CN118910893B - Nylon fabric and preparation method thereof - Google Patents

Nylon fabric and preparation method thereof Download PDF

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CN118910893B
CN118910893B CN202411409354.1A CN202411409354A CN118910893B CN 118910893 B CN118910893 B CN 118910893B CN 202411409354 A CN202411409354 A CN 202411409354A CN 118910893 B CN118910893 B CN 118910893B
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nylon fabric
nylon
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producing
fabric
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CN118910893A (en
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陈玉平
许磊
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Wujiang Lantian Textile Co ltd
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Wujiang Lantian Textile Co ltd
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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
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/65Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups
    • D06M15/652Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups comprising amino groups
    • 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
    • D06M11/73Treating 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 carbon or compounds thereof
    • D06M11/76Treating 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 carbon or compounds thereof with carbon oxides or carbonates
    • 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
    • D06M13/10Treating 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 oxygen
    • D06M13/144Alcohols; Metal alcoholates
    • D06M13/148Polyalcohols, e.g. glycerol or glucose
    • 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
    • D06M13/10Treating 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 oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/192Polycarboxylic acids; Anhydrides, halides or salts 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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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 oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts 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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating 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
    • D06M13/248Treating 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
    • D06M13/262Sulfated compounds thiosulfates
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    • 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
    • D06M13/244Treating 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
    • D06M13/282Treating 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 phosphorus
    • 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
    • D06M13/44Treating 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 containing nitrogen and phosphorus
    • D06M13/453Phosphates or phosphites containing nitrogen atoms
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    • 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
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34Polyamides
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    • 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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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
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Abstract

The invention belongs to the technical field of textile, and particularly relates to a nylon fabric and a preparation method thereof. According to the invention, the gamma-glycidol ether oxypropyl trimethoxy silane and aminopropyl triethoxy silane are polymerized on the surface of the nylon fabric in an emulsion polymerization mode to form the organic silicon flame retardant, and the flame retardant forms an oxygen insulation protection layer on the surface of the nylon fabric during combustion, so that the nylon fabric is effectively prevented from continuing to burn, and a good flame retardant effect is achieved. The limiting oxygen index of the nylon fabric provided by the invention can reach 29.4+/-0.1%, the weight gain rate can reach 18.24%, and the nylon fabric does not have molten drops and drops during combustion, and has a good flame retardant effect.

Description

Nylon fabric and preparation method thereof
Technical Field
The invention belongs to the technical field of textile, and particularly relates to a nylon fabric and a preparation method thereof.
Background
The nylon fiber is thermoplastic resin with repeated amide groups on the molecular main chain, has the advantages of light weight, easy washing and quick drying, mildew and moth resistance, high strength, acid and alkali resistance and the like, and is widely applied to the textile field. With the improvement of living standard of people, the requirements on textiles are higher and higher. Nylon fiber is very easy to shrink in the burning process because the melting point is lower than the ignition point, and a large number of molten drops are generated, so that skin can be burnt, and potential safety hazards are caused. Therefore, improvement of the flame retardant property of nylon fabrics is not desirable.
The common nylon flame-retardant methods mainly comprise three methods of blending flame retardants and finishing. The after-finishing method has the advantages of simple process and easy operation, but no active group in the nylon fiber structure, radiation, grafting of the functional group with the flame retardant function to the surface of the nylon fiber after the activation of the fabric, higher production cost, limited selectable monomers and difficult realization of large-scale production.
