CN112571907A - TPU waterproof moisture permeable barrier film for medical protective clothing - Google Patents
TPU waterproof moisture permeable barrier film for medical protective clothing Download PDFInfo
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- CN112571907A CN112571907A CN202011411428.7A CN202011411428A CN112571907A CN 112571907 A CN112571907 A CN 112571907A CN 202011411428 A CN202011411428 A CN 202011411428A CN 112571907 A CN112571907 A CN 112571907A
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- elastomer
- polyethylene glycol
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- 230000004888 barrier function Effects 0.000 title claims abstract description 17
- 230000001681 protective effect Effects 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 90
- 229920001971 elastomer Polymers 0.000 claims abstract description 72
- 239000000806 elastomer Substances 0.000 claims abstract description 70
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 70
- 239000012528 membrane Substances 0.000 claims abstract description 49
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 49
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 49
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 41
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 41
- 239000003292 glue Substances 0.000 claims abstract description 7
- 239000004433 Thermoplastic polyurethane Substances 0.000 claims description 81
- 238000003756 stirring Methods 0.000 claims description 47
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 45
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 36
- 229920002554 vinyl polymer Polymers 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 33
- 238000002156 mixing Methods 0.000 claims description 30
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000002105 nanoparticle Substances 0.000 claims description 22
- 239000000377 silicon dioxide Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- 239000000839 emulsion Substances 0.000 claims description 20
- 229920001296 polysiloxane Polymers 0.000 claims description 20
- 238000001291 vacuum drying Methods 0.000 claims description 20
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 20
- 239000003054 catalyst Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 16
- 239000000178 monomer Substances 0.000 claims description 16
- 238000009987 spinning Methods 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- 239000000835 fiber Substances 0.000 claims description 14
- 150000002334 glycols Chemical class 0.000 claims description 14
- 150000004687 hexahydrates Chemical class 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 12
- 239000004327 boric acid Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 claims description 12
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 6
- 235000011152 sodium sulphate Nutrition 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims 3
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims 1
- 238000001523 electrospinning Methods 0.000 claims 1
- 230000035699 permeability Effects 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract 3
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 69
- 238000010041 electrostatic spinning Methods 0.000 description 12
- 235000012239 silicon dioxide Nutrition 0.000 description 10
- 238000002604 ultrasonography Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 229920001843 polymethylhydrosiloxane Polymers 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
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- 238000005406 washing Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 229940037312 stearamide Drugs 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000000071 blow moulding Methods 0.000 description 1
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- 238000005266 casting Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- B32—LAYERED PRODUCTS
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
- B32B27/322—Layered products comprising a layer of synthetic resin comprising polyolefins comprising halogenated polyolefins, e.g. PTFE
-
- 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
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/02—Layered materials
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/10—Impermeable to liquids, e.g. waterproof; Liquid-repellent
- A41D31/102—Waterproof and breathable
-
- 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
- A41D31/12—Hygroscopic; Water retaining
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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
- A41D31/14—Air permeable, i.e. capable of being penetrated by gases
- A41D31/145—Air permeable, i.e. capable of being penetrated by gases using layered materials
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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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
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- B32B27/40—Layered products comprising a layer of synthetic resin comprising polyurethanes
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
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- D01F6/48—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 polymers of halogenated hydrocarbons
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- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/00—Properties of the layers or laminate
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- General Health & Medical Sciences (AREA)
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Abstract
本发明公开一种医疗防护服用TPU防水透湿阻隔膜，包括复合TPU膜和复合聚四氟乙烯膜；所述复合TPU膜的厚度为2mm，所述复合聚四氟乙烯膜的厚度为3mm，复合TPU膜与复合聚四氟乙烯膜之间通过tw‑2036胶水粘结；将聚乙二醇分子接枝在弹性体表面，制得处理后的弹性体，赋予其亲水性能，解决了聚乙二醇分子缺少可反应的活性基团，无法通过化学接枝的方法接枝在弹性体表明的技术问题，之后步骤S3中将处理后的弹性体与TPU混合纺丝，制备出复合TPU膜，通过处理后的弹性体上的亲水基团能够赋予该复合膜优异的透湿性能，而且复合膜表面无微孔，具有优异的防水性能。The invention discloses a TPU waterproof and moisture-permeable barrier film for medical protective wear, which includes a composite TPU film and a composite polytetrafluoroethylene film; the thickness of the composite TPU film is 2 mm, and the thickness of the composite polytetrafluoroethylene film is 3 mm. The composite TPU film and the composite PTFE film are bonded by tw‑2036 glue; the polyethylene glycol molecules are grafted on the surface of the elastomer to obtain the treated elastomer, which is endowed with hydrophilic properties and solves the problem of polyethylene glycol. The ethylene glycol molecule lacks reactive active groups and cannot be grafted on the elastomer by chemical grafting. The technical problem indicated, then in step S3, the treated elastomer and TPU are mixed and spun to prepare a composite TPU film , the hydrophilic group on the treated elastomer can give the composite membrane excellent moisture permeability, and the composite membrane has no micropores on the surface and has excellent waterproof performance.
