CN110656419B - Anti-static flame-retardant oil-proof washing cotton-hemp blended fabric and preparation method thereof - Google Patents

Anti-static flame-retardant oil-proof washing cotton-hemp blended fabric and preparation method thereof Download PDF

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CN110656419B
CN110656419B CN201910792743.XA CN201910792743A CN110656419B CN 110656419 B CN110656419 B CN 110656419B CN 201910792743 A CN201910792743 A CN 201910792743A CN 110656419 B CN110656419 B CN 110656419B
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fabric
flame
blended fabric
retardant
cotton
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CN110656419A (en
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唐雪金
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Jiangsu Da Mao Niu New Material Co.,Ltd.
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Jiangsu Da Mao Niu New Material Co ltd
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    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/04—Blended or other yarns or threads containing components made from different materials
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D13/00—Woven fabrics characterised by the special disposition of the warp or weft threads, e.g. with curved weft threads, with discontinuous warp threads, with diagonal warp or weft
    • D03D13/008—Woven fabrics characterised by the special disposition of the warp or weft threads, e.g. with curved weft threads, with discontinuous warp threads, with diagonal warp or weft characterised by weave density or surface weight
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
    • D06B3/18—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics combined with squeezing, e.g. in padding machines
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating 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
    • D06M11/32—Treating 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
    • D06M11/36—Treating 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
    • D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic System; Zincates; Cadmates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating 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
    • D06M11/32—Treating 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
    • D06M11/36—Treating 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
    • D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic System; Aluminates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating 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
    • D06M11/32—Treating 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
    • D06M11/36—Treating 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
    • D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating 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
    • D06M11/77—Treating 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 silicon or compounds thereof
    • D06M11/79—Treating 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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/15—Proteins or derivatives thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/667—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing phosphorus in the main chain
    • D06M15/673—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing phosphorus in the main chain containing phosphorus and nitrogen in the main chain
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/11—Oleophobic properties
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30—Flame or heat resistance, fire retardancy properties
    • 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
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/01—Natural vegetable fibres
    • 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
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/01—Natural vegetable fibres
    • D10B2201/02—Cotton
    • 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
    • D10B2211/00—Protein-based fibres, e.g. animal fibres
    • D10B2211/20—Protein-derived artificial fibres

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention relates to the technical field of textile fabrics, in particular to an anti-static, flame-retardant and oil-proof washing cotton-hemp blended fabric and a preparation method and application thereof. A preparation method of an antistatic flame-retardant oil-proof washing cotton-hemp blended fabric at least comprises the following steps: (1) preparing a primary blended fabric: the blended fabric is prepared from fibrilia, cotton fiber and protein fiber by slivering, spinning and weaving; (2) dipping protease dipping liquid to obtain a first dipped fabric; (3) dipping the nano particle dipping solution to obtain a second dipped fabric; (4) and (4) treating the flame-retardant finishing liquid, and drying to obtain the flame-retardant finishing liquid. The fabric is soft and comfortable in hand feeling, has excellent antistatic, flame retardant and oil resistant performances, is a cotton-hemp blended fabric integrating multiple functions, and can be widely applied to the fields of clothing and home textiles.

Description

Anti-static flame-retardant oil-proof washing cotton-hemp blended fabric and preparation method thereof
Technical Field
The invention relates to the technical field of textile fabrics, in particular to an anti-static, flame-retardant and oil-proof washing cotton-hemp blended fabric and a preparation method and application thereof.
Background
The cotton-flax blended fabric has the comfort of cotton and the softness of flax, has bright color and luster and smooth and full hand feeling, and is deeply loved by wide consumers. However, the fibrilia in the cotton-linen blended fabric has strong affinity to oil stains, is easy to adsorb the oil stains, and is easy to generate static electricity to adsorb dust in the wearing process.
Static electricity can adsorb dust, is not beautiful, affects wearing comfort and is not easy to clean. In some special cases, static electricity can generate sparks, which can cause fire and even explosion accidents. The textile can be quickly burnt once encountering fire, and the textile is often burnt to cause fire due to negligence in daily life or industrial production.
In order to enhance the safety protection of personnel, higher requirements are put forward on the functions of the cotton-linen blended fabric. Aiming at the problems, the antistatic, flame retardant and oil-proof performances of the textile are widely researched at present. However, the common cotton-hemp blended fabric in the market generally has only single functions of static electricity prevention, flame retardance and oil resistance, and can only meet a part of requirements. Aiming at the special working fields, such as labor protection clothes of petroleum, electric power and coal mining industry, the development of the cotton-hemp blended fabric which can not only prevent static electricity, but also has the functions of flame retardance and oil resistance is urgently needed.
Therefore, aiming at the problems, the invention provides the antistatic flame-retardant oil-proof washing cotton-hemp blended fabric and the preparation method thereof, and the prepared cotton-hemp blended fabric has excellent antistatic, flame-retardant and oil-proof performances.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of an antistatic flame-retardant oil-proof washing cotton-hemp blended fabric, which at least comprises the following steps:
(1) preparing a primary blended fabric: the blended fabric is prepared from fibrilia, cotton fiber and protein fiber by slivering, spinning and weaving;
(2) dipping protease dipping solution: spreading the primary blended fabric, slowly adding a protease impregnation liquid, heating to 25-50 ℃, standing and soaking for 10-20min, taking out, repeatedly washing with clear water, placing in a 70-90 ℃ water tank for soaking for 0.2-1h, taking out, and drying at 60-100 ℃ for 2-5h to obtain a first impregnated fabric; the mass concentration of the protease solution is 0.1-0.3 wt%;
(3) dipping nano particle dipping solution: adding the first impregnated fabric into the nanoparticle impregnation liquid, heating to 50-70 ℃, standing and soaking for 10-20min, taking out, repeatedly washing with clear water, placing in a 70-90 ℃ water tank, soaking for 10-45min, taking out, and drying at 60-100 ℃ for 2-5h to obtain a second impregnated fabric;
(4) and (3) treating the flame-retardant finishing liquid: according to the bath ratio of 1: (20-40) weighing the flame-retardant finishing liquid, immersing the second dipped fabric into a container containing the finishing liquid, treating for 20-40min at 60-90 ℃, then carrying out two-dipping and two-rolling to keep the rolling residue rate at 90% -100%, taking out, and drying for 5-10h at 80-120 ℃ to obtain the flame-retardant finishing liquid.
As a preferable technical scheme of the present invention, the protein fiber is a graphene oxide modified protein fiber.
As a preferable technical scheme of the invention, the weight ratio of the cotton fiber, the fibrilia and the protein fiber is 1: (0.5-1): (0.1-0.5).
As a preferable technical scheme of the invention, the warp-wise density of the primary blended fabric is 450-600 pieces/10 cm; the weft density is 400-500 pieces/10 cm; the fiber thickness is 40-70D.
In a preferred embodiment of the present invention, the nanoparticle impregnating solution contains nanoparticles and an inorganic base.
As a preferable technical scheme of the invention, the nano particles are selected from one or more of nano silicon dioxide, nano titanium dioxide, nano zinc oxide, nano aluminum oxide and mica powder.
As a preferable technical scheme of the invention, the particle size of the nano particles is 10-50 nm.
As a preferable technical scheme, the nano particles are modified by aminosiloxane derivatives; the aminosilicone derivative contains at least 2 ether bonds.
The second aspect of the invention provides the antistatic flame-retardant oil-proof washing cotton-linen blended fabric prepared by the preparation method.
The third aspect of the invention provides an application of the antistatic flame-retardant oil-proof washing cotton-hemp blended fabric, which can be applied to the fields of clothing and home textiles.
