WO2015099282A1 - Tissu non tissé composite et son procédé de préparation - Google Patents

Tissu non tissé composite et son procédé de préparation Download PDF

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WO2015099282A1
WO2015099282A1 PCT/KR2014/010397 KR2014010397W WO2015099282A1 WO 2015099282 A1 WO2015099282 A1 WO 2015099282A1 KR 2014010397 W KR2014010397 W KR 2014010397W WO 2015099282 A1 WO2015099282 A1 WO 2015099282A1
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Prior art keywords
nonwoven fabric
carboxymethyl cellulose
composite nonwoven
composite
substrate
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PCT/KR2014/010397
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English (en)
Korean (ko)
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임정남
김태희
도성준
김윤진
김채화
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한국생산기술연구원
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Publication of WO2015099282A1 publication Critical patent/WO2015099282A1/fr

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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326—Condensation or reaction polymers
    • D04H1/435—Polyesters
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
    • D04H1/587—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives characterised by the bonding agents used
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
    • D06M15/05—Cellulose or derivatives thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
    • D06M15/05—Cellulose or derivatives thereof
    • D06M15/09—Cellulose ethers
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D01D5/0038—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion the fibre formed by solvent evaporation, i.e. dry electro-spinning
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • D01F6/625—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters derived from hydroxy-carboxylic acids, e.g. lactones
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
    • D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters

Definitions

  • the present invention relates to a composite nonwoven fabric and a method for producing the same, and more particularly, to a composite nonwoven fabric having a good liquid absorption and a high transparency at the time of absorption, and directly coated on the wound surface to serve as a temporary artificial skin and a method for producing the same. .
  • Skin not only protects the human body from various harmful environments such as microorganisms, ultraviolet rays, and chemicals, but also inhibits water evaporation, thereby preventing dehydration and regulating body temperature. to be.
  • the skin of the human body has a property to protect the wound and to naturally heal when wounds, burns, etc.
  • the wound covering material is used as a method to effectively protect the wound and to speed up the healing.
  • the characteristics of wound coating should be excellent in biocompatibility, so that there is no rejection reaction to the wounded area, enough to absorb the body fluid discharged from the wounded area, and high moisture permeability to prevent the invasion of normal skin around the wound. It must be breathable to maintain.
  • the wound site was covered with the wound covering material, so that the wound healing process was not seen, the healing process could not be checked, and the wound infection or the need for replacement of the bandage could not be checked, so the wound covering material had to be removed. In this case, even if the wound is not sufficiently healed, the wound covering material is removed, which may cause serious problems such as damage to the skin and disruption of the healing process.
  • the problem to be solved by the present invention is to provide a composite non-woven fabric having excellent liquid absorption and high transparency at the time of liquid absorption, is directly coated on the wound surface to serve as a temporary artificial skin.
  • Another object of the present invention is to provide a method for producing the composite nonwoven fabric.
  • Another object of the present invention is to provide a sanitary article using the composite nonwoven fabric described above.
  • Nonwoven substrates composed of one or two or more fibers selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymers formed by electrospinning;
  • It comprises a carboxymethyl cellulose coating layer formed on at least one of the two sides of the nonwoven fabric substrate or the internal pores of the nonwoven substrate,
  • a composite nonwoven fabric is provided that is opaque in the non-absorbed state and becomes transparent in the absorbed state.
  • the average pore size of the composite nonwoven fabric may be 5 ⁇ m or less.
  • the average diameter of the fibers may be 100 to 4,000 nm.
  • the lactic acid content of the lactic acid-glycolic acid copolymer may be 10 to 90 molar ratio.
  • the loading amount of the carboxymethyl cellulose coating layer may be 1 to 30 parts by weight based on 100 parts by weight of the nonwoven fabric substrate.
  • Transparency after absorbing the composite nonwoven fabric in 0.9% saline for 30 seconds may be 60% or more.
