CN114984665A - Branched completely-degradable nanofiber mask filter element material and preparation method thereof - Google Patents
Branched completely-degradable nanofiber mask filter element material and preparation method thereof Download PDFInfo
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 80
- 239000000463 material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 123
- 239000004626 polylactic acid Substances 0.000 claims abstract description 123
- 238000009987 spinning Methods 0.000 claims abstract description 80
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 46
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 21
- 239000011162 core material Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 94
- 239000000243 solution Substances 0.000 claims description 82
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 claims description 46
- 238000003756 stirring Methods 0.000 claims description 35
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 28
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 26
- 239000004744 fabric Substances 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims description 2
- 238000001523 electrospinning Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 24
- 239000011148 porous material Substances 0.000 abstract description 6
- 239000012528 membrane Substances 0.000 abstract description 5
- 230000002045 lasting effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 description 9
- 239000000835 fiber Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 241000711573 Coronaviridae Species 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000013502 plastic waste Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
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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
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/02—Layered materials
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
- D01D5/0084—Coating by electro-spinning, i.e. the electro-spun fibres are not removed from the collecting device but remain integral with it, e.g. coating of prostheses
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4326—Condensation or reaction polymers
- D04H1/435—Polyesters
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D2500/00—Materials for garments
- A41D2500/30—Non-woven
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D2500/00—Materials for garments
- A41D2500/50—Synthetic resins or rubbers
-
- 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
- B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
- B01D2239/025—Types of fibres, filaments or particles, self-supporting or supported materials comprising nanofibres
-
- 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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- General Health & Medical Sciences (AREA)
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Abstract
The invention belongs to the field of air filtration, relates to preparation of mask filter core materials, and particularly relates to a branched completely degradable nanofiber mask filter core material and a preparation method thereof. Polylactic acid is used as a raw material, based on the extremely dilute solution spinning theory, the branched PLA nanofiber with the average diameter of 35-45nm is prepared by an electrostatic spinning technology, and a multi-scale three-dimensional space structure with stacked coarse and fine nanofibers is constructed on the basis, so that efficient, low-resistance and lasting and stable filtration of nano-grade pore diameters is realized. And the PLA non-woven fabric is taken as a base material, and the branched PLA nanofiber membrane is sprayed and coated on the base material through an electrostatic spinning process to form the nanofiber mask filter element and is used for producing masks. The product has excellent filtering performance, the filtering efficiency is as high as 99.99%, the filtering resistance is only 106Pa, and the prepared branched nano-fiber mask filter core material is completely biodegradable.
Description
Technical Field
The invention belongs to the field of air filtration, relates to preparation of mask filter core materials, and particularly relates to a branch-shaped completely degradable nanofiber mask filter core material and a preparation method thereof.
Background
First, the need and usage of masks have exploded due to the aggravation of air pollution and the global outbreak of new coronaviruses. However, the large amount of plastic waste caused by the use and incorrect treatment of the disposable masks further aggravates the white plastic pollution and causes great harm to the environment. According to the latest report published by Oceans Asia, ocean protection organization shows that about 520 hundred million masks are produced globally in 2020, and at least 15.6 hundred million masks are littered into the ocean, seriously threatening the ocean ecological environment. Because the main raw materials of the existing mask are polypropylene (PP) and the like, the degradation in the environment may require 400 + 500 years, and the decomposed plastic fragments can cause continuous harm to the environment.
Secondly, the outbreak of new crown epidemic situation leads to unprecedented improvement of personal hygiene protection consciousness, and the demand of people on the biosafety protection mask product is sharply increased. However, the traditional mask on the market at present has the problems of no degradability, poor filtering durability and the like.
