KR20150125213A - The method of preparing material of fire retard using natural cotton - Google Patents

The method of preparing material of fire retard using natural cotton Download PDF

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KR20150125213A
KR20150125213A KR1020140052180A KR20140052180A KR20150125213A KR 20150125213 A KR20150125213 A KR 20150125213A KR 1020140052180 A KR1020140052180 A KR 1020140052180A KR 20140052180 A KR20140052180 A KR 20140052180A KR 20150125213 A KR20150125213 A KR 20150125213A
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flame retardant
flame
weight
cotton
agent
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KR1020140052180A
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Korean (ko)
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KR101621368B1 (en
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윤갑호
송운학
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주식회사 코리아코튼
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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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating 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 nitrogen
    • D06M13/402Amides imides, sulfamic acids
    • D06M13/432Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/07Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/50Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
    • D03D15/513Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads heat-resistant or fireproof
    • 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
    • D04H1/02Cotton wool; Wadding
    • 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
    • D06M11/07Treating 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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11Treating 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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/13Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table
    • DTEXTILES; PAPER
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    • 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
    • D06M11/07Treating 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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11Treating 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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/155Halides of elements of Groups 2 or 12 of the Periodic Table
    • 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
    • D06M11/47Oxides or hydroxides of elements of Groups 5 or 15 of the Periodic Table; Vanadates; Niobates; Tantalates; Arsenates; Antimonates; Bismuthates
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    • 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
    • D06M11/73Treating 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 carbon or compounds thereof
    • D06M11/76Treating 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 carbon or compounds thereof with carbon oxides or carbonates
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    • 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
    • D06M13/02Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
    • D06M13/03Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons with unsaturated hydrocarbons, e.g. alkenes, or alkynes
    • D06M13/07Aromatic hydrocarbons
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    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/08Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with halogenated hydrocarbons
    • 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
    • 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
    • D06M13/244Treating 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 sulfur or phosphorus
    • D06M13/248Treating 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 sulfur or phosphorus with compounds containing sulfur
    • D06M13/256Sulfonated compounds esters thereof, e.g. sultones
    • 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
    • D06M13/322Treating 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 nitrogen
    • D06M13/325Amines
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/01Natural vegetable fibres
    • D10B2201/02Cotton
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
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    • D10B2401/00Physical properties
    • D10B2401/04Heat-responsive characteristics

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Fireproofing Substances (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The present invention relates to a method for producing a fire retardant material using a natural cotton wool. Natural cotton wool is dipped in a solution having 3-6 wt% of a reactive flame retardant agent, and temperature of 100-150°C is maintained in a high pressure part, so the natural cotton wool is reacted for 30-40 minutes and the natural cotton wool made to be fire retardant is taken out to be dehydrated and dried. Accordingly, cotton wool firstly made to be fire retardant is obtained. In 4-8 wt% of a solution of a secondary fire retardant composition including an additive fire retardant agent, a solubilizer, a dispersing agent, a mycostat, a water repelling agent, and a silane coupling agent, the cotton wool firstly made to be fire retardant is dipped and agitated at room temperature for 20-30 minutes. Then, a dipped solution is adjusted to be acid or alkali neutral, and cotton wool secondly made to be fire retardant is taken out and dehydrated. Cotton wool dried to have a moisture content of 7% is modified and beaten to be made into a nonwoven fabric shape.

Description

천연 솜을 이용한 난연성 소재의 제조방법 {The method of preparing material of fire retard using natural cotton}BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a flame-

반응성 난연재 수용액에 천연 솜을 침지하여 고압부에 넣고 가온하여 온도 100~150℃로 유지시킨 상태에서 교반하면서 반응시킨 다음 천연 솜을 취출하여 탈수하고 건조시켜 1차 난연화된 솜을 얻고 첨가형난연제, 가용화제, 분산제, 방미제, 발수제, 실란카프링제로 조성되는 2차 난연화 조성물 수용액에 상기 1차 난연화된 솜을 침지하여 상온에서 교반한다음 산 또는 알카리로 수소이온 농도를 중성으로 조절하고 천연 솜을 취출하여 탈수하고 건조하여 2차 난연화된 솜을 얻고 이를 개면 하고 타면 하여 부직포 상태로 한 천연 솜을 이용한 난연성 소재의 제조방법에 관한 것이다.The natural cotton is immersed in an aqueous solution of reactive flame retardant and heated at a temperature of 100 to 150 ° C. The natural cotton is removed, dehydrated and dried to obtain a primary flame retardant cotton, The first flame retarded cotton is immersed in an aqueous solution of a secondary flame retardant composition composed of a topical agent, a dispersant, a antiseptic agent, a water repellent agent, and a silane coupling agent, stirred at room temperature, neutralized with acid or alkali, The present invention relates to a method for producing a flame retardant material using natural cotton which is dewatered and dried to obtain a second flame-retarded cotton, which is then turned into a non-woven fabric.

섬유의 방염 가공의 역사는 4세기 전에 목재를 초산으로 처리하여 난연성을 갖게 하는 것이 경험적으로 알려져 시행되어 왔다.The history of flame-retarding processing of fibers has been empirically known to have flame retardancy by treating wood with acetic acid four centuries ago.

문헌에 나타난 처음의 방염가공은 1735년경 영국의 Wide가 명반과 황산제2철, 붕사의 혼합물로 섬유류를 처리하여 방염가공을 하였다고 기록되어 있다.The first flame-retarding process in the literature was recorded around 1735, when the Wide of England treated flour with a mixture of alum, ferric sulfate and borax, and flame-retarded.

1821년에 이르러 프랑스의 유명한 Gay-Lussicc가 아마 및 황마의 방염가공에 많은 염의 종류를 이용해 본 다음 그 중에서 인산암모늄, 염화암모늄, 붕사와 붕산의 혼합물을 사용하면 난연효과가 있음을 발견하였고, 이어서 영국의 Vermann과 Oppenheim도 약 40개의 화합물을 섬유의 방염가공에 적용한 결과 인산암모늄과 염화암모늄의 혼합물이 효과가 있다고 문헌에 보고하였다.In 1821, the famous Frenchman, Gay-Lussicc, discovered that flame-retardant effect was obtained by using many kinds of salts in the flame retarding process of flax and jute, and then using a mixture of ammonium phosphate, ammonium chloride, borax and boric acid among them. Vermann and Oppenheim in the UK have also reported in the literature that a mixture of ammonium phosphate and ammonium chloride is effective when about 40 compounds are applied to the flame retarding treatment of the fibers.

또 프랑스의 King 및 Florentine은 붕사와 붕산의 혼합물이 효과가 있다고 발표하였고 이 혼합물은 지금도 사용되고 있는 경우가 있다.King and Florentine of France also announced that a mixture of borax and boric acid is effective, and this mixture is still in use today.

