CN104785018B - A kind of PVDF nanofiber multi-functional air filtering material and preparation method - Google Patents
A kind of PVDF nanofiber multi-functional air filtering material and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of PVDF nanofiber multi-functional air filtering material, comprise a layer polypropylene microfiber layer and one deck PVDF layers of nanofibers, described PVDF nanofiber is made up of spinning solution, count by weight, described spinning solution comprises 1 part of PVDF resin and 9-13 part mixed solvent, described mixed solvent comprises amide solvent and ketone, and its preparation method comprises the following steps: step 1) using polypropylene microfiber layer as base material; Step 2) PVDF resin, mixed solvent and tetrabutylammonium perchlorate are uniformly mixed, obtain spinning solution and add in electrostatic spinning apparatus; Step 3) base material is passed through the hot pressing of high-temperature high-pressure smooth roll, then send in electrostatic spinning apparatus and spray; Step 4) namely obtain finished product after end to be sprayed.The present invention can greatly reduce the medium oil particle of air and ion particles content in the growth of effective anti-bacteria, and long service life, production efficiency is high.
Description
Technical field
The present invention relates to filtering material field, be specifically related to a kind of PVDF nanofiber multi-functional air filtering material and preparation method.
Background technology
At present, global environment goes from bad to worse, and the air ambient closely bound up with the mankind is all the more so, seriously injures the health of the mankind.Meanwhile, the purification of some key component to environment of modern high technology requires high.Therefore, modern society to have efficient, low-resistance, the advantage such as antibacterial air filting material demand very big, the technology such as nanofiber, glass fibre, electret are widely applied.
Existing more nanofiltration material, its function singleness, the scope of application has larger restriction, the resistance of many filtering materials to air-flow is higher, secondly, containing metallic bacteriostatic agents such as nano level silver ions in multiple antimicrobial filtering material, according to current research, metal nano powder is that one can suction-type carcinogen, limits use at present in the many countries of America and Europe; Also there is nanofiber filtration material to apply high boiling solvent when producing simultaneously, result is that high boiling solvent can not volatilize completely, containing residual solvent in the nano fibrous membrane made, can damage human body, and not possess fungistatic effect according to the tunica fibrosa that patented technology is made; Electret filter efficiency also has obvious defect, electret contains the rising of ionized water steam in meeting is along with the rising of temperature, the delay of time and air, electric charge in electret can sharply decline, it can sharply decline to the adsorption capacity of particulate in air, thus causes strainability sharply to decline.Also have such as in patent CN103774345A, do not mention that aerocolloidal size grade scale is used in test, secondly the pressure drop of 28mmH2O is too high, and is not suitable for the typical filter materials such as mouth mask.
So so far, nanofiber suitability for industrialized production is faced with problems always, the performance that the nano fibrous membrane that therefore performance of above-mentioned nanofiber filtration material is also only confined to prepare under laboratory condition possesses.
Summary of the invention
The object of the invention is to the above problem overcoming prior art existence, a kind of PVDF nanofiber multi-functional air filtering material and preparation method are provided, can the growth of effective anti-bacteria, the medium oil particle of filtered air and ion particles, and filtering material long service life of the present invention, production efficiency is high.
For realizing above-mentioned technical purpose, reach above-mentioned technique effect, the present invention is achieved through the following technical solutions:
A kind of PVDF nanofiber multi-functional air filtering material, comprise at least one layer polypropylene microfiber layer and at least one deck PVDF layers of nanofibers, described PVDF nanofiber is made up of spinning solution, count by weight, described spinning solution comprises 1 part of PVDF resin and 9-13 part mixed solvent, count by weight, described mixed solvent comprises 10 parts of amide solvents and 1-10 part ketone, described amide solvent is N, dinethylformamide or N, N-dimethylacetylamide, described ketone is butanone or acetone.
Further, also comprise tetrabutylammonium perchlorate in described PVDF nanofiber, by weight mark meter, the tetrabutylammonium perchlorate of every 100 parts of spinning solutions configuration 0.05-0.1 part.
Further, the weight of described polypropylene microfiber layer is 5-30gsm, and the weight of described PVDF layers of nanofibers is 0.1-0.5gsm.
Further, described polypropylene microfiber layer and PVDF layers of nanofibers are arranged alternately mutually.
A preparation method for PVDF nanofiber multi-functional air filtering material, comprises the following steps:
Step 1) using polypropylene microfiber layer as base material, be placed on take-off device;
Step 2) PVDF resin, mixed solvent and tetrabutylammonium perchlorate are uniformly mixed, obtain spinning solution;
Step 3) by base material by the hot pressing of high-temperature high-pressure smooth roll, then send in electrostatic spinning apparatus and spray PVDF layers of nanofibers, in the solution storage device of wherein electrostatic spinning apparatus, place the spinning solution in step 2;
Step 4) reeled by coiler device by the hot pressing of low temperature felt wrapped roll after end to be sprayed, obtain finished product.