In addition, at the present stage, the mask industry in China mainly focuses on repeated manufacturing with low technical content, and the traditional single melt-blown fiber filter material depends on a filtering mechanism of electrostatic adsorption, so that the filtering performance of the traditional mask is unstable, the service life of the traditional mask is short, and the like. Compared with the traditional gauze mask filter element on the market, the electrostatic spinning nanofiber material is widely applied to the field of air filtration due to the fact that the fineness of the fibers is in the nanometer level, the specific surface area is large, the pore size is small, the porosity is high, functional modification is easy to achieve, and the like. However, the conventional electrospun fiber has the fiber diameter of more than 100nm, is difficult to further refine, seriously limits the great improvement of the filtering performance of the material, and still has the bottleneck problem of insufficient filtering efficiency of particulate matters with the most penetrable particle size (0.3 mu m). Therefore, the development of the biodegradable branched nanofiber mask filter core material with excellent filtering performance and lasting stability is of great significance.
Disclosure of Invention
Aiming at the technical problems, the invention provides a branched completely degradable nanofiber mask filter element material and a preparation method thereof. Selecting a green bio-based degradable material polylactic acid, and successfully preparing the branched nano-fiber with the diameter being 10 times thinner than that of the conventional nano-fiber by an electrostatic spinning technology based on the extremely dilute solution theory, wherein the diameter is distributed between 35 and 45 nm. By regulating the proportion of thick and thin fibers, a multi-scale three-dimensional space structure with stacked thick and thin nanofibers is successfully constructed, high-efficiency and low-resistance filtration of nanometer-level pores is realized, and high-efficiency filtration performance on harmful particulate matters of PM10, PM5, PM2.5, even PM0.3 level with the strongest penetrability is achieved. The constructed multi-scale three-dimensional space filtering structure can capture particles through physical interception instead of electrostatic adsorption, so that the filtering stability and durability of the mask are greatly improved.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the utility model provides a branching form complete degradable nanofiber gauze mask filter core material, by branching form polylactic acid nanofiber and polylactic acid non-woven fabrics complex composition, wherein branching form polylactic acid nanofiber's average diameter is 35-45nm, and filter core material's overall structure is the multiscale three-dimensional space structure that thick, thin nanofiber pile up.
Furthermore, the branched polylactic acid nano fiber is spun on the composite surface of the polylactic acid non-woven fabric.
Further, the preparation method of the branched completely degradable nanofiber mask filter element material comprises the following steps:
(1) preparing a polylactic acid spinning solution: adding the polylactic acid master batch into the mixed solution, and violently stirring to obtain a polylactic acid spinning solution;
(2) preparing an ultra-thin polylactic acid spinning solution: adding tetrabutylammonium chloride into the mixed solution, and carrying out first vigorous stirring to prepare a tetrabutylammonium chloride mixed solution; adding the polylactic acid master batch into the tetrabutylammonium chloride mixed solution, and carrying out secondary vigorous stirring to prepare an ultra-dilute polylactic acid spinning solution;
(3) preparing polylactic acid nano fibers: filling the polylactic acid spinning solution obtained in the step (1) into a needle tube, and spinning the polylactic acid spinning solution to the surface of a polylactic acid non-woven fabric through electrostatic spinning to obtain polylactic acid nano fiber;
(4) preparing a branched completely degradable nanofiber mask filter element material: and (3) filling the ultra-dilute polylactic acid spinning solution obtained in the step (2) into a needle tube, and spinning the ultra-dilute polylactic acid spinning solution onto the surface of the polylactic acid nano-fiber obtained in the step (3) through electrostatic spinning to obtain the branched completely degradable nano-fiber mask filter element material.
Further, M of the polylactic acid master batch in the step (1) W 200000, the addition amount is 12% of the polylactic acid spinning solution, the mixed solution is N, N-dimethyl formamide and dimethyl carbonate, and the volume ratio of the N, N-dimethyl formamide to the dimethyl carbonate is 3: 7.
Further, the temperature of the violent stirring in the step (1) is 65 ℃, the rotation speed of the violent stirring is 400r/min, and the time of the violent stirring is 6 hours; the concentration of the polylactic acid spinning solution prepared in the step (1) is 10-15%.
