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CN114801375A - Insect-proof heat-insulation fabric and preparation method thereof - Google Patents

Insect-proof heat-insulation fabric and preparation method thereof Download PDF

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Publication number
CN114801375A
CN114801375A CN202210555524.1A CN202210555524A CN114801375A CN 114801375 A CN114801375 A CN 114801375A CN 202210555524 A CN202210555524 A CN 202210555524A CN 114801375 A CN114801375 A CN 114801375A
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China
Prior art keywords
fabric
base layer
mass
insect
stirring
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Chinese (zh)
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盛建浩
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Individual
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Individual
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Priority to CN202210555524.1A priority Critical patent/CN114801375A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/026—Knitted fabric
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/08—Impregnating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • 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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
    • 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
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
    • 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 Table; 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
    • D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts 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
    • 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
    • D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
    • 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
    • D06M17/00—Producing multi-layer textile fabrics
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02—Synthetic macromolecular fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02—Synthetic macromolecular fibres
    • B32B2262/0253—Polyolefin fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/304—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/71—Resistive to light or to UV
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/764—Insect repellent
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/22—Polymers or copolymers of halogenated mono-olefins
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • 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

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses an insect-proof heat-insulating fabric and a preparation method thereof, and relates to the technical field of textiles. The insect-proof heat-insulation fabric comprises a fabric base layer and a heat-insulation layer from bottom to top; firstly, blending and spinning o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane and 3-hydroxy anthranilic acid dichloroacetamide to form silica aerogel and benzotriazole, and preparing a thermal insulation layer after weaving; then blending and spinning the polytetrafluoroethylene prepolymer and 3-hydroxy-5-amino propenyl butenone, and preparing a fabric base layer after weaving; then sequentially layering a fabric base layer and a heat insulation layer from bottom to top, and performing steam rolling treatment by using phosphorus pentasulfide to form phosphate and thiobenzamide compounds to prepare the insect-proof heat insulation fabric; the insect-proof heat-insulating fabric prepared by the invention has good heat preservation, ultraviolet resistance, flame retardance and insect resistance.

Description

Insect-proof heat-insulation fabric and preparation method thereof
Technical Field
The invention relates to the technical field of textiles, in particular to an insect-proof heat-insulating fabric and a preparation method thereof.
Background
In the daily fire fighting process, the most contact of fire fighters is the work of fire extinguishing in a fire scene, and the fabric of the protective clothing needs to be flame-retardant and fireproof and also has a certain thermal insulation and protection function. In all the developed flame-retardant materials at present, the fabric used as the firefighter uniform is woven by high-temperature-resistant organic fibers, or the fabric is subjected to flame retardant treatment by using a flame retardant to obtain the flame-retardant functional fabric. The fabrics prepared by these two methods have only some flame retardancy, but are not heat insulating.
In addition, in areas such as Hainan, Yunnan, Guangxi, Guizhou and the like which are remote in China, mosquitoes, midges, gnats and fleas have more blood sucking insects, the density of the insects around the human body can reach hundreds of insects per cubic meter of space, and the blood sucking insects not only disturb the human body through stings, but also can transmit a plurality of diseases such as plague, dengue fever, malaria and the like. Firefighters often encounter these blood-sucking insects when serving people (e.g., eliminating wildlife and eliminating potential safety hazards), which requires that the fabric of the protective clothing has good insect-proof properties. Therefore, the fabric has the flame retardance, the heat insulation performance and the insect prevention performance, which is a great problem to be solved urgently in the current textile field.
The invention focuses on the problem, and solves the problem by preparing the insect-proof heat-insulating fabric.
Disclosure of Invention
The invention aims to provide an insect-proof heat-insulating fabric and a preparation method thereof, and aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the insect-proof heat-insulating fabric comprises a fabric base layer and a heat-insulating layer from top to bottom, wherein the fabric base layer and the heat-insulating layer are layered from top to bottom, and phosphorus pentasulfide is used for steam rolling treatment to prepare the insect-proof heat-insulating fabric;
further, the heat insulation layer is obtained by blending, spinning and weaving o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane and 3-hydroxy anthranilic acid dichloroacetamide;
furthermore, the fabric base layer is obtained by blending, spinning and weaving polytetrafluoroethylene and 3-hydroxy-5-amino propenyl benzyl ketone.
Further, the preparation method of the insect-proof heat-insulating fabric comprises the following preparation steps:
(1) putting the fabric base layer fiber master batch into a 327-329 ℃ spinning box, spinning by using a screw extruder under the condition of a spinning speed of 800-1000 m/min, and carrying out side-blowing cooling solidification for 25-35 min under the conditions of 10-14 ℃, humidity of 60-80% and wind speed of 0.9-1.3 m/s to prepare the fabric base layer fiber; co-twisting and tatting fabric base layer fibers to obtain 100-140 g/m 2 The fabric base layer of (1);
(2) at the temperature of 24-26 ℃, mixing o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane, 3-hydroxy anthranilic acid dichloroacetamide and ethanol according to the mass ratio of 1: 0.8: 3-1: 1.2: 5, mixing, stirring at 900-1100 r/min for 20-30 min, then dripping ethanol water solution with the mass fraction of 3-5% and 0.6-0.8 time of the mass of the o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane at 60-80 drops/min, continuously stirring for 2-4 h at 60-80 ℃, under the protection of argon gas at 0-5 ℃, 60 to 80 drops/min of sodium dodecyl benzene sulfonate with the mass of 0.003 to 0.007 time of that of the o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane is dripped, stirring for 15-25 min at 1000-1200 r/min, dropwise adding 18-22% by mass of sodium hydroxide solution at 60-80 drops/min to adjust the pH value to 7-9, continuously stirring for 1-3 h, adding aluminum trichloride which is 0.01-0.03 time of the mass of o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane, and continuously stirring for 6-8 h to obtain the heat insulation material.A layer fiber masterbatch; putting the fabric base layer fiber master batch into a spinning box at the temperature of 180-190 ℃, spinning by using a screw extruder under the condition of the spinning speed of 800-1000 m/min, and carrying out side-blowing cooling solidification for 25-35 min under the conditions of 0-4 ℃, humidity of 20-40% and wind speed of 0.9-1.3 m/s to prepare a thermal insulation layer fiber; co-twisting and tatting the fibers of the heat insulation layer to obtain 100-140 g/m 2 The heat insulating layer of (2);
(3) under the conditions of room temperature and argon protection, paving a material base layer and a heat insulation layer from bottom to top in sequence, dipping the material base layer and the heat insulation layer in an acetic acid solution of ammonium acetate with the mass fraction of 10-20% and the mass fraction of 1-2 times of that of the fabric base layer, treating the material base layer and the heat insulation layer under the microwave conditions of 2400-2500 MHz and 700-900W for 10-20 min, then dripping an ethanol solution of sodium ethoxide with the mass fraction of 1-3% and the mass fraction of 3-5 times of that of the fabric base layer at 40-60 drops/min, continuing the microwave treatment for 8-18 min, adding tribromooxyphosphorus oxide with the mass fraction of 0.7-0.9 time of the fabric base layer, continuing the microwave treatment for 18-28 min, adding potassium persulfate with the mass fraction of 1-2 times of the fabric base layer at 60-70 ℃, continuing the microwave treatment for 5-10 min, then dripping a 20% sodium hydroxide solution at 40-60 drops/min to adjust the pH to 7-9, continuing the microwave treatment for 1-3 min, then dripping thionyl chloride with the mass fraction of 1-1.4 times of the fabric base layer at 40-60 drops/min, continuing the microwave treatment for 30-50 min, then adding nano titanium dioxide which is 0.06-0.08 times of the mass of the base layer of the fabric, continuing the microwave treatment for 8-18 min, then immersing into a phosphorus pentasulfide solution which is 5-10 times of the mass of the base layer of the fabric, continuing the microwave treatment for 50-70 min, and performing microwave treatment for 2-4 m 3 Introducing 100-120 ℃ steam for 5-7 min/min, rolling for 1-3 times at 188-190 ℃ and 8-10 MPa at 220-240 m/min, and preparing to obtain 210-290 g/m 2 The insect-proof heat-insulating fabric.
