WO2021075837A1 - Non-cytotoxic hydrophilic modifying coating agent, non-cytotoxic nonwoven fabric including same, and preparation method therefor - Google Patents

Non-cytotoxic hydrophilic modifying coating agent, non-cytotoxic nonwoven fabric including same, and preparation method therefor Download PDF

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Publication number
WO2021075837A1
WO2021075837A1 PCT/KR2020/013971 KR2020013971W WO2021075837A1 WO 2021075837 A1 WO2021075837 A1 WO 2021075837A1 KR 2020013971 W KR2020013971 W KR 2020013971W WO 2021075837 A1 WO2021075837 A1 WO 2021075837A1
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Prior art keywords
coating agent
nonwoven fabric
modified coating
hydrophilic modified
hydrophilic
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PCT/KR2020/013971
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French (fr)
Korean (ko)
Inventor
김주희
서영석
김대희
Original Assignee
도레이첨단소재 주식회사
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Priority to JP2022521400A priority Critical patent/JP7342256B2/en
Priority to CN202080069232.6A priority patent/CN114502786B/en
Publication of WO2021075837A1 publication Critical patent/WO2021075837A1/en

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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-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
    • D04H1/42Non-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
    • D04H1/4282Addition polymers
    • D04H1/4291Olefin series
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H13/00Other non-woven fabrics
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/68Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
    • D06M11/71Salts of phosphoric acids
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/203Unsaturated carboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53Polyethers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0002Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
    • D06N3/0011Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using non-woven fabrics
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0002Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
    • D06N3/0015Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
    • D06N3/0038Polyolefin fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/007Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
    • D06N3/0077Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/04Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/12Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2209/00Properties of the materials
    • D06N2209/14Properties of the materials having chemical properties
    • D06N2209/141Hydrophilic
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/02Moisture-responsive characteristics
    • D10B2401/022Moisture-responsive characteristics hydrophylic
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Definitions

  • the present invention relates to a product having a hydrophobic surface with little cytotoxicity, for example, a hydrophilic modified coating agent suitable for modifying a hydrophobic nonwoven fabric to be hydrophilic, and to a nonwoven fabric manufactured using the same.
  • non-woven fabrics are used for hygiene products, for example, disposable absorbent products such as baby diapers, adult diapers for urinary incontinence, sanitary napkin for women, and panty liner.
  • disposable absorbent products such as baby diapers, adult diapers for urinary incontinence, sanitary napkin for women, and panty liner.
  • the synthetic nonwoven fabric is a nonwoven fabric made of a polyolefin material such as polyethylene and polypropylene.
  • such hygiene products are required to have hydrophilicity, and since the nonwoven fabric made of polyolefin material is hydrophobic, it is applied after imparting hydrophilicity to the nonwoven fabric.
  • a synthetic hydrophilic modified coating agent is applied to the nonwoven fabric, but when used on a surface in contact with the skin, the synthetic hydrophilic modified coating agent is not discharged and remains on the body.
  • the synthetic hydrophilic modified coating that has entered through the skin cell membrane has a risk of causing disorders in cells such as the brain, heart, liver, spleen, etc., traveling around the body through blood, and also has a problem that can cause atopic dermatitis.
  • hydrophilic modified coating agent that provides hydrophilicity to a product made of a hydrophobic material that is in direct contact with the human body, preferably a hydrophobic nonwoven fabric, and does not harm the human body.
  • the object of the present invention is to solve the problems of these nonwovens based on the background of the problems of the conventional nonwovens as described above, and its main purpose is to have an optimal composition and composition ratio with low cytotoxicity.
  • the non-toxic hydrophilic modified coating agent of the present invention includes sodium salt, maleic acid salt, phosphate and alcohol ether compounds.
  • the cell non-toxic hydrophilic modified coating agent may include 15 to 20% by weight of sodium salt, 10 to 16% by weight of maleate, 2 to 8% by weight of phosphate, and the balance of alcohol ether compounds. .
  • the sodium salt in the composition of the cell-free hydrophilic modified coating agent is octyl sodium sulfosuccinic acid (docusate sodium), sodium dodecylbenzenesulfonate, ammonium alpha-sulfo-omega-(nonylphenoxy ) Poly(oxy-1,2-ethanediyl), sulfobutanedioxane 1,4-bis(2-(C 1 to C 3 alkyl) (C 4 to C 8 alkyl) ester sodium salt, sodium taloate, It may contain at least one selected from sodium cocoate and sodium palm kernelate.
  • the maleate in the composition of the non-toxic hydrophilic modified coating agent is bis(2-(C 1 ⁇ C 3 alkyl) (C 4 ⁇ C 8 alkyl) maleate, ethylene male anhydride It may include at least one selected from an acid copolymer and an isobutylene maleic anhydride copolymer.
  • the phosphate in the composition of the non-toxic hydrophilic modified coating agent is poly(oxy-1,2-ethanediyl), polyoxyethylene nonyl phenyl ether phosphoric acid, polyoxyethylene nonyl phenyl ether phosphoric acid, phosphoric acid Tris(2-ethylhexyl)ester and (Z)-alpha-2-octadekenyl-omega-hydroxypoly(oxy-1,2-ethandyl)phosphate.
  • the alcohol ether-based compound in the composition of the cell non-toxic hydrophilic modified coating agent includes at least one selected from dipropylene glycol monomethyl ether, polyvinyl ether, polyethylene glycol, and alcohol polyoxyethylene ether. can do.
  • the cell-free hydrophilic modified coating agent may have a viscosity of 950 to 1,100 mPa.s measured according to ASTM D7042 standard test (20°C).
  • a solution obtained by dissolving the cell non-toxic hydrophilic modified coating agent in water at a concentration of 10% by weight may have a pH of 5 to 8 (when analyzed at 20°C).
  • the cell non-toxic hydrophilic modified coating agent may have a melting point of -2 to 2°C.
  • Another object of the present invention relates to a method of manufacturing a non-toxic non-woven fabric using the previously described cell non-toxic hydrophilic modified coating agent, the first step of preparing the non-woven fabric; A second step of coating part or all of the nonwoven fabric with a non-toxic hydrophilic modified coating agent; And a 3 step of thermally fixing the hydrophilic modified coating agent to the nonwoven fabric by heat treatment to modify the nonwoven fabric to be hydrophilic.
  • the nonwoven fabric may include hydrophobic fibers.
  • the hydrophobic fiber may be a polyolefin-based fiber including at least one selected from polyethylene fiber, polypropylene fiber, and propylene ethylene copolymer fiber.
  • the hydrophobic fiber may have an average diameter of 1 to 50 ⁇ m.
  • Another object of the present invention relates to a non-woven non-woven fabric containing hydrophobic fibers, as a non-woven fabric in which part or all of the non-woven fabric containing hydrophobic fibers is modified with a hydrophilic non-woven fabric, wherein the cell-free hydrophilic modified coating agent is 0.1 to 3% by weight of the total weight of the nonwoven Can include.
  • the cell viability when measuring IC 50 according to the ISO 10993-5 method, may be 70 to 100%.
  • the nonwoven fabric may be a spunbond nonwoven fabric, a melt blown nonwoven fabric, an air-laid, wet-laid, or dry-laid nonwoven fabric.
  • the hydrophilic modified coating of the present invention does not have cytotoxicity, has excellent coating properties, and has low rewetability when hydrophilic modification of a fiber material product using this, is suitable for use in modifying a hydrophobic fiber product into a hydrophilic fiber. , In particular, it is suitable for application to products that come into direct contact with the skin.
  • the non-toxic hydrophilic modified coating agent of the present invention includes sodium salt, maleate, phosphate and alcohol ether compounds.
  • the sodium salt is octyl sodium sulfosuccinic acid (docusate sodium), sodium dodecylbenzenesulfonic acid, ammonium alpha-sulfo-omega-(nonylphenoxy)poly(oxy-1,2-ethandiyl), sulfobutanedioxane sulfobutane Dioxane 1,4-bis (2-(C 1 ⁇ C 3 alkyl) (C 4 ⁇ C 8 alkyl) ester sodium salt, sodium taloate, sodium cocoate and one or two selected from sodium palm kernelate It may contain the above, preferably octyl sodium sulfosuccinic acid (docusate sodium), sodium dodecylbenzenesulfonate, ammonium alpha-sulfo-omega-(nonylphenoxy)poly(oxy-1,2-ethandiyl) And sulfobutanediox
  • the content of the sodium salt may include 15 to 20% by weight, preferably 16 to 18.5% by weight, more preferably 16.5 to 18.0% by weight of the total weight of the hydrophilic modified coating agent.
  • the sodium salt content is less than 15% by weight, there may be a problem that the pH of the modified coating agent is too low, and when it exceeds 20% by weight, the pH of the modified coating agent is rather increased, and after the nonwoven fabric is modified, rewetting is lowered Since there may be a problem, it is better to use it within the above range.
  • the maleic acid salt is bis(2-(C 1 ⁇ C 3 alkyl) (C 4 ⁇ C 8 alkyl) maleate, ethylene maleic anhydride copolymer, and isobutylene maleic anhydride copolymer. It may include one or two or more selected, preferably bis (2- (C 2 ⁇ C 3 alkyl) (C 5 ⁇ C 7 alkyl) maleate and ethylene maleic anhydride copolymer 1 selected from the type or two types, may be more preferably used a (hexyl 2- (alkyl of C 2 ⁇ C 3)) bis maleate.
  • the content of maleate may include 10 to 16% by weight, preferably 11.0 to 14.8% by weight, and more preferably 12.0 to 14.0% by weight, based on the total weight of the hydrophilic modified coating agent.
  • the maleate content is less than 10% by weight, there may be a problem that the hydrophilicity improvement effect of the modified nonwoven fabric is lowered, and if it exceeds 16% by weight, there may be a problem of increasing cytotoxicity, so it is recommended to use it within the above range. good.
  • the phosphate in the composition of the hydrophilic modified coating agent is poly(oxy-1,2-ethanediyl), polyoxyethylene nonyl phenyl ether phosphoric acid, polyoxyethylene nonyl phenyl ether phosphoric acid, phosphate tris(2-ethylhexyl) ester, ( Z)-alpha-2-octadekenyl-omega-hydroxypoly(oxy-1,2-ethandyl)phosphate and poly(oxy-1,2-ethaninyl), ⁇ -dodecyl- ⁇ -hydroxy- , Phosphate, potassium salt (Poly(oxy-1,2-ethanediyl), ⁇ -dodecyl- ⁇ -hydroxy-,phosphate, potassium salt/cas no. 58318-92-6 ⁇ may include one or two or more selected from.
  • the content of phosphate may include 2 to 8% by weight, preferably 2.5 to 7.5% by weight, and more preferably 3.0 to 6.2% by weight, based on the total weight of the hydrophilic modified coating agent.
  • the phosphate content is less than 2% by weight, there may be a problem in that the durability absorption improvement effect of the modified nonwoven fabric is insufficient, and if it exceeds 8% by weight, there may be a problem that the durability absorption is rather lowered, so use within the above range. It is good to do.
  • the alcohol ether compound in the composition of the hydrophilic modified coating agent serves as a solvent for the other compositions of the hydrophilic modified coating agent, and is selected from dipropylene glycol monomethyl ether, polyvinyl ether, polyethylene glycol and alcohol polyoxyethylene ether.
  • One or two or more may be included, preferably one or two selected from dipropylene glycol monomethyl ether, polyvinyl ether and alcohol polyoxyethylene ether, more preferably dipropylene glycol monomethyl ether And alcohol polyoxyethylene ether.
  • the content of the alcohol ether compound is used in the remaining amount excluding other compositions of 100% by weight of the total hydrophilic modified coating agent.
  • the cell non-toxic hydrophilic modified coating agent of the present invention prepared by mixing the above-described compositions may have a viscosity of 950 to 1,100 mPa.s measured according to ASTM D7042 standard test (20°C), and preferably 980 to 1,080 mPa. s, more preferably 1,000 to 1,060 mPa.s.
  • the solution dissolved in water at a concentration of 9 to 12% by weight, preferably at a concentration of 10% by weight, of the cell non-toxic hydrophilic modified coating agent of the present invention has a pH of 5 to 8, preferably pH 5.5 when analyzed at 20°C. It may be ⁇ 7.5, more preferably a pH of 5.8 ⁇ 7.0.