The above-described and other features, aspects, and advantages of the present application will become more apparent with reference to the following detailed description.
Has the advantages that: the invention provides an antistatic flame-retardant oil-proof washing cotton-hemp blended fabric and a preparation method and application thereof. The cotton-linen blended fabric is prepared by four steps of preparing a primary blended fabric of fibrilia, cotton fiber and graphene oxide modified protein fiber, impregnating protease impregnating solution, impregnating nano particle impregnating solution and treating flame-retardant finishing solution. The fabric has excellent antistatic, flame-retardant and oil-proof performances, and can be widely applied to the fields of clothes and home textiles.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
"Polymer" means a polymeric compound prepared by polymerizing monomers of the same or different types. The generic term "polymer" embraces the terms "homopolymer", "copolymer", "terpolymer" and "interpolymer".
"interpolymer" means a polymer prepared by polymerizing at least two different monomers. The generic term "interpolymer" includes the term "copolymer" (which is generally used to refer to polymers prepared from two different monomers) and the term "terpolymer" (which is generally used to refer to polymers prepared from three different monomers). It also includes polymers made by polymerizing four or more monomers. "blend" means a polymer formed by two or more polymers being mixed together by physical or chemical means.
The invention provides a preparation method of an antistatic flame-retardant oil-proof washing cotton-hemp blended fabric, which at least comprises the following steps:
(1) preparing a primary blended fabric: the blended fabric is prepared from fibrilia, cotton fiber and protein fiber by slivering, spinning and weaving;
(2) dipping protease dipping solution: spreading the primary blended fabric, slowly adding a protease impregnation liquid, heating to 25-50 ℃, standing and soaking for 10-20min, taking out, repeatedly washing with clear water, placing in a 70-90 ℃ water tank for soaking for 0.2-1h, taking out, and drying at 60-100 ℃ for 2-5h to obtain a first impregnated fabric; the mass concentration of the protease solution is 0.1-0.3 wt%;
(3) dipping nano particle dipping solution: adding the first impregnated fabric into the nanoparticle impregnation liquid, heating to 50-70 ℃, standing and soaking for 10-20min, taking out, repeatedly washing with clear water, placing in a 70-90 ℃ water tank, soaking for 10-45min, taking out, and drying at 60-100 ℃ for 2-5h to obtain a second impregnated fabric;
(4) and (3) treating the flame-retardant finishing liquid: according to the bath ratio of 1: (20-40) weighing the flame-retardant finishing liquid, immersing the second dipped fabric into a container containing the finishing liquid, treating for 20-40min at 60-90 ℃, then carrying out two-dipping and two-rolling to keep the rolling residue rate at 90% -100%, taking out, and drying for 5-10h at 80-120 ℃ to obtain the flame-retardant finishing liquid.
In a preferred embodiment, the preparation method of the antistatic flame-retardant oil-proof washing cotton-hemp blended fabric at least comprises the following steps:
(1) preparing a primary blended fabric: the blended fabric is prepared from fibrilia, cotton fiber and protein fiber by slivering, spinning and weaving;
(2) dipping protease dipping solution: spreading the primary blended fabric, slowly adding a protease impregnation liquid, heating to 40 ℃, standing and soaking for 15min, taking out, repeatedly washing with clear water, placing in a 90 ℃ water tank for soaking for 0.5h, taking out, and drying at 100 ℃ for 5h to obtain a first impregnated fabric; the mass concentration of the protease solution is 0.15 wt%;
(3) dipping nano particle dipping solution: adding the first impregnated fabric into the nanoparticle impregnation liquid, heating to 60 ℃, standing and soaking for 15min, taking out, repeatedly washing with clear water, placing in a 90 ℃ water tank, soaking for 30min, taking out, and drying at 100 ℃ for 5h to obtain a second impregnated fabric;
(4) and (3) treating the flame-retardant finishing liquid: according to the bath ratio of 1: 30, weighing the flame-retardant finishing liquid, immersing the second dipped fabric into a container containing the finishing liquid, treating for 30min at 80 ℃, then carrying out two-time dipping and two-time rolling to keep the rolling residual rate at 90-100%, taking out, and drying for 10h at 100 ℃ to obtain the flame-retardant finishing liquid.
In the invention, the protein fiber is modified by graphene oxide.
Preferably, the protein fiber is modified porous graphene oxide modified protein fiber.
Preferably, the modified porous graphene oxide is an aminosiloxane derivative-modified porous graphene oxide.
Graphene oxide
In the invention, the preparation method of the porous graphene oxide comprises the following steps:
(1) preparing polystyrene nano-spheres:
introducing nitrogen to remove air in the three-mouth bottle at room temperature, adding deionized water and styrene monomer, continuously introducing nitrogen to remove air in the solution, and magnetically stirring for 20-40 min; gradually raising the temperature to 30-90 ℃, dissolving an initiator potassium persulfate in deionized water, then adding the solution into a three-necked bottle at one time, continuing to react for 10-24h, and centrifugally drying to obtain polystyrene spheres;
(2) preparing graphene oxide with a three-dimensional porous structure:
preparing graphene oxide into a solution with the concentration of 2-5g/L, ultrasonically mixing polystyrene spheres and the graphene oxide for 2-3h to form colloidal particles, adjusting the pH value of the solution to 6-8 to uniformly disperse the polystyrene nano spheres in the graphene oxide, performing suction filtration and drying, calcining at high temperature in a nitrogen environment to thermally decompose the polystyrene spheres and thermally reduce the graphene oxide to obtain the graphene oxide with a three-dimensional porous structure.
Preferably, the volume ratio of the deionized water to the styrene monomer in the step (1) is 10: (0.5-3), wherein the mass of the initiator is 0.2-1% of that of the styrene monomer.
Preferably, the mass ratio of the polystyrene to the graphene oxide in the step (2) is (2-5): 1; the temperature for calcining the polystyrene spheres by heat at high temperature is 300-550 ℃, and the calcining time is 1-2 h; the temperature of the high-temperature thermal reduction graphite oxide is 700-.
Preferably, the graphene oxide is not particularly limited, and may be obtained by purchase or preparation.
Preferably, the preparation method of the graphene oxide comprises the following steps: under the condition of ice-water bath, 30g of graphite powder and 15g of NaNO are mixed3And 900mL of concentrated H2SO4(H2SO498 percent of the mass fraction) is put into a three-neck flask and stirred for 0.5 h; then 90g KMnO was slowly added4Keeping the ice-water bath condition to continue stirring and reacting for 2 hours, and at the moment, changing the reactant from black to dark green; transferring the three-neck flask into a 35 ℃ constant temperature water bath, stirring for 3h, then dropwise adding 2000mL of distilled water, controlling the temperature not to exceed 98 ℃, and then continuing to react for 30min at 70 ℃ until the solution is yellow brown; then 100mL of 30% H2O2Adding the reactant and stirring for 30min, wherein the solution turns bright yellow; and (3) centrifugally washing by using 0.01mol/L HCl to remove metal ions in the solution, centrifugally washing by using absolute ethyl alcohol and deionized water respectively until the pH value of the filtrate is neutral, carrying out ultrasonic treatment, and carrying out freeze drying to obtain the product.
In a preferred embodiment, the preparation method of the porous graphene oxide comprises the following steps:
(1) adding 90mL of deionized water and 9mL of styrene monomer into a three-necked bottle, continuously introducing nitrogen to remove air in the solution, and magnetically stirring for 30 min; gradually raising the temperature to 70 ℃, and adding 10mL of 0.03g/mL potassium persulfate; continuously reacting for 24 hours, and centrifugally drying to obtain polystyrene spheres;
(2) ultrasonically stripping the prepared graphite oxide at room temperature to obtain a graphene oxide solution with the concentration of 5g/L, adding polystyrene spheres and the graphene oxide into the solution according to the mass ratio of 3:1, mixing and ultrasonically treating for 2h to form colloidal particles, adjusting the pH value to 8, uniformly dispersing the polystyrene nanospheres in the graphene oxide, filtering and drying, calcining at high temperature in a nitrogen environment to thermally decompose the polystyrene nanospheres, and thermally reducing the graphene oxide to obtain the porous graphene oxide.
