CN111851059B - Graphene modified non-woven fabric for filtering fine particles and preparation method thereof - Google Patents
Graphene modified non-woven fabric for filtering fine particles and preparation method thereof Download PDFInfo
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- CN111851059B CN111851059B CN202010757338.7A CN202010757338A CN111851059B CN 111851059 B CN111851059 B CN 111851059B CN 202010757338 A CN202010757338 A CN 202010757338A CN 111851059 B CN111851059 B CN 111851059B
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Abstract
The invention discloses a graphene modified non-woven fabric for filtering fine particles and a preparation method thereof. The preparation method of the non-woven fabric comprises the following steps: (1) preparing a carboxylated chitosan solution; (2) preparing a graphene oxide solution; (3) immersing the non-woven fabric into a carboxylation chitosan solution, and carrying out freeze drying and vacuum heat drying to obtain a modified non-woven fabric deposited with carboxylation chitosan; (4) and (3) immersing the modified non-woven fabric obtained in the step (3) into a graphene oxide solution, and carrying out freeze drying and vacuum heat drying to finally obtain the graphene modified non-woven fabric. The non-woven fabric can reduce pressure drop which can reach 10Pa at least while improving the absorption efficiency of fine particles, and has the advantages of low cost, simple preparation method and convenient practical application.
Description
Technical Field
The invention relates to a graphene modified non-woven fabric and a preparation method thereof, and more particularly relates to a graphene modified non-woven fabric for filtering fine particles and a preparation method thereof
Background
With the development of human industrialization, the atmospheric pollution level is increased continuously, and the fine particulate matters, namely PM2.5, refer to particulate matters with the aerodynamic equivalent diameter of less than or equal to 2.5 microns in the atmosphere, and the content of the particulate matters in the atmosphere is small, but the particulate matters have important influence on human health and air quality. Studies show that PM2.5 can be inhaled into the lung by human bodies, and the risk of suffering from acute respiratory diseases and cardiovascular and cerebrovascular diseases is increased. Therefore, the research on a material which can effectively capture PM2.5 and has low pressure drop has important practical significance. At present, the common filter material is a composite membrane material which is formed by preparing a polymer into fibers by using an electrostatic spinning technology and then assembling the fibers and other materials, the filtration efficiency of the composite membrane material prepared by the method can reach 99.8 percent, but the pressure drop is generally higher, the electrostatic spinning cost is higher, the process flow is complex, the preparation difficulty is higher, and the practical application is difficult.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide the graphene modified non-woven fabric for filtering fine particles, which has the advantages of high fine particle filtering efficiency, low pressure drop, low cost and simple preparation, and the invention also aims to provide the preparation method of the non-woven fabric.
The technical scheme is as follows: the graphene modified non-woven fabric for filtering fine particles comprises a non-woven fabric substrate, carboxylated chitosan is deposited on the non-woven fabric substrate, graphene oxide is assembled on the carboxylated chitosan, and the graphene modified non-woven fabric is of a porous loose structure.
Wherein the filtering efficiency of the fine particles is 90.08-99.91%, and the pressure drop is 10-60 Pa.
The preparation method of the graphene modified non-woven fabric for filtering fine particles comprises the following steps:
(1) preparing a carboxylated chitosan solution;
(2) preparing a graphene oxide solution;
(3) immersing the non-woven fabric into a carboxylation chitosan solution, and carrying out freeze drying and vacuum heat drying to obtain a modified non-woven fabric deposited with carboxylation chitosan;
(4) and (3) immersing the modified non-woven fabric obtained in the step (3) into a graphene oxide solution, and carrying out freeze drying and vacuum heat drying to finally obtain the graphene modified non-woven fabric.
Wherein the concentration of the carboxylated chitosan solution in the step 1 is 2-20mg/ml, the concentration of the graphene oxide solution in the step 2 is 4-15mg/ml, the time for immersing the non-woven fabric into the carboxylated chitosan solution in the step 3 is 1-5h, the freeze-drying time is 24-72h, the time for immersing the modified non-woven fabric into the graphene oxide solution in the step 4 is 1-5h, and the freeze-drying time is 24-72 h.
The preparation principle is as follows: the graphene oxide is large in specific surface area and rich in functional groups, and the physical property of the chitosan is mild, so that the chitosan can still keep good affinity with skin after being compounded with the non-woven fabric, the compound synergistic effect of the chitosan and the graphene can provide a large adsorption and filtration area for the fabric, attachment sites of fine particles are increased, a fiber structure of the non-woven fabric provides pores of tens of microns, and the pressure drop can be effectively reduced.
Has the beneficial effects that: compared with the prior art, the invention has the following remarkable advantages: 1. the absorption efficiency of fine particles is improved, and simultaneously, the pressure drop can be reduced and can reach 10Pa at the lowest; 2. low cost, simple preparation method and convenient practical application.
Drawings
FIG. 1 is a scanning electron microscope photograph of example 1;
FIG. 2 is a scanning electron microscope photograph of the modified nonwoven fabric deposited with carboxylated chitosan in example 1;
FIG. 3 is a scanning electron microscope image of a pure nonwoven fabric;
FIG. 4 is an X-ray diffraction pattern of example 1.
