CN111501347A - Preparation method of catalytic nanofiber - Google Patents

Preparation method of catalytic nanofiber Download PDF

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CN111501347A
CN111501347A CN201910089520.7A CN201910089520A CN111501347A CN 111501347 A CN111501347 A CN 111501347A CN 201910089520 A CN201910089520 A CN 201910089520A CN 111501347 A CN111501347 A CN 111501347A
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nanofibers
dopamine
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CN111501347B (en
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裴小强
郭国良
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Ningbo Fotile Kitchen Ware Co Ltd
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Abstract

The invention relates to a preparation method of catalytic nano-fibers, 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 A with the concentration of 5-30 wt%; dissolving dopamine in 5EAdjusting pH in 50mM Tris-HCl buffer solution to prepare 0.5-10 g/L dopamine solution, immersing the nanofibers prepared in the step 1) in the dopamine solution, shaking and soaking at 20-60 ℃, then washing for 2-3 times with pure water, drying the surface moisture of the fibers to obtain modified nanofibers, and preparing KMnO4Soaking the modified nano-fiber into a catalyst aqueous solution with the concentration of 0.005-0.5 mol/L and the concentration of metal salt of 0.005-0.05 mmol/L, then washing away the floating matters by deionized water, and drying for 5-12 h at the temperature of 20-70 ℃ to obtain the catalytic nano-fiber.

