CN112549717A - Composite cloth and preparation method and application thereof - Google Patents
Composite cloth and preparation method and application thereof Download PDFInfo
- Publication number
- CN112549717A CN112549717A CN202011395369.9A CN202011395369A CN112549717A CN 112549717 A CN112549717 A CN 112549717A CN 202011395369 A CN202011395369 A CN 202011395369A CN 112549717 A CN112549717 A CN 112549717A
- Authority
- CN
- China
- Prior art keywords
- polyolefin
- composite
- microporous membrane
- composite cloth
- cloth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004744 fabric Substances 0.000 title claims abstract description 189
- 239000002131 composite material Substances 0.000 title claims abstract description 184
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
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- 239000012982 microporous membrane Substances 0.000 claims abstract description 118
- 230000001681 protective effect Effects 0.000 claims abstract description 73
- 238000001125 extrusion Methods 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 40
- 230000035699 permeability Effects 0.000 claims abstract description 33
- 238000002844 melting Methods 0.000 claims abstract description 24
- 230000008018 melting Effects 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 20
- 238000005266 casting Methods 0.000 claims abstract description 16
- 238000009998 heat setting Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- -1 propylene, butylene, 4-methyl-1-pentene Chemical class 0.000 claims description 89
- 239000003242 anti bacterial agent Substances 0.000 claims description 45
- 239000004745 nonwoven fabric Substances 0.000 claims description 44
- 239000000945 filler Substances 0.000 claims description 40
- 239000012528 membrane Substances 0.000 claims description 34
- 230000002209 hydrophobic effect Effects 0.000 claims description 25
- 239000000178 monomer Substances 0.000 claims description 18
- 239000002759 woven fabric Substances 0.000 claims description 18
- 239000008280 blood Substances 0.000 claims description 17
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- 238000001914 filtration Methods 0.000 claims description 16
- 230000035515 penetration Effects 0.000 claims description 16
- 239000011148 porous material Substances 0.000 claims description 16
- 239000004698 Polyethylene Substances 0.000 claims description 15
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 10
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- 229910052709 silver Inorganic materials 0.000 claims description 10
- 239000004332 silver Substances 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 8
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 7
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- 239000004902 Softening Agent Substances 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
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- 229920000578 graft copolymer Polymers 0.000 claims description 6
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- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 5
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
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- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
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- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 claims description 3
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical class COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims description 3
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- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- CBOQJANXLMLOSS-UHFFFAOYSA-N ethyl vanillin Chemical class CCOC1=CC(C=O)=CC=C1O CBOQJANXLMLOSS-UHFFFAOYSA-N 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 229910052621 halloysite Inorganic materials 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising 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
- A41D13/12—Surgeons' or patients' gowns or dresses
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/02—Layered materials
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- 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
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- A41D31/085—Heat resistant; Fire retardant using layered materials
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- A—HUMAN NECESSITIES
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- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
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- A41D31/102—Waterproof and breathable
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- A—HUMAN NECESSITIES
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- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
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- A41D31/12—Hygroscopic; Water retaining
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- A—HUMAN NECESSITIES
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- 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
- A41D31/24—Resistant to mechanical stress, e.g. pierce-proof
- A41D31/245—Resistant to mechanical stress, e.g. pierce-proof using layered materials
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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
- A41D31/305—Antimicrobial, e.g. antibacterial using layered materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0018—Combinations of extrusion moulding with other shaping operations combined with shaping by orienting, stretching or shrinking, e.g. film blowing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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Abstract
The invention discloses a composite cloth and a preparation method and application thereof, wherein the composite cloth comprises a polyolefin microporous membrane and non-woven cloth and/or woven cloth which are compounded with the polyolefin microporous membrane; the polyolefin microporous membrane is prepared by adopting a co-extrusion process: melting and extruding at least two polyolefins with different functions by using a double-screw extruder, and forming at least two co-extruded films by traction, cooling and heat treatment of a casting roll, wherein at least one of the at least two co-extruded films is a high-strength polyolefin co-extruded film; and the co-extruded film is subjected to stretching and heat setting treatment to obtain the polyolefin microporous film. The composite cloth has better thermal stability, and can meet the use requirement of high-temperature steam sterilization; the composite cloth inherits the advantages of air permeability, moisture permeability, barrier property, high mechanical strength, softness, crease resistance and the like of the battery diaphragm, and provides a high-performance composite material for medical protective clothing.
Description
Technical Field
The invention relates to the field of medical protective materials, in particular to composite cloth and a preparation method and application thereof.
Background
In the medical industry, the requirements for medical protection and medical appliances, such as protective clothing, protective gloves, hemostatic forceps and the like, are huge, and the protective clothing is very important for protecting the life safety of medical workers. The medical protective clothing must have multiple functionalities including liquid barrier, breaking strength and elongation at break, filtration efficiency, flame retardancy, antistatic properties, softness and wrinkle resistance, etc.; wherein the liquid barrier function includes, for example, water resistance, moisture permeability, synthetic blood penetration, and hydrophobic grade. In general, the performance of medical protective garments depends largely on the medical protective materials from which the garments are made.
At present, the existing medical protective materials generally comprise the following materials: (1) non-woven fabrics which take polypropylene as raw materials, namely polypropylene non-woven fabrics; (2) a composite spunlace fabric of wood pulp and polyester fiber; (3) a polypropylene spunbond-meltblown-spunbond composite nonwoven fabric; (4) polyethylene breathable film and non-woven fabric composite cloth. Wherein, the polypropylene non-woven fabric has high porosity and good air permeability; but the bacterium-blocking performance and the permeability-preventing performance are poor, so that the invasion of bacteria and viruses is easily caused, the good protection effect cannot be achieved, and the wearing comfort is poor. The composite spunlace fabric of wood pulp and polyester fiber has good capacity of resisting alcohol, blood and oil stains, and has no adhesion; meanwhile, the fabric has the characteristic of high temperature resistance, can be sterilized by high temperature or ultraviolet rays, and has very soft texture; but weak in hydrostatic pressure. The polypropylene spun-bonded-melt-blown-spun composite non-woven fabric has the advantages of small filtration resistance, softness, strong hydrostatic pressure resistance, high filtration efficiency and the like; however, the protection of the solid visible particles is not very strong, and can only reach about 60 percent at most. In order to meet the requirements of safety and comfort, the polyethylene breathable film and the non-woven fabric composite fabric are generally compounded together by adopting a mode of combining the non-woven fabric and the waterproof breathable polyethylene microporous film in the market, and have good breathability, moisture permeability and barrier property. However, the fabric/non-woven fabric and the protective clothing made of the conventional polyolefin material have thick and hard handfeel and are easy to generate creases, and the creases not only affect the overall beauty and wearing comfort of the clothing, but also can become the hiding place of viruses and bacteria, reduce the protective performance of the protective clothing and increase the disease probability of patients and medical workers.
In order to ensure the use safety, the medical protective material needs to be sterilized and packaged before use, so that the effect of blocking microorganisms is achieved. At present, the sterilization modes commonly used in the medical sterilization field are ethylene oxide sterilization, irradiation (gamma ray) sterilization, high-pressure steam sterilization, low-temperature formaldehyde sterilization and the like. Common sterilization modes for protective clothing are ethylene oxide sterilization and high-pressure steam sterilization. Ethylene oxide sterilization is a common low-temperature sterilization mode, and the sterilization needs 7 to 14 days of resolution time, so that the time cost is increased, and residual ethylene oxide is harmful to the body. The high-temperature steam sterilization mode has the temperature of between 121 ℃ and 135 ℃, the sterilization lasts for about 15-40 minutes, the cost is lower, the equipment is simple, the operation is convenient, the sterilization time is short, and no environmental pollution exists, but the sterilization article and the packaging system thereof need to be capable of resisting the high-temperature and high-humidity environment, the sterilization effective period is generally 5-7 days, and the method is the most reliable and most popular physical sterilization method.