The Chinese patent application document with publication number of CN103866563A discloses a flame-retardant grafting modification method for nylon 66 fabric, adopts a microwave method to carry out grafting reaction, adopts allylthiourea as grafting monomer, obviously improves the combustion performance of the grafted nylon 66 fabric, and modifies the nylon 66 fabric by microwave irradiation. The Chinese patent application publication No. CN116200027A discloses a flame-retardant nylon and a preparation method thereof, wherein the flame-retardant nylon comprises nylon, a phosphorus-nitrogen-silicon cross-linked polymer, wherein the phosphorus-nitrogen-silicon cross-linked polymer is a reaction product of a phosphorus-nitrogen-containing diacid monomer and a silicon-containing epoxy monomer under the action of a catalyst, and comprises a beta-hydroxyl ester bond formed by transesterification of epoxy groups and carboxyl groups, and a product of melt mixing reaction of the phosphorus-nitrogen-silicon cross-linked polymer and the nylon part, wherein the product comprises an exchange product of the beta-hydroxyl ester bond and an amide bond in the nylon, and a chain extension product of amino groups and carboxyl groups in the nylon, and hydroxyl groups and epoxy groups in the phosphorus-nitrogen-silicon cross-linked polymer.
Disclosure of Invention
The invention aims to solve the technical problems of dripping, poor flame retardant effect, high production cost and the like in the related art, and provides a nylon fabric and a preparation method thereof.
In order to achieve the above object, the present invention has the following technical scheme:
the preparation method of the nylon fabric comprises the following steps:
S1, soaking a nylon fabric in a sodium carbonate solution, heating to boiling, boiling for 1-2 hours, cooling, taking out the nylon fabric, and cleaning with clear water to obtain a pretreated nylon fabric;
S2, immersing the pretreated nylon fabric prepared in the step S1 in glycol aqueous solution, adding tartaric acid, stirring for 0.5-1h under the condition of the rotating speed of 1200-1400rpm, taking out the nylon fabric, drying, washing with clear water to be neutral, and airing at room temperature to obtain a modified nylon fabric I;
s3, immersing the modified nylon fabric I prepared in the step S2 in an ethanol mixed solution of p-hydroxybenzoic acid and phosphoric acid ester amide, heating to 50-60 ℃ for 1-1.5h, taking out the nylon fabric, and washing with clear water to obtain a modified nylon fabric II;
S4, soaking the modified nylon fabric II obtained in the step S3 in an aqueous solution of tetramethyl phosphorus hydroxide and sodium dodecyl sulfate, heating to 40-50 ℃, dropwise adding a mixture of gamma-glycidol ether oxypropyl trimethoxy silane and aminopropyl triethoxy silane, stirring for 3.5-4 hours, taking out the nylon fabric, washing with clear water, and drying to obtain the modified nylon fabric II.
The heating and boiling process of the nylon fabric in the alkaline solution can change the macromolecular chain end group of the nylon fiber fabric into a reducing end group, thereby creating conditions for the subsequent reaction. The nylon fabric is subjected to carboxymethylation modification by adopting glycol and tartaric acid, and carboxyl is introduced to a macromolecular chain of the nylon fiber, so that a foundation is laid for the connection of a subsequent flame retardant.
According to the invention, the carboxymethyl modified nylon fabric is impregnated with the ethanol solution of the parahydroxybenzoic acid and the phosphoric acid ester amide, and the hydroxyl group in the parahydroxybenzoic acid and the amino group in the phosphoric acid ester amide react with the carboxyl group on the molecular surface of the carboxymethyl modified nylon fabric, so that the parahydroxybenzoic acid and the phosphoric acid ester amide are grafted on the surface of the nylon fabric, and the benzene ring and the organic phosphorus are introduced, so that the flame retardant property of the nylon fabric is greatly improved.
The invention adopts an emulsion polymerization mode to polymerize gamma-glycidol ether oxypropyl trimethoxy silane and aminopropyl triethoxy silane on the surface of nylon fabric to form the organosilicon flame retardant. The molecular main chain of the flame retardant contains a large number of silica bonds, when the nylon fabric burns, a layer of silica bonds and/or silica carbon bonds with excellent thermal stability and oxidation stability can be formed on the surface of the nylon fabric, an inorganic oxygen-insulating heat-insulating protective layer is formed, the burning is prevented, the thermal decomposition of nylon polymers is inhibited, and the branched chain structure of the flame retardant is favorable for forming a cross-linked structure in solid phase residues, so that the thermal stability of the nylon fabric is improved. In addition, the amino group contained in the polymer molecule formed by the gamma-glycidol ether oxypropyl trimethoxy silane and the aminopropyl triethoxy silane can also react with the carboxyl group on the modified nylon fabric molecule, so that the binding force between the flame retardant and the nylon molecule is further enhanced, and the flame retardant performance of the nylon fabric is improved.
