Flexible metal hydroxide nanofiber material as well as preparation method and application thereof

Abstract

The invention relates to a flexible metal hydroxide nanofiber material and a preparation method and application thereof.The preparation method of the flexible metal hydroxide nanofiber material comprises the following steps that 1, an inorganic precursor is dissolved in a solvent, then a coordination protective agent is added, and ligand protection type low-branching-degree linear inorganic sol is obtained through sufficient stirring; 2) controlling hydrolysis and polycondensation of the inorganic precursor to prepare linear inorganic spinning sol with high polymerization degree and low branching degree; (3) preparing gel nanofibers from the linear inorganic spinning sol by adopting a temperature / alkali steam assisted spinning process; and 4) carrying out ultrasonic-assisted aqueous alkali treatment on the gel nanofiber, and then cleaning and drying the gel nanofiber. Compared with the prior art, the material disclosed by the invention consists of a large number of nanofibers with nanoscale diameters and a length-diameter ratio of more than 1000, has the advantages of large specific surface area, rich and adjustable pore structure, multiple active sites, capability of being independently used, simplicity and convenience in recovery after use and the like, and greatly widens the application field of the metal hydroxide material.

Description

technical field

[0001] The invention belongs to the technical field of metal hydroxide materials, and relates to a flexible metal hydroxide nanofiber material and a preparation method and application thereof. Background technique

[0002] Metal hydroxides are a series of compounds with metal ions as cations and hydroxide ions as anions, mainly including zirconium hydroxide, aluminum hydroxide, magnesium hydroxide, lanthanum hydroxide, titanium hydroxide, etc., in daily production and life It is widely used in the field of photoelectric energy, catalytic degradation, adsorption and separation and other fields. At present, researchers have used various techniques to prepare metal hydroxide particles, metal hydroxide rods, metal hydroxide wires and other dispersed materials. Although they have a large specific surface area, due to their dispersed form, they require Composite with other materials, it is easy to lose powder and difficult to recycle; while the hydroxide sheet has...

Examples

preparation example Construction

[0032] The invention provides a method for preparing a flexible metal hydroxide nanofiber material, comprising the following steps:

[0033] 1) Dissolving the inorganic precursor in a solvent, then adding a coordination protective agent, and stirring thoroughly to obtain a ligand-protected linear inorganic sol with low branching degree;

[0034] 2) Control the hydrolysis and polycondensation of the inorganic precursor to prepare a linear inorganic spinning sol with a high degree of polymerization and a low degree of branching;

[0035] 3) Using a temperature / alkali steam-assisted spinning process, the linear inorganic spinning sol is prepared into gel nanofibers;

[0036] 4) The gel nanofibers are treated with an ultrasonic-assisted alkaline solution to complete an alcoholysis reaction with a high degree of hydroxyl substitution, and then cleaned and dried to obtain a flexible metal hydroxide nanofiber material.

[0037] In step 1), the inorganic precursor includes zirconium ...

Embodiment 1

[0044] Dissolve 12wt% zirconium n-propoxide into a mixed solvent of n-propanol and ethanol (the solvent mass ratio is 1:1), the stirring rate is 500rpm, and the stirring temperature is 26°C. After fully stirring, add acetylacetone 8wt, a coordination protection agent %, and then stirred at room temperature for 8 hours to obtain a homogeneous multidentate ligand-protected inorganic sol. The sol was passed through a low-branched inorganic polymer sol spinning solution batch preparation device to control the hydrolysis and polycondensation of the inorganic precursor, and the polycondensation negative The pressure was controlled at 0.1MPa, the reaction temperature was 60°C, and the polycondensation time was 3h. Finally, a linear inorganic spinning sol with a degree of polymerization of 6500 and a degree of branching of ~0.05 was obtained, with a viscosity of 1800mpa·s.

[0045] Put the high degree of polymerization and low degree of branching linear inorganic spinning sol prepared ...