Description
Technical Field
The invention belongs to the technical field of TPU film preparation, and particularly relates to a TPU waterproof moisture permeable barrier film for medical protective clothing.
Background
TPU (thermoplastic polyurethane) is an environment-friendly high polymer, overcomes the defects of PVC and PU films, has most of the characteristics of rubber and common plastics, and also has excellent comprehensive physical and chemical properties, so that the TPU is also called as a future material. The TPU intermediate-permeability waterproof moisture-permeable film is a film prepared from TPU granules through a special process, inherits the excellent physical properties of TPU and has a wide application range. Because of the advantage of nontoxicity, accord with the requirement of environmental protection, TPU middle permeable waterproof moisture permeable membrane products are widely applied to the fields of advanced clothing, shoe materials, air blowing bags, packaging, artware and the like.
The Chinese invention patent CN103507191A discloses a novel casting and coiling middle-permeation waterproof moisture-permeable TPU film. The invention relates to a novel product of a novel cast reeling middle-transmission waterproof moisture-permeable TPU film, which comprises the steps of selecting TPU granules with a new formula, melting at high temperature, extruding from a die head of an extruder, cooling, forming and reeling. The device comprises a die head, a pattern shaping wheel, a forming cooling wheel, a driving wheel, a rubber unfolding wheel, a rolling driving wheel, an electrostatic elimination wheel, an anti-skid Teflon and a rolling device, wherein the pattern shaping wheel, the forming cooling wheel and the driving wheel are arranged below the die head of the extruder. The invention has unique and novel formula, breaks through the limitation that other intermediate-permeation waterproof moisture-permeable films can be produced only by blow molding and attaching PE, ensures that the subsequent operation is more convenient, reduces the double waste of polyethylene and thermoplastic polyurethane, saves the cost and improves the product quality.
Disclosure of Invention
The invention provides a TPU waterproof moisture permeable barrier film for medical protective clothing.
According to the invention, polyethylene glycol molecules are grafted on the surface of the elastomer to prepare the treated elastomer, so that the hydrophilic performance is endowed to the treated elastomer, and the technical problem that the polyethylene glycol molecules lack reactive active groups and cannot be grafted on the elastomer by a chemical grafting method is solved, then the treated elastomer and TPU are mixed and spun in step S3 to prepare the composite TPU membrane, the excellent moisture permeability can be endowed to the composite membrane through the hydrophilic groups on the treated elastomer, and the surface of the composite membrane is free of micropores and has excellent waterproof performance.