In the invention, the modified porous graphene oxide is porous graphene oxide modified by aminosiloxane derivatives.
Preferably, the weight ratio of the aminosiloxane derivative to the porous graphene oxide is 1: (2-5).
Most preferably, the weight ratio of the aminosiloxane derivative to the porous graphene oxide is 1: 4.
preferably, the aminosiloxane derivative is one or more of N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine, 1, 3-bis (4-aminobutyl) tetramethyldisiloxane, 2-amino-1- (butyldimethylsiloxy) butane, 3-aminopropylbis (trimethylsiloxy) methylsilane, in combination.
Most preferably, the aminosiloxane derivative is N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine.
The N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine, CAS number: 49869-07-0.
In a preferred embodiment, the preparation method of the modified porous graphene oxide comprises the following steps: adding 5g of graphene oxide into 1.5L of absolute ethyl alcohol, performing ultrasonic dispersion for 10min, adding an aminosiloxane derivative with a certain mass ratio, continuing to perform ultrasonic dispersion for 1h, adding the dispersion into a three-neck flask, and performing magnetic stirring reaction for 24h at 80 ℃; cooling the product to room temperature, centrifugally washing the product with absolute ethyl alcohol for 6 times, and then washing the product with distilled water for 1 time to remove residual aminosiloxane derivatives; and completely drying the product at 60 ℃ to obtain the aminosiloxane derivative modified porous graphene oxide.
In a more preferred embodiment, the preparation method of the modified porous graphene oxide comprises the following steps: adding 5g of graphene oxide into 1.5L of absolute ethyl alcohol, performing ultrasonic dispersion for 10min, adding 20g of N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine, continuing to perform ultrasonic dispersion for 1h, adding the dispersion into a three-neck flask, and performing magnetic stirring reaction at 80 ℃ for 24 h; after the product was cooled to room temperature, it was washed 6 times by centrifugation with anhydrous ethanol and 1 time with distilled water to remove the residual N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine; and completely drying the product at the temperature of 60 ℃ to obtain the N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine modified porous graphene oxide.
Modified protein fiber
In the invention, the addition amount of the modified porous graphene oxide is 2-6% of the total mass of the modified protein fiber.
Preferably, the addition amount of the modified porous graphene oxide is 5% of the total mass of the modified protein fiber.
Preferably, the blending spinning process of the modified porous graphene oxide modified protein fiber comprises the following steps:
(1) melting: taking a certain amount of protein fiber and modified porous graphene oxide as raw materials according to a mass ratio, and melting the raw materials into spinning solution by a screw;
(2) metering and spinning: the spinning stock solution is sprayed out of a 12-hole spinneret plate for spinning and forming after the flow of the spinning stock solution is regulated by a metering pump, so that a modified protein fiber bundle is prepared; a slow cooling heating device is arranged below the spinneret plate; the temperature of the slow cooling heating device is 8-12 ℃ higher than the plate surface temperature of the spinneret plate;
(3) cooling and oiling: performing circular air blowing cooling on the modified protein fiber bundle by hot air equipment, and then performing double-oil-nozzle oiling treatment by adopting a polyester oiling agent, wherein the oiling rate is 0.85-0.95;
(4) pre-networking: pre-networking the oiled modified protein fiber bundle by a pre-networking device;
(5) stretching and shaping: adopting three pairs of rollers to stretch and shape the pre-networked modified protein fiber bundle, wherein the stretching multiple is 1.75-1.85;
(6) a main network: carrying out main networking on the stretched and shaped modified protein fiber bundle by a main networking device;
(7) winding: and (3) fully automatically winding the modified protein fiber bundle passing through the main network at the winding speed of 2450-2500m/min to obtain a modified protein fiber finished product.
Preferably, in the step (1), the temperature at the time of melting is 272 ℃ to 275 ℃.
Preferably, in the step (2), the temperature of the plate surface of the spinneret plate is controlled to be between 293 ℃ and 295 ℃.
Preferably, in the step (2), the diameter of the spinneret plate is 0.13 mm.
Preferably, in the step (3), the air temperature of the hot air device for air-cooling the modified protein fiber bundle is 20 ℃ +/-1 ℃.
Preferably, in the step (5), the temperatures of the three pairs of rollers during the stretching and setting are respectively: 90-100 ℃, 120-130 ℃ and 210-220 ℃.
More preferably, in the step (5), the temperatures of the three pairs of rolls during the stretching and setting are respectively: 95 ℃, 125 ℃ and 215 ℃.
In a preferred embodiment, the modified porous graphene oxide modified protein fiber blend spinning process comprises the following steps:
(1) melting: weighing 95 parts of protein fiber and 5 parts of modified graphene oxide as raw materials in parts by mass, and melting the raw materials by a screw to form a spinning solution; the temperature at the time of the melting was 275 ℃;
(2) metering and spinning: the spinning stock solution is sprayed out of a 12-hole spinneret plate for spinning and forming after the flow of the spinning stock solution is regulated by a metering pump, so that a modified protein fiber bundle is prepared; a slow cooling heating device is arranged below the spinneret plate; the temperature of the slow cooling heating device is 10 ℃ higher than the plate surface temperature of the spinneret plate; the plate surface temperature of the spinneret plate is 295 ℃; the aperture of the spinneret plate is 0.13 mm;
(3) cooling and oiling: performing circular air blowing cooling on the modified protein fiber bundle by hot air equipment, and then performing double-oil-nozzle oiling treatment by adopting a polyester oiling agent, wherein the oiling rate is 0.9; the air temperature of the hot air equipment is 20 ℃ when the modified protein fiber bundle is cooled by blowing air;
(4) pre-networking: pre-networking the oiled modified protein fiber bundle by a pre-networking device;
(5) stretching and shaping: stretching and shaping the pre-networked modified protein fiber bundle by three pairs of rollers, wherein the stretching ratio is 1.85; the temperatures of the three pairs of rollers during stretching and setting are respectively as follows: 95 ℃, 125 ℃ and 215 ℃;
(6) a main network: carrying out main networking on the stretched and shaped modified protein fiber bundle by a main networking device;
(7) winding: and (3) fully automatically winding the modified protein fiber bundle passing through the main network at a winding speed of 2450m/min to obtain a modified protein fiber finished product.
The natural protein fiber is adopted, so that the natural protein fiber has soft hand feeling, soft luster, excellent moisture absorption, moisture conduction and heat preservation performance, good skin affinity, obvious antibacterial function and especially excellent characteristics of very soft and good moisture absorption effect. The invention can well improve the softness and skin-friendly property of the cotton and linen fibers by selecting the protein fibers to be blended with the cotton fibers and the linen fibers. However, the protein fiber and the cotton and hemp fiber are easy to break the cotton net in the blending process, which causes the poor quality of the textile. The inventor selects the aminosiloxane modified graphene oxide to modify the terylene, so that the antistatic effect can be effectively improved, and the quality and the softness of the fiber can be remarkably improved. The inventors consider that possible reasons are: the graphene oxide can conduct and disperse charges, so that the accumulation of the charges is avoided, and the antistatic effect is improved; the aminosiloxane modifies the graphene oxide, particularly the selected N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine has a special claw-shaped structural characteristic, each claw contains a plurality of oxygen atoms, the structural monomer is attached to the surface of the polyester fiber, and the protein fiber has more polar groups, so that the cohesive force of the polyester fiber on the protein fiber can be improved in the blending process, the quality uniformity of the blended fiber is improved, and the quality of a product is improved.
