Preparation method for SnO2/ZnO compound micro-nano fibers and product thereof

A kind of micro-nano fiber, a certain amount of technology, applied in the direction of fiber chemical characteristics, rayon manufacturing, textile and paper making, etc., can solve the problems of one-dimensional continuous fiber easy to break, complex synthesis process, poor stability of surface heterojunction, etc., to achieve Steady improvement of physical and chemical properties, increased stability, improved composition and effects of pyrolysis and nucleation and growth of inorganic substances

Inactive Publication Date: 2017-09-08
UNIV OF JINAN
5 Cites 17 Cited by

AI-Extracted Technical Summary

Problems solved by technology

The above synthesis process is relatively complicated, and the one-dimensional contin...
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Abstract

The invention discloses a preparation method for SnO2/ZnO compound micro-nano fibers. The preparation method comprises the following steps: firstly preparing Zif-8 by zinc salt and 2-methylimidazole; adding ammonium citrate dibasic, octadecylamine and ethyecellulose to prepare the Zif-8 solution; preparing tin salt solution by tin salt and polyvinylpyrrolidone, and slowly dropwise adding to the Zif-8 solution, to obtain precursor spinning solution, and executing the electrostatic spinning and heat treatment to obtain a final product. The body of the prepared SnO2/ZnO compound micro-nano fibers is formed by SnO2 and ZnO nano-particle combination, and the surface has the SnO2 nano-particles. According to the preparation method, a zinc-based metal organic framework material is introduced into the SnO2 micro-nano fibers, the synthetic process is simple, the reaction parameters are easily set, and the ingredients of the obtained product are adjustable. The obtained SnO2/ZnO compound micro-nano fibers have the important application value in the fields, such as air-sensitive and photocatalysis.

Application Domain

Technology Topic

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  • Preparation method for SnO2/ZnO compound micro-nano fibers and product thereof
  • Preparation method for SnO2/ZnO compound micro-nano fibers and product thereof
  • Preparation method for SnO2/ZnO compound micro-nano fibers and product thereof

Examples

  • Experimental program(6)
  • Comparison scheme(6)

Example Embodiment

[0031] Example 1
[0032] (1) Add 0.7419 g of zinc nitrate hexahydrate (Zn(NO 3 ) 2 ∙6H 2 O) and 0.8188 g of 2-methylimidazole were respectively dissolved in 50mL methanol solvent, stirred to obtain a transparent solution, mixed well and stirred for 1 h, after standing for 24 h, centrifuged and washed with methanol solvent for 3 times, placed in an evaporating dish Dry naturally to obtain Zif-8 product;
[0033] (2) Dissolve 0.0041 g of diammonium hydrogen citrate, 0.0082 g of octadecylamine, 0.0186 g of ethyl cellulose and 0.0068 g of Zif-8 in 2.0 mL of ethanol solvent, and stir to obtain a transparent solution;
[0034] (3) Add 0.3541 g of tin tetrachloride pentahydrate (SnCl 4 ∙5H 2 O) and 0.7000 g of PVP were added to a mixed solvent of 1.0 mL of ethanol and 4.0 mL of DMF, stirred to obtain a transparent solution, and then slowly added dropwise to the solution obtained in (2) at 0.2 mL/min, and stirred at room temperature for 10 h The precursor spinning solution is obtained, and the precursor fiber is obtained by electrospinning. The spinning parameters are: positive voltage is 18 KV, negative voltage is 0.5 KV, receiving distance is 20 cm, and syringe advancing speed is 0.002 mm/s;
[0035] (4) Put the precursor fiber in a muffle furnace, raise the temperature from room temperature to 600 ℃ at a temperature rise rate of 1 ℃/min, and keep it for 2 hours. After the sample is cooled in the furnace, SnO is obtained. 2 /ZnO composite micro-nano fiber.
[0036] The XRD results of the product are as follows figure 1 As shown in the figure, it can be seen that all the diffraction peaks are consistent with the standard XRD card (41-1445), which proves that the obtained product is tetragonal SnO2. Due to the low addition of Zif-8, the XRD detection limit There is no obvious ZnO crystal phase in the XRD results; the SEM of the product is as figure 2 with 3 As shown in the figure, it can be seen that the product obtained by the present invention has SnO on the surface of the fiber 2 Granular SnO 2 /ZnO composite micro-nano fiber structure, the main fiber is made of SnO 2 It is compounded with ZnO nanoparticles, the fiber diameter is 0.12-0.14 μm, the spherical structure on the fiber surface is composed of SnO2 nanoparticles, and the diameter of the spherical structure is 0.12-0.17 μm; the TEM of the product is as Figure 4 As shown, it can be seen from the figure that the morphology of the sample is basically consistent with the SEM result; the HRTEM of the product is as Figure 5 As shown in the figure, it can be seen that the main fiber part is made of SnO 2 Compounded with ZnO nanoparticles, the spherical structure on the fiber surface is made of SnO 2 Composition of nanoparticles.