The purpose of the invention can be realized by the following technical scheme:
a TPU waterproof moisture permeable barrier film for medical protective clothing comprises a composite TPU film and a composite polytetrafluoroethylene film;
the composite TPU film is prepared by the following method:
step S1, adding vinyl polysiloxane and polymethylhydrosiloxane into a reaction kettle according to the weight ratio of 1: 3, then adding chloroplatinic acid hexahydrate and a polyvinyl monomer, stirring at a constant speed for 15min, then adding a sodium sulfate solution with the mass fraction of 10%, mixing uniformly, injecting into a mold, and curing at 65-85 ℃ for 10h to obtain an elastomer, wherein the weight of the chloroplatinic acid hexahydrate is controlled to be 0.5-0.8% of the weight of the vinyl polysiloxane, and the weight of the polyvinyl monomer is controlled to be 10% of the weight of the vinyl polysiloxane;
step S2, adding a polyethylene glycol derivative into isopropanol, uniformly mixing, adding a catalyst to prepare a mixed solution A, adding the elastomer prepared in the step S1 into the mixed solution A, heating in a water bath at 50-60 ℃ and magnetically stirring for 30min, taking out, respectively placing into acetone and deionized water for ultrasonic treatment for 2min, controlling the ultrasonic power to be 50-60W, preparing a treated elastomer, and controlling the weight ratio of the polyethylene glycol to the isopropanol to the catalyst to the elastomer to be 1: 10: 0.1-0.2: 1;
and S3, respectively adding the processed elastomer and TPU prepared in the step S2 into dimethylformamide, heating in a water bath at 50-65 ℃ and magnetically stirring for 4 hours to prepare spinning solution, then carrying out electrostatic spinning to prepare a composite TPU membrane, and controlling the weight ratio of the elastomer, the TPU and the dimethylformamide to be 1: 3: 10-20.
Mixing vinyl polysiloxane and polymethylhydrosiloxane in step S1, adding chloroplatinic acid hexahydrate as a catalyst, adding a polyvinyl monomer to prepare an elastomer, wherein the elastomer is provided with a silicon-hydrogen bond led out by the polyvinyl monomer, preparing a mixed solution A by using a polyethylene glycol derivative and isopropanol in step S2, adding the elastomer into the mixed solution A, carrying out addition reaction on the silicon-hydrogen bond on the elastomer and a double bond on the derivative, grafting polyethylene glycol molecules on the surface of the elastomer to prepare the treated elastomer, endowing the treated elastomer with hydrophilic performance, solving the technical problem that the polyethylene glycol molecules lack reactive active groups and cannot be grafted on the elastomer by a chemical grafting method, mixing and spinning the treated elastomer and TPU in step S3 to prepare a composite TPU membrane, and endowing the composite membrane with excellent moisture permeability by the hydrophilic groups on the treated elastomer, and the surface of the composite membrane has no micropores, and the composite membrane has excellent waterproof performance.
Further, the polyethylene glycol derivative is formed by mixing polyethylene glycol methyl ether acrylate and polyethylene glycol methyl ether methacrylate according to the weight ratio of 1: 1.
Further, the catalyst in step S2 is karstedt catalyst.
Further, the composite polytetrafluoroethylene membrane is prepared by the following method:
step S11, uniformly mixing polytetrafluoroethylene resin and stearic acid amide according to the weight ratio of 5: 1, transferring the mixture into a vacuum drying oven at 45-60 ℃ for drying, controlling the vacuum degree of the vacuum drying oven at-0.10 MPa and the drying time to be 8-10h, extruding and pressing to obtain a prefabricated product, placing the prefabricated product into the vacuum drying oven at 50 ℃ for drying for 10h to obtain a material, adding the material into deionized water, and magnetically stirring for 20min to obtain an emulsion B with the mass fraction of 60%;
step S12, dripping 10% of dilute hydrochloric acid by mass into 15% of ethanol aqueous solution by volume fraction, magnetically stirring at a rotating speed of 120r/min for 5min, then dripping KH550, controlling the dripping time to be 10min, uniformly stirring for 3min after the dripping is finished, adding tetraethoxysilane while stirring, continuously stirring at a uniform speed for 4h to prepare suspension, filtering and washing to prepare hydrophilic silica nanoparticles, wherein the weight ratio of the 10% of dilute hydrochloric acid to the 15% of ethanol aqueous solution to the KH550 to the tetraethoxysilane is controlled to be 2: 10: 0.1-0.2: 0.5;
step S13, adding hydrophilic silica nanoparticles into 60% emulsion B, adding 3% boric acid solution, mixing uniformly to obtain spinning solution, performing electrostatic spinning to obtain nascent fiber membrane, transferring to a muffle furnace, heating to 350 ℃ at a heating rate of 3-5 ℃/min, and roasting for 2h to obtain the composite polytetrafluoroethylene membrane, wherein the weight ratio of the hydrophilic silica nanoparticles to the 60% emulsion B to the 3% boric acid solution is 1: 15-20: 3-5.