가일층 진보하여 세탁에 견디는 방염가공을 최초로 성공시킨 것은 1912년에 Perkin의 연구결과도 있다.Perkin's research in 1912 was also the first to succeed in flame-retardant processing, which progresses even further by washing.

그는 섬유 내부에 산화주석의 침전을 형성시키는 방법에 의해 불꽃 중에 노출된 섬유가 불에 잘 견디는 방법을 연구해 냈다.He studied how flame-resistant fibers can withstand exposure to flame by forming a precipitate of tin oxide inside the fiber.

근년에는 합성섬유사들의 등장과 함께 고분자재료에 할로겐, 인, 질소 그리고 수산화금속화합물등 난연성 부여 효과가 큰 화합물을 첨가함으로써 발화를 늦춰주고 연소의 확대를 막아주는 물질이라고 설명하고 있으며 최근에 선진국에서는 난연효과가 우수한 수많은 난연제가 개발되어 전기, 전기기기, 자동차, 건축용 재료, 선박, 항공기, 전선분야 및 그 밖의 제품분야에 널리 이용되고 있으나 우리나라에서는 난연제의 개발이나 난연제를 이용한 제품 개발이 활발하지 못한 실정이다. 본 발명에서 난연화를 시도하는 천연 솜은 예로부터 우리 생활 주변에 흔히 사용되는 섬유로서 의류를 비롯한 이브자리등의 보온재로서 셀루로스 섬유가 대부분이고 소량의 지방, 전분, 리그닌 성분으로 구성되어 있으며 셀루로스 섬유의 조직은 수많은 증공(lumen)이 이루어져 꼬임을 하고 있어 열의 전도를 막는 우수한 단열, 보온 및 흡음기능을 보유하고 있는 섬유로 알려져 있다.In recent years, with the emergence of synthetic fiber yarn, halogen-containing compounds such as halogens, phosphorus, nitrogen, and metal hydroxide compounds have been added to polymer materials to slow the ignition and prevent the expansion of combustion. Many flame retardants with excellent flame retarding effect have been developed and widely used in electric, electric appliances, automobiles, building materials, ships, aircraft, electric wires and other products. However, in Korea, development of flame retardants and development of products using flame retardants It is true. In the present invention, the natural cotton which is tried to soften the flame is a fiber commonly used in the living environment of the past, such as clothing, etc., and most of the cellulose fibers are composed of a small amount of fat, starch and lignin, The structure of the fiber is known as a fiber having excellent heat insulation, heat insulation and sound absorbing function to prevent heat conduction due to a lot of lumens formed and twisted.

함으로써 면 솜은 다른 대부분의 단열재보다 보온, 단열 및 흡음성이 우수할 뿐 아니라 유해성분이 없고 환경공해를 발생시키지 않는 섬유라 할 수 있다. 그러나 난연솜은 난연 및 방염성이 약하고 흡습성이 있으며 곰팡이나 세균의 번식이 용이할 뿐 아니라 부피가 크고 지지력이 부족한 결점 때문에 지금까지 의류나 이브자리용도의 범주를 벗어나지 못하고 있다.As a result, cotton wool is superior to most other thermal insulation materials in terms of heat insulation, insulation and sound absorption, as well as being free of harmful substances and not causing environmental pollution. However, flame retardant cotton has low flame retardancy and flame retardancy, is hygroscopic, is easy to reproduce mold and germs, and is bulky and lacks bearing capacity.

본 발명은 천연 솜의 우수한 단열, 보온, 방음 기능을 살리면서 취약점을 개선 보완하고 특히 난연성 및 방염성을 극대화하여 산업분야의 이용도를 높임에 목적이 있다 하겠다.The present invention aims at enhancing and improving the vulnerability of natural cotton by utilizing the excellent heat insulation, heat insulation and soundproofing function, and maximizing the flame retardancy and flame resistance, thereby improving the utilization of the industrial field.

본 발명에서 시도하고 있는 관련기술분야에 속하는 섬유소재로서 단열 보온 기능을 가지면서 난연성을 갖는 종래의 섬유소재를 알아보면 유리섬유, 암면, 그라스울, 셀라쿨 등을 난연성 단열재 및 보온재로 많이 사용하여 왔으나 석면은 인체에 대한 유해성 때문에 상용이 금지되고 있으며, 유리섬유, 그라스울 등은 쉽게 소편이나 분말이 되어 비산하게 됨으로써 피부병을 유발시킴으로써 산업용을 제외한 주택용등 일부를 규제하고 있고 환경 측면에서 사용을 기피하고 있어 현재에는 그 수요가 점점 줄어들고 있는 실정이다.As a fiber material belonging to the related art attempted in the present invention, fiberglass, rock wool, glass wool, and celluloid have been frequently used as a flame retardant insulation material and a thermal insulation material when a conventional fiber material having a heat insulating and warming function and having flame retardancy is examined Asbestos is banned from commercial use because of its harmful effects on the human body. Glass fibers and glass wool are scattered easily as small pieces or powder, thereby causing skin diseases, thus regulating some parts such as residential use except for industrial use. Nowadays, the demand is getting smaller.

또한, 합성수지섬유소재로서 난연성의 아라미트섬유, 노맥스 섬유등이 있으나 350℃를 초과하는 경우에는 연화되거나 용융되어 본래의 형태를 유지하지 못함으로써 본래의 난연 및 방염기능을 발휘하지 못하고 사용범위가 한정되어 있고 고가이며 환경오염을 발생시키는 문제점을 안고 있다.In addition, flame retardant aramid fibers and Normax fibers are used as synthetic resin fiber materials. However, when they exceed 350 ° C, they are not softened or melted and can not maintain their original shape, It is limited, expensive, and has problems causing environmental pollution.

또한, 비교적 융점이 높은 폴리에터, 폴리아미드 및 아크릴수지의 중합시에 난연제를 첨가하거나 수지자체에 난연제를 첨가하여 용융방사시켜 얻어진 난연성 합성수지 섬유사들이 있으나 우선 고가이어서 경쟁력이 없고 300℃ 이상에서는 연화되거나 용융되어 단열, 보온, 흡음기능이 상실되고 화재시는 유해가스등을 발생하며 사용이 끝나면 환경공해를 유발시키는 문제점을 갖고 있다. 그 밖에도 섬유소재는 아니지만 기능성의 측면에서 유사한 스티로폼, 폴리우레탄 발포체 그밖에 열가소성합성수지 발포체들도 단열, 보온 및 흡음 기능이 우수하여 단열, 보온 및 방음재들로 널리 사용하고 있으나 스티로폼발포체는 80℃에서 연화되기 시작하고 온도가 더욱 상승하면 용융되어 본래의 형태가 허물어지게 되고 100~120℃에서는 용융액으로 되어 발포성형체 형태는 사라지게 되며 소량의 용융체만 남게 된다.Further, there are flame retardant synthetic fiber fiber yarns obtained by adding a flame retardant agent to a polyurethane, polyamide and acrylic resin having a relatively high melting point, or by adding a flame retardant agent to a resin material and melt spinning. However, It is softened or melted to lose heat insulation, heat insulation, and sound absorption function, generates harmful gas at the time of fire, and causes environmental pollution when it is used. Styrofoam, polyurethane foam and other thermoplastic synthetic resin foams are also widely used as insulation, heat insulation and soundproofing materials because they are excellent in heat insulation, insulation and sound absorbing properties, but styrofoam foam is softened at 80 ° C. When the temperature is further elevated, it melts and the original shape is broken down. At 100-120 ° C, the melt becomes a melt, the foamed mold shape disappears, and only a small amount of the melt remains.