  • the liquid absorption ratio of the composite nonwoven fabric may be 4 g / g or more.
  • Preparing an electrospinning solution by dissolving one or two or more mixtures selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymers in a solvent;
  • a method for producing a composite nonwoven fabric comprising coating a carboxymethyl cellulose solution on the nonwoven substrate to form a carboxymethyl cellulose coating layer.
  • the carboxymethyl cellulose solution may be prepared by dissolving carboxymethyl cellulose in a mixed solvent of water and a non-solvent having a surface tension lower than that of the carboxymethyl cellulose.
  • the content of the non-solvent in the mixed solvent may be 5 to 60% by weight.
  • the method may further include calendering the nonwoven substrate after the electrospinning to form the nonwoven substrate before or after coating the carboxymethyl cellulose solution.
  • a sanitary article using the above-described composite nonwoven fabric is provided.
  • the hygiene article may be a medical coating, an absorbent hygiene article, a food packaging material, or a mask pack.
  • FIG. 1 is a graph evaluating the hydrophilicity of the composite nonwoven fabric prepared in Example 1 and the nonwoven fabric prepared in Comparative Example 1.
  • FIG. 1 is a graph evaluating the hydrophilicity of the composite nonwoven fabric prepared in Example 1 and the nonwoven fabric prepared in Comparative Example 1.
  • Example 4 is a photograph showing the results of comparative evaluation of the transparency of the liquid absorption of Example 1 and Comparative Example 3.
  • 5 and 6 are SEM pictures of the surface of the composite nonwoven fabric prepared in Example 1 and Comparative Example 3, respectively.
  • Polylactic acid refers to the entire polymer composed of lactic acid (Lactic acid) as a monomer, and is a polymer synthesized by using L-lactic acid, which is fermented by microorganisms from renewable resources such as polymer lactic acid and starch, as a monomer.
  • L-lactic acid which is fermented by microorganisms from renewable resources such as polymer lactic acid and starch, as a monomer.
  • thermal and physical properties may vary.
  • Lactic acid-glycolic acid copolymers are copolymers having a common repeating unit derived from polylactic acid and polyglycolic acid, respectively. At this time, the polyglycolic acid has a characteristic of being absorbed and degraded in vivo by aliphatic polyester having a very simple structural unit (-O-CH 2 -CO-).
  • polylactic acid and lactic acid-glycolic acid copolymers are generally used as medical products and biomaterials as biocompatible and biodegradable thermoplastic polyesters which are recognized worldwide.
  • the polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymers are characterized as being hydrophobic or having a low degree of wettability, in whole or in part. Therefore, when polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymers are used as a medical, in particular, wound covering material, the liquid absorption characteristics of the secretion discharged from the wound area are lowered, thereby adhering to the wound area, and as temporary artificial skin. There was a limit to not functioning enough.
  • the present inventors include a nonwoven substrate made of fibers of polylactic acid, polycaprolactone or lactic acid-glycolic acid copolymer formed by electrospinning; And a carboxymethyl cellulose coating layer formed on at least one of both surfaces of the nonwoven fabric substrate or the internal pores of the nonwoven fabric substrate, which is opaque in the non-absorbed state and transparent in the absorbed state.
  • the nonwoven substrate of the composite nonwoven fabric consists of one or two or more fibers selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymers formed by electrospinning.
  • polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymers as described above, provide excellent biocompatibility, biodegradability, and the like, which are basic properties of the composite nonwoven fabric.
  • the content of lactic acid in the lactic acid-glycolic acid copolymer may be adjusted to preferably 10 to 90 molar ratio, more preferably 10 to 70 molar ratio.
  • the content of lactic acid it is easy to prepare a solution for electrospinning, and the biodegradation property is improved, and biodegradation may occur well over time even if it remains on the wound surface.
