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Aperture adjustable composite inorganic oxide nanopore fiber with communication pores and single-spray head electro-spinning preparation method thereof

A technology of inorganic oxides and connected pores, which is applied in fiber processing, chemical characteristics of fibers, rayon of inorganic raw materials, etc., to achieve the effect of broadening the control range, avoiding preparation conditions and reducing waste.

Inactive Publication Date: 2014-08-06
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the use of single-nozzle electrospinning technology to prepare inorganic oxide porous fibers with interconnected channels and adjustable pore size distribution without sacrificial pore formers or microemulsions has not been reported.

Method used

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  • Aperture adjustable composite inorganic oxide nanopore fiber with communication pores and single-spray head electro-spinning preparation method thereof
  • Aperture adjustable composite inorganic oxide nanopore fiber with communication pores and single-spray head electro-spinning preparation method thereof
  • Aperture adjustable composite inorganic oxide nanopore fiber with communication pores and single-spray head electro-spinning preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] Example 1: Ti / Si-1

[0086] Mesoporous TiO 2 / SiO 2 Preparation of nanofibers:

[0087] (1) Preparation of spinning solution: at a humidity of 10% RH and a temperature of 20°C, add 2g of polyvinylpyrrolidone to a mixture of 10g of absolute ethanol and 2g of glacial acetic acid, stir until clear, and then add 5.5g of titanium Acetate tetrabutyl ester and 0.5g ethyl orthosilicate, continue to stir for 1h to obtain a viscous spinning solution.

[0088] (2) Mesoporous TiO 2 / SiO 2 Fiber spinning preparation: control the flow rate to 4ml / h, inject the electrospinning solution prepared above into a syringe equipped with a stainless steel dispensing needle with an inner diameter of 1.37mm, the spinning distance is 30cm, the electrospinning humidity is 10%RH, and the temperature is Electrospinning was carried out under the spinning conditions of 20°C and a voltage of 13KV to obtain TiO 2 / SiO 2 / PVP composite fiber, and then dried in a drying oven at 60°C for 6h, put the...

Embodiment 2

[0089] Example 2: Ti / Si-2

[0090] Mesoporous-Macroporous Secondary Porous TiO 2 / SiO 2 Preparation of nanofibers:

[0091] Similar to Example 1, when adjusting the preparation and spinning, the amount of tetrabutyl titanate added is 2.5g, the amount of tetraethyl orthosilicate is 3.5g, other conditions are similar, the flow rate is controlled at 6ml / h, and the above prepared The electrospinning solution is injected into a syringe equipped with a stainless steel dispensing needle with an inner diameter of 1.55 mm, the spinning distance is 25 cm, the electrospinning humidity is 30% RH, the temperature is 24 ° C, and the electrospinning voltage is 16 KV under the spinning conditions to obtain TiO 2 / SiO 2 / PVP composite fiber, then dried in a drying oven at 30°C for 10 hours, put the dried fiber in a muffle furnace, raised the temperature to 700°C at 5°C / min, kept it warm for 6 hours, and cooled down naturally to obtain a medium Pore-Macropore Secondary Pore TiO 2 / SiO 2 C...

Embodiment 3

[0092] Example 3: Ti / Si-3

[0093] Microporous-mesoporous-macroporous tertiary TiO 2 / SiO 2 Preparation of nanofibers:

[0094] Similar to Example 1, when adjusting the preparation and spinning, the amount of tetrabutyl titanate added is 0.5g, the amount of tetraethyl orthosilicate is 5.5g, other conditions are similar, the flow rate is controlled at 8ml / h, and the above prepared The electrospinning solution was injected into a syringe equipped with a stainless steel needle with an inner diameter of 1.23 mm, the spinning distance was 30 cm, the electrospinning humidity was 30% RH, the temperature was 30 ° C, and the electrospinning voltage was 18 KV under the spinning conditions to obtain TiO 2 / SiO 2 / Dry the PVP composite fiber in a drying oven at 60°C for 8 hours, put the dried fiber in a muffle furnace, raise the temperature to 1000°C under programmed temperature control at 20°C / min, keep it warm for 10 hours, and cool down naturally to obtain micropores- Mesoporous-Ma...

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Abstract

The invention discloses an aperture adjustable composite inorganic oxide nanopore fiber with communication pores and a single-spray head electro-spinning preparation method thereof, and belongs to the technical field of preparation of inorganic oxide nanopore fibers. The composite inorganic oxide nanopore fiber is controllable in aperture distribution, pore passages are communicated with one another, and the composite inorganic oxide nanopore fiber comprises a mesoporous material, a mesoporous-macroporous material and a microporous-mesoporous-macroporous material. The method is used for preparing the target product by the single-spray head electro-spinning technology in one step based on an inorganic ester hydrolytic polycondensation spontaneous pore formation principle; in the method, a sacrifice pore-forming agent or a microemulsion is not used, and an electro-spinning device with the special design of multiple spray heads or co-axis and the like are also not used. The composite inorganic oxide nanopore fiber prepared by the method is high in controllability of apertures, high in community of pore passages, high in yield and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of composite inorganic oxide nanoporous fibers, and in particular relates to a composite inorganic oxide nanoporous fiber with interconnected holes and adjustable pore diameters and a single-nozzle electrostatic spinning preparation method thereof. Background technique [0002] According to the pore size classification, porous materials can be divided into micropores (<2nm), mesoporous (2~50nm) and macropores (>50nm). Porous materials whose main structure contains two or more pore size scales and connected channels are called hierarchical porous materials. Hierarchical porous materials include secondary porous (micropore-mesoporous and mesopore-macropore) and tertiary porous (micropore-mesopore-macropore) materials. The pore connectivity of graded porous materials makes this kind of materials have the advantages of multiple channels. [0003] Inorganic oxide nanofibers have rich and ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/08D01F11/00D01D5/00D01D5/247
Inventor 徐雁王赟高建雄赵肖娟于晴胡家博
Owner JILIN UNIV
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