WO2014019334A1 - 一种疏水阻燃纤维及其制造方法 - Google Patents

一种疏水阻燃纤维及其制造方法 Download PDF

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Publication number
WO2014019334A1
WO2014019334A1 PCT/CN2013/000589 CN2013000589W WO2014019334A1 WO 2014019334 A1 WO2014019334 A1 WO 2014019334A1 CN 2013000589 W CN2013000589 W CN 2013000589W WO 2014019334 A1 WO2014019334 A1 WO 2014019334A1
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WIPO (PCT)
Prior art keywords
fiber
flame
retardant
flame retardant
hydrophobic
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PCT/CN2013/000589
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English (en)
French (fr)
Inventor
齐鲁
丁致家
高德康
高晓东
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波司登股份有限公司
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Application filed by 波司登股份有限公司 filed Critical 波司登股份有限公司
Priority to EP13825054.3A priority Critical patent/EP2862965B1/en
Publication of WO2014019334A1 publication Critical patent/WO2014019334A1/zh
Priority to US14/560,653 priority patent/US10006150B2/en

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30—Conjugate filaments; Spinnerette packs therefor
    • D01D5/34—Core-skin structure; Spinnerette packs therefor
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01G—PRELIMINARY TREATMENT OF FIBRES, e.g. FOR SPINNING
    • D01G13/00—Mixing, e.g. blending, fibres; Mixing non-fibrous materials with fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2427/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08J2427/06—Homopolymers or copolymers of vinyl chloride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D10B2321/02—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polyolefins
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D10B2321/04—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of halogenated hydrocarbons
    • D10B2321/042—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of halogenated hydrocarbons polymers of fluorinated hydrocarbons, e.g. polytetrafluoroethene [PTFE]
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/02—Moisture-responsive characteristics
    • D10B2401/021—Moisture-responsive characteristics hydrophobic

Definitions

  • Hydrophobic flame retardant fiber and method for manufacturing the same
  • the present invention relates to functional chemical fiber technology, and more particularly to a hydrophobic flame retardant fiber and a method of making the same.
  • Hydrophobic flame retardant fiber is a functional fiber with certain hydrophobic and flame retardant properties.
  • a patent document has been reported.
  • Chinese Patent Publication No. CN101143923 discloses a water-repellent polyester fiber for a tarpaulin, which is characterized in that it is added during the polymerization of purified terephthalic acid and ethylene glycol.
  • the water-reducing polyester is prepared by using the B-type additive silicone or dimer acid, and the polyester is spun, and the water-reducing fiber having a square cross-section is obtained through the special-shaped spinneret (the cross section of the spinning hole is square).
  • this kind of fiber has a hydrophobic action, it has no flame retarding function.
  • Chinese patent document CN102337667A discloses a textile containing flame-retardant and water-repellent fiber-containing flame-retardant polyester fiber and a production method thereof, wherein the textile has a bromine content of 5 ⁇ g/g and a fluorine content of 5 ug/go.
  • the textile is made by non-halogen flame retardant processing agent and non-fluorine water repellent processing agent for functional finishing. Since the fabric is obtained by finishing, on the one hand, the hand of the fabric is poor, and on the other hand, the fabric is not washable, and the functional finishing agent is easily peeled off.
  • Chinese Patent Publication No. CN101787579A discloses a flame-retardant polyester fiber and a preparation method and apparatus thereof.
  • the flame-retardant polyester fiber has an inner and outer two-layer structure, the inner layer is a PET resin to which a flame retardant is added, and the outer layer is a PET resin. Since the fiber is made of ordinary polyester or the outer layer of the fiber, it does not have hydrophobic properties, and since the flame retardant is added to the inner layer of the fiber, it is disadvantageous for the flame retardant performance.
  • the technical problem to be solved by the present invention is to provide a hydrophobic flame-retardant fiber and a method of manufacturing the same.
  • the fiber has both good hydrophobic properties and flame retardant properties, is water-resistant, has a long-lasting function, and has a good hand feeling, and is suitable for textiles and taking.
  • the fiber manufacturing method adopts the sheath-core composite spinning technology, which can make the two functions of the fiber complement and strengthen, and the process is simple, and is suitable for industrialization and implementation.