Description

Preparation method of catalytic nanofiber
Technical Field
The invention relates to the field of air purification, in particular to a preparation method of catalytic nanofibers.
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 catalytic nanofiber, which has high effective utilization rate and can remove particles and decompose ozone and formaldehyde, aiming at the current situation of the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of catalytic nano-fiber is characterized by comprising the following steps:
1) preparation of nanofibers
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 A with the concentration of 5-30 wt%;
the polymer is selected from at least one of polyacrylonitrile, polyvinylidene fluoride, polymethyl methacrylate, polysulfone PSF, polystyrene, cellulose acetate and chitosan;
the solvent is at least one selected from water, ethanol, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone;
2) modified nanofibers
Dissolving dopamine in 5-50 mM Tris-HCl buffer solution, adjusting the pH value to 8.0-8.8, and preparing 0.5-10 g/L dopamine solution, immersing the nanofibers prepared in the step 1) in the dopamine solution, shaking and soaking for 1-12 hours at 20-60 ℃ to enable dopamine to be polymerized on the surfaces of the nanofibers, then washing the nanofibers coated with dopamine for 2-3 times by pure water until no free dopamine exists, and then drying the surface moisture of the fibers at the normal temperature-60 ℃ to obtain the modified nanofibers;
3) preparation of catalytic nanofibers
Preparing KMnO4Soaking the modified nano-fiber into the catalyst aqueous solution for 1-12 h, then washing with deionized water to remove floating matters, and drying at 20-70 ℃ for 5-12 h to obtain the catalytic nano-fiber with ozonolysis and formaldehyde decomposition functions.
Preferably, the noble metal salt is selected from at least one of chloroplatinic acid, chloroauric acid or chloropalladic acid.
Preferably, the electrostatic spinning in the step 2) has the technological parameters that the flow rate of the injection pump is 3-200 mu L/min, the distance between the needle and the 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 ℃, and the humidity is 40-70%;
collecting the web on a nonwoven.
Preferably, the flow rate of the injection pump is 5-20 mu L/min, the voltage is 15-25 KV., and the noble metal salt is at least one selected from chloroplatinic acid, chloroauric acid and chloropalladic acid.
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 a non-woven fabric.
The flow rate of the injection pump is 5-20 mu L/min, and the voltage is 15-25 KV.
According to the invention, the high-specific surface area nanofiber is prepared by electrostatic spinning, and then the nanofiber surface is soaked in a dopamine solution for self-polymerization modification, so that a dopamine-coated modified nanofiber membrane with strong reducibility and biological adhesion is obtained; re-immersion in KMnO4In the noble metal salt solution, through oxidation-reduction reaction with dopamine, MnOx with ozone catalytic activity and a noble metal simple substance nano structure with formaldehyde catalytic activity are formed on the surface of the modified nano fiber; and because the noble metal simple substance has good moisture resistance, the pollutants can be catalytically decomposed by utilizing the moisture in the air, so that the competitive adsorption effect of the relative humidity in the air on the ozone catalyst can be effectively weakened when the noble metal simple substance is catalytically compounded with MnOx ozone, and the moisture resistance of the ozone catalyst is improved. Compared with the conventional ozone catalyst, the catalyst has extremely high specific surface area and catalytic activity point sites, and is beneficial to the decomposition of ozone; and the limiting can be prepared into a filter screen which is used as an air cleaning and fresh air filter screen to provide a particle filtering function.
Drawings
FIG. 1 is an SEM photograph of nanofibers in example 1 of the present invention;
FIG. 2 is an SEM photograph of modified nanofibers obtained in example 1 of the present invention.
FIG. 3 is an SEM photograph of the catalytic nanofiber prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
(1) preparation of nanofibers
Dissolving 12g of polyacrylonitrile in 88g of N, N-dimethylformamide DMF solvent, stirring for 3h at 40 ℃ and the rotating speed of 500rpm to prepare uniform and transparent polymer solution;
and (2) loading the polymer solution into an electrostatic spinning device, adjusting electrostatic parameters, fixing the flow rate of an injection pump at 15 mu L/min, setting the distance between a needle and a collector at 15cm, applying a voltage of 15KV, setting the rotating speed of the collector at 500rpm, setting the spinning temperature at 25 ℃ and the humidity at 50%, and collecting the dense nanofiber web on a non-woven fabric support layer.
The prepared nanofiber is subjected to electron microscope scanning, and the photo is shown in figure 1.
(2) Nanofiber modification
Soaking the nanofiber formed in the mode into 2 g/L of dopamine solution, adjusting the pH value to 8.5 by taking 10mM Tris-HCl solution as a buffer solution, shaking and soaking for 10 hours at 25 ℃ to enable dopamine to be polymerized on the surface of the nanofiber, then washing the nanofiber covered with dopamine for 2-3 times by pure water until no free dopamine exists, and then airing the surface moisture of the modified nanofiber at normal temperature.
Scanning the prepared dopamine composite nanofiber by an electron microscope, and taking a photograph as shown in fig. 2.
(3) Catalytic nanofiber preparation
Soaking the above nanofibers in 0.05 mol/L KMnO4And 0.01 mmol/L chloroplatinic acid solution for 10h, then washing with deionized water for 3 times, and airing at room temperature to prepare the catalytic nano-fiber.
The prepared catalytic nanofiber is subjected to electron microscope scanning, and the photo thereof is shown in fig. 3.
As can be seen from fig. 1 and 2, after the PAN nanofibers are composited with dopamine, a dopamine adhesion layer covers the surface layer of the fibers, and after the dopamine composite nanofibers are immersed in a catalyst solution, the dopamine layer and the catalyst active ingredients undergo an oxidation-reduction reaction on the surfaces of the nanofibers to generate nanoparticles of MnOx and elemental platinum with the size of 50nm, and due to the bioadhesion of dopamine, the catalytic components are firmly bonded on the nanofibers to increase the stability of the nanofibers.