본 발명은 천연 솜 본래의 취약점인 물성보완과 함께 특히 난연성을 극대화 함으로써 종래 난연성 소재 및 이 소재를 이용한 2차 제품의 문제점을 해결할 수 있을 뿐만 아니라 고열용 관체보온재, 반응조보온재, 열차단재, 흡음재등 그 이용도를 높일 수 있는 섬유소재를 제조함에 목적이 있다.The present invention can solve the problems of the conventional flame retardant materials and the secondary products using the flame retardant materials by maximizing the flame retardancy as well as the physical properties of natural wool, which are inherent weaknesses of the natural cotton, and also can be used as a high temperature thermal insulation material for a bath, a reactor heat insulation material, And a fiber material capable of increasing its utilization.

본 발명은 천연 솜의 우수한 단열, 보온 및 방음성을 살려 천연 솜의 취약점인 물성은 물론 난연성(방염성) 극대화함으로써 종래 단순히 의류 및 이브자리용의 범주를 벗어나 단열, 보온 및 방음기능이 요구되는 건축자재를 비롯한 다양한 2차 가공제품으로의 이용도를 높일 수 있는 천연 솜 섬유소재를 제조함에 목적이 있다.The present invention maximizes the flame retardancy (flame retardancy) as well as the physical properties which are the weak point of the natural cotton by utilizing the excellent heat insulation, the warmth and the soundproofing property of the natural cotton, so that the building material, And to improve the usability of a variety of secondary processed products such as cotton.

천연면솜과 반응성 난연제의 수용액을 고압부에 채우고 승온시켜 온도 100℃~150℃로 유지시킨 상태에서 30~40분간 반응시킨 후 1차 난연화된 솜을 취출하여 탈수하고 건조시켜 1차 난연화된 솜을 얻고 첨가형 난연제, 가용화제, 분산제, 방미제, 발수제, 실란가프링제로 조성된 2차 난연화조성물의 수용액에 상기 1차 난연화된 솜을 침지하여 상온에서 20~30분간 교반한 다음 침지처리액을 산 또는 알카리로 수소이온농도를 PH6~7로 조절하고 2차 난연화된 솜을 취출하여 탈수하고 건조시킨 2차 난연화된 솜을 개면 하고 타면 하여 카딩기로 적층하여 부직포 상태로 한 천연 솜을 이용한 난연성 소재의 제조방법을 제공함으로써 본 발명의 목적을 달성할 수 있었다.After the reaction was carried out for 30 to 40 minutes with the temperature of 100 ° C to 150 ° C being maintained at a high pressure, an aqueous solution of natural cottonseed flame retardant and reactive flame retardant was filled in the high pressure part, and the first flame retarded cotton was taken out, dehydrated and dried, And the primary flame retarded cotton was immersed in an aqueous solution of a secondary flame retardant composition composed of an additive type flame retardant, a solubilizing agent, a dispersant, a antiseptic agent, a water repellent agent and a silane gel finishing agent, stirred at room temperature for 20 to 30 minutes, The pH of the solution is adjusted to PH6 ~ 7 with acid or alkali, the second flame retarded cotton is taken out, dehydrated and dried, and the second flame retarded cotton is laid face to face with the carding machine to form a natural cotton The object of the present invention can be achieved.

본 발명에 의하여 제조된 난연성 소재는 제조과정을 통하여 내흡수성의 향상 및 지지력 보강을 비롯하여 난연성을 극대화함으로써 천연 솜의 취약물성을 크게 개선한데다 천연 솜 고유의 물성인 가볍고 공해성이 없으며 특히 우수한 보온성 단열성 및 방음성을 지니고 있어 건축자재를 비롯한 산업용 자재로 이용도를 높일 수 있는 소재라 할 수 있다.The flame retardant material produced by the present invention has improved flame retardancy by improving the resistance to water absorption and supporting ability through the manufacturing process, and it has greatly improved the vulnerable physical properties of natural cotton. Also, it has no inherent physical properties such as natural cotton, And soundproofing, it can be used as a material for industrial materials including building materials.

본 발명은 천연 솜의 우수한 보온성, 단열성 및 흡음성을 살려 천연 솜의 취약한 물성의 개선과 함께 난연성과 방염 성을 극대화함으로써 단열, 보온 및 방음 기능이 요구되는 건축자재를 비롯한 다양한 2차 제품으로의 이용도를 크게 높일 수 있는 난연성 천연 솜 섬유소재를 제조함에 있으며 이의 제조방법은 공정별로 구체적으로 설명하기로 한다.The present invention utilizes natural cotton as a secondary product including a building material which requires heat insulation, heat insulation and soundproofing function by maximizing flame retardancy and flame resistance by utilizing the excellent thermal insulation, heat insulation and sound absorption property of natural cotton, A flame-retardant natural cotton fiber material capable of greatly increasing the degree of flame retardancy is produced. The production method thereof will be described in detail by process.

(1) 천연 솜(원료)(1) Natural cotton (raw material)

본 발명에서 천연 솜이라 함은 목화로부터 직접 채취한 솜을 탈지하고 개면 하여 타면 한 솜, 수명이 다하거나 오염되어 폐기된 솜을 정선하여 세척하고 건조시킨 솜을 개면기로 개면 하고 타면한 솜, 폐기된 면직물을 정선하여 세척하고 건조시켜 소편으로 절단하여 해섬하고 개면하여 타면한 솜 모두를 천연 솜이라 하며 수분함량 5% 이내의 천연 솜이다.In the present invention, natural cotton wool means cotton wool which is directly taken from cotton, is degreased, cotton wool is washed away, cotton wool is dirty or contaminated, wool cotton wool is selected and washed, dried wool cotton wool is opened, The selected cotton fabric is selected, washed, dried, cut into small pieces, fibrillated, and all cotton is called natural cotton, and it is natural cotton with a moisture content of 5% or less.