Detailed Description
Example 1
(1) Dispersing 10mg of carboxylated chitosan into 5ml of water, uniformly mixing for 1min by oscillation, and carrying out ultrasonic treatment for 5min to obtain a carboxylated chitosan solution with good dispersion degree and concentration of 2 mg/ml;
(2) Dispersing 24mg of graphene oxide into 6ml of water, uniformly mixing for 1min by oscillation, and carrying out ultrasonic treatment for 6min to obtain a graphene oxide solution with good dispersion degree and 4mg/ml concentration;
(3) immersing the non-woven fabric into a carboxylated chitosan solution with the concentration of 2mg/ml for 1 hour, freeze-drying for 24 hours, and vacuum-heat drying for 8 hours to obtain a modified non-woven fabric assembled with a layer of carboxylated chitosan;
(4) and (3) immersing the modified non-woven fabric assembled with the layer of carboxylated chitosan into a graphene oxide solution with the concentration of 4mg/ml for 1h, freeze-drying for 24h, and vacuum-heat drying for 8h to obtain the graphene modified non-woven fabric.
As can be seen from fig. 4, the diffraction peak of 2 θ ═ 25.3 ° corresponds to graphene type carbon, which illustrates that graphene is deposited on the nonwoven fabric, as can be seen from fig. 3, the nonwoven fabric is composed of smooth micron-sized fibers, as can be seen from fig. 2, chitosan covers the surface of the nonwoven fabric as a smooth surface, as can be seen from fig. 1, the graphene modified nonwoven fabric is a porous and loose structure.
Example 2
(1) Dispersing 10mg of carboxylated chitosan into 2ml of water, uniformly mixing for 2min by oscillation, and carrying out ultrasonic treatment for 10min to obtain a carboxylated chitosan solution with good dispersion degree and concentration of 5 mg/ml;
(2) dispersing 24mg of graphene oxide into 4ml of water, uniformly mixing for 4min in an oscillating way, and carrying out ultrasonic treatment for 10min to obtain a graphene oxide solution with good dispersion degree and 6mg/ml concentration;
(3) Immersing the non-woven fabric into a carboxylated chitosan solution with the concentration of 5mg/ml for 2 hours, freeze-drying for 48 hours, and vacuum-heat drying for 12 hours to obtain a modified non-woven fabric assembled with a layer of carboxylated chitosan;
(4) and (3) immersing the modified non-woven fabric assembled with the layer of carboxylated chitosan into a graphene oxide solution with the concentration of 6mg/ml for 2 hours, freeze-drying for 48 hours, and vacuum-heat drying for 12 hours to obtain the graphene modified non-woven fabric.
Example 3
(1) Dispersing 10mg of carboxylated chitosan into 1ml of water, oscillating and uniformly mixing for 5min, and performing ultrasonic treatment for 20min to obtain a carboxylated chitosan solution with good dispersion degree and concentration of 10 mg/ml;
(2) dispersing 24mg of graphene oxide into 3ml of water, uniformly mixing for 6min by oscillation, and carrying out ultrasonic treatment for 15min to obtain a graphene oxide solution with good dispersion degree and 8mg/ml concentration;
(3) immersing the non-woven fabric into a carboxylated chitosan solution with the concentration of 10mg/ml for 3 hours, freeze-drying for 48 hours, and vacuum-heat drying for 12 hours to obtain a modified non-woven fabric assembled with a layer of carboxylated chitosan;
(4) and (3) immersing the modified non-woven fabric assembled with the layer of carboxylated chitosan into a graphene oxide solution with the concentration of 8mg/ml for 3h, freeze-drying for 48h, and vacuum-heat drying for 12h to obtain the graphene modified non-woven fabric.
Example 4
(1) Dispersing 12mg of carboxylated chitosan into 1ml of water, oscillating and uniformly mixing for 5min, and performing ultrasonic treatment for 20min to obtain a carboxylated chitosan solution with good dispersion degree and concentration of 12 mg/ml;
(2) Dispersing 10mg of graphene oxide into 1ml of water, uniformly mixing for 10min in an oscillating way, and carrying out ultrasonic treatment for 20min to obtain a graphene oxide solution with good dispersion degree and 10mg/ml concentration;
(3) immersing the non-woven fabric into a carboxylated chitosan solution with the concentration of 12mg/ml for 4 hours, freeze-drying for 72 hours, and vacuum-heat drying for 24 hours to obtain a modified non-woven fabric assembled with a layer of carboxylated chitosan;
(4) and (3) immersing the modified non-woven fabric assembled with the layer of carboxylated chitosan into a graphene oxide solution with the concentration of 10mg/ml for 4h, freeze-drying for 72h, and vacuum-heat drying for 24h to obtain the graphene modified non-woven fabric.