Primary blended fabric
In the invention, the weight ratio of the cotton fiber, the fibrilia and the protein fiber is 1: (0.5-1): (0.1-0.5).
Preferably, the weight ratio of the cotton fibers, the hemp fibers and the protein fibers is 1: 0.8: 0.25.
the primary blended fabric is prepared from fibrilia, cotton fiber and protein fiber through the processes of slivering, spinning, weaving and the like.
Preferably, the protein fiber can be selected from milk fiber or/and soybean protein fiber.
In the invention, the composition of the warp and the weft in the primary blended fabric is the same, and the warp and the weft are blended by fibrilia, cotton fiber and protein fiber.
In the invention, the warp density of the primary blended fabric is 450-600 pieces/10 cm; the weft density is 400-500 pieces/10 cm; the fiber thickness is 40-70D.
Preferably, the warp density of the primary blended fabric is 550 threads/10 cm; the weft density is 450 pieces/10 cm; the fiber thickness was 60D.
Protease impregnation liquid
In the invention, the prepared blended fabric is impregnated by the impregnating solution, and the impregnating method comprises the following steps: and (3) paving the primary blended fabric, slowly adding 0.15 wt% of protease impregnation liquid, heating to 40 ℃, standing and soaking for 15min, taking out, repeatedly washing with clear water, placing in a 90 ℃ water tank for soaking for 0.5h, taking out, and drying at 100 ℃ for 5h to obtain the first impregnated fabric.
According to the invention, cotton fibers, fibrilia and protein fibers are blended, and the blended fabric is soaked in the special soaking solution by the inventor, so that the comfortable softness of the fabric can be further improved, and the air permeability of the fabric can be effectively improved. The inventors believe that this may be due to the specific impregnation of the fabric with the enzyme solution of the present invention. The protease is utilized to carry out degradation action to certain degree on protein fibers in the fabric to generate more three-dimensional void structures on the surfaces of the fibers, so that the air permeability of the fabric can be improved. Meanwhile, the surface of the fabric is also provided with a plurality of microporous structures, namely micropores generated on the surface of the fiber, so that the internal structure of the fiber can generate looseness to a certain extent, and the fabric is softer and more comfortable.
Nanoparticle impregnating solution
In the invention, the prepared blended fabric is impregnated by the impregnating solution, and the impregnating method comprises the following steps: adding the first impregnated fabric into the nanoparticle impregnation liquid, heating to 60 ℃, standing and soaking for 15min, taking out, repeatedly washing with clear water, placing in a 90 ℃ water tank, soaking for 30min, taking out, and drying at 100 ℃ for 5h to obtain a second impregnated fabric.
In the present invention, the nanoparticle impregnating solution contains nanoparticles and an inorganic base.
In the invention, the nano particles are selected from one or more of nano silicon dioxide, nano titanium dioxide, nano zinc oxide, nano aluminum oxide and mica powder.
Preferably, the nano particles are selected from one or more of nano silicon dioxide, nano titanium dioxide and nano zinc oxide.
Most preferably, the nanoparticles are selected from nanosilica.
In the present invention, the inorganic base is selected from one or more of sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide, aluminum hydroxide, lithium hydroxide, magnesium hydroxide, zinc hydroxide, copper hydroxide, iron hydroxide, lead hydroxide, cobalt hydroxide, chromium hydroxide, zirconium hydroxide, nickel hydroxide, ammonium hydroxide, soda ash (anhydrous sodium carbonate), sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, potassium phosphate, and sodium sulfate.
Preferably, the inorganic base is sodium hydroxide.
In the invention, the preparation method of the nanoparticle impregnating solution comprises the following steps: adding the nano particles into the alkaline solution, fully stirring and uniformly mixing to obtain the nano particle impregnation liquid.
Preferably, the alkaline solution is an aqueous sodium hydroxide solution.
More preferably, the concentration of the aqueous sodium hydroxide solution is 0.1 to 0.5 g/mL.
Most preferably, the concentration of the aqueous sodium hydroxide solution is 0.3 g/mL.
Preferably, the concentration of nanoparticles in the nanoparticle-impregnating solution is 0.1 to 0.3 g/mL.
Most preferably, the concentration of nanoparticles in the nanoparticle impregnating solution is 0.25 g/mL.
Preferably, the particle size of the nanoparticles is 10-50 nm.
Most preferably, the nanoparticles have a particle size of 20nm and are available from Shanghai Ulowei nanotechnology, Inc.
In the invention, the nano particles are modified by aminosiloxane derivatives.
Preferably, the aminosilicone derivative contains at least 2 ether linkages.
More preferably, the aminosiloxane derivative is one or a combination of N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine, 1, 3-bis (4-aminobutyl) tetramethyldisiloxane, 2-amino-1- (butyldimethylsiloxy) butane, 3-aminopropylbis (trimethylsiloxy) methylsilane.
Most preferably, the aminosiloxane derivative is N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine.
In the invention, the preparation method of the modified silica nanoparticle comprises the following steps:
(1) adding deionized water into ethanol, and uniformly oscillating by ultrasonic to obtain a solution 1;
(2) under ultrasonic oscillation, adding tetraethoxysilane (TEOS for short) into the solution 1, wherein the molar ratio of tetraethoxysilane to ethanol is 1: (50-100), wherein the molar ratio of the ethyl orthosilicate to the deionized water is 1: (4-8), uniformly oscillating by ultrasonic to obtain a solution 2;
(3) adjusting the pH value of the solution 2 to 3-5 by hydrochloric acid, dropwise adding N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine into the solution 2 at the speed of 0.5-1.0g/min to obtain a reaction system, wherein the using amount of the N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine is 5% -20% of the mass of ethyl orthosilicate, and stirring and reacting the obtained reaction system at the reaction temperature of 40-60 ℃ for 4-6h to obtain a solution 3;
(4) adjusting the pH value of the solution 3 to 7-10 by ammonia water, and reacting for 1-4h under the condition of heat preservation to obtain modified nano-silica sol;
(5) drying, crushing, screening, centrifugally washing with absolute ethyl alcohol, washing with water, vacuum drying and grinding the modified nano-silica sol to obtain the in-situ modified nano-silica.
Preferably, in the step (3), the concentration of the hydrochloric acid solution is 0.1 mol/L; the N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine was added dropwise to the solution using a constant pressure funnel.
Preferably, in the step (4), the concentration of the ammonia water is 0.05 mol/L.
Preferably, in the step (5), the vacuum drying is performed under the specific condition of 40-80 ℃ for 10-24 h.
In a preferred embodiment, the modified silica nanoparticles are prepared by the following steps:
(1) adding deionized water into ethanol, and uniformly oscillating by ultrasonic to obtain a solution 1;
(2) under ultrasonic oscillation, adding tetraethoxysilane (TEOS for short) into the solution 1, wherein the molar ratio of tetraethoxysilane to ethanol is 1: 80, the molar ratio of the ethyl orthosilicate to the deionized water is 1: 6, uniformly oscillating by ultrasonic to obtain a solution 2;
(3) adjusting the pH value of the solution 2 to be 4 by using hydrochloric acid with the concentration of 0.1mol/L, dropwise adding N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine into the solution 2 through a constant pressure funnel at the speed of 0.8g/min to obtain a reaction system, wherein the using amount of the N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine is 15% of the mass of tetraethoxysilane, and stirring and reacting the obtained reaction system at the reaction temperature of 50 ℃ for 6 hours to obtain a solution 3;
(4) keeping the pH value of the solution 3 at 8 by using ammonia water with the concentration of 0.05mol/L, and reacting for 4 hours under the condition of heat preservation to obtain modified nano-silica sol;
(5) drying, crushing and screening the modified nano-silica sol, centrifugally washing with absolute ethyl alcohol, washing with water, drying in vacuum at 80 ℃ for 24 hours, and grinding to obtain the in-situ modified nano-silica.
