CN108379933B - Silk fibroin nanofiber filtering material and air filtering equipment based on filtering material - Google Patents
Silk fibroin nanofiber filtering material and air filtering equipment based on filtering material Download PDFInfo
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- CN108379933B CN108379933B CN201810138468.5A CN201810138468A CN108379933B CN 108379933 B CN108379933 B CN 108379933B CN 201810138468 A CN201810138468 A CN 201810138468A CN 108379933 B CN108379933 B CN 108379933B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/02—Loose filtering material, e.g. loose fibres
- B01D39/04—Organic material, e.g. cellulose, cotton
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/30—Particle separators, e.g. dust precipitators, using loose filtering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0631—Electro-spun
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2258/00—Sources of waste gases
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Abstract
The invention provides a silk fibroin nanofiber filtering material and air filtering equipment based on the filtering material. The silk fibroin nanofiber filtering material is obtained by combining an electrostatic spinning technology with ethanol and water vapor post-treatment, and has the advantages of environmental protection, good biocompatibility, high filtering efficiency and the like.
Description
Technical Field
The invention relates to a silk fibroin nanofiber filtering material and air filtering equipment based on the filtering material.
Background
In recent years, air pollution, especially particulate air pollution (haze), has become an important environmental problem, in which PM2.5 and smaller particles can enter alveoli of human body and even pass through cell membrane to enter other organs, posing a serious threat to human health. How effectual haze protection that carries on receives extensive concern, develops the novel PM2.5 protective facial mask of high-efficient low resistance and becomes market demand.
With the development of nanotechnology, the electrostatic spinning technology becomes a main method for preparing nanofibers, and the electrostatic spinning nanofibers as air filter materials have the advantages of large specific surface area, strong adsorption capacity and the like, can effectively improve the filtration efficiency of fine particles, and reduce air resistance through the special 'slip effect' of nanometer size. Most of the existing nanofiber filter materials are chemically synthesized copolymers or carbon nano tubes and graphene-based materials, and the nanofibers have the problems of uncertain toxicity, environmental pollution caused by the preparation process or harm to human bodies and the like, so that the conventional nanofiber filter materials can have various problems when being used for daily protective masks.
In order to solve the problem, various methods are adopted in the prior art, for example, CN201510009971.7 is an efficient and low-resistance nanofiber air filter material for masks and a preparation method thereof, the nanofiber air filter material adopts a sandwich structure, the upper layer and the lower layer are nanofiber layers in a uniform cylindrical shape, and the middle is a nanofiber layer with beads. For another example, titanium dioxide is added into a polymer solution, and after electrostatic spinning, the surface appearance of the obtained fiber membrane has a porous structure, so that the filtration efficiency is increased, and the filtration resistance is reduced. However, the above processes have the problems of complicated process, low production efficiency, increased cost, poor uniformity of pores of the nanofiber membrane, poor filtration performance of the membrane, and the like.
As a natural protein fiber that has been used for thousands of years, silk is a renewable natural material that is abundant in sources, edible, biocompatible, and environmentally friendly. The silk is mainly composed of silk fibroin and sericin, wherein the silk fibroin is used as a main component and accounts for about 70-80% of the total mass of the silk. The fibroin obtained after degumming the silk is used for preparing the nanofiber for the air filter material by the electrostatic spinning technology, and has higher market value. However, mulberry silk has the problems of water shrinkage, large fiber brittleness, poor mechanical properties and the like. The materials with different forms such as membranes, non-woven nets, porous scaffolds and the like, which are prepared by directly drying, electrostatic spinning or freeze drying the regenerated silk fibroin solution under the prior art conditions, mainly have random curls as aggregation structures, weak intermolecular binding force and high dissolution rate in water, and limit the application of the silk fibroin material in biomedical materials. CN201610539592.3 is an air filtration device based on silk nanofibers, but its filtration efficiency is not stable under high humidity environment, and is not suitable for long-term use. Therefore, the silk fibroin nanofiber-based filtering material prepared by the invention can meet the requirements of environmental protection, high filtering efficiency and good air permeability, and can ensure stable filtering efficiency in a high-humidity environment, the filtering efficiency is not remarkably reduced, and the service life is long.
Disclosure of Invention
One of the purposes of the invention is to provide a silk fibroin nanofiber filtering material.
The invention also aims to provide a preparation method of the silk fibroin nanofiber filter material.