At present, the composite cloth material which gives consideration to various protective properties and comfortableness in the market is the composite cloth of a polyethylene breathable film and non-woven cloth; the composite cloth can only adopt low-temperature sterilization modes such as ethylene oxide sterilization and the like generally, and the high-pressure steam sterilization can cause the melting or size shrinkage of the waterproof breathable microporous membrane layer to damage the structure of the waterproof breathable microporous membrane layer. However, as previously mentioned, ethylene oxide sterilization time is costly and may present a deleterious safety hazard to the body; therefore, how to solve the problem of the sterilization time cost of the composite cloth or how to improve the sterilization efficiency of the composite cloth and how to solve the potential safety hazard of the existing sterilization mode is a key and difficult point of research on the composite cloth.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a composite fabric and a preparation method and application thereof.
The technical scheme of the invention is as follows:
a composite fabric, which comprises a polyolefin microporous membrane and a non-woven fabric and/or a woven fabric which is compounded with the polyolefin microporous membrane;
the polyolefin microporous membrane is prepared by adopting a co-extrusion process: melting and extruding at least two polyolefins with different functions by using a double-screw extruder, and forming at least two co-extruded films by traction, cooling and heat treatment of a casting roll, wherein at least one of the at least two co-extruded films is a high-strength polyolefin co-extruded film; and the co-extruded film is subjected to stretching and heat setting treatment to obtain the polyolefin microporous film.
The composite cloth is characterized in that the melting point of the polyolefin is greater than or equal to 135 ℃; the polyolefin is composed of polyolefin and functional filler which are copolymerized and synthesized by screening different functional monomers and regulating and controlling the proportion of the monomers; the functional monomer comprises at least one of propylene, butylene, 4-methyl-1-pentene, cyclopentadiene, ethylene, oxyethylene, siloxane and glycol; the functional filler comprises at least one of an antibacterial agent, a hydrophobic filler, a hydrophilic filler, a softener and a reinforcing filler.
The composite cloth comprises an antibacterial agent, an organic antibacterial agent, an inorganic antibacterial agent and a natural antibacterial agent, wherein the organic antibacterial agent is one or more of vanillin compounds, ethyl vanillin compounds, anilides, imidazoles, thiazoles, isothiazolone derivatives, quaternary ammonium salts, guars and phenols; the inorganic antibacterial agent is prepared by fixing silver, copper, zinc, titanium or ions thereof on the surface of fluorite or silica gel; the natural antibacterial agent is one or more of chitin, mustard, castor oil and horseradish.
The composite cloth is characterized in that the hydrophobic filler is one or more of vinyltrimethoxysilane, vinyltriethoxysilane, epoxysiloxane, isobutyltriethoxysilane, polyphenylmethylsiloxane, active wax, long-chain alkane with the carbon atom number being more than or equal to 10, fluorocarbon silane and functional fluorocarbon compound; the hydrophilic filler is one or more of polyethylene glycol, polypropylene glycol, polyvinylpyrrolidone, acrylate, acrylic acid graft polymer, acrylate graft polymer, polyurethane acrylate and polyvinyl alcohol; the reinforcing filler is one or more of glass fiber, carbon tubes, graphene, carbon powder, silicon dioxide, titanium dioxide, halloysite, mica, talcum powder, calcium carbonate and barium sulfate.
The polyolefin microporous membrane comprises an A-type co-extrusion membrane, a B-type co-extrusion membrane and a C-type co-extrusion membrane which are sequentially stacked from outside to inside, wherein the A-type co-extrusion membrane comprises polyolefin, hydrophobic filler and an antibacterial agent; the B-type co-extrusion film is a high-strength polyolefin co-extrusion film, and comprises polyolefin and reinforcing filler; the C-type coextruded film includes a polyolefin and a hydrophilic filler.
In the composite cloth, at least one of the A-type co-extrusion film, the B-type co-extrusion film and the C-type co-extrusion film comprises a softener for improving flexibility and crease resistance; the softener is one or more of anionic, cationic, amphoteric, organosilicon, polyethylene and nonionic oxyethylene softening agents.
The porosity of the polyolefin microporous membrane is 10-95%, and the average pore diameter of the polyolefin microporous membrane is 50-2000 nm.
The composite cloth is characterized in that the polyolefin microporous membrane is 3-200um thick;
and/or the longitudinal breaking strength of the composite cloth is greater than or equal to 130N, and the transverse breaking strength of the composite cloth is greater than or equal to 58N;
and/or the longitudinal elongation at break of the composite fabric is more than or equal to 20 percent, and the transverse elongation at break of the composite fabric is more than or equal to 50 percent;
and/or the moisture permeability of the composite cloth is more than or equal to 5500 g/(m)2·d)；
And/or, the thermal shrinkage of the composite cloth is 0.1-5%;
and/or the composite cloth has the synthetic blood penetration resistance of more than or equal to grade 6;
and/or the filtration efficiency of the composite cloth is more than or equal to 99.93 percent.
A preparation method of composite cloth comprises the following steps:
melting and extruding at least two polyolefins with different functions by using a double-screw extruder, and forming at least two co-extruded films through traction, cooling and heat treatment of a casting roll, wherein at least one of the at least two co-extruded films is a high-strength polyolefin co-extruded film; the co-extruded film is stretched and heat-set to prepare the polyolefin microporous film;
and compounding the polyolefin microporous membrane with non-woven fabric and/or woven fabric in a thermal compounding or adhesive compounding mode to obtain the composite fabric.
The application of the composite cloth is characterized in that the composite cloth is used for preparing an outer cover for protection, and the outer cover for protection comprises medical protective clothing, a tent, a jacket and a medical packaging bag.
Has the advantages that: compared with the prior art, the composite cloth provided by the invention has the advantages of good one-way moisture permeability, seepage resistance, bacteria resistance and the like due to the adoption of the polyolefin microporous membrane, and has good barrier property, comfortable wearing and good thermal stability; in addition, the composite cloth has better mechanical strength, and is not easy to damage when being worn; the waterproof breathable microporous membrane has the characteristics of good thermal stability and high temperature resistance, solves the problem that the traditional waterproof breathable microporous membrane is easy to melt and shrink at high temperature, is suitable for high-pressure steam sterilization, and greatly reduces the production time and cost. In addition, the introduction of the functional monomer and the functional auxiliary agent endows the outer hydrophobic layer and the inner hydrophobic layer of the composite membrane with the performances of hydrophilicity, softness, crease resistance and the like. The melt stretching method is a microporous membrane preparation method which is conventionally used in battery diaphragm preparation, the melt stretching method is also called dry stretching, the polyolefin microporous membrane preparation method is simple, and the price is low, so that the composite cloth becomes an advanced medical protective material with high performance and high cost performance.
Drawings
Fig. 1 is a schematic structural diagram of a composite fabric of the present invention.
FIG. 2 is a flow chart of a preferred embodiment of the method of making the composite fabric of the present invention.
FIG. 3 is an SEM image of the outer surface layer of the polyolefin microporous membrane of the composite cloth of example 1.
