CN114635289A - Antibacterial composite fabric and preparation method thereof - Google Patents

Antibacterial composite fabric and preparation method thereof Download PDF

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CN114635289A
CN114635289A CN202210339595.8A CN202210339595A CN114635289A CN 114635289 A CN114635289 A CN 114635289A CN 202210339595 A CN202210339595 A CN 202210339595A CN 114635289 A CN114635289 A CN 114635289A
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袁波
吴陶生
黄婷婷
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    • 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
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    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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    • C08G83/008—Supramolecular polymers
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/208—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads cellulose-based
    • D03D15/217—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads cellulose-based natural from plants, e.g. cotton
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/283—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads synthetic polymer-based, e.g. polyamide or polyester fibres
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    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
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    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
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    • 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
    • D06M2101/38—Polyurethanes
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties

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Abstract

The invention discloses an antibacterial composite fabric, which belongs to the field of fabric antibacterial and comprises an antibacterial agent and a composite fabric, wherein the antibacterial agent is prepared from the following raw materials: 0.5-5 parts of modified MOF; 0.5-5 parts of modified polyacrylamide; 0.5-5 parts of sodium alkyl benzene sulfonate; 20-30 parts of purified water. The antibacterial agent can improve the breaking strength and the tearing strength of the fabric on the premise of ensuring the wear resistance times, hydrostatic pressure resistance and puncture resistance of the fabric, has a very remarkable effect on the antibacterial performance of the fabric, particularly obviously improves the antibacterial performance of the fabric after high-temperature treatment, light treatment and saline water treatment, and in addition, the modified MOF is used for ensuring the high hydrophobicity of the fabric.

Description

Antibacterial composite fabric and preparation method thereof
Technical Field
The invention relates to the field of fabric antibiosis, in particular to an antibacterial composite fabric, an antibacterial agent and a preparation method thereof.
Background
The antibacterial fabric is a novel functional material with the function of killing or inhibiting microorganisms, and some fiber materials in nature have good antibacterial performance, such as bamboo fiber fabrics, but the antibacterial performance is weaker and weaker along with the continuous use of the bamboo fiber fabrics.
In addition, the antibacterial material used in the market generally refers to a kind of functional material which can inhibit or kill bacteria by adding a certain amount of substance with antibacterial function, but the antibacterial performance is insufficient in light stability, high temperature stability and stability after saline water treatment, and particularly the performance in the composite fabric containing cotton threads is very poor.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides an antibacterial composite fabric, an antibacterial agent and a preparation method thereof.
The antibacterial composite fabric comprises an antibacterial agent and the composite fabric, wherein the antibacterial agent is prepared from the following raw materials:
Figure BDA0003578505290000011
preferably, the preparation raw materials of the modified MOF comprise the following components:
Figure BDA0003578505290000012
preferably, the modified MOF comprises the following preparation steps:
s1, weighing 5-tert-butyl isophthalic acid, N-dimethylacetamide, copper acetate, methanol, PAA, magnesium borate, leucine, manganese dioxide and ferric oxide in parts by weight;
s2, dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing A and B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate, manganese dioxide and leucine, and pouring the mixture into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 500-;
s5, pouring the ferric oxide into the solution E in an emulsifying machine, wherein the rotating speed of the emulsifying machine is 500-;
s6, adding methanol into the F solution, standing at the reaction temperature of 15-50 ℃ to obtain modified MOF containing impurities;
s7: and (5) purifying the modified MOF containing the impurities obtained in the step S6 to obtain the modified MOF.
Preferably, the preparation raw materials of the modified acrylamide comprise the following components:
20-50 parts of acrylamide;
0.5-3 parts of potassium persulfate;
1-15 parts of lignin.
Preferably, the modified polyacrylamide comprises the following preparation steps:
s1, weighing acrylamide, potassium persulfate and lignin according to parts by weight.
S2, pouring acrylamide, potassium persulfate and lignin into a ball mill, wherein the rotating speed of the ball mill is 500-1000r/min, the temperature is 40-100 ℃, and the reaction time is 0.2-1h, so as to obtain the modified polyacrylamide.
The inventor of the invention finds that the composite fabric is poor in antibacterial stability without adding the modified polyacrylamide, especially the antibacterial light stability is remarkably reduced, and the antibacterial agent prepared from the modified polyacrylamide and the modified MOF can play a role in jointly enhancing the performance of products.
Preferably, the preparation method of the antibacterial agent comprises the following steps:
s1: weighing modified MOF, modified polyacrylamide, sodium alkyl benzene sulfonate and purified water according to parts by weight;
s2: and (3) pouring the modified MOF, the modified polyacrylamide, the sodium alkyl benzene sulfonate and the purified water which are weighed in the S1 into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 1000-2000r/min, the temperature is 40-100 ℃, and the reaction time is 0.2-1h to obtain the antibacterial agent.
