6。Weigh 1gKIT-6 and be placed in bottle,suction, use the plug seal bottle,suction with separatory funnel, separatory funnel is gone to sealing state, is evacuated to vacuum and reaches 0.1Mpa, and keep this vacuum 1h。
Weigh 3.02g copper nitrate (Cu (NO3)2·3H2O) and the manganese nitrate solution of 4.47g50% be dissolved in 15mL dehydrated alcohol, stirring to dissolve。This solution is transferred in above-mentioned separatory funnel, rotates piston, slowly instill in KIT-6, after dripping off to solution, continue evacuation 0.45h, be transferred in crystallizing dish。Crystallizing dish is placed in 50 DEG C of vacuum drying ovens and continues dry 2 days。Take out sample, grinding is sieved, sample is placed in crucible, rise to 300 DEG C with the speed of 1 DEG C/min, and keep 2h at such a temperature, gained sample is placed in the beaker of the NaOH filling 2moL/L, 40 DEG C of water-baths are stirred repeatedly, sucking filtration, through 100 DEG C of oven dryings after, obtains the national standard method of three-dimensional ordered mesoporous structure。
Embodiment 2:
Reference literature [R.M.Grudzienetal., Appli.Surf.Sci., 253 (2007) 5660] synthesis SBA-16。Weigh 1gSBA-16 and be placed in bottle,suction, use the plug seal bottle,suction with separatory funnel, separatory funnel is gone to sealing state, is evacuated to vacuum and reaches 0.1Mpa, and keep this vacuum 1h。
Weigh 3.02g copper nitrate (Cu (NO3)2·3H2O) and the manganese nitrate solution of 4.47g50% be dissolved in 15mL dehydrated alcohol, stirring to dissolve。This solution is transferred in above-mentioned separatory funnel, rotates piston, slowly instill in KIT-6, after dripping off to solution, continue evacuation 0.5h, be transferred in crystallizing dish。Crystallizing dish is placed in 50 DEG C of vacuum drying ovens and continues dry 2 days。Take out sample, grinding is sieved, sample is placed in crucible, rise to 300 DEG C with the speed of 1 DEG C/min, and keep 2h at such a temperature, gained sample is placed in the beaker of the NaOH filling 2moL/L, 40 DEG C of water-baths are stirred repeatedly, sucking filtration, through 100 DEG C of oven dryings after, obtains the national standard method of three-dimensional ordered mesoporous structure。
Embodiment 3:
Reference literature [ZhaoDYetal., Science , 279 (1998) 548] and synthesis SBA-15。Weigh 1gSBA-15 and be placed in bottle,suction, use the plug seal bottle,suction with separatory funnel, separatory funnel is gone to sealing state, is evacuated to vacuum and reaches 0.1MPa, and keep this vacuum 1h。
Weigh 3.02g copper nitrate (Cu (NO3)2·3H2O) and the manganese nitrate solution of 4.47g50% be dissolved in 15mL dehydrated alcohol, stirring to dissolve。This solution is transferred in above-mentioned separatory funnel, rotates piston, slowly instill in KIT-6, after dripping off to solution, continue evacuation 1h, be transferred in crystallizing dish。Crystallizing dish is placed in 50 DEG C of vacuum drying ovens and continues dry 2 days。Take out sample, grinding is sieved, sample is placed in crucible, rise to 300 DEG C with the speed of 1 DEG C/min, and keep 2h at such a temperature, gained sample is placed in the beaker of the NaOH filling 2moL/L, 40 DEG C of water-baths are stirred repeatedly, sucking filtration, through 100 DEG C of oven dryings after, obtains the national standard method of ordered mesopore structure。
Claims (1)
1. the preparation method of an order mesoporous Cu-Mn complex oxide, it is characterised in that comprise the steps:
(1) being dissolved in alcoholic solution by copper nitrate and manganese nitrate, metal total mol concentration is 1～2.3mol/L, and copper manganese mol ratio is0～3, stir standby；
(2) with ordered mesoporous silica dioxide for template, metal total mole number: template mole=1:1～25:16, it is placed in the bottle,suction of evacuation, continues evacuation 1 hour, upper end uses separatory funnel to seal；
(3) solution that step (1) is prepared is placed in separatory funnel, is slowly dropped in the template in step (2) under vacuum state, after dripping off, keep vacuum state 0.5～1 hour；
(4) solution of bottle,suction in step (3) is transferred in crystallizing dish, is placed in 50 DEG C of vacuum drying ovens dry；
(5) product that step (4) obtained grinds, and is placed in Muffle furnace roasting, is warming up to 300 DEG C with 1 DEG C/min, and keeps 2 hours；
(6) product that step (5) obtains is placed in the beaker of the sodium hydroxide filling 2mol/L, repeatedly stirs in a water bath, sucking filtration, through oven drying after, obtain the national standard method of ordered mesopore structure；
Step (4) described drying time is 2 days；
The described bath temperature of step (6) 40 DEG C, oven drying temperature is 100 DEG C。
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| RU2763063C1 (en) * | 2020-08-12 | 2021-12-27 | Общество с ограниченной ответственностью "ТЕХНОХИМ" | Functional filler for a fire extinguishing powder composition |
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| CN105289642A (en) * | 2015-10-30 | 2016-02-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing copper-manganese composite oxide of porous structure |
| CN112916016B (en) * | 2021-01-26 | 2022-10-21 | 成都科特瑞兴科技有限公司 | Mesoporous composite copper catalyst for preparing carbon monoxide from methanol and preparation method and application thereof |
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| CN101391753A (en) * | 2008-11-05 | 2009-03-25 | 中国科学院上海硅酸盐研究所 | Method for preparing mesoporous metallic oxide material |
| CN101514001A (en) * | 2009-03-10 | 2009-08-26 | 中国科学院上海硅酸盐研究所 | Bar-shaped ordered mesopore silicon dioxide nano material and preparation method thereof |
| CN102240570A (en) * | 2010-05-11 | 2011-11-16 | 北京化工大学 | Catalyst with meso pore characteristics and application thereof |
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| JPH10139417A (en) * | 1996-10-31 | 1998-05-26 | Mitsubishi Heavy Ind Ltd | Silicate of large specific surface area and its synthesis |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101391753A (en) * | 2008-11-05 | 2009-03-25 | 中国科学院上海硅酸盐研究所 | Method for preparing mesoporous metallic oxide material |
| CN101514001A (en) * | 2009-03-10 | 2009-08-26 | 中国科学院上海硅酸盐研究所 | Bar-shaped ordered mesopore silicon dioxide nano material and preparation method thereof |
| CN102240570A (en) * | 2010-05-11 | 2011-11-16 | 北京化工大学 | Catalyst with meso pore characteristics and application thereof |
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| "Facile preparation of Cu–Mn/CeO2/SBA-15 catalysts using ceria as an auxiliary for advanced oxidation processes";Jianwei Fan et al.;《J. Mater. Chem. A》;20140516;第2卷;第10654–10661页 * |
| "MCM-41 Supported Cu-Mn Catalysts for Catalytic Oxidation of Toluene at Low Temperatures";W. B. Li et al.;《J. Phys. Chem. B》;20061006;第110卷(第43期);21568-21571 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2763063C1 (en) * | 2020-08-12 | 2021-12-27 | Общество с ограниченной ответственностью "ТЕХНОХИМ" | Functional filler for a fire extinguishing powder composition |
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