Detailed Description
The invention provides a composite cloth and a preparation method and application thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a composite cloth, which comprises a polyolefin microporous membrane and a non-woven cloth and/or a woven cloth which are compounded with the polyolefin microporous membrane;
the polyolefin microporous membrane is prepared by adopting a co-extrusion process: melting and extruding at least two polyolefins with different functions by using a double-screw extruder, and forming at least two co-extruded films by traction, cooling and heat treatment of a casting roll, wherein at least one of the at least two co-extruded films is a high-strength polyolefin co-extruded film; and the co-extruded film is subjected to stretching and heat setting treatment to obtain the polyolefin microporous film.
Specifically, the existing composite cloth of the polyethylene breathable film and the non-woven cloth can not be sterilized by high-pressure steam, and the key point is that the polyethylene breathable film adopts linear low-density polyethylene (LLDPE), calcium carbonate is added into the LLDPE, micropores are formed at the joint of inorganic filler particles and a plastic film matrix in the stretching process, and the pore diameter is 0.4-2 mu m. The melting point of the polyethylene breathable film formed in the way is only about 120 ℃, and the polyethylene breathable film cannot reach the temperature of 121 ℃ and 135 ℃ for high-temperature steam sterilization; therefore, if high-pressure steam sterilization is used, the micropores of the polyethylene breathable film are melted, the size of the film is shrunk, and the breathability of the film is damaged.
In the embodiment, a mode of producing the base film by using the battery diaphragm is creatively adopted, namely a melt stretching method, a polyolefin microporous film is prepared by adopting a polyolefin raw material treated by a special process and a multilayer co-extrusion process, and then the polyolefin microporous film is compounded with non-woven fabric and/or woven fabric to prepare the composite fabric. Therefore, in one implementation of the present application, the basic structure of the composite fabric is shown in fig. 1, and is composed of a polyolefin microporous membrane 1 and a non-woven fabric and/or a woven fabric 2, wherein the polyolefin microporous membrane 1 is used as an outer surface layer of the composite fabric, the non-woven fabric and/or the woven fabric 2 is used as an inner surface layer of the composite fabric, and the inner surface layer may be a single layer or multiple layers.
In the embodiment, the polyolefin microporous membrane is adopted, so that the composite cloth has the advantages of good one-way moisture permeability, seepage resistance, bacteria resistance and the like, and not only has good barrier property, but also is comfortable to wear and has good thermal stability; in addition, the composite cloth provided by the embodiment has better mechanical strength, and is not easy to damage when being worn; the heat stability is good, the high temperature resistance is realized, the problem that the traditional waterproof breathable microporous membrane is easy to melt and shrink at high temperature is solved, and the method is suitable for high-pressure steam sterilization; the melt stretching method adopted by the embodiment is a microporous membrane preparation method which is conventionally used in battery diaphragm preparation, and is also called dry stretching, and the preparation method is simple and low in price, so that the composite cloth becomes an advanced medical protective material with high performance and high cost performance.
The polyolefin microporous membrane prepared by the method has a high melting point, so that the use requirement of high-pressure steam sterilization can be met; however, during use, it has been found that the softness and comfort of polyolefin microporous films with too high a melting point are affected; therefore, in the embodiment, the melting point of the prepared polyolefin microporous membrane is greater than or equal to 135 ℃, preferably in the range of 155-170 ℃ through the selection and the process control of polyolefin raw materials, so that the high-pressure steam sterilization can be met, and the special use requirements of the polyolefin microporous membrane applied to protective clothing can be considered. Therefore, the composite cloth of the embodiment is not only wear-resistant and can be used repeatedly, but also can be sterilized by high-pressure steam, and can be sterilized and reused quickly after being used.
In some embodiments, the polyolefin is composed of polyolefin synthesized by screening different functional monomers and regulating the monomer ratio and functional filler; the functional monomer comprises at least one of propylene, butylene, 4-methyl-1-pentene, cyclopentadiene, ethylene, oxyethylene, siloxane and ethylene glycol. By way of example, the polyolefin may be polypropylene, poly-1-butene, poly-4-methyl-1-pentene, and a series of polyolefins obtained by copolymerizing propylene with butene, propylene with 4-methyl-1-pentene, and cyclopentadiene in different monomer ratios.
In some embodiments, the functional filler comprises at least one of an antimicrobial agent, a hydrophobic filler, a hydrophilic filler, a softening agent, a reinforcing filler.
In some specific embodiments, a double-screw extruder is used for melt extrusion of three polyolefins with different functions, and the three-layer co-extruded film is formed through traction, cooling and heat treatment of a casting roll, wherein the polyolefin microporous film comprises an A-type co-extruded film, a B-type co-extruded film and a C-type co-extruded film which are sequentially stacked from outside to inside, and the A-type co-extruded film comprises polyolefin, hydrophobic filler and an antibacterial agent; the B-type co-extrusion film is a high-strength polyolefin co-extrusion film, and comprises polyolefin and reinforcing filler; the C-type coextruded film includes a polyolefin and a hydrophilic filler.
In the polyolefin microporous membrane prepared in the embodiment, the A-type co-extrusion membrane has self-antibacterial super-hydrophobic property as an outer surface layer, the B-type co-extrusion membrane has higher mechanical strength as an intermediate layer, and the C-type co-extrusion membrane has hydrophilic property as an inner surface layer. On one hand, due to the characteristics of hydrophobic outer layer and hydrophilic inner layer of the polyolefin microporous membrane, the polyolefin microporous membrane and the composite cloth prepared from the polyolefin microporous membrane have one-way moisture permeability, so that the wearing comfort and smooth perspiration can be ensured, and meanwhile, the outer surface layer with the sterilization characteristic also has good barrier property and filtering effect; on the other hand, the middle layer of the polyolefin microporous membrane is made of high-strength polyolefin, so that the polyolefin microporous membrane and the composite fabric prepared by the polyolefin microporous membrane have high mechanical strength and are not easy to damage; in the embodiment, the polyolefin with high melting point is used for replacing the traditional polyethylene material, so that the size shrinkage can be reduced as much as possible at higher temperature under the condition of considering various protective properties and comfortableness, and the stability of micropores is kept; therefore, the composite cloth can be suitable for general high-pressure steam sterilization, and can be rapidly sterilized and rapidly recycled after being used; solves the technical problem that the prior polyethylene breathable film and non-woven fabric composite cloth can only adopt low-temperature sterilization modes such as ethylene oxide sterilization and the like. Meanwhile, the problem that the use of the protective clothing is influenced due to poor tensile strength and tearing strength of the existing polyolefin porous membrane protective clothing is solved.
In this embodiment, the melt index of the high molecular weight polyolefin is 0.2 to 1.5g/10min, preferably 0.3 to 1.0g/10 min; the low molecular weight polyolefin has a melt index of 0.8 to 10g/10min, preferably 1.0 to 5.0g/10 min.
The composite cloth of the embodiment is formed by improving the existing polyethylene breathable film and non-woven cloth composite cloth, and the difference is that the embodiment adopts the polyolefin microporous film formed by the modified three-layer co-extrusion film, and the embodiment can be compounded with the non-woven cloth and the woven cloth. The nonwoven fabrics and woven fabrics used in this example were those conventionally used for protective clothing; for example, a polymer nonwoven fabric described in patent document CN2045199U, a nonwoven fabric described in patent document CN110409057A, a woven fabric of synthetic fibers described in patent document CN110760990A, a woven fabric of natural fibers described in "natural plant fibers — hemp fibers" of the non-patent document, and the like.