Step S11, polytetrafluoroethylene resin and stearic acid amide are mixed to prepare a prefabricated product, then the stearic acid amide is removed through vacuum drying, the polytetrafluoroethylene resin is made to be a hollow structure, hydrophilic silica nanoparticles are prepared in step S12, the hydrophilic silica nanoparticles are mixed with 60% of emulsion B to prepare spinning solution, electrostatic spinning is conducted to prepare a fiber membrane, then roasting is conducted to prepare a composite polytetrafluoroethylene membrane, and the added nano silica particles can increase the roughness and pores of the surface of the prepared fiber and endow the fiber membrane with excellent air permeability and moisture permeability.
Further, the thickness of the composite TPU film is 2-3mm, the thickness of the composite polytetrafluoroethylene film is 2-3mm, and the composite TPU film and the composite polytetrafluoroethylene film are bonded through tw-2036 glue.
The invention has the beneficial effects that:
(1) the invention relates to a TPU waterproof and moisture permeable barrier film for medical protective clothing, which comprises a composite TPU film and a composite polytetrafluoroethylene film, wherein the composite TPU film is prepared by mixing vinyl polysiloxane and polymethyl hydrogen siloxane in a step S1, adding hexachloroplatinic acid hexahydrate as a catalyst, then adding a polyvinyl monomer to prepare an elastomer, wherein a silicon-hydrogen bond led out by the polyvinyl monomer is arranged on the elastomer, then preparing a mixed solution A by a polyethylene glycol derivative and isopropanol in a step S2, adding the elastomer into the mixed solution A, carrying out addition reaction on the silicon-hydrogen bond on the elastomer and a double bond on the derivative, further grafting polyethylene glycol molecules on the surface of the elastomer to prepare the treated elastomer, endowing the treated elastomer with hydrophilic property, solving the technical problems that the polyethylene glycol molecules lack reactive active groups and cannot be grafted on the surface of the elastomer by a chemical grafting method, and then, in step S3, the processed elastomer and the TPU are mixed and spun to prepare a composite TPU membrane, the composite membrane can be endowed with excellent moisture permeability through the hydrophilic groups on the processed elastomer, and the surface of the composite membrane has no micropores and has excellent waterproof performance.
(2) The invention prepares a composite polytetrafluoroethylene membrane, in the preparation process, step S11 mixes polytetrafluoroethylene resin and stearamide to prepare a prefabricated product, then vacuum drying is carried out to remove the stearamide, so that the polytetrafluoroethylene resin is of a hollow structure, step S12 prepares hydrophilic silica nanoparticles, then the hydrophilic silica nanoparticles are mixed with 60% of emulsion B to prepare spinning solution, electrostatic spinning is carried out to prepare a fiber membrane, and then roasting is carried out to prepare the composite polytetrafluoroethylene membrane.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A TPU waterproof moisture permeable barrier film for medical protective clothing comprises a composite TPU film and a composite polytetrafluoroethylene film;
the thickness of the composite TPU film is 2mm, the thickness of the composite polytetrafluoroethylene film is 3mm, and the composite TPU film and the composite polytetrafluoroethylene film are bonded through tw-2036 glue.
