CN113897781A - High-strength flame-retardant antibacterial fabric and preparation method thereof - Google Patents

High-strength flame-retardant antibacterial fabric and preparation method thereof Download PDF

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CN113897781A
CN113897781A CN202111383469.4A CN202111383469A CN113897781A CN 113897781 A CN113897781 A CN 113897781A CN 202111383469 A CN202111383469 A CN 202111383469A CN 113897781 A CN113897781 A CN 113897781A
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flame
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vinylon
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antibacterial fabric
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徐唐
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/35Heterocyclic compounds
    • D06M13/355Heterocyclic compounds having six-membered heterocyclic rings
    • D06M13/358Triazines
    • D06M13/364Cyanuric acid; Isocyanuric acid; Derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/18Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/24Polymers or copolymers of alkenylalcohols or esters thereof; Polymers or copolymers of alkenylethers, acetals or ketones
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties

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Abstract

The invention provides a high-strength flame-retardant antibacterial fabric and a preparation method thereof, belonging to the technical field of fabrics and prepared from flame-retardant modified vinylon, deionized water and tetraethyl titanate, wherein the flame-retardant modified vinylon is prepared by graft copolymerization of a flame retardant and vinylon, and the chemical structural formula of the flame-retardant modified vinylon is as shown in the following formula, wherein n is 100-500-. The flame-retardant modified vinylon prepared by the invention is prepared by polymerizing and modifying vinylon fibers and the prepared intermediate B, so that a branched chain part rich in nitrogen is grafted to a vinylon molecular chain, and a good flame-retardant modification effect is achieved.
Figure DDA0003366515230000011

Description

High-strength flame-retardant antibacterial fabric and preparation method thereof
Technical Field
The invention relates to the technical field of fabrics, in particular to a high-strength flame-retardant antibacterial fabric and a preparation method thereof.
Background
With the development of society, the requirements of people on fabrics are increasingly improved, especially in special occasions. The flame retardant property of the fabric is completely determined by the flame retardant property of the fabric fiber.
The flame-retardant fiber is a fiber which can not burn or can not burn sufficiently after being contacted with a fire source, only has small flame and can extinguish the flame quickly and automatically after the fire source is removed. Currently, the commonly used flame-retardant fibers are: PBI fibers, PVC fibers, PTFE, PPTA, pryianitz fibers, polyamide-imide fibers. The Prylanitz fiber has good hygroscopicity, does not melt under the action of radiant heat or flame, and can be used for a water-resisting vapor layer of fire-fighting clothing.
The autogenous fiber with flame retardant property has excellent solid flame retardant property, but has poor wearability and higher manufacturing cost, so that most of the existing flame retardant fibers carry out flame retardant modification on the traditional fiber. Proban finishing (Pulex finishing) of cotton fabrics is a common flame-retardant finishing method for the cotton fabrics, and is characterized in that low-molecular-weight aqueous solutions of tetrakis hydroxymethyl phosphonium sulfate, tetrakis hydroxymethyl phosphonium chloride and the like are adopted to be padded into the fabrics, the content of appropriate active ingredients is controlled, phosphorus compounds are infiltrated into amorphous regions and gaps of cotton fibers, the water content of the phosphorus compounds is controlled, then NH3 and hydroxymethyl groups in phosphorus precondensates are crosslinked through quantitative fumigation of ammonia gas, a flame-retardant polymer is formed inside the fibers, and a flame-retardant synergistic effect of phosphorus-nitrogen synergy is established; and then the trivalent phosphorus in the flame retardant in the fiber is converted into pentavalent phosphorus through oxidation, so that the flame retardant is further stabilized in the fiber. After the cotton fabric finished and processed by the method meets high-temperature flame, the phosphorus-containing compound is firstly decomposed to generate phosphoric acid or polyphosphoric anhydride which is not easy to volatilize, and the phosphoric acid or polyphosphoric anhydride and hydroxyl of cellulose are subjected to dehydration reaction to carbonize the fiber, so that the flame retardant effect is achieved. The fabric treated by the Proban method is soft in hand feeling, durable in flame retardant property, capable of bearing 50 (even 200) washes, still capable of keeping good flame retardant property and comfort of the fabric, suitable for being made into various protective clothing, bedding, decorative articles, flame retardant pajamas for children and the like, and is an important method for durable flame retardant finishing of cotton fabrics at present. But the biggest defect of the Pulubenzene finishing is that the breaking strength of the finished fabric is obviously reduced, and the strength is usually reduced by 20%; in particular, there is a significant reduction in tear strength. Thus, the application of such flame retardant processing techniques is seriously affected.
