CN107051059B - Multifunctional biological filter membrane and preparation method thereof - Google Patents
Multifunctional biological filter membrane and preparation method thereof Download PDFInfo
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- CN107051059B CN107051059B CN201710259080.6A CN201710259080A CN107051059B CN 107051059 B CN107051059 B CN 107051059B CN 201710259080 A CN201710259080 A CN 201710259080A CN 107051059 B CN107051059 B CN 107051059B
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- B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
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Abstract
The invention provides a chitosan/electrostatic filter cotton nano-aperture biological filter membrane which is composed of a chitosan nano-film and organic electrostatic filter cotton, wherein the chitosan solution used in the preparation process accounts for 0.5-2.5% of the total weight of the membrane, dibutyl phthalate accounts for 0.5-2.5% of the volume of the solution in the preparation process, the chitosan content accounts for 10-30%, and the organic electrostatic filter cotton content accounts for 60-80%.
Description
Background
Compared with the thicker atmospheric particulate matters, the PM2.5 has small particle size, large area, strong activity, easy attachment of toxic and harmful substances (such as heavy metals, microorganisms and the like), long retention time in the atmosphere and long conveying distance, thereby having larger influence on human health and atmospheric environmental quality. At present, PM2.5 pollutes and influences people's life increasingly seriously, and the trip and the work of people have not only been influenced to many haze weather, more seriously influence resident health, consequently, under the condition that air quality descends gradually, the filtration and the entrapment of PM2.5 granule become more and more important.
The industrial base of the PM2.5 filter material in China is weak, the product structure is single, the product price is high, and the development of the PM2.5 filter material industry is seriously challenged; with the increasing prominence of the problem of PM2.5 pollution, higher market application requirements are put on the PM2.5 filter material. Therefore, the development of PM2.5 filter materials with independent intellectual property rights, the establishment of an industrial technical system, the reduction of cost and the wide application of popularization products are urgently needed in China.
Chitosan (CS) is a dephthaloyl product of chitin, a naturally biodegradable polycationic polysaccharide. The chitosan has the advantages of no toxicity, good biocompatibility, biodegradability and the like, and is widely applied in biomedicine, pharmacy and the like.
The chitosan is the only macromolecular aminopolysaccharide with positive charge in nature, has biological functions of antibiosis, bacteriostasis, metal ion adsorption and the like, has no toxic or side effect, has good film forming property and easy chemical modification property, and all the characteristics endow the chitosan with excellent performance as PM2.5 filtering material.
Disclosure of Invention
The invention aims to provide a multifunctional biological filter membrane and a preparation method thereof, and also provides application of the biological filter membrane in PM2.5 masks and air purification.
The invention is realized by the following technical scheme:
a chitosan/electrostatic filter cotton nano-aperture biological filter membrane comprises a chitosan nano-film and organic electrostatic filter cotton, wherein the chitosan solution used in the preparation process accounts for 0.5-2.5% in percentage by weight of the total weight of the membrane, dibutyl phthalate accounts for 0.5-2.5% in volume percentage of the solution in the preparation process, the chitosan content accounts for 10-30%, and the organic electrostatic filter cotton content accounts for 60-80%.
The preparation method of the chitosan/electrostatic filter cotton nano-aperture biological filter membrane comprises the following steps:
1) dissolving chitosan with acetic acid to prepare a solution with the mass concentration of 0.5-2.5%, and stirring until the chitosan is completely dissolved, and sterilizing at high temperature and high pressure;
2) dropwise adding the dibutyl phthalate solution into the chitosan acetic acid solution, and ultrasonically mixing to prepare a chitosan solution containing 0.5-2.5% (v/v) dibutyl phthalate nanoparticles for later use;
3) immersing the electrostatic filter cotton in a chitosan solution to fully immerse the chitosan solution containing the dibutyl phthalate nanoparticles in the electrostatic filter cotton layer;
4) drying the immersed electrostatic filter cotton, and then, washing the electrostatic filter cotton with ethanol to remove dibutyl phthalate to obtain the multifunctional PM2.5 biological filter membrane with the nano-aperture pores;
preferably, the multifunctional PM2.5 biological filter membrane comprises 1.2% of chitosan solution by mass, 1.0% of dibutyl phthalate in the mixed solution by volume, 20% of chitosan nano-membrane by weight and 75% of electrostatic filter cotton by weight.