  • the nonwoven substrate is formed of the fiber by electrospinning, which can thin the substrate while fully exhibiting the properties of biodegradable, biocompatible polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer, This is because the pore size of the substrate can be easily adjusted, has high flexibility, and improves the coating property on the skin.
  • the fibers of the lactic acid, polycaprolactone and lactic acid-glycolic acid copolymers forming the nonwoven substrate have an average diameter of 100 to 4,000 nm, more preferably 500 to 3,000 nm. When the diameter of the fiber satisfies this range, the pore size of the substrate can be controlled sufficiently small without increasing the thickness of the nonwoven substrate, and the flexibility of the nonwoven fabric can be improved.
  • the composite nonwoven fabric according to the present invention includes a carboxymethyl cellulose coating layer on at least one of both sides of the nonwoven fabric substrate or internal pores of the nonwoven substrate.
  • the carboxymethyl cellulose coating layer improves hydrophilicity, liquid absorption, and the like by improving the disadvantages of the hydrophobic property of the nonwoven substrate made of one or two or more fibers selected from the group consisting of polylactic acid, polycaprolactone, and lactic acid-glycolic acid copolymers. And maintain a moist environment at the wound site. Also,
  • the loading amount of the carboxymethyl cellulose coating layer may be 1 to 30 parts by weight based on 100 parts by weight of the nonwoven fabric substrate.
  • the loading amount of the carboxymethyl cellulose coating layer satisfies this range, pore control is easily improved to improve the absorption characteristics of the final composite nonwoven fabric and to prevent bacterial invasion from external infectious agents.
  • the carboxymethyl cellulose coating layer may be coated on at least one surface of the nonwoven fabric substrate, or in accordance with the pore size control of the nonwoven substrate, carboxymethyl cellulose may be incorporated into the space inside the pores to form a coating layer.
  • carboxymethyl cellulose coating layer may be coated on at least one surface of the nonwoven fabric substrate, or in accordance with the pore size control of the nonwoven substrate, carboxymethyl cellulose may be incorporated into the space inside the pores to form a coating layer.
  • the greater the degree of penetration of the carboxymethyl cellulose coating layer into the voids inside the pores of the nonwoven fabric substrate the better the liquid absorption characteristics as well as the surface of the nonwoven fabric substrate, thereby increasing the overall liquid absorption ratio of the nonwoven substrate.
  • the composite nonwoven fabric of the present invention is applied to the wound site, the absorption property to secretion such as body fluids is excellently improved, which may result in better wound healing.
  • the average pore size of the composite nonwoven fabric may be 5 ⁇ m or less, preferably 0.2 to 5 ⁇ m, more preferably 0.5 to 2 ⁇ m.
  • the average pore size of this composite nonwoven fabric may be affected by the average size of the original nonwoven substrate and the loading amount and coating aspect of the carboxymethyl cellulose coating layer to be coated.
  • the average pore size of the composite nonwoven fabric can be controlled according to the conditions of the calendering process, that is, the temperature and the pressure.
  • the composite nonwoven fabric has a carboxymethyl cellulose coating layer on a nonwoven substrate made of one or two or more fibers selected from the group consisting of hydrophobic polylactic acid, polycaprolactone, and lactic acid-glycolic acid copolymers, thereby improving hydrophilicity, particularly absorption characteristics. It is characterized by being improved. Absorption characteristics of such a composite nonwoven fabric can be evaluated through the weight change before and after the absorption in the sample of a predetermined weight, as follows.
  • Absorption magnification (g / g) [(weight of sample after absorption)-(weight of sample before absorption)] / (weight of sample before absorption)
  • the liquid absorption ratio of such a composite nonwoven fabric may be 4 g / g or more, preferably 4 to 30 g / g, more preferably 6 to 20 g / g.
  • the absorption ratio of the composite nonwoven fabric satisfies this range, the wound site is placed in an appropriate wet environment when coated on the wound site, and the body adhesiveness discharged from the wound site is absorbed to improve skin adhesion of the nonwoven fabric.