A preparation method of an antibacterial composite fabric comprises the following steps:
s1, weighing 5-tert-butyl isophthalic acid, N-dimethylacetamide, copper acetate, methanol, PAA, leucine, magnesium borate, manganese dioxide and ferric oxide according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving the N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing the solution A and the solution B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in the S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate, manganese dioxide and leucine, and pouring the mixture into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 500-;
s5, pouring the ferric oxide into the solution E in an emulsifying machine, wherein the rotating speed of the emulsifying machine is 500-;
s6, adding methanol into the F solution, standing at the reaction temperature of 15-50 ℃ to obtain modified MOF containing impurities;
s7: purifying the modified MOF containing impurities obtained from S6 to obtain the modified MOF;
s8: weighing acrylamide, potassium persulfate and lignin according to parts by weight;
s9, pouring acrylamide, potassium persulfate and lignin into a ball mill, wherein the rotating speed of the ball mill is 500-1000r/min, the temperature is 40-100 ℃, and the reaction time is 0.2-1h to obtain modified polyacrylamide;
s10: weighing the modified MOF prepared by S7, the modified polyacrylamide prepared by S9, sodium alkyl benzene sulfonate and purified water in parts by weight, and pouring the 4 materials into an emulsifying machine together, wherein the rotating speed of the emulsifying machine is 1000-2000r/min, the temperature is 40-100 ℃, and the reaction time is 0.2-1h to obtain the antibacterial agent;
s11: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, one strand of warps and two strands of wefts with the arrangement ratio of 2:1 are interwoven to form the polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent at the temperature of 60-80 ℃, reacting for not less than 1h, and after the reaction is finished, performing pre-setting treatment on the fabric at the temperature of 110 ℃ by using an open-width setting machine, dehydrating and drying to obtain the antibacterial composite fabric.
The invention has the beneficial effects that: the antibacterial agent can improve the breaking strength and the tearing strength of the fabric on the premise of ensuring the wear-resisting times, hydrostatic pressure resistance and puncture resistance of the fabric, has a very obvious effect on the antibacterial performance of the fabric, particularly obviously improves the antibacterial property of the fabric after high-temperature treatment, light treatment and saline water treatment, and in addition, the high hydrophobicity of the fabric is ensured by using the modified MOF.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present solution is explained below by way of specific embodiments.
Untreated fabric:
the method comprises the steps of taking polyurethane fibers as warps, enabling the length of the polyurethane fibers to be 35mm, enabling the linear density to be 1.6dtex, enabling cotton fibers to be used as wefts, enabling the length of the cotton threads to be 35mm, enabling one strand of warps and two strands of wefts in a surface-to-inner arrangement ratio of 2:1 to be interwoven to form a polyurethane and cotton composite primary fabric, enabling the primary fabric to be subjected to pre-shaping treatment at 110 ℃ by using an open-width shaping machine, and dehydrating and drying to obtain the antibacterial composite fabric.
Example 1:
s1, weighing 2 parts of 5-tert-butyl isophthalic acid, 30 parts of N, N-dimethylacetamide, 3 parts of hydrated copper acetate, 30 parts of methanol, 1.3 parts of leucine, 1.3 parts of PAA, 5 parts of magnesium borate, 0.7 part of manganese dioxide and 0.7 part of ferric oxide according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving the N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing the solution A and the solution B to obtain a solution C;
s3, dissolving PAA with ethanol, and adding the dissolved PAA solution into the C solution prepared by the S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate, manganese dioxide and leucine, and pouring into an emulsifying machine at the rotating speed of 2000r/min and the temperature of 80 ℃ for reaction for 1h to obtain a solution E;
s5, pouring iron oxide into the solution E in an emulsifying machine, wherein the rotating speed of the emulsifying machine is 2000r/min, the temperature is 70 ℃, and the reaction time is 1.2h to obtain a solution F;
s6, adding methanol into the F solution, standing at the reaction temperature of 30 ℃ to obtain modified MOF containing impurities;
s7: purifying the modified MOF containing impurities obtained in the step S6 to obtain modified MOF;
s8: weighing 35 parts of acrylamide, 2 parts of potassium persulfate and 3 parts of lignin according to parts by weight;
and S9, pouring acrylamide, potassium persulfate and lignin into a ball mill, wherein the rotating speed of the ball mill is 700r/min, the temperature is 60 ℃, and the reaction time is 0.7h to obtain the modified polyacrylamide.