In the embodiment, the three-layer co-extrusion polyolefin microporous membrane treated by a special process is adopted to prepare the composite cloth, so that the prepared composite cloth has higher tensile strength and tearing strength. Specifically, the breaking strength of the composite fabric of the embodiment is greater than or equal to 50N, wherein the longitudinal breaking strength of the composite fabric is greater than or equal to 130N, and the transverse breaking strength of the composite fabric is greater than or equal to 58N. The three-layer co-extrusion polyolefin microporous membrane adopted by the embodiment ensures that the prepared composite cloth has higher breaking strength under the condition of high moisture permeability, particularly the longitudinal breaking strength is basically over 130N, and the transverse breaking strength is over 58N; thereby ensuring the mechanical strength of the composite cloth and the protective clothing made of the composite cloth. The composite fabric of the embodiment has an elongation at break of 20% or more, wherein the elongation at break in the machine direction of the composite fabric is 20% or more, and the elongation at break in the transverse direction of the composite fabric is 50% or more. It should be noted that, in the embodiment, the three-layer co-extrusion polyolefin microporous membrane is adopted, so that the prepared composite cloth has a larger elongation at break under the condition of high moisture permeability, and particularly, the transverse elongation at break is basically over 50%, and the longitudinal elongation at break is over 20%; therefore, the protective clothing made of the composite cloth has better softness and elasticity, improves the wearing comfort of the protective clothing made of the composite cloth with the polyolefin microporous membrane, and can meet the use requirements of the key parts of the protective clothing on breaking strength and breaking elongation.
In the embodiment, the three-layer co-extrusion polyolefin microporous membrane is adopted, and under the condition of ensuring the tensile property and the tearing strength, the polyolefin microporous membrane and the composite cloth prepared by the polyolefin microporous membrane have excellent one-way moisture permeability by controlling the large aperture of the microporous membrane and special process treatment, so that the use requirement of the protective clothing can be better met; in particular to protective clothing with higher requirement on mechanical strength.
In the embodiment, the polyolefin microporous membrane is prepared by a melt stretching method, micropores of the polyolefin microporous membrane meander in the polyolefin microporous membrane, and the hydrophobic filler and the antibacterial agent are added into the A-type co-extruded membrane on the outer surface layer, so that the polyolefin microporous membrane has good barrier property on bacteria and viruses, and the bacteria and the viruses are prevented from penetrating through the polyolefin microporous membrane.
In some embodiments, the polyolefin microporous membrane has a porosity of 10 to 95% and an average pore size of 50 to 1200 nm. Preferably, the polyolefin microporous membrane has a porosity of 50 to 80%, and an average pore diameter of 50 to 1000 nm.
In some embodiments, the polyolefin microporous membrane has a thickness of 3 to 200 μm, and may be, for example, 8 to 120 μm, 12 to 100 μm, or 20 to 40 μm. The thickness of the polyolefin microporous membrane directly influences the thickness of the composite cloth, and further influences the thickness of the protective clothing; the thickness of the polyolefin microporous membrane can be selected according to the grade requirement of the protective clothing or the product performance design, and is not particularly limited herein.
In some embodiments, the antimicrobial agent includes organic antimicrobial agents, inorganic antimicrobial agents, and natural antimicrobial agents, wherein the organic antimicrobial agents are one or more of vanillic aldehyde compounds, ethyl vanillic aldehyde compounds, anilides, imidazoles, thiazoles, isothiazolone derivatives, quaternary ammonium salts, guars, and phenols, such as citric acid, potassium sorbate, tea polyphenols, polyhexamethylene guanidine and its derivatives, and the like; the inorganic antibacterial agent is prepared by fixing silver, copper, zinc, titanium or their ions on fluorite or silica gel, such as silver-carrying antibacterial agent, silver-carrying copper antibacterial agent, TiO2Etc.; the natural antibacterial agentIs one or more of chitin, mustard, castor oil and horseradish.
It should be noted that blending of plastic and antimicrobial powder is a common method for preparing antimicrobial plastic. The antibacterial agents blended with plastics are classified into organic antibacterial agents and inorganic antibacterial agents. The organic antibacterial agent is a traditional antibacterial agent, is widely applied to the medical and industrial fields, and has the defects of strong toxicity, poor heat resistance, easy decomposition, possibility of causing microbial drug resistance and the like of partial organic matters. Inorganic antibacterial agents are superior to organic antibacterial agents in terms of antibacterial properties, safety, durability, heat resistance, and the like. The silver ion has the characteristics of broad-spectrum antibacterial property, high sterilization efficiency and difficult generation of drug resistance, so the silver ion is an important variety in inorganic antibacterial agents.
In some embodiments, the hydrophobic filler is one or more of vinyltrimethoxysilane, vinyltriethoxysilane, epoxysiloxane, isobutyltriethoxysilane, polyphenylmethylsiloxane, reactive wax, long chain alkane having 10 or more carbon atoms, fluorocarbon silane, and functional fluorocarbon compounds, but is not limited thereto. The hydrophilic filler is one or more of polyethylene glycol, polypropylene glycol, polyvinylpyrrolidone, acrylate, acrylic acid graft polymer, acrylate graft polymer, urethane acrylate, and polyvinyl alcohol, but is not limited thereto.
In some embodiments, at least one of the type a coextruded film, the type B coextruded film, and the type C coextruded film includes a softener for improving flexibility and wrinkle resistance; the softener is one or more of anionic, cationic, amphoteric, organosilicon, polyethylene and nonionic oxyethylene softening agents.
The embodiment proposes that the functional auxiliary agent is added into the polyolefin, so that the flexibility of the molecular chains and the interaction between the molecular chains can be improved, the friction force between fibers is reduced, the smoothness and the softness of the material are enhanced, and the wrinkle recovery angle of the material is improved, so that the super-softness and anti-wrinkle effects of the protective material are realized.
In some embodiments, the compoundThe moisture permeability of the combined fabric is more than or equal to 5500 g/(m)2·d)。
In some embodiments, the composite fabric has a heat shrinkage of 0.1 to 5%, for example, implementations of the present application can achieve a heat shrinkage of less than 3%; and the heat shrinkage in the MD direction is 0.2% -2.7%, and the heat shrinkage in the TD direction is only 0.1% -0.3%.
In some embodiments, the composite cloth has a synthetic blood penetration resistance of greater than or equal to grade 6.
In some embodiments, the filtration efficiency of the composite cloth is greater than or equal to 99.93%.
In some embodiments, there is also provided a method for preparing a composite fabric, as shown in fig. 2, comprising the steps of:
s10, melting and extruding at least two polyolefins with different functions by using a double-screw extruder, and forming at least two co-extruded films through traction, cooling and heat treatment of a casting roll, wherein at least one of the at least two co-extruded films is a high-strength polyolefin co-extruded film; the co-extruded film is stretched and heat-set to prepare the polyolefin microporous film;
s20, compounding the polyolefin microporous membrane with non-woven fabric and/or woven fabric in a thermal compounding or adhesive compounding mode to obtain the composite fabric.
The preparation method of the polyolefin microporous membrane in this embodiment is a melt stretching method or a dry stretching method, and specifically includes: extruding and casting polyolefin particles to obtain a casting film; carrying out high-temperature annealing treatment on the casting membrane to perfect the lamella to obtain an annealing membrane; performing cold drawing and hot drawing on the annealed membrane to obtain a stretched porous membrane; and (3) performing heat setting on the stretched porous membrane to obtain the polyolefin microporous membrane.