Further, the preparation method of the fabric base layer fiber master batch in the step (1) comprises the following steps: under the conditions of 60-80 ℃ and 2-4 MPa, polytetrafluoroethylene and 3-hydroxy-5-amino propenyl butenone are mixed according to the mass ratio of 1: 0.3-1: 0.5 mixing, stirring for 30-50 min at 500-700 r/min, then dripping dibenzoyl peroxide with the mass of 0.1-0.3 time that of polytetrafluoroethylene at 40-60 drops/min, stirring for 2-4 h at 900-1100 r/min, cooling to room temperature at 3-5 ℃/min, filtering, washing for 2-4 times with absolute ethyl alcohol and deionized water respectively, and drying for 2-3 h at 30-50 ℃ to prepare the fabric base layer fiber master batch.
Further, the preparation method of the 3-hydroxy-5-amino propenyl butenone comprises the following steps: under the conditions of room temperature and argon protection, mixing 2-chloropropylamine and o-hydroxy crotone according to a mass ratio of 1: 1.2-1: 1.4, stirring for 10-20 min at 500-700 r/min, then adding aluminum trichloride accounting for 0.01-0.03 time of the mass of 2-chloropropene amine, cooling to 1-5 ℃ at 3-5 ℃/min, and continuously stirring for 6-8 h to prepare the 3-hydroxy-5-amino propenyl benzyl ketone.
Furthermore, the molecular weight of the polytetrafluoroethylene is 1600-2000.
Further, the preparation method of the o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane in the step (2) is as follows: at the temperature of 60-80 ℃, mixing tris (hydroxyethoxy) chlorosilane and maleic acid according to the mass ratio of 1: 1.3-1: 1.7, stirring for 10-20 min at 500-700 r/min, then dripping concentrated sulfuric acid with the mass fraction of 98% and the mass fraction of 0.03-0.04 times of that of the tris (hydroxyethoxy) chlorosilane into the solution at 40-60 drops/min, and stirring for 2-4 h at 1200-1300 r/min to prepare the tris (maleic diethoxy) chlorosiloxane; under the conditions of room temperature and argon protection, mixing tris (maleic acid diethyl ester) chlorosiloxane and o-nitrophenylhydrazine according to a mass ratio of 1: 0.4-1: 0.6, stirring for 10-20 min at 500-700 r/min, then adding aluminum trichloride with the mass of 0.01-0.03 time of that of the tri (diethyl maleate) chlorosiloxane, cooling to 1-5 ℃ at 3-5 ℃/min, and continuously stirring for 6-8 h to prepare the o-nitrophenyl hydrazino tri (diethyl maleate) siloxane.
Further, the preparation method of the 3-hydroxy anthranilic acid dichloroacetamide in the step (2) is as follows: under the conditions of room temperature and argon protection, 3-hydroxy anthranilic acid and dichloroacetamide are mixed according to the mass ratio of 1: 0.6-1: 0.8, stirring for 20-30 min at 500-700 r/min, then adding nano titanium dioxide with the mass of 0.06-0.08 times of that of 3-hydroxy anthranilic acid, heating to 80-100 ℃ at 9-10 ℃/min, and continuously stirring for 2-4 h to prepare the 3-hydroxy anthranilic acid dichloroacetamide.
Further, the preparation method of the phosphorus pentasulfide solution in the step (3) is as follows: under the conditions of room temperature and argon protection, phosphorus pentasulfide, sodium carbonate and ethyl acetate are mixed according to the mass ratio of 1: 0.3: 10-1: 0.5: 12, stirring for 1-3 h at 500-700 r/min to prepare the phosphorus pentasulfide solution.
Compared with the prior art, the invention has the following beneficial effects:
the insect-proof heat-insulation fabric comprises a fabric base layer and a heat-insulation layer from bottom to top; firstly, blending and spinning o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane and 3-hydroxy anthranilic acid dichloroacetamide, and preparing a heat insulation layer after weaving; laying the fabric base layer and the thermal insulation layer from the lower part and the upper part, and performing steam rolling treatment by using phosphorus pentasulfide to prepare the insect-proof thermal insulation fabric; the fabric base layer is prepared from a polytetrafluoroethylene prepolymer and 3-hydroxy-5-amino propenyl benzyl ketone.
Firstly, 3-hydroxy anthranilic acid dichloroacetamide and 3-hydroxy anthranilic acid are formed by hydrolysis of dichloroacetamide and dichloroanthranilic acid, and o-nitrophenylhydrazino tri (maleic acid diethoxy) siloxane is formed by hydrolysis and condensation of silicon dioxide aerogel, so that the heat insulation performance of the heat insulation layer is enhanced; the method comprises the following steps of coupling and reducing o-nitrophenylhydrazine on o-nitrophenylhydrazino tri (diethyl maleate) siloxane and phenol of 3-hydroxy anthranilic acid to form benzotriazole, reacting and crosslinking with dichloroacetamide to form (N-benzotriazole) ketone, wherein during illumination, the benzotriazole forms unstable phenol-quinoid tautomer, converts redundant energy into heat energy, and releases or consumes the heat energy in a non-radiation manner to form a stable ground state, so that the ultraviolet resistance of a heat insulation layer is enhanced.