Further, the mixed solution in the step (2) is N, N-dimethylformamide and dimethyl carbonate, the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 5:5, the temperature of the first violent stirring is 45 ℃, the rotation speed of the violent stirring is 400r/min, and the time of the violent stirring is 2 hours; the concentration of tetrabutylammonium chloride is 3% -7%, the addition amount of the polylactic acid master batch is 7% of the ultra-dilute polylactic acid spinning solution, the second vigorous stirring temperature is 65 ℃, the vigorous stirring rotating speed is 400r/min, the vigorous stirring time is 6h, and the concentration of the ultra-dilute polylactic acid spinning solution prepared in the step (2) is 1-7%.
Further, the gram weight of the non-woven fabric in the step (3) is 50g/m 2 The electrostatic spinning conditions are as follows: the voltage of the high-voltage generator is 20-30 kV; the distance from the nozzle to the non-woven fabric is 15-18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.5-3.0 mL/h; the receiving time is 10-60 min.
Further, the diameter of the polylactic acid nano fiber prepared in the step (3) is 100-400nm, and the aperture is more than 0 and less than or equal to 10 μm.
Further, the electrostatic spinning conditions in the step (4) are as follows: the voltage of the high-voltage generator is 20-30 kV; the distance from the nozzle to the receiving base cloth is 15-18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.3-1.0 mL/h; the receiving time is 10-60 min.
Further, the diameter of the branched completely degradable nanofiber mask filter core material prepared in the step (4) is 25-100nm, and the aperture is more than 0 and less than or equal to 10 microns.
Furthermore, the branched completely degradable nanofiber mask filter element material is applied to the mask.
Further, the application is as follows: spinning the branched completely degradable nano fiber mask filter element material on polylactic acid non-woven fabric (50 g/m) 2 ) And (5) carrying out ultrasonic compounding on the surface to obtain the mask.
The invention has the following beneficial effects:
1. the polylactic acid selected in the invention is a green bio-based degradable material, and the branched polylactic acid nanofiber is a branched nanofiber which is 10 times thinner than the conventional nanofiber in diameter and is distributed between 35 and 45nm, and is successfully prepared by an electrostatic spinning technology based on the extremely dilute solution theory. Meanwhile, a multi-scale three-dimensional space structure with stacked coarse and fine nano fibers is successfully constructed by regulating the proportion of the coarse and fine fibers, high-efficiency and low-resistance filtration of nano-grade apertures is realized, and high-efficiency filtration performance on harmful particulate matters of PM10, PM5, PM2.5 and even PM0.3 grade with the strongest penetrability is achieved. The constructed multi-scale three-dimensional space filtering structure can capture particles through physical interception instead of electrostatic adsorption, so that the filtering stability and durability of the mask are greatly improved.
2. The product has excellent filtering performance, the filtering efficiency is as high as 99.99%, and the filtering resistance is only 106 Pa.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an electron microscope image of a PLA coarse nanofiber membrane prepared in step (3) of example 1 of the present invention.
FIG. 2 is an electron microscope image of the branched PLA nanofiber membrane prepared in step (4) of example 1 of the present invention.
Fig. 3 is a diagram of a multi-scale PLA nanofiber mask filter element prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art based on the embodiments of the present invention without inventive step, are within the scope of the present invention.