The common vinylon and the high-strength vinylon are both prepared by acetalizing hydroxyl groups of the PVA fiber with formaldehyde, and the hydroxyl groups in the PVA fiber are terminated with formaldehyde, so that the content of the hydroxyl groups in the fiber is greatly reduced, and the problem that the PVA fiber is easy to swell, adhere and dissolve is solved. However, the hydroxyl end-capping treatment by using formaldehyde has the problem of high requirement on the air tightness of hydroformylation processing equipment, and even if trace formaldehyde is leaked, the environment is polluted and workers are injured. Today, with increasing awareness of environmental protection, the use of formaldehyde as a method for controlling the hydroxyl content is not suitable for the current environmental protection requirements.
Disclosure of Invention
The invention aims to provide a high-strength flame-retardant antibacterial fabric and a preparation method thereof.
The technical scheme of the invention is realized as follows:
the invention provides a high-strength flame-retardant antibacterial fabric which is prepared from flame-retardant modified vinylon, deionized water and tetraethyl titanate, wherein the flame-retardant modified vinylon is prepared by graft copolymerization of a flame retardant and vinylon, and the chemical structural formula of the flame-retardant modified vinylon is shown as a formula I:
Figure BDA0003366515210000031
wherein n is 100-.
As a further improvement of the invention, the preparation method of the flame-retardant modified vinylon comprises the following steps:
s1, adjusting the pH value of a formaldehyde solution to 8-10 by using a NaOH solution, adding melamine, heating to 75-85 ℃, reacting for 1-2h, adding a saturated sodium bicarbonate solution to quench the reaction, then adding an extract to extract, taking an oil phase, and removing the solvent under reduced pressure to obtain an intermediate A, wherein the chemical structural formula is shown as a formula II:
Figure BDA0003366515210000032
s2, dissolving the intermediate A and 3-bromopropylene in an organic solvent, heating to 70-90 ℃, adding potassium carbonate, reacting for 3-5h, adding a saturated sodium bicarbonate solution, quenching, taking an organic phase, and removing the solvent under reduced pressure to obtain an intermediate B, wherein the chemical structural formula is shown as a formula III:
Figure BDA0003366515210000041
and S3, mixing the intermediate B, the vinylon fiber and an initiator, melting under a heating condition to perform graft copolymerization, feeding into a screw extruder, heating, extruding, cooling, and finally cutting into uniform flame-retardant modified vinylon.
As a further improvement of the present invention, in step S1, the quantitative ratio of the methanol to the melamine is 1: (1-1.1).
As a further improvement of the present invention, the ratio of the amounts of the intermediate a, 3-bromopropene and potassium carbonate in step S2 is 1: (0.9-1.2): (0.01-0.1).
As a further improvement of the present invention, the mass ratio of the intermediate B, the vinylon fiber and the initiator in step S3 is 5: (3-5): (0.01-0.02).
As a further improvement of the invention, the extract is at least one selected from dichloromethane, chloroform, tetrahydrofuran, petroleum ether, ethyl acetate, methyl acetate and cyclohexane; the organic solvent is at least one selected from dichloromethane, toluene, benzene, xylene, chloroform, tetrahydrofuran, petroleum ether, ethyl acetate, methyl acetate and cyclohexane; the initiator is selected from one or a mixture of a plurality of azodiisobutyronitrile, azodiisoheptonitrile, sodium bisulfite, tert-butyl hydroperoxide, benzoyl peroxide, lauroyl peroxide, cumene hydroperoxide, di-tert-butyl peroxide, tert-butyl peroxybenzoate, dicumyl peroxide, cyclohexanone peroxide, tert-butyl peroxypivalate, methyl ethyl ketone peroxide, diisopropyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, sodium persulfate, potassium persulfate and ammonium persulfate; the melting temperature is 245-250 ℃.