Further, the concentration of the sodium carbonate solution in the step S1 of the preparation method of the nylon fabric is 0.06-0.08mol/L, and the pH value is 8.5-9.
Further, in the step S2 of the preparation method of the nylon fabric, the mass percentage of the ethylene glycol is 20-25%.
Further, the amount of tartaric acid in the step S2 of the preparation method of the nylon fabric is 15-17% of the mass of the nylon fabric.
Further, the dipping temperature in the step S2 of the preparation method of the nylon fabric is 75-80 ℃.
Further, in the step S3 of the preparation method of the nylon fabric, the concentration of the parahydroxybenzoic acid is 0.5-0.7mol/L, and the concentration of the phosphoric acid ester amide is 0.15-0.2mol/L.
Further, in the step S4 of the preparation method of the nylon fabric, the concentration of the tetramethyl phosphorus hydroxide is 0.02-0.03mol/L, and the concentration of the sodium dodecyl sulfate is 0.03-0.04mol/L.
Further, in the step S4 of the preparation method of the nylon fabric, the dripping speed of the mixture of the gamma-glycidol ether oxypropyl trimethoxysilane and the aminopropyl triethoxysilane is 2.2-2.6m 3/h.
Further, in the step S4 of the preparation method of the nylon fabric, the mixing mass ratio of the gamma-glycidol ether oxypropyl trimethoxysilane to the aminopropyl triethoxysilane is 2-5:9-13.
The invention also provides a nylon fabric prepared by the preparation method of the nylon fabric.
Compared with the prior art, the nylon fabric and the preparation method thereof have the following technical advantages:
(1) The limiting oxygen index of the nylon fabric provided by the invention can reach 29.4+/-0.1%, the weight gain rate can reach 18.24%, and the nylon fabric does not have molten drops and drops during combustion, and has a good flame retardant effect;
(2) According to the invention, the flame retardant molecules are grafted to the molecular structure of the nylon fabric through emulsion polymerization, and when the flame retardant is burnt, an oxygen-insulating heat-insulating protective layer is formed on the surface of the nylon fabric, so that the nylon fabric is effectively prevented from continuing burning;
(3) The nylon fabric provided by the invention can be grafted with flame retardant molecules without radiation, so that the production cost is effectively reduced, and the realization of large-scale production is facilitated.
Drawings
FIG. 1 is a graph of the heat release rate of nylon fabric;
FIG. 2 is a graph of heat of combustion for nylon fabric;
FIG. 3 is a molecular structural formula of a phosphoric acid ester amide.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples. Various modifications may be made by those skilled in the art in light of the basic idea of the invention, but are within the scope of the invention without departing from the basic idea of the invention.
The phosphoric acid ester amide used in this embodiment is purchased from Changzhou fast metallocene chemical Co., ltd, and has a molecular structural formula shown in FIG. 3.