Example 1
The embodiment is a preparation method of a branched completely degradable nanofiber mask filter element material, which comprises the following steps:
(1) weighing polylactic acid master batch (M) W = 200000) to a mixture containing only N, N-Dimethylformamide (DMF) and dimethyl carbonate (DMC) at 65%Violently stirring for 6 hours at the temperature of 400r/min to prepare spinning solution with the concentration of the polylactic acid of 10 percent; the adding amount of the polylactic acid master batch is 12 percent of the polylactic acid spinning solution, and the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 3: 7;
(2) weighing tetrabutylammonium chloride, adding the tetrabutylammonium chloride into a mixed solution only containing N, N-Dimethylformamide (DMF) and dimethyl carbonate (DMC), and vigorously stirring for 2 hours at the temperature of 45 ℃ and at the speed of 400r/min to prepare a mixed solution with the tetrabutylammonium chloride concentration of 3%. Adding a certain mass of polylactic acid master batch, and violently stirring for 6 hours at the temperature of 65 ℃ and at the speed of 400r/min to prepare an ultra-dilute spinning solution with the polylactic acid concentration of 3%; the addition amount of the polylactic acid master batch is 7 percent of the ultra-dilute polylactic acid spinning solution, and the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 5: 5;
(3) putting the spinning solution obtained in the step (1) into a needle tube, performing electrostatic spinning, and spinning the spinning solution on the surface of polylactic acid non-woven fabric (the gram weight of the non-woven fabric is 50 g/m) 2 ). Electrostatic spinning conditions are as follows: the voltage of the high-voltage generator is 25 kV; the distance from the nozzle to the receiving base cloth is 18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.8 mL/h; the receiving time is 20 min;
(4) and (3) filling the spinning solution obtained in the step (2) into a needle tube, carrying out electrostatic spinning, and spinning the spinning solution on the surface of the polylactic acid nano fiber obtained in the step (3). Electrostatic spinning conditions: the voltage of the high-voltage generator is 25 kV; the distance from the nozzle to the receiving base cloth is 18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.5 mL/h; the receiving time is 20 min.
The diameter of the PLA nanofiber obtained in the step (3) is 150-250nm, and the pore diameter is more than 0 and less than or equal to 6 mu m.
The diameter of the PLA superfine nano-fiber obtained in the step (4) is 50-80nm, and the aperture is more than 0 and less than or equal to 3 mu m.
Fig. 1 shows the PLA coarse nanofiber membrane prepared in step (3) of this example 1, and it can be seen from fig. 1 that the PLA nanofibers have good morphology, uniform diameter and distribution, and no beaded structure.
FIG. 2 is an electron microscope image of the branched PLA nanofiber membrane prepared in step (4) of example 1 of the present invention, wherein the diameter of the coarse fiber is 150-300nm, and the diameter of the fine fiber is 35-45 nm.
Fig. 3 is a schematic diagram of a multi-scale PLA nanofiber mask filter element prepared in example 1 of the present invention.
Example 2
The embodiment is a preparation method of a branched completely degradable nanofiber mask filter element material, which comprises the following steps:
(1) weighing polylactic acid master batch (M) W = 200000) is added into a mixed solution only containing N, N-Dimethylformamide (DMF) and dimethyl carbonate (DMC), and the mixture is stirred vigorously for 6 hours at the temperature of 65 ℃ and the speed of 400r/min, so as to prepare a spinning solution with the polylactic acid concentration of 13%; the addition amount of the polylactic acid master batch is 12 percent of the polylactic acid spinning solution, and the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 3: 7.
(2) Weighing tetrabutylammonium chloride, adding the tetrabutylammonium chloride into a mixed solution only containing N, N-Dimethylformamide (DMF) and dimethyl carbonate (DMC), and vigorously stirring for 2 hours at the temperature of 45 ℃ and at the speed of 400r/min to prepare a mixed solution with the tetrabutylammonium chloride concentration of 5%. Adding a certain mass of polylactic acid master batch, and violently stirring for 6 hours at the temperature of 65 ℃ and at the speed of 400r/min to prepare an ultra-dilute spinning solution with the polylactic acid concentration of 3%; the addition amount of the polylactic acid master batch is 7 percent of the ultra-dilute polylactic acid spinning solution, and the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 5: 5.
(3) Filling the spinning solution obtained in the step (1) into a needle tube, performing electrostatic spinning, and spinning the spinning solution on the surface of polylactic acid non-woven fabric (the gram weight of the non-woven fabric is 50 g/m) 2 ). Electrostatic spinning conditions: the voltage of the high-voltage generator is 25 kV; the distance from the nozzle to the receiving base cloth is 18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.8 mL/h; the receiving time is 30 min.
(4) And (3) filling the spinning solution obtained in the step (2) into a needle tube, carrying out electrostatic spinning, and spinning the spinning solution on the surface of the polylactic acid nano fiber obtained in the step (3). Electrostatic spinning conditions: the voltage of the high voltage generator is 25 kV; the distance from the nozzle to the receiving base cloth is 18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.6 mL/h; the receiving time is 10 min.