  • the composite nonwoven fabric according to the present invention has the property of being opaque in the non-absorbed state and transparent in the absorbed state. This property is due to the fact that the skin adhesion of the nonwoven fabric is improved and the scattering of light is reduced with absorption.
  • the normal nonwoven fabric has a problem of removing the wound covering made of the nonwoven fabric to observe the skin condition in order to observe the wound site. In this case, the wound site is not completely treated. Removing the wound covering can cause extreme pain for the patient.
  • the transparency after absorbing the composite nonwoven fabric in 0.9% saline for 30 seconds may be 60% or more, preferably 60 to 95%, more preferably 75 to 90%.
  • Transparency was compared using the Gretag Macbeth colorimeter (CE 3100) using the reflectance measurement method in the visible wavelength range of 400 ⁇ 700nm under the D65 standard light source by the following equation.
  • the transparency of the composite nonwoven fabric satisfies this range, when the body fluid or saline solution is absorbed into the composite nonwoven fabric, the wound site may be easily observed even when the composite nonwoven fabric is attached.
  • the composite nonwoven fabric when the composite nonwoven fabric is opaque in the non-absorbed state, it means that the transparency is less than 60% by the transparency measurement method.
  • the composite nonwoven fabric of the present invention may have a thickness of 50 to 500 ⁇ m, more preferably 100 to 300 ⁇ m. When satisfying the thickness range of the composite nonwoven fabric, it is advantageous to improve the transparency and flexibility of the nonwoven fabric.
  • a method for preparing a composite nonwoven fabric includes preparing a electrospinning solution by dissolving one or two or more mixtures selected from the group consisting of polylactic acid, polycaprolactone, and lactic acid-glycolic acid copolymers in a solvent. step; Electrospinning the spinning solution to form a nonwoven substrate; And coating a carboxymethyl cellulose solution on the nonwoven substrate to form a carboxymethyl cellulose coating layer.
  • Electrospinning is used to produce the nonwoven substrate of the present invention.
  • one or two or more mixtures selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymers must be dissolved in a solvent to prepare an electrospinning solution.
  • the solvent used may uniformly dissolve one or two or more mixtures selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymers, and radioactive. Any of these high solvents can be used without limitation, examples being trifluoroacetic acid, dimethylformamide, dimethylsulfoxide, chloroform, trifluoroethylene, acetone, hexafluoroisopropanol, methylene chloride, tetrahydrofuran, acetic acid and formic acid Etc. may be used, and they may be used as one or two or more mixed solvents.
  • the content of one or two or more mixtures selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer added in the electrospinning solution is 5 to 20% by weight in the total electrospinning solution, more preferably. Preferably from 8 to 15% by weight.
  • the weight percentage is adjusted in this way, it is possible to obtain an electrospinning solution which is uniformly dissolved and has an appropriate viscosity and is easy to handle. As a result, spinning properties may be improved, and the diameter distribution of the manufactured fiber may be uniform.
  • one or two or more mixtures selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymers are used as co-solvents of dimethyl formamide and chloroform with excellent emissivity for easy removal of residual solvents. It can be completely dissolved so that there are no impurities, and stirred at room temperature for about 12 hours before being used for electrospinning.
  • the prepared electrospinning solution is electrospun to form a nonwoven substrate.
  • polymers such as polylactic acid, polycaprolactone, or lactic acid-glycolic acid copolymers do not have a constant molecular weight due to their properties, so it is important to control process conditions when producing fibers by electrospinning.
  • the basic electrospinning device used in the present invention is equipped with a syringe fitted with 21G to 24G nozzles made of stainless steel in an integrally configured positive charge high voltage generator, an integrated drum and a metered discharge pump.
  • a syringe fitted with 21G to 24G nozzles made of stainless steel in an integrally configured positive charge high voltage generator, an integrated drum and a metered discharge pump.