Example 1, method for producing Nylon Fabric
The preparation method of the nylon fabric comprises the following steps:
s1, soaking a nylon fabric in a sodium carbonate solution with the concentration of 0.06mol/L, pH and the value of 9, heating to boiling, boiling for 1h, cooling, taking out the nylon fabric, and cleaning with clear water to obtain a pretreated nylon fabric;
s2, immersing the pretreated nylon fabric prepared in the step S1 in an ethylene glycol aqueous solution with the mass percentage of 20% at the temperature of 75 ℃, adding tartaric acid, stirring at 1200rpm for 1h, taking out the nylon fabric, drying, washing with clear water to be neutral, and airing at room temperature to obtain a modified nylon fabric I;
S3, immersing the modified nylon fabric I prepared in the step S2 in an ethanol mixed solution of parahydroxybenzoic acid and phosphoric acid ester amide, wherein the concentration of parahydroxybenzoic acid is 0.5mol/L, the concentration of phosphoric acid ester amide is 0.15mol/L, heating to 50 ℃, immersing for 1h, taking out the nylon fabric, and washing with clear water to obtain a modified nylon fabric II;
S4, soaking the modified nylon fabric II prepared in the step 3 in an aqueous solution of tetramethyl phosphorus hydroxide and sodium dodecyl sulfate, wherein the concentration of the tetramethyl phosphorus hydroxide is 0.02mol/L, the concentration of the sodium dodecyl sulfate is 0.04mol/L, heating to 40 ℃, dropwise adding a mixture of gamma-glycidoxypropyl trimethoxysilane and aminopropyl triethoxysilane at the speed of 2.2m 3/h, mixing the gamma-glycidoxypropyl trimethoxysilane and the aminopropyl triethoxysilane at the mass ratio of 2:9, stirring for 3.5h, taking out the nylon fabric, washing with clear water, and drying to obtain the nylon fabric.
Example 2 preparation method of Nylon Fabric
The preparation method of the nylon fabric comprises the following steps:
S1, soaking a nylon fabric in a sodium carbonate solution with the concentration of 0.08mol/L, pH and the value of 8.5, heating to boiling, boiling for 2 hours, cooling, taking out the nylon fabric, and cleaning with clear water to obtain a pretreated nylon fabric;
S2, immersing the pretreated nylon fabric prepared in the step S1 in an ethylene glycol aqueous solution with the mass percentage of 25% at 80 ℃, adding tartaric acid, stirring at 1400rpm for 0.5h, taking out the nylon fabric, drying, washing with clear water to be neutral, and airing at room temperature to obtain a modified nylon fabric I;
S3, immersing the modified nylon fabric I prepared in the step S2 in an ethanol mixed solution of parahydroxybenzoic acid and phosphoric acid ester amide, wherein the concentration of parahydroxybenzoic acid is 0.7mol/L, the concentration of phosphoric acid ester amide is 0.2mol/L, heating to 60 ℃, immersing for 1.5 hours, taking out the nylon fabric, and washing with clear water to obtain a modified nylon fabric II;
S4, soaking the modified nylon fabric II prepared in the step 3 in an aqueous solution of tetramethyl phosphorus hydroxide and sodium dodecyl sulfate, wherein the concentration of tetramethyl phosphorus hydroxide is 0.03mol/L, the concentration of sodium dodecyl sulfate is 0.03mol/L, heating to 50 ℃, dropwise adding a mixture of gamma-glycidoxypropyl trimethoxysilane and aminopropyl triethoxysilane at the speed of 2.6m 3/h, mixing the gamma-glycidoxypropyl trimethoxysilane and the aminopropyl triethoxysilane at the mass ratio of 5:13, stirring for 4h, taking out the nylon fabric, washing with clear water, and drying to obtain the nylon fabric.