The invention also aims to provide air filtering equipment adopting the silk fibroin nanofiber filtering material.
The invention adopts the following technical scheme that the silk fibroin nanofiber filtering material is prepared by obtaining the silk fibroin nanofibers through electrostatic spinning, soaking the silk fibroin nanofibers obtained through electrostatic spinning in ethanol or ethanol solution for more than 30s, preferably 30-120s, drying and then performing water vapor treatment for more than 1 time, wherein the treatment time is more than 30s, preferably 30-90s, and the silk fibroin nanofiber filtering material is obtained.
Preferably, the gram weight of the silk fibroin nanofibers is 50g/m2Below, preferably 10g/m2Hereinafter, 2g/m is more preferable2More preferably 0.1 to 1.5g/m2。
Preferably, the diameter of the silk fibroin nanofiber is within the range of 100-800nm, preferably within the range of 120-780 nm.
A preparation method of a silk fibroin nanofiber filter material, which is characterized in that,
(1) removing sericin from the silk to obtain silk fibroin fiber;
(2) dissolving the mixture in a solution system, and desalting to obtain a spinning solution;
(3) performing electrostatic spinning on the obtained spinning solution to obtain silk fibroin nanofibers;
(4) soaking the silk fibroin nanofiber obtained by electrostatic spinning in ethanol or ethanol solution for more than 30s, preferably 30-120s, drying, and then carrying out water vapor treatment for more than 1 time for more than 30s, preferably 30-90s to obtain the silk fibroin nanofiber filtering material.
The specific preparation method is that silk fibroin nano-fiber is prepared by using silkworm cocoon silk as a raw material and utilizing a roller type receiving electrostatic spinning device.
Boiling silkworm cocoon in sodium bicarbonate water solution to remove sericin, and placing silk fibroin fiber in CaCl2/C2H5OH/H2Dissolving the solution in the ternary salt solution system at high temperature, dialyzing the solution in deionized water to obtain a silk fibroin aqueous solution, and centrifuging the silk fibroin aqueous solution to remove precipitates. And (3) putting the silk fibroin solution into a refrigerator to be frozen into ice, and then freezing and drying to obtain the silk fibroin sponge. Dissolving the obtained silk fibroin sponge in formic acid to obtain a silk fibroin formic acid solution;
by utilizing the electrostatic spinning technology, the working voltage is positive and high-voltage 20kV, the negative and high-voltage-3 kV, the spinning distance is 20cm, the translation stroke is 300mm, the translation speed is 500mm/min, and the receiving speed of a winding roller is 100 r/min. The injection speed of the silk fibroin formic acid solution is 0.8ml/hPerforming electrostatic spinning to deposit the silk fibroin nano-fiber at 10-30 g/m2Nonwoven (e.g. 10 g/m)2、20g/m2、30g/m2) Obtaining the silk fibroin nano-fiber.
Treating the silk fibroin nanofiber membrane with ethanol and water vapor: soaking the silk fibroin nanofiber membrane obtained by electrostatic spinning in ethanol for multiple times, then airing, carrying out multiple water vapor treatment on the sample after ethanol treatment, and then airing.
An air filtration device employing silk fibroin nanofiber filtration material, comprising:
an optional substrate layer, wherein the substrate layer,
the silk fibroin nanofiber filter material, and
optionally a cover layer.
Preferably, the equipment is a mask, and is characterized in that the mask is formed by sequentially overlapping and compounding more than four layers of structures, wherein the structures are sequentially arranged from inside to outside and respectively comprise a non-woven fabric layer (1), a melt-blown fabric layer and/or an electrostatic electret material layer (2), a silk fibroin nanofiber filter material layer (3) and a non-woven fabric layer (4).
Preferably, the gram weight of the non-woven fabric layer is 10-30 g/m2。
Preferably, the gram weight of the melt-blown fabric layer is 20-80 g/m2。
Preferably, the gram weight of the electrostatic electret material layer is 30-100 g/m2。
The term "silk fibroin nanofibers" as used herein refers to regenerated silk fibroin fibers having a diameter on the nanometer (nm) scale, e.g., the diameter can be in the range of 10-1500nm, particularly 50-1000 nm. In some embodiments of the invention, the silk fibroin nanofibers have a diameter in the range of 100-800 nm. The silk fibroin nanofiber of the present invention can be prepared by using natural silk or silk leftovers as starting materials, or by other methods known in the art, and the raw materials are not limited to natural silk.
