Preparation method of ozone catalytic nanofiber

文档序号:1290915 发布日期:2020-08-07 浏览:25次 中文

阅读说明:本技术 一种臭氧催化纳米纤维的制备方法 (Preparation method of ozone catalytic nanofiber ) 是由 裴小强 郭国良 于 2019-01-30 设计创作,主要内容包括:本发明涉及一种臭氧催化纳米纤维的制备方法,其特征在于包括下述步骤:1)将聚合物溶于溶剂中,在室温~80℃温度下,搅拌3~12h,制成均匀透明的浓度为5~20wt%聚合物溶液;2)将所述聚合物溶液装入静电纺丝设备进行静电纺丝,制备成纤维网;3)将步骤2)制备的纤维网以1~5℃/min的速率升温至200~300℃,在空气中预氧化2~5h;然后以2~10℃/min的速率升温至600-1200℃,在惰性氛围中碳化2~5小时,得到碳纳米纤维;4)将步骤3)制备得到的碳纳米纤维浸入浓度为0.005~0.5mol/L的KMnO4溶液中浸泡10~120min,然后用去离子水清洗,除去表面粘附物后,在60~110℃下干燥5~12h,制得臭氧催化复合纳米纤维。(The invention relates to a preparation method of ozone catalytic nanofiber, which is characterized by comprising the following steps of 1) dissolving a polymer in a solvent, stirring for 3-12 hours at the temperature of room temperature to 80 ℃ to prepare a uniform and transparent polymer solution with the concentration of 5-20 wt%, 2) putting the polymer solution into an electrostatic spinning device for electrostatic spinning to prepare a fiber web, 3) heating the fiber web prepared in the step 2) to 200-300 ℃ at the speed of 1-5 ℃/min, pre-oxidizing in air for 2-5 hours, heating to 600-1200 ℃ at the speed of 2-10 ℃/min, carbonizing in an inert atmosphere for 2-5 hours to obtain carbon nanofiber, and 4) immersing the carbon nanofiber prepared in the step 3) into a KMnO4 solution with the concentration of 0.005-0.5 mol/L for 10-120 minutes, cleaning with deionized water, removing surface adherents, and drying for 5-12 hours at the temperature of 60-110 ℃ to prepare the ozone catalytic composite nanofiber.)

1. The preparation method of the ozone catalytic nanofiber is characterized by comprising the following steps of:

1) preparing a Polymer solution

Dissolving a polymer in a solvent, and stirring for 3-12 hours at the temperature of room temperature-80 ℃ to prepare a uniform and transparent polymer solution with the concentration of 5-20 wt%;

the polymer is selected from at least one of polyvinylpyrrolidone, polyvinyl alcohol, polyacrylonitrile, polyethylene oxide and chitosan;

the solvent is at least one selected from water, ethanol, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone;

2) nanofiber preparation

Putting the polymer solution into electrostatic spinning equipment for electrostatic spinning to prepare a fiber web;

3) preparation of carbon nanofibers

Heating the fiber net prepared in the step 2) to 200-300 ℃ at the speed of 1-5 ℃/min, and pre-oxidizing in air for 2-5 h; then heating to 600-1200 ℃ at the speed of 2-10 ℃/min, and carbonizing for 2-5 hours in an inert atmosphere to obtain the carbon nanofiber;

4) supported ozone catalyst

Soaking the carbon nanofiber prepared in the step 3) into a KMnO4 solution with the concentration of 0.005-0.5 mol/L for 10-120 min, then cleaning with deionized water, removing surface adherents, and drying at 60-110 ℃ for 5-12 h to prepare the ozone catalytic composite nanofiber.

2. The method for preparing the ozone catalytic nanofiber as claimed in claim 1, wherein the diameter of the carbon nanofiber is 100-600 nm.

3. The method for preparing the ozone catalysis nanofiber as claimed in claim 1 or 2, wherein the electrostatic spinning in step 2) has the process parameters that the flow rate of an injection pump is 3-200 μ L/min, the distance between a needle and a collector is 5-25 cm, the applied voltage is 8-30 KV, the rotation speed of the collector is 300-3000rpm, the spinning temperature is 20-30 ℃, the humidity is 40-70%, and the fiber web is collected on an aluminum foil.

4. The method for preparing the ozone catalytic nanofiber as claimed in claim 3, wherein the flow rate of the injection pump is 5-20 μ L/min, and the voltage is 15-25 KV.