(2) 천연 솜을 이용한 난연성 소재의 제조방법(2) Manufacturing method of flame retardant material using natural cotton

요소-인산염계 화합물, 염화파라핀과 삼산화안디몬, 히드록시 메틸화 포스포노 카르복시 아미드, 테트라 크로르 무수푸탈산, 인을 함유하는 에스텔 중에서 선택되는 하나 이상의 반응성 난연제 3~6중량%의 수용액과 수용액중량의 1/3에 해당하는 수분 함량 5% 이하의 천연 솜을 고압반응부내에 채워 넣고 서서히 가온하여 온도 100℃~150℃로 유지시킨 상태에서 30~40분간 교반하면서 반응시킨 다음 천연 솜을 취출하여 수분함량 50%로 탈수시킨 상태에서 수분함량 5% 이하로 건조시킨 1차 난연화된 솜을 제조하는 1단계공정.An aqueous solution of 3 to 6% by weight of at least one reactive flame retardant selected from urea-phosphate-based compounds, chlorinated paraffin and anthocyanide trioxide, hydroxymethylated phosphonocarboxamide, tetrachlorosuccinic anhydride, And the water content of 5% or less is filled in the high-pressure reaction part, and the mixture is gradually heated. While maintaining the temperature at 100 ° C to 150 ° C, the reaction is carried out with stirring for 30 to 40 minutes. A one-step process to produce a primary flame-retarded cotton that has been dried to a water content of 5% or less under dehydration to a water content of 50%.

황산암몬, 염화암몬, 염화마그네슘, 황산알루미늄, 인산암몬, 붕산 중에서 선택되는 하나 이상의 첨가형 난연제 72~85중량%, 토루엔슬폰산염, 크시렌슬폰산소다, 에틸알콜, 프로피렌 클리콜 중에서 선택되는 하나 이상의 가용화제 7~10중량%, 알킬나프텐슬폰산염, 폴리에티렌글리콜, 아민류, 중합인산염, 계면 활성제 중에서 선택되는 하나 이상의 분산제 5~7중량%, 8옥시퀴노린, 도데실 디메틸렌 벤질암모늄클로라이드, 나프텐산등 트리클롤칼바니리드, 나프텐산 아연 중에서 선택되는 하나 이상의 방미제 3~5중량%, 발수제로서 염화파라핀 2~3중량%, 실란카프링제 1~2중량%로 조성된 2차 난연화 조성물을 조성하는 2단계공정.72 to 85% by weight of at least one additive type flame retardant selected from the group consisting of ammonium sulfate, ammonium chloride, magnesium chloride, aluminum sulfate, ammonium phosphate, and boric acid, toluene sulfonate, xylene sulfonated oxygen, ethyl alcohol and propylene glycol 7 to 10% by weight of at least one solubilizing agent, 5 to 7% by weight of at least one dispersing agent selected from alkylnaphthenene sulfonates, polyethyleneglycol, amines, polymeric phosphates and surfactants, 8-oxyquinoline, dodecyldimethylbenzyl 3 to 5% by weight of at least one antimicrobial agent selected from trichloroalkanilide and zinc naphthenate such as ammonium chloride and naphthenic acid, 2 to 3% by weight of paraffin chloride as a water repellent agent and 1 to 2% by weight of silane coupling agent A two-step process to form an embrittling composition.

2차 난연화 조성물 4~8중량%의 수용액에 수용액중량의 1/3에 해당하는 1차 난연화된 천연 솜을 침지하여 20~30분간 교반하고 PH를 6~7의 범위로 산 또는 알카리로 조절한 다음 2차 난연화된 솜을 취출하여 수분함량 70%로 탈수한 상태에서 수분함량 7%로 건조시킨 2차 난연화된 솜을 제조하는 3단계공정.The primary flame retarded natural cotton, which corresponds to 1/3 of the weight of the aqueous solution, is immersed in an aqueous solution of 4 to 8 wt% of the secondary flame retardant composition and agitated for 20 to 30 minutes, and the pH is adjusted to 6-7 by acid or alkali A three-step process to prepare a second flame-retarded cotton that has been dried to a water content of 7% under dehydration to a moisture content of 70% by removing the second flame-retarded cotton.

2차난연화된 천연 솜을 개면하고 타면하여 부직포형태로 하는 4단계 공정을 포함하는 천연 솜을 이용한 난연성 소재의 제조방법에 관한 것이다.The present invention relates to a method for producing a flame-retardant material using a natural cotton, which comprises a four-step process of forming a non-woven fabric by rubbing a two-layer soft cotton natural cotton.

이상의 제조방법에서 반응성 난연제는 섬유소와 반응을 하는 인산화 셀루로즈를 만들어 방염성을 천연 솜에 부여하는 경우로서 본 발명 제조방법 1단계공정에서 사용되는 요소-인산염계 화합물로 달성할 수 있으며 염화파라핀과 삼산화안티몬은 섬유소와 반응하여 섬유소를 염소화세루로즈로 되게 함으로써 천연 솜에 난연성을 부여하게 되며 그 밖의 반응성 난연제 또한 섬유소와 복잡한 반응을 거쳐 섬유소를 난연화 시키는 반응성 난연제들이다.In the above production process, the reactive flame retardant is a phosphorus-containing cellulose which reacts with cellulose to give flame retardancy to the natural cotton, which can be achieved with the urea-phosphate compound used in the first step of the present invention, Antimony reacts with fibrin to make fibrinous chlorosulfuric acid, which gives flame retardancy to natural cotton. Other reactive flame retardants are reactive flame retardants which also soften fibrils through complex reactions with fibrin.

이와 같이 반응성 난연제에 의하여 난연화된 천연 솜은 세탁이나 물의 접촉에도 견디는 영구적인 방염가공의 하나라 할 수 있다.As such, natural flame-retarded natural cotton by reactive flame retardant is one of the permanent flame retarding processes that can withstand washing or water contact.

또한, 상기 제조방법 2단계공정에서 2차난연화조성물로 사용되는 첨가형 난연제는 반응성 난연제와는 달리 천연 솜의 조직내에 난연액의 침투에 의한 침착, 코팅, 접착에 의한 물리적인 메커니즘에 의해 섬유소에 난연 또는 방염기능을 부여하는 첨가형 난연제로서 이와 같은 난연제는 반응성 난연제와는 달리 일반적으로 난연화된 솜을 물과 접촉시키면 다시 용해되는 경향이 있고 진한 농도의 난연용액으로 처리하여 건조시킨 천연 솜은 건조시 표면에 결정을 석출하는 경향이 있다. In addition, unlike the reactive flame retardant, the additive type flame retardant used as the second flame retardant composition in the second step of the above-described manufacturing method is a flame retardant agent for flameproofing due to the physical mechanism by deposition, coating, Or flame retarding function. Unlike reactive flame retardants, such flame retardants generally tend to dissolve when the flame retarded cotton is contacted with water. The natural cotton, which is dried by treating with a flame retardant solution of a high concentration, There is a tendency to deposit crystals on the surface.

