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 郭国良 裴小强 高婷婷 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：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；将锰盐和过渡金属盐溶于溶剂中,配制成锰盐浓度为2～20wt％、金属盐浓度为0～1wt％的催化剂溶液；将所述聚合物溶液和锰盐溶液混合,搅拌5～12h,然后静置或者真空脱泡,得到复合凝胶溶液；将所述的复合凝胶溶液装入静电纺丝设备进行静电纺丝,制备成纤维网；将制备得到的纤维网在50～120℃下干燥5～12h,然后以2～10℃/min的升温速率升至300-1000℃煅烧3～10小时,得到具有臭氧催化功能的纳米纤维。(The invention relates to a preparation method of ozone catalytic nanofiber, which is characterized by comprising the following steps: 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%; dissolving manganese salt and transition metal salt in a solvent to prepare a catalyst solution with the manganese salt concentration of 2-20 wt% and the metal salt concentration of 0-1 wt%; mixing the polymer solution and the manganese salt solution, stirring for 5-12 h, and then standing or defoaming in vacuum to obtain a composite gel solution; putting the composite gel solution into electrostatic spinning equipment for electrostatic spinning to prepare a fiber web; drying the prepared fiber net at 50-120 ℃ for 5-12 h, and then raising the temperature to 300-1000 ℃ at a heating rate of 2-10 ℃/min and calcining for 3-10 h to obtain the nanofiber with the ozone catalysis function.)

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) preparation of catalyst solution

Dissolving manganese salt and transition metal salt in a solvent to prepare a catalyst solution with the manganese salt concentration of 2-20 wt% and the metal salt concentration of 0-1 wt%;

the manganese salt is selected from at least one of manganese nitrate, manganese acetate, manganese sulfate, manganese chloride and manganese carbonate;

the metal salt is selected from at least one of copper nitrate, silver nitrate, cobalt nitrate, ferric nitrate, copper acetate, silver acetate, cobalt acetate and ferric acetate;

the solvent is the same as the solvent used for the polymer solution;

3) mixing the polymer solution and the manganese salt solution, stirring for 5-12 h, and then standing or defoaming in vacuum to obtain a composite gel solution;

4) nanofiber preparation

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

5) post-treatment

Drying the prepared fiber net at 50-120 ℃ for 5-12 h, and then raising the temperature to 300-1000 ℃ at a heating rate of 2-10 ℃/min and calcining for 3-10 h to obtain the nanofiber with the ozone catalysis function.

2. The method of claim 1, wherein the concentration of the metal salt in the catalyst solution is 0.05-1 wt%.

3. The method for preparing the ozone catalysis nanofiber as claimed in claim 1 or 2, wherein during the electrostatic spinning, the flow rate of an injection pump in the electrostatic spinning device is controlled to be 3-200 μ L/min, the distance between a needle and a collector is controlled to be 5-25 cm, the voltage is 8-30 KV, preferably 15-25 KV, the rotating speed of the collector is 300-3000rpm, the spinning temperature is 20-30 ℃, the humidity is 40-70%, and a dense fiber web is collected on an aluminum foil.

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

5. The method for preparing the ozone catalytic nanofiber as claimed in claim 4, wherein the diameter of the nanofiber obtained after calcination is 50-500 nm.

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) preparation of catalyst solution

Dissolving manganese salt and transition metal salt in a solvent to prepare a catalyst solution with the manganese salt concentration of 2-20 wt% and the metal salt concentration of 0-1 wt%;

the manganese salt is selected from at least one of manganese nitrate, manganese acetate, manganese sulfate, manganese chloride and manganese carbonate;

the metal salt is selected from at least one of copper nitrate, silver nitrate, cobalt nitrate, ferric nitrate, copper acetate, silver acetate, cobalt acetate and ferric acetate;

the solvent is the same as the solvent used for the polymer solution;

3) mixing the polymer solution and the manganese salt solution, stirring for 5-12 h, and then standing or defoaming in vacuum to obtain a composite gel solution;

4) nanofiber preparation

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

5) post-treatment

Drying the prepared fiber net at 50-120 ℃ for 5-12 h, and then raising the temperature to 300-1000 ℃ at a heating rate of 2-10 ℃/min and calcining for 3-10 h to obtain the nanofiber with the ozone catalysis function.

Preferably, the concentration of the metal salt in the catalyst solution is 0.05-1 wt%. The metal salt plays a role in promoting catalysis, so that the ozone decomposition effect can be greatly improved, and the moisture resistance of the fiber can be provided; can keep the ozone decomposition function in a humid environment.

Further, when the electrostatic spinning is carried out, the flow speed of an injection pump in the electrostatic spinning equipment is controlled to be 3-200 mu L/min, the distance between a needle and a collector is 5-25 cm, the voltage is 8-30 KV, the preferred voltage is 15-25 KV, the rotating speed of the collector is 300-3000rpm, the spinning temperature is 20-30 ℃, the humidity is 40-70%, and a compact fiber net is collected on an aluminum foil.

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

Preferably, the diameter of the nanofiber obtained after calcination is 50-500 nm.

Compared with the prior art, the preparation method has the advantages that after the high molecular polymer and the catalytic precursor solution are blended, the composite nanofiber is directly prepared by an electrostatic spinning method, high molecular components in the fiber are burnt by a high-temperature calcination method, so that MnOx forms a nanofiber shape at high temperature, and the MnOx is made into a nanofiber-shaped material and used as an active catalyst for ozone decomposition to improve the specific surface area and the reaction contact point of the MnOx catalyst, so that the reaction activity and the effective utilization rate of the catalyst are improved; and the fiber is made into a net shape and also has the function of particle filtration.

Drawings

FIG. 1 is an electron micrograph of a nanofiber web prepared in step 4 of example 1 of the present invention;

FIG. 2 is an SEM photograph of calcined nanofibers obtained in step 5 of example 1 of the present invention;

fig. 3 is a partially enlarged view of fig. 2.

Detailed Description

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