S10: weighing 3 parts of modified MOF prepared by S7, 3 parts of modified polyacrylamide prepared by S9, 8 parts of sodium alkyl benzene sulfonate and 25 parts of purified water in parts by weight, and pouring the 4 parts of modified MOF, sodium alkyl benzene sulfonate and purified water into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 1500r/min, the temperature is 60 ℃, and the reaction time is 0.7h, so as to obtain the antibacterial agent;
s11: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, one strand of warps and two strands of wefts with the arrangement ratio of 2:1 are interwoven to form the polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent at the temperature of 70 ℃, reacting for 2 hours, and after the reaction is finished, performing pre-shaping treatment on the fabric at the temperature of 110 ℃ by using an open-width shaping machine, dehydrating and drying to obtain the antibacterial composite fabric.
Example 2:
s1, weighing 0.2 part of 5-tert-butyl isophthalic acid, 10 parts of N, N-dimethylacetamide, 0.2 part of hydrated copper acetate, 2 parts of methanol, 0.8 part of leucine, 0.8 part of PAA, 2 parts of magnesium borate, 0.5 part of manganese dioxide and 0.5 part of ferric oxide according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving the N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing the solution A and the solution B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in the S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate, manganese dioxide and leucine, and pouring the mixture into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 500r/min, the temperature is 50 ℃, and the reaction time is 0.1h to obtain a solution E;
s5, pouring iron oxide into the solution E in an emulsifying machine, wherein the rotating speed of the emulsifying machine is 500r/min, the temperature is 50 ℃, and the reaction time is 0.1h to obtain a solution F;
s6, adding methanol into the F solution, standing at the reaction temperature of 15 ℃ to obtain modified MOF containing impurities;
s7: purifying the modified MOF containing impurities obtained in the step S6 to obtain modified MOF;
s8: weighing 20 parts of acrylamide, 0.5 part of potassium persulfate and 1 part of lignin according to parts by weight;
s9, pouring acrylamide, potassium persulfate and lignin into a ball mill, wherein the rotating speed of the ball mill is 500r/min, the temperature is 40 ℃, and the reaction time is 0.2h to obtain modified polyacrylamide;
s10: weighing 0.5 part of modified MOF prepared by S7, 0.5 part of modified polyacrylamide prepared by S9, 5 parts of sodium alkyl benzene sulfonate and 20 parts of purified water in parts by weight, and pouring the 4 parts into an emulsifying machine together, wherein the rotating speed of the emulsifying machine is 1000r/min, the temperature is 40 ℃, and the reaction time is 0.2h to obtain the antibacterial agent;
s11: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, one strand of warps and two strands of wefts with the arrangement ratio of 2:1 are interwoven to form the polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent at the temperature of 60 ℃ for 1h, and after the reaction is finished, performing pre-setting treatment on the fabric at the temperature of 110 ℃ by using an open-width setting machine, dehydrating and drying to obtain the antibacterial composite fabric.
Example 3:
s1, weighing 5 parts of 5-tert-butyl isophthalic acid, 50 parts of N, N-dimethylacetamide, 5 parts of hydrated copper acetate, 50 parts of methanol, 2 parts of leucine, 2 parts of PAA, 10 parts of magnesium borate, 1 part of manganese dioxide and 3 parts of ferric oxide according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving the N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing the solution A and the solution B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in the S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate, manganese dioxide and leucine, and pouring into an emulsifying machine at the rotation speed of 5000r/min and the temperature of 100 ℃ for 2 hours to obtain a solution E;
s5, pouring iron oxide into the solution E in an emulsifying machine, wherein the rotating speed of the emulsifying machine is 5000r/min, the temperature is 100 ℃, and the reaction time is 2 hours to obtain a solution F;
s6, adding methanol into the F solution, standing at the reaction temperature of 50 ℃ to obtain modified MOF containing impurities;
s7: purifying the modified MOF containing impurities obtained from S6 to obtain the modified MOF;
s8: weighing 50 parts of acrylamide, 3 parts of potassium persulfate and 15 parts of lignin according to parts by weight;
s9, pouring acrylamide, potassium persulfate and lignin into a ball mill, wherein the rotating speed of the ball mill is 1000r/min, the temperature is 100 ℃, and the reaction time is 1h to obtain modified polyacrylamide;
s10: weighing 5 parts of modified MOF prepared by S7, 5 parts of modified polyacrylamide prepared by S9, 10 parts of sodium alkyl benzene sulfonate and 30 parts of purified water in parts by weight, and pouring 4 of the materials into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 2000r/min, the temperature is 100 ℃, and the reaction time is 1h to obtain the antibacterial agent;
s11: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, one strand of warps and two strands of wefts with the arrangement ratio of 2:1 are interwoven to form the polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent, wherein the temperature is 80 ℃, the reaction time is 5 hours, and after the reaction is finished, performing pre-setting treatment on the fabric at 110 ℃ by using an open-width setting machine, dehydrating and drying to obtain the antibacterial composite fabric.