  • the technical solution of the invention to solve the fiber technical problem is: designing a hydrophobic flame retardant fiber, 8%, 8%, the mass ratio of the fiber sheath material is: polyethylene terephthalate 79. 9-88. 8%, 6%;
  • the polyvinylidene fluoride polyethylene is a fluorinated polyethylene.
  • the fluorinated polyethylene is 8-13%, the flame retardant is 3-6%, the compatibilizer is 0.1-0.5%, the coupling agent is 0.1-0.66%.
  • the compatibilizer is one of an acrylate grafted polyolefin elastomer and a maleic anhydride grafted polyolefin elastomer
  • the coupling agent is triisostearoyl titanic acid Isopropyl ester, tris(dodecanylbenzoyl) isopropyl titanate, tris(dioctylphosphoryloxy) isopropyl titanate and tris(dioctylpyrophosphoryloxy)titanate a mixture of ester and paraffin 1:1 mass ratio
  • the mass percentage composition of the fiber core material is: polyethylene terephthalate 91-95%, flame retardant 5-9%; cortex and
  • the flame retardant described in the core material is one of polyphenol bisphenol sulfone ester, aryl polyphosphate, polyparaphenylene phenyl phosphate, and polyparaphenylene sulfone phenyl phosphate.
  • the technical solution to solve the technical problem of the manufacturing method of the present invention is: designing a method for manufacturing a hydrophobic flame-retardant fiber, which adopts the mass percentage composition of the hydrophobic flame-retardant fiber according to the present invention and the following process:
  • the hydrophobic flame-retardant fiber of the invention has both good hydrophobic properties and flame retardant function.
  • the hydrophobic flame retardant fiber skin layer designed by the invention contains polyvinylidene fluoride polyethylene and a flame retardant, It has a permanent hydrophobicity and a certain flame retardant effect; while the core material of the fiber has a permanent flame retardant function due to the inclusion of a flame retardant, the main object of the present invention is achieved.
  • the hydrophobic flame-retardant fiber of the present invention is a fiber which is spun after being melt-mixed with various additives and a polymer.
  • the method for manufacturing the hydrophobic flame-retardant fiber of the invention is to spin the mixture of two different functions into a fiber with a sheath-core composite structure, so that the manufactured fiber has the dual functions of hydrophobicity and flame retardancy, and realizes two functions independently and without interference. And the complementary characteristics, and the composite spinning technology used is easy to industrialize and the manufacturing cost is relatively low.
  • the hydrophobic flame-retardant fiber (abbreviated as fiber) designed by the invention has a sheath-core composite structure, and the volume ratio of the skin and the core is 2: 8-6: 4, which is characterized in that the mass percentage composition of the fiber sheath material is: poly-p-phenylene 5%, 5%, 5%, 6%, 6%, 6%, 5%, 5%, Coupling agent 0. 1—0. 6%; the sum of the components is 100%; the mass percentage composition of the fiber core material is: polyethylene terephthalate (PET) 91-95%, resistance The fuel is 5-9%, and the sum of the components is 100%.
  • PET polyethylene terephthalate
  • the PET described in the fiber sheath of the present invention and the PET described in the core material are the same polymer, both of which are conventional polyethylene terephthalate.
  • another polymer PVDF is also mixed in the cortical material.
  • the flame retardant described in the fiber sheath material of the present invention is one of polyphenyl bisphenol sulfone ester, aryl polyphosphate, polyparaphenylene phenyl phosphate, and polyparaphenylene sulfone phenyl phosphate.
  • the compatibilizing agent described in the fiber sheath of the present invention is one of an acrylate-grafted polyolefin elastomer and a maleic anhydride-grafted polyolefin elastomer.
  • the coupling agent described in the fiber sheath material of the present invention is isopropyl triisostearyl titanate, isopropyl tris(dodecylbenzenesulfonyl) titanate, and tris(dioctylphosphoryloxy)titanium.
  • the flame retardant of the fiber core material of the present invention is a polyphenol bisphenol sulfone ester, an aryl polyphosphate, a polyparaphenylene phenyl phosphate and a polyparaphenylene sulfone phenyl phosphate. That is, the same as the flame retardant described in the skin layer.