  • the structure and morphology are analyzed and the best reproducible electrospinning condition is obtained. Applied.
  • the electrospinning device in an embodiment of the present invention, the electrospinning solution prepared by dissolving one or two or more mixtures selected from the group consisting of polylactic acid, polycaprolactone and lactic acid-glycolic acid copolymer in a solvent
  • Any device capable of electrospinning may be applied without limitation, and examples thereof include a syringe type, a wire type, a drum type, and the like, but are not limited thereto.
  • the electrospinning is preferably carried out under the electrospinning conditions of 5 to 20% by weight of the mixed solution, voltage 5 to 100 kV, discharge rate of the solution of 0.1 to 10 ml / h and spinning distance of 3 to 50 cm. .
  • the carboxymethyl cellulose solution is coated on the obtained nonwoven fabric substrate to form a carboxymethyl cellulose coating layer.
  • the carboxymethyl cellulose solution may be prepared by dissolving carboxymethyl cellulose in a mixed solvent of water and alcohol.
  • carboxymethyl cellulose is well soluble in water, whereas polylactic acid, polycaprolactone, or lactic acid-glycolic acid copolymers are hydrophobic.
  • a nonwoven substrate made of one or two or more fibers selected from the group consisting of coalescing, it is difficult to uniformly attach the aqueous solution of carboxymethyl cellulose to the nonwoven substrate.
  • the non-solvent having a lower surface tension than water and a non-solvent of carboxymethyl cellulose as a solvent is mixed, the surface tension of the resulting solution is lower than that of the aqueous solution, thereby uniformly coating the carboxymethyl cellulose solution on the nonwoven fabric substrate.
  • the content of the non-solvent in the mixed solvent is 5 to 60% by weight, more preferably 10 to 30% by weight.
  • the content of the non-solvent is less than 5%, the effect of adding the non-solvent is insignificant, and when the content of the non-solvent is greater than 60%, the non-solvent cannot dissolve the carboxymethyl cellulose. have.
  • alcohols such as methanol, ethanol, isopropyl alcohol, acetone, methylene chloride, chloroform, and the like may be used alone or as a mixture of two or more thereof.
  • the coating amount of the carboxymethyl cellulose solution may be adjusted so that the loading amount of the carboxymethyl cellulose coating layer is 1 to 30 parts by weight based on 100 parts by weight of the nonwoven substrate. have.
  • the non-woven substrate coated with the carboxymethyl cellulose solution may be hot air dried or vacuum dried at room temperature or 40 to 120 ° C. to obtain a composite nonwoven fabric.
  • the obtained composite nonwoven fabric may be further subjected to a calendering process at a temperature of 200 to 600 psi at room temperature to 100 ° C. By passing through such a calendering process, the pore size and thickness of the finally obtained composite nonwoven fabric can be adjusted.
  • the composite nonwoven fabric of the present invention may be usefully used in various medical coatings, absorbent hygiene products, food packaging materials, mask packs, and the like, and may have particularly suitable properties as a wound coating material serving as a temporary artificial skin during burn treatment.
  • DMF dimethylformamide
  • a voltage of 15 kV, a spinning distance of 20 cm, and a fluid velocity of 6 ml / h were fixed using an electrospinning apparatus and spun for 5 hours on a rotating drum current collector to obtain a nonwoven substrate. Thereafter, the obtained nonwoven substrate was washed with ethanol and dried in a vacuum oven for 24 hours at room temperature to finally prepare a nonwoven substrate having an average pore size of 11.6 ⁇ m.
  • the prepared nonwoven fabric substrate was immersed in 0.4 wt% carboxymethyl cellulose solution prepared by dissolving carboxymethyl cellulose in a mixed solvent having a weight ratio of ethanol and water of 20:80 for 10 seconds, and then dried at 80 ° C. for 1 hour to average A composite nonwoven fabric having a pore size of 4.9 ⁇ m and a thickness of 159 ⁇ m was prepared. At this time, the loading amount of carboxymethyl cellulose was 21 parts by weight based on 100 parts by weight of the nonwoven fabric.