The invention further provides a preparation method of the high-strength flame-retardant antibacterial fabric, which comprises the following steps:
(1) performing melt spinning on the flame-retardant modified vinylon to obtain flame-retardant modified vinylon fibers;
(2) blowing the flame-retardant modified vinylon fibers to a roller, collecting the flame-retardant modified vinylon fibers on a flat plate to form single-layer yarns, and replacing the flat plate in time to ensure that the single-layer yarns are formed on the flat plate;
(3) stacking the single-layer yarns, weighing to obtain a weight a, placing the single-layer yarns in a closed hydrothermal reaction kettle, heating and ultrasonically treating the single-layer yarns to obtain melt-blown fabric containing interlayer water, drying and weighing to obtain a weight b, and obtaining melt-blown fabric containing interlayer water;
(4) tetraethyl titanate with a certain water content is added according to a hydrolysis equation of the tetraethyl titanate; ultrasonically dispersing under a sealed condition until full reaction is achieved, and cleaning with absolute ethyl alcohol and performing suction filtration once; reacting in a closed hydrothermal reaction kettle at a certain temperature to prepare TiO2And (3) performing intercalation melt-blown fabric to obtain the high-strength flame-retardant antibacterial fabric.
As a further improvement of the invention, the melting temperature in the step S1 is 245-250 ℃; in the step S2, the ultrasonic temperature is 40-60 ℃, the ultrasonic power is 1000-2000W, and the drying method is drying for 1-2h at 80-90 ℃.
As a further improvement of the invention, in the step S4, the water content is b-a, and the addition amount of the absolute ethyl alcohol is 2-6% of the total mass of the melt-blown fabric containing interlayer water; the hydrothermal reaction temperature is 90-100 ℃.
As a further improvement of the present invention, the ratio of the amounts of the tetraethyl titanate and water in step S4 is 1: 4.
the invention has the following beneficial effects: the flame-retardant modified vinylon prepared by the invention is prepared by polymerizing and modifying vinylon fibers and the prepared intermediate B, so that a branched chain part rich in nitrogen is grafted to a vinylon molecular chain, and a good flame-retardant modification effect is achieved.
According to the invention, the single-layer yarn is prepared, the melt-blown yarn containing water between layers is prepared, after drying, water molecules between the layers are combined with amino groups on the flame-retardant modified vinylon graft chains, the yarns cannot be dried, and further undergo hydrolysis reaction with tetraethyl titanate to generate titanium dioxide in the interlayer reaction, and the obtained fabric contains titanium dioxide and has good photocatalytic antibacterial performance.
The preparation method is simple, the prepared melt-blown non-woven fabric has excellent flame retardance, high strength and antibacterial performance, and the flame-retardant structure is grafted on the vinylon molecular chain, so that the fabric has good water washing resistance and durability, and the service life of the material is prolonged.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a synthesis scheme of the flame retardant modified vinylon of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
The embodiment provides a high-strength flame-retardant antibacterial fabric, which comprises the following steps:
(1) the preparation method of the flame-retardant modified vinylon comprises the following steps:
the reaction equation is shown in FIG. 1.
S1, adjusting the pH value of a formaldehyde solution to 8 by using a NaOH solution, adding melamine, heating to 75-85 ℃, reacting for 1h, adding a saturated sodium bicarbonate solution to quench the reaction, then adding dichloromethane with the same volume as the reaction solution to extract, taking an oil phase, and removing the solvent under reduced pressure to obtain an intermediate A; the mass ratio of the methanol to the melamine is 1: 1;
s2, dissolving the intermediate A and 3-bromopropylene in dichloromethane, heating to 70 ℃, adding potassium carbonate, reacting for 3 hours, adding a saturated sodium bicarbonate solution, quenching, taking an organic phase, and removing the solvent under reduced pressure to obtain an intermediate B; the mass ratio of the intermediate A, the 3-bromopropylene and the potassium carbonate is 1: 0.9: 0.01;
s3, mixing the intermediate B, vinylon fibers and azodiisobutyronitrile, heating to 245 ℃, carrying out graft copolymerization, feeding into a screw extruder, heating, extruding, cooling, and finally cutting into uniform flame-retardant modified vinylon; the mass ratio of the intermediate B to the vinylon fibers to the initiator is 5: 3: 0.01.
