CN112342636B - Preparation method of graphene metal organic framework composite modified polypropylene melt-blown material - Google Patents
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- D—TEXTILES; PAPER
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- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- 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
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- 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
- A41D31/30—Antimicrobial, e.g. antibacterial
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- 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
- D04H1/54—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 by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/542—Adhesive fibres
- D04H1/544—Olefin series
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- 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
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/005—Synthetic yarns or filaments
- D04H3/007—Addition polymers
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- 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
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0442—Antimicrobial, antibacterial, antifungal additives
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention provides a preparation method of a graphene metal organic framework composite modified polypropylene melt-blown material.
Description
Technical Field
The invention relates to a method for preparing a melt-blown nonwoven material by utilizing graphene and metal-organic framework material modified polypropylene, belonging to the field of material preparation technology and nonwoven fabric modification.
The background technology is as follows:
the polypropylene (PP) melt-blown nonwoven material has the advantages of small pore diameter, high porosity, large specific surface area, low cost and the like, and is a main filter element layer material of the traditional medical protective mask. The conventional filter element layer for the mask is mainly a PP melt-blown non-woven material subjected to electret treatment, and mainly retains pollutants such as dust, spray and the like in the air through mechanical and electrostatic adsorption. Because the material has the phenomenon of charge attenuation, the filtering efficiency of the PP melt-blown material can be drastically reduced along with the actions of time, gas (water vapor) and the like, the effective filtering time of the conventional PP melt-blown non-woven material is only 4 hours, and the conventional PP melt-blown non-woven material has no antibacterial capability, and bacteria on a mask can be harmful to human health. Furthermore, conventional PP meltblown nonwoven materials are single in functionality and have failed to meet increasingly complex use requirements.
Disclosure of Invention
In order to solve the defects of the existing materials, the invention provides a preparation method of a long-acting, efficient, low-resistance, good in antibacterial property and rich in function composite PP melt-blown nonwoven material. According to the preparation method, firstly, graphene A and graphene B containing different charges are prepared, secondly, salicylic acid is used for modifying the graphene, modified graphene is used for blending and modifying polypropylene resin, then a melt-blowing process is used for preparing graphene/polypropylene melt-blowing cloth, and finally, a metal organic framework material is loaded on the modified melt-blowing cloth through a post-treatment process. The novel graphene/metal organic framework composite modified polypropylene melt-blown material is prepared. The material has the characteristics of lasting efficacy, high efficiency, low resistance, strong antibacterial property, rich functions and the like, can replace the conventional PP melt-blown non-woven melt-blown filter material, greatly improves the protective performance and the service time of the existing protective mask, and can be used for developing other medical and health products.
The first object of the invention is to provide a preparation method of a graphene/metal organic framework composite modified polypropylene melt-blown material, which comprises the following steps: preparing graphene A and graphene B containing different charges, preparing graphene/polypropylene melt-blown cloth by utilizing salicylic acid modified graphene, blending and granulating the modified graphene and polypropylene resin, carrying out post-treatment on the loaded metal-organic frame material, and then washing and drying to obtain the graphene/metal-organic frame composite modified polypropylene melt-blown material.
In one embodiment, salicylic acid modified graphene is subjected to magnetic stirring and ultrasonic treatment for 1-4 hours at room temperature, and then dried to obtain a modified graphene material.
In one embodiment, the concentration of the salicylic acid/DMF solution is 0.5-3.0 g/L, and the rotation speed of magnetic stirring is 50-100 r/min.
In one embodiment, the drying temperature is 80 ℃ and the drying time is 3-5 hours after the reaction is completed.
In one embodiment, the modified graphene and the polypropylene resin are blended by using a screw extruder, wherein the temperature of a heating zone and a die head of the screw extruder is 180-220 ℃ in the first zone, 200-230 ℃ in the second zone, 210-240 ℃ in the third zone, 220-250 ℃ in the fourth zone, 190-240 ℃ in the die head, and the rotating speed of the screw is 20-60 r/min.
In one embodiment, a graphene/polypropylene meltblown fabric is prepared using a meltblowing line, wherein the melt temperature in the meltblowing process is 270-330 ℃, the spinneret temperature is 210-250 ℃, and the high-velocity hot gas stream temperature is 270-320 ℃.