  • the invention simultaneously designs a method for manufacturing hydrophobic flame-retardant fiber (abbreviated as a manufacturing method), and the manufacturing method adopts the mass percentage composition of the hydrophobic flame-retardant fiber of the invention and the following process:
  • hydrophobic flame retardant fiber sheath material according to the mass percentage composition of the skin material, after drying another portion (the remaining flame retardant chips) PET, PVDF and the obtained flame retardant chips, and the compatibilizing agent, After the mixture is uniformly mixed, it is extruded at a temperature of 255-26 CTC through a twin-screw machine, and after granulation, a hydrophobic flame-retardant fiber sheath material is obtained;
  • the flame retardant section in the fiber sheath material of the present invention is prepared by melt granulation after mixing a part of PET and the proportion of the flame retardant; the flame retardant in the flame retardant section has a mass content of 6-9 %. Another part of the remaining part of the flame retardant section is produced. After the PET is dried, it is used to make a skin layer. The sum of the two parts of PET constitutes the proportion of PET in the sheath. The use of flame retardant chips first and then mixed with other materials is to make the material mix more evenly.
  • sheath-core composite hydrophobic flame-retardant fiber The skin material and the core material obtained by the above steps (2) and (3) are composited with a sheath core according to a fiber sheath and a core volume ratio of 2:8-6:4. The spinning machine spun the wound filaments, and after stretching, the filaments were formed to obtain the hydrophobic flame-retardant fiber of the present invention.
  • the sheath-to-core ratio is related to the flame retardancy of the fiber. If the proportion of the cortex of the fiber is too large, the ratio of the core layer is too small, the flame retardant effect of the fiber core layer is not obvious, which affects the flame retardant effect of the fiber; on the contrary, if the ratio of the cortex of the fiber is too small, the proportion of the core layer is too large, which will affect the fiber.
  • the hydrophobic property therefore, requires that the core layer volume ratio be controlled within the range described, but a preferred sheath-to-core volume ratio is 3:7 - 5:5.
  • the stretching is a known stretching or a conventional stretching, and is generally stretched by 3 to 5 times.
  • the fibers of the present invention have been tested to have a hydrophobic angle of 86-90 degrees and a limiting oxygen index of 27-29, hence the name hydrophobic hydrophobic fibers.
  • the general physical indicators such as the strength of the fiber also meet the requirements of conventional textiles.
  • the fiber has a hydrophobic angle of 90 degrees and a limiting oxygen index of 29.
  • the fiber has a hydrophobic angle of 86 degrees and a limiting oxygen index of 27.
  • the fiber was tested to have a hydrophobic angle of 89 degrees and a limiting oxygen index of 29.
  • the fiber filaments were tested to have a hydrophobic angle of 88 degrees and a limiting oxygen index of 28.
  • the styrene-grafted polyolefin elastomer is 0. 2 kg, glycerol-grafted polyolefin elastomer. Isopropyl ester 0. 15 kg, paraffin wax 0.