According to the invention, the oil resistance of the cotton and linen fabric is improved by introducing the nano silicon dioxide particles, but the inventor finds that although the oil resistance of the cotton and linen fibers can be improved to a certain extent by the introduced nano silicon dioxide particles, the oil resistance of the cotton and linen fabric is reduced with the increase of the washing times of the cotton and linen fabric. After the N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine is used for modifying the nano silicon dioxide, the washing resistance of the cotton and linen fabric can be effectively improved, and the fabric is ensured to have excellent oil-proof performance after being washed for many times. The inventors believe that this may be due to the N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine itself having abundant ether linkages and amino groups which may further increase the oil repellency of textiles. In addition, the modified nano silicon dioxide can be dispersed in a three-dimensional microporous structure generated after the textile fabric is treated by protease in the dipping process, and the N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine has special claw-shaped structural characteristics, and each claw is respectively provided with a plurality of oxygen atoms, so that the whole oil resistance can be further improved; because a plurality of claws can firmly lock the modified nano silicon dioxide in gaps of the cotton and linen fabric, the water washing resistance of the fabric is effectively improved.
Flame-retardant finishing liquid
In the invention, the second impregnated fabric prepared by the method is subjected to flame-retardant finishing liquid treatment, and the treatment method comprises the following steps: according to the bath ratio of 1: 30, weighing the flame-retardant finishing liquid, immersing the second dipped fabric into a container containing the finishing liquid, treating for 30min at 80 ℃, then carrying out two-time dipping and two-time rolling to keep the rolling residual rate at 90-100%, taking out, and drying for 8h at 120 ℃ to obtain the flame-retardant finishing liquid.
According to the invention, the flame-retardant finishing liquid comprises a poly-type phosphorus-nitrogen intumescent flame retardant and trimethyl silicic acid caged thioPEPA ester; the polymeric phosphorus-nitrogen intumescent flame retardant is poly (trimethylolpropane thiophosphoryl urea).
Poly (trimethylolpropane thiophosphoryl urea)
The poly (trimethylolpropane thiophosphoryl urea) is called PDTPT for short.
The preparation method of the poly-ditrimethylolpropane thiophosphoryl urea comprises the following steps:
(1) synthesis of intermediate ditrimethylolpropane diphosphoryl chloride (DTDC)
Adding Ditrimethylolpropane (DTMP) and dichloroethane as solvent in a certain proportion into a four-mouth flask, slowly heating to 40 deg.C under electric stirring, adding POCl after DTMP is completely dissolved3Absorbing HCl gas generated by the reaction with alkali liquor, keeping the temperature for reaction for 6 hours, cooling to room temperature after the reaction is finished, and removing dichloroethane and unreacted POCl by reduced pressure distillation3And adding a certain amount of absolute ethyl alcohol into the obtained white solid crude product, placing the obtained product in a freezer (-20 ℃) for 2 hours, filtering the obtained white solid, and drying the obtained white solid at 70 ℃ in vacuum to constant weight to obtain white powdery solid DTDC.
(2) Synthesis of poly (trimethylolpropane thiophosphoryl urea)
Adding a certain amount of DTDC and acetonitrile serving as a solvent into a flask, heating, adding thiourea in a certain proportion after the DTDC is completely dissolved, heating to 80 ℃, carrying out heat preservation reaction for 6 hours, cooling to room temperature after the reaction is finished, filtering to remove a white byproduct, distilling the solution under reduced pressure to evaporate the acetonitrile serving as the solvent, and drying the obtained yellow sticky substance at 120 ℃ for 12 hours to obtain yellow crystal PDTPT.
Preferably, in the step (1), the mass ratio of the dichloroethane solvent to the DTMP solvent is 2.0: 1.
preferably, in step (1), the DTMP and POCl are3In a molar ratio of 1: 2.2.
preferably, in the step (2), the mass ratio of the solvent acetonitrile to DTDC is 2.0: 1.
preferably, in the step (2), the molar ratio of the thiourea to the DTDC is 1.2: 1.
trimethylsilicic acid caged thioPEPA ester
The trimethyl silicic acid caged thioPEPA ester is short for TMSSPE
The preparation method of the trimethyl silicic acid caged thioPEPA ester comprises the following steps:
(1) preparation of 4-hydroxymethyl-1-thio-1-phospha-2, 6, 7-trioxabicyclo [2,2,2] -octane (SPEPA)
10mol of pentaerythritol and 10mol of trichlorothion were charged into a 1000mL four-necked flask equipped with a thermometer and a reflux condenser. The reaction mixture was heated with stirring in an oil bath at an external bath temperature of 145-160 deg.C and was maintained at this temperature until no hydrogen chloride gas was evolved (as detected by pH paper), which took about 8 h. Then raising reaction temperature to about 170 deg.C, heating for 1h, cooling to obtain block solid, extracting with 20L boiling water for four times, and removing sticky substance deposited on the bottom of the bottle by decantation. In the cooled aqueous solution, a large amount of white solid was precipitated and filtered. Heating the mother liquor to evaporate most of water to obtain a plurality of white solids, drying the white solids obtained twice, and recrystallizing with dimethylbenzene to obtain white flaky crystals.
(2) Preparation of caged thiopepa trimethylsilanoate
In a 1000mL four-mouth reaction bottle provided with a stirrer, a thermometer, a condenser tube and a hydrogen chloride (HCl) absorption device, nitrogen is used for completely removing air in the bottle, 196.0-276.5g (1.0-1.4mol) SPEPA and 800mL dioxane are added at room temperature, stirring is carried out to completely dissolve SPEA, 108.6g (1.0mol) Trimethylchlorosilane (TMCS) is slowly dripped, the system temperature is not higher than 20 ℃ in the dripping process, after dripping is finished, reaction is carried out at 30-50 ℃ for 9 hours under heat preservation, after HCl gas is discharged, the pH value of the system is adjusted to 5-6 by melamine, suction filtration is carried out, and organic solvent is removed from filtrate by a reduced pressure distillation method; washing the obtained solid powder with ethanol, filtering, and vacuum drying.
Preferably, in the step (1), the molar ratio of the pentaerythritol to the trichloro-sulfur is 1: 1.
preferably, in step (2), the molar ratio of SPEPA to TMCS is 1.2: 1.
in the invention, the mass ratio of the poly (trimethylolpropane thiophosphoryl urea) to the trimethyl silicic acid caged thioPEPA ester is 1: (0.6-2.5).
Preferably, the mass ratio of the poly (trimethylolpropane thiophosphoryl urea) to the trimethyl silicic acid caged thioPEPA ester is 1: 1.8.
in the invention, the mass concentration of the flame retardant in the finishing liquid is 50-200 g/L.
Preferably, the mass concentration of the flame retardant in the finishing liquid is 100 g/L.
In a preferred embodiment, the finishing liquid is prepared by the following method: 50g of PDTPT and 60g of TMSSPE are weighed in a container according to the mass ratio respectively, 1.1L of ethanol is added to dissolve the PDTPT and the TMSSPE to prepare finishing liquid, and the finishing liquid is placed in a water bath kettle at the temperature of 80 ℃ for heat preservation.