In one embodiment, the graphene/polypropylene melt-blown fiber web is pretreated by an impregnation process, wherein the pretreatment solution is a sodium dodecyl sulfate aqueous solution with the concentration of 1-5 wt% and the impregnation time is 0.5-5 h.
In one embodiment, the pretreated graphene/polypropylene meltblown fabric is loaded with a metal organic framework material by in-situ polymerization, the reaction temperature is 100-160 ℃, and the reaction time is 5-24 hours.
In one embodiment, the central metal ion of the metal organic framework material supported on graphene/polypropylene meltblown is Cu 2+ 、Fe 3+ 、Zn 2+ The organic ligand is one or more of terephthalic acid, tannic acid and 2-amino terephthalic acid.
In one embodiment, the metal organic framework material loaded on the graphene/polypropylene melt-blown cloth has a mass ratio of center metal ion to organic ligand of (1.0-1.2): (1.2 to 1.4).
The second object of the invention is to provide the graphene/metal organic framework composite modified polypropylene melt-blown material prepared by the method.
The third object of the invention is to provide a filter element layer material containing the medical protective mask.
A fourth object of the present invention is to provide a medical protective mask comprising the present invention.
A fifth object of the present invention is to provide a separator material for lithium batteries comprising the present invention.
Compared with the prior art, the invention has the following advantages:
1. the graphene/metal organic framework composite modified polypropylene melt-blown material prepared by the invention is a novel functional material. The material has the characteristics of lasting efficacy, high efficiency, low resistance, enrichment of graphene on the surface of the fiber, improved filtering performance, strong antibacterial property, rich functions and the like, can replace the conventional PP melt-blown non-woven melt-blown filter material, and greatly improves the protective performance and the service life of the existing protective mask;
2. the graphene/polypropylene melt-blown cloth is loaded with the metal organic frame material, so that the metal organic frame material has strong adjustability and can be used as a container loaded medicine or material to prepare other types of functional medical and health materials, and has a wide application prospect.
3. According to the invention, salicylic acid is introduced into a modified graphene preparation technology, a modified graphene material which can be uniformly dispersed in a polymer melt is developed, and a new way is developed for the application of the graphene material in polymer modification.
4. The composite material prepared by the invention has strong functionality, can be developed into water filtering materials, heat conducting materials, lithium battery diaphragms and the like, and has wide application fields.
Drawings
FIG. 1 is a schematic of positive and negative charges during spinning;
Detailed Description
The invention is further illustrated, but is not limited, by the following examples. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
Example 1: preparation method of graphene/metal organic framework composite modified polypropylene melt-blown material
The first step: mixing 0.1-3 parts of graphene and 100 parts of ethanol, shearing to disperse the graphene in the ethanol, adding 0.2-5 parts of silane coupling agent, controlling the temperature to be 50-80 ℃ for reaction, carrying out suction filtration, washing and drying to obtain graphene A with positive charges on the surface, adding 0.5-2 parts of sodium dodecyl benzene sulfonate into 100 parts of deionized water, stirring, adding 0.1-3 parts of graphene, stirring for 30-60 minutes at 50-60 ℃, and carrying out suction filtration, washing and drying to obtain graphene B with negative charges on the surface;
preparing 200mL of salicylic acid/DMF solution with the concentration of 2g/L, adding 1g of graphene A, stirring and carrying out ultrasonic treatment for 1h, washing three times by deionized water/ethanol (mass ratio of 1:1) after the reaction is finished, and drying in an 80 ℃ air oven for 5h to obtain modified graphene A powder; the steps are repeated by using the graphene B to prepare graphene B powder, wherein salicylic acid can not only modify the surface of the graphene, but also form a protective layer on the surface of the graphene to prevent charge migration on the surface of the graphene.
And a second step of: weighing 5g of modified graphene A powder, 5g of graphene B powder and 990g of polypropylene resin, uniformly stirring by using a glass rod, and feeding into a screw extruder, wherein the temperature of a heating zone and a die head of the screw extruder is as follows: the first zone is 190 ℃, the second zone is 210 ℃, the third zone is 220 ℃, the fourth zone is 230 ℃, the die head temperature is 200 ℃, and the screw rotating speed is 20r/min. And (3) preparing graphene modified polypropylene master batches by using a granulator after melt extrusion.