  • non-toxic hydrophilic modified coating agent of the present invention may have a melting point of -3 to 3°C, preferably a melting point of -2 to 2°C.
  • Hydrophobic products can be modified to be hydrophilic using the previously described cell non-toxic hydrophilic modified coating agent, and as a preferred example, description will be given of the hydrophilic modification of the nonwoven fabric as follows.
  • Step 1 of preparing a nonwoven fabric A second step of coating part or all of the nonwoven fabric with a non-toxic hydrophilic modified coating agent; And 3 step of modifying the nonwoven fabric to be hydrophilic by thermally fixing the hydrophilic modified coating agent to the nonwoven fabric by heat treatment, thereby producing a hydrophilic modified nonwoven fabric.
  • the nonwoven fabric in step 1 may include hydrophobic fibers, some hydrophilic fibers may be included, or all nonwoven fabrics may be made of hydrophobic fibers. Some or all of the nonwoven fabric may have hydrophobicity.
  • the hydrophobic fiber may be a polyolefin-based fiber including at least one selected from polyethylene fiber, polypropylene fiber, and propylene ethylene copolymer fiber.
  • the hydrophobic fiber may have an average diameter of 1 ⁇ m to 50 ⁇ m, preferably 1 ⁇ m to 30 ⁇ m.
  • the nonwoven fabric of the first step may be a spunbond nonwoven fabric, a melt blown nonwoven fabric, an air-laid, a wet-laid, or a dry-laid nonwoven fabric.
  • the cell non-toxic hydrophilic modified coating agent of step 2 is as described above.
  • the coating of the second step may be performed by a general coating method used in the art, and preferably, it may be performed through a kiss roll coating method or a spray coating method.
  • the heat treatment in the third step may be performed by applying heat of 100 to 150°C, preferably 110 to 140°C in a drum dryer. At this time, if the heat treatment temperature is less than 100°C, there may be a problem that drying of the nonwoven fabric is less, and if the heat treatment temperature exceeds 150°C, there may be a problem that the nonwoven fabric becomes hard.
  • the prepared hydrophilic modified non-woven fabric may contain a cell non-toxic hydrophilic modified coating agent in an amount of 0.1 to 3.0% by weight, preferably 0.4 to 2.8% by weight, and more preferably 0.5 to 1.5% by weight. At this time, if the content of the non-toxic hydrophilic modified coating agent is less than 0.1% by weight, the hydrophilicity modifying effect may be insufficient, and if it exceeds 3% by weight, the rewetability of the nonwoven fabric may increase and there may be a problem of moistening.
  • the cell-free non-woven fabric of step 3 may have a basis weight of 10 to 100 gsm.
  • the cell-free nonwoven fabric of the present invention may have a cell viability of 70 to 100%, preferably 85 to 100%, more preferably 90 to 100%, when IC 50 is measured according to the ISO 10993-5 method.
  • the cellular non-toxic nonwoven fabric of the present invention is 2.50 to 3.50 seconds, preferably 2.50 to 3.20 seconds, when the liquid absorption rate is measured according to WSP 70.3(08) (Standard Test Method for Nonwoven Coverstock Liquid Strike-Through Time Using Simulated Urine). I can.
  • the cellular non-toxic nonwoven fabric of the present invention was measured for durability absorption according to WSP 70.7(09) (Standard Test Method for Nonwoven-Repeated Liquid Strike-Through Time), the first durability absorption was 1.50 to 2.80 seconds, and the second time Durable absorption is 2.00 to 3.50 seconds, and the third durability absorption may be 2.30 to 3.80 seconds.
  • the non-woven fabric of the present invention has a rewetability of 2.0 to 3.5 g, preferably 2.2 to when measuring the rewetability of a liquid according to WSP 70.8 (09) (Standard Test Method for Wetback After Repeated Strike-Through Time). May be 3.3g.
  • the cell-free nonwoven fabric of the present invention may have a cell viability of 70 to 100%, preferably 85 to 100%, more preferably 90 to 100%, when IC 50 is measured according to the ISO 10993-5 method.
  • Sodium salt sulfobutanedioxane 1,4-bis(2-ethylhexyl) ester sodium salt (cas no. 577-11-7), maleate bis(2-ethylhexyl) maleate (bis(2-ethylhexyl) maleate, cas no.142-16-5), phosphate poly(oxy-1,2-etheindinyl), ⁇ -dodecyl- ⁇ -hydroxy-, phosphate, potassium salt (Poly(oxy-1,2- ethanediyl), ⁇ -dodecyl- ⁇ -hydroxy-,phosphate, potassium salt/cas no. 58318-92-6) and dipropylene glycol monomethyl ether, an alcohol ether compound, are mixed and stirred to prepare a non-toxic hydrophilic modified coating agent. I did.
  • a hydrophilic modified coating agent was prepared in the same manner as in Example 1, but a hydrophilic modified coating agent having a composition and composition ratio as shown in Table 1 was prepared, respectively.
  • Isopropyl alcohol was prepared as a hydrophilic modified coating.
  • a solution containing 20% by weight of a diester (Di-ester) and a remaining amount of a propylene glycol compound was prepared as a hydrophilic modified coating agent.
  • a siloxane-based hydrophilic modified coating agent was prepared as a hydrophilic modified coating agent.
  • CTFA Dimethylsiloxane, 3-(3-((3-cocoamidopropyl)dimethylammonio)-2-hydroxyprpoxy)propyl groupterminated acetate / CAS 134737-05-6
  • CTFA Dimethylsiloxane, 3-(3-((3-cocoamidopropyl)dimethylammonio)-2-hydroxyprpoxy)propyl groupterminated acetate / CAS 134737-05-6
  • the viscosity was measured according to the ASTM D7042 standard test (20°C), and the pH was the pH of a solution in which a hydrophilic modified coating agent was dissolved in water at a concentration of 10% by weight, and analyzed at 20°C.
  • Example 1 1,015 ⁇ 1,025 6.0 to 6.1 -1 to 1
  • Example 2 990 ⁇ 995 5.2 ⁇ 5.3 -1 to 1
  • Example 3 1,005 ⁇ 1,010 6.4 ⁇ 6.5 -1 to 1
  • Example 4 1,050 ⁇ 1,060 5.8 ⁇ 5.9 -1 to 1
  • Example 5 1,035 ⁇ 1,040 6.0 to 6.1 -1 to 1
  • Example 6 990 ⁇ 995 5.7 ⁇ 5.8 0 to 2
  • Example 7 1,080 ⁇ 1,085 6.2 ⁇ 6.3 -3 to -1
  • Comparative Example 1 980 ⁇ 985 4.5 ⁇ 4.6 -1 to 1 Comparative Example 2 1,070 ⁇ 1,075 7.4 ⁇ 7.5 -1 to 1
  • Comparative Example 3 985 ⁇ 990 6.5 ⁇ 6.7 -1 to 1
  • Comparative Example 4 1,095 ⁇ 1,100 5.7 ⁇ 5.8 -1 to 1
  • Comparative Example 5 975-980 5.7 ⁇ 5.8 3 to
  • Examples 1 to 7 showed an appropriate range of properties ranging from viscosity 990 to 1,060 mPa.s, pH 5.2 to 6.3, and melting point -3°C to 1°C.
  • sodium in the case of Comparative Example 1 in which the salt was used in an amount of less than 15% by weight, when compared with Examples 1 and 2, there was a problem that the pH was rapidly lowered and thus acidified, and in the case of Comparative Example 2 in which the sodium salt was used in excess of 20% by weight , When compared with Example 1 and Example 3, the pH showed a tendency to increase rapidly.
  • a spunbond nonwoven fabric having a basis weight of 18 gsm made of polypropylene fibers having an average diameter of 17 ⁇ m was prepared (manufacturer Toray Advanced Materials, brand name LIVSEN).
  • Example 1 the hydrophilic modified coating agent prepared in Example 1 was coated and dried with a nonwoven fabric by a kiss roll coating method.
  • heat treatment was performed in a drum dryer under a temperature condition of about 125 to 130° C. to prepare a non-woven fabric that was modified to be hydrophilic.
  • the content of the hydrophilic modified coating agent in the prepared non-toxic nonwoven fabric was about 0.7% by weight.
  • a nonwoven fabric having been modified to be hydrophilic in the same manner as in Preparation Example 1 was prepared, but each nonwoven fabric modified to be hydrophilic using each of the hydrophilic modified coating agents prepared in Examples 2 to 5 and Comparative Examples 1 to 9 instead of the hydrophilic modified coating agent of Example 1 To prepare, Preparation Examples 2 to 7 and Comparative Preparation Examples 1 to 11 were each performed as shown in Table 3 below.
  • a measurement sample was prepared by cutting the nonwoven fabric prepared in Preparation Example and Comparative Preparation Example into a size of 10 cm x 10 cm (width x length).
  • the absorption rate of the measurement sample (specifically, the liquid absorption rate of the hydrophilic nonwoven layer) was measured according to WSP 70.3 (08) (Standard Test Method for Nonwoven Coverstock Liquid Strike-Through Time Using Simulated Urine), and the result It is shown in Table 4 below.
  • WSP 70.3 8
  • Table 4 Standard Test Method for Nonwoven Coverstock Liquid Strike-Through Time Using Simulated Urine
  • a measurement sample was prepared by cutting the nonwoven fabric prepared in Preparation Example and Comparative Preparation Example into a size of 10 cm x 10 cm (width x length).
  • the durability absorption of the measurement sample (specifically, the repeated absorption of the hydrophilic nonwoven layer) was measured according to WSP 70.7 (09) (Standard Test Method for Nonwoven-Repeated Liquid Strike-Through Time), and the results are as follows. It is shown in Table 4.
  • Durable absorbency was measured three times for the same type of measurement sample, and then the durability absorbance was recorded. Specifically, after placing the measurement sample on the absorbent paper, the time to absorb a total of 15 ml of 5 ml of 0.9% by weight NaCl aqueous solution through the absorbent paper once, twice, and three times was evaluated for durable absorption, and the evaluation record is Recorded once, twice, and three times, respectively.
  • IC 50 inhibitor concentration 50, colony formation inhibition
  • ISO 10993-5 Biological evaluation of medical devices-Part 5: Tests for in-vitro cytotoxicity
  • hydrophilic modified coating agent isopropyl alcohol (Comparative Example 7), diester and propylene glycol mixture (Comparative Example 8) and CTFA (Comparative Example 9) hydrophilic
  • the hydrophilicity was excellent, but it was confirmed that there is a problem of cytotoxicity.
  • hydrophilic modified coating agent of the present invention effectively modified hydrophobicity to hydrophilicity, and it was confirmed that there was no cytotoxicity.
  • the hydrophilic modified coating agent of the present invention is expected to be able to greatly expand the application range of the industrial nonwoven fabric and/or the nonwoven fabric for hygiene products, which had limited application uses.
  • the hydrophilic modified nonwoven fabric using the hydrophilic modified coating agent of the present invention can provide a variety of skin-friendly and nonwoven fabric products requiring hydrophilicity, such as industrial nonwoven fabric and/or nonwoven fabric for hygiene products.

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Abstract

The present invention relates to a hydrophilic modifying coating agent without cytotoxicity and a textile product hydrophilically modified using same and, more particularly, to a hydrophilic modifying coating agent suitable for hydrophilically modifying a product having a hydrophobic surface, for example, a hydrophobic nonwoven fabric, and to a non-cytotoxic nonwoven fabric prepared using same.

Description

세포무독성 친수성 개질 코팅제, 이를 포함하는 세포무독성 부직포 및 이의 제조방법 Cell non-toxic hydrophilic modified coating agent, non-toxic non-woven fabric containing same, and manufacturing method thereof
본 발명은 세포독성이 거의 없으면서 소수성 표면을 지닌 제품, 일례를 들면 소수성 부직포를 친수성으로 개질시키기에 적합한 친수성 개질 코팅제, 이를 이용하여 제조한 세포무독성 부직포에 관한 것이다. The present invention relates to a product having a hydrophobic surface with little cytotoxicity, for example, a hydrophilic modified coating agent suitable for modifying a hydrophobic nonwoven fabric to be hydrophilic, and to a nonwoven fabric manufactured using the same.