In the embodiment, a mode of producing the base film by using the battery diaphragm is creatively adopted, namely a melt stretching method, a polyolefin microporous film is prepared by adopting a polyolefin raw material treated by a special process and a multilayer co-extrusion process, and then the polyolefin microporous film is compounded with non-woven fabric and/or woven fabric to prepare the composite fabric. In the embodiment, the composite cloth is prepared by adopting the multilayer co-extrusion polyolefin microporous membrane of the special process of the battery diaphragm, so that the thermal stability of the composite cloth can be improved, and the use requirement of high-temperature steam sterilization can be met; the composite cloth inherits the advantages of air permeability, moisture permeability, barrier property, high mechanical strength and the like of the battery diaphragm, and provides a high-performance composite material for medical protective clothing. Further, in the embodiment, by adding a functional monomer or a softener or performing surface treatment on the polyolefin microporous membrane, the flexibility of the molecular chains and the interaction between the molecular chains are improved, the friction force between fibers is reduced, the smoothness and the softness of the material are improved, and the super-soft and anti-wrinkle effects of the composite fabric can be realized.
The key point of the embodiment is that the polyolefin microporous membrane is adopted to prepare the composite cloth, and as for a specific compounding mode, the compounding of the existing protective clothing composite material can be referred, such as thermal compounding or adhesive compounding; of course, it is not excluded that other combinations may also be used.
Preferably, in the composite fabric of the present embodiment, the nonwoven fabric is a polymer nonwoven fabric and/or a nonwoven fiber fabric, and the woven fabric is a woven fabric of synthetic fibers and/or a woven fabric of natural fibers. The polymer nonwoven fabric may be at least one of a spunlace nonwoven fabric, a melt-blown nonwoven fabric, or a spunbond nonwoven fabric.
The composite fabric of the present embodiment may be formed by combining a polyolefin microporous membrane and a nonwoven fabric, may be formed by combining a polyolefin microporous membrane and a woven fabric, or may be formed by combining a polyolefin microporous membrane, a woven fabric, and a nonwoven fabric. Further, the nonwoven fabric and the woven fabric may be single-layered or multi-layered. The composite mode of the composite cloth can be cross-laminated composite of layers or other modes, and can be determined according to requirements. In an implementation manner of the present application, specifically, a polyolefin microporous membrane is used as an outer surface layer, a non-woven fabric or a woven fabric is used as an inner surface layer, and the two layers are thermally compounded or compounded by an adhesive to form a composite fabric.
In some embodiments, the invention also provides application of the composite cloth, wherein the composite cloth is used for preparing an outer cover for protection, and the outer cover for protection comprises medical protective clothing, tents, outdoor jacket and medical packaging bags.
The medical protective clothing has the characteristics of one-way moisture permeability, seepage resistance, bacteria resistance, softness, wearing comfort and the like because the medical protective clothing is prepared from the composite fabric; moreover, the mechanical strength is high, and the clothes are not easy to damage when worn; the heat stability is good, the high temperature resistance is good, and high-pressure steam sterilization can be adopted; is an advanced medical protective garment with high performance and high cost performance. It can be understood that the protective clothing of this application can sterilize fast, recycle fast after using, has alleviated the problem that such emergency like new coronavirus epidemic situation is huge to the protective clothing demand to a certain extent.
The application further discloses application of the composite cloth in preparation of medical or non-medical protective equipment.
It is understood that the composite fabric of the present application, due to its good one-way air permeability, moisture permeability, barrier property, thermal stability and mechanical strength, can be used for preparing other medical protective equipment or other non-medical protective equipment besides protective clothing, and is not limited herein.
The present application is described in further detail below with reference to specific embodiments and the attached drawings. The following examples are intended to be illustrative of the present application only and should not be construed as limiting the present application. Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
In the embodiment, polypropylene with the melt index of 2g/10min is used as the layer A and the layer C, polypropylene with the melt index of 0.5g/10min is used as the layer B to prepare a three-layer co-extrusion polypropylene microporous membrane which is used as the outer surface layer of the medical protective clothing material, and the outer surface layer is compounded with polypropylene non-woven fabric with the thickness of 200 μm purchased from the market in a heat sealing mode to form the composite cloth of the embodiment. Among them, commercially available polypropylene nonwoven fabrics are available from Hunan Xinlong nonwoven materials Co. The hydrophobic filler adopted in the layer A is 2 wt% of epoxy resin, and the antibacterial agent is 0.5 wt% of silver-loaded antibacterial agent; the hydrophilic filler used in layer C is 2 wt% polypropylene glycol.
The specific preparation method of the composite cloth comprises the following steps:
(1) extrusion casting: extruding and casting two different polypropylene particles through a double-screw extruder and a flow divider to obtain a casting film. The casting speed is 120m/min, and the extrusion temperature is 230 ℃;
(2) annealing: carrying out high-temperature annealing treatment on the casting membrane to perfect the lamella to obtain an annealing membrane, wherein the annealing temperature is 150 ℃;
(3) stretching: and carrying out cold drawing and hot drawing on the annealed membrane to obtain the stretched porous membrane. The cold drawing temperature is 20 ℃, the hot drawing temperature is 140 ℃, and the drawing ratio is 3.5;
(4) heat setting: carrying out heat setting on the stretched porous membrane to obtain a polypropylene microporous membrane, wherein the heat setting temperature is 160 ℃;
(5) thermal compounding: the polypropylene microporous membrane and the non-woven fabric are thermally compounded at 160 ℃ and rolled to obtain the composite fabric of the embodiment.
The composite cloth of this example was subjected to moisture permeability, areal density, breaking strength, elongation at break, heat shrinkage, melting point, porosity, synthetic blood penetration resistance, filtration efficiency and average pore diameter tests. The pore diameter is tested according to the enterprise standard, specifically, the pore diameter is tested by using a capillary flow method, a sample which is completely saturated by the immersion liquid is placed in a closed sample chamber with a certain volume, under a series of pressures, gas overcomes the capillary action of the liquid in the pore, the immersion liquid in the pore is discharged until the pore is emptied, the gas pressure and the flow rate are recorded, and then the pore diameter size and the pore diameter distribution are calculated according to a corresponding formula. Testing equipment: a PMI aperture analyzer; the instrument model is as follows: CFP-1500 AEP. The surface density, the thermal shrinkage, the thickness and the porosity are tested by adopting a method in GB/T36363-2018; melting point test reference standard GB/T19466-2004; the moisture permeability is tested by the method in GB/T12704-2009; the breaking strength and the breaking elongation are tested by the method in GB/T3923.1-2013; the filtration efficiency, surface moisture resistance, and resistance to synthetic blood penetration were tested using the method in GB/T19082-. In each test, each sample was tested 5 times in total, and the average value was obtained, and the test results are shown in table 1.
Example 2
In the embodiment, polypropylene with the melt index of 1g/10min is used as the layer A and the layer C, polypropylene with the melt index of 0.8g/10min is used as the layer B to prepare the three-layer co-extrusion polypropylene microporous membrane which is used as the outer surface layer of the medical protective clothing material, and the rest is the same as the embodiment 1.
The composite fabric of this example was tested as in example 1, and the test results are shown in table 1.