As used herein, the terms "silk fibroin nanofibers" and "silk fibroin nanofiber membrane" are used interchangeably and refer to a layer of non-woven structural fibers formed from regenerated silk fibroin nanofibers.
The term "grammage" as used herein refers to the mass of a material per unit area of size. The grammage can be used to describe the thickness of the silk fibroin nanofiber membrane. For example, the silk fibroin nanofiber membranes of the present invention can have a basis weight of less than 10g/m2。
The term "air filtration device" as used herein is to be understood in a broad sense and includes respirators, air conditioners, residential air purifiers, industrial air filters, and the like.
The term "mask" as used herein is to be understood broadly as referring to an air filtration device for wearing by a person. Typical masks are cotton gauze masks, KN90 masks, and the like.
The term "optionally" as used herein means "optionally" or "not necessarily". For example, "optional substrate layer" means that the substrate layer may or may not be present, which can be selected by one skilled in the art as the case may be.
Advantageous effects
1. The silk fibroin nanofiber filtering material suitable for air filtration is obtained by combining an electrostatic spinning technology with ethanol and water vapor post-treatment, and is high in filtering efficiency, good in filtering stability in a high-humidity environment, and good in durability and size stability.
2. The preparation process is simple, has good structural controllability, and can control the filtration stability of the silk fibroin nanofiber filtering material by controlling the electrostatic spinning process and the ethanol and water vapor treatment process.
3. The raw materials of the filter material are renewable natural materials, the source of the filter material is rich, the biocompatibility is good, the filter material is environment-friendly, and the filter material cannot cause environmental pollution or harm to human bodies.
4. The filtering effect of the filtering material of the invention meets the requirements of national standard GB2626-2006 and American standard NOISH standard in China.
Drawings
Fig. 1 is a scanning electron microscope image of silk fibroin nanofibers prepared by the electrospinning technique of the present invention.
Fig. 2 is a curve showing the change of loading filtration efficiency of the silk fibroin nanofibers after ethanol and water vapor treatment.
Detailed Description
The invention will be further explained with reference to specific examples.
Example 1: silk fibroin nanofiber membrane prepared from silkworm cocoon silk serving as raw material by using roller type receiving electrostatic spinning equipment
Boiling silkworm cocoon in 0.5 wt% sodium bicarbonate water solution for 30min to remove sericin, and placing silk fibroin fiber in CaCl2/C2H5OH/H2Dissolving O (molar ratio 1:2:8) in ternary salt solution system at 80 deg.C for 2h, dialyzing in deionized water for three days to obtain silk fibroin aqueous solution, centrifuging silk fibroin solution at 3500r/min for 5min, and removing precipitate. And (3) freezing the silk fibroin solution into ice at the temperature of-4 ℃, and then freezing and drying to obtain the silk fibroin sponge. Dissolving the obtained silk fibroin sponge in 98-100% anhydrous formic acid to obtain 20 wt% silk fibroin formic acid solution. Then, by utilizing an electrostatic spinning technology, the working voltage is positive 20kV, the negative high voltage is-3 kV, the spinning distance is 20cm, the translation stroke is 300mm, the translation speed is 500mm/min, and the receiving speed of a winding roller is 100 r/min. The injection speed of the silk fibroin formic acid solution is 0.8ml/h, electrostatic spinning is carried out, and the silk fibroin nano-fiber is deposited at 10g/m2The nano/micron composite filter material is obtained on the non-woven fabric.
The appearance of the electrostatic spinning cellulose nanofiber is shown in figure 1, the upper layer is silk fibroin nanofiber, and the lower layer is traditional micron-sized non-woven fabric filter material. The diameter range of the silk fibroin nano-fiber obtained under the electrospinning condition is 0.25-0.63 μm, and the average diameter is about 0.43 μm. By controlling the electrostatic spinning deposition time, the filtration efficiency and air resistance of the obtained silk fibroin nanofiber membrane to PM2.5 can be controlled. E.g. at 10g/m2As a nonwoven fabricWhen the silk fibroin nanofibers are used for bearing a substrate, under the electrospinning condition, the silk fibroin nanofiber membrane is semitransparent after 10min of electrospinning, and the silk fibroin nanofiber membranes with different weights are obtained after 10min,20min, 30min, 40min and 50min of electrospinning, and the thin silk fibroin nanofibers are difficult to support in a large area, so that the weight of the thin silk fibroin nanofibers is 10g/m2The non-woven fabric is a substrate layer and a covering layer, a filter disc with a sandwich structure of non-woven fabric + silk fibroin nanofiber membrane + non-woven fabric is manufactured, and the filtering efficiency and the filtering resistance are tested, and the specific test is shown in the following table 1.