The diameter of the PLA nanofiber obtained in the step (3) is 100-250 nm, and the aperture is more than 0 and less than or equal to 5 mu m.
The diameter of the PLA superfine nano-fiber obtained in the step (4) is 30-60nm, and the aperture is more than 0 and less than or equal to 5 mu m.
Example 3
The embodiment is a preparation method of a branched completely degradable nanofiber mask filter element material, which comprises the following steps:
(1) weighing polylactic acid mother particle (M) W = 200000) is added into a mixed solution only containing N, N-Dimethylformamide (DMF) and dimethyl carbonate (DMC), and is stirred vigorously for 6 hours at the temperature of 65 ℃ and the speed of 400r/min, so as to prepare a spinning solution with the polylactic acid concentration of 13%; the adding amount of the polylactic acid master batch is 12 percent of the polylactic acid spinning solution, and the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 3: 7;
(2) weighing tetrabutylammonium chloride, adding the tetrabutylammonium chloride into a mixed solution only containing N, N-Dimethylformamide (DMF) and dimethyl carbonate (DMC), and vigorously stirring for 2 hours at the temperature of 45 ℃ and at the speed of 400r/min to prepare a mixed solution with the tetrabutylammonium chloride concentration of 7%. Adding a certain mass of polylactic acid master batch, and violently stirring for 6 hours at the temperature of 65 ℃ and at the speed of 400r/min to prepare an ultra-dilute spinning solution with the polylactic acid concentration of 5%; the addition amount of the polylactic acid master batch is 7 percent of the ultra-dilute polylactic acid spinning solution, and the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 5: 5.
(3) Putting the spinning solution obtained in the step (1) into a needle tube, performing electrostatic spinning, and spinning the spinning solution on the surface of polylactic acid non-woven fabric (the gram weight of the non-woven fabric is 50 g/m) 2 ). Electrostatic spinning conditions: the voltage of the high-voltage generator is 25 kV; the distance from the nozzle to the receiving base cloth is 18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.8 mL/h; the receiving time is 50 min.
(4) And (3) filling the spinning solution obtained in the step (2) into a needle tube, carrying out electrostatic spinning, and spinning the spinning solution on the surface of the polylactic acid nano fiber obtained in the step (3). Electrostatic spinning conditions: the voltage of the high-voltage generator is 25 kV; the distance from the nozzle to the receiving base cloth is 18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.5 mL/h; the receiving time is 20 min.
The diameter of the PLA nanofiber obtained in the step (3) is 200-400nm, and the pore diameter is more than 0 and less than or equal to 4 mu m.
The diameter of the PLA superfine nano-fiber obtained in the step (4) is 50-100nm, and the aperture is more than 0 and less than or equal to 4 mu m.
Example 4
The preparation method of the filter element material of the branched completely degradable nanofiber mask comprises the following steps:
(1) weighing polylactic acid master batch (M) W = 200000) is added into a mixed solution only containing N, N-Dimethylformamide (DMF) and dimethyl carbonate (DMC), and is stirred vigorously for 6 hours at the temperature of 65 ℃ and the speed of 400r/min, so as to prepare a spinning solution with the polylactic acid concentration of 15%; the addition amount of the polylactic acid master batch is 12 percent of the polylactic acid spinning solution, and the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 3: 7.
(2) Weighing tetrabutylammonium chloride, adding the tetrabutylammonium chloride into a mixed solution only containing N, N-Dimethylformamide (DMF) and dimethyl carbonate (DMC), and vigorously stirring for 2 hours at the temperature of 45 ℃ and at the speed of 400r/min to prepare a mixed solution with the tetrabutylammonium chloride concentration of 7%. Adding a certain mass of polylactic acid master batch, and violently stirring for 6 hours at the temperature of 65 ℃ and at the speed of 400r/min to prepare an ultra-dilute spinning solution with the polylactic acid concentration of 3%; the addition amount of the polylactic acid master batch is 7 percent of the ultra-dilute polylactic acid spinning solution, and the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 5: 5.
