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A kind of preparation method of inorganic porous nanofiber

A nanofiber, inorganic porous technology, applied in fiber treatment, nanotechnology, nanotechnology, etc., can solve the problems of poor interface bonding between inorganic nanoparticles and polymer matrix, limited specific surface area and porosity of porous nanofibers, and different diameters of nanofibers. Uniformity and other issues, to achieve the effect of regular porous structure, controllable structure and low relative density

Active Publication Date: 2017-08-15
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional method of preparing porous nanofibers by electrospinning technology by directly mixing inorganic nanoparticles, polymer matrix and solvent to obtain a solution has many disadvantages: due to the poor dispersion and stability of inorganic nanoparticles in organic solutions, resulting in The diameter of the obtained nanofibers is not uniform, and the shape is irregular; the interface bonding between the inorganic nanoparticles and the polymer matrix is ​​poor, and the inorganic nanoparticles are seriously agglomerated in the nanofibers, and the distribution is uneven, resulting in the distribution of the porous structure in the final porous nanofibers. Inhomogeneous and uncontrollable pore size; the prepared porous nanofibers have limited specific surface area and porosity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] step 1

[0032]Get 5ml of ammonia water (mass percent concentration is 28%, the following examples are the same), 10ml of deionized water and 30ml of ethanol, mix well on a magnetic stirrer, then add 3ml of TEOS, 52ml of ethanol and 0.5g of cetyltrimethyl bromide Ammonium chloride, pour it into the previously mixed solution, stir at a speed of 1100r / min for 2 minutes, then reduce the speed to 300r / min, and react in a water bath at 25°C for 5 hours. After the reaction was completed, the solution was taken out and washed with a centrifuge for 3 times, each time for 30 min. The washing liquid was absolute ethanol, and the rotation speed was 4000 r / min. Filter and dry the centrifuged product, put it in the air and raise the temperature to 350°C at a rate of 5°C / min, keep it for 30 minutes, then raise it to 600°C at a rate of 10°C / min, keep it for 10 hours, and finally collect the product and put it away. Preserve in 40ml deionized water to obtain a particle size of 100nm S...

Embodiment 2

[0050] step 1

[0051] Take 9ml of ammonia water, 16ml of deionized water and 25ml of ethanol, put it on a magnetic stirrer and mix evenly, then add 9ml of TEOS, 41ml of ethanol and 1.0g of cetyltrimethylammonium bromide, and pour it into the previously mixed solution , stirred at a speed of 1100r / min for 2 minutes, then lowered the speed to 300-400r / min, and reacted in a water bath at 25°C for 5 hours. After the reaction was completed, the solution was taken out and washed with a centrifuge for 3 times, each time for 30 min. The washing liquid was absolute ethanol, and the rotation speed was 4000 r / min. The centrifuged product was suction-filtered and dried, placed in the air and raised to 360°C at a heating rate of 5°C / min, kept for 30 minutes, then raised to 600°C at a heating rate of 10°C / min, kept for 10 hours, and finally the product was collected and released Preserve in 40ml deionized water to obtain a particle size of 480nm SiO 2 aqueous solution;

[0052] Prepare ...

Embodiment 3

[0055] Embodiment 3: prepare SiO according to step 1-step 5 in embodiment 1 2 -Br.

[0056] step 6

[0057] Take 0.25g of ground SiO 2 -Br was dissolved in 18ml DMF, 8ml MMA, 0.08ml PMDETA were added. Ultrasonic dispersion was performed for 30 minutes, and nitrogen gas was passed through for 20 minutes. Finally, 0.027g of CuBr was added, and the reaction was sealed at 50°C for 24 hours. After the reaction was completed, the solution was transferred to 500 ml of absolute ethanol for precipitation. After the supernatant has no floating silica, change to 500ml of absolute ethanol for precipitation, and repeat the operation 5 times. After precipitation, centrifuge in a centrifuge. The rotation speed is 4000r / min, and the separation is performed twice, 20 minutes each time, and the washing liquid added is ethanol. After centrifugation, the product was stored in DMF solvent to obtain wet SiO 2 -PMMA.

[0058] step 7

[0059] SiO in wet state 2 -PMMA An electrospinning sol...

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Abstract

The invention provides a preparation method of an inorganic porous nanometer fiber, and belongs to the field of inorganic / organic nanometer fiber preparation. The invention is characterized in that: A, uniformly dispersed inorganic nanoparticles with uniform particle sizes are prepared, a structure-directing agent is removed by roast, inorganic nanoparticles with porous structures are obtained, and the diameters of the inorganic nanoparticles are 50-70nm; B. inorganic nanoparticles are modified by compounds with responsive end groups, a chemical polymerization method is used, a reaction between inorganic nanoparticles and a polymer monomer is carried out, inorganic nanoparticles with surface grafted high-molecular polymers are obtained, the inorganic nanoparticles are dissolved in an organic solvent for preparing a precursor solution, and the solution concentration is 10wt%-50wt%; C. a nanometer fiber film is prepared from the precursor solution by using a polymer electrostatic spinning method, the film is roasted in an inert atmosphere and porous structures between the inorganic nanoparticles in the nanometer fiber are generated, and the inorganic porous nanometer fiber with secondary porous structures are finally obtained, wherein, the aperture is 2nm-50nm, and the amount of porosity is 0.2-1.0cm<3> / g.

Description

technical field [0001] The invention belongs to the technical field of inorganic / organic nanofiber preparation, and mainly relates to a preparation method of inorganic nanoparticle porous nanofiber. Background technique [0002] Inorganic nanoparticles have the advantages of large specific surface area, strong adsorption, and good chemical stability, and have been widely used in various fields. In recent years, the preparation of inorganic nanoparticles porous nanofibers with regular morphology and controllable structure has gradually become one of the research hotspots at home and abroad. Due to their high porosity and low dielectric constant, inorganic porous nanofibers play an irreplaceable role in high-efficiency thermal insulation layers, low dielectric constant insulating layers, adsorption and separation of macromolecules, filtration barriers, and nano-assembly materials. [0003] At present, researchers at home and abroad have conducted a lot of research on the prep...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/08D01F9/10C01B33/12D01D5/00B82Y30/00B82Y40/00
Inventor 贾晓龙张苒蔡晴杨小平
Owner BEIJING UNIV OF CHEM TECH
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