And a third step of: feeding the graphene modified polypropylene master batch into a melt-blowing test line, wherein the die head contains an electric field, as shown in figure 1; the melt-blown test line screw and the die head temperature are set as follows: the temperature of the spray head is 230 ℃ and the temperature of the high-speed hot air flow is 290 ℃ in the first area 280 ℃, the second area 290 ℃, the third area 300 ℃, the fourth area 315 ℃, the fifth area 315 ℃. Preparing graphene/polypropylene melt-blown cloth through a melt-blown test line, wherein graphene is enriched on the surface of the fiber;
fourth step: preparing a sodium dodecyl sulfate pretreatment liquid with the mass percentage of 3wt%, shearing graphene/polypropylene melt-blown cloth with the size of 4 multiplied by 4cm, ultrasonically washing the cloth for 30min by using absolute ethyl alcohol, then placing the cloth into the pretreatment liquid, immersing the cloth for 1h, and drying the cloth in an oven at 80 ℃ for later use after the reaction is completed.
Fifth step: preparing an in-situ polymerization reaction liquid for post-treatment; 1.250g of terephthalic acid and 1.012g of ferric trichloride hexahydrate are weighed, and are respectively and fully dissolved in 30mL of DMF (the mass ratio of terephthalic acid to ferric trichloride hexahydrate is 1.2:1), and after the terephthalic acid to the ferric trichloride are completely dissolved, the two solutions are mixed and dispersed for 30min by ultrasonic. Transferring the obtained mixture into a reaction kettle, adding the pretreated graphene/polypropylene melt-blown cloth, reacting for 6 hours at 110 ℃, cooling to room temperature after the reaction is finished, washing and drying to obtain the graphene/metal organic framework composite modified polypropylene melt-blown material.
Sixth step: the resulting composite meltblown material was labeled 1 # And (3) a sample.
Pair 1 # The filtering performance of the sample is tested, and the result shows that the filtering efficiency of the sample on sodium chloride gas with the thickness of 2-10 mu m is more than 95%, the filtering resistance is 89Pa, the filtering efficiency is still more than 70% after 48 hours of filtering, and the filtering resistance is lower than 200Pa.
Example 2: preparation method of graphene/metal organic framework composite modified polypropylene melt-blown material
The preparation process was essentially the same as in example 1, except that: an improved graphene modification solution is adopted, and the concentration of the modified graphene solution is 3g/L. The prepared composite melt-blown material is manufactured into a mask, and the test results show that the filtering efficiency, the air suction resistance and the antibacterial performance of the medical protective mask manufactured by the material all reach the standard of GB19083-2010 technical requirements of medical protective masks.
Example 3: preparation method of graphene/metal organic framework composite modified polypropylene melt-blown material
The preparation process was essentially the same as in example 1, except that: an improved in-situ polymerization solution for post-treatment is adopted to replace ferric trichloride hexahydrate with anhydrous copper acetate. The prepared composite melt-blown material is manufactured into a mask, and the test results show that the filtering efficiency, the air suction resistance and the antibacterial performance of the medical protective mask manufactured by the material all reach the standard of GB19083-2010 technical requirements of medical protective masks.
The graphene/metal organic framework composite modified polypropylene melt-blown material provided by the invention can be widely applied to air filtration and development of functional medical and health materials, and can be used as a catalytic material for wastewater treatment, and can be developed for application in the aspect of lithium battery diaphragm materials.