Comparative example 1:
s1: weighing 35 parts of acrylamide, 2 parts of potassium persulfate and 3 parts of lignin according to parts by weight;
s2, pouring acrylamide, potassium persulfate and lignin into a ball mill at the rotation speed of 700r/min and the temperature of 60 ℃ for reaction for 0.7h to obtain modified polyacrylamide;
s3: weighing 3 parts of modified polyacrylamide prepared by S2, 5-10 parts of sodium alkyl benzene sulfonate and 25 parts of purified water in parts by weight, and pouring the 3 parts into an emulsifying machine together, wherein the rotating speed of the emulsifying machine is 1500r/min, the temperature is 60 ℃, and the reaction time is 0.7h to obtain the antibacterial agent;
s4: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, one strand of warps and two strands of wefts with the arrangement ratio of 2:1 are interwoven to form the polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent at the temperature of 70 ℃, reacting for 2 hours, and after the reaction is finished, performing pre-setting treatment on the fabric at the temperature of 110 ℃ by using an open-width setting machine, dehydrating and drying to obtain the antibacterial composite fabric.
Comparative example 2:
s1, weighing 2 parts of 5-tert-butyl isophthalic acid, 30 parts of N, N-dimethylacetamide, 3 parts of hydrated copper acetate, 30 parts of methanol, 1.3 parts of leucine, 1.3 parts of PAA, 5 parts of magnesium borate, 0.7 part of manganese dioxide and 0.7 part of ferric oxide according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving the N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing the solution A and the solution B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in the S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate, manganese dioxide and leucine, and pouring into an emulsifying machine at the rotating speed of 2000r/min and the temperature of 80 ℃ for reaction for 1h to obtain a solution E;
s5, pouring iron oxide into the solution E in an emulsifying machine, wherein the rotating speed of the emulsifying machine is 2000r/min, the temperature is 70 ℃, and the reaction time is 1.2h to obtain a solution F;
s6, adding methanol into the F solution, standing at the reaction temperature of 30 ℃ to obtain modified MOF containing impurities;
s7: purifying the modified MOF containing impurities obtained from S6 to obtain the modified MOF;
s8: weighing 3 parts of modified MOF prepared by S7, 5-10 parts of sodium alkyl benzene sulfonate and 25 parts of purified water in parts by weight, and pouring 3 of the modified MOF, the sodium alkyl benzene sulfonate and the purified water into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 1500r/min, the temperature is 60 ℃, and the reaction time is 0.7h to obtain the antibacterial agent;
s9: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, one strand of warps and two strands of wefts with the arrangement ratio of 2:1 are interwoven to form the polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent, controlling the temperature to be 70 ℃, reacting for 2 hours, and after the reaction is finished, performing pre-setting treatment on the fabric at 110 ℃ by using an open-width setting machine, dehydrating and drying to obtain the antibacterial composite fabric.
Comparative example 3:
s1, weighing 2 parts of 5-tert-butyl isophthalic acid, 30 parts of N, N-dimethylacetamide, 3 parts of hydrated copper acetate, 30 parts of methanol, 1.3 parts of PAA, 5 parts of magnesium borate, 0.7 part of manganese dioxide and 0.7 part of ferric oxide according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving the N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing the solution A and the solution B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in the S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate and manganese dioxide, and pouring the mixture into an emulsifying machine at the rotating speed of 2000r/min and the temperature of 80 ℃ for 1h to obtain a solution E;
s5, pouring iron oxide into the solution E in an emulsifying machine, wherein the rotating speed of the emulsifying machine is 2000r/min, the temperature is 70 ℃, and the reaction time is 1.2h to obtain a solution F;
s6, adding methanol into the F solution, standing at the reaction temperature of 30 ℃ to obtain modified MOF containing impurities;
s7: purifying the modified MOF containing impurities obtained from S6 to obtain the modified MOF;
s8: weighing 35 parts of acrylamide, 2 parts of potassium persulfate and 3 parts of lignin according to parts by weight;
s9, pouring acrylamide, potassium persulfate and lignin into a ball mill, wherein the rotating speed of the ball mill is 700r/min, the temperature is 60 ℃, and the reaction time is 0.7h to obtain modified polyacrylamide;
s10: weighing 3 parts of modified MOF prepared by S7, 3 parts of modified polyacrylamide prepared by S9, 8 parts of sodium alkyl benzene sulfonate and 25 parts of purified water in parts by weight, and pouring the 4 parts of the modified MOF, the sodium alkyl benzene sulfonate and the purified water into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 1500r/min, the temperature is 60 ℃, and the reaction time is 0.7h to obtain the antibacterial agent;
s11: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, and one warp and two surface wefts and two inner wefts in the arrangement ratio of 2:1 are interwoven to form a polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent, controlling the temperature to be 70 ℃, reacting for 2 hours, and after the reaction is finished, performing pre-setting treatment on the fabric at 110 ℃ by using an open-width setting machine, dehydrating and drying to obtain the antibacterial composite fabric.