In a preferred embodiment, the process of treating the modified polyester base fabric by the finishing liquid comprises the following steps: according to the bath ratio of 1: 30, weighing finishing liquid, immersing the modified polyester base fabric into a container containing the finishing liquid, treating for 30min at 80 ℃, then carrying out two-time soaking and two-time rolling to keep the rolling residual rate at 90-100%, taking out, and drying for 10h at 100 ℃ to obtain the polyester fabric.
The inventors found that when the content of the modified graphene oxide in the soy protein fiber is too high, the thermal stability is reduced due to the fact that the thermal conductivity of the graphene oxide is excellent, and the heat transfer rate of the graphene oxide is increased. The inventor finds that the PDTPT and the TMSSPE are selected for compounding in the invention, so that the thermal stability of the thermal fabric can be improved, and the fabric has good fireproof and flame-retardant properties. Especially when the fabric is subjected to local high temperature, the fabric has excellent thermal stability and flame-retardant self-extinguishing property, and the human body can not hurt the skin because the fabric is heated. The inventors consider that possible reasons are: the-N-H in the PDTPT and the oxygen in the TMSSPE form a hydrogen bond to play a role of a coupling agent, so that the small molecular TMSSPE is uniformly distributed around the polymer PDTPT to form the uniformly dispersed blending finishing liquid. The PDTPT finally forms a porous foam carbon layer, so that internal fibers are effectively protected, and the overall thermal stability of the fabric is improved. Meanwhile, when the fabric is in a high-temperature environment for a long time, and heat is transferred to the inner layer through the outer expanded carbon layer, the amide bond of the N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine of the modified graphene oxide is broken under the high-temperature condition, and a C-Si-O-C protective layer is formed on the inner layer of the expanded carbon layer, so that the inward transfer of heat is further blocked, and the thermal stability and the flame retardant property of the fabric are improved.
The second aspect of the invention provides the antistatic flame-retardant oil-proof washing cotton-linen blended fabric prepared by the preparation method.
The third aspect of the invention provides an application of the antistatic flame-retardant oil-proof washing cotton-hemp blended fabric, which can be applied to the fields of clothing and home textiles.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the raw materials used are commercially available from national chemical reagents, unless otherwise specified.
Examples
In the following examples:
1. the preparation method of the modified porous graphene oxide comprises the following steps: adding 5g of porous graphene oxide into 1.5L of absolute ethyl alcohol, performing ultrasonic dispersion for 10min, adding N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine with a certain mass ratio, continuing to perform ultrasonic dispersion for 1h, adding the dispersion into a three-neck flask, and performing magnetic stirring reaction at 80 ℃ for 24 h; after the product was cooled to room temperature, it was washed 6 times by centrifugation with anhydrous ethanol and 1 time with distilled water to remove the residual N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine; and completely drying the product at 60 ℃ to obtain the modified porous graphene oxide.
2. The blending spinning process of the modified porous graphene oxide modified protein fiber comprises the following steps:
(1) melting: weighing protein fibers and modified porous graphene oxide as raw materials in parts by mass, and melting the raw materials by a screw to form a spinning solution; the temperature at the time of the melting was 275 ℃;
(2) metering and spinning: the spinning stock solution is sprayed out of a 12-hole spinneret plate for spinning and forming after the flow of the spinning stock solution is regulated by a metering pump, so that a modified protein fiber bundle is prepared; a slow cooling heating device is arranged below the spinneret plate; the temperature of the slow cooling heating device is 10 ℃ higher than the plate surface temperature of the spinneret plate; the plate surface temperature of the spinneret plate is 295 ℃; the aperture of the spinneret plate is 0.13 mm;
(3) cooling and oiling: performing circular air blowing cooling on the modified protein fiber bundle by hot air equipment, and then performing double-oil-nozzle oiling treatment by adopting a polyester oiling agent, wherein the oiling rate is 0.9; the air temperature of the hot air equipment is 20 ℃ when the modified protein fiber bundle is cooled by blowing air;
(4) pre-networking: pre-networking the oiled modified protein fiber bundle by a pre-networking device;
(5) stretching and shaping: stretching and shaping the pre-networked modified protein fiber bundle by three pairs of rollers, wherein the stretching ratio is 1.85; the temperatures of the three pairs of rollers during stretching and setting are respectively as follows: 95 ℃, 125 ℃ and 215 ℃;
(6) a main network: carrying out main networking on the stretched and shaped modified protein fiber bundle by a main networking device;
(7) winding: and (3) fully automatically winding the modified protein fiber bundle passing through the main network at a winding speed of 2450m/min to obtain a modified protein fiber finished product.
3. The preparation method of the modified silicon dioxide nano particle comprises the following steps:
(1) adding deionized water into ethanol, and uniformly oscillating by ultrasonic to obtain a solution 1;
(2) under ultrasonic oscillation, adding Tetraethoxysilane (TEOS) into the solution 1, wherein the molar ratio of tetraethoxysilane to ethanol is 1: 80, the molar ratio of the ethyl orthosilicate to the deionized water is 1: 6, uniformly oscillating by ultrasonic to obtain a solution 2;
(3) adjusting the pH value of the solution 2 to be 4 by using hydrochloric acid with the concentration of 0.1mol/L, dropwise adding N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine into the solution 2 through a constant pressure funnel at the speed of 0.8g/min to obtain a reaction system, wherein the using amount of the N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine is 15% of the mass of tetraethoxysilane, and stirring and reacting the obtained reaction system at the reaction temperature of 50 ℃ for 6 hours to obtain a solution 3;
(4) keeping the pH value of the solution 3 at 8 by using ammonia water with the concentration of 0.05mol/L, and reacting for 4 hours under the condition of heat preservation to obtain modified nano-silica sol;
(5) drying, crushing and screening the modified nano-silica sol, centrifugally washing with absolute ethyl alcohol, washing with water, drying in vacuum at 80 ℃ for 24 hours, and grinding to obtain the in-situ modified nano-silica.
4. The preparation method of the flame-retardant finishing liquid comprises the following steps: respectively weighing a certain amount of PDTPT and TMSSPE in a container according to the mass ratio, adding ethanol in proportion to dissolve the PDTPT and the TMSSPE to prepare flame-retardant finishing liquid with a certain concentration, and placing the flame-retardant finishing liquid in a water bath kettle at 80 ℃ for heat preservation.
Example 1
Embodiment 1 provides a method for preparing an antistatic flame-retardant oil-proof washing cotton-hemp blended fabric, which at least comprises the following steps:
(1) preparing a primary blended fabric: the blended fabric is prepared from fibrilia, cotton fiber and protein fiber by slivering, spinning and weaving;
(2) dipping protease dipping solution: spreading the primary blended fabric, slowly adding a protease impregnation liquid, heating to 40 ℃, standing and soaking for 15min, taking out, repeatedly washing with clear water, placing in a 90 ℃ water tank for soaking for 0.5h, taking out, and drying at 100 ℃ for 5h to obtain a first impregnated fabric;
(3) dipping nano particle dipping solution: adding the first impregnated fabric into the nanoparticle impregnation liquid, heating to 60 ℃, standing and soaking for 15min, taking out, repeatedly washing with clear water, placing in a 90 ℃ water tank, soaking for 30min, taking out, and drying at 100 ℃ for 5h to obtain a second impregnated fabric;
(4) and (3) treating the flame-retardant finishing liquid: according to the bath ratio of 1: 30, weighing the flame-retardant finishing liquid, immersing the second dipped fabric into a container containing the finishing liquid, treating for 30min at 80 ℃, then carrying out two-time dipping and two-time rolling to keep the rolling residual rate at 90-100%, taking out, and drying for 10h at 100 ℃ to obtain the flame-retardant finishing liquid.