  • the filament length has a hydrophobic angle of 87 degrees and a limiting oxygen index of 28.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Multicomponent Fibers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Artificial Filaments (AREA)

Abstract

本发明公开一种疏水阻燃纤维及其制造方法。该纤维的皮、芯体积比为2:8-6:4，其特征在于该纤维皮层料质量百分比组成为：PET 79. 9-88. 8%、PVDF 8-13%，阻燃剂3-6%、相容剂0.1-0.5%、偶联剂0.1-0.6%；相容剂为丙烯酸酯接枝聚烯烃弹性体和马来酸酐接枝聚烯烃弹性体中的一种；该纤维芯层料质量百分比组成为：PET 91-95%、阻燃剂5-9%；阻燃剂均为聚苯磷酸双酚砜酯、芳基聚磷酸酯、聚对亚苯基苯基磷酸酯和聚对二苯砜苯基磷酸酯中的一种。该纤维制造方法采用下述工艺：1．制造阻燃切片；2．制造纤维皮层料；3．制造纤维芯层料；4．制造皮芯复合疏水阻燃纤维。

Description

一种疏水阻燃纤维及具制适万法 技术领域
本发明涉及功能性化学纤维技术， 具体为一种疏水阻燃纤维及其制造方 法。
背景技术
疏水阻燃纤维是一种具有一定疏水和阻燃性能的功能纤维。 对于疏水阻燃 纤维已有专利文献报道， 例如， 中国专利文献 CN101143923公开了一种用于防 雨布的拒水聚酯纤维，其特征是在精对苯二甲酸和乙二醇聚合制浆时加入 B 型 添加剂硅酮或二聚酸制取拒水聚酯，再用该聚酯紡丝，通过异形喷丝板 （喷丝孔 截面呈方型） ，制得具有方型截面拒水纤维。 该种纤维虽然具有疏水作用， 但 没有阻燃功能。 中国专利文献 CN102337667A 公开了一种具有阻燃拒水功能的 含有阻燃聚酯纤维的纺织品及其生产方法,该纺织品中溴元素的含量 5 μ g/g, 氟元素的含量 5 u g/go 该纺织品采用非卤素阻燃加工剂及非氟素拒水加工剂 进行功能性整理加工制得。 由于该种织物是通过整理加工制得的， 因此一方面 织物的手感差， 另一方面织物不耐洗， 功能整理剂容易脱落。 中国专利文献 CN101787579A 公开一种阻燃聚酯纤维及其制备方法和装置，该阻燃聚酯纤维为 内外两层结构， 内层为添加有阻燃剂的 PET树脂， 外层为 PET树脂。 该纤维由 于皮或外层原料为普通涤纶， 因而不具备疏水性能， 而且由于阻燃剂添加在纤 维的内层， 不利于阻燃性能的发挥。
发明内容
针对现有技术的不足， 本发明拟解决的技术问题是， 提供一种疏水阻燃纤 维及其制造方法。 该纤维同时具有良好的疏水性能和阻燃性能， 具有耐水洗， 功能持久， 同时手感好， 适于纺织和服用。 该纤维制造方法采用皮芯复合纺丝 技术， 可使纤维的两种功能互补并得到加强， 同时工艺简单， 适于工业化实施 推广。