The preparation method of the multifunctional PM2.5 biological filter membrane comprises the following steps:
1) dissolving chitosan with acetic acid to prepare a solution with the mass concentration of 1.2%, and stirring until the chitosan is completely dissolved, and sterilizing at high temperature and high pressure;
2) dropwise adding the dibutyl phthalate solution into the chitosan acetic acid solution, and ultrasonically mixing to prepare a chitosan solution containing 1.0% (v/v) dibutyl phthalate nanoparticles for later use;
3) immersing the electrostatic filter cotton in a chitosan solution to fully immerse the chitosan solution containing the dibutyl phthalate nanoparticles in the electrostatic filter cotton layer;
4) and drying the immersed electrostatic filter cotton, and then, washing the electrostatic filter cotton with ethanol to remove dibutyl phthalate to obtain the multifunctional PM2.5 biological filter membrane with the nano-aperture pores.
The deacetylation degree of the chitosan is 94.5%.
The multifunctional PM2.5 biological filter membrane is applied to PM2.5 masks and air purification equipment.
The invention has the beneficial effects that: 1) the preparation of the multifunctional PM2.5 biofiltration membrane has the advantages of standardized process flow, rich raw material source, low price and large market potential. The project has obvious PM2.5 particle interception effect on the basis of ensuring the safety and reliability of the selected material, and has strong feasibility; 2) the chitosan is the only macromolecular aminopolysaccharide with positive charge in nature, has biological functions of antibiosis, bacteriostasis, metal ion adsorption and the like, has no toxic or side effect, has good film-forming property and easy chemical modification property, and has excellent performance of being used as a PM2.5 filtering material, and the finally prepared shell PM2.5 biological filter membrane has multiple biological functions on the basis of effectively filtering PM2.5 particles; 3) the product meets the PM2.5 interception effect and other various biological functions of the PM2.5 biological filter membrane, and simultaneously utilizes nanotechnology to manufacture the PM2.5 biological filter membrane into an even nano-aperture structure, thereby ensuring the good air permeability and water vapor permeability of the PM2.5 biological filter membrane and ensuring the use comfort.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to be illustrative only and not to be limiting of the invention in any way, and any person skilled in the art can modify the present invention by applying the teachings disclosed above and applying them to equivalent embodiments with equivalent modifications. Any simple modification or equivalent changes made to the following embodiments according to the technical essence of the present invention, without departing from the technical spirit of the present invention, fall within the scope of the present invention.
Example 1
The embodiment provides a specific multifunctional PM2.5 biological filter membrane and a preparation method thereof, and the specific multifunctional PM2.5 biological filter membrane comprises the following steps:
1) dissolving chitosan with acetic acid to prepare a solution with the mass concentration of 1.2%, and stirring until the chitosan is completely dissolved, and sterilizing at high temperature and high pressure;
2) dropwise adding the dibutyl phthalate solution into the chitosan acetic acid solution, and ultrasonically mixing to prepare a chitosan solution containing 1.0% (v/v) dibutyl phthalate nanoparticles for later use;
3) immersing the electrostatic filter cotton in a chitosan solution to fully immerse the chitosan solution containing the dibutyl phthalate nanoparticles in the electrostatic filter cotton layer;
4) and drying the immersed electrostatic filter cotton, and then, washing the electrostatic filter cotton with ethanol to remove dibutyl phthalate to obtain the multifunctional PM2.5 biological filter membrane with the nano-aperture pores.
Example 2
The embodiment provides a specific multifunctional PM2.5 biological filter membrane and a preparation method thereof, and the specific multifunctional PM2.5 biological filter membrane comprises the following steps:
1) dissolving chitosan with acetic acid to prepare a solution with the mass concentration of 1.5%, and stirring until the chitosan is completely dissolved, and sterilizing at high temperature and high pressure;
2) dropwise adding the dibutyl phthalate solution into the chitosan acetic acid solution, and ultrasonically mixing to prepare a chitosan solution containing 0.5% (v/v) dibutyl phthalate nanoparticles for later use;
3) immersing the electrostatic filter cotton in a chitosan solution to fully immerse the chitosan solution containing the dibutyl phthalate nanoparticles in the electrostatic filter cotton layer;
4) and drying the immersed electrostatic filter cotton, and then, washing the electrostatic filter cotton with ethanol to remove dibutyl phthalate to obtain the multifunctional PM2.5 biological filter membrane with the nano-aperture pores.
Example 3 PM2.5 filtration experiment
Grouping experiments: the electrostatic filter cotton material without any treatment is used as a negative control group, the 3M PM2.5 filter mask is used as a positive control group, and the material is used as an experimental group. Each set was prepared with 20 parallel samples.