(3) Putting the spinning solution obtained in the step (1) into a needle tube, performing electrostatic spinning, and spinning the spinning solution on the surface of polylactic acid non-woven fabric (the gram weight of the non-woven fabric is 50 g/m) 2 ). Electrostatic spinning conditions: the voltage of the high-voltage generator is 25 kV; the distance from the nozzle to the receiving base cloth is 18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.8 mL/h; the receiving time is 30 min.
(4) And (3) filling the spinning solution obtained in the step (2) into a needle tube, carrying out electrostatic spinning, and spinning the spinning solution on the surface of the polylactic acid nano fiber obtained in the step (3). Electrostatic spinning conditions: the voltage of the high-voltage generator is 25 kV; the distance from the nozzle to the receiving base cloth is 16cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.8 mL/h; the receiving time is 30 min.
The diameter of the PLA nanofiber obtained in the step (3) is 200-400nm, and the pore diameter is more than 0 and less than or equal to 6 mu m.
The diameter of the PLA superfine nano-fiber obtained in the step (4) is 20-60nm, and the aperture is more than 0 and less than or equal to 4 mu m.
Example 5
The embodiment is a preparation method of a branched completely degradable nanofiber mask filter element material, which comprises the following steps:
(1) weighed polylactic acid master batch (M) W = 200000) is added into a mixed solution only containing N, N-Dimethylformamide (DMF) and dimethyl carbonate (DMC), and is stirred vigorously for 6 hours at the temperature of 65 ℃ and the speed of 400r/min, so as to prepare a spinning solution with the polylactic acid concentration of 12%; the addition amount of the polylactic acid master batch is 12 percent of the polylactic acid spinning solution, and the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 3: 7.
(2) Weighing tetrabutylammonium chloride, adding the tetrabutylammonium chloride into a mixed solution only containing N, N-Dimethylformamide (DMF) and dimethyl carbonate (DMC), and vigorously stirring for 2 hours at the temperature of 45 ℃ and at the speed of 400r/min to prepare a mixed solution with the tetrabutylammonium chloride concentration of 7%. Adding a certain mass of polylactic acid master batch, and violently stirring for 6 hours at the temperature of 65 ℃ and at the speed of 400r/min to prepare an ultra-dilute spinning solution with the polylactic acid concentration of 7%; the addition amount of the polylactic acid master batch is 7 percent of the ultra-dilute polylactic acid spinning solution, and the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 5: 5.
(3) Putting the spinning solution obtained in the step (1) into a needle tube, performing electrostatic spinning, and spinning the spinning solution on the surface of polylactic acid non-woven fabric (the gram weight of the non-woven fabric is 50 g/m) 2 ). Electrostatic spinning conditions are as follows: the voltage of the high voltage generator is 20 kV; the distance from the nozzle to the receiving base cloth is 15cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.5 mL/h; the receiving time is 60 min;
(4) and (3) filling the spinning solution obtained in the step (2) into a needle tube, carrying out electrostatic spinning, and spinning the spinning solution on the surface of the polylactic acid nano fiber obtained in the step (3). Electrostatic spinning conditions: the voltage of the high-voltage generator is 30 kV; the distance from the nozzle to the receiving base cloth is 18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 1 mL/h; the receiving time is 60 min.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (10)
1. The utility model provides a branching complete degradable nanofiber gauze mask filter core material which characterized in that: the composite filter element is formed by compounding branched polylactic acid nano fibers and polylactic acid non-woven fabrics, wherein the average diameter of the branched polylactic acid nano fibers is 35-45nm, and the whole structure of the filter element material is a multi-scale three-dimensional structure formed by stacking thick nano fibers and thin nano fibers.