본 발명에서 사용된 첨가형 난연제들의 특징을 알아보면 황산암모늄은 무색투명하고 비중 1.76이며 사방정계 결정 또는 입상형 결정으로 물에 대한 용해도는 0℃에서 물 100중량부에 대하여 70.6중량부, 100℃에서 물 100중량부에 대하여 103.3 중량부가 용해되므로 물에 대한 용해도가 아주 높으나 에틸알콜, 아세톤에는 불용성이다.Amorphous ammonium sulfate is colorless and transparent and has a specific gravity of 1.76, which is an orthorhombic crystal or granular crystal. Its solubility in water is 70.6 parts by weight based on 100 parts by weight of water at 0 ° C, 103.3 parts by weight are dissolved in 100 parts by weight of water, so that the solubility in water is very high but insoluble in ethyl alcohol and acetone.

많은 양을 물에 첨가하면 난연화된 천연 솜이 건조되면 결정이 석출하여 솜으로부터 탈리되는 방화제의 기능을 갖는 첨가형 난연제이다.It is an additive type flame retardant that has the function of an embrittlement agent in which crystals precipitate and desorb from the cotton when the softened natural cotton is dried when a large amount is added to water.

염화암몬은 백색의 결정으로서 1g을 물 3g에 용해시키면 포화용액이되며 시간이 경과하면 암모니아가 희산 함으로써 중성에서 산성으로 변하며 알콜, 글리세린에는 용해되나 아세톤과 에텔에는 불용으로 이 난연제 역시 과량을 사용하면 천연 솜의 건조시에 결정이 석출하여 탈리되며 승화승이 있어 시간이 경과 할수록 난연기능이 저감되는 첨가형 난연제라 할 수 있다.Ammonium chloride is a white crystal, dissolved in 3 g of water, and becomes a saturated solution. Ammonia is refined by neutralization with time. It changes from neutral to acid. It dissolves in alcohol and glycerin but insoluble in acetone and ether. The additive type flame retardant can be said to be a additive type flame retardant in which the flame retarding function is reduced with the lapse of time since the crystal is precipitated and desorbed when the natural cotton is dried.

염화마그네슘은 무색조해성의 단사정, 비중 2.2이고 20℃의 용해도는 31.14g/100g(물)으로 물에 잘 녹으며 가열하면 무수물로 되지않고 가수분해하여 약 200℃에서 염화수소를 발생하고 옥시염화물로되며 600℃에서는 마그네시아로 되며 방화제의 기능을 가지면서 천연 솜의 방부기능도 동시에 갖는 첨가형 난연제이다.Magnesium chloride is colorless and has a specific gravity of 2.2 and its solubility at 20 ℃ is 31.14g / 100g (water). It dissolves well in water. When heated, it does not become an anhydrous but hydrolyzes to produce hydrogen chloride at about 200 ℃. And at 600 ° C, it is a magnesia, which is an additive type flame retardant having the function of a fire retardant and also the function of preserving natural cotton.

황산알미늄은 순수한 것은 18수가물과 무수물이 있으면 18수가물은 무색결정으로 비중 1.69, 융점 86.5℃ 물, 산, 알카리에서 가용 알콜에 불용이고 무수물은 비중 2.71로서 770℃에서 분해되어 소화 기능을 상실하게 되는 첨가형 난연제이다.It is colorless crystals of 18 water and anhydrous substance. 18 Water is colorless crystal. Specific gravity is 1.69, melting point is 86.5 ℃. It is insoluble in soluble alcohol in water, acid and alkali. Anhydride has specific gravity of 2.71 and decomposed at 770 ℃ to lose digestion function. Based flame retardant.

인산암몬은 백색의 결정 또는 분말로서 물에 쉽게 녹고 불연성의 물질로서 목재, 종이, 섬유에 난연 효과가 큰 방화성 난연제이다.Ammonium Phosphate is a white crystal or powder that easily dissolves in water and is a nonflammable material and has an excellent flame retardant effect on wood, paper and fiber.

붕산은 물, 알콜에 가용, 에텔 및 벤젠에 불이용이며 방화제, 방부제, 살충제의 기능을 갖는 난연제이다. 또한 2차 난연제 조성물에 첨가되는 가용화제는 2차 난연제 조성물중에서 물에 쉽게 녹지않는 조성물을 용해하며 물에 용해하는 조성물이라 하더라도 용해도를 높히는 작용을 하는 물질이다.Boric acid is a flame retardant that is used in water, alcohol, and ether and benzene, and has the function of fire retardant, preservative and insecticide. Further, the solubilizer added to the secondary flame retardant composition dissolves a composition that is not readily soluble in water in the secondary flame retardant composition, and is a substance that acts to increase the solubility even when it is dissolved in water.

분산제는 2차 조성물 중에서 물에 녹지 않는 조성물을 액중에 고르게 분산시켜 균질성의 조성액을 만들고 조성액의 침투성을 높임으로써 난연효과를 향상시킬 수 있다.The dispersing agent can improve the flame retarding effect by dispersing the water-insoluble composition evenly in the secondary composition to make a homogenous composition liquid and to increase permeability of the composition liquid.

발수제의 사용은 천연 솜의 흡성성을 방지하므로서 천연 솜에 침착, 코팅 또는 접착되어 있는 첨가형 난연제의 용해를 방지함과 동시에 천연 솜의 보온, 단열 기능의 저감을 방지함에 목적이 있다.The use of the water repellent agent is intended to prevent dissolution of the additive type flame retardant which is deposited, coated or adhered to the natural cotton by preventing the absorption of the natural cotton, and at the same time, prevents the natural cotton from deteriorating the thermal insulation and the heat insulating function.