The composite TPU film is prepared by the following method:
step S1, adding vinyl polysiloxane and polymethylhydrosiloxane into a reaction kettle according to the weight ratio of 1: 3, then adding chloroplatinic acid hexahydrate and a polyvinyl monomer, stirring at a constant speed for 15min, then adding a sodium sulfate solution with the mass fraction of 10%, mixing uniformly, injecting into a mold, and curing at 65 ℃ for 10h to obtain an elastomer, wherein the weight of the chloroplatinic acid hexahydrate is controlled to be 0.5% of the weight of the vinyl polysiloxane, and the weight of the polyvinyl monomer is controlled to be 10% of the weight of the vinyl polysiloxane;
step S2, adding a polyethylene glycol derivative into isopropanol, uniformly mixing, adding a karstedt catalyst to prepare a mixed solution A, adding the elastomer prepared in the step S1 into the mixed solution A, heating in a water bath at 50 ℃ and magnetically stirring for 30min, taking out, respectively placing into acetone and deionized water for ultrasound for 2min, controlling the ultrasound power to be 50W, preparing a treated elastomer, and controlling the weight ratio of the polyethylene glycol to the isopropanol to the karstedt catalyst to the elastomer to be 1: 10: 0.1: 1;
and S3, respectively adding the processed elastomer and TPU prepared in the step S2 into dimethylformamide, heating in a water bath at 50 ℃ and magnetically stirring for 4 hours to prepare spinning solution, then carrying out electrostatic spinning to prepare a composite TPU membrane, and controlling the weight ratio of the elastomer, the TPU and the dimethylformamide to be 1: 3: 10.
The polyethylene glycol derivative is formed by mixing polyethylene glycol methyl ether acrylate and polyethylene glycol methyl ether methacrylate according to the weight ratio of 1: 1.
The composite polytetrafluoroethylene membrane is prepared by the following method:
step S11, uniformly mixing polytetrafluoroethylene resin and stearic acid amide according to the weight ratio of 5: 1, transferring the mixture into a vacuum drying oven at 45 ℃ for drying, controlling the vacuum degree of the vacuum drying oven to be-0.10 MPa, drying for 8 hours, extruding and pressing to obtain a prefabricated product, placing the prefabricated product into the vacuum drying oven at 50 ℃ for drying for 10 hours to obtain a material, adding the material into deionized water, and magnetically stirring for 20 minutes to obtain an emulsion B with the mass fraction of 60%;
step S12, dripping 10% of dilute hydrochloric acid by mass into 15% of ethanol aqueous solution by volume fraction, magnetically stirring at a rotating speed of 120r/min for 5min, then dripping KH550, controlling the dripping time to be 10min, uniformly stirring for 3min after the dripping is finished, adding tetraethoxysilane while stirring, continuously stirring at a uniform speed for 4h to prepare suspension, filtering and washing to prepare hydrophilic silica nanoparticles, wherein the weight ratio of the 10% of dilute hydrochloric acid to the 15% of ethanol aqueous solution to the KH550 to the tetraethoxysilane is controlled to be 2: 10: 0.1: 0.5;
step S13, adding hydrophilic silicon dioxide nano particles into 60% emulsion B, adding 3% boric acid solution, mixing uniformly to obtain spinning solution, carrying out electrostatic spinning to obtain a nascent fiber membrane, transferring the nascent fiber membrane into a muffle furnace, heating to 350 ℃ at a heating rate of 3 ℃/min, and roasting for 2h to obtain the composite polytetrafluoroethylene membrane, wherein the weight ratio of the hydrophilic silicon dioxide nano particles to the 60% emulsion B to the 3% boric acid solution is 1: 15-20: 3-5.
Example 2
A TPU waterproof moisture permeable barrier film for medical protective clothing comprises a composite TPU film and a composite polytetrafluoroethylene film;
the thickness of the composite TPU film is 2mm, the thickness of the composite polytetrafluoroethylene film is 3mm, and the composite TPU film and the composite polytetrafluoroethylene film are bonded through tw-2036 glue.