종래에 공지된 폴리프로필렌 등의 폴리올레핀 소재로 제조된 부직포 등은 강한 소수성이기 때문에 이로 인하여 친수성이 요구되는 산업용 부직포 및 위생용품으로서의 적용용도가 매우 제한적이라는 문제가 있다. Since the conventionally known nonwoven fabrics made of polyolefin materials such as polypropylene have strong hydrophobicity, there is a problem that their application as industrial nonwoven fabrics and hygiene products requiring hydrophilicity is very limited.
특히, 위생용품 예를 들면, 일회용 흡수제품인 유아가 사용하는 기저귀(baby diaper), 요실금자가 사용하는 기저귀(adult diaper), 여성용 생리대(sanitary napkin), 및 팬티라이너(panty liner) 등에는 부직포가 사용되며, 상기 부직포로는 대부분 합성부직포가 적용되며, 합성부직포는 폴리에틸렌, 폴리프로필렌 등의 폴리올레핀 소재의 부직포가 적용되고 있다. 그런데, 이러한 위생용품은 친수성이 요구되는데, 폴리올레핀 소재의 부직포는 소수성이라서, 부직포에 친수성을 부여한 후 적용된다. In particular, non-woven fabrics are used for hygiene products, for example, disposable absorbent products such as baby diapers, adult diapers for urinary incontinence, sanitary napkin for women, and panty liner. As the nonwoven fabric, most synthetic nonwoven fabrics are applied, and the synthetic nonwoven fabric is a nonwoven fabric made of a polyolefin material such as polyethylene and polypropylene. However, such hygiene products are required to have hydrophilicity, and since the nonwoven fabric made of polyolefin material is hydrophobic, it is applied after imparting hydrophilicity to the nonwoven fabric.
이를 해결하기 위하여 합성 친수성 개질 코팅제를 부직포에 도포하지만, 피부에 맞닿는 면에 사용할 경우 합성 친수성 개질 코팅제가 배출되지 않고 몸에 남게 되는 문제점이 있다. 더욱이 피부 세포막을 통하여 들어온 합성 친수성 개질 코팅제는 혈액을 타고 전신을 돌며 뇌, 심장, 간장, 비장 등의 세포에 장애를 일으킬 위험이 있고, 또한 아토피 피부염을 야기시킬 수 있는 문제점이 있다.In order to solve this problem, a synthetic hydrophilic modified coating agent is applied to the nonwoven fabric, but when used on a surface in contact with the skin, the synthetic hydrophilic modified coating agent is not discharged and remains on the body. Moreover, the synthetic hydrophilic modified coating that has entered through the skin cell membrane has a risk of causing disorders in cells such as the brain, heart, liver, spleen, etc., traveling around the body through blood, and also has a problem that can cause atopic dermatitis.
따라서, 인체와 직접 접촉되는 소수성 소재의 제품, 바람직하게는 소수성 부직포에 친수성을 부여하면서 인체에 해가 없는 친수성 개질 코팅제 개발이 필요한 실정이다.Accordingly, there is a need to develop a hydrophilic modified coating agent that provides hydrophilicity to a product made of a hydrophobic material that is in direct contact with the human body, preferably a hydrophobic nonwoven fabric, and does not harm the human body.
본 발명의 목적은 상기와 같은 종래 부직포의 제반 문제점에 대한 배경을 기초로 하여 이들 부직포에 대한 문제점을 해결하기 위한 것을 그 주요 목적으로 하는 것으로, 자세하게는 세포 독성이 적은 최적의 조성 및 조성비를 가지는 친수성 개질 코팅제를 제조하고, 이를 이용하여 소수성 부직포에 친수성을 부여한 세포 무독성 부직포를 제공하고자 한다. The object of the present invention is to solve the problems of these nonwovens based on the background of the problems of the conventional nonwovens as described above, and its main purpose is to have an optimal composition and composition ratio with low cytotoxicity. To prepare a hydrophilic modified coating agent, and use it, to provide a non-toxic cell nonwoven fabric imparting hydrophilicity to the hydrophobic nonwoven fabric.
상술한 과제를 해결하기 위하여 본 발명의 세포무독성 친수성 개질 코팅제는 소듐염, 말레산염, 인산염 및 알코올 에테르계 화합물을 포함한다.In order to solve the above problems, the non-toxic hydrophilic modified coating agent of the present invention includes sodium salt, maleic acid salt, phosphate and alcohol ether compounds.
본 발명의 바람직한 일실시예로서, 상기 세포무독성 친수성 개질 코팅제는 소듐염 15 ~ 20 중량%, 말레산염 10 ~ 16 중량%, 인산염 2 ~ 8 중량% 및 잔량의 알코올 에테르계 화합물을 포함할 수 있다.As a preferred embodiment of the present invention, the cell non-toxic hydrophilic modified coating agent may include 15 to 20% by weight of sodium salt, 10 to 16% by weight of maleate, 2 to 8% by weight of phosphate, and the balance of alcohol ether compounds. .
본 발명의 바람직한 일실시예로서, 상기 세포무독성 친수성 개질 코팅제의 조성 중 상기 소듐염은 옥틸 나트륨 설포숙신산(도큐세이트 소듐), 도데실벤젠설폰산 나트륨, 암모늄 알파-설포-오메가-(노닐페녹시)폴리(옥시-1,2-에탄디일), 설포부탄다이옥산 1,4-비스(2-(C1 ~ C3의 알킬)(C4 ~ C8의 알킬)에스터 나트륨염, 소듐탈로에이트, 소듐코코에이트 및 소듐팜커넬레이트 중에서 선택된 1종 이상을 포함할 수 있다.As a preferred embodiment of the present invention, the sodium salt in the composition of the cell-free hydrophilic modified coating agent is octyl sodium sulfosuccinic acid (docusate sodium), sodium dodecylbenzenesulfonate, ammonium alpha-sulfo-omega-(nonylphenoxy ) Poly(oxy-1,2-ethanediyl), sulfobutanedioxane 1,4-bis(2-(C 1 to C 3 alkyl) (C 4 to C 8 alkyl) ester sodium salt, sodium taloate, It may contain at least one selected from sodium cocoate and sodium palm kernelate.
본 발명의 바람직한 일실시예로서, 상기 세포무독성 친수성 개질 코팅제의 조성 중 상기 말레산염은 비스(2-(C1 ~ C3의 알킬)(C4 ~ C8의 알킬)말레이트, 에틸렌 무수 말레산 공중합체 및 이소부틸렌 무수 말레산 공중합체 중에서 선택된 1종 이상을 포함할 수 있다.As a preferred embodiment of the present invention, the maleate in the composition of the non-toxic hydrophilic modified coating agent is bis(2-(C 1 ~ C 3 alkyl) (C 4 ~ C 8 alkyl) maleate, ethylene male anhydride It may include at least one selected from an acid copolymer and an isobutylene maleic anhydride copolymer.
본 발명의 바람직한 일실시예로서, 상기 세포무독성 친수성 개질 코팅제의 조성 중 상기 인산염은 폴리(옥시-1,2-에탄디일), 폴리옥시에틸렌 노닐 페닐 에테르 인산, 폴리옥시에틸렌 노닐 페닐 에테르 인산, 인산 트리스(2-에틸헥실)에스터 및 (Z)-알파-2-옥타데켄일-오메가-하이드록시폴리(옥시-1,2-에탄딜)인산염 중에서 선택된 1종 이상을 포함할 수 있다.As a preferred embodiment of the present invention, the phosphate in the composition of the non-toxic hydrophilic modified coating agent is poly(oxy-1,2-ethanediyl), polyoxyethylene nonyl phenyl ether phosphoric acid, polyoxyethylene nonyl phenyl ether phosphoric acid, phosphoric acid Tris(2-ethylhexyl)ester and (Z)-alpha-2-octadekenyl-omega-hydroxypoly(oxy-1,2-ethandyl)phosphate.
본 발명의 바람직한 일실시예로서, 상기 세포무독성 친수성 개질 코팅제의 조성 중 상기 알콜 에테르계 화합물은 디프로필렌 글리콜 모노메틸 에테르, 폴리비닐 에테르,폴리에틸렌 글리콜 및 알콜 폴리 옥시 에틸렌 에테르 중에서 선택된 1종 이상을 포함할 수 있다.As a preferred embodiment of the present invention, the alcohol ether-based compound in the composition of the cell non-toxic hydrophilic modified coating agent includes at least one selected from dipropylene glycol monomethyl ether, polyvinyl ether, polyethylene glycol, and alcohol polyoxyethylene ether. can do.
본 발명의 바람직한 일실시예로서, 상기 세포무독성 친수성 개질 코팅제는 ASTM D7042 표준 시험(20℃)에 의거하여 측정한 점도가 950 ~ 1,100 mPa.s일 수 있다.As a preferred embodiment of the present invention, the cell-free hydrophilic modified coating agent may have a viscosity of 950 to 1,100 mPa.s measured according to ASTM D7042 standard test (20°C).
본 발명의 바람직한 일실시예로서, 상기 세포무독성 친수성 개질 코팅제를 물에 10 중량% 농도로 용해시킨 용액은 pH가 5 ~ 8(20℃ 분석시)일 수 있다.As a preferred embodiment of the present invention, a solution obtained by dissolving the cell non-toxic hydrophilic modified coating agent in water at a concentration of 10% by weight may have a pH of 5 to 8 (when analyzed at 20°C).
본 발명의 바람직한 일실시예로서, 상기 세포무독성 친수성 개질 코팅제는 융점이 -2 ~ 2℃일 수 있다.As a preferred embodiment of the present invention, the cell non-toxic hydrophilic modified coating agent may have a melting point of -2 to 2°C.
본 발명의 다른 목적은 앞서 설명한 세포무독성 친수성 개질 코팅제를 이용하여 세포무독성 부직포를 제조하는 방법에 관한 것으로서, 부직포를 준비하는 1단계; 세포무독성 친수성 개질 코팅제를 상기 부직포의 일부 또는 전체를 코팅하는 2단계; 및 열처리하여 친수성 개질 코팅제를 부직포에 열적 고정시켜서 부직포를 친수성으로 개질시키는 3단계;를 포함하는 공정을 수행하여 제조할 수 있다.Another object of the present invention relates to a method of manufacturing a non-toxic non-woven fabric using the previously described cell non-toxic hydrophilic modified coating agent, the first step of preparing the non-woven fabric; A second step of coating part or all of the nonwoven fabric with a non-toxic hydrophilic modified coating agent; And a 3 step of thermally fixing the hydrophilic modified coating agent to the nonwoven fabric by heat treatment to modify the nonwoven fabric to be hydrophilic.
본 발명의 바람직한 일실시예로서, 상기 부직포는 소수성 섬유를 포함할 수 있다.As a preferred embodiment of the present invention, the nonwoven fabric may include hydrophobic fibers.
본 발명의 바람직한 일실시예로서, 상기 소수성 섬유는 폴리에틸렌 섬유, 폴리프로필렌 섬유 및 프로필렌 에틸렌 공중합 섬유 중에서 선택된 1종 이상을 포함하는 폴리올레핀계 섬유일 수 있다.As a preferred embodiment of the present invention, the hydrophobic fiber may be a polyolefin-based fiber including at least one selected from polyethylene fiber, polypropylene fiber, and propylene ethylene copolymer fiber.
본 발명의 바람직한 일실시예로서, 상기 소수성 섬유는 평균직경이 1 ~ 50μm일 수 있다.As a preferred embodiment of the present invention, the hydrophobic fiber may have an average diameter of 1 to 50 μm.
본 발명의 또 다른 목적은 세포무독성 부직포에 관한 것으로서, 소수성 섬유를 포함하는 부직포의 일부 또는 전부가 친수성 부직포로 개질된 부직포로서, 부직포 전체 중량 중 상기 세포무독성 친수성 개질 코팅제를 0.1 ~ 3 중량%로 포함할 수 있다.Another object of the present invention relates to a non-woven non-woven fabric containing hydrophobic fibers, as a non-woven fabric in which part or all of the non-woven fabric containing hydrophobic fibers is modified with a hydrophilic non-woven fabric, wherein the cell-free hydrophilic modified coating agent is 0.1 to 3% by weight of the total weight of the nonwoven Can include.
본 발명의 바람직한 일실시예로서, ISO 10993-5 방법에 의거하여 IC50 측정시, 세포생존율이 70 ~ 100%일 수 있다.As a preferred embodiment of the present invention, when measuring IC 50 according to the ISO 10993-5 method, the cell viability may be 70 to 100%.