(2) heating the flame-retardant modified vinylon to 245 ℃ for spinning to obtain flame-retardant modified vinylon fibers;
(3) blowing the flame-retardant modified vinylon fibers to a roller, collecting the flame-retardant modified vinylon fibers on a flat plate to form single-layer yarns, and replacing the flat plate in time to ensure that the single-layer yarns are formed on the flat plate;
(4) stacking the single-layer yarns, weighing to obtain 18.5g of single-layer yarns, placing the single-layer yarns in a closed hydrothermal reaction kettle, heating to 40 ℃, performing 1000W ultrasonic treatment to obtain melt-blown fabric containing interlayer water, drying at 80 ℃ for 1h, weighing to obtain 20.1g of melt-blown fabric containing interlayer water;
(5) adding 81g of tetraethyl titanate by taking the water content of 1.6g, carrying out ultrasonic dispersion under a sealed condition until the reaction is fully carried out, cleaning with absolute ethyl alcohol, and carrying out suction filtration once, wherein the addition amount of the absolute ethyl alcohol is 2% of the total mass of the meltblown fabric containing interlayer water; TiO is prepared by reaction in a closed hydrothermal reaction kettle at the temperature of 90 DEG C2The high-strength flame-retardant antibacterial fabric is obtained by intercalation melt-blown fabric;
the hydrolysis equation for tetraethyl titanate is as follows:
Ti(O-C2H5)4+4H2O=Ti(OH)4+4C2H5OH。
example 2
The embodiment provides a high-strength flame-retardant antibacterial fabric, which comprises the following steps:
(1) the preparation method of the flame-retardant modified vinylon comprises the following steps:
the reaction equation is shown in FIG. 1.
S1, adjusting the pH value of a formaldehyde solution to 10 by using a NaOH solution, adding melamine, heating to 85 ℃, reacting for 2 hours, adding a saturated sodium bicarbonate solution to quench the reaction, then adding dichloromethane with the same volume as the reaction solution to extract, taking an oil phase, and removing the solvent under reduced pressure to obtain an intermediate A; the mass ratio of the methanol to the melamine is 1: 1.1;
s2, dissolving the intermediate A and 3-bromopropylene in chloroform, heating to 90 ℃, adding potassium carbonate, reacting for 5 hours, adding a saturated sodium bicarbonate solution to quench the reaction, taking an organic phase, and removing the solvent under reduced pressure to obtain an intermediate B; the mass ratio of the intermediate A, the 3-bromopropylene and the potassium carbonate is 1: 1.2: 0.1;
s3, mixing the intermediate B, vinylon fibers and tert-butyl peroxybenzoate, heating to 250 ℃, carrying out graft copolymerization, feeding into a screw extruder, heating, extruding, cooling, and finally cutting into uniform flame-retardant modified vinylon; the mass ratio of the intermediate B to the vinylon fibers to the initiator is 5: 5: 0.02.
(2) heating the flame-retardant modified vinylon to 250 ℃ for spinning to obtain flame-retardant modified vinylon fibers;
(3) blowing the flame-retardant modified vinylon fibers to a roller, collecting the flame-retardant modified vinylon fibers on a flat plate to form single-layer yarns, and replacing the flat plate in time to ensure that the single-layer yarns are formed on the flat plate;
(4) stacking the single-layer yarns, weighing to obtain 18.5g of single-layer yarns, placing the single-layer yarns in a closed hydrothermal reaction kettle, heating to 60 ℃, performing 2000W ultrasonic treatment to obtain melt-blown fabric containing interlayer water, drying at 90 ℃ for 2h, weighing to obtain 20.3g of melt-blown fabric containing interlayer water;
(5) based on the water content of 18g, 91.2g of tetraethyl titanate is added, ultrasonic dispersion is carried out under a sealing condition until full reaction is achieved, absolute ethyl alcohol is cleaned and filtered once, and the addition amount of the absolute ethyl alcohol is 6% of the total mass of the meltblown fabric containing interlayer water; TiO is prepared by reaction in a closed hydrothermal reaction kettle at the temperature of 100 DEG C2And (3) performing intercalation melt-blown fabric to obtain the high-strength flame-retardant antibacterial fabric.