本发明解决所述纤维技术问题的技术方案是： 设计一种疏水阻燃纤维， 具 有皮芯结构， 皮、 芯体积比为 2： 8— 6： 4， 其特征在于该纤维皮层料的质量 百分比组成为： 聚对苯二甲酸乙二醇酯 79. 9-88. 8%、 聚偏氟聚乙烯 8— 13%, 阻燃剂 3-6%、 相容剂 0. 1—0. 5%、 偶联剂 0. 1—0. 6%； 所述聚偏氟聚乙烯的熔 融指数 MI=18-45 ; 所述相容剂为丙烯酸酯接枝聚烯烃弹性体和马来酸酐接枝 聚烯烃弹性体中的一种； 所述偶联剂为三异硬脂酰基钛酸异丙酯、 三 （十二垸 基苯磧酰基） 钛酸异丙酯、 三 （二辛磷酰氧基） 钛酸异丙酯和三 （二辛基焦磷 酰氧基） 钛酸异丙酯的一种与石蜡 1 : 1 质量比的混合物； 该纤维芯层料的质 量百分比组成为： 聚对苯二甲酸乙二醇酯 91一 95%、 阻燃剂 5— 9%; 皮层料和 芯层料中所述的阻燃剂均为聚苯磷酸双酚砜酯、 芳基聚磷酸酯、 聚对亚苯基苯 基磷酸酯和聚对二苯砜苯基磷酸酯中的一种。
本发明解决所述制造方法技术问题的技术方案是： 设计一种疏水阻燃纤维 制造方法， 该制造方法采用本发明所述的疏水阻燃纤维质量百分比组成和下述 工艺：
( 1 ) . 制造阻燃切片； 把皮层料中所述的阻燃剂和干燥的部分聚对苯二 甲酸乙二醇酯均匀混合后， 在 255-260Ό温度下， 经双螺杆机挤出， 造粒， 获 得阻燃切片； 阻燃切片中阻燃剂的质量含量为 6— 9% ;
(2 ) .制造疏水阻燃纤维皮层料： 把皮层料中的聚偏氟聚乙烯、 所得的阻 燃切片和制造阻燃切片余下的聚对苯二甲酸乙二醇酯干燥后， 与相容剂、 偶联 剂按所述皮层料质量百分比组成均匀混合， 在 255- 260°C温度下， 经双螺杆机 挤出， 造粒， 即获得疏水阻燃纤维皮层料；
(3 ) .制造疏水阻燃纤维芯层料： 按所述芯层料重量百分比组成， 把所述 聚对苯二甲酸乙二醇酯与阻燃剂均匀混合后， 在 260- - 265°C温度下， 经双螺 杆机挤出， 造粒， 即获得疏水阻燃纤维芯层料；
(4 ) .制造皮芯复合疏水阻燃纤维： 将上述 （2 ) 、 ( 3 ) 步所得的皮层料 和芯层料， 按 2： 8-6： 4 的纤维皮、 芯体积比， 用皮芯复合紡丝机纺出卷绕 丝， 经拉伸后， 制成纤维长丝， 即得到所述的疏水阻燃纤维。
与现有技术相比， 本发明疏水阻燃纤维既具有良好的疏水性能， 又具有 阻燃功能。 本发明设计的疏水阻燃纤维皮层料含有聚偏氟聚乙烯和阻燃剂， 会 具有永久的疏水和一定的阻燃作用； 而纤维的芯层料因含有阻燃剂而具有永久 阻燃功能， 实现本发明的主要目的。 另外， 本发明疏水阻燃纤维由于是各种添 加材料与聚合物熔融混合后纺制的纤维， 因此， 与涂层织物相比， 具有耐水洗 和手感好等特点， 更适于纺织和服用。 本发明疏水阻燃纤维制造方法是将两种 不同功能的混合料纺制成具有皮芯复合结构的纤维， 使制造的纤维具有疏水和 阻燃双重功能， 实现两种功能既独立、 不干扰， 且又互补的特点， 而所采用的 复合纺丝技术， 容易工业化生产， 制造成本比较低。
具体实施方式
下面结合实施例进一步叙述本发明：
本发明设计的疏水阻燃纤维 （简称纤维） ， 具有皮芯复合结构， 皮、 芯体 积比为 2： 8-6： 4, 其特征在于该纤维皮层料的质量百分比组成为： 聚对苯 二甲酸乙二醇酯 (PET) 79. 9-88. 8%、 聚偏氟聚乙烯 ( PVDF) 8— 13%， 阻燃剂 3 - 6%、 相容剂 0. 1—0. 5%、 偶联剂 0. 1—0. 6%； 各组分之和为 100%; 该纤维芯 层料的质量百分比组成为： 聚对苯二甲酸乙二醇酯 （PET) 91— 95%、 阻燃剂 5 —9%, 各组分之和为 100%。
本发明纤维皮层料中所述的 PET和芯层料中所述的 PET为同一种聚合物， 都是常规的聚对苯二甲酸乙二醇酯。 但皮层料中还混有另一种聚合物 PVDF。 所述 PVDF的熔融指数 MI=18-45。