Secondly, part of phosphorus pentasulfide is hydrolyzed to form phosphoric acid, and the phosphoric acid reacts with hydroxyl on the fabric base layer and the heat insulation layer to form phosphate ester, so that the flame retardant property of the insect-proof heat insulation fabric is enhanced; the (N-benzotriazole) ketone on the heat-insulating layer and the butenone on the fabric base layer are subjected to ring closure and diazotization to form 2-hydrazino-3-chloropyridine, the obtained product is subjected to cyclization with diethyl maleate on the heat-resistant layer, bromination, pyrazole epoxidation and saponification to form 3-bromo-1- (3-chloropyridine-2-yl) -1H-pyrazole-5-formic acid, the amino propylene on the fabric on the base layer and the anthranilic acid on the heat-insulating layer are subjected to reaction and crosslinking to form anthranilamide, the anthranilamide reacts with part of phosphorus pentasulfide to form 2-amino-3-methyl-5-halogeno-thiobenzamide, and the 2-amino-3-methyl-5-halogeno-thiobenzamide reacts with the 3-bromo-1- (3-chloropyridine-2-yl) -1H-pyrazole-5-formic acid Carboxyl reaction to form thiobenzamide compound, which can activate ryanodine receptor in mosquito body, make calcium ion release out of control and loss, finally exhaust calcium in calcium reservoir in cell, make contraction function of muscle cell paralyze, thus achieve the effect of preventing insect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for detailed description, and the index test methods of the insect-proof heat-insulating fabric prepared in the following examples are as follows:
thermal insulation performance: the heat preservation performance of the insect-proof heat-insulation fabric prepared by the same mass of the embodiment and the comparative example is measured according to the GB/T11048 standard method.
Ultraviolet resistance: the insect-proof heat-insulating fabric prepared by the same mass of the examples and the comparative examples is tested for the UPF value according to the GB/T18330 standard method to determine the ultraviolet resistance.
Flame retardant property: and measuring the extreme oxygen index of the insect-proof heat-insulating fabric prepared by the same mass example and the comparative example according to a GB/T17591 standard method to measure the flame retardant property.
Mosquito-proof performance: the insect-preventing and heat-insulating fabric prepared by the same mass of the embodiment and the comparative example is fed with sugar water after the mosquitoes contact the fabric according to WHO/CDS/WHOPES/GCDPP, and the mosquito-preventing performance is tested by testing the mosquito knockdown rate for 3 hours and the mosquito mortality rate for 24 hours.
Example 1
The preparation method of the insect-proof heat-insulating fabric comprises the following preparation steps:
(1) under the conditions of room temperature and argon protection, mixing 2-chloropropylamine and o-hydroxy crotone according to a mass ratio of 1: 1.2, stirring for 10min at 500r/min, then adding aluminum trichloride of which the mass is 0.01 time of that of 2-chloropropylamine, cooling to 1 ℃ at 3 ℃/min, and continuously stirring for 6h to prepare 3-hydroxy-5-amino propenyl benzyl ketone; at the temperature of 60 ℃ and under the pressure of 2MPa, polytetrafluoroethylene with the molecular weight of 1600 and 3-hydroxy-5-amino propenyl benzyl ketone are mixed according to the mass ratio of 1: 0.3, stirring for 30min at 500r/min, then dripping dibenzoyl peroxide with the mass of 0.1 time of that of polytetrafluoroethylene at 40 drops/min, stirring for 2h at 900r/min, cooling to room temperature at 3 ℃/min, filtering, washing for 2 times by using absolute ethyl alcohol and deionized water respectively, and drying for 2h at 30 ℃ to prepare the fabric base layer fiber master batch;
(2) putting the fabric base layer fiber master batch into a 327 ℃ spinning box, spinning by using a screw extruder under the condition of a spinning speed of 800m/min, and carrying out side-blowing cooling and curing for 25min under the conditions of 10 ℃, humidity of 60% and wind speed of 0.9m/s to prepare fabric base layer fibers; the fabric base layer fiber is co-twisted and woven to prepare 100g/m 2 The fabric base layer of (1);
(3) under the conditions of room temperature and argon protection, 3-hydroxy anthranilic acid and dichloroacetamide are mixed according to the mass ratio of 1: 0.6, stirring for 20min at 500r/min, then adding nano titanium dioxide with the mass of 0.06 time of that of the 3-hydroxy anthranilic acid, heating to 80 ℃ at the speed of 9 ℃/min, and continuously stirring for 2h to prepare 3-hydroxy anthranilic acid dichloroacetamide; at 60 ℃, mixing tris (hydroxyethoxy) chlorosilane and maleic acid according to a mass ratio of 1: 1.3, stirring for 10min at 500r/min, then dripping concentrated sulfuric acid with the mass fraction of 98 percent, which is 0.03 time of the mass of the tris (hydroxyethoxy) chlorosilane, at 40 drops/min, and stirring for 2h at 1200r/min to prepare the tris (maleic acid diethyl ester) chlorosiloxane; under the conditions of room temperature and argon protection, mixing tris (maleic acid diethyl ester) chlorosiloxane and o-nitrophenylhydrazine according to a mass ratio of 1: 0.4, stirring for 10min at 500r/min, then adding aluminum trichloride of which the mass is 0.01 time of that of the tri (maleic acid diethyl ester) chlorosiloxane, cooling to 1 ℃ at 3 ℃/min, and continuously stirring for 6h to prepare the o-nitrophenylhydrazine tri (maleic acid diethyl ester) siloxane; at 24 ℃, mixing o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane, 3-hydroxy anthranilic acid dichloroacetamide and ethanol according to a mass ratio of 1: 0.8: 3, mixing, stirring for 20min at 900r/min, then dropwise adding an ethanol aqueous solution with the mass fraction of 3% and the mass fraction of 0.6 time of that of o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane at 60 drops/min, continuously stirring for 2h at 60 ℃, dropwise adding sodium dodecyl benzene sulfonate with the mass fraction of 0.003 time of that of o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane at 60 drops/min under the conditions of 0 ℃ and argon protection, stirring for 15min at 1000r/min, dropwise adding a sodium hydroxide solution with the mass fraction of 18% at 60 drops/min to adjust the pH to 7, continuously stirring for 1h, adding aluminum trichloride with the mass fraction of 0.01 time of that of the o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane, and continuously stirring for 6h to prepare a thermal insulation layer fiber master batch;
(4) putting the fabric base layer fiber master batch into a spinning box at 180 ℃, spinning by using a screw extruder under the condition of a spinning speed of 800m/min, and carrying out side-blowing cooling and curing for 25min under the conditions of 0 ℃, 20% of humidity and 0.9m/s of wind speed to prepare a heat-insulating layer fiber; the heat insulation layer fiber is co-twisted and woven to prepare 100g/m 2 The heat insulating layer of (2);
(5) under the conditions of room temperature and argon protection, phosphorus pentasulfide, sodium carbonate and ethyl acetate are mixed according to the mass ratio of 1: 0.3: 10, mixing, and stirring for 1h at 500r/min to prepare a phosphorus pentasulfide solution; paving a material base layer and a heat insulation layer sequentially from bottom to top under the conditions of room temperature and argon protection, dripping acetic acid solution of ammonium acetate with the mass fraction of 10% and the mass fraction of 1 time of the mass of the fabric base layer, processing for 10min under the microwave conditions of 2400MHz and 700W, dripping ethanol solution of sodium ethoxide with the mass fraction of 1% and the mass fraction of 3 times of the mass of the fabric base layer at 40 drops/min, continuing microwave processing for 8min, adding tribromooxyphosphorus with the mass fraction of 0.7 time of the mass of the fabric base layer, continuing microwave processing for 18min, adding potassium persulfate with the mass fraction of 1 time of the mass of the fabric base layer at 60 ℃, continuing microwave processing for 5min, then dripping 20% of hydroxide at 40 drops/minAdjusting the pH value of the sodium water solution to 7, continuing microwave treatment for 1min, dripping 1 time of thionyl chloride of the fabric base layer at a rate of 40 drops/min, continuing microwave treatment for 30min, then adding nano titanium dioxide of which the mass is 0.06 time of that of the fabric base layer, continuing microwave treatment for 8min, then immersing 5 times of phosphorus pentasulfide solution of which the mass is 5 times of that of the fabric base layer, continuing microwave treatment for 50min, and continuing microwave treatment for 2m 3 Introducing 100 deg.C steam for 5min, rolling at 188 deg.C and 8MPa for 1 time at 220m/min to obtain 210g/m 2 The insect-proof heat-insulating fabric.