Table 1 test results of various properties of the composite fabric of the examples
It can be seen from comparison of examples 1 and 2 that the polypropylene microporous membrane has good air permeability as the outer surface layer of the medical protective clothing material, and is comfortable to wear and not prone to smoldering and sweating at higher temperature. The data of breaking strength and breaking elongation show that the polypropylene microporous membrane has good mechanical strength, and the moisture permeability, porosity and mechanical property can be regulated and controlled by regulating and controlling the preparation process of the membrane.
In order to meet the requirement of comfort, according to GB/T19082-2D). As can be seen from the data in Table 1, the examples have moisture permeabilities of more than 5500 g/(m)2D) satisfies the moisture permeability requirement. In addition, according to GB/T19082-.
Therefore, the composite cloth prepared in the embodiments 1 and 2 can meet various service performances of the protective clothing, and is a high-performance medical protective composite material.
Example 3
In this example, different polypropylene microporous membrane stretching preparation processes were tested on the basis of example 1, specifically as follows:
test 1: performing cold drawing and hot drawing on the annealed membrane to obtain a stretched porous membrane; the cold drawing temperature is 40 ℃, the hot drawing temperature is 150 ℃, the drawing rate is 1.8, and the heat setting temperature is 150 ℃;
test 2: performing cold drawing and hot drawing on the annealed membrane to obtain a stretched porous membrane; the cold drawing temperature is 60 ℃, the hot drawing temperature is 140 ℃, the drawing ratio is 2.3, and the heat setting temperature is 140 ℃;
test 3: performing cold drawing and hot drawing on the annealed membrane to obtain a stretched porous membrane; the cold drawing temperature is 80 ℃, the hot drawing temperature is 140 ℃, the drawing ratio is 3.2, and the heat setting temperature is 140 ℃.
The polypropylene microporous membrane prepared above was used to prepare a composite cloth according to the protocol of example 1. The composite fabric of this example was tested as in example 1, and the test results are shown in table 2.
Table 2 test results of various properties of composite cloth
The results in table 2 show that, comprehensively, the tensile preparation process parameters of the polypropylene microporous membrane are that the cold drawing temperature is 60 ℃, the hot drawing temperature is 140 ℃, the tensile ratio is 2.3, and the polypropylene microporous membrane with high breaking strength, high elongation at break, good synthetic blood penetration resistance and large moisture permeability can be prepared at the heat setting temperature of 140 ℃, so that the test requirements of the composite fabric of the protective clothing are met.
In addition, by controlling the parameters of melt stretching, the average pore diameter of the polypropylene microporous membrane is 50-120nm, and the porosity is 10-95%, so that the use requirements of protective clothing and high-pressure steam sterilization are met. Wherein, the polypropylene microporous membrane with the average pore diameter of 50-80nm and the porosity of 50-80% has better effect; can effectively ensure the air permeability, the moisture permeability and the comfort, can also play a good role in isolation and protection, and is particularly suitable for medical protective clothing.
Example 4
In this example, the addition of filler was tested on the basis of example 1:
test 1: the hydrophobic filler adopted in the layer A is 2 wt% of epoxy resin, and the antibacterial agent is 1 wt% of silver-loaded antibacterial agent; the hydrophilic filler adopted by the layer C is 3 wt% of polypropylene glycol;
test 2: the hydrophobic filler adopted in the layer A is 2 wt% of fluorinated silane, and the antibacterial agent is 1 wt% of silver-loaded antibacterial agent; the hydrophilic filler adopted by the layer C is 2 wt% of polypropylene glycol;
test 3: the hydrophobic filler adopted in the layer A is 2 wt% of fluorinated silane, and the antibacterial agent is 1 wt% of silver-loaded antibacterial agent; the hydrophilic filler used in layer C was 3 wt% polypropylene glycol.
The polypropylene microporous membrane prepared above was used to prepare a composite cloth according to the protocol of example 1. The composite fabric of this example was tested as in example 1, and the test results are shown in table 3.
Table 3 test results of various properties of the composite cloth
The results show that the surface moisture resistance, the resistance to penetration by synthetic blood and the filtration efficiency can be consistently high under all process conditions. The sample obtained under the process condition of the experiment 3 has the best perspective and can reach 15000 g/(m)2D), indicating that a small increase in the amount of hydrophilic filler is advantageous for the improvement of moisture permeability. However, if the amount of the additive is further increased, too much compounding is carried out in the polypropylene melt, which affects the pore-forming consistency of the microporous membrane. Meanwhile, the polypropylene can be used for preparing the polypropylene with the melting point of more than 135 ℃, particularly the melting point of 155-The polypropylene microporous membrane can be used for preparing composite cloth meeting the use requirement of protective clothing, so that the prepared composite cloth has good moisture permeability, barrier property, thermal stability and mechanical strength, and can be suitable for high-pressure steam sterilization.
In addition, the thickness of the polypropylene microporous membrane can be determined according to the use requirement of the protective clothing, and the polypropylene microporous membrane with the thickness of 3-200 μm can be used for preparing the composite cloth meeting the use requirement.
Example 5
In this example, the addition of polyolefin raw material and filler was tested on the basis of example 1:
test 1: the polyolefin adopted in the layer A is a copolymer of 95 percent of propylene and 5 percent of vinyl silicone oil, the hydrophobic filler is 2 weight percent of epoxy resin, and the antibacterial agent is 1 weight percent of silver-loaded antibacterial agent; the layer C adopts polypropylene added with 0.6 wt% of nonionic polyoxyethylene ether softener, and the hydrophilic filler is 3 wt% of polypropylene glycol;
test 2: the polyolefin adopted in the layer A is a copolymer of 85 percent of propylene and 15 percent of vinyl silicone oil, the hydrophobic filler is 2 weight percent of epoxy resin, and the antibacterial agent is 1 weight percent of silver-loaded antibacterial agent; the layer C adopts polypropylene added with 0.6 wt% of nonionic polyoxyethylene ether softener, and the hydrophilic filler is 3 wt% of polypropylene glycol;
test 3: the polyolefin adopted in the layer A is a copolymer of 95 percent of propylene and 5 percent of vinyl silicone oil, the hydrophobic filler is 2 weight percent of epoxy resin, and the antibacterial agent is 1 weight percent of silver-loaded antibacterial agent; the layer C adopts polypropylene added with 1 wt% of nonionic polyoxyethylene ether type softening agent, and the hydrophilic filler is 3 wt% of polypropylene glycol.
The polypropylene microporous membrane prepared above was used to prepare a composite cloth according to the protocol of example 1. The overall performance of the composite cloth was tested as in example 1, and in addition, the wrinkle recovery angle of the rechecked cloth was measured by a digital fabric wrinkle recovery instrument. The test results are shown in table 4.
Table 4 test results of various properties of the composite cloth
The results show that the surface moisture resistance, the resistance to penetration by synthetic blood and the filtration efficiency can be consistently high under all process conditions. The samples obtained under the process conditions of test 2 and test 3 had a greater wrinkle recovery angle, indicating that the samples of test 2 and test 3 had better softness than test 1. The results show that the moisture resistance, the synthetic blood penetration resistance and the filtering efficiency of the material can be ensured by the copolymerization of the functional monomer and the addition of the softener, and the flexibility and the crease resistance of the material can be improved. In addition, the higher the content of the functional monomer or the softener, the larger the wrinkle recovery angle of the material, which indicates that the flexibility and the anti-wrinkle effect of the material are higher. However, if the proportion of the functional monomer or the filler is further increased, too much mixing material is mixed in the polypropylene melt, which affects the pore-forming consistency of the microporous membrane.