Example 3 preparation method of Nylon Fabric
The preparation method of the nylon fabric comprises the following steps:
s1, soaking a nylon fabric in a sodium carbonate solution with the concentration of 0.07mol/L, pH and the value of 8.8, heating to boiling, boiling for 1.5 hours, cooling, taking out the nylon fabric, and cleaning with clear water to obtain a pretreated nylon fabric;
S2, immersing the pretreated nylon fabric prepared in the step S1 in an ethylene glycol aqueous solution with the mass percentage of 23% at 79 ℃, adding tartaric acid, stirring at 1300rpm for 0.8h, taking out the nylon fabric, drying, washing with clear water to be neutral, and airing at room temperature to obtain a modified nylon fabric I;
s3, immersing the modified nylon fabric I prepared in the step S2 in an ethanol mixed solution of parahydroxybenzoic acid and phosphoric acid ester amide, wherein the concentration of parahydroxybenzoic acid is 0.6mol/L, the concentration of phosphoric acid ester amide is 0.18mol/L, heating to 57 ℃, immersing for 1.2 hours, taking out the nylon fabric, and washing with clear water to obtain a modified nylon fabric II;
S4, soaking the modified nylon fabric II prepared in the step3 in an aqueous solution of tetramethyl phosphorus hydroxide and sodium dodecyl sulfate, wherein the concentration of tetramethyl phosphorus hydroxide is 0.027mol/L, the concentration of sodium dodecyl sulfate is 0.035mol/L, heating to 46 ℃, dropwise adding a mixture of gamma-glycidoxypropyl trimethoxysilane and aminopropyl triethoxysilane at the speed of 2.4m 3/h, mixing the gamma-glycidoxypropyl trimethoxysilane and aminopropyl triethoxysilane at the mass ratio of 4:11, stirring for 3.7h, taking out the nylon fabric, washing with clear water, and drying to obtain the nylon fabric.
Comparative example 1
The preparation method of the nylon fabric in the comparative example is similar to that of the example 3, and the step S4 in the comparative example is that the modified nylon fabric II prepared in the step S3 is soaked in an aqueous solution of tetramethyl phosphorus hydroxide and sodium dodecyl sulfate, the concentration of tetramethyl phosphorus hydroxide is 0.027mol/L, the concentration of sodium dodecyl sulfate is 0.035mol/L, the temperature is raised to 46 ℃, gamma-glycidol ether oxypropyl trimethoxy silane is dripped at the speed of 2.4m 3/h, the mixture is stirred for 3.7h, the nylon fabric is taken out, and the nylon fabric is cleaned and dried by clear water, thus obtaining the nylon fabric.
Namely, this comparative example is different from example 3 in that the same amount of gamma-glycidoxypropyl trimethoxysilane was used instead of aminopropyl triethoxysilane.
Comparative example 2
The preparation method of the nylon fabric in the comparative example is similar to that of the example 3, and the step S4 in the comparative example is specifically that the modified nylon fabric II prepared in the step S3 is soaked in an aqueous solution of tetramethyl phosphorus hydroxide and sodium dodecyl sulfate, the concentration of tetramethyl phosphorus hydroxide is 0.027mol/L, the concentration of sodium dodecyl sulfate is 0.035mol/L, the temperature is raised to 46 ℃, aminopropyl triethoxysilane is dropwise added at the speed of 2.4m 3/h, stirring is carried out for 3.7h, the nylon fabric is taken out, and the nylon fabric is cleaned with clear water and dried, thus obtaining the nylon fabric.
Namely, this comparative example is different from example 3 in that the same amount of aminopropyl triethoxysilane was used instead of γ -glycidoxypropyl trimethoxysilane.
Comparative example 3
The nylon fabric of this comparative example was prepared similarly to example 3, and the difference between this comparative example and example 3 was that the mixing mass ratio of gamma-glycidoxypropyl trimethoxysilane and aminopropyl triethoxysilane in step S4 of this comparative example was 11:4.
Comparative example 4
The nylon fabric of this comparative example was prepared similarly to example 3, and was distinguished from example 3 in that the mixture of gamma-glycidoxypropyl trimethoxysilane and aminopropyl triethoxysilane of step S4 of this comparative example had a dropping speed of 3.9m 3/h.
Comparative example 5
The method for producing the nylon fabric described in this comparative example is similar to example 3, and this comparative example differs from example 3 in that the nylon fabric is not subjected to carboxylation modification, i.e., the method for producing the nylon fabric in this comparative example is not subjected to the operation in step S2.
Test example I, combustion Performance test
Test samples were nylon fabrics prepared in examples 1 to 3 and comparative examples 1 to 5, and blank samples were made using a nylon fabric base fabric.
Test method according to GB/T5454-2008 "oxygen index method for textile Combustion Performance test", the Limiting Oxygen Index (LOI) of the fabric is measured by adopting an FT0002 type oxygen index measuring instrument.