In the step (1), the weight ratio of the cotton fibers, the fibrilia and the protein fibers is 1: 0.5: 0.1; the protein fiber is soybean protein fiber modified by modified porous graphene oxide; the adding amount of the modified porous graphene oxide is 2% of the total mass of the modified protein fiber; the ratio of N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine to porous graphene oxide in the modified porous graphene oxide is 1: 2; the warp density of the primary blended fabric is 450 pieces/10 cm; the weft density is 400 pieces/10 cm; the fiber thickness was 40D.
In the step (2), the concentration of the protease dipping solution is 0.1 wt%.
In the step (3), the concentration of the nanoparticle impregnation solution is 0.1 g/mL; the nano particles are silicon dioxide particles with the particle size of 10 nm.
In the step (4), the mass ratio of poly (trimethylolpropane thiophosphoryl urea) to trimethylsilyl caged thioPEPA ester in the flame-retardant finishing liquid is 1: 0.6; the mass concentration of the flame retardant in the finishing liquid is 50 g/L.
Example 2
Embodiment 2 provides a method for preparing an antistatic flame-retardant oil-proof washing cotton-hemp blended fabric, which at least comprises the following steps:
(1) preparing a primary blended fabric: the blended fabric is prepared from fibrilia, cotton fiber and protein fiber by slivering, spinning and weaving;
(2) dipping protease dipping solution: spreading the primary blended fabric, slowly adding a protease impregnation liquid, heating to 40 ℃, standing and soaking for 15min, taking out, repeatedly washing with clear water, placing in a 90 ℃ water tank for soaking for 0.5h, taking out, and drying at 100 ℃ for 5h to obtain a first impregnated fabric;
(3) dipping nano particle dipping solution: adding the first impregnated fabric into the nanoparticle impregnation liquid, heating to 60 ℃, standing and soaking for 15min, taking out, repeatedly washing with clear water, placing in a 90 ℃ water tank, soaking for 30min, taking out, and drying at 100 ℃ for 5h to obtain a second impregnated fabric;
(4) and (3) treating the flame-retardant finishing liquid: according to the bath ratio of 1: 30, weighing the flame-retardant finishing liquid, immersing the second dipped fabric into a container containing the finishing liquid, treating for 30min at 80 ℃, then carrying out two-time dipping and two-time rolling to keep the rolling residual rate at 90-100%, taking out, and drying for 10h at 100 ℃ to obtain the flame-retardant finishing liquid.
In the step (1), the weight ratio of the cotton fibers, the fibrilia and the protein fibers is 1: 1: 0.5; the protein fiber is soybean protein fiber modified by modified porous graphene oxide; the addition amount of the modified porous graphene oxide is 6% of the total mass of the modified protein fiber; the ratio of N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine to porous graphene oxide in the modified porous graphene oxide is 1: 5; the warp density of the primary blended fabric is 600 pieces/10 cm; the weft density is 450 pieces/10 cm; the fiber thickness was 70D.
In the step (2), the concentration of the protease dipping solution is 0.3 wt%.
In the step (3), the concentration of the nanoparticle impregnation liquid is 0.3 g/mL; the nano particles are silicon dioxide particles with the particle size of 50 nm.
In the step (4), the mass ratio of poly (trimethylolpropane thiophosphoryl urea) to trimethylsilyl caged thioPEPA ester in the flame-retardant finishing liquid is 1: 2.5; the mass concentration of the flame retardant in the finishing liquid is 200 g/L.
Example 3
Embodiment 3 provides a method for preparing an antistatic flame-retardant oil-proof washing cotton-hemp blended fabric, which at least comprises the following steps:
(1) preparing a primary blended fabric: the blended fabric is prepared from fibrilia, cotton fiber and protein fiber by slivering, spinning and weaving;
(2) dipping protease dipping solution: spreading the primary blended fabric, slowly adding a protease impregnation liquid, heating to 40 ℃, standing and soaking for 15min, taking out, repeatedly washing with clear water, placing in a 90 ℃ water tank for soaking for 0.5h, taking out, and drying at 100 ℃ for 5h to obtain a first impregnated fabric;
(3) dipping nano particle dipping solution: adding the first impregnated fabric into the nanoparticle impregnation liquid, heating to 60 ℃, standing and soaking for 15min, taking out, repeatedly washing with clear water, placing in a 90 ℃ water tank, soaking for 30min, taking out, and drying at 100 ℃ for 5h to obtain a second impregnated fabric;
(4) and (3) treating the flame-retardant finishing liquid: according to the bath ratio of 1: 30, weighing the flame-retardant finishing liquid, immersing the second dipped fabric into a container containing the finishing liquid, treating for 30min at 80 ℃, then carrying out two-time dipping and two-time rolling to keep the rolling residual rate at 90-100%, taking out, and drying for 10h at 100 ℃ to obtain the flame-retardant finishing liquid.
In the step (1), the weight ratio of the cotton fibers, the fibrilia and the protein fibers is 1: 0.8: 0.25; the protein fiber is soybean protein fiber modified by modified porous graphene oxide; the addition amount of the modified porous graphene oxide is 5% of the total mass of the modified protein fiber; the ratio of N- [3- [ tri (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine to porous graphene oxide in the modified porous graphene oxide is 1: 4; the warp density of the primary blended fabric is 550 threads/10 cm; the weft density is 450 pieces/10 cm; the fiber thickness was 60D.
In the step (2), the concentration of the protease dipping solution is 0.15 wt%.
In the step (3), the concentration of the nanoparticle impregnation liquid is 0.25 g/mL; the nano particles are silica particles with the particle size of 20 nm.
In the step (4), the mass ratio of poly (trimethylolpropane thiophosphoryl urea) to trimethylsilyl caged thioPEPA ester in the flame-retardant finishing liquid is 1: 1.8; the mass concentration of the flame retardant in the finishing liquid is 100 g/L.
Example 4
Example 4 differs from example 3 in that the protein fibres are unmodified.
Example 5
Example 5 differs from example 3 in that the protein fiber is a porous graphene oxide-modified protein fiber.
Example 6
Example 6 differs from example 3 in that the protein fiber is a graphene oxide modified protein fiber.
Example 7
Example 7 differs from example 3 in that the protein fiber is a modified porous graphene oxide-modified protein fiber; the modified porous graphene oxide is octadecylamine-modified porous graphene oxide.
Example 8
Example 8 differs from example 3 in that the ratio of N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine to porous graphene oxide in the modified porous graphene oxide is 1: 0.1.
example 9
Example 9 differs from example 3 in that the ratio of N- [3- [ tris (2-methoxyethoxy) silyl ] propyl ] ethane-1, 2-diamine to porous graphene oxide in the modified porous graphene oxide is 1: 10.
example 10
Example 8 differs from example 3 in that the protein fiber is a modified porous graphene oxide-modified protein fiber; the addition amount of the modified porous graphene oxide is 0.5% of the total mass of the modified protein fiber.
Example 11
Example 9 differs from example 3 in that the protein fiber is a modified porous graphene oxide-modified protein fiber; the addition amount of the modified porous graphene oxide is 20% of the total mass of the modified protein fiber.
Example 12
Example 12 differs from example 3 in that the weight ratio of cotton fibers, hemp fibers and protein fibers is 1: 0.1: 0.05.
example 13
Example 13 differs from example 3 in that the weight ratio of cotton fibers, hemp fibers and protein fibers is 1: 3: 2.
example 14
Example 14 differs from example 3 in that the fiber thickness was 10D.
Example 15
Example 15 differs from example 3 in that the fiber thickness was 100D.
Example 16
Example 16 differs from example 3 in that the warp density of the preliminary blended fabric was 300 threads/10 cm; the weft density was 200 pieces/10 cm.