The composite TPU film is prepared by the following method:
step S1, adding vinyl polysiloxane and polymethylhydrosiloxane into a reaction kettle according to the weight ratio of 1: 3, then adding chloroplatinic acid hexahydrate and a polyvinyl monomer, stirring at a constant speed for 15min, then adding a sodium sulfate solution with the mass fraction of 10%, mixing uniformly, injecting into a mold, and curing at 65 ℃ for 10h to obtain an elastomer, wherein the weight of the chloroplatinic acid hexahydrate is controlled to be 0.6% of the weight of the vinyl polysiloxane, and the weight of the polyvinyl monomer is controlled to be 10% of the weight of the vinyl polysiloxane;
step S2, adding a polyethylene glycol derivative into isopropanol, uniformly mixing, adding a karstedt catalyst to prepare a mixed solution A, adding the elastomer prepared in the step S1 into the mixed solution A, heating in a water bath at 50 ℃ and magnetically stirring for 30min, taking out, respectively placing into acetone and deionized water for ultrasound for 2min, controlling the ultrasound power to be 50W, preparing a treated elastomer, and controlling the weight ratio of the polyethylene glycol to the isopropanol to the karstedt catalyst to the elastomer to be 1: 10: 0.1: 1;
and S3, respectively adding the processed elastomer and TPU prepared in the step S2 into dimethylformamide, heating in a water bath at 50 ℃ and magnetically stirring for 4 hours to prepare spinning solution, then carrying out electrostatic spinning to prepare a composite TPU membrane, and controlling the weight ratio of the elastomer, the TPU and the dimethylformamide to be 1: 3: 14.
The polyethylene glycol derivative is formed by mixing polyethylene glycol methyl ether acrylate and polyethylene glycol methyl ether methacrylate according to the weight ratio of 1: 1.
The composite polytetrafluoroethylene membrane is prepared by the following method:
step S11, uniformly mixing polytetrafluoroethylene resin and stearic acid amide according to the weight ratio of 5: 1, transferring the mixture into a vacuum drying oven at 45 ℃ for drying, controlling the vacuum degree of the vacuum drying oven to be-0.10 MPa, drying for 8 hours, extruding and pressing to obtain a prefabricated product, placing the prefabricated product into the vacuum drying oven at 50 ℃ for drying for 10 hours to obtain a material, adding the material into deionized water, and magnetically stirring for 20 minutes to obtain an emulsion B with the mass fraction of 60%;
step S12, dripping 10% of dilute hydrochloric acid by mass into 15% of ethanol aqueous solution by volume fraction, magnetically stirring at a rotating speed of 120r/min for 5min, then dripping KH550, controlling the dripping time to be 10min, uniformly stirring for 3min after the dripping is finished, adding tetraethoxysilane while stirring, continuously stirring at a uniform speed for 4h to prepare suspension, filtering and washing to prepare hydrophilic silica nanoparticles, wherein the weight ratio of the 10% of dilute hydrochloric acid to the 15% of ethanol aqueous solution to the KH550 to the tetraethoxysilane is controlled to be 2: 10: 0.1: 0.5;
step S13, adding hydrophilic silicon dioxide nano particles into 60% emulsion B, adding 3% boric acid solution, mixing uniformly to obtain spinning solution, carrying out electrostatic spinning to obtain a nascent fiber membrane, transferring the nascent fiber membrane into a muffle furnace, heating to 350 ℃ at a heating rate of 3 ℃/min, and roasting for 2h to obtain the composite polytetrafluoroethylene membrane, wherein the weight ratio of the hydrophilic silicon dioxide nano particles to the 60% emulsion B to the 3% boric acid solution is 1: 18: 5.
Example 3
A TPU waterproof moisture permeable barrier film for medical protective clothing comprises a composite TPU film and a composite polytetrafluoroethylene film;
the thickness of the composite TPU film is 2mm, the thickness of the composite polytetrafluoroethylene film is 3mm, and the composite TPU film and the composite polytetrafluoroethylene film are bonded through tw-2036 glue.