And carrying out performance test on the prepared composite nanofiber.
Firstly, ozone catalytic performance, wherein the size of a sample is 15cm × 15cm, the sample is placed into a testing device, and the space velocity is adjusted to 150000h-1The ozone inlet gas concentration is c0Was 10 ppm. The Model 202 Seri is adoptedThe al ozone analyzer detects the ozone concentration c at the outlet of the pipeline, detects the stable concentration at the outlet, and the ozone removal rate is calculated according to the following formula:
Figure BDA0001962837090000031
secondly, formaldehyde catalytic performance, namely the size of a sample is 15cm × 15cm, the sample is placed into a testing device, and the space velocity is adjusted to 150000h-1The feed concentration of formaldehyde was c0 and was 1 ppm. The method comprises the following steps of detecting the concentration c of formaldehyde at the outlet of a pipeline by adopting British Stanford PPM400ST, detecting the stable concentration of the outlet, and calculating the formaldehyde removal rate according to the following formula:
Figure BDA0001962837090000041
thirdly, the filtering performance of the particles is as follows:
the filtering performance of the composite nanofiber membrane is tested by adopting a TSI 8130 type automatic filter material tester, the sample size is 15cm × 15cm, NaCl aerosol with the mass median diameter of particle particles of 0.26um is generated, and the air flow speed is 32L/min.
The filtration efficiency η of the particles was obtained by testing the concentration of the particles at both ends of the membrane.
Figure BDA0001962837090000042
C1As outlet aerosol concentration, C2Is the inlet aerosol concentration.
(4) And (3) performance testing: the catalytic decomposition efficiency of ozone of the sample is 88 percent, the catalytic efficiency of formaldehyde is 66 percent, and the filtering performance of PM0.3 is 99 percent.
The mechanism of ozone decomposition:
(1) first, O3And MnO with MnOXThe vacancy on the surface of the catalyst is combined and dissociative adsorption is carried out, and an oxygen atom is inserted into the oxygen vacancy to form O2-And release one oxygen molecule;
(2) then, another gaseous ozone molecule is reacted with O2-Reacting to form peroxide O in an adsorbed state2 2-Simultaneously release a gaseous oxygen molecule O2；
(3) Finally, peroxide O2 2-And decomposing to form an oxygen molecule, desorbing from the surface of the catalyst, recovering oxygen vacancies, and continuing to participate in the next reaction.
O3+V0→O2+O2-
O3+O2-→O2+O2 2-
O2 2-→O2+V0
Wherein: v0Representing the oxygen vacancies at the surface of the catalyst.
In addition, in the MnOx catalyst, the chemical valence of Mn influences the number of surface active sites, and it has been found that Mn3 +/Mn4+The larger the value of (A), the lower the average chemical valence of Mn, the more surface oxygen vacancies and the better the catalytic performance.
Example 2
(1) Preparation of nanofibers
Dissolving 16g of polyvinylidene fluoride in 84g of N, N-dimethylformamide DMF solvent, stirring at 60 ℃ for 12h at the rotating speed of 500r/min, and preparing a uniform and transparent polymer solution;
the polymer solution is loaded into an electrostatic spinning device, electrostatic parameters are adjusted, the flow rate of an injection pump is fixed at 20 mu L/min, the distance between a needle and a collector is 17cm, the applied voltage is 20KV, the rotating speed of the collector is 500rpm, the spinning temperature is 25 ℃, the humidity is 50%, and a dense fiber web is collected on a non-woven fabric support layer.
(2) Nanofiber modification
Soaking the nanofiber formed in the mode into 2 g/L of dopamine solution, adjusting the pH value to 8.5 by taking 10mM of Tris-HCl solution as a buffer solution, shaking and soaking for 10 hours at 25 ℃ to enable dopamine to be polymerized on the surface of the nanofiber, then washing the nanofiber coated with dopamine for 2-3 times by pure water until no free dopamine exists, and then airing the surface moisture of the modified nanofiber at normal temperature.
(3) Preparation of catalytic nanofibers
Soaking the nanofibers in 0.1 mol/L KMnO4And 0.01 mmol/L chloroauric acid solution for 10h, then washing with deionized water for 3 times, and airing at room temperature to prepare the composite ozone catalytic nanofiber.
(4) And (3) performance testing: the catalytic decomposition efficiency of ozone of the sample is 85%, the catalytic efficiency of formaldehyde is 53%, and the filtering performance of PM0.3 is 91%.
Example 3:
(1) preparation of nanofibers
Dissolving 30g of polystyrene PS in 70g of N, N-dimethylformamide DMF solvent, stirring at the temperature of 30 ℃ for 12h at the rotating speed of 500rpm, and preparing a uniform and transparent polymer solution;
the polymer solution is loaded into an electrostatic spinning device, electrostatic parameters are adjusted, the flow rate of an injection pump is fixed at 15 mu L/min, the distance between a needle and a collector is 15cm, an applied voltage is 16KV, the rotating speed of the collector is 500rpm, the spinning temperature is 25 ℃, the humidity is 40%, and a dense fiber web is collected on a non-woven fabric support layer.
(2) Nanofiber modification
Soaking the nanofiber formed in the mode into 5 g/L of dopamine solution, taking 10mM Tris-HCl solution as buffer solution, adjusting the pH value to 8.5, soaking for 5 hours at 25 ℃ to enable dopamine to be polymerized on the surface of the nanofiber in a self-polymerization mode, then washing the nanofiber coated with dopamine for 2-3 times by pure water until no free dopamine exists, and then airing the surface moisture of the modified nanofiber at normal temperature.
(3) Preparation of catalytic nanofibers
Soaking the nanofibers in 0.01 mol/L KMnO4And 0.01 mmol/L chloropalladate solution for 10h, then washing with deionized water for 3 times, and airing at room temperature to prepare the composite ozone catalytic nanofiber.
(4) And (3) performance testing: the catalytic decomposition efficiency of ozone of the sample is 92%, the catalytic efficiency of formaldehyde is 61%, and the filtering performance of PM0.3 is 95%.