TABLE 1 filtration efficiency and filtration resistance of Filter discs of Sandwich construction
Wherein the filtration efficiency of the mask meeting KN90 can be obtained by spinning for 30min, the pressure drop is less than 60Pa, and the filtration efficiency of the silk fibroin nanofiber membrane obtained by spinning for 50min to PM2.5 reaches 99.6%, while the pressure drop is only 94.1 Pa. In PM2.5In the standard of protective masks, the air resistance of a secondary filtering-effect mask with the filtering efficiency of more than 90% is less than 100Pa, the air resistance of a primary filtering-effect mask with the filtering efficiency of more than 95% is less than 120Pa, and the silk fibroin nanofiber membrane prepared by the method completely meets and is far superior to the standard of the protective masks when used as an air filtering material.
Example 2: silk fibroin nanofiber membrane prepared by ethanol and water vapor treatment
Under the electrospinning conditions described in example 1, at a rate of 10g/m2The non-woven fabric is used as a silk fibroin nanofiber carrying substrate, a silk fibroin nanofiber membrane with the electrostatic spinning time of 50min is made into a filter disc with a sandwich structure of 'non-woven fabric + silk fibroin nanofiber membrane + non-woven fabric', the filter disc is soaked in ethanol for 30s and dried, then the filter disc is subjected to one or more water vapor treatments for 30s and dried, the filter disc is placed in a simulated mask wearing environment (85% high humidity environment, 25 ℃ normal temperature), and the filtration efficiency of the filter disc is tested at 0, 1, 2, 4, 8, 15, 30 and 60min in the temperature and humidity environment, which is shown in table 2, compared with the untreated silk fibroin nanofiber membraneCompared with the prior art, the filter disc treated by ethanol and water vapor has obviously prolonged filtration efficiency retention time under high-humidity environment.
TABLE 2 filtration efficiency of Sandwich-structured filter elements after ethanol and steam treatment
While the invention has been described in conjunction with specific embodiments thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art. Accordingly, the present invention is intended to embrace all such alternatives, modifications and variances which fall within the spirit and broad scope of the appended claims. All publications, patents and patent applications mentioned in this specification are herein incorporated in their entirety by reference into the specification, to the same extent as if each individual publication, patent or patent application was specifically and individually indicated to be incorporated herein by reference. In addition, citation or identification of any reference in this application shall not be construed as an admission that such reference is available as prior art to the present invention.
Claims (21)
1. The silk fibroin nanofiber filtering material is characterized in that silk fibroin nanofibers are obtained through electrostatic spinning, the silk fibroin nanofibers obtained through electrostatic spinning are soaked in ethanol or an ethanol solution for more than 30s, water vapor treatment is carried out for more than 1 time after drying, and the silk fibroin nanofiber filtering material is obtained after the treatment time is more than 30 s.
2. The silk fibroin nanofiber filter material of claim 1, wherein the silk fibroin nanofibers obtained by electrospinning are soaked in ethanol or an ethanol solution for 30-120 s.
3. The silk fibroin nanofiber filter material of claim 1, wherein the treatment time is 30-90 s.
4. The silk fibroin nanofiber filter material of claim 1, wherein the silk fibroin nanofibers have a grammage of 50g/m2The following.
5. The silk fibroin nanofiber filter material of claim 1, wherein the silk fibroin nanofibers have a grammage of 10g/m2The following.
6. The silk fibroin nanofiber filter material of claim 1, wherein the silk fibroin nanofibers have a grammage of 2g/m2The following.
7. The silk fibroin nanofiber filter material of claim 1, wherein the gram weight of the silk fibroin nanofibers is 0.1-1.5 g/m2。
8. The silk fibroin nanofiber filter material of claim 1, wherein the silk fibroin nanofibers have a diameter in the range of 100-800 nm.