Example 3
The embodiment provides a high-strength flame-retardant antibacterial fabric, which comprises the following steps:
(1) the preparation method of the flame-retardant modified vinylon comprises the following steps:
the reaction equation is shown in FIG. 1.
S1, adjusting the pH value of a formaldehyde solution to 9 by using a NaOH solution, adding melamine, heating to 80 ℃, reacting for 1.5h, adding a saturated sodium bicarbonate solution to quench the reaction, then adding dichloromethane with the same volume as the reaction solution to extract, taking an oil phase, and removing the solvent under reduced pressure to obtain an intermediate A; the mass ratio of the methanol to the melamine is 1: 1.05;
s2, dissolving the intermediate A and 3-bromopropylene in toluene, heating to 80 ℃, adding potassium carbonate, reacting for 4 hours, adding a saturated sodium bicarbonate solution, quenching, taking an organic phase, and removing the solvent under reduced pressure to obtain an intermediate B; the mass ratio of the intermediate A, the 3-bromopropylene and the potassium carbonate is 1: 1: 0.05;
s3, mixing the intermediate B, vinylon fibers and sodium persulfate, heating to 247 ℃, carrying out graft copolymerization, feeding into a screw extruder, heating, extruding, cooling, and finally cutting into uniform flame-retardant modified vinylon; the mass ratio of the intermediate B to the vinylon fibers to the initiator is 5: 4: 0.015.
(2) heating the flame-retardant modified vinylon to 247 ℃ for spinning to obtain flame-retardant modified vinylon fibers;
(3) blowing the flame-retardant modified vinylon fibers to a roller, collecting the flame-retardant modified vinylon fibers on a flat plate to form single-layer yarns, and replacing the flat plate in time to ensure that the single-layer yarns are formed on the flat plate;
(4) stacking the single-layer yarns, weighing to obtain 18.9g of single-layer yarns, placing the single-layer yarns in a closed hydrothermal reaction kettle, heating to 50 ℃, performing 1500W ultrasonic treatment to obtain meltblown fabric containing interlayer water, drying at 85 ℃ for 1.5h, weighing to obtain 20.9g of meltblown fabric containing interlayer water;
(5) adding 101g of tetraethyl titanate by taking the water content of 2g, ultrasonically dispersing under a sealed condition until the reaction is fully performed, cleaning with absolute ethyl alcohol, and performing suction filtration once, wherein the addition amount of the absolute ethyl alcohol is 4% of the total mass of the meltblown fabric containing interlayer water; TiO is prepared by reaction in a closed hydrothermal reaction kettle at the temperature of 95 DEG C2And (3) performing intercalation melt-blown fabric to obtain the high-strength flame-retardant antibacterial fabric.
Comparative example 1
Compared with the example 3, the flame-retardant modified vinylon fiber is replaced by the equivalent vinylon fiber, and other conditions are not changed.
Comparative example 2
In comparison with example 3, no tetraethyl titanate was added, and the other conditions were unchanged.
Test example 1
The mechanical property test of the high-strength flame-retardant antibacterial fabric prepared in the embodiments 1-3 and the comparative examples 1-2 is carried out, and the results are shown in table 1.
TABLE 1
Group of Breaking strength (N) Elongation at Break (%)
Example 1 802 28
Example 2 807 29
Example 3 810 30
Comparative example 1 798 26
Comparative example 2 800 27
As can be seen from the above table, the high-strength flame-retardant antibacterial fabric prepared by the invention has good mechanical properties.