Further, the polypropylene microfiber layer in described step 1 is sprayed by melt-spraying spinning device and makes, and the fibre diameter of described polypropylene microfiber layer is 1-3 micron.
Further, the spinning voltage of described electrostatic spinning apparatus is 20-80kv, and spinning environment temperature is 10-30 DEG C, and the flow of the spinning syringe needle of described electrostatic spinning apparatus is 0.01-1ml/h, and described spinning syringe needle arranges upward and is arranged in solution recovery device.
Further, the fibre diameter of described PVDF layers of nanofibers is 150 nanometers, and the aperture of described PVDF layers of nanofibers is 0.5-1.5 micron
Further, the temperature of described high-temperature high-pressure smooth roll is 40-120 DEG C, and pressure is 1000-10000N/ ㎡, and the temperature of described low temperature optical press roll is 30-80 DEG C, and pressure is 1000-2000N/ ㎡.
The invention has the beneficial effects as follows:
1, air filting material of the present invention has low-resistance, antibacterial, environmental protection, aging-resistant function, and preparation is simple, has based on industrialized efficient production capacity.
2, the complete noresidue of solvent in the PVDF nanofiber produced of the present invention, is applicable in the filtering materials such as application and the mouth mask of direct body contact.
The filter efficiency of air filting material to 0.075 micron of sodium chloride aerosol of the double-layer structure 3, prepared by the present invention reaches more than 90%, within pressure drop resistance 100Pa, more than 80% is reached to colibacillary bacteriostasis rate, be a kind of mouth mask air filting material very well, meet the technical standard of GB2626-2006 about KN90.
The filtration of air filting material to 0.075 micron of sodium chloride aerosol of the four-layer structure 4, prepared by the present invention reaches more than 97%, pressure drop resistance is within 160Pa, more than 90% is reached to colibacillary bacteriostasis rate, meets the technical standard of GB2626-2006 about KN95.
5, special auxiliary agent is added in spinning solution of the present invention, the temperature tolerance of last PVDF nanofiber can be improved, the air filting material of this polypropylene electret layer and PVDF layers of nanofibers MULTILAYER COMPOSITE can be applied and the fields such as air-conditioning, automobile, air purifier, industrial waste gas process, and lower pressure drop resistance and very high appearance dirt rate can reduce the energy consumption in air handling process.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of description, coordinates accompanying drawing to be described in detail as follows below with preferred embodiment of the present invention.The specific embodiment of the present invention is provided in detail by following examples and accompanying drawing thereof.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in embodiment of the present invention technology, be briefly described to the accompanying drawing used required in the description of embodiment technology below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the device structure schematic diagram of the embodiment of the present invention one;
Fig. 2 is the finished product structure schematic diagram of the embodiment of the present invention one;
Fig. 3 is the device structure schematic diagram of the embodiment of the present invention two;
Fig. 4 is the finished product structure schematic diagram of the embodiment of the present invention two.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment one
With reference to shown in Fig. 1 and Fig. 2, a kind of PVDF nanofiber multi-functional air filtering material, comprise a layer polypropylene microfiber layer 1 and one deck PVDF layers of nanofibers 2, PVDF nanofiber is made up of spinning solution, spinning solution comprises the PVDF resin of 1kg, the mixed solvent of 9kg, and mixed solvent comprises the amide solvent of 4.5kg and the ketone of 4.5kg, and amide solvent is N, dinethylformamide, ketone is butanone.The tetrabutylammonium perchlorate of 0.01kg is also comprised in PVDF nanofiber, tetrabutylammonium perchlorate is for increasing the electric conductivity of solution, increase the splitting degree of fiber in electrostatic spinning process, thus obtain thinner nanofiber, the volatilization completely of solvent in spinning solution can be ensured; The quantity of the electrostatic charge of PVDF fiber can be increased in PVDF layers of nanofibers after shaping containing tetrabutylammonium perchlorate's salt, make PVDF layers of nanofibers also become electret, to improve the ability catching fine particle thing.
Wherein the weight of polypropylene microfiber layer is the weight of 5-30gsm, PVDF layers of nanofibers is 0.1-0.5gsm.PVDF resin can adopt the Kynar761PVDF powdery resin of French ARKEMA.