본 발명의 바람직한 일실시예로서, 상기 부직포는 스펀본드 부직포, 멜트블로운 부직포, 에어레이드(Air-laid), 웻레이드(Wet-laid) 또는 드라이레이드 부직포(Dry-laid)일 수 있다.In a preferred embodiment of the present invention, the nonwoven fabric may be a spunbond nonwoven fabric, a melt blown nonwoven fabric, an air-laid, wet-laid, or dry-laid nonwoven fabric.
본 발명의 친수성 개질 코팅제는 세포독성이 없으면서, 코팅성이 우수하며, 이를 이용하여 섬유 소재 제품을 친수성 개질시키는 경우, 낮은 재젖음성을 가지는 바, 소수성 섬유 제품을 친수성 섬유로 개질시키는데 사용하기 적합하며, 특히, 피부에 직접 접촉되는 제품에 적용하기에 적합하다. The hydrophilic modified coating of the present invention does not have cytotoxicity, has excellent coating properties, and has low rewetability when hydrophilic modification of a fiber material product using this, is suitable for use in modifying a hydrophobic fiber product into a hydrophilic fiber. , In particular, it is suitable for application to products that come into direct contact with the skin.
이하, 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명의 세포무독성 친수성 개질 코팅제는 소듐염, 말레산염, 인산염 및 알코올 에테르계 화합물을 포함한다.The non-toxic hydrophilic modified coating agent of the present invention includes sodium salt, maleate, phosphate and alcohol ether compounds.
상기 소듐염은 옥틸 나트륨 설포숙신산(도큐세이트 소듐), 도데실벤젠설폰산 나트륨, 암모늄 알파-설포-오메가-(노닐페녹시)폴리(옥시-1,2-에탄디일), 설포부탄다이옥산 설포부탄다이옥산 1,4-비스(2-(C1 ~ C3의 알킬)(C4 ~ C8의 알킬)에스터 나트륨염, 소듐탈로에이트, 소듐코코에이트 및 소듐팜커넬레이트 중에서 선택된 1종 또는 2종 이상을 포함할 수 있고, 바람직하게는 옥틸 나트륨 설포숙신산(도큐세이트 소듐), 도데실벤젠설폰산 나트륨, 암모늄 알파-설포-오메가-(노닐페녹시)폴리(옥시-1,2-에탄디일) 및 설포부탄다이옥산 설포부탄다이옥산 1,4-비스(2-(C1 ~ C3의 알킬)(C4 ~ C8의 알킬)에스터 나트륨염 중에서 선택된 선택된 1종 또는 2종 이상을 포함할 수 있으며, 더욱 바람직하게는 암모늄 알파-설포-오메가-(노닐페녹시)폴리(옥시-1,2-에탄디일) 및 설포부탄다이옥산 설포부탄다이옥산 1,4-비스(2-(C2 ~ C3의 알킬)헥실)에스터 나트륨염 중에서 선택된 선택된 1종 또는 2종 이상을 포함할 수 있다.The sodium salt is octyl sodium sulfosuccinic acid (docusate sodium), sodium dodecylbenzenesulfonic acid, ammonium alpha-sulfo-omega-(nonylphenoxy)poly(oxy-1,2-ethandiyl), sulfobutanedioxane sulfobutane Dioxane 1,4-bis (2-(C 1 ~ C 3 alkyl) (C 4 ~ C 8 alkyl) ester sodium salt, sodium taloate, sodium cocoate and one or two selected from sodium palm kernelate It may contain the above, preferably octyl sodium sulfosuccinic acid (docusate sodium), sodium dodecylbenzenesulfonate, ammonium alpha-sulfo-omega-(nonylphenoxy)poly(oxy-1,2-ethandiyl) And sulfobutanedioxane sulfobutanedioxane 1,4-bis(2-(C 1 to C 3 alkyl) (C 4 to C 8 alkyl) ester sodium salt selected from one or more selected from, , More preferably ammonium alpha-sulfo-omega-(nonylphenoxy)poly(oxy-1,2-ethandiyl) and sulfobutanedioxane sulfobutanedioxane 1,4-bis(2-(C 2 ~ C 3 of Alkyl) hexyl) ester may include one or two or more selected from sodium salts.
그리고, 소듐염의 함량은 친수성 개질 코팅제 전체 중량 중 15 ~ 20 중량%를, 바람직하게는 16 ~ 18.5 중량%를, 더욱 바람직하게는 16.5 ~ 18.0 중량%로 포함할 수 있다. 이때, 소듐염 함량이 15 중량% 미만이면 개질 코팅제의 pH가 너무 낮아지는 문제가 있을 수 있고, 20 중량%를 초과하면 오히려 개질 코팅제의 pH가 너무 높아지는 문제 및 부직포 개질 후, 재젖음이 저하되는 문제가 있을 수 있으므로, 상기 범위 내로 사용하는 것이 좋다.And, the content of the sodium salt may include 15 to 20% by weight, preferably 16 to 18.5% by weight, more preferably 16.5 to 18.0% by weight of the total weight of the hydrophilic modified coating agent. At this time, if the sodium salt content is less than 15% by weight, there may be a problem that the pH of the modified coating agent is too low, and when it exceeds 20% by weight, the pH of the modified coating agent is rather increased, and after the nonwoven fabric is modified, rewetting is lowered Since there may be a problem, it is better to use it within the above range.
친수성 개질 코팅제 조성 중 상기 말레산염은 비스(2-(C1 ~ C3의 알킬)(C4 ~ C8의 알킬)말레이트, 에틸렌 무수 말레산 공중합체 및 이소부틸렌 무수 말레산 공중합체 중에서 선택된 1종 또는 2종 이상을 포함할 수 있고, 바람직하게는 비스(2-(C2 ~ C3의 알킬)(C5 ~ C7의 알킬)말레이트 및 에틸렌 무수 말레산 공중합체 중에서 선택된 1종 또는 2종을, 더욱 바람직하게는 비스(2-(C2 ~ C3의 알킬)헥실)말레이트를 사용할 수 있다.In the composition of the hydrophilic modified coating agent, the maleic acid salt is bis(2-(C 1 ~ C 3 alkyl) (C 4 ~ C 8 alkyl) maleate, ethylene maleic anhydride copolymer, and isobutylene maleic anhydride copolymer. It may include one or two or more selected, preferably bis (2- (C 2 ~ C 3 alkyl) (C 5 ~ C 7 alkyl) maleate and ethylene maleic anhydride copolymer 1 selected from the type or two types, may be more preferably used a (hexyl 2- (alkyl of C 2 ~ C 3)) bis maleate.
그리고, 말레산염의 함량은 친수성 개질 코팅제 전체 중량 중 10 ~ 16 중량%를, 바람직하게는 11.0 ~ 14.8 중량%를, 더욱 바람직하게는 12.0 ~ 14.0 중량%로 포함할 수 있다. 이때, 말레산염 함량이 10중량% 미만이면 개질된 부직포의 친수성 향상 효과가 저하되는 문제가 있을 수 있고, 16 중량%를 초과하면 세포 독성이 증가하는 문제가 있을 수 있으므로, 상기 범위 내로 사용하는 것이 좋다.In addition, the content of maleate may include 10 to 16% by weight, preferably 11.0 to 14.8% by weight, and more preferably 12.0 to 14.0% by weight, based on the total weight of the hydrophilic modified coating agent. At this time, if the maleate content is less than 10% by weight, there may be a problem that the hydrophilicity improvement effect of the modified nonwoven fabric is lowered, and if it exceeds 16% by weight, there may be a problem of increasing cytotoxicity, so it is recommended to use it within the above range. good.
다음으로, 친수성 개질 코팅제 조성 중 상기 인산염은 폴리(옥시-1,2-에탄디일), 폴리옥시에틸렌 노닐 페닐 에테르 인산, 폴리옥시에틸렌 노닐 페닐 에테르 인산, 인산 트리스(2-에틸헥실)에스터, (Z)-알파-2-옥타데켄일-오메가-하이드록시폴리(옥시-1,2-에탄딜)인산염 및 폴리(옥시-1,2-에테인디닐), α-도데실-ω-하이드록시-, 포스페이트, 포타슘염{Poly(oxy-1,2-ethanediyl), α-dodecyl-ω-hydroxy-,phosphate, potassium salt/cas no. 58318-92-6} 중에서 선택된 1종 또는 2종 이상을 포함할 수 있다.Next, the phosphate in the composition of the hydrophilic modified coating agent is poly(oxy-1,2-ethanediyl), polyoxyethylene nonyl phenyl ether phosphoric acid, polyoxyethylene nonyl phenyl ether phosphoric acid, phosphate tris(2-ethylhexyl) ester, ( Z)-alpha-2-octadekenyl-omega-hydroxypoly(oxy-1,2-ethandyl)phosphate and poly(oxy-1,2-ethaninyl), α-dodecyl-ω-hydroxy- , Phosphate, potassium salt (Poly(oxy-1,2-ethanediyl), α-dodecyl-ω-hydroxy-,phosphate, potassium salt/cas no. 58318-92-6} may include one or two or more selected from.
그리고, 인산염의 함량은 친수성 개질 코팅제 전체 중량 중 2 ~ 8 중량%를, 바람직하게는 2.5 ~ 7.5 중량%를, 더욱 바람직하게는 3.0 ~ 6.2 중량%로 포함할 수 있다. 이때, 인산염 함량이 2 중량% 미만이면 개질된 부직포의 내구 흡수도 향상 효과가 미비한 문제가 있을 수 있고, 8 중량%를 초과하면 오히려 내구 흡수도가 저하되는 문제가 있을 수 있으므로, 상기 범위 내로 사용하는 것이 좋다.In addition, the content of phosphate may include 2 to 8% by weight, preferably 2.5 to 7.5% by weight, and more preferably 3.0 to 6.2% by weight, based on the total weight of the hydrophilic modified coating agent. At this time, if the phosphate content is less than 2% by weight, there may be a problem in that the durability absorption improvement effect of the modified nonwoven fabric is insufficient, and if it exceeds 8% by weight, there may be a problem that the durability absorption is rather lowered, so use within the above range. It is good to do.
다음으로, 친수성 개질 코팅제 조성 중 알콜 에테르계 화합물은 상기 친수성 개질 코팅제의 다른 조성물들에 대한 용매 역할을 하는 것으로서, 디프로필렌 글리콜 모노메틸 에테르, 폴리비닐 에테르, 폴리에틸렌 글리콜 및 알콜 폴리 옥시 에틸렌 에테르 중에서 선택된 1종 또는 2종 이상을 포함할 수 있고, 바람직하게는 디프로필렌 글리콜 모노메틸 에테르, 폴리비닐 에테르 및 알콜 폴리 옥시 에틸렌 에테르 중에서 선택된 1종 또는 2종을, 더욱 바람직하게는 디프로필렌 글리콜 모노메틸 에테르 및 알콜 폴리 옥시 에틸렌 에테르 중에서 선택된 1종 또는 2종을 사용할 수 있다.Next, the alcohol ether compound in the composition of the hydrophilic modified coating agent serves as a solvent for the other compositions of the hydrophilic modified coating agent, and is selected from dipropylene glycol monomethyl ether, polyvinyl ether, polyethylene glycol and alcohol polyoxyethylene ether. One or two or more may be included, preferably one or two selected from dipropylene glycol monomethyl ether, polyvinyl ether and alcohol polyoxyethylene ether, more preferably dipropylene glycol monomethyl ether And alcohol polyoxyethylene ether.
그리고, 알콜 에테르계 화합물의 함량은 친수성 개질 코팅제 전체 100 중량% 중 다른 조성물을 제외한 잔량으로 사용된다. In addition, the content of the alcohol ether compound is used in the remaining amount excluding other compositions of 100% by weight of the total hydrophilic modified coating agent.
앞서 설명한 조성물들을 혼합하여 제조한 본 발명의 세포무독성 친수성 개질 코팅제는 ASTM D7042 표준 시험(20℃)에 의거하여 측정한 점도가 950 ~ 1,100 mPa.s일 수 있으며, 바람직하게는 980 ~ 1,080 mPa.s, 더욱 바람직하게는 1,000 ~ 1,060 mPa.s일 수 있다.The cell non-toxic hydrophilic modified coating agent of the present invention prepared by mixing the above-described compositions may have a viscosity of 950 to 1,100 mPa.s measured according to ASTM D7042 standard test (20°C), and preferably 980 to 1,080 mPa. s, more preferably 1,000 to 1,060 mPa.s.