Example 2
The preparation method of the insect-proof heat-insulating fabric comprises the following preparation steps:
(1) under the conditions of room temperature and argon protection, mixing 2-chloropropylamine and o-hydroxy crotone according to a mass ratio of 1: 1.3, stirring for 15min at the speed of 600r/min, then adding aluminum trichloride of which the mass is 0.02 time of that of 2-chloropropylamine, cooling to 3 ℃ at the speed of 4 ℃/min, and continuously stirring for 7h to prepare 3-hydroxy-5-amino propenyl benzyl ketone; under the conditions of 70 ℃ and 3MPa, polytetrafluoroethylene with the molecular weight of 1800 and 3-hydroxy-5-amino propenyl benzyl ketone are mixed according to the mass ratio of 1: 0.4, stirring for 40min at 600r/min, then dripping 50 drops/min of dibenzoyl peroxide with the mass of 0.2 time that of polytetrafluoroethylene, stirring for 3h at 1000r/min, cooling to room temperature at 4 ℃/min, filtering, washing for 3 times by using absolute ethyl alcohol and deionized water respectively, and drying for 2.5h at 40 ℃ to prepare the fabric base layer fiber master batch;
(2) putting the fabric base layer fiber master batch into a spinning box at 328 ℃, spinning by using a screw extruder under the condition of a spinning speed of 900m/min, and carrying out side-blowing cooling and curing for 30min under the conditions of 12 ℃, 70% of humidity and 1.1m/s of wind speed to prepare fabric base layer fibers; the fabric base layer fiber is co-twisted and woven to prepare 120g/m 2 The fabric base layer of (1);
(3) under the conditions of room temperature and argon protection, 3-hydroxy anthranilic acid and dichloroacetamide are mixed according to the mass ratio of 1: 0.7, stirring at 600r/min for 25min, then adding nano titanium dioxide with the mass of 0.07 time of that of the 3-hydroxy anthranilic acid, heating to 90 ℃ at the speed of 9.5 ℃/min, and continuously stirring for 3h to prepare 3-hydroxy anthranilic acid dichloroacetamide; at 70 ℃, mixing tris (hydroxyethoxy) chlorosilane and maleic acid according to a mass ratio of 1: 1.5, stirring for 15min at 600r/min, then dropwise adding concentrated sulfuric acid with the mass fraction of 98 percent, which is 0.035 times of the mass of the tris (hydroxyethoxy) chlorosilane, at 50 drops/min, and stirring for 3h at 1250r/min to prepare tris (maleic acid diethyl ester) chlorosiloxane; under the conditions of room temperature and argon protection, mixing tris (maleic acid diethyl ester) chlorosiloxane and o-nitrophenylhydrazine according to a mass ratio of 1: 0.5, stirring for 15min at the speed of 600r/min, then adding aluminum trichloride of which the mass is 0.02 time of that of the tri (maleic acid diethyl ester) chlorosiloxane, cooling to 3 ℃ at the speed of 4 ℃/min, and continuously stirring for 7h to prepare the o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane; at 25 ℃, mixing o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane, 3-hydroxy anthranilic acid dichloroacetamide and ethanol according to a mass ratio of 1: 1: 4, stirring for 25min at 1000r/min, then dropwise adding an ethanol aqueous solution with the mass fraction of 4% and the mass fraction of 0.7 time of that of o-nitrophenyl hydrazino tri (diacetoxy maleate) siloxane at 70 drops/min, continuously stirring for 3h at 70 ℃, dropwise adding sodium dodecyl benzene sulfonate with the mass fraction of 0.005 time of that of o-nitrophenyl hydrazino tri (diacetoxy maleate) siloxane at 70 drops/min under the conditions of 2 ℃ and argon protection, stirring for 20min at 1100r/min, dropwise adding a sodium hydroxide solution with the mass fraction of 20% at 70 drops/min to adjust the pH to 8, continuously stirring for 2h, adding aluminum trichloride with the mass fraction of 0.02 time of that of o-nitrophenyl hydrazino tri (diacetoxy maleate) siloxane, and continuously stirring for 7h to prepare a thermal insulation layer fiber master batch;
(4) putting the fabric base fiber master batch into a spinning box at 170 ℃, spinning by using a screw extruder under the condition of a spinning speed of 900m/min, and carrying out side-blowing, cooling and curing for 30min under the conditions of 2 ℃, 30% of humidity and 1.1m/s of wind speed to prepare a heat-insulating layer fiber; the heat insulation layer fiber is co-twisted and woven to prepare 120g/m 2 The heat insulating layer of (2);
(5) under the conditions of room temperature and argon protection, phosphorus pentasulfide, sodium carbonate and ethyl acetate are mixed according to the mass ratio of 1: 0.4: 11, mixing, and stirring for 2 hours at the speed of 600r/min to prepare a phosphorus pentasulfide solution; room temperature and argon protective conditionsPaving a material base layer and a heat insulation layer in sequence from bottom to top, dripping 15 mass percent of ammonium acetate acetic acid solution 1.5 times of the mass of the fabric base layer, processing for 15min under microwave conditions of 2450MHz and 800W, dripping 2 mass percent of sodium ethoxide ethanol solution 4 times of the mass of the fabric base layer by 50 drops/min, continuing to perform microwave processing for 13min, adding 0.8 mass percent of tribromooxyphosphorus of the fabric base layer, continuing to perform microwave processing for 13min, adding 1.5 mass percent of potassium persulfate 1.5 times of the mass of the fabric base layer at 65 ℃, continuing to perform microwave processing for 7.5min, dripping 20 mass percent of sodium hydroxide aqueous solution by 50 drops/min to adjust the pH value to 8, continuing to perform microwave processing for 2min, dripping 1.2 mass percent of thionyl chloride of the fabric base layer by 50 drops/min, continuing to perform microwave processing for 40min, then adding 0.07 mass percent of nano titanium dioxide of the fabric base layer, continuing to perform microwave processing for 13min, then immerging into phosphorus pentasulfide solution 7.5 times of the base layer of the fabric, continuing microwave treatment for 60min at 3m 3 Introducing 110 deg.C steam for 6min, rolling at 189 deg.C and 9MPa for 2 times at 230m/min to obtain 250g/m 2 The insect-proof heat-insulating fabric.