Example 6
In this example, the mode of the material after-treatment was tested on the basis of example 1:
test 1: performing ultrasonic finishing on the polyolefin microporous membrane: the power is 0.4W/cm2Ultrasonic treatment at frequency of 30kHz and 50 deg.C for 5 min; the polypropylene non-woven fabric is not treated;
test 2: and (3) carrying out organic silicon softening agent treatment on the polypropylene non-woven fabric without post-treatment on the polyolefin microporous membrane: the concentration of the organosilicon softener is 60g/L, the baking temperature is 130 ℃, the baking time is 70s, and the pH value of the finishing liquid is 6.
Test 3: performing ultrasonic finishing on the polyolefin microporous membrane: the power is 0.4W/cm2Ultrasonic treatment is carried out for 10min at the temperature of 50 ℃ with the frequency of 30 kHz; carrying out organic silicon softening agent treatment on the polypropylene non-woven fabric;
the polypropylene microporous membrane prepared above was used to prepare a composite cloth according to the protocol of example 1. The overall performance of the composite cloth was tested as in example 1, and in addition, the wrinkle recovery angle of the rechecked cloth was measured by a digital fabric wrinkle recovery instrument. The test results are shown in table 5.
Table 5 test results of various properties of composite cloth
The results show that the composite cloths prepared in tests 1 to 3 all stably meet high requirements for surface moisture resistance, synthetic blood penetration resistance and filtration efficiency. In addition, the samples obtained from tests 1-3 all had a higher crease recovery angle than the samples prepared in example 1, indicating that post-treatment of both microporous films and nonwoven films can improve the softness and crease resistance of the composite films. In addition, the sample crease recovery angle obtained under the process condition of the test 3 is larger than that of the samples of the test 2 and the test 1, which shows that the microporous membrane and the non-woven fabric are subjected to post-treatment simultaneously, so that the composite membrane has the advantages of ensuring the moisture resistance, the synthetic blood penetration resistance and the filtering efficiency of the material, and simultaneously improving the flexibility and the crease resistance of the material.
Example 7
The polyolefin used in this example was a polyolefin prepared by copolymerizing 94 mol% of 1-butene with 6 mol% of vinyltrimethoxysilane. The polyolefin had a melt index of 1.4g/10min as the A and C layers of the microporous membrane. Layer B was 95 wt% polypropylene with a melt index of 1.0g/10min blended with 5% glass fiber as layer B. The raw materials are prepared into a three-layer co-extrusion microporous membrane through a co-extrusion process, the three-layer co-extrusion microporous membrane is used as an outer surface layer of the medical protective clothing material, and the outer surface layer is compounded with a commercially available polypropylene non-woven fabric with the thickness of 200 mu m in a heat sealing mode to form the composite cloth of the embodiment. Among them, commercially available polypropylene nonwoven fabrics are available from Hunan Xinlong nonwoven materials Co. (test 1)
On the basis of example 7, further tests were carried out on the raw material work-up mode:
test 2: carrying out hydrophobic treatment on the layer A of the microporous membrane: the surface of the microporous membrane A is coated by using fluorinated silane/ethanol solution with the concentration of 5 wt% as a hydrophobic modifier, and then is dried at the temperature of 80 ℃;
test 3: carrying out organic silicon softener spraying treatment on a commercially available polypropylene non-woven fabric: the organosilicon softener A33 has a concentration of 50g/L and a spraying amount of 10g/m2And then dried at 80 ℃.
The microporous membrane and the nonwoven fabric prepared above were used to prepare a composite fabric according to the protocol of example 1. The overall performance of the composite fabric was tested as in example 1 and the results are shown in table 6.
Table 6 test results of various properties of composite cloth
The results show that the surface moisture resistance, the synthetic blood penetration resistance and the filtration efficiency of the composite cloths prepared in the tests 1 to 3 can all stably meet high requirements. The composite cloth prepared by the embodiment has better strength, which is related to the glass fiber reinforced filler added in the microporous membrane B layer; the composite cloth prepared by the embodiment has a higher wrinkle recovery angle, which shows that the flexibility of the composite cloth can be improved by taking vinyl trimethoxy silane as a functional monomer. The wrinkle recovery angle of the composite cloth in the test 3 is larger than that of the composite cloth in the tests 1 and 2, which shows that the flexibility of the composite film can be improved by performing flexibility post-treatment on the material besides adding the functional monomer in the raw material. In addition, the surface moisture resistance of the composite cloth in test 2 is more excellent than that in tests 1 and 3, which shows that the surface moisture resistance of the composite cloth can be effectively improved by performing hydrophobic treatment on the surface of the microporous membrane.
Example 8
The polyolefin adopted in the embodiment is polyolefin copolymerized by 75 percent of propylene and 25 percent of 1-butene and has a melt index of 1.3g/10min as the layer A and the layer C of the microporous membrane; the raw material of the layer B is a blend of the poly (propylene-butylene) and 4 wt% of carbon fiber. The raw materials are prepared into a three-layer co-extrusion microporous membrane through a co-extrusion process, and the three-layer co-extrusion microporous membrane is used as an outer surface layer of the medical protective clothing material. The inner layer of the protective clothing has a gram weight of 25g/m2Poly 4-methyl-1-pentene meltblown nonwoven fabric. The above materials were thermally bonded and combined to form the composite cloth of this example. (test 1)
On the basis of example 8, further tests were carried out on the material work-up:
test 2: 2 wt% of polydimethylsiloxane and 3 wt% of fluorinated silane are added into the microporous membrane layer A;
test 3: 2 wt% of polydimethylsiloxane and 3 wt% of fluorinated silane are added into the microporous membrane layer A, and 4 wt% of polydimethylsiloxane non-woven fabric is added into the inner layer raw material poly-4-methyl-1-pentene of the protective clothing.
The microporous membrane and the nonwoven fabric prepared above were used to prepare a composite fabric according to the protocol of example 1. The overall performance of the composite fabric was tested as in example 1 and the results are shown in table 7.
Table 7 test results of various properties of composite cloth
The results show that the composite cloths prepared in tests 1 to 3 all have a porosity, a melting point, a resistance to penetration by synthetic blood and a filtration efficiency which are all stably high. The composite cloth prepared by the embodiment has better strength, which is related to the carbon fiber reinforced filler added in the microporous membrane layer B; the surface moisture resistance of the composite cloth of test 2 and test 3 is more excellent than that of test 1, which shows that the addition of the functional monomer fluorinated silane to the microporous membrane material can improve the surface hydrophobicity of the microporous membrane and the moisture resistance of the composite cloth. In addition, the wrinkle recovery angle of the composite fabric in the test 3 is larger than that of the composite fabric in the test 2 and larger than that of the composite fabric in the test 1, and the flexibility of the composite film can be improved by adding polydimethylsiloxane softener filler into the surface microporous film and the non-woven fabric raw materials.
Comparative example 1
The commercially available protective clothing material is used as a research object, and the preparation method can refer to the preparation method in patent CN 107536136A. The commercial protective garment material of this example was purchased from nono-health care equipment.
The commercial protective clothing material of this example was tested as in example 1, and the test results are shown in table 8.