Embodiment 2

[0049] Dissolve 13wt% aluminum n-propoxide into n-propanol with a stirring rate of 500rpm and a stirring temperature of 26°C. After fully stirring, add 11wt% of coordination protective agent acetylacetone, and then stir at room temperature for 8 hours to obtain a homogeneous multi-dentate complex. Body-protected inorganic sol, the sol is passed through a low-branched inorganic polymer sol spinning solution batch preparation device to control the hydrolysis and polycondensation of the inorganic precursor, the polycondensation negative pressure is controlled at 0.1MPa, the reaction temperature is 60 ° C, the polycondensation time After 3 hours, a linear inorganic spinning sol with a degree of polymerization of 8200 and a degree of branching of ~0.05 was finally obtained, with a viscosity of 2400 mpa·s.

[0050] Put the high degree of polymerization and low branching linear inorganic spinning sol prepared above into the slit nozzle, and apply 25kV high voltage to the tip, control ...

technical field

[0001] The invention belongs to the technical field of metal hydroxide materials, and relates to a flexible metal hydroxide nanofiber material and a preparation method and application thereof. Background technique

[0002] Metal hydroxides are a series of compounds with metal ions as cations and hydroxide ions as anions, mainly including zirconium hydroxide, aluminum hydroxide, magnesium hydroxide, lanthanum hydroxide, titanium hydroxide, etc., in daily production and life It is widely used in the field of photoelectric energy, catalytic degradation, adsorption and separation and other fields. At present, researchers have used various techniques to prepare metal hydroxide particles, metal hydroxide rods, metal hydroxide wires and other dispersed materials. Although they have a large specific surface area, due to their dispersed form, they require Composite with other materials, it is easy to lose powder and difficult to recycle; while the hydroxide sheet has...

Examples

preparation example Construction

[0032] The invention provides a method for preparing a flexible metal hydroxide nanofiber material, comprising the following steps:

[0033] 1) Dissolving the inorganic precursor in a solvent, then adding a coordination protective agent, and stirring thoroughly to obtain a ligand-protected linear inorganic sol with low branching degree;

[0034] 2) Control the hydrolysis and polycondensation of the inorganic precursor to prepare a linear inorganic spinning sol with a high degree of polymerization and a low degree of branching;

[0035] 3) Using a temperature / alkali steam-assisted spinning process, the linear inorganic spinning sol is prepared into gel nanofibers;

[0036] 4) The gel nanofibers are treated with an ultrasonic-assisted alkaline solution to complete an alcoholysis reaction with a high degree of hydroxyl substitution, and then cleaned and dried to obtain a flexible metal hydroxide nanofiber material.

[0037] In step 1), the inorganic precursor includes zirconium ...

Embodiment 1

[0044] Dissolve 12wt% zirconium n-propoxide into a mixed solvent of n-propanol and ethanol (the solvent mass ratio is 1:1), the stirring rate is 500rpm, and the stirring temperature is 26°C. After fully stirring, add acetylacetone 8wt, a coordination protection agent %, and then stirred at room temperature for 8 hours to obtain a homogeneous multidentate ligand-protected inorganic sol. The sol was passed through a low-branched inorganic polymer sol spinning solution batch preparation device to control the hydrolysis and polycondensation of the inorganic precursor, and the polycondensation negative The pressure was controlled at 0.1MPa, the reaction temperature was 60°C, and the polycondensation time was 3h. Finally, a linear inorganic spinning sol with a degree of polymerization of 6500 and a degree of branching of ~0.05 was obtained, with a viscosity of 1800mpa·s.

[0045] Put the high degree of polymerization and low degree of branching linear inorganic spinning sol prepared ...

Embodiment 2

[0049] Dissolve 13wt% aluminum n-propoxide into n-propanol with a stirring rate of 500rpm and a stirring temperature of 26°C. After fully stirring, add 11wt% of coordination protective agent acetylacetone, and then stir at room temperature for 8 hours to obtain a homogeneous multi-dentate complex. Body-protected inorganic sol, the sol is passed through a low-branched inorganic polymer sol spinning solution batch preparation device to control the hydrolysis and polycondensation of the inorganic precursor, the polycondensation negative pressure is controlled at 0.1MPa, the reaction temperature is 60 ° C, the polycondensation time After 3 hours, a linear inorganic spinning sol with a degree of polymerization of 8200 and a degree of branching of ~0.05 was finally obtained, with a viscosity of 2400 mpa·s.

[0050] Put the high degree of polymerization and low branching linear inorganic spinning sol prepared above into the slit nozzle, and apply 25kV high voltage to the tip, control ...

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