Example 3
The preparation method of the insect-proof heat-insulating fabric comprises the following preparation steps:
(1) under the conditions of room temperature and argon protection, mixing 2-chloropropylamine and o-hydroxy crotone according to a mass ratio of 1: 1.4, stirring for 20min at 700r/min, then adding aluminum trichloride of which the mass is 0.03 time that of 2-chloropropylamine, cooling to 5 ℃ at the speed of 5 ℃/min, and continuously stirring for 8h to prepare 3-hydroxy-5-amino propenyl benzyl ketone; at the temperature of 80 ℃ and under the condition of 4MPa, polytetrafluoroethylene with the molecular weight of 2000 and 3-hydroxy-5-amino propenyl benzyl ketone are mixed according to the mass ratio of 1: 0.5, stirring for 50min at 700r/min, then dripping 60 drops/min of dibenzoyl peroxide with the mass of 0.3 time that of polytetrafluoroethylene, stirring for 4h at 1100r/min, cooling to room temperature at 5 ℃/min, filtering, washing for 4 times by using absolute ethyl alcohol and deionized water respectively, and drying for 3h at 50 ℃ to prepare the fabric base layer fiber master batch;
(2) the master batch of the fabric base layer fiber is put into a 329 ℃ spinning box, and is spun by a screw extruder under the condition of the spinning speed of 1000m/minUnder the conditions of 14 ℃, humidity of 80 percent and wind speed of 1.3m/s, carrying out side-blowing cooling and curing for 35min to prepare fabric base layer fibers; the fabric base layer fiber is co-twisted and woven to prepare 140g/m 2 The fabric base layer of (1);
(3) under the conditions of room temperature and argon protection, 3-hydroxy anthranilic acid and dichloroacetamide are mixed according to the mass ratio of 1: 0.8, stirring for 30min at 700r/min, then adding nano titanium dioxide with the mass of 0.08 times of that of 3-hydroxy anthranilic acid, heating to 100 ℃ at the speed of 10 ℃/min, and continuously stirring for 4h to prepare 3-hydroxy anthranilic acid dichloroacetamide; at 80 ℃, mixing tris (hydroxyethoxy) chlorosilane and maleic acid according to a mass ratio of 1: 1.7, stirring for 20min at 700r/min, then dropwise adding concentrated sulfuric acid with the mass fraction of 98 percent, which is 0.04 time of the mass of the tris (hydroxyethoxy) chlorosilane, at 60 drops/min, and stirring for 4h at 1300r/min to prepare the tris (maleic acid diethyl ester) chlorosiloxane; under the conditions of room temperature and argon protection, mixing tris (maleic acid diethyl ester) chlorosiloxane and o-nitrophenylhydrazine according to a mass ratio of 1: 0.6, stirring for 20min at 700r/min, then adding aluminum trichloride of which the mass is 0.03 time that of the tri (maleic acid diethyl ester) chlorosiloxane, cooling to 5 ℃ at the speed of 5 ℃/min, and continuously stirring for 8h to prepare the o-nitrophenylhydrazine tri (maleic acid diethyl ester) siloxane; at 26 ℃, mixing o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane, 3-hydroxy anthranilic acid dichloroacetamide and ethanol according to a mass ratio of 1: 1.2: 5, mixing, stirring for 30min at 1100r/min, then dropwise adding an ethanol aqueous solution with the mass fraction of 5% and the mass fraction of 0.8 time of that of o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane at 80 drops/min, continuously stirring for 4h at 80 ℃, dropwise adding sodium dodecyl benzene sulfonate with the mass fraction of 0.007 time of that of o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane at 80 drops/min under the conditions of 5 ℃ and argon protection, stirring for 25min at 1200r/min, dropwise adding a sodium hydroxide solution with the mass fraction of 22% at 80 drops/min to adjust the pH to 9, continuously stirring for 3h, adding aluminum trichloride with the mass fraction of 0.03 time of that of o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane, and continuously stirring for 8h to prepare a thermal insulation layer fiber master batch;
(4) putting the fabric basic layer fiber master batch into a spinning box at 190 DEG CSpinning by using a screw extruder under the condition of a spinning speed of 1000m/min, and carrying out side-blowing cooling and curing for 35min under the conditions of 4 ℃, 40% of humidity and 1.3m/s of wind speed to prepare a thermal insulation layer fiber; the thermal insulation layer fiber is co-twisted and woven to prepare 140g/m 2 The heat insulating layer of (2);
(5) under the conditions of room temperature and argon protection, phosphorus pentasulfide, sodium carbonate and ethyl acetate are mixed according to the mass ratio of 1: 0.5: 12, mixing, and stirring for 3 hours at 700r/min to prepare a phosphorus pentasulfide solution; paving a material base layer and a heat insulation layer in sequence from bottom to top under the conditions of room temperature and argon protection, dripping an acetic acid solution of ammonium acetate with the mass fraction of 20 percent, which is 2 times of the mass of the fabric base layer, into the material base layer, treating the material base layer for 20min under the microwave conditions of 2500MHz and 900W, dripping an ethanol solution of sodium ethoxide with the mass fraction of 3 percent, which is 5 times of the mass of the fabric base layer, into the fabric base layer for 60 drops/min, continuing to perform microwave treatment for 18min, adding tribromooxyphosphorus oxide with the mass fraction of 0.9 time of the mass of the fabric base layer, continuing to perform microwave treatment for 28min, adding potassium persulfate with the mass fraction of 2 times of the mass of the fabric base layer at the temperature of 70 ℃, continuing to perform microwave treatment for 10min, dripping a 20 percent sodium hydroxide aqueous solution with the mass fraction of 60 drops/min to adjust the pH value to 9, continuing to perform microwave treatment for 3min, dripping thionyl chloride with the mass fraction of 1.4 times of the fabric base layer with the mass of 60 drops/min, continuing to perform microwave treatment for 50min, and then adding nano titanium dioxide with the mass fraction of the fabric base layer, 0.08 times, continuing microwave treatment for 18min, soaking in phosphorus pentasulfide solution 10 times of the base layer of the fabric, continuing microwave treatment for 70min at a speed of 4m 3 Introducing 120 deg.C steam for 7min, rolling at 190 deg.C and 10MPa for 3 times at 240m/min to obtain 290g/m 2 The insect-proof heat-insulation fabric.