Example 5
(1) Dispersing 15mg of carboxylated chitosan into 1ml of water, uniformly mixing for 10min by oscillation, and carrying out ultrasonic treatment for 30min to obtain a carboxylated chitosan solution with good dispersion degree and concentration of 15 mg/ml;
(2) dispersing 12mg of graphene oxide into 1ml of water, uniformly mixing for 15min in an oscillating way, and carrying out ultrasonic treatment for 25min to obtain a graphene oxide solution with good dispersion degree and a concentration of 12 mg/ml;
(3) immersing the non-woven fabric into a carboxylated chitosan solution with the concentration of 15mg/ml for 5 hours, freeze-drying for 72 hours, and vacuum-heat drying for 24 hours to obtain a modified non-woven fabric assembled with a layer of carboxylated chitosan;
(4) and (3) immersing the modified non-woven fabric assembled with the layer of carboxylated chitosan into a graphene oxide solution with the concentration of 12mg/ml for 5h, freeze-drying for 72h, and vacuum-heat drying for 24h to obtain the graphene modified non-woven fabric.
Example 6
(1) Dispersing 20mg of carboxylated chitosan into 1ml of water, uniformly mixing for 15min by oscillation, and carrying out ultrasonic treatment for 30min to obtain a carboxylated chitosan solution with good dispersion degree and 20mg/ml concentration;
(2) dispersing 15mg of graphene oxide into 1ml of water, uniformly mixing for 15min in an oscillating way, and carrying out ultrasonic treatment for 25min to obtain a graphene oxide solution with good dispersion degree and concentration of 15 mg/ml;
(3) immersing the non-woven fabric into a carboxylated chitosan solution with the concentration of 20mg/ml for 5 hours, freeze-drying for 72 hours, and vacuum-heat drying for 24 hours to obtain a modified non-woven fabric assembled with a layer of carboxylated chitosan;
(4) and (3) immersing the modified non-woven fabric assembled with the layer of carboxylated chitosan into a graphene oxide solution with the concentration of 15mg/ml for 5h, freeze-drying for 72h, and vacuum-heat drying for 24h to obtain the graphene modified non-woven fabric.
Comparative example
(1) Dispersing 24mg of graphene oxide into 6ml of water, uniformly mixing for 1min by oscillation, and carrying out ultrasonic treatment for 6min to obtain a graphene oxide solution with good dispersion degree and 4mg/ml concentration;
(2) and (3) immersing the non-woven fabric into a graphene oxide solution with the concentration of 4mg/ml for 1h, freeze-drying for 24h, and vacuum-heat drying for 8h to obtain the non-woven fabric with deposited graphene.
The results of PM filtration tests were conducted on examples 1 to 6 and comparative examples with the burnt incense stick as the PM generating source, the concentration of the fine particulate matter PM2.5 being 200 to 4000. mu.g/m 3, and the flow rate being 2.83L/min, as shown in Table 1:
Table 1 PM filtration test results of examples 1 to 6, comparative examples
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative example | |
| Efficiency of filtration | 90.08％ | 91.44％ | 95.40％ | 98.11％ | 99.33％ | 99.91％ | 89.58％ |
| Pressure drop (Pa) | 10 | 20 | 40 | 50 | 30 | 60 | 75 |
Claims (7)
1. The utility model provides a filter fine particles and use modified non-woven fabrics of graphite alkene which characterized in that, includes the non-woven fabrics substrate, the non-woven fabrics substrate deposit has carboxylation chitosan, the last graphene oxide that has assembled of carboxylation chitosan, the modified non-woven fabrics of graphite alkene is porous loose structure.
2. The graphene-modified non-woven fabric for filtering fine particulate matter according to claim 1, wherein the fine particulate matter filtering efficiency is 90.08% -99.91%, and the pressure drop is 10-60 Pa.
3. The method for preparing the graphene modified non-woven fabric for filtering fine particulate matters according to claim 1, which is characterized by comprising the following steps of:
(1) preparing a carboxylated chitosan solution;
(2) preparing a graphene oxide solution;
(3) immersing the non-woven fabric into a carboxylation chitosan solution, and carrying out freeze drying and vacuum heat drying to obtain a modified non-woven fabric deposited with carboxylation chitosan;
(4) and (3) immersing the modified non-woven fabric obtained in the step (3) into a graphene oxide solution, and carrying out freeze drying and vacuum heat drying to finally obtain the graphene modified non-woven fabric.
4. The method of preparing a graphene-modified non-woven fabric for filtering fine particulate matter according to claim 3, wherein the concentration of the carboxylated chitosan solution in the step 1 is 2 to 20 mg/ml.
5. The method for preparing the graphene modified non-woven fabric for filtering fine particulate matter according to claim 3, wherein the concentration of the graphene oxide solution in the step 2 is 4-15 mg/ml.
6. The method for preparing the graphene-modified non-woven fabric for filtering fine particulate matter according to claim 3, wherein the non-woven fabric is immersed in the carboxylated chitosan solution for 1 to 5 hours and freeze-dried for 24 to 72 hours in the step 3.
7. The method for preparing the graphene modified non-woven fabric for filtering fine particulate matters according to claim 3, wherein the modified non-woven fabric in the step 4 is immersed in the graphene oxide solution for 1-5 hours, and the freeze-drying time is 24-72 hours.
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