Comparative example 4:
s1, weighing 2 parts of 5-tert-butyl isophthalic acid, 30 parts of N, N-dimethylacetamide, 3 parts of hydrated copper acetate, 30 parts of methanol, 1.3 parts of tryptophan, 1.3 parts of PAA, 5 parts of magnesium borate, 0.7 part of manganese dioxide and 0.7 part of ferric oxide according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing A and B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in the S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate, manganese dioxide and tryptophan, and pouring the mixture into an emulsifying machine at the rotating speed of 2000r/min and the temperature of 80 ℃ for 1h to obtain a solution E;
s5, pouring iron oxide into the solution E in an emulsifying machine, wherein the rotating speed of the emulsifying machine is 2000r/min, the temperature is 70 ℃, and the reaction time is 1.2h to obtain a solution F;
s6, adding methanol into the F solution, standing at the reaction temperature of 30 ℃ to obtain modified MOF containing impurities;
s7: purifying the modified MOF containing impurities obtained in the step S6 to obtain modified MOF;
s8: weighing 35 parts of acrylamide, 2 parts of potassium persulfate and 3 parts of lignin according to parts by weight;
s9, pouring acrylamide, potassium persulfate and lignin into a ball mill, wherein the rotating speed of the ball mill is 700r/min, the temperature is 60 ℃, and the reaction time is 0.7h to obtain modified polyacrylamide;
s10: weighing 3 parts of modified MOF prepared by S7, 3 parts of modified polyacrylamide prepared by S9, 8 parts of sodium alkyl benzene sulfonate and 25 parts of purified water in parts by weight, and pouring the 4 parts of the modified MOF, the sodium alkyl benzene sulfonate and the purified water into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 1500r/min, the temperature is 60 ℃, and the reaction time is 0.7h to obtain the antibacterial agent;
s11: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, one strand of warps and two strands of wefts with the arrangement ratio of 2:1 are interwoven to form the polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent, controlling the temperature to be 70 ℃, reacting for 2 hours, and after the reaction is finished, performing pre-setting treatment on the fabric at 110 ℃ by using an open-width setting machine, dehydrating and drying to obtain the antibacterial composite fabric.
Comparative example 5:
s1, weighing 2 parts of 5-tert-butyl isophthalic acid, 30 parts of N, N-dimethylacetamide, 3 parts of hydrated copper acetate, 30 parts of methanol, 1.3 parts of leucine, 1.3 parts of PAA, 0.7 part of manganese dioxide and 0.7 part of ferric oxide according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving the N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing the solution A and the solution B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in the S2 to obtain a D solution;
s4, uniformly mixing the solution D, manganese dioxide and leucine, and pouring the mixture into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 2000r/min, the temperature is 80 ℃, and the reaction time is 1h to obtain a solution E;
s5, pouring iron oxide into the solution E in an emulsifying machine, wherein the rotating speed of the emulsifying machine is 2000r/min, the temperature is 70 ℃, and the reaction time is 1.2h to obtain a solution F;
s6, adding methanol into the F solution, standing at the reaction temperature of 30 ℃ to obtain modified MOF containing impurities;
s7: purifying the modified MOF containing impurities obtained in the step S6 to obtain modified MOF;
s8: weighing 35 parts of acrylamide, 2 parts of potassium persulfate and 3 parts of lignin according to parts by weight;
s9, pouring acrylamide, potassium persulfate and lignin into a ball mill, wherein the rotating speed of the ball mill is 700r/min, the temperature is 60 ℃, and the reaction time is 0.7h to obtain modified polyacrylamide;
s10: weighing 3 parts of modified MOF prepared by S7, 3 parts of modified polyacrylamide prepared by S9, 8 parts of sodium alkyl benzene sulfonate and 25 parts of purified water in parts by weight, and pouring the 4 parts of modified MOF, sodium alkyl benzene sulfonate and purified water into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 1500r/min, the temperature is 60 ℃, and the reaction time is 0.7h, so as to obtain the antibacterial agent;
s11: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, and one warp and two surface wefts and two inner wefts in the arrangement ratio of 2:1 are interwoven to form a polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent, wherein the temperature is 70 ℃, the reaction time is not less than 2 hours, and after the reaction is finished, performing pre-setting treatment on the fabric at 110 ℃ by using an open-width setting machine, dehydrating and drying to obtain the antibacterial composite fabric.