A preparation method for PVDF nanofiber multi-functional air filtering material, comprises the following steps:
Step 1) be that the polypropylene microfiber layer of 2 microns is as base material using fiber diameter, be placed on take-off device 3, wherein polypropylene microfiber layer can be sprayed by melt-spraying spinning device and make, also ready-made polypropylene micrometer fibers non-woven fabrics can be bought, in polypropylene non-woven fabric, the diameter of fiber evenly, must guarantee that the aperture of non-woven fabrics is relatively uniform;
Step 2) PVDF resin, mixed solvent and tetrabutylammonium perchlorate are uniformly mixed, obtain spinning solution, the configuration of solution must in airtight container for stirring evenly to prevent the volatilization of solvent;
Step 3) base material is passed through high-temperature high-pressure smooth roll 4 hot pressing, the temperature of high-temperature high-pressure smooth roll is 120 DEG C, pressure is 10000N/ ㎡, ensure that a relative smooth of nanofiber attachment is smooth, then send in electrostatic spinning apparatus 5 and spray PVDF layers of nanofibers, the spinning solution in step 2 is placed in the solution storage device of wherein electrostatic spinning apparatus, the spinning voltage of electrostatic spinning apparatus is 80kv, spinning environment temperature 30 DEG C, humidity is 0-70%, the flow of the spinning syringe needle 8 of electrostatic spinning apparatus is 1ml/h, spinning syringe needle arranges upward and is arranged in solution recovery device 9, like this guarantee each spinning syringe needle in spinning process under the effect of a part of spinning solution at high-pressure electrostatic drawing and forming be nanofiber, remainingly trickle solution collection groove from the surrounding of spinning syringe needle mouth along outer wall, can reuse, avoid the waste of material,
Step 4) reeled by coiler device 7 by low temperature felt wrapped roll 6 hot pressing after end to be sprayed, obtain finished product, wherein the temperature of low temperature optical press roll is 80 DEG C, and pressure is 2000N/ ㎡.
Wherein the fibre diameter of PVDF layers of nanofibers is 150 nanometers, and the aperture of PVDF layers of nanofibers is 0.5 micron.
The filter efficiency of finished product obtained by the present embodiment to 0.075 micron of sodium chloride aerosol reaches more than 90%, within pressure drop resistance 100Pa, reaches more than 80% to colibacillary bacteriostasis rate.
Polypropylene microfiber layer is after high-voltage electrostatic spinning device, polypropylene microfiber layer can by the high voltage electret process of high-voltage electrostatic spinning device, after electret process, a large amount of space charge on polypropylene microfiber layer band, it has very strong adsorption capacity to the particle within 0.075 micron, and can the growth of effective anti-bacteria; The medium oil particle of air that PVDF layers of nanofibers is pretreated and ion particles content greatly reduce, and can reduce the electrostatic decline of polypropylene microfiber layer electret, improve the service life of electret.
Embodiment two
Embodiment two is with the difference of embodiment one, and spinning solution comprises the PVDF resin of 1kg, the mixed solvent of 13kg, and mixed solvent comprises the amide solvent of 10kg and the ketone of 3kg, and amide solvent is DMA, and ketone is acetone.The tetrabutylammonium perchlorate of 0.007kg is also comprised in PVDF nanofiber
The fibre diameter of polypropylene microfiber layer is 1 micron, and the temperature of high-temperature high-pressure smooth roll is 40 DEG C, and pressure is 1000N/ ㎡, the temperature of low temperature optical press roll is 30 DEG C, pressure is 1000N/ ㎡, and the flow of the spinning syringe needle of electrostatic spinning apparatus is 0.1ml/h, and the spinning voltage of electrostatic spinning apparatus is 20kv.
The filter efficiency of finished product obtained by the present embodiment to 0.075 micron of sodium chloride aerosol reaches more than 90%, within pressure drop resistance 100Pa, reaches more than 80% to colibacillary bacteriostasis rate.
Embodiment three
Embodiment three is with the difference of embodiment one, the fibre diameter of polypropylene microfiber layer is 3 microns, the temperature of high-temperature high-pressure smooth roll is 80 DEG C, pressure is 5000N/ ㎡, the temperature of low temperature optical press roll is 60 DEG C, pressure is 1500N/ ㎡, and the flow of the spinning syringe needle of electrostatic spinning apparatus is 0.5ml/h, and the spinning voltage of electrostatic spinning apparatus is 60kv.
The filter efficiency of finished product obtained by the present embodiment to 0.075 micron of sodium chloride aerosol reaches more than 90%, within pressure drop resistance 100Pa, reaches more than 80% to colibacillary bacteriostasis rate.