9. The silk fibroin nanofiber filter material of claim 1, wherein the silk fibroin nanofibers have a diameter in the range of 120-780 nm.
10. A method of preparing the silk fibroin nanofiber filter material of claim 1, wherein:
(1) removing sericin from the silk to obtain silk fibroin fiber;
(2) dissolving the mixture in a solution system, and desalting to obtain a spinning solution;
(3) performing electrostatic spinning on the obtained spinning solution to obtain silk fibroin nanofibers;
(4) and soaking the silk fibroin nanofiber obtained by electrostatic spinning in ethanol for more than 30s, drying, and then performing steam treatment, wherein the number of times of steam treatment is more than 1, and the time is more than 30s, so as to obtain the silk fibroin nanofiber filtering material.
11. The preparation method of the silk fibroin nanofiber filter material of claim 10, wherein the silk fibroin nanofibers obtained by electrospinning are soaked in ethanol for 30-120 s.
12. The method of claim 10, wherein the silk fibroin nanofiber filter material has a grammage of 50g/m2The following.
13. The method of claim 10, wherein the silk fibroin nanofiber filter material has a grammage of 10g/m2The following.
14. The method of claim 10, wherein the silk fibroin nanofiber filter material has a grammage of 2g/m2The following.
15. The method for preparing the silk fibroin nanofiber filter material of claim 10, wherein the gram weight of the silk fibroin nanofibers is 0.1-1.5 g/m2。
16. The method for preparing the silk fibroin nanofiber filter material of claim 10, wherein the diameter of the silk fibroin nanofiber is within the range of 100-800 nm.
17. The method for preparing the silk fibroin nanofiber filter material of claim 10, wherein the diameter of the silk fibroin nanofibers is within the range of 120-780 nm.
18. An air filter device using the filter material of claim 1, comprising:
an optional substrate layer, wherein the substrate layer,
the silk fibroin nanofiber filter material of claim 1, and
optionally a cover layer.
19. The air filtration device of claim 18, wherein the device is a mask, wherein the mask is formed by sequentially overlapping and compounding more than four layers of structures, and the structures are sequentially arranged from inside to outside and respectively comprise a non-woven fabric layer (1), a melt-blown fabric layer and/or an electrostatic electret material layer (2), a silk fibroin nanofiber filter material layer (3) and a non-woven fabric layer (4).
20. An air filtration device as recited in claim 19, wherein the nonwoven fabric layer has a grammage of 10 to 30g/m2。
21. An air filtration device as recited in claim 19 wherein the meltblown fabric layer has a grammage of 20 to 80g/m2The gram weight of the electrostatic electret material layer is 30-100 g/m2。
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| CN201810138468.5A CN108379933B (en) | 2018-02-10 | 2018-02-10 | Silk fibroin nanofiber filtering material and air filtering equipment based on filtering material |
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| CN111350029A (en) * | 2020-02-02 | 2020-06-30 | 江苏大学 | Fibroin-based multifunctional nanofiber membrane for smoke filtration and preparation method thereof |
| GB202005276D0 (en) * | 2020-04-09 | 2020-05-27 | Whitfield James | An air filter |
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| WO2014012099A1 (en) * | 2012-07-13 | 2014-01-16 | Tufts University | Encapsulation of fragrance and/or flavors in silk fibroin biomaterials |
| CN104474914A (en) * | 2014-12-09 | 2015-04-01 | 张丽明 | Nano filtering membrane containing silk fibroin and preparation method thereof |
| CN104621784A (en) * | 2015-03-07 | 2015-05-20 | 黄学亮 | Respirator for preventing automobile exhaust and haze |
| CN106422522A (en) * | 2015-08-11 | 2017-02-22 | 清华大学 | Silk nano-fiber-based air filtering device |
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| WO2014012099A1 (en) * | 2012-07-13 | 2014-01-16 | Tufts University | Encapsulation of fragrance and/or flavors in silk fibroin biomaterials |
| CN104474914A (en) * | 2014-12-09 | 2015-04-01 | 张丽明 | Nano filtering membrane containing silk fibroin and preparation method thereof |
| CN104621784A (en) * | 2015-03-07 | 2015-05-20 | 黄学亮 | Respirator for preventing automobile exhaust and haze |
| CN106422522A (en) * | 2015-08-11 | 2017-02-22 | 清华大学 | Silk nano-fiber-based air filtering device |
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| Title |
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