Weight gain ratio the sample before and after combustion test is dried in an oven at 100 deg.C for 2h, dried in a drier, the weight of the sample is measured after the weight of the sample is balanced, and the weight gain ratio is calculated, wherein the weight gain ratio= (m 1-m0)/m0 x 100), m 0 is the weight of the sample before test, and m 1 is the weight of the sample after test.
Test results the limiting oxygen index and the weight gain are shown in Table 1.
TABLE 1 limiting oxygen index and weight gain Rate test results
As shown in Table1, the limiting oxygen index of the nylon fabric provided by the invention can reach 29.4+/-0.1%, the weight gain rate can reach 18.24%, and compared with a blank control group, the nylon fabric has obvious improvement, does not have molten drops during combustion, and has good flame retardant effect. The nylon fabric prepared in example 3 has the best limiting oxygen index and weight gain rate, and is the best example of the invention.
Compared with the example 3, the step S4 of the comparative example 1 is not added with aminopropyl triethoxysilane, the step S4 of the comparative example 2 is not added with gamma-glycidyloxypropyl trimethoxysilane, but the limit oxygen index and the weight gain of the prepared nylon fabric are obviously reduced compared with that of a blank control group, which shows that the flame retardant effect of the aminopropyl triethoxysilane and gamma-glycidyloxypropyl trimethoxysilane polymerized together is better than that of the aminopropyl triethoxysilane self-polymerization or gamma-glycidyloxypropyl trimethoxysilane self-polymerization, the comparative example 3 changes the mixing mass ratio of gamma-glycidyloxypropyl trimethoxysilane and aminopropyl triethoxysilane, but the limit oxygen index and the weight gain of the prepared nylon fabric are reduced to different degrees, which shows that the use amount of the gamma-glycidyloxypropyl trimethoxysilane and the aminopropyl triethoxysilane is optimized, the change the structure of the flame retardant on the surface of the nylon fabric, thereby influencing the grafting rate of the nylon fabric, the comparative example 4 changes the flame retardant effect of the gamma-glycidyloxypropyl trimethoxysilane and the acceleration rate of the nylon fabric, but the graft ratio of the aminopropyl trimethoxysilane and the graft ratio of the aminopropyl trimethoxysilane on the surface of the nylon fabric is obviously reduced on the nylon fabric is improved, the flame retardant has the limit oxygen index of the nylon fabric is obviously reduced when the nylon fabric is prepared by the nylon fabric, the graft ratio of the gamma-glycidyloxypropyl triethoxysilane is changed, the nylon fabric is prepared on the nylon fabric, the graft ratio of the nylon fabric is obviously is greatly reduced, effectively improves the flame retardance of nylon fabrics.
Test example two, thermal performance test
Test samples were nylon fabrics prepared in example 3 and comparative examples 1 to 5, and blank samples were made using nylon fabric base fabric.
The cone calorimetric test is carried out according to ISO/DIS 13927-2001, simple thermal energy release test with conical radiant heater and thermopile detector for plastics, test size 100mm×100mm, heat flow 50kW/m 2.
Test results the test results are shown in figures 1 and 2.
As can be seen from FIG. 1, the peak heat release rate of the nylon fabric of the blank group was 456.9kW/m 2, and the peak heat release rate of the nylon fabric prepared in example 3 was 298.2kW/m 2, which is significantly lower than that of the blank group. As can be seen from FIG. 2, the peak of the heat of combustion of the nylon fabric prepared in example 3 of the present invention was significantly shifted backward and the peak was significantly reduced. In conclusion, the nylon fabric provided by the invention has good flame retardance.
The above examples are only illustrative of the preparation method of the present invention and are not intended to limit the present invention. Modifications to the above would be obvious to those of ordinary skill in the art, but would not bring the invention so modified beyond the scope of the present invention. Therefore, all equivalent modifications and changes which are accomplished by those skilled in the art without departing from the technical spirit provided by the present invention are intended to be covered by the claims of the present invention.