The composite TPU film is prepared by the following method:
step S1, adding vinyl polysiloxane and polymethylhydrosiloxane into a reaction kettle according to the weight ratio of 1: 3, then adding chloroplatinic acid hexahydrate and a polyvinyl monomer, stirring at a constant speed for 15min, then adding a sodium sulfate solution with the mass fraction of 10%, mixing uniformly, injecting into a mold, and curing at 65 ℃ for 10h to obtain an elastomer, wherein the weight of the chloroplatinic acid hexahydrate is controlled to be 0.7% of the weight of the vinyl polysiloxane, and the weight of the polyvinyl monomer is controlled to be 10% of the weight of the vinyl polysiloxane;
step S2, adding a polyethylene glycol derivative into isopropanol, uniformly mixing, adding a karstedt catalyst to prepare a mixed solution A, adding the elastomer prepared in the step S1 into the mixed solution A, heating in a water bath at 50 ℃ and magnetically stirring for 30min, taking out, respectively placing into acetone and deionized water for ultrasound for 2min, controlling the ultrasound power to be 50W, preparing a treated elastomer, and controlling the weight ratio of the polyethylene glycol to the isopropanol to the karstedt catalyst to the elastomer to be 1: 10: 0.2: 1;
and S3, respectively adding the processed elastomer and TPU prepared in the step S2 into dimethylformamide, heating in a water bath at 50 ℃ and magnetically stirring for 4 hours to prepare spinning solution, then carrying out electrostatic spinning to prepare a composite TPU membrane, and controlling the weight ratio of the elastomer, the TPU and the dimethylformamide to be 1: 3: 18.
The polyethylene glycol derivative is formed by mixing polyethylene glycol methyl ether acrylate and polyethylene glycol methyl ether methacrylate according to the weight ratio of 1: 1.
The composite polytetrafluoroethylene membrane is prepared by the following method:
step S11, uniformly mixing polytetrafluoroethylene resin and stearic acid amide according to the weight ratio of 5: 1, transferring the mixture into a vacuum drying oven at 45 ℃ for drying, controlling the vacuum degree of the vacuum drying oven to be-0.10 MPa, drying for 8 hours, extruding and pressing to obtain a prefabricated product, placing the prefabricated product into the vacuum drying oven at 50 ℃ for drying for 10 hours to obtain a material, adding the material into deionized water, and magnetically stirring for 20 minutes to obtain an emulsion B with the mass fraction of 60%;
step S12, dripping 10% of dilute hydrochloric acid by mass into 15% of ethanol aqueous solution by volume fraction, magnetically stirring at a rotating speed of 120r/min for 5min, then dripping KH550, controlling the dripping time to be 10min, uniformly stirring for 3min after the dripping is finished, adding tetraethoxysilane while stirring, continuously stirring for 4h at a uniform speed to prepare suspension, filtering and washing to prepare hydrophilic silicon dioxide nano particles, wherein the weight ratio of the 10% of dilute hydrochloric acid to the 15% of ethanol aqueous solution to the KH550 to the tetraethoxysilane is controlled to be 2: 10: 0.2: 0.5;
step S13, adding hydrophilic silicon dioxide nano particles into 60% emulsion B, adding 3% boric acid solution, mixing uniformly to obtain spinning solution, carrying out electrostatic spinning to obtain a nascent fiber membrane, transferring the nascent fiber membrane into a muffle furnace, heating to 350 ℃ at a heating rate of 5 ℃/min, and roasting for 2h to obtain the composite polytetrafluoroethylene membrane, wherein the weight ratio of the hydrophilic silicon dioxide nano particles to the 60% emulsion B to the 3% boric acid solution is 1: 18: 4.
Example 4
A TPU waterproof moisture permeable barrier film for medical protective clothing comprises a composite TPU film and a composite polytetrafluoroethylene film;
the thickness of the composite TPU film is 2mm, the thickness of the composite polytetrafluoroethylene film is 3mm, and the composite TPU film and the composite polytetrafluoroethylene film are bonded through tw-2036 glue.