Comparative example 6:
s1, weighing 2 parts of 5-tert-butyl isophthalic acid, 30 parts of N, N-dimethylacetamide, 3 parts of hydrated copper acetate, 30 parts of methanol, 1.3 parts of leucine, 1.3 parts of PAA and 5 parts of magnesium borate according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving the N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing the solution A and the solution B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in the S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate and leucine, and pouring the mixture into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 2000r/min, the temperature is 80 ℃, and the reaction time is 1h to obtain a solution E;
s5, adding methanol into the solution E, standing at the reaction temperature of 30 ℃ to obtain modified MOF containing impurities;
s6: purifying the modified MOF containing impurities obtained in the step S6 to obtain modified MOF;
s7: weighing 35 parts of acrylamide, 2 parts of potassium persulfate and 3 parts of lignin according to parts by weight;
s8, pouring acrylamide, potassium persulfate and lignin into a ball mill, wherein the rotating speed of the ball mill is 700r/min, the temperature is 60 ℃, and the reaction time is 0.7h to obtain modified polyacrylamide;
s9: weighing 3 parts of modified MOF prepared by S6, 3 parts of modified polyacrylamide prepared by S8, 8 parts of sodium alkyl benzene sulfonate and 25 parts of purified water in parts by weight, and pouring the 4 parts of modified MOF, sodium alkyl benzene sulfonate and purified water into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 1500r/min, the temperature is 60 ℃, and the reaction time is 0.7h, so as to obtain the antibacterial agent;
s10: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, one strand of warps and two strands of wefts with the arrangement ratio of 2:1 are interwoven to form the polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent, wherein the temperature is 70 ℃, the reaction time is not less than 2 hours, and after the reaction is finished, performing pre-setting treatment on the fabric at 110 ℃ by using an open-width setting machine, dehydrating and drying to obtain the antibacterial composite fabric.
Comparative example 7:
s1, weighing 2 parts of 5-tert-butyl isophthalic acid, 30 parts of N, N-dimethylacetamide, 3 parts of hydrated copper acetate, 30 parts of methanol, 1.3 parts of leucine, 1.3 parts of PAA, 5 parts of magnesium borate, 0.7 part of manganese dioxide and 0.7 part of ferric oxide according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving the N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing the solution A and the solution B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in the S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate, manganese dioxide and leucine, and pouring the mixture into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 2000r/min, the temperature is 80 ℃, and the reaction time is 1h to obtain a solution E;
s5, pouring iron oxide into the solution E in an emulsifying machine, wherein the rotating speed of the emulsifying machine is 2000r/min, the temperature is 70 ℃, and the reaction time is 1.2h to obtain a solution F;
s6, adding methanol into the F solution, standing at the reaction temperature of 30 ℃ to obtain modified MOF containing impurities;
s7: purifying the modified MOF containing impurities obtained in the step S6 to obtain modified MOF;
s8: weighing 35 parts of acrylamide, 2 parts of potassium persulfate and 3 parts of lignin according to parts by weight;
s9, pouring acrylamide and potassium persulfate into a ball mill at the rotating speed of 700r/min and the temperature of 60 ℃ for 0.7h to obtain modified polyacrylamide;
s10: weighing 3 parts of modified MOF prepared by S7, 3 parts of modified polyacrylamide prepared by S9, 8 parts of sodium alkyl benzene sulfonate and 25 parts of purified water in parts by weight, and pouring the 4 parts of the modified MOF, the sodium alkyl benzene sulfonate and the purified water into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 1500r/min, the temperature is 60 ℃, and the reaction time is 0.7h to obtain the antibacterial agent;
s11: polyurethane fibers are used as warps, the length of the polyurethane fibers is 35mm, the linear density is 1.6dtex, cotton fibers are used as wefts, the length of the cotton is 35mm, and the linear density is 1.40dtex, one strand of warps and two strands of wefts with the arrangement ratio of 2:1 are interwoven to form the polyurethane and cotton composite primary fabric; and (3) immersing the primary fabric into an antibacterial agent, wherein the temperature is 70 ℃, the reaction time is not less than 2 hours, and after the reaction is finished, performing pre-setting treatment on the fabric at 110 ℃ by using an open-width setting machine, dehydrating and drying to obtain the antibacterial composite fabric.
Examples 1 to 3 and comparative examples 1 to 7 were examined according to the following examination methods, and the results are shown in tables 1 to 3.