本发明纤维皮层料中所述的阻燃剂为聚苯磷酸双酚砜酯、 芳基聚磷酸酯、 聚对亚苯基苯基磷酸酯和聚对二苯砜苯基磷酸酯的一种。
本发明纤维皮层料中所述的相容剂为丙烯酸酯接枝聚烯烃弹性体和马来酸 酐接枝聚烯烃弹性体中的一种。
本发明纤维皮层料中所述的偶联剂为三异硬脂酰基钛酸异丙酯、 三 （十二 垸基苯磺酰基） 钛酸异丙酯、 三 （二辛磷酰氧基） 钛酸异丙酯和三 （二辛基焦 磷酰氧基） 钛酸异丙酯一种与石蜡 1 : 1的混合物。
本发明纤维芯层料所述的阻燃剂为聚苯磷酸双酚砜酯、 芳基聚磷酸酯、 聚 对亚苯基苯基磷酸酯和聚对二苯砜苯基磷酸酯的一种， 即与皮层料中所述的阻 燃剂一样。 本发明同时设计了疏水阻燃纤维的制造方法 （简称制造方法） ， 该制造方 法采用本发明所述疏水阻燃纤维质量百分比组成和下述工艺：
1. 制造阻燃切片； 把皮层料中所述的阻燃剂和干燥的部分聚对苯二甲酸 乙二醇酯均勾混合后， 在 255-26CTC温度下， 经双螺杆机挤出， 造粒， 获得阻 燃切片； 所述阻燃切片中阻燃剂的质量含量为 6— 9 % ;
2. 制造疏水阻燃纤维皮层料： 按照所述皮层料质量百分比组成， 把另一 部分 （制造阻燃切片余下的） PET、 PVDF和所得阻燃切片干燥后， 与所述的相 容剂、 偶联剂均匀混合后， 在 255-26CTC温度下， 经双螺杆机挤出， 造粒后， 获得疏水阻燃纤维皮层料；
本发明纤维皮层料中的阻燃切片是由部分 PET 和所述比例的阻燃剂混和 后， 通过熔融造粒制备的； 阻燃切片中阻燃剂的质量含量为 6— 9 %。 制造阻 燃切片余下的另一部分 PET干燥后， 用于制造皮层料。 两部分 PET之和构成皮 层料中所述比例的 PET。 采用先制造阻燃切片再与其他原料混合是为了使物料 混合更加均匀。
3.制造疏水阻燃纤维芯层料： 按照所述芯层料重量百分比组成， 把所述 PET和阻燃剂均匀混合后， 在 260- 265Ό温度下， 经双螺杆机挤出， 造粒， 获 得疏水阻燃纤维芯层料；
4.制造皮芯复合疏水阻燃纤维： 将上述 （2 ) 、 ( 3 ) 步所得的皮层料和芯 层料， 按 2： 8— 6： 4 的纤维皮、 芯体积比， 用皮芯复合纺丝机纺出卷绕丝， 经拉伸后， 制成纤维长丝， 即得到本发明所述的疏水阻燃纤维。
所述的皮芯体积比关系到纤维的阻燃性能。 如果纤维的皮层比例过大， 芯 层比例太小， 纤维芯层阻燃作用不明显， 影响纤维阻燃效果； 反之， 如果纤维 的皮层比例过小， 芯层比例太大， 这将会影响纤维的疏水性能， 因此要求皮芯 层体积比控制在所述的范围内， 但优选的皮芯体积比为 3： 7— 5： 5。 所述的 拉伸为公知拉伸或常规拉伸， 一般拉伸 3— 5 倍。 经检测， 本发明纤维的疏水 角为 86-90度， 极限氧指数为 27-29， 因此称之为疏水阻燃纤维。 该纤维的强 力等一般物理指标也满足常规纺织要求。
本发明未述及之处适用于现有技术。 以下给出本发明的几个具体实施例。 具体实施例仅是对本发明技术方案的 进一步具体说明， 不限制本申请权利要求的保护范围。
实施例 1
取干燥后的 PET 60. 7 公斤， 聚苯磷酸双酚砜酯 6 公斤， 经充分混合后， 在 255Ό下经双螺杆机挤出， 制备出 66. 7公斤阻燃切片。