Example Embodiment

[0037] Example 2
[0038] (1) Add 0.7419 g of Zn(NO 3 ) 2 ∙6H 2 O and 0.7269 g of 2-methylimidazole were respectively dissolved in 46 mL of methanol solvent and stirred to obtain a transparent solution. After mixing, stir for 2 h. After standing for 24 h, after centrifugal washing with methanol solvent for 3 times, place it in an evaporating dish. Dry naturally to obtain Zif-8 product;
[0039] (2) Dissolve 0.0010 g of diammonium hydrogen citrate, 0.0014 g of octadecylamine, 0.0037 g of ethyl cellulose and 0.0014 g of Zif-8 in 2.0 mL of ethanol solvent, and stir to obtain a transparent solution;
[0040] (3) Add 0.3541 g of SnCl 4 ∙5H 2 O and 0.6200 g of PVP were added to a mixed solvent of 1.1 mL of ethanol and 4.4 mL of DMF, stirred to obtain a transparent solution, and then slowly added dropwise to the solution obtained in (2) at 0.3 mL/min, and stirred at room temperature for 10 h to obtain The precursor spinning solution, the precursor fiber is obtained by the electrospinning method, the spinning parameters are: the positive voltage is 16KV, the negative voltage is 0.5KV, the receiving distance is 18 cm, and the injector advancing speed is 0.001 mm/s;
[0041] (4) Put the precursor fiber in a muffle furnace, raise it from room temperature to 550 ℃ at a temperature rise rate of 1 ℃/min, and keep it for 1 hour. After the sample is cooled in the furnace, the surface of the fiber has SnO 2 Granular SnO 2 /ZnO composite micro-nano fiber structure, the main fiber is made of SnO 2 Compounded with ZnO nanoparticles, the fiber diameter is 0.08-0.10 μm, and the spherical structure on the fiber surface is made of SnO 2 The diameter of the spherical structure is 0.08-0.12 μm.

Example Embodiment

[0042] Example 3
[0043] (1) Add 0.7419 g of Zn(NO 3 ) 2 ∙6H 2 O and 0.9009 g of 2-methylimidazole were respectively dissolved in 48 mL of methanol solvent and stirred to obtain a transparent solution. After mixing evenly, stir for 1 h. After standing for 24 h, after centrifugal washing with methanol solvent for 3 times, place in an evaporating dish. Dry naturally to obtain Zif-8 product;
[0044] (2) Dissolve 0.0325 g of diammonium hydrogen citrate, 0.0594 g of octadecylamine, 0.1327 g of ethyl cellulose and 0.0431 g of Zif-8 in 2.0 mL of ethanol solvent, and stir to obtain a transparent solution;
[0045] (3) Add 0.3541 g of SnCl 4 ∙5H 2 O and 0.7700 g of PVP were added to the mixed solvent of 1.2 mL of ethanol and 4.8 mL of DMF, stirred to obtain a transparent solution, and then slowly added dropwise to the solution obtained in (2) at 0.2 mL/min, and stirred at room temperature for 8 h to obtain The precursor spinning solution, the precursor fiber is obtained by the electrospinning method, the spinning parameters are: positive voltage is 17 KV, negative voltage is 0.5 KV, receiving distance is 22 cm, and syringe advancing speed is 0.003 mm/s;
[0046] (4) Put the precursor fiber in a muffle furnace, raise it from room temperature to 650 ℃ at a heating rate of 2 ℃/min, and keep it for 4 hours. After the sample is cooled in the furnace, the surface of the fiber has SnO 2 Granular SnO 2 /ZnO composite micro-nano fiber structure, the main fiber is made of SnO 2 Compounded with ZnO nanoparticles, the fiber diameter is 0.95-1.2 μm, and the spherical structure on the fiber surface is made of SnO 2 Composed of nanoparticles, the diameter of the spherical structure is 1.7-2.2 μm.
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PUM

PropertyMeasurementUnit
Diameter0.05 ~ 1.5µm
Diameter0.05 ~ 2.5nm
Diameter0.12 ~ 0.14µm
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
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