또한, 본 발명의 세포무독성 친수성 개질 코팅제를 9 ~ 12 중량% 농도로, 바람직하게는 10 중량% 농도로 물에 용해된 용액은 20℃에서 분석시, pH가 5 ~ 8, 바람직하게는 pH 5.5 ~ 7.5, 더욱 바람직하게는 pH 5.8 ~ 7.0일 수 있다.In addition, the solution dissolved in water at a concentration of 9 to 12% by weight, preferably at a concentration of 10% by weight, of the cell non-toxic hydrophilic modified coating agent of the present invention has a pH of 5 to 8, preferably pH 5.5 when analyzed at 20°C. It may be ~ 7.5, more preferably a pH of 5.8 ~ 7.0.
그리고, 본 발명의 세포무독성 친수성 개질 코팅제는 융점이 -3 ~ 3℃, 바람직하게는 융점이 -2 ~ 2℃일 수 있다.In addition, the non-toxic hydrophilic modified coating agent of the present invention may have a melting point of -3 to 3°C, preferably a melting point of -2 to 2°C.
앞서 설명한 세포무독성 친수성 개질 코팅제를 이용하여 소수성 제품을 친수성으로 개질시킬 수 있으며, 바람직한 일례로서, 부직포를 친수성 개질시키는 내용에 대해 설명하면 다음과 같다. Hydrophobic products can be modified to be hydrophilic using the previously described cell non-toxic hydrophilic modified coating agent, and as a preferred example, description will be given of the hydrophilic modification of the nonwoven fabric as follows.
부직포를 준비하는 1단계; 세포무독성 친수성 개질 코팅제를 상기 부직포의 일부 또는 전체를 코팅하는 2단계; 및 열처리하여 친수성 개질 코팅제를 부직포에 열적 고정시켜서 부직포를 친수성으로 개질시키는 3단계;를 포함하는 공정을 수행하여 친수성 개질된 부직포를 제조할 수 있다.Step 1 of preparing a nonwoven fabric; A second step of coating part or all of the nonwoven fabric with a non-toxic hydrophilic modified coating agent; And 3 step of modifying the nonwoven fabric to be hydrophilic by thermally fixing the hydrophilic modified coating agent to the nonwoven fabric by heat treatment, thereby producing a hydrophilic modified nonwoven fabric.
1단계의 상기 부직포는 소수성 섬유를 포함하며, 일부 친수성 섬유를 포함할 수도 있고, 전부 소수성 섬유로 제조된 부직포일 수도 있다. 부직포의 일부 또는 전부는 소수성을 가질 수 있다. The nonwoven fabric in step 1 may include hydrophobic fibers, some hydrophilic fibers may be included, or all nonwoven fabrics may be made of hydrophobic fibers. Some or all of the nonwoven fabric may have hydrophobicity.
상기 소수성 섬유로는 폴리에틸렌 섬유, 폴리프로필렌 섬유 및 프로필렌 에틸렌 공중합 섬유 중에서 중에서 선택된 1종 이상을 포함하는 폴리올레핀계 섬유일 수 있다.The hydrophobic fiber may be a polyolefin-based fiber including at least one selected from polyethylene fiber, polypropylene fiber, and propylene ethylene copolymer fiber.
그리고, 상기 소수성 섬유는 평균직경 1μm ~ 50μm, 바람직하게는 1μm ~ 30 μm일 수 있다.In addition, the hydrophobic fiber may have an average diameter of 1 μm to 50 μm, preferably 1 μm to 30 μm.
그리고, 1단계의 부직포는 스펀본드 부직포, 멜트블로운 부직포, 에어레이드(Air-laid), 웻레이드(Wet-laid) 또는 드라이레이드 부직포(Dry-laid)일 수 있다. In addition, the nonwoven fabric of the first step may be a spunbond nonwoven fabric, a melt blown nonwoven fabric, an air-laid, a wet-laid, or a dry-laid nonwoven fabric.
다음으로, 2단계의 세포무독성 친수성 개질 코팅제는 앞서 설명한 바와 같다. 그리고, 2단계의 코팅은 당업계에서 사용하는 일반적인 코팅 방법으로 통해 수행할 수 있으며, 바람직하게는 키스롤 코팅법 또는 스프레이 코팅법 등을 통해서 수행할 수 있다. Next, the cell non-toxic hydrophilic modified coating agent of step 2 is as described above. In addition, the coating of the second step may be performed by a general coating method used in the art, and preferably, it may be performed through a kiss roll coating method or a spray coating method.
다음으로, 3단계의 열처리는 드럼 드라이어에서 100 ~ 150℃, 바람직하게는 110 ~ 140℃의 열을 가하여 수행할 수 있다. 이때, 열처리 온도가 100℃ 미만이면 부직포 건조가 덜 되는 문제가 있을 수 있고, 열처리 온도가 150℃ 를 초과하면 부직포가 딱딱해 지는 문제가 있을 수 있다.Next, the heat treatment in the third step may be performed by applying heat of 100 to 150°C, preferably 110 to 140°C in a drum dryer. At this time, if the heat treatment temperature is less than 100°C, there may be a problem that drying of the nonwoven fabric is less, and if the heat treatment temperature exceeds 150°C, there may be a problem that the nonwoven fabric becomes hard.
제조된 친수성으로 개질된 세포무독성 부직포는 세포무독성 친수성 개질 코팅제를 0.1 ~ 3.0 중량%로, 바람직하게는 0.4 ~ 2.8 중량%로, 더욱 바람직하게는 0.5 ~ 1.5 중량%로 포함할 수 있다. 이때, 세포무독성 친수성 개질 코팅제 함량이 0.1 중량% 미만이면 친수성 개질 효과가 미비할 수 있고, 3 중량%를 초과하면 부직포의 재젖음성이 높아져 축축하게 하는 문제가 있을 수 있다.The prepared hydrophilic modified non-woven fabric may contain a cell non-toxic hydrophilic modified coating agent in an amount of 0.1 to 3.0% by weight, preferably 0.4 to 2.8% by weight, and more preferably 0.5 to 1.5% by weight. At this time, if the content of the non-toxic hydrophilic modified coating agent is less than 0.1% by weight, the hydrophilicity modifying effect may be insufficient, and if it exceeds 3% by weight, the rewetability of the nonwoven fabric may increase and there may be a problem of moistening.
그리고, 3단계의 세포무독성 부직포는 평량이 10 ~ 100 gsm일 수 있다.In addition, the cell-free non-woven fabric of step 3 may have a basis weight of 10 to 100 gsm.
그리고, 본 발명의 세포무독성 부직포는 ISO 10993-5 방법에 의거하여 IC50 측정시, 세포생존율이 70 ~ 100%, 바람직하게는 85 ~ 100%, 더욱 바람직하게는 90 ~ 100%일 수 있다.In addition, the cell-free nonwoven fabric of the present invention may have a cell viability of 70 to 100%, preferably 85 to 100%, more preferably 90 to 100%, when IC 50 is measured according to the ISO 10993-5 method.
또한, 본 발명의 세포무독성 부직포는 WSP 70.3(08)(Standard Test Method for Nonwoven Coverstock Liquid Strike-Through Time Using Simulated Urine) 에 따라 액체 흡수 속도 측정시, 2.50 ~ 3.50초, 바람직하게는 2.50 ~ 3.20초일 수 있다.In addition, the cellular non-toxic nonwoven fabric of the present invention is 2.50 to 3.50 seconds, preferably 2.50 to 3.20 seconds, when the liquid absorption rate is measured according to WSP 70.3(08) (Standard Test Method for Nonwoven Coverstock Liquid Strike-Through Time Using Simulated Urine). I can.
또한, 본 발명의 세포무독성 부직포는WSP 70.7(09)(Standard Test Method for Nonwoven-Repeated Liquid Strike-Through Time)에 따라 내구 흡수도 측정시, 1회째 내구 흡수도가 1.50 ~ 2.80초이고, 2회째 내구 흡수도가 2.00 ~ 3.50초이며, 3회째 내구 흡수도가 2.30 ~ 3.80초일 수 있다.In addition, the cellular non-toxic nonwoven fabric of the present invention was measured for durability absorption according to WSP 70.7(09) (Standard Test Method for Nonwoven-Repeated Liquid Strike-Through Time), the first durability absorption was 1.50 to 2.80 seconds, and the second time Durable absorption is 2.00 to 3.50 seconds, and the third durability absorption may be 2.30 to 3.80 seconds.
또한, 본 발명의 세포무독성 부직포는 WSP 70.8(09)(Standard Test Method for Wetback After Repeated Strike-Through Time)에 따라 액체에 대한 재젖음성 측정시, 재젖음성이 2.0 ~ 3.5g, 바람직하게는 2.2 ~ 3.3g일 수 있다.In addition, the non-woven fabric of the present invention has a rewetability of 2.0 to 3.5 g, preferably 2.2 to when measuring the rewetability of a liquid according to WSP 70.8 (09) (Standard Test Method for Wetback After Repeated Strike-Through Time). May be 3.3g.
그리고, 본 발명의 세포무독성 부직포는 ISO 10993-5 방법에 의거하여 IC50 측정시, 세포생존율이 70 ~ 100%, 바람직하게는 85 ~ 100%, 더욱 바람직하게는 90 ~ 100%일 수 있다.In addition, the cell-free nonwoven fabric of the present invention may have a cell viability of 70 to 100%, preferably 85 to 100%, more preferably 90 to 100%, when IC 50 is measured according to the ISO 10993-5 method.
이하에서는 본 발명을 실시예에 의거하여 더욱 구체적으로 설명한다. 하기 실시예는 본 발명의 이해를 돕기 위한 것이며, 실시예에 의해 본 발명의 권리범위를 한정하여 해석해서는 안된다.Hereinafter, the present invention will be described in more detail based on examples. The following examples are intended to aid understanding of the present invention, and should not be interpreted to limit the scope of the present invention by examples.
[실시예][Example]
실시예 1 : 세포무독성 친수성 개질 코팅제의 제조Example 1: Preparation of cell non-toxic hydrophilic modified coating agent
소듐염인 설포부탄다이옥산 1,4-비스(2-에틸헥실)에스터 나트륨염(cas no. 577-11-7), 말레산염인 비스(2-에틸헥실)말레에이트(bis(2-ethylhexyl) maleate, cas no. 142-16-5), 인산염인 폴리(옥시-1,2-에테인디닐), α-도데실-ω-하이드록시-, 포스페이트, 포타슘염(Poly(oxy-1,2-ethanediyl), α-dodecyl-ω-hydroxy-,phosphate, potassium salt/cas no. 58318-92-6) 및 알코올 에테르계 화합물인 디프로필렌 글리콜 모노메틸 에테르를 혼합 및 교반하여 세포무독성 친수성 개질 코팅제를 제조하였다.Sodium salt sulfobutanedioxane 1,4-bis(2-ethylhexyl) ester sodium salt (cas no. 577-11-7), maleate bis(2-ethylhexyl) maleate (bis(2-ethylhexyl) maleate, cas no.142-16-5), phosphate poly(oxy-1,2-etheindinyl), α-dodecyl-ω-hydroxy-, phosphate, potassium salt (Poly(oxy-1,2- ethanediyl), α-dodecyl-ω-hydroxy-,phosphate, potassium salt/cas no. 58318-92-6) and dipropylene glycol monomethyl ether, an alcohol ether compound, are mixed and stirred to prepare a non-toxic hydrophilic modified coating agent. I did.
그리고, 친수성 개질 코팅제 내 소듐염, 말레산염, 인산염 및 알코올 에테르계 화합물 각각의 함량은 하기 표 1과 같다.In addition, the contents of each of the sodium salt, maleic acid salt, phosphate and alcohol ether compounds in the hydrophilic modified coating agent are shown in Table 1 below.
실시예 2 ~ 실시예 7 및 비교예 1 ~ 비교예 6Examples 2 to 7 and Comparative Examples 1 to 6
상기 실시예 1과 동일한 방법으로 친수성 개질 코팅제를 제조하되, 하기 표 1과 같은 조성 및 조성비를 가지는 친수성 개질 코팅제를 각각 제조하였다.A hydrophilic modified coating agent was prepared in the same manner as in Example 1, but a hydrophilic modified coating agent having a composition and composition ratio as shown in Table 1 was prepared, respectively.