然后取干燥后的 PET 19. 2 公斤、 熔融指数 45的 PVDF 13公斤， 干燥后 的所得阻燃切片 66. 7公斤， 丙烯酸酯接枝聚烯烃弹性体 0. 5公斤， 三异硬脂 酰基钛酸异丙酯 0. 3公斤，石蜡 0. 3公斤， 经充分混合后， 在 255°C下经双螺 杆机挤出， 造粒， 制造出纤维皮层料； 取干燥后的 PET 91 公斤， 聚苯磷酸双 酚砜酯 9公斤， 经充分混合后， 在 260Ό下经双螺杆机挤出， 造粒， 制造出纤 维芯层料； 将所得皮芯料充分烘干后， 按 2： 8 的纤维皮、 芯体积比用皮芯复 合纺丝机纺制出卷绕丝， 再将所得的卷绕丝在 120°C温度下拉伸 3 倍，得到成 品疏水阻燃纤维长丝。
经检测， 该纤维的疏水角度为 90度， 极限氧指数为 29。
实施例 2
取干燥后的 PET 47 公斤， 芳基聚磷酸酯 3 公斤， 经充分混合后， 在 260°C下经双螺杆机挤出， 制备出 50公斤阻燃切片。
然后取干燥后的 PET 41. 8 公斤、 熔融指数 18的聚偏氟聚乙烯 （PVDF) 8 公斤， 干燥后的阻燃切片 50公斤， 马来酸酐接枝聚烯烃弹性体 0. 1公斤， 三 (十二烷基苯磺酰基） 钛酸异丙酯 0. 05公斤，石蜡 0. 05公斤， 经充分混合后， 在 260Ό下经双螺杆机挤出， 造粒， 制造出纤维皮层料； 取干燥后的 PET 95 公斤， 芳基聚磷酸酯 5公斤， 经充分混合后， 在 265°C下经双螺杆机挤出， 造 粒， 制造出纤维芯层料； 将所得皮芯料充分烘干后， 按 6： 4 的纤维皮、 芯体 积比用皮芯复合纺丝机纺制出卷绕丝， 再将所得的卷绕丝在 120°C温度下拉伸 3. 5倍,得到成品疏水阻燃纤维长丝。
经检测， 该纤维的疏水角度为 86度， 极限氧指数 27。
实施例 3
取干燥后的 PET 57. 5公斤， 聚对亚苯基苯基磷酸酯 5公斤， 经充分混合 后， 在 255°C下经双螺杆机挤出， 制备出 62. 5公斤阻燃切片。
然后取干燥后的 PET 24. 6公斤、 熔融指数 35的 PVDF 12公斤， 干燥后 的所得阻燃切片 62. 5公斤， 丙烯酸酯接枝聚烯烃弹性体 0. 4公斤， 三（二辛 磷酰氧基） 钛酸异丙酯 0. 25公斤，石蜡 0. 25公斤， 经充分混合后， 在 255°C 下经双螺杆机挤出， 造粒， 制造出纤维皮层料； 取干燥后的 PET 92 公斤， 聚 苯磷酸双酚砜酯 8公斤， 经充分混合后， 在 260°C下经双螺杆机挤出， 造粒， 制造出纤维芯层料； 将所得皮芯料充分烘干后， 按 3： 7 的纤维皮、 芯体积比 用皮芯复合纺丝机纺制出卷绕丝， 再将所得的卷绕丝在 120°C温度下拉伸 4倍, 得到成品疏水阻燃纤维长丝。
经检测， 该纤维的疏水角度为 89度， 极限氧指数为 29。
实施例 4
取干燥后的 PET 53. 2公斤， 聚对二苯砜苯基磷酸酯 4公斤， 经充分混合 后， 在 255°C下经双螺杆机挤出， 制备出 57. 2公斤阻燃切片。
然后取干燥后的 PET 32. 1公斤、 熔融指数 30的 PVDF10公斤， 干燥后的 所得阻燃切片 57. 2份， 马来酸酐接枝聚烯烃弹性体 0. 3公斤， 三（二辛基焦 磷酰氧基） 钛酸异丙酯 0. 2公斤，石蜡 0. 2公斤， 经充分混合后， 在 255°C下 经双螺杆机挤出， 造粒， 制造出纤维皮层料； 取干燥后的 PET 91 公斤， 聚苯 磷酸双酚砜酯 9公斤， 经充分混合后， 在 265°C下经双螺杆机挤出， 造粒， 制 造出纤维芯层料； 将所得皮芯料充分烘干后， 按 4： 6 的纤维皮、 芯体积比用 皮芯复合纺丝机纺制出卷绕丝， 再将所得的卷绕丝在 120°C温度下拉伸 4. 5倍: 得到疏水阻燃纤维长丝。
经检测， 该纤维长丝的疏水角度为 88度， 极限氧指数为 28。