또한 실란카프링제는 아미노기, 에폭시기, 이중결합등의 관능기를 가지고 있으며 유기질재료와 무기질재료, 유기질재료와 유기질재료를 강력하게 결합시키는 카프링제로서 유효하며 지지력이 없는 천연 솜에 강도를 부여하므로서 스티프니스(stilfness)성을 갖게하며 천연 솜과 2차 난연화 조성물과의 접착력을 향상시킨다. 그리고 방미제는 천연 솜의 부패를 방지하고 곰팡이나 세균의 서식을 방지하며 살균 또는 정균 작용을 가지는 약제라 할 수 있다. 그밖에 PH 조정제로서 산은 초산을 사용하고 PH 조절제로 알카리는 탄산소다를 사용함이 솜이나 처리제에 무리가 없다. 이상의 방법으로 제조된 난연화된 천연 솜은 보온, 단열 및 흡음 기능이 있어서는 미미한 손실이 있지만, 난연성 및 방염성은 난연화된 열가소성수지의 합성섬유에 비하여 상회하고 있으며 흡습성의 감소와 스티프니스성이 보강된 난연성 소재를 얻을 수 있다. 이와 같은 천연 솜으로 된 난연성소재는 아주 가볍고, 공해성이 없는 잇점이 있으며 난연화된 천연삼 섬유 또는 야자피섬유와 혼합하여 지지력을 보강하거나 소량의 난연화된 합성섬유와 혼합하여 열성형성을 갖게 하므로서 지지력을 보강하여 벽체, 천정재 등의 건축자재를 비롯 고온의 열관, 고온의 반응조 등 산업용자재로 널리 이용할 수 있는 소재라 할 수 있다.The silane coupling agent has functional groups such as an amino group, an epoxy group and a double bond and is effective as a capping agent which strongly bonds an organic material, an inorganic material, an organic material and an organic material, and imparts strength to a natural cotton having no supporting force, stilfness and improves the adhesion between the natural cotton and the secondary flame retardant composition. Antimicrobial agents are drugs that prevent the decay of natural cotton, inhibit the growth of fungi and bacteria, and have a bactericidal or bacteriostatic action. In addition, acetic acid is used as a PH regulator, PH is used as a pH regulator, and alkali carbonate is used as a pH regulator. The flame retardancy and flame retardancy of the flame retardant natural cotton wool produced by the above method is slightly higher than that of the synthetic fiber of the flame retardant thermoplastic resin. However, the flame retardancy and the flame retardancy are superior to the synthetic fibers of the flame retardant thermoplastic resin. A flame retardant material can be obtained. Such a natural cotton flame retardant material has the advantage of being lightweight and non-polluting, and it can be mixed with natural flour or coconut fiber to strengthen it or to mix it with a small amount of flame retarded synthetic fiber , It can be widely used as industrial materials such as building materials such as walls and ceiling materials, high-temperature heat pipes, and high-temperature reactors.

상기 발명의 기술구성을 구체화하고 효과를 알아보기 위하여 실시예를 들기로 한다.The embodiments of the present invention will be described in order to illustrate the effect of the present invention.

본 발명 1단계 공정에서 반응온도에 따라 반응 수율이 크게 영향을 받으므로 각각 다른 조건의 반응온도로 1차 난연화 시키는 실시예를 들기로 한다.The reaction yield is largely influenced by the reaction temperature in the first step of the present invention. Therefore, the first embodiment will be described.

실시예(1)Example (1)

요소-인산염계화합물, 염소화파라핀-삼산화안티몬을 각각 2.5중량%씩 5중량%의 수용액을 고압부에 주입시킨다음 수용액 중량의 1/3에 해당하는 천연 솜을 투입하여 온도 120~130℃의 온도를 유지하여 40분간 교반하여 반응시킨 다음 난연화된 천연 솜을 수분함량 50%로 탈수 한 다음 건조하여 수분함량 5%의 난연화된 솜을 제조하였다.A 5 wt% aqueous solution of 2.5 wt% each of urea-phosphate compound and chlorinated paraffin-antimony trioxide was injected into the high-pressure part, and natural cotton at a weight corresponding to 1/3 of the weight of the aqueous solution was added thereto. And the mixture was stirred for 40 minutes. The reaction mixture was dehydrated to a water content of 50% and then dried to prepare an egg-softened cotton having a moisture content of 5%.

비교실시예(2)Comparative Example (2)

실시예(1)과 동일한 방법으로 1차공정의 난연화된 솜을 제조하되 온도조건을 70~80℃ 범위로 달리하여 난연화 솜을 얻었다.The flame retarded cotton of the first step was prepared in the same manner as in Example (1) except that the temperature was changed to 70 to 80 ° C to obtain the flame retarded cotton.

비교실시예(3)Comparative Example (3)

실시예(1)로 동일한 방법으로 1차 공정의 난연화된 솜을 제조하되 온도조건을 25~30℃ 범위로 달리하여 난연화 솜을 얻었다.The flame retarded cotton of the first step was prepared in the same manner as in Example (1) except that the temperature was changed in the range of 25 to 30 ° C to obtain the flame retarded cotton.

상기 실시예(1)의 고압부에 남은 수용액과 탈수 수용액의 혼합액(A), 비교실시예(2)의 고압부에 남은 수용액과 탈수수용액의 혼합액(B), 비교실시예(3)의 고압부의 잔액과 탈수수용액의 혼합액(C)을 각각 채취하여 각각의 농도를 측정한 결과 다음과 같은 표1을 얻었다.(B) of the aqueous solution and the dehydrated aqueous solution remaining in the high-pressure portion of the comparative example (2), the balance of the high-pressure part of the comparative example (3), the mixed solution of the aqueous solution and the dehydrated aqueous solution remaining in the high- And a dehydrated aqueous solution (C) were respectively sampled and their concentrations were measured. As a result, the following Table 1 was obtained.

혼합액 A,B,C의 농도 측정 결과표 Concentration measurement result of mixed solution A, B, C 구분\항목Category \ Item 농도density 반응전 농도Concentration before reaction 반응후 농도Concentration after reaction 감소농도율(%)Decrease concentration ratio (%) 혼합액(A)
실시예(1)
The mixed solution (A)
Example (1)
5중량%의 수용액5% by weight aqueous solution 1.8중량%수용액1.8 wt% aqueous solution 64%64%
혼합액(B)
실시예(2)
The mixed liquid (B)
Example (2)
5중량%의 수용액5% by weight aqueous solution 3.3중량%수용액3.3 wt% aqueous solution 32%32%
혼합액(C)
실시예(3)
The mixture liquid (C)
Example (3)
5중량%의 수용액5% by weight aqueous solution 4.1중량%수용액4.1 wt% aqueous solution 18%18%

이상의 표 1에서 1단계 공정의 1차난연화 반응결과로 감소농도율(%)에 나타난 바와 같이 저온에서는 반응이 미미하고 승온될수록 반응이 활발함을 알 수 있고 온도 150℃ 이상에서는 반응시간을 연장시켜도 감소농도율(%)이 미미하게 증가하므로 효율적인 방법이라 할 수 없다.As can be seen from the results of the first softening reaction in Table 1 above, as shown by the decreasing concentration ratio (%), the reaction is small at low temperature and the reaction becomes active as the temperature is raised. The reduction concentration ratio (%) is increased to an insignificant extent, which is not an efficient method.

또한 2단계 공정에서 조성한 2차 난연화조성물에 물을 첨가하여 얻어진 수용액에 1차 난연화된 천연 솜을 침지하여 2차난연화하는 방법에서는 침투침적, 코팅, 접착등의 메카니즘에 의하여 난연화되므로서 온도의 영향은 없고 첨가형 난연재 이외의 조성물 첨가 여부에 따라 감소농도율(%)의 영향이 크므로 그 영향을 알아보기 위해 실시예를 들기로 한다.In addition, since the secondarily softened natural cotton is immersed in an aqueous solution obtained by adding water to the secondarily flameproofed composition prepared in the second step process, the second natural softened cotton is flame retarded by a mechanism such as penetration deposition, coating and adhesion, The influence of temperature is not influenced, and the influence of the decrease concentration ratio (%) on the addition of the composition other than the additive type flame retardant is large, so that the effect will be described.