Technical Field

The invention relates to the field of air purification, in particular to a preparation method of ozone catalytic nanofiber.

Background

CN201310309595.4 discloses an electrostatic spinning preparation method of manganese dioxide/polyacrylonitrile-based oxidative decomposition formaldehyde type nanofiber membrane, which comprises the following steps: (1) preparing nano manganese dioxide by using potassium permanganate and cyclohexanol through a hydrothermal method, wherein the diameter of the nano manganese dioxide is 50-600 nm; (2) mixing Polyacrylonitrile (PAN) and nano Manganese Dioxide (MD), dissolving in N-N Dimethylformamide (DMF), and stirring to obtain uniformly dispersed electrostatic spinning solution; wherein the mass ratio of MD to PAN is 0.01-0.5: 1; (3) and (3) performing electrostatic spinning by using the prepared electrostatic spinning solution to obtain the manganese dioxide/polyacrylonitrile (MD/PAN) based formaldehyde oxidative decomposition type nanofiber membrane. The nanofiber membrane has the function of oxidizing and decomposing formaldehyde.

However, in the nanofiber membrane, the nano manganese dioxide is directly added into the spinning solution, so that the spinnability of the original spinning solution is reduced, and a part of Mn ions are wrapped in the inside of the fiber, so that the effective utilization rate is reduced.

Disclosure of Invention

The invention aims to solve the technical problem of providing a preparation method of ozone catalytic nanofiber, which has high effective utilization rate and can remove particles and decompose ozone, aiming at the current situation of the prior art.

The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the ozone catalytic nanofiber is characterized by comprising the following steps of:

1) preparing a Polymer solution

Dissolving a polymer in a solvent, and stirring for 3-12 hours at the temperature of room temperature-80 ℃ to prepare a uniform and transparent polymer solution with the concentration of 5-20 wt%;

the polymer is selected from at least one of polyvinylpyrrolidone, polyvinyl alcohol, polyacrylonitrile, polyethylene oxide and chitosan;

the solvent is at least one selected from water, ethanol, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone;

2) nanofiber preparation

Putting the polymer solution into electrostatic spinning equipment for electrostatic spinning to prepare a fiber web;

3) preparation of carbon nanofibers

Heating the fiber net prepared in the step 2) to 200-300 ℃ at the speed of 1-5 ℃/min, and pre-oxidizing in air for 2-5 h; then heating to 600-1200 ℃ at the speed of 2-10 ℃/min, and carbonizing for 2-5 hours in an inert atmosphere to obtain the carbon nanofiber;

4) supported ozone catalyst

Soaking the carbon nanofiber prepared in the step 3) into a KMnO4 solution with the concentration of 0.005-0.5 mol/L for 10-120 min, then cleaning with deionized water, removing surface adherents, and drying at 60-110 ℃ for 5-12 h to prepare the ozone catalytic composite nanofiber.

The diameter of the carbon nanofiber is 100-600 nm.

The technological parameters of the electrostatic spinning in the step 2) are that the flow rate of an injection pump is 3-200 mu L/min, the distance between a needle and a collector is 5-25 cm, the applied voltage is 8-30 KV, the rotating speed of the collector is 300-3000rpm, the spinning temperature is 20-30 ℃, the humidity is 40-70%, and the fiber web is collected on an aluminum foil.

The flow rate of the injection pump is 5-20 mu L/min, and the voltage is 15-25 KV.

Compared with the prior art, the invention has the advantages that the high specific surface area nanofiber is prepared by electrostatic spinning, then the carbon nanofiber is formed by the high-temperature carbonization process, and then the carbon nanofiber is immersed in the KMnO4Carrying out oxidation-reduction reaction on the solution to form MnOx nano-particles with ozone catalytic activity on the surface of the carbon nano-fiber; compared with the conventional ozone catalyst, the catalyst has extremely high specific surface area and catalytic activity point positions, is favorable for the decomposition of ozone, and can be used for preparing a composite filter screen by one-step molding with a particulate matter filter screen when preparing air purification and fresh air filter screen products, so that the preparation process and cost of the air purification and fresh air filter screens are greatly reduced.

Drawings

FIG. 1 is an electron micrograph of a carbon nanofiber according to example 1 of the present invention;

FIG. 2 is an SEM photograph of the ozone-catalyzed nanofibers of example 1 of the present invention.

Detailed Description

The present invention will be described in further detail with reference to examples.

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