Embodiment four
Embodiment four is with the difference of embodiment one, use two electrostatic spinning apparatus and a melt-spraying spinning device combination, its composition structure as shown in Figure 3, in the step 4 of the preparation method of embodiment one, after treating the hot pressing of low temperature felt wrapped roll, pass through turning device, continue to be fed in melt-spraying spinning device, at PVDF layers of nanofibers spray coating polypropylene microfiber layer 21 ', then continue through in turning device feeding electrostatic spinning apparatus and spray PVDF layers of nanofibers 2 ', so both complete the making of the air filting material of four-layer structure, as shown in Figure 4, collect finally by coiler device, integral manufacturing automation performance is high, convenient and reliable operation, more than 97% is reached to the filtration of 0.075 micron of sodium chloride aerosol, pressure drop resistance is within 160Pa, more than 90% is reached to colibacillary bacteriostasis rate.
Embodiment five
Embodiment five and the difference of embodiment four are to utilize the electrostatic spinning apparatus of more than two and melt-spraying spinning device can the composite air filtering film piled up alternately of production multilayer; The schematic diagram of the nanofiber membrane production equipment that the program is all does not provide, except increasing some electrostatic spinning apparatus and melt-spraying spinning device more, other structures are substantially identical, it reaches more than 99% to the filtration of 0.075 micron of sodium chloride aerosol, reaches more than 95% to colibacillary bacteriostasis rate.
The spinning technique of all not mentioned melt-spraying spinning equipment in above scheme, reason is very ripe in the manufacturing process of polypropylene melt blown non-woven fabric, is not described in detail in this patent.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (8)
1. a PVDF nanofiber multi-functional air filtering material, it is characterized in that: comprise at least one layer polypropylene microfiber layer and at least one deck PVDF layers of nanofibers, described PVDF nanofiber is made up of tetrabutylammonium perchlorate and spinning solution, mark meter by weight, the tetrabutylammonium perchlorate of every 100 parts of spinning solutions configuration 0.05-0.1 part; Count by weight, described spinning solution comprises 1 part of PVDF resin and 9-13 part mixed solvent, and described mixed solvent comprises amide solvent and ketone, and described amide solvent is DMF or DMA, and described ketone is butanone or acetone.
2. a kind of PVDF nanofiber multi-functional air filtering material according to claim 1, it is characterized in that: the weight of described polypropylene microfiber layer is 5-30gsm, the weight of described PVDF layers of nanofibers is 0.1-0.5gsm.
3. a kind of PVDF nanofiber multi-functional air filtering material according to claim 1, is characterized in that: described polypropylene microfiber layer and PVDF layers of nanofibers are arranged alternately mutually.
4. the preparation method of a kind of PVDF nanofiber multi-functional air filtering material as claimed in claim 1, is characterized in that: comprise the following steps:
Step 1) using polypropylene microfiber layer as base material, be placed on take-off device;
Step 2) PVDF resin, mixed solvent and tetrabutylammonium perchlorate are uniformly mixed, obtain spinning solution;
Step 3) by base material by the hot pressing of high-temperature high-pressure smooth roll, then send in electrostatic spinning apparatus and spray PVDF layers of nanofibers, in the solution storage device of wherein electrostatic spinning apparatus, place the spinning solution in step 2;
Step 4) reeled by coiler device by the hot pressing of low temperature felt wrapped roll after end to be sprayed, obtain finished product.
5. the preparation method of a kind of PVDF nanofiber multi-functional air filtering material as claimed in claim 4, it is characterized in that: the polypropylene microfiber layer in described step 1 is sprayed by melt-spraying spinning device and makes, and the fibre diameter of described polypropylene microfiber layer is 1-3 micron.
6. the preparation method of a kind of PVDF nanofiber multi-functional air filtering material as claimed in claim 4, it is characterized in that: the spinning voltage of described electrostatic spinning apparatus is 20-80kv, spinning environment temperature is 10-30 DEG C, the flow of the spinning syringe needle of described electrostatic spinning apparatus is 0.01-1ml/h, and described spinning syringe needle arranges upward and is arranged in solution recovery device.
7. the preparation method of a kind of PVDF nanofiber multi-functional air filtering material as claimed in claim 4, it is characterized in that: the fibre diameter of described PVDF layers of nanofibers is for being less than or equal to 150 nanometers, and the aperture of described PVDF layers of nanofibers is 0.5-1.5 micron.
8. the preparation method of a kind of PVDF nanofiber multi-functional air filtering material as claimed in claim 4, it is characterized in that: the temperature of described high-temperature high-pressure smooth roll is 40-120 DEG C, pressure is 1000-10000N/ ㎡, and the temperature of described low temperature felt wrapped roll is 30-80 DEG C, and pressure is 1000-2000N/ ㎡.
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