실시예(4)Example (4)

염화암몬 및 염화마그네슘 각각 40중량%씩 첨가형 난연제80중량%, 가용화제로 토루엔 슬폰산염 8중량%, 아민류 6중량%, 8옥시퀴노린, 나프텐산을 동량으로 혼합한 방미제 3중량%, 염화파라핀 2중량%, 실란카프링제 1중량%로 조성된 2차 난연제 조성물 6중량%의 수용액에 수용액 중량의 1/3에 해당하는 1차 난연화된 천연 솜을 침지하여 30분간 교반 한다음 PH 6.5로 조절하고 솜을 취출하여 수분함량 70중량%로 탈수한 상태로 수분함량7%로 건조시켜 2차 난연화된 천연 솜(난연성소재)을 개면하고 타면해서 카딩기로 적층하여 부직포로 한 난연성 소재를 제조하였다.Ammonium chloride and magnesium chloride were added in an amount of 40 wt% each, 80 wt% of a flame retardant of addition type, 8 wt% of a toluenesulfonate as a solubilizer, 6 wt% of amines, 3 wt% of a flavoring agent containing an equal amount of 8-oxyquinoline and naphthenic acid, The flame retardant natural cotton, which is 1/3 of the weight of the aqueous solution, is immersed in an aqueous solution of 6% by weight of the secondary flame retardant composition composed of 2% by weight of paraffin and 1% by weight of silane coupling agent and stirred for 30 minutes. And the cotton was taken out and dried to a water content of 7% in a dehydrated state with a moisture content of 70% by weight to form a second flame retarded natural cotton (flame retardant material), which was laid by a carding machine .

실시예(4)와 같은 방법으로 2차 난연화된 솜을 제조하되 첨가형 난연제 100중량%로 한 6중량%의 수용액에 수용액 중량의 1/3에 해당하는 1차 난연화된 천연 솜을 침지하여 30분간 교반한 다음 PH 6.5로 조절한 다음 천연 솜을 취출하여 수분함량 70중량%로 탈수한 상태로 수분함량 7중량%로 건조시켜 2차 난연화된 솜을 개면하고, 타면해서 카딩기로 적층하여 부직포로 한 난연성 소재를 제조하였다.Secondary flame retarded cotton was prepared in the same manner as in Example (4), but the first flame retarded natural cotton, which was one third of the weight of the aqueous solution, was immersed in an aqueous solution of 6% by weight of 100% The mixture was stirred for 30 minutes and then adjusted to pH 6.5. Then, the natural cotton was taken out and dried at a water content of 7% by weight in dehydrated water content of 70% by weight to prepare a second flame retarded cotton, To prepare a flame retardant material as a nonwoven fabric.

상기 실시예(4)에서 침지처리가 끝난 2차 난연화된 솜을 취출하고 남은 처리조의 잔액과 탈수과정의 탈수액의 혼합액(D)과 비교실시예(5)의 처리조의 잔액과 탈수과정의 탈수액의 혼합액(E)을 채취하여 각각의 농도를 측정한 결과 다음과 같은 표1을 얻었다.The second flame retarded cotton after the immersion treatment was taken out in Example (4), and the balance of the remaining treatment tank and the dewatered solution (D) of the dehydration process and the balance of the treatment tank of Comparative Example (5) (E) of the dehydrated solution was collected and the concentrations thereof were measured. As a result, the following Table 1 was obtained.

혼합액 D 및 E의 농도 측정 결과표 Concentration measurement result of mixed solution D and E 구분\항목
Category \ Item
농도density
처리 전 농도Concentration before treatment 처리 후 농도Concentration after treatment 감소농도율(%)Decrease concentration ratio (%) 홉합액(D)
실시예(4)
Hop Dissolution (D)
Example (4)
6중량%의 수용액6% by weight aqueous solution 2.6중량%의 수용액2.6% by weight aqueous solution 56.6%56.6%
홉합액(E)
실시예(5)
Hopping solution (E)
Example (5)
6중량%의 수용액6% by weight aqueous solution 3.4중량%의 수용액3.4% by weight aqueous solution 43%43%

표2에서와 같이 실시예(4)에서는 첨가형 난연제 80중량%, 가용화제 8중량%, 분산제6중량%, 방미제 3중량%, 분산제 2중량%, 실란카프링제 1중량%로 조성된 2차 난연화 조성물의 6중량%의 수용액에 1차 난연화된 솜을 침지처리했고 비교실시예(5)에서는 첨가형 난연제 6중량% 수용액으로 동일중량의 1차 난연화된 솜을 침지처리했음을 알 수 있다. 그러나 1차 난연화된 천연 솜에 침적, 코팅, 접착 매카니즘 중 어느 매카니즘에 의한 것인지는 확실치 않으나 혼합용액의 농도감소율을 보면 실시예(4)가 효과적인 침지처리 방법임을 알 수 있다. As shown in Table 2, in Example (4), the addition amount of the flame retardant was 80% by weight, the solubilization agent was 8% by weight, the dispersant was 6% by weight, the antimicrobial agent was 3% by weight, the dispersant was 2% by weight and the silane coupling agent was 1% It can be seen that the primary flame retarded cotton was immersed in an aqueous solution of 6% by weight of the flame retardant composition and in Comparative Example (5), the primary flame retarded cotton of the same weight was immersed in the 6% by weight aqueous solution of the addition type flame retardant . However, it is unclear whether the primary flame-retarded natural cotton is caused by immersion, coating, or adhesion mechanism. However, it can be seen that Example 4 is an effective immersion treatment method in view of the concentration reduction rate of the mixed solution.

또한 실시예(4)로 제조된 본 발명 난연성소재(2차 난연화된 천연 솜)의 난연성을 알아보기 위해 FITI시험연구원에 부직포상 난연성 소재를 의뢰하여 FITI 시험연구원에 의뢰하여 소방법시설설치 및 안전관리에 관한 볍률시행령의 기준에 따라 멕컬버너법에 의한 시험결과를 표3에 나타내었다.In order to investigate the flame retardancy of the inventive flame retardant material (the second flame retarded natural cotton) prepared in Example (4), a non-woven flame retardant material was requested to the FITI test institute, Table 3 shows the results of the test by the Macal burner method according to the criteria of the ordinance for the management.

