CN117364488A - Preparation method of polyester/cotton blended fabric with durable and expanded carbon flame-retardant coating - Google Patents

Preparation method of polyester/cotton blended fabric with durable and expanded carbon flame-retardant coating Download PDF

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CN117364488A
CN117364488A CN202311640433.9A CN202311640433A CN117364488A CN 117364488 A CN117364488 A CN 117364488A CN 202311640433 A CN202311640433 A CN 202311640433A CN 117364488 A CN117364488 A CN 117364488A
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polyester
flame
retardant
blended fabric
durable
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CN117364488B (en
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赵金广
汤方明
张烨
沈建根
张建光
熊克
张怡
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Jiangsu Hengli Chemical Fiber Co Ltd
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Jiangsu Hengli Chemical Fiber 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
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/327Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
    • D06M15/333Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
    • 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
    • D06M11/68Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
    • 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
    • D06M13/322Treating 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
    • D06M13/325Amines
    • D06M13/342Amino-carboxylic acids; Betaines; Aminosulfonic acids; Sulfo-betaines
    • 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
    • D06M13/402Amides imides, sulfamic acids
    • D06M13/432Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
    • 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
    • D06M13/46Compounds containing quaternary nitrogen atoms
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    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • 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
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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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)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a preparation method of a durable-expansion charcoal-forming flame-retardant coating polyester/cotton blended fabric, which comprises the steps of dissolving polyvinyl alcohol, ammonium phytate, ethylenediamine tetraacetic acid, pentaerythritol, dicyandiamide and sodium hypophosphite in distilled water to prepare a flame-retardant finishing liquid, and then treating the polyester/cotton blended fabric by a padding-baking method to prepare the durable-expansion charcoal-forming flame-retardant coating polyester/cotton blended fabric; the molar ratio of the ammonium phytate, the pentaerythritol and the ethylenediamine tetraacetic acid is 1:2-2.2:1.3-1.5. According to the preparation method, esterification reaction can be carried out between ammonium phytate, pentaerythritol and ethylenediamine tetraacetic acid in the baking process, and a linear or network-shaped intumescent flame retardant is generated in situ; and the ammonium phosphate radical and the carboxylate radical in the intumescent flame retardant are subjected to esterification reaction with the hydroxyl groups of cotton fibers and polyvinyl alcohol, so that the flame retardant radical and the polyvinyl alcohol film are firmly fixed on the polyester/cotton blended fabric, and the fabric has excellent washing resistance and flame retardant efficiency.