구분
(중량%)
division
(weight%)
소듐염Sodium salt 말레산염Maleate 인산염phosphate 알코올 에테르계 화합물Alcohol ether compounds
실시예 1Example 1 17.217.2 13.013.0 4.64.6 나머지 잔량Remaining balance
실시예 2Example 2 15.315.3 13.213.2 4.94.9 나머지 잔량Remaining balance
실시예 3Example 3 18.518.5 13.013.0 4.24.2 나머지 잔량Remaining balance
실시예 4Example 4 17.217.2 11.011.0 4.84.8 나머지 잔량Remaining balance
실시예 5Example 5 17.217.2 14.814.8 4.84.8 나머지 잔량Remaining balance
실시예 6Example 6 17.217.2 13.013.0 2.52.5 나머지 잔량Remaining balance
실시예 7Example 7 17.217.2 13.013.0 7.57.5 나머지 잔량Remaining balance
비교예 1Comparative Example 1 13.513.5 13.013.0 4.64.6 나머지 잔량Remaining balance
비교예 2Comparative Example 2 21.021.0 13.013.0 4.64.6 나머지 잔량Remaining balance
비교예 3Comparative Example 3 17.217.2 9.39.3 4.84.8 나머지 잔량Remaining balance
비교예 4Comparative Example 4 17.217.2 16.616.6 4.84.8 나머지 잔량Remaining balance
비교예 5Comparative Example 5 17.217.2 13.013.0 1.01.0 나머지 잔량Remaining balance
비교예 6Comparative Example 6 17.217.2 13.013.0 9.09.0 나머지 잔량Remaining balance
비교예 7Comparative Example 7
이소프로필 알코올을 친수성 개질 코팅제로 준비하였다.Isopropyl alcohol was prepared as a hydrophilic modified coating.
비교예 8Comparative Example 8
다이에스테르(Di-ester) 20 중량% 및 잔량의 프로필렌글리콜 화합물을 포함하는 용액을 친수성 개질 코팅제로 준비하였다.A solution containing 20% by weight of a diester (Di-ester) and a remaining amount of a propylene glycol compound was prepared as a hydrophilic modified coating agent.
비교예 9Comparative Example 9
실록산계 친수성 개질 코팅제인 CTFA(Dimethylsiloxane, 3-(3-((3- cocoamidopropyl)dimethylammonio)-2-hydroxyprpoxy)propyl groupterminated acetate / CAS 134737-05-6)를 친수성 개질 코팅제로 준비하였다.A siloxane-based hydrophilic modified coating agent, CTFA (Dimethylsiloxane, 3-(3-((3-cocoamidopropyl)dimethylammonio)-2-hydroxyprpoxy)propyl groupterminated acetate / CAS 134737-05-6), was prepared as a hydrophilic modified coating agent.
실험예 1 : 친수성 개질 코팅제의 점도 및 pH 측정Experimental Example 1: Measurement of viscosity and pH of a hydrophilic modified coating agent
상기 실시예 1 ~ 7 및 비교예 1 ~ 9에서 제조한 친수성 개질 코팅제 각각에 대한 점도 및 pH를 측정하였고, 그 결과를 하기 표 2에 나타내었다.The viscosity and pH of each of the hydrophilic modified coatings prepared in Examples 1 to 7 and Comparative Examples 1 to 9 were measured, and the results are shown in Table 2 below.
이때, 점도는 ASTM D7042 표준 시험(20℃)에 의거하여 측정하였으며, pH는 물에 친수성 개질 코팅제를 10 중량% 농도로 용해한 용액에 대한 pH이고, 20℃에서 분석한 것이다.At this time, the viscosity was measured according to the ASTM D7042 standard test (20°C), and the pH was the pH of a solution in which a hydrophilic modified coating agent was dissolved in water at a concentration of 10% by weight, and analyzed at 20°C.
구분division 점도
(mPa.s)
Viscosity
(mPa.s)
pHpH 융점(℃)Melting point(℃)
실시예 1Example 1 1,015 ~ 1,0251,015 ~ 1,025 6.0 ~ 6.16.0 to 6.1 -1 ~ 1-1 to 1
실시예 2Example 2 990 ~ 995990 ~ 995 5.2 ~ 5.35.2 ~ 5.3 -1 ~ 1-1 to 1
실시예 3Example 3 1,005 ~ 1,0101,005 ~ 1,010 6.4 ~ 6.56.4 ~ 6.5 -1 ~ 1-1 to 1
실시예 4Example 4 1,050 ~ 1,060 1,050 ~ 1,060 5.8 ~ 5.95.8 ~ 5.9 -1 ~ 1-1 to 1
실시예 5Example 5 1,035 ~ 1,0401,035 ~ 1,040 6.0 ~ 6.16.0 to 6.1 -1 ~ 1-1 to 1
실시예 6Example 6 990 ~ 995990 ~ 995 5.7 ~ 5.85.7 ~ 5.8 0 ~ 20 to 2
실시예 7Example 7 1,080 ~ 1,0851,080 ~ 1,085 6.2 ~ 6.36.2 ~ 6.3 -3 ~ -1-3 to -1
비교예 1Comparative Example 1 980 ~ 985980 ~ 985 4.5 ~ 4.64.5 ~ 4.6 -1 ~ 1-1 to 1
비교예 2Comparative Example 2 1,070 ~ 1,0751,070 ~ 1,075 7.4 ~ 7.57.4 ~ 7.5 -1 ~ 1-1 to 1
비교예 3Comparative Example 3 985 ~ 990985 ~ 990 6.5 ~ 6.76.5 ~ 6.7 -1 ~ 1-1 to 1
비교예 4Comparative Example 4 1,095 ~ 1,1001,095 ~ 1,100 5.7 ~ 5.85.7 ~ 5.8 -1 ~ 1-1 to 1
비교예 5Comparative Example 5 975 ~ 980975-980 5.7 ~ 5.85.7 ~ 5.8 3 ~ 53 to 5
비교예 6Comparative Example 6 1,095 ~ 1,1001,095 ~ 1,100 6.3 ~ 6.46.3 ~ 6.4 -3 ~ -1-3 to -1
표 2의 개질 코팅제의 물성 측정 결과를 살펴보면, 실시예 1 ~ 7은 점도 990 ~ 1,060 mPa.s, pH 5.2 ~ 6.3 및 융점 -3℃ ~ 1℃ 범위의 적정 물성 범위를 보였다.이에 반해, 소듐염을 15 중량% 미만으로 사용한 비교예 1의 경우, 실시예 1및 실시예 2와 비교할 때, pH가 급격하게 낮아져서 산성화되는 문제가 있었고, 소듐염을 20 중량% 초과하여 사용한 비교예 2의 경우, 실시예 1및 실시예 3과 비교할 때, pH가 급격하게 증가하는 경향을 보였다.Looking at the physical properties measurement results of the modified coating agent in Table 2, Examples 1 to 7 showed an appropriate range of properties ranging from viscosity 990 to 1,060 mPa.s, pH 5.2 to 6.3, and melting point -3°C to 1°C. On the other hand, sodium In the case of Comparative Example 1 in which the salt was used in an amount of less than 15% by weight, when compared with Examples 1 and 2, there was a problem that the pH was rapidly lowered and thus acidified, and in the case of Comparative Example 2 in which the sodium salt was used in excess of 20% by weight , When compared with Example 1 and Example 3, the pH showed a tendency to increase rapidly.
또한, 실시예 6 ~ 7 및 비교예 5 ~ 6의 융점을 살펴보면, 인산염 함량이 개질 코팅제의 융점에 영향을 주는 것을 확인할 수 있는데, 인산염 사용량이 감소하면 개질제의 융점이 증가하는 경향이 있음을 확인할 수 있으며, 비교예 5가 융점이 가장 높았으며, 실시예 7과 비교예 6을 비교해보면, 인산염을 8 중량% 초과해도 융점 하락이 없는 경향을 보였다.In addition, looking at the melting points of Examples 6 to 7 and Comparative Examples 5 to 6, it can be seen that the phosphate content affects the melting point of the modified coating agent.It was confirmed that the melting point of the modifying agent tends to increase when the amount of phosphate used decreases. In addition, Comparative Example 5 had the highest melting point, and when comparing Example 7 and Comparative Example 6, there was a tendency that there was no decrease in the melting point even when the phosphate was exceeded 8% by weight.
제조예 1 : 친수성 개질된 세포무독성 부직포의 제조Preparation Example 1: Preparation of hydrophilic modified non-toxic non-woven fabric
평균직경 17μm 인 폴리프로필렌 섬유로 제조된 평량 18gsm인 스펀본드 부직포를 준비하였다(제조사 도레이첨단소재, 상품명 LIVSEN).A spunbond nonwoven fabric having a basis weight of 18 gsm made of polypropylene fibers having an average diameter of 17 μm was prepared (manufacturer Toray Advanced Materials, brand name LIVSEN).
다음으로, 상기 실시예 1에서 제조한 친수성 개질 코팅제를 키스롤 코팅 방식으로 부직포로 코팅 및 건조하였다.Next, the hydrophilic modified coating agent prepared in Example 1 was coated and dried with a nonwoven fabric by a kiss roll coating method.
다음으로, 드럼드라이어에서 약 125 ~ 130℃ 온도 조건 하에서, 열처리하여 친수성으로 개질된 세포무독성 부직포를 제조하였다. Next, heat treatment was performed in a drum dryer under a temperature condition of about 125 to 130° C. to prepare a non-woven fabric that was modified to be hydrophilic.
제조된 세포무독성 부직포 내 친수성 개질 코팅제 함량은 약 0.7 중량%였다.The content of the hydrophilic modified coating agent in the prepared non-toxic nonwoven fabric was about 0.7% by weight.
제조예 2 ~ 7 및 비교제조졔 1 ~ 11Preparation Examples 2 to 7 and Comparative Manufacturing 1 to 11
상기 제조예 1과 동일한 방법으로 친수성 개질된 부직포를 제조하되, 실시예 1의 친수성 개질 코팅제 대신 실시예 2 ~ 5 및 비교예 1 ~ 9에서 준비한 친수성 개질 코팅제 각각을 사용하여 친수성으로 개질된 부직포 각각을 제조하여, 하기 표 3과 같이 제조예 2 ~ 7 및 비교제조예 1 ~ 11을 각각 실시하였다.A nonwoven fabric having been modified to be hydrophilic in the same manner as in Preparation Example 1 was prepared, but each nonwoven fabric modified to be hydrophilic using each of the hydrophilic modified coating agents prepared in Examples 2 to 5 and Comparative Examples 1 to 9 instead of the hydrophilic modified coating agent of Example 1 To prepare, Preparation Examples 2 to 7 and Comparative Preparation Examples 1 to 11 were each performed as shown in Table 3 below.
구분division 친수성 개질 코팅제 종류Types of hydrophilic modified coatings 부직포 내 함량Content in non-woven fabric
제조예 1Manufacturing Example 1 실시예 1Example 1 0.7 중량%0.7% by weight
제조예 2Manufacturing Example 2 실시예 1Example 1 0.4 중량%0.4% by weight
제조예 3Manufacturing Example 3 실시예 1Example 1 2.6 중량%2.6% by weight
제조예 4Manufacturing Example 4 실시예 2Example 2 0.7 중량%0.7% by weight
제조예 5Manufacturing Example 5 실시예 3Example 3 0.7 중량%0.7% by weight
제조예 6Manufacturing Example 6 실시예 4Example 4 0.7 중량%0.7% by weight
제조예 7Manufacturing Example 7 실시예 5Example 5 0.7 중량%0.7% by weight
제조예 8Manufacturing Example 8 실시예 6Example 6 0.7 중량%0.7% by weight
제조예 9Manufacturing Example 9 실시예 7Example 7 0.7 중량%0.7% by weight
비교제조예 1Comparative Production Example 1 실시예 1Example 1 0.08 중량%0.08% by weight
비교제조예 2Comparative Production Example 2 실시예 1Example 1 3.1 중량%3.1% by weight
비교제조예 3Comparative Production Example 3 비교예 1Comparative Example 1 0.7 중량%0.7% by weight
비교제조예 4Comparative Production Example 4 비교예 2Comparative Example 2 0.7 중량%0.7% by weight
비교제조예 5Comparative Production Example 5 비교예 3Comparative Example 3 0.7 중량%0.7% by weight
비교제조예 6Comparative Production Example 6 비교예 4Comparative Example 4 0.7 중량%0.7% by weight
비교제조예 7Comparative Production Example 7 비교예 5Comparative Example 5 0.7 중량%0.7% by weight
비교제조예 8Comparative Production Example 8 비교예 6Comparative Example 6 0.7 중량%0.7% by weight
비교제조예 9Comparative Production Example 9 비교예 7Comparative Example 7 0.7 중량%0.7% by weight
비교제조예 10Comparative Production Example 10 비교예 8Comparative Example 8 0.7 중량%0.7% by weight
비교제조예 11Comparative Production Example 11 비교예 9Comparative Example 9 0.7 중량%0.7% by weight
실험예 1: 액체의 흡수속도(스트라이크 쓰루, Strike through)의 평가Experimental Example 1: Evaluation of liquid absorption rate (strike through)
제조예 및 비교제조예에서 제조한 부직포를 10㎝ x 10㎝(가로 x 세로)의 크기로 절단하여 측정 시료를 준비하였다. A measurement sample was prepared by cutting the nonwoven fabric prepared in Preparation Example and Comparative Preparation Example into a size of 10 cm x 10 cm (width x length).