The testing process comprises the following steps: in a volume of 1m
3Place small-size PM2.5 tester in the transparent airtight container, set up a diameter in container one end and be 10 centimetres's blow vent, the vacuum pump is connected to the other end for after opening the vacuum pump, the air can stable speed pass through airtight container. Before use, the device components except for the vent were checked for tightness. Opening a vacuum pump to pump the closed container, and firstly measuring PM2.5 data M in the atmosphere
0Fixing the sample to be tested at the vent part, opening a vacuum pump to pump the closed container, and reading the PM2.5 data M on the closed container after the data of the instrument to be tested is stable
x. The PM2.5 retention rates of the negative control group, the positive control group and the experimental group were measured, respectively, according to the following formula.
R=（M
0-M
x）/M
0×100%
Statistical treatment: all data were statistically processed using SPSS12.0 statistical software, and comparisons between groups were by t-test, with P <0.05 indicating significant differences.
As a result: the PM2.5 particle retention rate of the negative control group is 83.27 +/-2.16%, the PM2.5 particle retention rate of the positive control group is 93.81 +/-2.54%, and the PM2.5 particle retention rate of the experimental group is 98.17 +/-1.29%. Compared with the negative control group, the PM2.5 particle retention rate of the positive control group and the experimental group exceeds 90% and has a significant difference (P < 0.05).
Table 1 PM2.5 filter test assay results (n = 20)
| Grouping | PM2.5 particle rejection |
| Negative control group | 83.27±2.16% |
| Positive control group | 93.81±2.54% |
| Experimental group | 98.17±1.29% |
EXAMPLE 4 bacteriostatic experiments
The bacteriostatic test method selects a quinine test. The principle of the test is that the bacterial suspension is directly dripped on an antibacterial product, a culture medium is covered, and the contact between the microorganism and the bacteriostatic agent is strengthened to show the bacteriostatic action of the product. The experiment judges whether the bacteriostatic ability is possessed according to the bacteriostatic rate. The test is suitable for the identification of the antibacterial (bacteriostatic) product of the non-dissoluble hard surface.
Test equipment: (1) staphylococcus aureus (ATCC 6538), Escherichia coli (25922), Candida albicans (ATCC 10231) bacterial suspensions. (2) Phosphate buffer (PBS, 0.03mol/L, pH 7.2-7.4). (3) Nutrient agar medium, sandcastle agar medium and semi-solid nutrient agar medium.
The operation procedure is as follows: (1) pour agar medium plate. (2) And (4) preparing a bacterial suspension. Diluting the bacterial suspension to 10
5cfu/ml～10
6cfu/ml was used as the test bacterial suspension. (3) And (3) sterilizing a sample to be tested, shearing the biological filter membrane into the shape same as the bottom of the flat plate before the experiment, and covering the bottom of the flat plate with the biological filter membrane. 0.1ml of test bacterial suspension is dripped into the center of the sample and is evenly coated, so that the distance between the bacterial liquid and the edge of the sample is 5 mm. (4) And (3) uniformly covering the surface of the fungus-infected sample wafer with 3.0-5.0 ml of semisolid agar, placing the fungus-infected sample wafer in a 37 ℃ incubator, and observing the result. Each experimental group was run in 5 replicates. (5) The test bacterial suspension was diluted appropriately to a concentration of 1X 10
3cfu/ml～2×10
3cfu/ml, 0.1ml of the cfu/ml was applied to a plate of the corresponding medium, spread, treated in the same manner as the test piece, and cultured by covering with semi-solid agar as a positive control. Positive control groups were run in 5 replicates. (6) In the test, the test bacterial suspension is used for counting the viable bacteria, and the culture counts of the test bacteria in the experimental group and the test bacteria in the control group are observed. (7) Test weightRepeat for 3 times. (8) The bacteriostasis rate is calculated according to the following formula.
As a result: the sample material can inhibit the growth of escherichia coli, staphylococcus aureus and candida albicans, the bacteriostasis rates within 72 hours are respectively 100%, 98.2% and 97.9%, and the bacteriostasis effect is good.
2.3 Metal ion adsorption test
Grouping experiments: the electrostatic filter cotton material without any treatment is used as a negative control group, the 3M PM2.5 filter mask is used as a positive control group, and the material is used as an experimental group. Each set was prepared with 20 parallel samples.
