Tubular and tube-in-tube structure organic oxide and preparation method thereof

An inorganic oxide, tube-in-tube technology, which is applied in the fields of inorganic raw material rayon, textiles and papermaking, fiber processing, etc., can solve the problems of difficult control, complicated device, unable to build fibers, etc., achieves simple operation and overcomes complex structure. , Universal effect

Inactive Publication Date: 2009-09-30
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although metal oxide nanotubes can be formed by this method, the device is relatively complicated and difficult to control, and only tubular fibers can be prepared, and fibers with a tube-in-tube structure cannot be constructed.
Theoretically, by improving the electrospinning device and adding one or more coaxial needles, the synthesis of tube-in-tube fibers can be achieved, but this device is more complicated and less controllable
So far, the synthesis of tube-in-tube fibers of metal oxides has rarely been reported, and only one case is a tube-in-tube of ferric oxide prepared by hydrothermal synthesis, while TiO 2 , SiO 2 , ZrO 2 A series of tube-in-tube structures have not been reported so far, so the synthesis of metal oxides with tube-in-tube structures is a challenging subject

Method used

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  • Tubular and tube-in-tube structure organic oxide and preparation method thereof
  • Tubular and tube-in-tube structure organic oxide and preparation method thereof
  • Tubular and tube-in-tube structure organic oxide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Weigh 2.5g of PVP-K30 (molecular weight 25000-40000) and dissolve it in 5ml of ethanol to form a transparent and uniform solution, then add 0.5ml of acetic acid to it, stir uniformly and add 1.5ml of butyl titanate (the amount of butyl titanate is A relatively good TiO can be formed between 0.5-4ml 2 Tube-in-tube), mix evenly to form a transparent electrospinning solution with a certain viscosity, and then put it into a 10ml glass syringe, the needle used is a No. 15cm, the advancing speed of the syringe pump is 0.3ml / min, the ambient temperature is 10°C, and the relative humidity is lower than 50%. Calcined at 700°C for 5 hours to obtain TiO 2 Tube in tube. figure 1 is TiO 2 XRD pattern of tube-in-tube, figure 2 a is a large-area scan image, figure 2 b is a high-magnification scan image, image 3 a is a transmission electron microscope image at low magnification, image 3 b is the tube-in-tube transmission picture alone, from figure 2 and image 3 It can be...

Embodiment 2

[0040] Weigh 2.5g of PVP-K30 (molecular weight 25,000-40,000) and dissolve it in 3ml of ethanol to form a transparent and uniform solution, then add 1ml of acetic acid to it, stir uniformly and add 6ml of butyl titanate (the amount of butyl titanate should be more than 4ml The formation is basically TiO 2 Porous fiber), mixed evenly to form a transparent electrospinning solution with a certain viscosity, and then put it into a 10ml glass syringe, the needle used is No. 15cm, the propulsion speed of the syringe pump is 0.1ml / min, the ambient temperature is 0°C, and the relative humidity is 35%. After the electrospinning, the fiber is removed and placed in a tube furnace to raise the temperature to 500°C at a rate of 2°C / min. Calcined for 10 hours to get TiO 2 Solid porous fiber. from Figure 4 It can be seen that the prepared TiO 2 Most of them are porous fibers with a relatively uniform diameter between 350 and 450 nm.

Embodiment 3

[0042] Weigh 2.5g of PVP-K30 (molecular weight 25,000-40,000) and dissolve it in 5ml of ethanol to form a transparent and uniform solution, then add 0.5ml of acetic acid to it, stir uniformly and add 0.3ml of butyl titanate (the amount of butyl titanate is TiO is basically formed below 0.5ml 2 single tube), mix evenly to form a transparent electrospinning solution with a certain viscosity, and then put it into a 10ml glass syringe, the needle used is a No. 15cm, the advancing speed of the syringe pump is 0.3ml / min, the ambient temperature is 20°C, and the relative humidity is lower than 35%. Calcined at 500°C for 2 hours to obtain TiO 2 hollow fiber. from Figure 5 It can be seen that the prepared TiO 2 Most of them are single tubes, and there are a small number of tubes with very thin nanowires. The diameter of the tubes is relatively uniform, between 300 and 400nm.

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Abstract

The invention discloses a tubular and tube-in-tube structure organic oxide and a preparation method thereof. The organic oxide has a caliber from 100 nanometers to 1 micron and a tube wall of a porous structure. The preparation method utilizes various organic salts and comprises the following steps: using metal alkoxide and nitrate as raw materials; fully mixing salt solutions with an alcoholic solution of PVP to be electrically spun into fibers under a high-pressure electrostatic field; and treating the fibers at a high temperature to form the tubular and tube-in-tube structure organic oxide. The method is used to prepare the tubular and tube-in-tube structure organic oxide comprising Ti, Si, Zr, V, In, Sn, B, Fe and Co. The invention adopts a traditional single-tube nozzle electrostatic spinning technology to prepare a tubular and tube-in-tube nanometer material, is different from a traditional hydrothermal method, an electrochemic method and a coaxial nozzle electric spinning method for preparing organic tubes, only needs the simplest electric spinning process and the roasting process, has convenient and rapid operation, simple method, novel product structure and strong universality and is suitable for mass production.

Description

technical field [0001] The invention relates to an inorganic oxide, in particular to a tubular inorganic oxide with a tube-in-tube structure and a method for preparing the inorganic tubular and tube-in-tube structure by electrospinning with a traditional single-tube nozzle. Background technique [0002] One-dimensional nanomaterials have attracted extensive attention in recent years due to their potential applications in sensing, catalysis, optics, and electronic devices. The morphology of one-dimensional nanomaterials has a great influence on its properties, and the control of the morphology has become the focus of attention. Metal oxide nanotubes have aroused great interest of scientists due to their excellent electrochemical, photoelectric conversion and photocatalytic properties. Some synthetic methods have been established, such as using layered materials as Thermal preparation, electrodeposition, electrochemical etching, and electrospinning techniques, etc. Electrosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/08D01D5/00
Inventor 徐正郎雷鸣李保军刘威朱国兴
Owner NANJING UNIV
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