Claims (4)

1. A preparation method of catalytic nano-fiber is characterized by comprising the following steps:
1) preparation of nanofibers
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 A with the concentration of 5-30 wt%;
the polymer is selected from at least one of polyacrylonitrile, polyvinylidene fluoride, polymethyl methacrylate, polysulfone PSF, polystyrene, cellulose acetate and chitosan;
the solvent is at least one selected from water, ethanol, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone;
2) modified nanofibers
Dissolving dopamine in 5-50 mM Tris-HCl buffer solution, adjusting the pH value to 8.0-8.8, and preparing 0.5-10 g/L dopamine solution, immersing the nanofibers prepared in the step 1) in the dopamine solution, shaking and soaking for 1-12 hours at 20-60 ℃ to enable dopamine to be polymerized on the surfaces of the nanofibers, taking out the nanofibers, washing the nanofibers coated with dopamine for 2-3 times by pure water until no free dopamine exists, and drying the surface moisture of the fibers at the normal temperature-60 ℃ to obtain modified nanofibers;
3) preparation of catalytic nanofibers
Preparing KMnO4Soaking the modified nano-fiber into the catalyst aqueous solution for 1-12 h, then washing with deionized water to remove floating matters, and drying at 20-70 ℃ for 5-12 h to obtain the catalytic nano-fiber with ozonolysis and formaldehyde decomposition functions.
2. The method of claim 1, wherein the noble metal salt is at least one selected from chloroplatinic acid, chloroauric acid, and chloropalladic acid.
3. The preparation method of the catalytic nanofiber as claimed in claim 1 or 2, wherein the electrostatic spinning in step 2) has the process parameters of a flow rate of an injection pump of 3-200 μ L/min, a distance between a needle and a collector of 5-25 cm, an applied voltage of 8-30 KV, a rotation speed of the collector of 300-3000rpm, a spinning temperature of 20-30 ℃ and a humidity of 40-70%;
collecting the web on a nonwoven.
4. The preparation method of the 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.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112522862A (en) * 2020-11-13 2021-03-19 南通大学 Visible light driven antibacterial nanofiber and preparation method and application thereof

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