Test example 2
The flame retardant performance test of the high-strength flame-retardant antibacterial fabric prepared in the examples 1-3 and the comparative examples 1-2 of the invention is carried out, and the results are shown in table 2.
Figure BDA0003366515210000101
Figure BDA0003366515210000111
As can be seen from the above table, the high-strength flame-retardant antibacterial fabric prepared by the invention has good flame-retardant performance.
Test example 3
The high-strength flame-retardant antibacterial fabrics prepared in the examples 1-3 and the comparative examples 1-2 are tested by adopting an oscillation method (GB/T20944.3-2008). The results are shown in Table 3.
TABLE 3
Group of Antibacterial ratio of Escherichia coli (%) Staphylococcus aureus antibacterial ratio (%)
Example 1 >99 >99
Example 2 >99 >99
Example 3 >99 >99
Comparative example 1 92 94
Comparative example 2 70 67
The high-strength flame-retardant antibacterial fabric prepared in the examples 1-3 and the comparative examples 1-2 is subjected to an anti-mite test, the test indexes are according to the national standard GBT24253-2009, and the results are shown in Table 4.
TABLE 4
Group of Anti-mite ratio (%)
Example 1 91
Example 2 92
Example 3 94
Comparative example 1 88
Comparative example 2 52
As can be seen from the table above, the high-strength flame-retardant antibacterial fabric prepared by the invention has good antibacterial and anti-mite performances.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. The high-strength flame-retardant antibacterial fabric is characterized by being prepared from flame-retardant modified vinylon, deionized water and tetraethyl titanate, wherein the flame-retardant modified vinylon is prepared by graft copolymerization of a flame retardant and vinylon, and the chemical structural formula of the flame-retardant modified vinylon is shown as a formula I:
Figure FDA0003366515200000011
wherein n is 100-.
2. The high-strength flame-retardant antibacterial fabric according to claim 1, wherein the flame-retardant modified vinylon is prepared by the following method:
s1, adjusting the pH value of a formaldehyde solution to 8-10 by using a NaOH solution, adding melamine, heating to 75-85 ℃, reacting for 1-2h, adding a saturated sodium bicarbonate solution to quench the reaction, then adding an extract to extract, taking an oil phase, and removing the solvent under reduced pressure to obtain an intermediate A, wherein the chemical structural formula is shown as a formula II:
Figure FDA0003366515200000012
s2, dissolving the intermediate A and 3-bromopropylene in an organic solvent, heating to 70-90 ℃, adding potassium carbonate, reacting for 3-5h, adding a saturated sodium bicarbonate solution, quenching, taking an organic phase, and removing the solvent under reduced pressure to obtain an intermediate B, wherein the chemical structural formula is shown as a formula III:
Figure FDA0003366515200000021
and S3, mixing the intermediate B, the vinylon fiber and an initiator, melting under a heating condition to perform graft copolymerization, feeding into a screw extruder, heating, extruding, cooling, and finally cutting into uniform flame-retardant modified vinylon.
3. The high-strength flame-retardant antibacterial fabric according to claim 2, wherein the mass ratio of the methanol to the melamine in step S1 is 1: (1-1.1).
4. The high-strength flame-retardant antibacterial fabric according to claim 2, wherein in the step S2, the ratio of the amounts of the intermediate a, 3-bromopropylene and potassium carbonate is 1: (0.9-1.2): (0.01-0.1).
5. The high-strength flame-retardant antibacterial fabric according to claim 2, wherein the mass ratio of the intermediate B, the vinylon fibers and the initiator in the step S3 is 5: (3-5): (0.01-0.02).
6. The high-strength flame-retardant antibacterial fabric according to claim 2, wherein the extract is at least one selected from dichloromethane, chloroform, tetrahydrofuran, petroleum ether, ethyl acetate, methyl acetate and cyclohexane; the organic solvent is at least one selected from dichloromethane, toluene, benzene, xylene, chloroform, tetrahydrofuran, petroleum ether, ethyl acetate, methyl acetate and cyclohexane; the initiator is selected from one or a mixture of a plurality of azodiisobutyronitrile, azodiisoheptonitrile, sodium bisulfite, tert-butyl hydroperoxide, benzoyl peroxide, lauroyl peroxide, cumene hydroperoxide, di-tert-butyl peroxide, tert-butyl peroxybenzoate, dicumyl peroxide, cyclohexanone peroxide, tert-butyl peroxypivalate, methyl ethyl ketone peroxide, diisopropyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, sodium persulfate, potassium persulfate and ammonium persulfate; the melting temperature is 245-250 ℃.