Comparative example 1
(1) Putting polytetrafluoroethylene with the molecular weight of 1800 into a spinning box at 328 ℃, spinning by using a screw extruder under the condition of the spinning speed of 900m/min, and carrying out side-blowing cooling and curing for 30min under the conditions of 12 ℃, the humidity of 70% and the wind speed of 1.1m/s to prepare the fabric base layer fiber; the fabric base layer fiber is co-twisted and woven to prepare 120g/m 2 The fabric base layer of (1);
(2) under the conditions of room temperature and argon protection, 3-hydroxy anthranilic acid and dichloroacetamide are mixed according to the mass ratio of 1: 0.7, stirring at 600r/min for 25min, then adding nano titanium dioxide with the mass of 0.07 time of that of the 3-hydroxy anthranilic acid, heating to 90 ℃ at the speed of 9.5 ℃/min, and continuously stirring for 3h to prepare 3-hydroxy anthranilic acid dichloroacetamide; at 70 ℃, mixing tris (hydroxyethoxy) chlorosilane and maleic acid according to a mass ratio of 1: 1.5, stirring for 15min at 600r/min, then dropwise adding concentrated sulfuric acid with the mass fraction of 98 percent, which is 0.035 times of the mass of the tris (hydroxyethoxy) chlorosilane, at 50 drops/min, and stirring for 3h at 1250r/min to prepare tris (maleic acid diethyl ester) chlorosiloxane; under the conditions of room temperature and argon protection, mixing tris (maleic acid diethyl ester) chlorosiloxane and o-nitrophenylhydrazine according to a mass ratio of 1: 0.5, stirring for 15min at the speed of 600r/min, then adding aluminum trichloride of which the mass is 0.02 time of that of the tri (maleic acid diethyl ester) chlorosiloxane, cooling to 3 ℃ at the speed of 4 ℃/min, and continuously stirring for 7h to prepare the o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane; at 25 ℃, mixing o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane, 3-hydroxy anthranilic acid dichloroacetamide and ethanol according to a mass ratio of 1: 1: 4, mixing, stirring for 25min at 1000r/min, then dropwise adding an ethanol aqueous solution with the mass fraction of 4% and the mass fraction of 0.7 time of that of o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane at 70 drops/min, continuously stirring for 3h at 70 ℃, dropwise adding sodium dodecyl benzene sulfonate with the mass fraction of 0.005 time of that of o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane at 70 drops/min under the conditions of 2 ℃ and argon protection, stirring for 20min at 1100r/min, dropwise adding a sodium hydroxide solution with the mass fraction of 20% at 70 drops/min to adjust the pH to 8, continuously stirring for 2h, adding aluminum trichloride with the mass fraction of 0.02 time of that of o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane, and continuously stirring for 7h to prepare a thermal insulation layer fiber master batch;
(3) putting the fabric base layer fiber master batch into a spinning box at 170 ℃, spinning by using a screw extruder under the condition of a spinning speed of 900m/min, and carrying out side-blowing cooling and curing for 30min under the conditions of 2 ℃, 30% of humidity and 1.1m/s of wind speed to prepare the thermal insulation layer fiber; the heat insulation layer fiber is co-twisted and woven to prepare 120g/m 2 The heat insulating layer of (2);
(4) at room temperature under the protection of argon gas, the mixture isPhosphorus pentasulfide, sodium carbonate and ethyl acetate in a mass ratio of 1: 0.4: 11, mixing, and stirring for 2 hours at the speed of 600r/min to prepare a phosphorus pentasulfide solution; paving a material base layer and a heat insulation layer in sequence from bottom to top under the conditions of room temperature and argon protection, dripping an acetic acid solution of ammonium acetate with the mass fraction of 15 percent, which is 1.5 times of the mass of the fabric base layer, treating for 15min under the microwave conditions of 2450MHz and 800W, dripping an ethanol solution of sodium ethoxide with the mass fraction of 2 percent, which is 4 times of the mass of the fabric base layer, continuing to perform microwave treatment for 13min, adding tribromooxyphosphorus with the mass fraction of 0.8 time of the mass of the fabric base layer, continuing to perform microwave treatment for 13min, adding potassium persulfate with the mass fraction of 1.5 times of the mass of the fabric base layer at 65 ℃, continuing to perform microwave treatment for 7.5min, dripping a 20 percent sodium hydroxide aqueous solution with the mass fraction of 50 drops/min to adjust the pH value to 8, continuing to perform microwave treatment for 2min, dripping thionyl chloride with the mass fraction of 1.2 times of the fabric base layer with the mass fraction of 50 drops/min, continuing to perform microwave treatment for 40min, and then adding nano titanium dioxide with the mass fraction of 0.07 time of the fabric base layer, continuing microwave treatment for 13min, soaking in phosphorus pentasulfide solution 7.5 times of the base layer of the fabric, and continuing microwave treatment for 60min at a speed of 3m 3 Introducing 110 deg.C steam for 6min, rolling at 189 deg.C and 9MPa for 2 times at 230m/min to obtain 250g/m 2 The insect-proof heat-insulating fabric.
Comparative example 2
Comparative example 2 differs from example 2 only in step (3), step (3) being modified: at 70 ℃, mixing tris (hydroxyethoxy) chlorosilane and maleic acid according to a mass ratio of 1: 1.5, stirring for 15min at 600r/min, then dropwise adding concentrated sulfuric acid with the mass fraction of 98 percent, which is 0.035 times of the mass of the tris (hydroxyethoxy) chlorosilane, at 50 drops/min, and stirring for 3h at 1250r/min to prepare tris (maleic acid diethyl ester) chlorosiloxane; under the conditions of room temperature and argon protection, mixing tris (maleic acid diethyl ester) chlorosiloxane and o-nitrophenylhydrazine according to a mass ratio of 1: 0.5, stirring for 15min at the speed of 600r/min, then adding aluminum trichloride of which the mass is 0.02 time of that of the tri (maleic acid diethyl ester) chlorosiloxane, cooling to 3 ℃ at the speed of 4 ℃/min, and continuously stirring for 7h to prepare the o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane; at 25 ℃, mixing o-nitrophenylhydrazino tri (maleic acid diethanoyl) siloxane and ethanol according to a mass ratio of 1: 4, stirring for 25min at 1000r/min, then dropwise adding 4% ethanol aqueous solution with the mass fraction being 0.7 time of the mass of o-nitrophenyl hydrazino tri (diacetoxy maleate) siloxane at 70 drops/min, continuously stirring for 3h at 70 ℃, dropwise adding sodium dodecyl benzene sulfonate with the mass fraction being 0.005 time of the mass of the o-nitrophenyl hydrazino tri (diacetoxy maleate) siloxane at 70 drops/min under the conditions of 2 ℃ and argon protection, stirring for 20min at 1100r/min, dropwise adding 20% sodium hydroxide solution at 70 drops/min to adjust the pH value to 8, continuously stirring for 2h, adding aluminum trichloride with the mass fraction being 0.02 time of the mass of the o-nitrophenyl hydrazino tri (diacetoxy maleate) siloxane, and continuously stirring for 7h to prepare the thermal insulation layer fiber master batch. The rest of the preparation steps are the same as example 2.