  • DMF dimethylformamide
  • a voltage of 20 kV, a spinning distance of 20 cm, and a fluid velocity of 6 ml / h were fixed and spun on a rotating drum current collector for 6 hours to obtain a nonwoven substrate.
  • the obtained nonwoven substrate was washed with ethanol and dried in a vacuum oven for 24 hours at room temperature to obtain a nonwoven substrate having an average pore size of 7 ⁇ m, which was then calendered at a pressure of 500 psi at room temperature, and the average pore size was 4.1 ⁇ m.
  • the phosphorous nonwoven substrate was finally produced.
  • the prepared nonwoven fabric substrate was immersed in 0.4 wt% carboxymethyl cellulose solution prepared by dissolving carboxymethyl cellulose in a mixed solvent having a weight ratio of ethanol and water of 20:80 for 10 seconds, and then dried at 80 ° C. for 1 hour to average A composite nonwoven fabric having a pore size of 3.1 ⁇ m and a thickness of 104 ⁇ m was prepared. At this time, the loading amount of the carboxymethyl cellulose was 14 parts by weight based on 100 parts by weight of the nonwoven fabric.
  • DMF dimethylformamide
  • a voltage of 20 kV, a spinning distance of 19 cm, and a fluid speed of 6 ml / h were fixed and spun on a rotating drum current collector for 8 hours to obtain a nonwoven substrate.
  • the obtained nonwoven substrate was washed with ethanol and dried in a vacuum oven for 24 hours at room temperature to prepare a nonwoven substrate having an average pore size of 5.4 ⁇ m.
  • the prepared nonwoven fabric substrate was immersed in 0.4 wt% carboxymethyl cellulose solution prepared by dissolving carboxymethyl cellulose in a mixed solvent having a weight ratio of ethanol and water of 20:80 for 10 seconds, and then dried at 80 ° C. for 1 hour to average A composite nonwoven fabric having a pore size of 1.9 ⁇ m and a thickness of 181 ⁇ m was prepared. At this time, the loading amount of the carboxymethyl cellulose was 20 parts by weight based on 100 parts by weight of the nonwoven fabric.
  • DMF methylformamide
  • a voltage of 20 kV, a spinning distance of 20 cm, and a fluid velocity of 5 ml / h were fixed and spun on a rotating drum current collector for 6 hours to obtain a nonwoven substrate.
  • the resulting nonwoven substrate was then prepared in a vacuum oven at 45 ° C. for 24 hours.
  • the prepared nonwoven fabric substrate was immersed in a 0.04 wt% carboxymethyl cellulose solution prepared by dissolving carboxymethyl cellulose in a mixed solvent having a weight ratio of ethanol and water of 30:70 for 10 seconds, and then dried at 40 ° C. for 30 minutes to average.
  • a composite nonwoven fabric having a pore size of 4.6 ⁇ m and a thickness of 78 ⁇ m was prepared.
  • a nonwoven substrate prepared in the same manner as in Example 1 was prepared except that the step of immersing the carboxymethyl cellulose solution was not performed.
  • a nonwoven substrate prepared in the same manner as in Example 3 was prepared except that the step of immersing the carboxymethyl cellulose solution was not performed.
  • a composite nonwoven fabric substrate was prepared in the same manner as in Example 1, except that only water was used instead of ethanol and water mixed solvent in the preparation of the carboxymethyl cellulose solution in the immersion treatment in the carboxymethyl cellulose solution.
  • the contact angle is measured based on the KS L 2110 standard using an image analyzer (Drop shape analysis system; DSA 100, KRUSS GmbH) using the image analyzer (Drop shape analysis system; DSA 100, KRUSS GmbH). It was. Using the above evaluation method, the hydrophilicity of the nonwoven fabrics prepared in Example 1 and Comparative Example 1 was evaluated, and the results are shown in FIG.