2. The method for preparing the branched completely degradable nanofiber mask filter element material of claim 1, which is characterized by comprising the following steps:
(1) preparing a polylactic acid spinning solution: adding the polylactic acid master batch into the mixed solution, and violently stirring to obtain a polylactic acid spinning solution;
(2) preparing an ultra-dilute polylactic acid spinning solution: adding tetrabutylammonium chloride into the mixed solution, and carrying out first vigorous stirring to prepare a tetrabutylammonium chloride mixed solution; adding the polylactic acid master batch into the tetrabutylammonium chloride mixed solution, and carrying out secondary vigorous stirring to prepare an ultra-dilute polylactic acid spinning solution;
(3) preparing polylactic acid nano fibers: filling the polylactic acid spinning solution obtained in the step (1) into a needle tube, and spinning the polylactic acid spinning solution onto the surface of a polylactic acid non-woven fabric through electrostatic spinning to obtain polylactic acid nano fibers;
(4) preparing a branched completely degradable nanofiber mask filter element material: and (3) filling the ultra-dilute polylactic acid spinning solution obtained in the step (2) into a needle tube, and spinning the ultra-dilute polylactic acid spinning solution onto the surface of the polylactic acid nano-fiber obtained in the step (3) through electrostatic spinning to obtain the branched completely degradable nano-fiber mask filter element material.
3. The method for preparing the branched completely degradable nanofiber mask filter element material according to claim 2, wherein the method comprises the following steps: m of the polylactic acid master batch in the step (1) W 200000, the addition amount is 12% of the polylactic acid spinning solution, the mixed solution is N, N-dimethyl formamide and dimethyl carbonate, and the volume ratio of the N, N-dimethyl formamide to the dimethyl carbonate is 3: 7.
4. The method for preparing the branched completely degradable nanofiber mask filter element material according to claim 3, wherein the method comprises the following steps: the temperature of the violent stirring in the step (1) is 65 ℃, the rotation speed of the violent stirring is 400r/min, and the time of the violent stirring is 6 hours; the concentration of the polylactic acid spinning solution prepared in the step (1) is 10-15%.
5. The method for preparing the branched completely degradable nanofiber mask filter element material according to claim 4, wherein the method comprises the following steps: the mixed solution in the step (2) is N, N-dimethylformamide and dimethyl carbonate, the volume ratio of the N, N-dimethylformamide to the dimethyl carbonate is 5:5, the temperature of the first violent stirring is 45 ℃, the rotation speed of the violent stirring is 400r/min, and the time of the violent stirring is 2 hours; the concentration of tetrabutylammonium chloride is 3% -7%, the addition amount of the polylactic acid master batch is 7% of the ultra-dilute polylactic acid spinning solution, the second vigorous stirring temperature is 65 ℃, the vigorous stirring rotating speed is 400r/min, the vigorous stirring time is 6h, and the concentration of the ultra-dilute polylactic acid spinning solution prepared in the step (2) is 1-7%.
6. The method for preparing the branched completely degradable nanofiber mask filter element material according to claim 5, wherein the method comprises the following steps: the gram weight of the non-woven fabric in the step (3) is 50g/m 2 The electrostatic spinning conditions are as follows: the voltage of the high-voltage generator is 20-30 kV; the distance from the nozzle to the non-woven fabric is 15-18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.5-3.0 mL/h; the receiving time is 10-60 min.
7. The method for preparing the branched completely degradable nanofiber mask filter element material according to claim 6, wherein the method comprises the following steps: the diameter of the polylactic acid nano fiber prepared in the step (3) is 100-400nm, and the aperture is more than 0 and less than or equal to 10 mu m.
8. The method for preparing the branched completely degradable nanofiber mask filter element material according to claim 7, wherein the electrospinning conditions in the step (4) are as follows: the voltage of the high-voltage generator is 20-30 kV; the distance from the nozzle to the receiving base cloth is 15-18cm, and the caliber of the nozzle is 0.15 cm; the flow rate of the sprayed electrostatic spinning solution is 0.3-1.0 mL/h; the receiving time is 10-60 min.
9. The method for preparing the branched completely degradable nanofiber mask filter element material according to claim 8, wherein the method comprises the following steps: the diameter of the branched completely degradable nanofiber mask filter core material prepared in the step (4) is 25-100nm, and the aperture is more than 0 and less than or equal to 10 microns.
10. Use of the branched fully degradable nanofiber respirator filter material of claim 1 in a respirator.
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