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Preparation method of hollow porous sulfated zirconium dioxide solid superacid nanofibers

A solid superacid and nanofiber technology, which is applied in the manufacture of hollow filaments, fiber types, fiber treatment, etc., can solve the problems of difficult control of shape and low specific surface area

Active Publication Date: 2021-02-19
DALIAN UNIV OF TECH PANJIN INST OF IND TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problems of serious agglomeration of nanoscale solid superacids, difficult shape control and low specific surface area, the present invention proposes a method for preparing hollow porous sulfated zirconia solid superacid nanofibers by combining electrospinning, surface coating and sulfation technologies Methods

Method used

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  • Preparation method of hollow porous sulfated zirconium dioxide solid superacid nanofibers
  • Preparation method of hollow porous sulfated zirconium dioxide solid superacid nanofibers
  • Preparation method of hollow porous sulfated zirconium dioxide solid superacid nanofibers

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Experimental program
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Effect test

Embodiment 1

[0038] Step 1: the preparation of spinning solution:

[0039]Add 10g of polymer carrier to 100g of good solvent, and keep stirring in an oil bath at 50°C for 8 hours to obtain a polymer solution, then add 2g of zirconia precursor, and stir at room temperature for 4 hours to obtain an electrospinning solution .

[0040] Step 2: Preparation of nanofibers containing zirconia precursors:

[0041] Inject the spinning solution in step 1 into an electrospinning device, and prepare nanofibers containing a zirconium dioxide precursor through electrospinning;

[0042] Step 3: Surface coating of nanofibers:

[0043] Place the nanofibers containing the zirconia precursor in step 2 in a vacuum oven at 70°C for 8 hours, then immerse in a solution of a precipitant with a concentration of 10% by mass percentage, age at a certain temperature for 12 hours, and obtain a surface coated with hydrogen after washing. Zirconia-coated nanofibers.

[0044] Step 4: the sulfation of nanofibers:

[0...

Embodiment 2

[0057] A method for preparing hollow porous sulfated zirconia solid superacid nanofibers, comprising the following steps:

[0058] Step 1: the preparation of spinning solution:

[0059] Add 15g of polymer carrier to 112g of good solvent, and keep stirring in an oil bath at 70°C for 10 hours to obtain a polymer solution, then add 3g of zirconia precursor, and stir at room temperature for 7 hours to obtain an electrospinning solution .

[0060] Step 2: Preparation of nanofibers containing zirconia precursors:

[0061] Inject the spinning solution in step 1 into an electrospinning device, and prepare nanofibers containing a zirconium dioxide precursor through electrospinning;

[0062] Step 3: Surface coating of nanofibers:

[0063] Place the nanofibers containing the zirconia precursor in step 2 in a vacuum oven at 80°C for 12 hours, then immerse in a precipitant solution with a mass percentage concentration of 12%, and age at a certain temperature for 16 hours. After washing,...

Embodiment 3

[0074] A method for preparing hollow porous sulfated zirconia solid superacid nanofibers, comprising the following steps:

[0075] Step 1: the preparation of spinning solution:

[0076] Add 21g of polymer carrier to 113g of good solvent, and continue stirring in an oil bath at 70°C for 12 hours to obtain a polymer solution, then add 4g of zirconia precursor, and stir at room temperature for 9 hours to obtain an electrospinning solution .

[0077] Step 2: Preparation of nanofibers containing zirconia precursors:

[0078] Inject the spinning solution in step 1 into an electrospinning device, and prepare nanofibers containing a zirconium dioxide precursor through electrospinning;

[0079] Step 3: Surface coating of nanofibers:

[0080] Place the nanofibers containing the zirconia precursor in step 2 in a vacuum oven at 85°C for 19 hours, then immerse in a precipitant solution with a mass percent concentration of 13%, and age at a certain temperature for 20 hours. After washing...

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Abstract

The invention relates to a preparation method of hollow porous sulfated zirconium dioxide solid superacid nanofibers, and belongs to the technical field of electrostatic spinning. The hollow porous sulfated zirconium dioxide solid superacid nanofibers are prepared by combining electrostatic spinning and sulfation technologies, and the prepared sulfated zirconium dioxide has a complete hollow fiberstructure and can provide a long-range low-resistance mass transfer channel. The diameter of the fibers can be controlled to be 100-1000 nm by changing spinning operation conditions, the fiber wall is of a porous structure, the specific surface area is high, and more active sites can be exposed. The surface acid strength Ho of the prepared hollow porous sulfated zirconium dioxide nanofibers is less than -12.7, and the hollow porous sulfated zirconium dioxide nanofibers have the property of solid superacid.

Description

technical field [0001] The invention belongs to the technical field of electrospinning, and in particular relates to a method for preparing hollow porous sulfated zirconia solid superacid nanofibers. [0002] technical background [0003] In the continuous development of petrochemical and fine chemical industry, acidic catalyst plays an important role. Since the 1950s and 1960s, the research on superacids has attracted the attention of researchers from various countries, and has been widely used in petroleum refining fields such as isomerization, cracking, reforming, oil deoxidation, and alkylation and polymerization. , esterification, acylation and other fine chemical and petrochemical fields. Superacids can be divided into liquid superacids and solid superacids. Because solid superacids do not contain halogens, catalysts and products are easily separated, low cost, weak corrosion on equipment, recyclable, and less "three wastes" emissions. The scope of application is grad...

Claims

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Application Information

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IPC IPC(8): D01F9/08D01F1/08D01F6/50D01F1/10D06M11/60D06M13/432D06M11/55D01D5/00D06M101/24
CPCD01F9/08D01F1/08D01F6/50D01F1/10D06M11/60D06M13/432D06M11/55D01D5/003D06M2101/24
Inventor 代岩郗元郭明钢闫志刚王国际
Owner DALIAN UNIV OF TECH PANJIN INST OF IND TECH