The composite TPU film is prepared by the following method:
step S1, adding vinyl polysiloxane and polymethylhydrosiloxane into a reaction kettle according to the weight ratio of 1: 3, then adding chloroplatinic acid hexahydrate and a polyvinyl monomer, stirring at a constant speed for 15min, then adding a sodium sulfate solution with the mass fraction of 10%, mixing uniformly, injecting into a mold, and curing at 65 ℃ for 10h to obtain an elastomer, wherein the weight of the chloroplatinic acid hexahydrate is controlled to be 0.8% of the weight of the vinyl polysiloxane, and the weight of the polyvinyl monomer is controlled to be 10% of the weight of the vinyl polysiloxane;
step S2, adding a polyethylene glycol derivative into isopropanol, uniformly mixing, adding a karstedt catalyst to prepare a mixed solution A, adding the elastomer prepared in the step S1 into the mixed solution A, heating in a water bath at 50 ℃ and magnetically stirring for 30min, taking out, respectively placing into acetone and deionized water for ultrasound for 2min, controlling the ultrasound power to be 50W, preparing a treated elastomer, and controlling the weight ratio of the polyethylene glycol to the isopropanol to the karstedt catalyst to the elastomer to be 1: 10: 0.2: 1;
and S3, respectively adding the processed elastomer and TPU prepared in the step S2 into dimethylformamide, heating in a water bath at 50 ℃ and magnetically stirring for 4 hours to prepare spinning solution, then carrying out electrostatic spinning to prepare a composite TPU membrane, and controlling the weight ratio of the elastomer, the TPU and the dimethylformamide to be 1: 3: 20.
The polyethylene glycol derivative is formed by mixing polyethylene glycol methyl ether acrylate and polyethylene glycol methyl ether methacrylate according to the weight ratio of 1: 1.
The composite polytetrafluoroethylene membrane is prepared by the following method:
step S11, uniformly mixing polytetrafluoroethylene resin and stearic acid amide according to the weight ratio of 5: 1, transferring the mixture into a vacuum drying oven at 45 ℃ for drying, controlling the vacuum degree of the vacuum drying oven to be-0.10 MPa, drying for 8 hours, extruding and pressing to obtain a prefabricated product, placing the prefabricated product into the vacuum drying oven at 50 ℃ for drying for 10 hours to obtain a material, adding the material into deionized water, and magnetically stirring for 20 minutes to obtain an emulsion B with the mass fraction of 60%;
step S12, dripping 10% of dilute hydrochloric acid by mass into 15% of ethanol aqueous solution by volume fraction, magnetically stirring at a rotating speed of 120r/min for 5min, then dripping KH550, controlling the dripping time to be 10min, uniformly stirring for 3min after the dripping is finished, adding tetraethoxysilane while stirring, continuously stirring for 4h at a uniform speed to prepare suspension, filtering and washing to prepare hydrophilic silicon dioxide nano particles, wherein the weight ratio of the 10% of dilute hydrochloric acid to the 15% of ethanol aqueous solution to the KH550 to the tetraethoxysilane is controlled to be 2: 10: 0.2: 0.5;
step S13, adding hydrophilic silicon dioxide nano particles into 60% emulsion B, adding 3% boric acid solution, mixing uniformly to obtain spinning solution, carrying out electrostatic spinning to obtain a nascent fiber membrane, transferring the nascent fiber membrane into a muffle furnace, heating to 350 ℃ at a heating rate of 3 ℃/min, and roasting for 2h to obtain the composite polytetrafluoroethylene membrane, wherein the weight ratio of the hydrophilic silicon dioxide nano particles to the 60% emulsion B to the 3% boric acid solution is 1: 20: 5.
Comparative example 1
This comparative example compares to example 1 with a TPU film replacing the composite TPU film.
Comparative example 2
This comparative example compares to example 1 with a polytetrafluoroethylene membrane instead of a composite polytetrafluoroethylene membrane.
Comparative example 3
The comparative example is a TPU waterproof moisture permeable barrier film in the market.
The moisture permeability, elongation and tear strength of examples 1 to 4 and comparative examples 1 to 3 were measured, and the results are shown in the following table;
from the above table, it can be seen that the moisture permeability of examples 1-4 is 186556-; the invention solves the technical problem that polyethylene glycol molecules lack reactive active groups and cannot be grafted on the surface of an elastomer by a chemical grafting method, then the treated elastomer and TPU are mixed and spun in step S3 to prepare a composite TPU membrane, the composite membrane can be endowed with excellent moisture permeability by hydrophilic groups on the treated elastomer, and the composite membrane has no micropores on the surface and has excellent waterproof performance.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (5)
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