实施例 5
取干燥后的 PET 62. 7 公斤， 聚苯磷酸双酚砜酯 4 公斤， 经充分混合后， 在 260°C下经双螺杆机挤出， 制备出 66. 7公斤阻燃切片。
然后取干燥后的 PET 23. 8公斤、 熔融指数 25的 PVDF 9公斤， 干燥后的 阻燃切片 66. 7公斤， 丙烯酸酯接枝聚烯烃弹性体 0. 2公斤， 三异硬脂酰基钛 酸异丙酯 0. 15公斤，石蜡 0. 15公斤， 经充分混合后， 在 255°C下经双螺杆机 挤出， 造粒， 制造出纤维皮层料； 取干燥后的 PET 92 公斤， 聚苯磷酸双酚砜 酯 8公斤， 经充分混合后， 在 265°C下经双螺杆机挤出， 造粒， 制造出纤维芯 层料； 将所得皮芯料充分烘干后， 按 5： 5 的纤维皮、 芯体积比用皮芯复合紡 丝机纺制出卷绕丝， 再将所得的卷绕丝在 120°C温度下拉伸 5 倍，得到疏水阻 燃纤维长丝。
经检测， 该纤长丝维的疏水角度为 87度， 极限氧指数为 28。

Claims

权 利 要 求 书
1. 一种疏水阻燃纤维， 具有皮芯结构， 皮、 芯体积比为 2： 8— 6： 4， 其特征在于该纤维皮层料的质量百分比组成为： 聚对苯二甲酸乙二醇酯 79. 9 一 88. 8%、 聚偏氟聚乙烯 8— 13%， 阻燃剂 3— 6%、 相容剂 0. 1— 0. 5%、 偶联剂 0. 1— 0. 6%; 所述聚偏氟聚乙烯的熔融指数 MI=18-45; 所述相容剂为丙烯酸酯 接枝聚烯烃弹性体和马来酸酐接枝聚烯烃弹性体中的一种； 所述偶联剂为三异 硬脂酰基钛酸异丙酯、 三 （十二烷基苯磺酰基） 钛酸异丙酯、 三 （二辛磷酰氧 基） 钛酸异丙酯和三 （二辛基焦磷酰氧基） 钛酸异丙酯的一种与石蜡 1 : 1 质 量比的混合物； 该纤维芯层料的质量百分比组成为： 聚对苯二甲酸乙二醇酯 91一 95%、 阻燃剂 5— 9%; 皮层料和芯层料中所述的阻燃剂均为聚苯磷酸双酚 砜酯、 芳基聚磷酸酯、 聚对亚苯基苯基磷酸酯和聚对二苯砜苯基磷酸酯中的一 种。
2. 根据权利要求 1所述的疏水阻燃纤维， 其特征在于所述的皮、 芯体积 比为 3： 7—5： 5。
3.一种疏水阻燃纤维制造方法， 该制造方法采用权利要求 1或 2所述的 疏水阻燃纤维质量百分比组成和下述工艺：
( 1 ) . 制造阻燃切片； 把皮层料中所述的阻燃剂和干燥的部分聚对苯二 甲酸乙二醇酯均匀混合后， 在 255-260°C温度下， 经双螺杆机挤出， 造粒， 获 得阻燃切片； 阻燃切片中阻燃剂的质量含量为 6— 9 % ;
( 2 ) .制造疏水阻燃纤维皮层料： 把皮层料中的聚偏氟聚乙烯、 所得的阻 燃切片和制造阻燃切片余下的聚对苯二甲酸乙二醇酯干燥后， 与相容剂、 偶联 剂按所述皮层料质量百分比组成均匀混合， 在 255-26CTC温度下， 经双螺杆机 挤出， 造粒， 即获得疏水阻燃纤维皮层料；
( 3 ) .制造疏水阻燃纤维芯层料： 按所述芯层料重量百分比组成， 把所述 聚对苯二甲酸乙二醇酯与阻燃剂均匀混合后， 在 260 265 °C温度下， 经双螺 杆机挤出， 造粒， 即获得疏水阻燃纤维芯层料；
(4) ，制造皮芯复合疏水阻燃纤维： 将上述 （2) 、 ( 3) 步所得的皮层料 和芯层料， 按 2： 8— 6： 4 的纤维皮、 芯体积比， 用皮芯复合纺丝机纺出卷绕 丝， 经拉伸后， 制成纤维长丝， 即得到所述的疏水阻燃纤维。
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