The testing process comprises the following steps: measuring 0ml, 2ml, 4ml, 6ml, 8ml and 10ml of metal ion standard solution to a 50ml volumetric flask by using a pipette respectively, shaking up, standing for 1min, diluting to a scale mark with water, shaking up, standing for 10min, and taking a reagent blank as a reference. And measuring the absorbance at the maximum absorption wavelength, and respectively drawing standard curves of iron ions, copper ions and calcium ions by taking the concentration of the metal ions as an abscissa and the absorbance as an ordinate. Weighing a certain amount of sample to be detected in an analytical balance, respectively placing the sample to be detected in three metal ion solutions, carrying out ultrasonic oscillation for 2h, taking out the sample, carrying out suction filtration, and measuring the absorbance value of the obtained filtrate. And calculating the metal ion adsorption amount according to the standard curve.
The result shows that the multifunctional PM2.5 biological filter membrane has a certain degree of adsorption capacity on iron ions, copper ions and calcium ions, wherein the adsorption capacity on the copper ions is strongest, the calcium ions are second, and the iron ions are lowest.
Table 2 maximum adsorption of iron, copper and calcium ions by multifunctional PM2.5 filters (n = 20)
| Grouping | Adsorption capacity g/kg |
| Copper ion | 15.09±1.24 |
| Calcium ion | 13.83±0.97 |
| Iron ion | 1.25±0.18 |
Claims (4)
1. A multifunctional PM2.5 biological filter membrane is characterized in that: the multifunctional biological filter membrane consists of a chitosan nano microporous membrane and organic electrostatic filter cotton, wherein the mass concentration of a used chitosan solution is 0.5-2.5%, the volume percentage of dibutyl phthalate in the solution is 0.5-2.5%, the content of the multifunctional biological filter membrane chitosan is 20-30%, the content of the organic electrostatic filter cotton is 75-80%, and the preparation method of the multifunctional PM2.5 biological filter membrane comprises the following steps:
1) dissolving chitosan with acetic acid to prepare a solution with the mass concentration of 0.5-2.5%, and stirring until the chitosan is completely dissolved, and sterilizing at high temperature and high pressure;
2) dropwise adding the dibutyl phthalate solution into the chitosan acetic acid solution, and ultrasonically mixing to prepare a chitosan solution containing 0.5-2.5% (v/v) dibutyl phthalate nanoparticles for later use;
3) immersing the electrostatic filter cotton in a chitosan solution to fully immerse the chitosan solution containing the dibutyl phthalate nanoparticles in the electrostatic filter cotton layer;
4) and drying the immersed electrostatic filter cotton, and then, leaching and washing the electrostatic filter cotton by using ethanol to remove dibutyl phthalate so as to obtain the multifunctional PM2.5 biological filter membrane with the nano-aperture pores.
2. A multifunctional PM2.5 biological filter membrane according to claim 1, characterised in that: the content of chitosan in the multifunctional biological filter membrane is 20%, and the content of the organic electrostatic filter cotton is 80%.
3. A multifunctional PM2.5 biological filter membrane according to claim 1 or claim 2, characterised in that: the deacetylation degree of the chitosan is 94.5%.
4. The use of the multifunctional PM2.5 biofiltration membrane of claim 1 as a PM2.5 mask and air purification device.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840774A (en) * | 2005-03-30 | 2006-10-04 | 中国科学技术大学 | Antibacterial active carbon fiber coated by chitosan porous membrane and process for preparing same |
| CN104815483A (en) * | 2015-04-20 | 2015-08-05 | 上海洁晟环保科技有限公司 | Composite anti-microbial air filtration material, preparation method and application |
| CN104892969A (en) * | 2015-06-23 | 2015-09-09 | 武汉工程大学 | Composite chitosan and cellulose membrane and preparation method and application thereof |
| CN106362601A (en) * | 2016-09-28 | 2017-02-01 | 扬州云彩新材料科技有限公司 | Nano fiber membrane filtering material with antibacterial function and preparation method thereof |
| CN106512759A (en) * | 2016-12-06 | 2017-03-22 | 周潇潇 | Macromolecule filter membrane material |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840774A (en) * | 2005-03-30 | 2006-10-04 | 中国科学技术大学 | Antibacterial active carbon fiber coated by chitosan porous membrane and process for preparing same |
| CN104815483A (en) * | 2015-04-20 | 2015-08-05 | 上海洁晟环保科技有限公司 | Composite anti-microbial air filtration material, preparation method and application |
| CN104892969A (en) * | 2015-06-23 | 2015-09-09 | 武汉工程大学 | Composite chitosan and cellulose membrane and preparation method and application thereof |
| CN106362601A (en) * | 2016-09-28 | 2017-02-01 | 扬州云彩新材料科技有限公司 | Nano fiber membrane filtering material with antibacterial function and preparation method thereof |
| CN106512759A (en) * | 2016-12-06 | 2017-03-22 | 周潇潇 | Macromolecule filter membrane material |
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