Claims (8)
1. The preparation method of the graphene metal organic framework composite modified polypropylene melt-blown material is characterized by comprising the following steps of:
step 1: mixing 0.1-3 parts of graphene and 100 parts of ethanol, shearing to disperse the graphene in the ethanol, adding 0.2-5 parts of silane coupling agent, controlling the temperature to be 50-80 ℃ for reaction, and carrying out suction filtration, washing and drying to obtain graphene A with positive charges on the surface;
step 2: adding 0.5-2 parts of sodium dodecyl benzene sulfonate into 100 parts of deionized water, stirring, adding 0.1-3 parts of graphene, stirring for 30-60 minutes at 50-60 ℃, and then carrying out suction filtration, washing and drying to obtain graphene B with negative charges on the surface;
step 3, modifying the graphene A and the graphene B by using salicylic acid to improve the compatibility of the graphene and the resin and performing a protective layer on the surface of the graphene;
step 4, mixing salicylic acid modified graphene A and graphene B with polypropylene resin, wherein the mass of the graphene A is the same as that of the graphene B, the mass of the graphene A is 5g, the mass of the polypropylene resin is 990g, and preparing graphene/polypropylene master batch by melt blending modification of a screw extruder;
step 5, adding the obtained graphene/polypropylene master batch into a melt-blown fiber spinning machine, enabling spinning solution to pass through a die head containing an electric field, enabling graphene to migrate towards the edge of a die head channel, finally enriching the graphene at the edge of a spinning flow fiber, and performing melt-blowing on a web-forming curtain to form graphene/polypropylene melt-blown cloth;
and 6, carrying out post-treatment on the obtained graphene/polypropylene melt-blown cloth, and loading a metal organic framework material on the melt-blown cloth to prepare the graphene/metal organic framework composite modified polypropylene melt-blown material.
2. The preparation method of the graphene metal organic framework composite modified polypropylene melt-blown material according to claim 1, wherein the method for modifying the salicylic acid graphene is mechanical stirring and ultrasonic treatment, the stirring speed is 50-100r/min, and the stirring time is 1-4 h; the ultrasonic frequency is 28KHz, and the ultrasonic time is 1-4 h.
3. The method for preparing the graphene metal organic framework composite modified polypropylene melt-blown material according to claim 2, wherein the temperature of a heating zone and a die head of a screw extruder is 180-220 ℃ in a first zone, 200-230 ℃ in a second zone, 210-240 ℃ in a third zone, 220-250 ℃ in a fourth zone, 190-240 ℃ in a die head, and the rotating speed of the screw is 20-60 r/min.
4. The method for preparing the graphene metal organic framework composite modified polypropylene melt-blown material according to claim 3, wherein the melt temperature in the melt-blown process is 270-330 ℃, the spinneret temperature is 210-250 ℃, and the high-speed hot air flow temperature is 270-320 ℃.
5. The method for preparing the graphene metal organic framework composite modified polypropylene melt-blown material according to claim 4, wherein the process of post-processing graphene/polypropylene melt-blown cloth is a hydrothermal method surface loading metal organic framework material.
6. The method for preparing the graphene metal organic framework composite modified polypropylene melt-blown material according to claim 5, wherein the post-treatment method comprises a coating process pretreatment substrate which is self-assembled layer by layer driven by electrostatic force, and the treatment solution is a sodium dodecyl sulfate aqueous solution with the concentration of 1-5 wt%.
7. The method for preparing the graphene metal organic framework composite modified polypropylene melt-blown material according to claim 6, wherein the graphene metal organic framework composite modified polypropylene melt-blown material is loaded on graphene/polypropylene melt-blown materialThe central metal ion of the metal organic framework material on the cloth is Cu 2+ 、Fe 3+ 、Zn 2+ The organic ligand is one or more of terephthalic acid, tannic acid and 2-amino terephthalic acid.
8. The preparation method of the graphene metal organic framework composite modified polypropylene melt-blown material according to claim 7, wherein the mass ratio of the central metal ion to the organic ligand of the metal organic framework material loaded on the graphene/polypropylene melt-blown cloth is (1.0-1.2): (1.2-1.4).
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| CN109881483A (en) * | 2019-01-24 | 2019-06-14 | 浙江理工大学 | It is a kind of to utilize metal-organic framework materials functional modification polypropylene/cellulose spunlace non-woven cloth method and its application |
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| CN107286473A (en) * | 2017-08-01 | 2017-10-24 | 山东圣泉新材料股份有限公司 | A kind of modified polypropylene agglomerate, fusion spray cloth and its preparation method and application |
| CN109881483A (en) * | 2019-01-24 | 2019-06-14 | 浙江理工大学 | It is a kind of to utilize metal-organic framework materials functional modification polypropylene/cellulose spunlace non-woven cloth method and its application |
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| 沈志明.熔喷纤维极化技术的发展.《新型非织造布技术》.中国纺织出版社,1998, * |
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