Example 17
Example 17 differs from example 3 in that the warp density of the greige blend fabric is 700 threads/10 cm; the weft density was 600 pieces/10 cm.
Example 18
Example 18 differs from example 3 in that the concentration of the protease impregnation solution was 0.01 wt%.
Example 19
Example 19 differs from example 3 in that the concentration of the protease impregnation solution was 0.5 wt%.
Example 20
Example 20 differs from example 3 in that the nanoparticle impregnating solution has a concentration of 0.01 g/mL.
Example 21
Example 21 differs from example 3 in that the nanoparticle impregnating solution has a concentration of 0.5 g/mL; the nano particles are silica particles with the particle size of 20 nm.
Example 22
Example 22 differs from example 3 in that the nanoparticles are unmodified.
Example 23
Example 23 differs from example 3 in that the nanoparticles are octadecylamine modified nanoparticles.
Example 24
Example 24 differs from example 3 in that the nanoparticles are silica particles having a particle size of 100 nm.
Example 25
Example 25 differs from example 3 in that the mass concentration of the flame retardant in the finishing liquor was 10 g/L.
Example 26
Example 26 differs from example 3 in that the mass concentration of the flame retardant in the finishing liquor was 400 g/L.
Evaluation of Performance test
1. Softness test
The soft antistatic textile fabrics prepared in the examples 1-13 and 18-19 are cut into rectangular blocks of 6cm multiplied by 10cm, 6 samples are prepared and tested in each group of examples, wherein the long sides of 3 samples are parallel to the longitudinal direction of the fabric, the long sides of 3 samples are parallel to the transverse direction of the fabric, the samples are subjected to humidity conditioning for 24 hours under standard atmospheric conditions before testing, and no flaw is generated on the samples. The bending stiffness of the test piece was measured by using an electronic stiffness meter model LLY-01 manufactured by electronics instruments, Inc. of Laizhou. The test result is the sum of the mean value of the longitudinal test values and the mean value of the transverse test values. The test results are shown in table 1.
Table 1 softness test results of textile fabrics
Examples Flexural rigidity (mN)
Example 1 428
Example 2 371
Example 3 362
Example 4 497
Example 5 486
Example 6 489
Example 7 475
Example 8 431
Example 9 376
Example 10 453
Example 11 371
Example 12 449
Example 13 364
Example 18 441
Example 19 364
2. Antistatic test
The test method is carried out according to the charge surface density method in GB/T12703-1991, textile static test method. The fabric charge was measured using an LFY-403A roller friction machine in combination with an LFY-403 fabric triboelectric charge tester (Faraday cage method), both of which were purchased from Shandong institute of textile science.
The cloth samples prepared in examples 1 to 11 were prepared according to the corresponding standards, with a size of 20cm x 20cm, and the samples were thrown into a friction drum, the instrument was started and run for 15min and stopped, the samples were taken out immediately (within 1 s) and placed into a faraday cage for charge measurement, and the readings on the charge measuring device were read and recorded. The antistatic properties were measured by the amount of charge obtained.
Calculating the formula: σ ═ CV/A, where σ is the charge areal density (μ C/m)2) C is total capacitance (F) of Faraday system, V is voltage reading value (V), A is test area (m) of sample2). The test results are shown in table 2.
Table 2 textile fabric charge areal density test results
Figure BDA0002179988000000231
3. Air permeability test
Reference is made to the test standard GB/T5453-1997 determination of the air permeability of textile fabrics. The test results are shown in table 3.
TABLE 3 test results of textile fabric air permeability
Figure BDA0002179988000000232
Figure BDA0002179988000000241
4. Oil repellency test
Tested according to GB/T19977-. The water washing method comprises the following steps: the washing procedure 4N is carried out according to GB/T8629-2017, and the drying procedure is A suspension drying. The test results are shown in table 4.
Table 4 textile fabric oil repellency test results
Examples Initial After washing for 10 times After washing for 40 times
Example 1 6 5 3
Example 2 6 6 4
Example 3 6 6 5
Example 20 5 4 3
Example 21 6 6 5
Example 22 5 4 2
Example 23 5 4 1
Example 24 5 4 2
5. Flame retardancy test
And measuring the afterflame time and the smoldering time by adopting an LFY-601 vertical method flame retardant property tester according to GB/T5455-2014' determination of the damage length, the smoldering time and the afterflame time of the textile in the vertical direction of the combustion property. The cloth sample was 89mm by 300 mm. The test results are shown in table 5.
TABLE 5 flame retardancy test results for textile fabrics
Figure BDA0002179988000000242
Figure BDA0002179988000000251
As can be seen from tables 1-5, the antistatic, flame-retardant and oil-proof washing cotton-hemp blended fabric prepared by the invention not only has soft hand feeling, but also has the performances of static resistance, oil repellency, flame retardance, air permeability and the like, is a cotton-hemp blended fabric integrating multiple functions, and is widely applied to the fields of clothing and home textiles.

Claims (7)

1. The preparation method of the antistatic flame-retardant oil-proof washing cotton-hemp blended fabric is characterized by at least comprising the following steps:
(1) preparing a primary blended fabric: the blended fabric is prepared from fibrilia, cotton fiber and protein fiber by slivering, spinning and weaving;
the protein fiber is modified porous graphene oxide modified protein fiber; the modified porous graphene oxide is porous graphene oxide modified by aminosiloxane derivatives;
(2) dipping protease dipping solution: paving the primary blended fabric, slowly adding a protease impregnation liquid, heating to 25-50 ℃, standing and soaking for 10-20min, taking out, repeatedly washing with clear water, placing in a 70-90 ℃ water tank for soaking for 0.2-1h, taking out, and drying at 60-100 ℃ for 2-5h to obtain a first impregnated fabric; the mass concentration of the protease impregnation liquid is 0.1-0.3 wt%;
(3) dipping nano particle dipping solution: adding the first impregnated fabric into the nanoparticle impregnation liquid, heating to 50-70 ℃, standing and soaking for 10-20min, taking out, repeatedly washing with clear water, placing in a 70-90 ℃ water tank, soaking for 10-45min, taking out, and drying at 60-100 ℃ for 2-5h to obtain a second impregnated fabric;
the nanoparticle impregnating solution comprises nanoparticles and inorganic base; the nano particles are modified nano particles of aminosiloxane derivatives; the aminosilicone derivative at least contains 2 ether bonds;
(4) and (3) treating the flame-retardant finishing liquid: according to the bath ratio of 1: (20-40) weighing the flame-retardant finishing liquid, immersing the second dipped fabric into a container containing the finishing liquid, treating for 20-40min at 60-90 ℃, then carrying out two-dipping and two-rolling to keep the rolling residue rate at 90% -100%, taking out, and drying for 5-10h at 80-120 ℃ to obtain the flame-retardant finishing liquid.
2. The method according to claim 1, wherein the weight ratio of the cotton fiber, the hemp fiber and the protein fiber is 1: (0.5-1): (0.1-0.5).
3. The method as claimed in claim 1, wherein the warp density of the primary blended fabric is 450-600 pieces/10 cm; the weft density is 400-500 pieces/10 cm.
4. The preparation method according to claim 1, wherein the nanoparticles are selected from one or more of nano-silica, nano-titanium dioxide, nano-zinc oxide, nano-alumina and mica powder.
5. The method of claim 4, wherein the nanoparticles have a particle size of 10 to 50 nm.
6. An antistatic flame-retardant oil-resistant washing cotton-linen blended fabric prepared by the preparation method according to any one of claims 1 to 5.
7. The application of the antistatic flame-retardant oil-proof washing cotton-linen blended fabric as claimed in claim 6, which is characterized by being applied to the fields of clothing and home textiles.
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