이후, WSP 70.3(08)(Standard Test Method for Nonwoven Coverstock Liquid Strike-Through Time Using Simulated Urine) 에 따라 상기 측정 시료의 흡수 속도(구체적으로, 친수성 부직포층의 액체 흡수속도)를 측정하였고, 그 결과를 하기 표 4에 나타내었다. 동종의 측정 시료에 대하여 10회씩 흡수도를 측정한 후, 그 평균값을 최종 흡수속도로 기록하였다. 구체적으로, 상기 측정 시료를 흡수지 위에 올려 놓은 후, 상기 흡수지를 통해 0.9 중량% NaCl 수용액 5ml를 모두 흡수하는 시간을 흡수속도로 평가하였다.Thereafter, the absorption rate of the measurement sample (specifically, the liquid absorption rate of the hydrophilic nonwoven layer) was measured according to WSP 70.3 (08) (Standard Test Method for Nonwoven Coverstock Liquid Strike-Through Time Using Simulated Urine), and the result It is shown in Table 4 below. After measuring the absorbance 10 times for the same type of measurement sample, the average value was recorded as the final absorption rate. Specifically, after placing the measurement sample on the absorbent paper, the time to absorb all 5 ml of 0.9 wt% NaCl aqueous solution through the absorbent paper was evaluated as the absorption rate.
실험예 2: 내구 흡수도의 평가Experimental Example 2: Evaluation of Durable Absorption
제조예 및 비교제조예에서 제조한 부직포를 10㎝ x 10㎝(가로 x 세로)의 크기로 절단하여 측정 시료를 준비하였다. A measurement sample was prepared by cutting the nonwoven fabric prepared in Preparation Example and Comparative Preparation Example into a size of 10 cm x 10 cm (width x length).
이후, WSP 70.7(09)(Standard Test Method for Nonwoven- Repeated Liquid Strike-Through Time)에 따라 상기 측정 시료의 내구 흡수도(구체적으로, 친수성 부직포층의 반복 흡수도)를 측정하였고, 그 결과를 하기 표 4에 나타내었다. 동종의 측정 시료에 대하여 3회씩 내구 흡수도를 측정한 후, 내구 흡수도로 기록하였다. 구체적으로, 상기 측정 시료를 흡수지 위에 올려 놓은 후, 상기 흡수지를 통해 0.9중량% NaCl 수용액 5ml를 1회, 2회, 3회에 걸처 총 15ml를 흡수하는 시간을 내구 흡수도록 평가하였으며, 평가 기록은 1회, 2회, 3회 각각 기록하였다.Thereafter, the durability absorption of the measurement sample (specifically, the repeated absorption of the hydrophilic nonwoven layer) was measured according to WSP 70.7 (09) (Standard Test Method for Nonwoven-Repeated Liquid Strike-Through Time), and the results are as follows. It is shown in Table 4. Durable absorbency was measured three times for the same type of measurement sample, and then the durability absorbance was recorded. Specifically, after placing the measurement sample on the absorbent paper, the time to absorb a total of 15 ml of 5 ml of 0.9% by weight NaCl aqueous solution through the absorbent paper once, twice, and three times was evaluated for durable absorption, and the evaluation record is Recorded once, twice, and three times, respectively.
실험예 3: 재젖음성(리웻, Re-wet)의 평가Experimental Example 3: Evaluation of rewetability (re-wet)
상기 실험예 1에 따라 액체의 흡수도를 평가한 측정 시료를 이용하여 WSP 70.8(09)(Standard Test Method for Wetback After Repeated Strike-Through Time)에 따라 상기 측정 시료의 재젖음성(구체적으로, 친수성 부직포층의 재젖음성)을 측정하였고, 그 결과를 하기 표 4에 나타내었다. 구체적으로, 상기 평가예 1에 따라 액체의 흡수도를 평가한 측정 시료를 새로운 흡수지 위에 올려 놓은 후, 0.9중량% NaCl 수용액 20ml를 상기 흡수지에 넣고, 상기 측정 시료에 5kg의 하중을 가한 후 상기 측정 시료로 역으로 재흡수되는 액체량을 측정하여 재젖음성으로 기록하였다.The rewetability of the measurement sample (specifically, hydrophilic nonwoven fabric) according to WSP 70.8(09) (Standard Test Method for Wetback After Repeated Strike-Through Time) using a measurement sample evaluating the absorption of liquid according to Experimental Example 1 The rewetability of the layer) was measured, and the results are shown in Table 4 below. Specifically, after placing the measurement sample for which the absorption of the liquid was evaluated according to Evaluation Example 1 on a new absorbent paper, 20 ml of a 0.9 wt% NaCl aqueous solution was added to the absorbent paper, and a load of 5 kg was applied to the measurement sample, and the measurement The amount of liquid reversely reabsorbed as a sample was measured and recorded as rewetability.
실험예 4: 세포독성의 평가Experimental Example 4: Evaluation of cytotoxicity
제조예 및 비교제조예에서 제조한 부직포로부터 시료를 채취하고, ISO 10993-5(Biological evaluation of medical devices-Part 5: Tests for in-vitro cytotoxicity)의 방법으로 IC50(inhibition concentration 50, 콜로니 형성 저해농도) 분석하였고, 그 결과를 하기 표 4에 나타내었다. IC50 평가 결과는 70 ~ 100% 이어야 세포 무독성 부직포인 것으로 평가한다. Samples were collected from the nonwoven fabrics prepared in Preparation Example and Comparative Preparation Example, and IC 50 (inhibition concentration 50, colony formation inhibition) by the method of ISO 10993-5 (Biological evaluation of medical devices-Part 5: Tests for in-vitro cytotoxicity) Concentration) was analyzed, and the results are shown in Table 4 below. The IC 50 evaluation result should be between 70 and 100% to be evaluated as a non-woven fabric.
구분division 부직포
평량
(gsm)
Non-woven
Basis weight
(gsm)
흡수
속도
(sec)
absorption
speed
(sec)
내구
흡수도(sec)
Durability
Absorption (sec)
재젖음성
(g)
Rewetability
(g)
IC50
(%)
IC 50
(%)
비고Remark
1회1 time 2회Episode 2 3회3rd time
제조예1Manufacturing Example 1 1818 2.942.94 1.861.86 2.522.52 2.862.86 2.92.9 100100 세포 무독성Cell nontoxic
제조예2Manufacturing Example 2 1818 3.153.15 2.502.50 3.273.27 3.413.41 2.22.2 100100 세포 무독성Cell nontoxic
제조예3Manufacturing Example 3 1818 2.522.52 1.551.55 2.252.25 2.432.43 3.33.3 9797 세포 무독성Cell nontoxic
제조예4Manufacturing Example 4 1818 2.872.87 1.791.79 2.402.40 2.722.72 2.92.9 100100 세포 무독성Cell nontoxic
제조예5Manufacturing Example 5 1818 2.982.98 1.951.95 2.672.67 3.023.02 2.32.3 9999 세포 무독성Cell nontoxic
제조예6Manufacturing Example 6 1818 3.183.18 2.352.35 3.073.07 3.283.28 2.72.7 100100 세포 무독성Cell nontoxic
제조예7Manufacturing Example 7 1818 2.682.68 1.721.72 2.302.30 2.572.57 3.13.1 9595 세포 무독성Cell nontoxic
제조예8Manufacturing Example 8 1818 3.043.04 2.082.08 2.882.88 3.123.12 2.72.7 100100 세포 무독성Cell nontoxic
제조예9Manufacturing Example 9 1818 2.982.98 2.022.02 2.632.63 3.203.20 3.03.0 100100 세포 무독성Cell nontoxic
비교제조예1Comparative Production Example 1 1818 4.424.42 3.283.28 4.924.92 5.595.59 1.21.2 100100 세포 무독성Cell nontoxic
비교제조예2Comparative Production Example 2 1818 2.482.48 1.501.50 2.172.17 2.392.39 4.64.6 7878 중간정도 세포독성Moderate cytotoxicity
비교제조예3Comparative Production Example 3 1818 2.852.85 1.721.72 2.462.46 2.782.78 2.82.8 100100 세포 무독성Cell nontoxic
비교제조예4Comparative Production Example 4 1818 3.053.05 2.092.09 2.982.98 3.103.10 1.71.7 100100 세포 무독성Cell nontoxic
비교제조예5Comparative Production Example 5 1818 3.863.86 2.772.77 3.463.46 3.8283.828 2.72.7 100100 세포 무독성Cell nontoxic
비교제조예6Comparative Production Example 6 1818 2.362.36 1.521.52 1.981.98 2.212.21 3.23.2 8181 중간정도 세포독성Moderate cytotoxicity
비교제조예7Comparative Production Example 7 1818 3.093.09 2.142.14 2.952.95 3.273.27 2.62.6 100100 세포 무독성Cell nontoxic
비교제조예8Comparative Production Example 8 1818 2.822.82 1.831.83 3.203.20 4.134.13 3.13.1 100100 세포 무독성Cell nontoxic
비교제조예9Comparative Production Example 9 1818 3.023.02 2.102.10 2.722.72 4.404.40 3.83.8 39.739.7 중간정도
세포독성
Medium
Cytotoxicity
비교제조예10Comparative Production Example 10 1818 2.542.54 1.611.61 2.452.45 2.432.43 4.54.5 16.416.4 중간정도
세포독성
Medium
Cytotoxicity
비교제조예11Comparative Production Example 11 1818 2.912.91 2.902.90 2.642.64 3.163.16 4.24.2 68.568.5 중간정도 세포독성Moderate cytotoxicity
상기 표 4의 물성 측정 결과를 살펴보면, 제조예 1 ~ 9의 경우, 소수성 섬유로 제조된 부직포를 친수성으로 개질되어 빠른 액체 흡수 속도, 반복 흡수에 대한 내구성(내구 흡수도) 및 재젖음성이 우수하면서도 세포 독성이 없음을 확인할 수 있다.이에 반해, 친수성 개질 코팅제를 0.1 중량% 미만으로 사용한 비교제조예 1의 경우, 제조예 1 및 제조예 2와 비교할 때, 친수성 개질 효과가 거의 없어서 흡수 속도, 내구 흡수도 및 재접음성이 매우 좋지 않은 결과를 보였다. 또한, 친수성 개질 코팅제를 3.0 중량% 초과 사용한 비교제조예 2의 경우, 제조예 1 및 제조예 3과 비교할 때, 친수성 증대 효과가 미약하였고, 재젖음성이 너무 높아서 부직포가 오히려 축축하였을 뿐만 아니라, 오히려 세포 독성만 증가하는 결과를 보였다.Looking at the measurement results of the physical properties in Table 4, in the case of Preparation Examples 1 to 9, the nonwoven fabric made of hydrophobic fibers was modified to be hydrophilic, so that the fast liquid absorption rate, durability against repeated absorption (durable absorption), and rewetability were excellent. On the other hand, in the case of Comparative Production Example 1 using less than 0.1% by weight of the hydrophilic modified coating agent, compared with Preparation Examples 1 and 2, there was almost no hydrophilic modification effect, so absorption rate and durability Absorption and refoldability showed very poor results. In addition, in the case of Comparative Production Example 2 in which the hydrophilic modified coating agent was used in excess of 3.0% by weight, the effect of increasing the hydrophilicity was weak, and the rewetability was too high, so that the nonwoven fabric was rather damp. Only the cytotoxicity was increased.