  • a sample of 3 cm 3 cm is cut out of the nonwoven fabric under standard conditions, and the weight is measured accurately.
  • the sample is immersed in 0.9% saline for 30 seconds. Thereafter, one end of the nonwoven fabric is pulled out with tweezers, and then waited until the saline solution no longer drops, the weight at the time of liquid absorption is measured, and the liquid absorption ratio is calculated by the following equation.
  • Example 2 After applying the composite nonwoven fabric prepared in Example 1 on the wound site and the substrate, the transparency was visually evaluated after the absorption of 0.9% physiological saline for 30 seconds (left picture) and after (right picture). Are shown in FIGS. 2 and 3, respectively.
  • Example 4 After the nonwoven fabrics prepared in Example 1 and Comparative Example 3 were absorbed with 0.9% physiological saline for 30 seconds, transparency was visually evaluated, and a photograph of the observed non-woven fabric was shown in FIG. 4.
  • the composite nonwoven fabrics prepared in Examples 1 and 3 and the nonwoven substrates prepared in Comparative Examples 1 and 2 were absorbed in 0.9% physiological saline for 30 seconds, and then visible light wavelength range was measured under a D65 standard light source using a Gretag Macbeth colorimeter (CE 3100). It was compared by the following formula using the reflectance measurement method at phosphorus 400 to 700nm.
  • the solvent used in the carboxymethyl cellulose solution for forming the carboxymethyl cellulose coating layer is a mixed solvent of water and ethanol
  • the carboxymethyl cellulose penetrates uniformly between the electrospun fibers while the water
  • the carboxymethyl cellulose is very nonuniformly distributed in a part of the sole solvent. This is because the nonwoven fabric made of the electrospun biodegradable polymer exhibits hydrophobicity, and when the water having a large surface tension is used as the sole solvent, the hydrophilicity is large, making it difficult to penetrate the aqueous solution of carboxymethyl cellulose.
  • the alcohol and water mixed solvent is used, the surface tension is lowered, thereby facilitating the penetration between the hydrophobic nonwoven fabrics.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials For Medical Uses (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

L'invention concerne un tissu non tissé composite et son procédé de préparation, le tissu non tissé composite comprenant : une matière de base de tissu non tissé, formée, par électrofilature, d'au moins un ou deux types de fibres choisies dans le groupe constitué par copolymères d'acide polylactique, polycaprolactone et acide lactique/acide glycolique ; et une couche de revêtement de carboxyméthylcellulose, formée sur les deux surfaces de la matière de base de tissu non tissé ou dans au moins un des pores à l'intérieur de la matière de base de tissu non tissé, la fibre de non-tissé composite devenant opaque dans un état de non-absorption de liquide et devenant transparente dans un état d'absorption de liquide.
PCT/KR2014/010397 2013-12-27 2014-10-31 Tissu non tissé composite et son procédé de préparation WO2015099282A1 (fr)

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CN115671404A (zh) * 2022-10-11 2023-02-03 中国科学院大学深圳医院(光明) 一种防粘连复合材料及其制备方法和应用

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KR101954875B1 (ko) * 2017-05-26 2019-05-30 단국대학교 산학협력단 전기자극을 이용한 마스크 팩
KR102272324B1 (ko) * 2019-12-03 2021-07-02 주식회사 피앤씨랩스 카르복실화 셀룰로오스 섬유포의 제조방법 및 이를 이용한 마스크 팩의 제조방법

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CN115671404A (zh) * 2022-10-11 2023-02-03 中国科学院大学深圳医院(光明) 一种防粘连复合材料及其制备方法和应用
CN115671404B (zh) * 2022-10-11 2023-12-26 中国科学院大学深圳医院(光明) 一种防粘连复合材料及其制备方法和应用

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