Table 8 results of testing various properties of comparative example protective clothing materials
As can be seen from the results of comparative analysis in tables 1 and 8, in examples 1 and 2 of the present application, the polypropylene microporous membrane is introduced as the outer surface layer of the protective clothing material, and the outer surface layer is hydrophobic, and the inner surface layer is hydrophilic, so that the composite cloth has good one-way moisture permeability, and the moisture permeability of the composite cloth is 3985.06 g/(m) of the existing commercial protective clothing material2D) to 15000 g/(m)2D) above; examples 1 and 2 significantly improve the moisture permeability of the protective clothing material, and can continuously exude sweat and sweat generated by a human body to the outside, thereby increasing the comfort.
In addition, examples 1 and 2 are also effective in improving the thermal stability of the material, making it suitable for autoclaving. In autoclaving, the sterilization temperature is typically 120-132 ℃. The melting point of the composite cloth of the embodiment is above 160 ℃, while the melting point of the existing commercialized protective clothing material is only 120.82 ℃; thus, the higher melting point of the composite cloth of the examples allows the composite cloth material to maintain structural integrity during autoclaving. In addition, by comparing the heat shrinkage of the polypropylene microporous membranes used in the examples with that of the comparative example 1, the heat shrinkage of the polypropylene microporous membranes used in the examples is low, the longitudinal shrinkage is not more than 1% at most, and the heat stability is good. The longitudinal shrinkage of the comparative example was as high as 33.37%, much higher than that of the example. Therefore, the characteristics of high melting point and excellent thermal stability of the polypropylene microporous membrane are suitable for the high-pressure steam sterilization process.
The mechanical properties of the medical protective garment material are also important in order to ensure that the protective garment has sufficient strength to resist physical damage. The three-layer co-extrusion polypropylene microporous membrane has the advantages that the polypropylene raw material with high strength is introduced into the middle layer, so that the overall strength of the protective clothing composite cloth is greatly improved, the breaking strength and the breaking elongation of the comparative example and the comparative example are visible, the mechanical strength of the example is higher than that of the comparative example, and the protective clothing composite cloth has better mechanical performance and protective effect.
The polypropylene microporous membrane outer surface layer of the composite cloth of the example of the present application is observed by using a Scanning Electron Microscope (SEM), wherein the observation result of the polypropylene microporous membrane outer surface layer of the composite cloth of the example 1 is shown in fig. 3. The results show that the outer surface layers of examples 1 and 2 have the characteristics of small pore size and uniform distribution, and can effectively isolate and protect bacteria, viruses, harmful gases and particles. Meanwhile, the results in table 1 show that the composite cloth of the embodiment of the present application has a synthetic blood penetration resistance of not less than 6 grade, which is much higher than the level of not less than 2 specified in GB/T19082-2009, and can prevent the blood penetration of the patient and reduce the risk of infection of the patient.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. The composite cloth is characterized by comprising a polyolefin microporous membrane and a non-woven cloth and/or a woven cloth which are compounded with the polyolefin microporous membrane;
the polyolefin microporous membrane is prepared by adopting a co-extrusion process: melting and extruding at least two polyolefins with different functions by using a double-screw extruder, and forming at least two co-extruded films by traction, cooling and heat treatment of a casting roll, wherein at least one of the at least two co-extruded films is a high-strength polyolefin co-extruded film; and the co-extruded film is subjected to stretching and heat setting treatment to obtain the polyolefin microporous film.
2. The composite fabric of claim 1, wherein the polyolefin has a melting point of greater than or equal to 135 ℃; the polyolefin is composed of polyolefin and functional filler which are copolymerized and synthesized by screening different functional monomers and regulating and controlling the proportion of the monomers; the functional monomer comprises at least one of propylene, butylene, 4-methyl-1-pentene, cyclopentadiene, ethylene, oxyethylene, siloxane and glycol; the functional filler comprises at least one of an antibacterial agent, a hydrophobic filler, a hydrophilic filler, a softener and a reinforcing filler.
3. The composite cloth according to claim 2, wherein the antibacterial agent comprises an organic antibacterial agent, an inorganic antibacterial agent and a natural antibacterial agent, wherein the organic antibacterial agent is one or more of vanillin compounds, ethyl vanillin compounds, anilides, imidazoles, thiazoles, isothiazolone derivatives, quaternary ammonium salts, guars and phenols; the inorganic antibacterial agent is prepared by fixing silver, copper, zinc, titanium or ions thereof on the surface of fluorite or silica gel; the natural antibacterial agent is one or more of chitin, mustard, castor oil and horseradish.
4. The composite cloth of claim 2, wherein the hydrophobic filler is one or more of vinyltrimethoxysilane, vinyltriethoxysilane, epoxysiloxane, isobutyltriethoxysilane, polyphenylmethylsiloxane, reactive wax, long-chain alkane with 10 or more carbon atoms, fluorocarbon silane, and functional fluorocarbon compound; the hydrophilic filler is one or more of polyethylene glycol, polypropylene glycol, polyvinylpyrrolidone, acrylate, acrylic acid graft polymer, acrylate graft polymer, polyurethane acrylate and polyvinyl alcohol; the reinforcing filler is one or more of glass fiber, carbon tubes, graphene, carbon powder, silicon dioxide, titanium dioxide, halloysite, mica, talcum powder, calcium carbonate and barium sulfate.
5. The composite cloth of claim 2, wherein the polyolefin microporous membrane comprises an A-type co-extrusion membrane, a B-type co-extrusion membrane and a C-type co-extrusion membrane which are sequentially stacked from outside to inside, and the A-type co-extrusion membrane comprises polyolefin, hydrophobic filler and an antibacterial agent; the B-type co-extrusion film is a high-strength polyolefin co-extrusion film, and comprises polyolefin and reinforcing filler; the C-type coextruded film includes a polyolefin and a hydrophilic filler.
6. The composite cloth of claim 5, wherein at least one of the A-type co-extruded film, the B-type co-extruded film and the C-type co-extruded film comprises a softener for improving flexibility and crease resistance; the softener is one or more of anionic, cationic, amphoteric, organosilicon, polyethylene and nonionic oxyethylene softening agents.
7. The composite cloth of claim 1, wherein the polyolefin microporous membrane has a porosity of 10 to 95% and an average pore size of 50 to 2000 nm.
8. The composite fabric of claim 1, wherein the polyolefin microporous membrane has a thickness of 3 to 200 um;
and/or the longitudinal breaking strength of the composite cloth is greater than or equal to 130N, and the transverse breaking strength of the composite cloth is greater than or equal to 58N;
and/or the longitudinal elongation at break of the composite fabric is more than or equal to 20 percent, and the transverse elongation at break of the composite fabric is more than or equal to 50 percent;
and/or the moisture permeability of the composite cloth is more than or equal to 5500 g/(m)2·d)；
And/or, the thermal shrinkage of the composite cloth is 0.1-5%;
and/or the composite cloth has the synthetic blood penetration resistance of more than or equal to grade 6;
and/or the filtration efficiency of the composite cloth is more than or equal to 99.93 percent.
9. The preparation method of the composite cloth is characterized by comprising the following steps:
melting and extruding at least two polyolefins with different functions by using a double-screw extruder, and forming at least two co-extruded films through traction, cooling and heat treatment of a casting roll, wherein at least one of the at least two co-extruded films is a high-strength polyolefin co-extruded film; the co-extruded film is stretched and heat-set to prepare the polyolefin microporous film;
and compounding the polyolefin microporous membrane with non-woven fabric and/or woven fabric in a thermal compounding or adhesive compounding mode to obtain the composite fabric.
10. Use of a composite cloth according to any one of claims 1 to 8 for the manufacture of protective garments comprising medical protective clothing, tents, jackets and medical packaging bags.
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