Breaking strength: the tests were carried out according to standard GB/T3923.1-1997
Puncture resistance tested according to standard GB/T20655
Tear Strength tested according to the Standard GB/T3917.3
Wear resistance times tested according to the standard GB/T21196.2-2007
Hydrostatic pressure resistance, tested according to the standard GB/T4744-1997
And (3) antibacterial light stability, namely treating for 72 hours under ultraviolet light, and detecting the antibacterial property according to a conventional method.
And (3) antibacterial property high-temperature stability, namely treating the fabric at 60 ℃ for 72h, and detecting the antibacterial property according to a conventional method.
And (3) stability of antibacterial saline water, namely soaking the fabric in 0.5% saline water at 30 ℃ for 72h, and detecting the antibacterial property according to a conventional method.
For the experimental reference GB/T19344-.
Before experiment, each strain is inoculated into nutrient agar culture medium, cultured for 1d at 37 ℃, prepared into bacterial suspension (1X 108CFU/mL) with certain concentration by using sterilized normal saline, and placed at 4 ℃ for standby.
And (3) putting the antibacterial polyurethane composite fabric sample to be detected into a triangular flask with a plug containing sterile physiological saline, adding bacterial suspension, oscillating for 1h under a certain condition, pouring 1ml of test solution into a flat plate for colony counting, comparing with a blank sample, and calculating the antibacterial rate.
The bacteriostasis rate is [ (C)0-C1)/C0]×100％
In the formula C0The number of colonies of the control sample which is not subjected to antibacterial finishing is counted; c1The colony number of the antibacterial finishing sample is shown.
TABLE 1 test results
Figure BDA0003578505290000111
Figure BDA0003578505290000121
TABLE 2 test results
Figure BDA0003578505290000122
TABLE 2 test results
Figure BDA0003578505290000131
According to the detection results of the examples 1-3 and the comparative example 1, the modified MOF in the antibacterial composite fabric can improve the breaking strength and the tearing strength of the fabric on the premise of ensuring the wear-resisting times, the hydrostatic pressure resistance and the puncture resistance of the fabric, has a very obvious effect on the antibacterial performance of the fabric, particularly obviously improves the antibacterial performance of the fabric after high-temperature treatment, light treatment and saline water treatment, and in addition, ensures the high hydrophobicity of the fabric by using the modified MOF.
The detection results of the examples 1-3 and the comparative example 2 show that the antibacterial property of the fabric subjected to light treatment is obviously reduced when the modified polyacrylamide is not used, which indicates that the modified polyacrylamide also has a certain effect on the antibacterial property of the composite fabric, and particularly the antibacterial effect of the fabric subjected to light treatment is obvious after the modified polyacrylamide and the modified MOF are simultaneously used.
According to the detection results of the examples 1-3 and the comparative examples 3 and 4, the fabric has no hydrophobic function when no leucine is used in the modified MOF, and the antibacterial stability of the fabric after light treatment and saline treatment is reduced after the leucine is replaced by the tryptophan in the example 4, which shows that the leucine not only plays a role in hydrophobic but also plays a role in improving the antibacterial stability.
From the test results of examples 1-3 and comparative example 5, it can be seen that the antibacterial property and stability of the fabric are reduced when the modified MOF does not use magnesium borate, indicating that the magnesium borate in the modified MOF plays a role in antibacterial property and stability thereof.
As can be seen from the results of the tests of examples 1 to 3 and comparative examples 1 and 6, the antibacterial properties and the stability of comparative examples 1 and 6 are substantially the same, which shows that the use of manganese dioxide and iron oxide together successfully modifies MOF and exerts its antibacterial properties, hydrophobicity, breaking strength and tearing strength.
The detection results of the examples 1-3 and the comparative example 7 show that the antibacterial property of the fabric is reduced by about 10% after no lignin exists, which indicates that the antibacterial property of the fabric is also improved by using the lignin-modified polyacrylamide.

Claims (10)

1. An antibacterial composite fabric comprises an antibacterial agent and the composite fabric, and is characterized in that the antibacterial agent is prepared from the following raw materials:
Figure FDA0003578505280000011
2. the antibacterial composite fabric according to claim 1, wherein the modified MOF is prepared from the following raw materials:
Figure FDA0003578505280000012
3. the antibacterial composite fabric according to claim 1, wherein the preparation of the modified MOF comprises the following steps:
s1, weighing 5-tert-butyl isophthalic acid, N-dimethylacetamide, copper acetate, methanol, PAA, magnesium borate, manganese dioxide and ferric oxide according to parts by weight;
s2, dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing A and B to obtain a solution C;
s3, dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared in S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate, manganese dioxide and leucine, pouring the mixture into an emulsifying machine, and setting reaction conditions to obtain a solution E;
s5, pouring iron oxide into the solution E in the emulsifying machine, and setting reaction conditions to obtain a solution F;
s6, adding methanol into the F solution, and setting reaction conditions to obtain modified MOF containing impurities;
s7: and (5) purifying the modified MOF containing the impurities obtained in the step S6 to obtain the modified MOF.