Claims (10)

1. The preparation method of the nylon fabric is characterized by comprising the following steps of:
S1, soaking a nylon fabric in a sodium carbonate solution, heating to boiling, boiling for 1-2 hours, cooling, taking out the nylon fabric, and cleaning with clear water to obtain a pretreated nylon fabric;
S2, immersing the pretreated nylon fabric prepared in the step S1 in glycol aqueous solution, adding tartaric acid, stirring for 0.5-1h under the condition of the rotating speed of 1200-1400rpm, taking out the nylon fabric, drying, washing with clear water to be neutral, and airing at room temperature to obtain a modified nylon fabric I;
s3, immersing the modified nylon fabric I prepared in the step S2 in an ethanol mixed solution of p-hydroxybenzoic acid and phosphoric acid ester amide, heating to 50-60 ℃ for 1-1.5h, taking out the nylon fabric, and washing with clear water to obtain a modified nylon fabric II;
S4, soaking the modified nylon fabric II obtained in the step S3 in an aqueous solution of tetramethyl phosphorus hydroxide and sodium dodecyl sulfate, heating to 40-50 ℃, dropwise adding a mixture of gamma-glycidol ether oxypropyl trimethoxy silane and aminopropyl triethoxy silane, stirring for 3.5-4 hours, taking out the nylon fabric, washing with clear water, and drying to obtain the modified nylon fabric II.
2. The method for producing nylon fabric according to claim 1, wherein the concentration of the sodium carbonate solution in step S1 is 0.06-0.08mol/L and the pH is 8.5-9.
3. The method for producing nylon fabric according to claim 1, wherein the mass percentage of the ethylene glycol in the step S2 is 20 to 25%.
4. The method for producing nylon fabric according to claim 1, wherein the amount of tartaric acid used in step S2 is 15-17% of the mass of the nylon fabric.
5. The method of producing nylon fabric according to claim 1, wherein the impregnation temperature in step S2 is 75 to 80 ℃.
6. The method for producing nylon fabric according to claim 1, wherein the concentration of parahydroxybenzoic acid in step S3 is 0.5 to 0.7mol/L, and the concentration of phosphoric acid ester amide is 0.15 to 0.2mol/L.
7. The method for producing nylon fabric according to claim 1, wherein the concentration of the tetramethyl phosphonium hydroxide in step S4 is 0.02 to 0.03mol/L and the concentration of the sodium dodecyl sulfate is 0.03 to 0.04mol/L.
8. The method for producing nylon fabric according to claim 1, wherein the dripping speed of the mixture of γ -glycidoxypropyl trimethoxysilane and aminopropyl triethoxysilane in step S4 is 2.2-2.6m 3/h.
9. The method for producing nylon fabric according to claim 1, wherein the mixing mass ratio of the gamma-glycidoxypropyl trimethoxysilane and the aminopropyl triethoxysilane in step S4 is 2-5:9-13.
10.A nylon fabric produced according to the method for producing a nylon fabric of any one of claims 1 to 9.
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CN104404772A (en) * 2014-12-06 2015-03-11 苏州大学 Surface-modified aramid fiber and preparation method thereof
CN105484031A (en) * 2016-01-04 2016-04-13 北京化工大学 Synthetic fiber/fabric inflaming retarding graft modified product and preparing method

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JP4695279B2 (en) * 2001-03-21 2011-06-08 日華化学株式会社 Flame retardant processing agent, flame retardant processing method, and flame retardant processed fiber
CN108589284B (en) * 2018-05-28 2024-02-20 苏州大学 Preparation method of flame-retardant carboxymethylated nylon fabric

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CN104404772A (en) * 2014-12-06 2015-03-11 苏州大学 Surface-modified aramid fiber and preparation method thereof
CN105484031A (en) * 2016-01-04 2016-04-13 北京化工大学 Synthetic fiber/fabric inflaming retarding graft modified product and preparing method

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