본 발명에 의한 난연성소재의 방염성 시험결과표 Flame resistance test result table of flame retardant material according to the present invention 구분division 시험기준Test basis 본발명 난연성 소재The flame retardant material 잔염시간(S)Residual salt time (S) 10(S) 이내Within 10 (S) 잔진시간(S)Residual time (S) 30(S) 이내Within 30 (S) 탄화면적Carbonized area 50(㎠)이내Within 50 (㎠) 30.2 30.2 탄화길이Carbonization length 20(㎠)이내Within 20 (㎠) 7.47.4

Claims (8)

반응성 난연제 3~6중량%의 수용액과 수용액중량의 1/3에 해당하는 수분함량 5% 이하의 천연 솜을 고압반응부에 넣고 가온하여 온도 100~150℃로 유지시키고 교반하면서 30~40분간 반응시킨 다음 천연 솜을 취출하여 수분함량 50%로 탈수하고 수분함량5%이하로 건조시킨 1차 난연화된 솜을 제조하는 1단계공정 첨가형 난연제 72~85중량%, 가용화제 7~10중량%, 분산제 5~7중량%, 방미제 3~5중량%, 발수제 2~3중량%, 실란카프링제 1~2중량%로 조성된 2차 난연화조성물을 조성하는 2단계 공정
2차 난연화조성물 4~8중량%의 수용액에 수용액 중량의 1/3에 해당하는 1차 난연화된 천연 솜을 침지하여 상온에서 20~30분간 교반하고 수소이온 농도로 6~7PH로 산 또는 알카리로 조절한 다음 2차 난연화된 솜을 취출하여 수분함량 70%로 탈수한 상태에서 수분함량 7%로 건조시킨 2차 난연화된 솜을 제조하는 3단계공정
2차 난연화된 솜을 개면하고 타면하여 부직포로한 4단계 공정을 포함하는 천연 솜을 이용한 난연성 소제의 제조방법.
3 to 6% by weight of an aqueous solution of a reactive flame retardant and a natural cotton having a moisture content of 5% or less, which corresponds to 1/3 of the weight of the aqueous solution, is heated to 100 to 150 ° C., 72 to 85% by weight of a flame retardant of the first stage process for preparing a primary flame retarded cotton which is dried to a water content of 50% and dried to a moisture content of 5% or less, 7 to 10% by weight of a solubilizer, 2-step process for forming a secondary flame retardant composition composed of 5 to 7% by weight of a dispersant, 3 to 5% by weight of antimicrobial agent, 2 to 3% by weight of a water repellent agent and 1 to 2% by weight of a silane coupling agent
The primary flame retarded natural cotton, which is one third of the weight of the aqueous solution, is immersed in an aqueous solution of 4 to 8 wt% of the secondary flame retardant composition, stirred at room temperature for 20 to 30 minutes, Alkali-regulated, second-order flame-retarded cotton is removed and dehydrated to 70% moisture content to produce a second flame-retarded cotton which is dried to a moisture content of 7%.
A method for manufacturing a flame retardant cleaning agent using natural cotton comprising a four-step process in which a second flame-retarded cotton is turned and rubbed into a nonwoven fabric.
청구항 제1항에 있어서, 반응성 난연제는 요소·인산염계화합물, 파라핀과 삼산화안티몬, 히드록시 메틸화포스포노카르복시아미드 중에서 선택되는 하나 이상의 반응성 난연제임을 특징으로 하는 천연 솜을 이용한 난연성 소재의 제조방법.The method of claim 1, wherein the reactive flame retardant is at least one reactive flame retardant selected from urea-phosphate compounds, paraffin, antimony trioxide, and hydroxymethylated phosphonocarboxamide. 청구항 제1항에 있어서, 첨가형 난연제는 황산암몬, 염화암몬, 염화마그네슘, 황산알루미늄, 인산암몬, 붕산 중에서 선택되는 하나 이상의 첨가형 난연제임을 특징으로 하는 천연 솜을 이용한 난연성 소재의 제조방법.The method of claim 1, wherein the additive type flame retardant is at least one addition type flame retardant selected from the group consisting of ammonium sulfate, ammonium chloride, magnesium chloride, aluminum sulfate, ammonium phosphate and boric acid. 청구항 제1항에 있어서, 가용화제는 토루엔슬폰산염, 크시렌슬폰산소다, 에틸알콜, 프로피렌글리콜 중에서 선택되는 하나 이상의 가용화제임을 특징으로 하는 천연 솜을 이용한 난연성 소재의 제조방법The method of claim 1, wherein the solubilizing agent is at least one solubilizing agent selected from the group consisting of a toluene sulfonate, a xylene sulfonated oxygen, an ethyl alcohol, and propylene glycol. 청구항 제1항에 있어서, 방미제는 8옥시퀴노린, 도데실디메틸렌벤질암모니움클로라이드, 나프텐산동, 트리크롤칼바니리드, 나프텐산아연 중에서 선택되는 하나 이상의 방미제임을 특징으로 하는 천연 솜을 이용한 난연성소재의 제조방법.The method of claim 1, wherein the antifungal agent is at least one antifungal agent selected from the group consisting of 8-oxyquinoline, dodecyldimethylbenzylammonium chloride, naphthenic acid, tricolol calanaviride, and zinc naphthenate. A method for producing a flame retardant material. 청구항 제1항에 있어서, 발수제는 염화파라핀임을 특징으로 하는 천연 솜을 이용한 난연성소재의 제조방법.The method according to claim 1, wherein the water repellent agent is chlorinated paraffin. 청구항 제1항에 있어서, PH 조절제로 알카리는 탄산소다임을 특징으로 하는 천연 솜을 이용한 난연성소재의 제조방법The method for producing a flame retardant material according to claim 1, wherein the alkaline phosphatase is sodium carbonate 청구항 제1항에 있어서, PH 조절제로 산은 초산임을 특징으로 하는 천연 솜을 이용한 난연성 소재의 제조방법.
The method according to claim 1, wherein the PH regulator is acetic acid.
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CN111893750A (en) * 2020-08-11 2020-11-06 盐城工学院 Preparation method of flame-retardant cotton fabric
CN115404700A (en) * 2022-10-17 2022-11-29 六安市皖兴羽绒有限公司 Preparation method of flame-retardant down fiber

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JP2006089534A (en) 2004-09-21 2006-04-06 Fuji Electric Holdings Co Ltd Flame-retardant resin processed product
KR101066276B1 (en) 2009-08-10 2011-09-26 (주)다담산업 Method for manufacturing of interior finishing material for construction and the interior finishing material thereof

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CN111893750A (en) * 2020-08-11 2020-11-06 盐城工学院 Preparation method of flame-retardant cotton fabric
CN111893750B (en) * 2020-08-11 2022-11-11 盐城工学院 Preparation method of flame-retardant cotton fabric
CN115404700A (en) * 2022-10-17 2022-11-29 六安市皖兴羽绒有限公司 Preparation method of flame-retardant down fiber
CN115404700B (en) * 2022-10-17 2024-01-16 六安市皖兴羽绒有限公司 Preparation method of flame-retardant down fiber

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