4. The antibacterial composite fabric according to claim 3,
the reaction conditions in the steps S4 and S5 are that the rotation speed of an emulsifying machine is 500-5000r/min, the temperature is 50-100 ℃, and the reaction time is 0.1-2 h;
the reaction conditions in the step S6 are that the reaction temperature is 15-50 ℃, and the mixture is kept stand.
5. The antibacterial composite fabric according to claim 1, wherein the modified acrylamide is prepared from the following raw materials:
20-50 parts of acrylamide;
0.5-3 parts of potassium persulfate;
1-15 parts of lignin.
6. The antibacterial composite fabric according to claim 5, wherein the preparation of the modified polyacrylamide comprises the following steps:
s1, weighing acrylamide, potassium persulfate and lignin in parts by weight;
and S2, pouring acrylamide, potassium persulfate and lignin into a ball mill, and setting reaction conditions to obtain the modified polyacrylamide.
7. The antibacterial composite fabric as claimed in claim 6, wherein the reaction conditions in step S2 are that the rotation speed of the ball mill is 500-1000r/min, the temperature is 40-100 ℃, and the reaction time is 0.2-1 h.
8. The antibacterial composite fabric according to claim 1, wherein the preparation method of the antibacterial agent comprises the following steps,
s1: weighing modified MOF, modified polyacrylamide, sodium alkyl benzene sulfonate and purified water according to parts by weight;
s2: and (3) pouring the modified MOF, the modified polyacrylamide, the sodium alkyl benzene sulfonate and the purified water which are weighed in the S1 into an emulsifying machine, wherein the rotating speed of the emulsifying machine is 1000-2000r/min, the temperature is 40-100 ℃, and the reaction time is 0.2-1h to obtain the antibacterial agent.
9. A preparation method of an antibacterial composite fabric is characterized by comprising the following steps,
s1: weighing 5-tert-butyl isophthalic acid, N-dimethylacetamide, copper acetate, methanol, PAA, magnesium borate, manganese dioxide and ferric oxide according to parts by weight;
s2: dissolving 5-tert-butyl isophthalic acid in N, N-dimethylacetamide to obtain a solution A, dissolving the N, N-dimethylacetamide with copper acetate hydrate to obtain a solution B, and uniformly mixing the solution A and the solution B to obtain a solution C;
s3: dissolving PAA in ethanol, and adding the dissolved PAA solution into the C solution prepared by S2 to obtain a D solution;
s4, uniformly mixing the solution D, magnesium borate, manganese dioxide and leucine, pouring the mixture into an emulsifying machine, and setting reaction conditions to obtain a solution E;
s5, pouring ferric oxide into the solution E in the emulsifying machine, and setting reaction conditions to obtain a solution F;
s6, adding methanol into the F solution, and setting reaction conditions to obtain modified MOF containing impurities;
s7: purifying the modified MOF containing impurities obtained in the step S6 to obtain modified MOF;
s8: weighing acrylamide, potassium persulfate and lignin according to parts by weight;
s9, pouring acrylamide, potassium persulfate and lignin into a ball mill, and setting reaction conditions to obtain modified polyacrylamide;
s10: weighing the modified MOF prepared by S7, the modified polyacrylamide prepared by S9, sodium alkyl benzene sulfonate and purified water in parts by weight, pouring 4 of the materials into an emulsifying machine, and setting reaction conditions to obtain the antibacterial agent;
s11: and (3) putting the polyurethane and cotton yarn composite fabric into an antibacterial agent, and setting reaction conditions to obtain the antibacterial composite fabric.
10. The method for preparing the antibacterial composite fabric according to claim 9,
the reaction conditions in steps S4 and S5 are both: the rotation speed of the emulsifying machine is 500-5000r/min, the temperature is 50-100 ℃, and the reaction time is 0.1-2 h;
the reaction conditions in step S6 are: the reaction temperature is 15-50 ℃, and standing is carried out;
the reaction conditions in step S9 are: the rotation speed of the ball mill is 500-1000r/min, the temperature is 40-100 ℃, and the reaction time is 0.2-1 h;
the reaction conditions in step S10 are: the rotation speed of the emulsifying machine is 1000-2000r/min, the temperature is 40-100 ℃, and the reaction time is 0.2-1 h;
the reaction conditions in step S11 are: the temperature is 60-80 ℃, and the reaction time is not less than 1 h.
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