Comparative example 3
Comparative example 3 differs from example 2 only in step (3), step (3) being modified: under the conditions of room temperature and argon protection, 3-hydroxy anthranilic acid and dichloroacetamide are mixed according to the mass ratio of 1: 0.7, stirring at 600r/min for 25min, then adding nano titanium dioxide with the mass of 0.07 time of that of the 3-hydroxy anthranilic acid, heating to 90 ℃ at the speed of 9.5 ℃/min, and continuously stirring for 3h to prepare 3-hydroxy anthranilic acid dichloroacetamide; at the temperature of 25 ℃, mixing 3-hydroxy anthranilic acid dichloroacetamide and ethanol according to the mass ratio of 1: 4, stirring for 25min at 1000r/min, then dropwise adding 4% ethanol aqueous solution with the mass fraction 0.7 times that of 3-hydroxyanthranilic acid dichloroacetamide at 70 drops/min, continuously stirring for 3h at 70 ℃, dropwise adding sodium dodecyl benzene sulfonate with the mass fraction 0.005 times that of 3-hydroxyanthranilic acid dichloroacetamide at 70 drops/min under the condition of 2 ℃ and argon protection, stirring for 20min at 1100r/min, dropwise adding 20% sodium hydroxide solution at 70 drops/min to adjust the pH value to 8, continuously stirring for 2h, adding aluminum trichloride with the mass fraction 0.02 times that of 3-hydroxyanthranilic acid dichloroacetamide, and continuously stirring for 7h to prepare the heat-insulating layer fiber master batch. The rest of the preparation steps are the same as example 2.
Comparative example 4
Comparative example 4 differs from example 2 only in step (2), step (2) being modified: paving the base layer, the heat-insulating layer and the dropping surface of the material from bottom to top under the room temperature and argon protection conditions1.5 times of ammonium acetate solution with the mass fraction of 15% based on the mass of the fabric base layer, treating for 15min under the microwave conditions of 2450MHz and 800W, then dropwise adding 2% of sodium ethoxide ethanol solution with the mass fraction of 4 times of the mass of the fabric base layer at 50 drops/min, continuing to perform microwave treatment for 13min, adding 0.8 times of tribromooxyphosphorus with the mass of the fabric base layer, continuing to perform microwave treatment for 13min, adding 1.5 times of potassium persulfate with the mass of the fabric base layer at 65 ℃, continuing to perform microwave treatment for 7.5min, then dropwise adding 20% of sodium hydroxide aqueous solution at 50 drops/min to adjust the pH to 8, continuing to perform microwave treatment for 2min, then dropwise adding 1.2 times of thionyl chloride with the mass of the fabric base layer at 50 drops/min, continuing to perform microwave treatment for 40min, then adding 0.07 times of nano titanium dioxide with the mass of the fabric base layer, continuing to perform microwave treatment for 13min, then immersing in phosphorus pentasulfide solution with the mass of the fabric base layer at 7.5 times, continuing to perform microwave treatment for 60min, subsequently rolling at 189 deg.C and 9MPa for 2 times at 230m/min to obtain 250g/m 2 The insect-proof heat-insulating fabric. The rest of the preparation steps are the same as example 2.
Examples of effects
Table 1 below shows the analysis results of the heat retaining property, the ultraviolet resistance, the flame retardancy and the insect resistance of the insect-proof heat-insulating fabric prepared by the examples 1 to 3 of the present invention and the comparative examples 1 to 4.
TABLE 1
Figure BDA0003652268360000121
Figure BDA0003652268360000131
From table 1, it can be seen that the heat insulating property, the ultraviolet resistance, the flame retardancy and the insect resistance of the insect-proof heat insulating fabric prepared in examples 1, 2 and 3 are strong; the experimental data comparison of examples 1, 2 and 3 and comparative example 1 shows that the insect-proof heat-insulating fabric prepared from the fabric base layer prepared from the 3-hydroxy-5-amino propenyl crotone can form thiobenzamide compounds and phosphate ester, and the insect-proof heat-insulating fabric prepared from the insect-proof heat-insulating fabric has strong insect resistance and flame retardance; from the experimental data of examples 1, 2 and 3 and comparative example 2, it can be found that benzotriazole can be formed by preparing the thermal insulation layer by using 3-hydroxy anthranilic acid dichloroacetamide, and thiobenzamide compounds and phosphate can be formed by subsequently preparing the insect-proof thermal insulation fabric, so that the prepared insect-proof thermal insulation fabric has strong ultraviolet resistance, flame retardance and insect resistance; from the experimental data of examples 1, 2 and 3 and comparative example 3, it can be found that benzotriazole and silicon dioxide aerogel can be formed by preparing the heat-insulating layer by using o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane, and a thiobenzamide compound can be formed by subsequently preparing the insect-proof heat-insulating fabric, so that the prepared insect-proof heat-insulating fabric has high heat-insulating property and ultraviolet resistance; from experimental data of examples 1, 2 and 3 and comparative example 4, it can be found that thiobenzamide compounds and phosphate can be formed by using phosphorus pentasulfide to prepare the insect-proof heat-insulating fabric through steam rolling treatment, and the prepared insect-proof heat-insulating fabric has high flame retardance and insect resistance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (10)

1. The insect-proof heat-insulating fabric is characterized in that the insect-proof heat-insulating fabric is prepared by layering the fabric base layer and the heat-insulating layer from top to bottom and performing steam rolling treatment by using phosphorus pentasulfide.
2. The preparation method of the insect-proof heat-insulating fabric as claimed in claim 1, wherein the heat-insulating layer is obtained by blending, spinning and weaving o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane and 3-hydroxy anthranilic acid dichloroacetamide.
3. The preparation method of the insect-proof heat-insulating fabric as claimed in claim 1, wherein the fabric base layer is obtained by blending, spinning and weaving polytetrafluoroethylene and 3-hydroxy-5-amino propenyl crotonyl ketone.
