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A three-dimensional ordered macroporous-mesoporous metal oxide or composite oxide gas phase infiltration-precipitation preparation method and the resulting product

A composite oxide, three-dimensional ordered technology, applied in the field of synthesis of nano-micro functional materials, can solve the problems of easy collapse of macroporous structure, and achieve the effects of reducing environmental hazards, simple structure, and cheap and easy-to-obtain raw materials

Active Publication Date: 2015-08-12
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since there is no solidification treatment during the synthesis process, the macroporous structure is relatively easy to collapse. Many three-dimensional ordered macroporous-mesoporous metal oxides and composite oxides, such as cerium-titanium composite oxides, dichromium trioxide, tricobalt tetroxide, and lanthanum oxide , zinc oxide, etc. are difficult to synthesize by this method

Method used

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  • A three-dimensional ordered macroporous-mesoporous metal oxide or composite oxide gas phase infiltration-precipitation preparation method and the resulting product
  • A three-dimensional ordered macroporous-mesoporous metal oxide or composite oxide gas phase infiltration-precipitation preparation method and the resulting product
  • A three-dimensional ordered macroporous-mesoporous metal oxide or composite oxide gas phase infiltration-precipitation preparation method and the resulting product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] At normal temperature and pressure, 0.7237 g Ce(NO 3 ) 3 ·6H 2 O, 1.9999 g Ti(SO 4 ) 2 , 2.1014 g citric acid and 1 g P123 dissolved in 10 g H 2 O, after mixing evenly, 5 g PMMA was added to the above solution, after soaking for 3 h, the excess precursor solution was removed by vacuum filtration, and the filtered sample was at 20 o C was dried for 2 h, and the dried sample was transferred to the gas phase osmosis-precipitation device, at 40 o C was reacted for 2 h, and the precipitated sample was o C and dried for 24 h, put the obtained solid into a porcelain boat and place it in a tube furnace, and use a two-step roasting method to firstly bake it with 1 o C / min rate of heating up to 300 o C and keep at this temperature for 3 h, after cooling down to room temperature, add 1 o C / min rate of heating up to 500 o C and kept at this temperature for 6 h, a three-dimensional ordered macroporous-mesoporous Ce-Ti composite oxide with a Ce / Ti molar ratio of 0.2 w...

Embodiment 2

[0059] At normal temperature and pressure, 1.9976 g Ce(NO 3 ) 3 ·6H 2 O, 3.6962 g Ti(SO 4 ) 2 , 2.1014 g citric acid and 1.5 g P123 dissolved in 10 g H 2 O, after mixing evenly, add 5 g PMMA to the above solution, soak for 3 h and completely infiltrate, then remove excess precursor solution by vacuum filtration; o C for 2 h, the dried sample was transferred to the gas phase osmosis-precipitation device, at 50 o C was reacted for 3 h, and the sample after precipitation was o C and dried for 24 h, put the obtained solid into a porcelain boat and put it in a tube furnace, and adopt a one-step roasting method in the air atmosphere (50 mL / min) at 1 o C / min rate of heating up to 300 o C and keep at this temperature for 3 h, then continue with 1 o C / min rate of heating up to 550 o C and kept at this temperature for 6 h, a three-dimensional ordered macroporous-mesoporous Ce-Ti composite oxide with a Ce / Ti molar ratio of 0.3 was prepared, and its TEM image is shown in i...

Embodiment 3

[0061] The operation is the same as in Example 2, except that ammonia water (25-28 wt%) is added dropwise to the dried sample to precipitate the metal salt between the templates, and the excess ammonia water is removed by filtration, and the obtained product is dried again, and the two-step roasting method is adopted. A composite oxide with a Ce / Ti molar ratio of 0.3 is obtained, and its SEM image is shown in Figure 4 It can be seen from the SEM image that although the structured Ce-Ti composite oxide has a macroporous structure, the order of the pore structure is poor, and some macroporous structures collapse, resulting in many granular products. Therefore, the Ce-Ti composite oxide prepared by using ammonia water as a curing agent does not have a large-scale three-dimensional ordered macroporous structure.

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Abstract

The invention discloses a preparation method of a three-dimensionally ordered macroporous-mesoporous metal oxide or composite oxide by using the gas phase permeability-precipitation technology, and a product obtained. The method comprises the following steps: dissolving metal soluble salt or a mixture of metal soluble salt, citric acid, and P123 in water to obtain a predecessor mixed solution; dipping a colloidal crystal template in the predecessor mixed solution, removing the superfluous solution after being completely dipped, and drying the sample; placing the dried sample in gas ammonia atmosphere to conduct curing on metal salts permeating into gaps of the colloid crystal template; drying the cured sample, and roasting to obtain the product. The method is simple in technology and convenient to operate, uses ammonia gas as a curing agent to avoid the collapse of pore structures and generation of massive by-products caused by the precipitation reaction in the solution, and obviously improves the productivity of a three-dimensionally ordered macroporous-mesoporous material; besides, water is used as a solvent, an organic solvent and an organic curing agent are not used, and the raw material is cheap and easy to obtain, so that the cost is low.

Description

technical field [0001] The present invention relates to a preparation method of a material with a three-dimensional ordered multi-level pore structure and the resulting product, especially a gas phase infiltration-precipitation preparation method of a three-dimensional ordered macroporous-mesoporous metal oxide and a composite oxide and the resulting product, The invention belongs to the technical field of synthesis of nano-micron functional materials. Background technique [0002] With its unique pore structure and excellent surface properties, three-dimensional macroporous materials have broad application prospects in the fields of catalysis, photonic crystals, adsorption and separation. The large pore channel structure is conducive to the entry of substances into the pores from all directions, reduces the diffusion resistance of substances, and provides the best flow rate and higher efficiency for the diffusion of substances. However, simple macroporous materials general...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B13/14
Inventor 张昭良辛颖蒋品于明强李倩
Owner UNIV OF JINAN
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