7. A preparation method of the high-strength flame-retardant antibacterial fabric as claimed in any one of claims 1 to 6, characterized by comprising the following steps:
(1) performing melt spinning on the flame-retardant modified vinylon to obtain flame-retardant modified vinylon fibers;
(2) blowing the flame-retardant modified vinylon fibers to a roller, collecting the flame-retardant modified vinylon fibers on a flat plate to form single-layer yarns, and replacing the flat plate in time to ensure that the single-layer yarns are formed on the flat plate;
(3) stacking the single-layer yarns, weighing to obtain a weight a, placing the single-layer yarns in a closed hydrothermal reaction kettle, heating and ultrasonically treating the single-layer yarns to obtain melt-blown fabric containing interlayer water, drying and weighing to obtain a weight b, and obtaining melt-blown fabric containing interlayer water;
(4) tetraethyl titanate with a certain water content is added according to a hydrolysis equation of the tetraethyl titanate; ultrasonically dispersing under a sealed condition until full reaction is achieved, and cleaning with absolute ethyl alcohol and performing suction filtration once; reacting in a closed hydrothermal reaction kettle at a certain temperature to prepare TiO2And (3) performing intercalation melt-blown fabric to obtain the high-strength flame-retardant antibacterial fabric.
8. The method as claimed in claim 7, wherein the melting temperature in step S1 is 245-250 ℃; in the step S2, the ultrasonic temperature is 40-60 ℃, the ultrasonic power is 1000-2000W, and the drying method is drying for 1-2h at 80-90 ℃.
9. The method according to claim 7, wherein the water content in step S4 is b-a, and the amount of absolute ethanol added is 2-6% of the total mass of the meltblown fabric containing interlayer water; the hydrothermal reaction temperature is 90-100 ℃.
10. The production method according to claim 7, wherein the ratio of the amounts of the tetraethyl titanate and water in step S4 is 1: 4.
CN202111383469.4A 2021-11-22 2021-11-22 High-strength flame-retardant antibacterial fabric and preparation method thereof Pending CN113897781A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1259594A (en) * 1998-12-16 2000-07-12 可乐丽股份有限公司 Thermoplastic polyvinyl alcohol fiber and mfg. method therefor
CN103436977A (en) * 2013-08-28 2013-12-11 江苏博特新材料有限公司 Flame-retardant melt-spun high-strength high-modulus polyvinyl alcohol fiber and preparation method thereof
CN104073903A (en) * 2014-07-08 2014-10-01 世源科技(嘉兴)医疗电子有限公司 High-temperature water soluble melt spinning flame retardant polyvinyl alcohol fiber and application thereof
US20150291786A1 (en) * 2014-04-11 2015-10-15 Georgia-Pacific Consumer Products Lp Polyvinyl alcohol fibers and films with mineral fillers and small cellulose particles

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1259594A (en) * 1998-12-16 2000-07-12 可乐丽股份有限公司 Thermoplastic polyvinyl alcohol fiber and mfg. method therefor
CN103436977A (en) * 2013-08-28 2013-12-11 江苏博特新材料有限公司 Flame-retardant melt-spun high-strength high-modulus polyvinyl alcohol fiber and preparation method thereof
US20150291786A1 (en) * 2014-04-11 2015-10-15 Georgia-Pacific Consumer Products Lp Polyvinyl alcohol fibers and films with mineral fillers and small cellulose particles
CN104073903A (en) * 2014-07-08 2014-10-01 世源科技(嘉兴)医疗电子有限公司 High-temperature water soluble melt spinning flame retardant polyvinyl alcohol fiber and application thereof

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Application publication date: 20220107