4. The preparation method of the insect-proof heat-insulating fabric as claimed in claim 1, wherein the preparation method of the insect-proof heat-insulating fabric comprises the following preparation steps:
(1) putting the fabric base layer fiber master batch into a 327-329 ℃ spinning box, spinning by using a screw extruder under the condition of a spinning speed of 800-1000 m/min, and carrying out side-blowing cooling solidification for 25-35 min under the conditions of 10-14 ℃, humidity of 60-80% and wind speed of 0.9-1.3 m/s to prepare the fabric base layer fiber; co-twisting and tatting fabric base layer fibers to obtain 100-140 g/m 2 The fabric base layer of (1);
(2) at the temperature of 24-26 ℃, mixing o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane, 3-hydroxy anthranilic acid dichloroacetamide and ethanol according to the mass ratio of 1: 0.8: 3-1: 1.2: 5, mixing, stirring at 900-1100 r/min for 20-30 min, then dripping ethanol water solution with the mass fraction of 3-5% and 0.6-0.8 time of the mass of the o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane at 60-80 drops/min, continuously stirring for 2-4 h at 60-80 ℃, under the protection of argon gas at 0-5 ℃, 60 to 80 drops/min of sodium dodecyl benzene sulfonate with the mass of 0.003 to 0.007 time of that of the o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane is dripped, stirring for 15-25 min at 1000-1200 r/min, dropwise adding 18-22% by mass of sodium hydroxide solution at 60-80 drops/min to adjust the pH value to 7-9, continuously stirring for 1-3 h, adding aluminum trichloride which is 0.01-0.03 times of the mass of o-nitrophenylhydrazino tri (maleic acid diethyl ester) siloxane, and continuously stirring for 6-8 h to prepare a heat-insulating layer fiber master batch; putting the fabric base layer fiber master batch into a spinning box at the temperature of 180-190 ℃, and using a spiral shell at the spinning speed of 800-1000 m/minSpinning by using a rod extruder, and carrying out side-blowing cooling and curing for 25-35 min under the conditions of 0-4 ℃, 20-40% of humidity and 0.9-1.3 m/s of wind speed to prepare a thermal insulation layer fiber; co-twisting and tatting the fibers of the heat insulation layer to obtain 100-140 g/m 2 The heat insulation layer of (2);
(3) under the conditions of room temperature and argon protection, paving a material base layer and a heat insulation layer in sequence from bottom to top, dipping the material base layer and the heat insulation layer in an acetic acid solution of ammonium acetate with the mass fraction of 10-20% and the mass fraction of 1-2 times of that of the fabric base layer, treating the material base layer for 10-20 min under the conditions of 2400-2500 MHz and 700-900W microwaves, then dripping an ethanol solution of sodium ethoxide with the mass fraction of 1-3% and the mass fraction of 3-5 times of that of the fabric base layer for 40-60 drops/min, continuing to perform microwave treatment for 8-18 min, adding tribromooxyphosphorus 0.7-0.9 time of that of the fabric base layer, continuing to perform microwave treatment for 18-28 min, adding potassium persulfate with the mass fraction of 1-2 times of the fabric base layer at the temperature of 60-70 ℃, continuing to perform microwave treatment for 5-10 min, then dripping a 20% sodium hydroxide solution with the mass fraction of 40-60 drops/min to adjust the pH to 7-9, continuing to perform microwave treatment for 1-3 min, then dripping thionyl chloride with the mass fraction of 1-1.4 times of the fabric base layer for 40-60 drops/min, continuing the microwave treatment for 30-50 min, then adding nano titanium dioxide with the mass of 0.06-0.08 times of the base layer of the fabric, continuing the microwave treatment for 8-18 min, then immersing into a phosphorus pentasulfide solution with the mass of 5-10 times of the base layer of the fabric, continuing the microwave treatment for 50-70 min, and performing microwave treatment for 2-4 m 3 Introducing 100-120 ℃ steam for 5-7 min/min, rolling for 1-3 times at 188-190 ℃ and 8-10 MPa at 220-240 m/min, and preparing to obtain 210-290 g/m 2 The insect-proof heat-insulating fabric.
5. The preparation method of the insect-proof heat-insulating fabric as claimed in claim 4, wherein the preparation method of the fabric base layer fiber master batch in the step (1) is as follows: under the conditions of 60-80 ℃ and 2-4 MPa, polytetrafluoroethylene and 3-hydroxy-5-amino propenyl butenone are mixed according to the mass ratio of 1: 0.3-1: 0.5 mixing, stirring for 30-50 min at 500-700 r/min, then dripping dibenzoyl peroxide with the mass of 0.1-0.3 time that of polytetrafluoroethylene at 40-60 drops/min, stirring for 2-4 h at 900-1100 r/min, cooling to room temperature at 3-5 ℃/min, filtering, washing for 2-4 times with absolute ethyl alcohol and deionized water respectively, and drying for 2-3 h at 30-50 ℃ to prepare the fabric base layer fiber master batch.
6. The preparation method of the insect-proof heat-insulating fabric as claimed in claim 5, wherein the preparation method of the 3-hydroxy-5-amino propenyl benzyl ketene is as follows: under the conditions of room temperature and argon protection, mixing 2-chloropropylamine and o-hydroxy crotone according to a mass ratio of 1: 1.2-1: 1.4, stirring for 10-20 min at 500-700 r/min, then adding aluminum trichloride accounting for 0.01-0.03 time of the mass of 2-chloropropene amine, cooling to 1-5 ℃ at 3-5 ℃/min, and continuously stirring for 6-8 h to prepare the 3-hydroxy-5-amino propenyl benzyl ketone.
7. The preparation method of the insect-proof heat-insulating fabric as claimed in claim 5, wherein the molecular weight of the polytetrafluoroethylene is 1600-2000.
8. The preparation method of the insect-proof heat-insulating fabric as claimed in claim 4, wherein the preparation method of the o-nitrophenylhydrazino tri (diacetoxy maleate) siloxane in the step (2) is as follows: at the temperature of 60-80 ℃, mixing tris (hydroxyethoxy) chlorosilane and maleic acid according to the mass ratio of 1: 1.3-1: 1.7, stirring for 10-20 min at 500-700 r/min, then dripping concentrated sulfuric acid with the mass fraction of 98% and the mass fraction of 0.03-0.04 times of that of the tris (hydroxyethoxy) chlorosilane into the solution at 40-60 drops/min, and stirring for 2-4 h at 1200-1300 r/min to prepare the tris (maleic diethoxy) chlorosiloxane; under the conditions of room temperature and argon protection, mixing tris (maleic acid diethyl ester) chlorosiloxane and o-nitrophenylhydrazine according to a mass ratio of 1: 0.4-1: 0.6, stirring for 10-20 min at 500-700 r/min, then adding aluminum trichloride of which the mass is 0.01-0.03 time that of the tri (maleic acid diethyl ester) chlorosiloxane, cooling to 1-5 ℃ at 3-5 ℃/min, and continuously stirring for 6-8 h to prepare the o-nitrophenylhydrazine tri (maleic acid diethyl ester) siloxane.
9. The preparation method of the insect-proof heat-insulating fabric as claimed in claim 4, wherein the preparation method of the 3-hydroxy anthranilic acid dichloroacetamide in the step (2) is as follows: under the conditions of room temperature and argon protection, 3-hydroxy anthranilic acid and dichloroacetamide are mixed according to the mass ratio of 1: 0.6-1: 0.8, stirring for 20-30 min at 500-700 r/min, then adding nano titanium dioxide with the mass of 0.06-0.08 times of that of 3-hydroxy anthranilic acid, heating to 80-100 ℃ at 9-10 ℃/min, and continuously stirring for 2-4 h to prepare the 3-hydroxy anthranilic acid dichloroacetamide.
10. The preparation method of the insect-proof heat-insulating fabric as claimed in claim 4, wherein the preparation method of the phosphorus pentasulfide solution in the step (3) is as follows: under the conditions of room temperature and argon protection, phosphorus pentasulfide, sodium carbonate and ethyl acetate are mixed according to the mass ratio of 1: 0.3: 10-1: 0.5: 12, stirring for 1-3 h at 500-700 r/min to prepare the phosphorus pentasulfide solution.
CN202210555524.1A 2022-05-19 2022-05-19 Insect-proof heat-insulation fabric and preparation method thereof Pending CN114801375A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115323777A (en) * 2022-08-15 2022-11-11 魏常印 Wear-resistant non-ironing fabric and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115323777A (en) * 2022-08-15 2022-11-11 魏常印 Wear-resistant non-ironing fabric and preparation method thereof

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