실시예 2의 개질 코팅제를 사용한 제조예 3 및 실시예 4의 개질 코팅제를 사용한 제조예 4의 경우, 제조예 1과 비교할 때, 친수성 개질 측면에서 큰 차이가 없었다. 이에 반해, 비교예 2의 개질 코팅제를 사용한 비교제조예 4의 경우, 제조예 5와 비교할 때, 재젖음성이 크게 감소하는 문제가 있었다.In the case of Preparation Example 3 using the modified coating agent of Example 2 and Preparation Example 4 using the modified coating agent of Example 4, compared to Preparation Example 1, there was no significant difference in terms of hydrophilic modification. On the other hand, in the case of Comparative Production Example 4 using the modified coating agent of Comparative Example 2, there was a problem in that the rewetability was greatly reduced as compared to Production Example 5.
또한, 비교예 3의 개질 코팅제를 사용한 비교제조예 5의 경우, 제조예 6(실시예 4 사용)와 비교할 때, 친수성 향상 효과가 저하된 결과를 보였고, 비교예 4의 개질 코팅제를 사용한 비교제조예 6의 경우, 제조예 1 및 제조예 7(실시예 5 사용)과 비교할 때, 친수성 개질 효과는 우수하나, 독성이 급격하게 증대하는 문제가 있었다.In addition, in the case of Comparative Production Example 5 using the modified coating agent of Comparative Example 3, when compared to Preparation Example 6 (using Example 4), the hydrophilicity improvement effect was decreased, and Comparative Production using the modified coating agent of Comparative Example 4 In the case of Example 6, when compared with Preparation Example 1 and Preparation Example 7 (using Example 5), the hydrophilicity modification effect was excellent, but there was a problem that toxicity rapidly increased.
그리고, 비교예 5의 개질 코팅제를 사용한 비교제조예 7의 경우, 제조예 1 및 제조예 8(실시예 6 사용)과 비교할 때, 흡수 속도, 내구 흡수도 향상 효과가 미비하였다. 또한, 비교예 6의 개질 코팅제를 사용한 비교제조예 8의 경우, 제조예 1 및 제조예 9(실시예 7 사용)과 비교할 때, 흡수 속도는 큰 차이가 없으나, 내구흡수도가 크게 감소하고, 세포 독성도 증가하는 문제가 있었다.And, in the case of Comparative Production Example 7 using the modified coating agent of Comparative Example 5, as compared with Production Examples 1 and 8 (using Example 6), the effect of improving the absorption rate and durability absorption was insufficient. In addition, in the case of Comparative Production Example 8 using the modified coating agent of Comparative Example 6, when compared with Preparation Example 1 and Preparation Example 9 (using Example 7), there was no significant difference in the absorption rate, but the durable water absorption was greatly reduced, There was also a problem of increasing cytotoxicity.
세포 독성이 없는 본 발명(제조예 1 ~ 9)와 달리, 기존 친수성 개질 코팅제인 이소프로필 알코올(비교예 7), 다이에스테르와 프로필렌글리콜 혼합액(비교예 8) 및 CTFA(비교예 9)로 친수성 개질 코팅된 부직포의 경우(비교제조예 9 ~ 11)의 친수성은 우수하나, 세포 독성이 있는 문제가 있음을 확인할 수 있었다.Unlike the present invention without cytotoxicity (Preparation Examples 1 to 9), the existing hydrophilic modified coating agent isopropyl alcohol (Comparative Example 7), diester and propylene glycol mixture (Comparative Example 8) and CTFA (Comparative Example 9) hydrophilic In the case of the modified coated nonwoven fabric (Comparative Preparation Examples 9 to 11), the hydrophilicity was excellent, but it was confirmed that there is a problem of cytotoxicity.
상기 실시예 및 실험예를 통하여, 본 발명의 친수성 개질 코팅제가 소수성을 친수성으로 효율적으로 개질시킴을 확인할 수 있었으며, 세포독성이 없음을 확인할 수 있었다. 이러한, 본 발명의 친수성 개질 코팅제를 이용하여 적용 용도가 제한적이던 산업용 부직포 및/또는 위생용품용 부직포의 적용 용도 범위를 크게 확장시킬 수 있을 것으로 기대된다.Through the above Examples and Experimental Examples, it was confirmed that the hydrophilic modified coating agent of the present invention effectively modified hydrophobicity to hydrophilicity, and it was confirmed that there was no cytotoxicity. Such, by using the hydrophilic modified coating agent of the present invention is expected to be able to greatly expand the application range of the industrial nonwoven fabric and/or the nonwoven fabric for hygiene products, which had limited application uses.
본 발명의 친수성 개질 코팅제를 이용하여 친수성 개질시킨 부직포는 산업용 부직포 및/또는 위생용품용 부직포 등 다양한 피부 친화적이면서 친수성을 요하는 부직포 제품을 제공할 수 있다.The hydrophilic modified nonwoven fabric using the hydrophilic modified coating agent of the present invention can provide a variety of skin-friendly and nonwoven fabric products requiring hydrophilicity, such as industrial nonwoven fabric and/or nonwoven fabric for hygiene products.

Claims (10)

  1. 소듐염, 말레산염, 인산염 및 알코올 에테르계 화합물을 포함하는 것을 특징으로 하는 세포무독성 친수성 개질 코팅제.A non-toxic hydrophilic modified coating agent comprising sodium salt, maleic acid salt, phosphate and alcohol ether-based compounds.
  2. 제1항에 있어서, 상기 소듐염은 옥틸 나트륨 설포숙신산(도큐세이트 소듐), 도데실벤젠설폰산 나트륨, 암모늄 알파-설포-오메가-(노닐페녹시)폴리(옥시-1,2-에탄디일), 설포부탄다이옥산 1,4-비스(2-(C1 ~ C3의 알킬)(C4 ~ C8의 알킬)에스터 나트륨염, 소듐탈로에이트, 소듐코코에이트 및 소듐팜커넬레이트 중에서 선택된 1종 이상을 포함하는 것을 특징으로 하는 세포무독성 친수성 개질 코팅제.The method of claim 1, wherein the sodium salt is octyl sodium sulfosuccinic acid (docusate sodium), sodium dodecylbenzenesulfonate, ammonium alpha-sulfo-omega-(nonylphenoxy)poly(oxy-1,2-ethandiyl) , Sulfobutanedioxane 1,4-bis(2-(C 1 ~ C 3 alkyl) (C 4 ~ C 8 alkyl) ester sodium salt, sodium taloate, sodium cocoate and one selected from sodium palm kernelate Cell non-toxic hydrophilic modified coating comprising the above.
  3. 제1항에 있어서, 상기 말레산염은 비스(2-(C1 ~ C3의 알킬)(C4 ~ C8의 알킬)말레이트, 에틸렌 무수 말레산 공중합체 및 이소부틸렌 무수 말레산 공중합체, 에틸렌 무수 말레산 공중합체 및 이소부틸렌 무수 말레산 공중합체 중에서 선택된 1종 이상을 포함하는 것을 특징으로 하는 세포무독성 친수성 개질 코팅제.The method of claim 1, wherein the maleic acid salt is bis(2-(C 1 ~ C 3 alkyl) (C 4 ~ C 8 alkyl) maleate, ethylene maleic anhydride copolymer, and isobutylene maleic anhydride copolymer. , Cell non-toxic hydrophilic modified coating comprising at least one selected from ethylene maleic anhydride copolymer and isobutylene maleic anhydride copolymer.
  4. 제1항에 있어서, 상기 인산염은 폴리(옥시-1,2-에탄디일), 폴리옥시에틸렌 노닐 페닐 에테르 인산, 폴리옥시에틸렌 노닐 페닐 에테르 인산, 인산 트리스(2-에틸헥실)에스터, (Z)-알파-2-옥타데켄일-오메가-하이드록시폴리(옥시-1,2-에탄딜)인산염 및 폴리(옥시-1,2-에테인디닐), α-도데실-ω-하이드록시-, 포스페이트, 포타슘염{Poly(oxy-1,2-ethanediyl), α-dodecyl-ω-hydroxy-,phosphate, potassium salt} 중에서 선택된 1종 이상을 포함하는 것을 특징으로 하는 세포무독성 친수성 개질 코팅제.The method of claim 1, wherein the phosphate is poly(oxy-1,2-ethanediyl), polyoxyethylene nonyl phenyl ether phosphoric acid, polyoxyethylene nonyl phenyl ether phosphoric acid, phosphoric acid tris(2-ethylhexyl) ester, (Z) -Alpha-2-octadekenyl-omega-hydroxypoly(oxy-1,2-ethanyl)phosphate and poly(oxy-1,2-ethaninyl), α-dodecyl-ω-hydroxy-, phosphate , Potassium salt {Poly(oxy-1,2-ethanediyl), α-dodecyl-ω-hydroxy-,phosphate, potassium salt} Cell non-toxic hydrophilic modified coating comprising at least one selected from.
  5. 제1항에 있어서, 상기 알콜 에테르계 화합물은 디프로필렌 글리콜 모노메틸 에테르, 폴리비닐 에테르, 폴리에틸렌 글리콜 및 알콜 폴리 옥시 에틸렌 에테르 중에서 선택된 1종 이상을 포함하는 것을 특징으로 하는 세포무독성 친수성 개질 코팅제.The method of claim 1, wherein the alcohol ether-based compound comprises at least one selected from dipropylene glycol monomethyl ether, polyvinyl ether, polyethylene glycol, and alcohol polyoxyethylene ether.
  6. 제1항 내지 제5항 중에서 선택된 어느 한 항에 있어서, ASTM D7042 표준 시험(20℃)에 의거하여 측정한 점도가 950 ~ 1,100 mPa.s인 것을 특징으로 하는 세포무독성 친수성 개질 코팅제.The cell-free hydrophilic modified coating agent according to any one of claims 1 to 5, wherein the viscosity measured according to ASTM D7042 standard test (20°C) is 950 to 1,100 mPa·s.
  7. 부직포를 준비하는 1단계;Step 1 of preparing a nonwoven fabric;
    제6항의 세포무독성 친수성 개질 코팅제를 상기 부직포의 일부 또는 전체를 코팅하는 2단계;A second step of coating part or all of the nonwoven fabric with the cell-free hydrophilic modified coating agent of claim 6;
    열처리하여 친수성 개질 코팅제를 부직포에 열적 고정시켜서 부직포를 친수성으로 개질시키는 3단계;를 포함하며,Including; 3 step of thermally fixing the hydrophilic modified coating agent to the non-woven fabric by heat treatment to modify the non-woven fabric to be hydrophilic; and,
    1단계의 부직포는 소수성 섬유를 포함하는 것을 특징으로 하는 세포무독성 부직포의 제조방법.The nonwoven fabric of step 1 is a method of manufacturing a non-woven non-woven fabric, characterized in that it contains hydrophobic fibers.
  8. 소수성 섬유를 포함하는 부직포의 일부 또는 전부가 친수성 부직포로 개질된 부직포로서, As a nonwoven fabric in which part or all of the nonwoven fabric containing hydrophobic fibers is modified with a hydrophilic nonwoven fabric,
    부직포 전체 중량 중 제6항의 세포무독성 친수성 개질 코팅제를 0.1 ~ 3 중량%로 포함하는 것을 특징으로 하는 세포무독성 부직포.Cell non-toxic non-woven fabric, characterized in that it comprises 0.1 to 3% by weight of the cell non-toxic hydrophilic modified coating agent of claim 6 of the total weight of the non-woven fabric.
  9. 제8항에 있어서, 상기 소수성 섬유는 평균직경이 1 μm ~ 50μm인 것을 특징으로 하는 세포무독성 부직포.The non-woven fabric of claim 8, wherein the hydrophobic fibers have an average diameter of 1 μm to 50 μm.
  10. 제8항에 있어서, ISO 10993-5 방법에 의거하여 IC50 측정시, 세포생존율이 70 ~ 100%인 것을 특징으로 하는 세포무독성 부직포.The non-woven fabric according to claim 8, wherein the cell viability is 70 to 100% when IC 50 is measured according to the ISO 10993-5 method.
PCT/KR2020/013971 2019-10-14 2020-10-14 Non-cytotoxic hydrophilic modifying coating agent, non-cytotoxic nonwoven fabric including same, and preparation method therefor WO2021075837A1 (en)

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