Description

Preparation method of polyester/cotton blended fabric with durable and expanded carbon flame-retardant coating
Technical Field
The invention belongs to the technical field of flame-retardant fabrics, and relates to a preparation method of a polyester/cotton blended fabric with a durable and expanded carbon flame-retardant coating.
Background
Polyester/cotton blend fabrics are one of the most widely used materials and are in the most important position in the modern textile industry. However, polyester/cotton blend fabrics are flammable materials, and the two components also have a 'candlewick effect', so that flame retardation modification is relatively difficult. There remains a great challenge to develop highly effective durable flame retardant polyester/cotton blend fabrics.
With the increasing demand for environmental protection, great attention is paid to the development of bio-based flame retardant materials and the use of the materials for improving the flame retardant function of textiles.
In the document 1 (phosphorus/nitrogen flame retardant is used for flame-retardant finishing [ J ]. Textile science newspaper, 2022,43 (6): 94-99,106) adopts biomass phytic acid and urea to synthesize ammonium phytate, and the polyester/cotton blended fabric is finished by a rolling-baking process, so that the flame retardant property of the polyester/cotton blended fabric is improved, and the cotton component in the polyester/cotton blended fabric is smaller, the phytic acid-based flame retardant generally reacts with cotton fibers and cannot generate crosslinking reaction with the polyester fibers, so that the grafting amount of the flame retardant is reduced, and a sufficient amount of the flame retardant cannot be fixed on the polyester/cotton blended fabric, therefore, the water-washing resistance of the finished polyester/cotton blended fabric is poor, and the flame retardant effect is lost after water washing.
In the literature 2 (research and development [ J ] of flame-retardant polyester fabrics based on phosphate, modern silk science and technology, 2020,35 (3): 4-6,40.) the linear phosphate flame retardant is synthesized by esterification reaction of phytic acid and polyvinyl alcohol (i.e. phytic acid is grafted on polyvinyl alcohol as a flame retardant), but the phosphate flame retardant is coated on the surface of the fabric, wherein the polyvinyl alcohol forms a film and is physically adhered to the fabric, the washing resistance is poor, and the further improvement is still needed.
The Chinese patent No. 115652642A discloses a preparation method of flame-retardant durable polyester/cotton blended fabric, which comprises the steps of adding macromolecular phosphorus/nitrogen flame retardant synthesized by phytic acid and urea, ammonia water and dicyandiamide into distilled water to prepare flame-retardant finishing liquid, immersing the polyester/cotton blended fabric into the flame-retardant finishing liquid, and treating the polyester/cotton blended fabric by a padding-baking method, wherein the macromolecular phosphorus/nitrogen flame retardant has film-forming property and can form covalent bond with cotton fibers, so that the modified fabric has certain durability; however, the film formed by the macromolecular phosphorus/nitrogen flame retardant has poor stability and poor adhesiveness to fabrics (except for the point of a covalent bond bonding area, other areas of the film are physically adhered to the fabrics), so that the film can be slowly hydrolyzed and redissolved in washing liquid after washing, the flame retardant performance is reduced, and the flame retardant polyester/cotton blended fabric can resist 20 times of washing and still needs to be further improved.
The preparation method of the polyester/cotton blended fabric with the durable expansion carbon flame-retardant coating is researched to solve the problem of poor flame-retardant durability of the polyester/cotton blended fabric, and has very important significance.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method of a polyester/cotton blended fabric with a durable and expanded carbon flame-retardant coating.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the durable-swelling-to-carbon flame-retardant coating polyester/cotton blended fabric comprises the steps of dissolving polyvinyl alcohol, ammonium phytate, ethylenediamine tetraacetic acid, pentaerythritol, dicyandiamide and sodium hypophosphite in distilled water (the distilled water is heated to 80-90 ℃ and then the reagents are added to facilitate the dissolution of the reagents such as the polyvinyl alcohol) to prepare a flame-retardant finishing liquid, and then treating the polyester/cotton blended fabric by a padding-baking method to prepare the durable-swelling-to-carbon flame-retardant coating polyester/cotton blended fabric;
the molar ratio of the ammonium phytate, the pentaerythritol and the ethylenediamine tetraacetic acid is 1:2-2.2:1.3-1.5;
the phytic acid ammonium molecule contains six active ammonium phosphate groups, and can carry out covalent bond crosslinking reaction with hydroxyl groups of pentaerythritol, hydroxyl groups of cotton fibers and hydroxyl groups of polyvinyl alcohol in the presence of dicyandiamide catalyst; the ethylene diamine tetraacetic acid contains four carboxyl groups, and can carry out covalent bond crosslinking reaction with hydroxyl groups of pentaerythritol, hydroxyl groups of cotton fibers and hydroxyl groups of polyvinyl alcohol in the presence of a sodium hypophosphite catalyst;
therefore, the ammonium phytate, pentaerythritol and ethylenediamine tetraacetic acid can undergo esterification reaction in the baking process to generate linear or network expansion flame retardant in situ; and the ammonium phosphate radical and the carboxylate radical in the linear or network expansion type flame retardant react with the hydroxyl of the cotton fiber and the polyvinyl alcohol in an esterification way, so that the flame retardant radical and the polyvinyl alcohol film are firmly fixed on the polyester/cotton blended fabric;
the phosphate radical of the ammonium phosphate flame retardant is used as an acid source, the ammonium radical is used as a gas source, the ethylenediamine tetraacetic acid is rich in nitrogen element and carboxylic acid groups, the ethylenediamine tetraacetic acid can be used as a gas source and a char former, the pentaerythritol can be used as the char former, and several flame retardant groups are organically combined to construct an intumescent flame retardant system, so that the flame retardant system has good intumescent foaming performance in the combustion process and high flame retardant efficiency.
As a preferable technical scheme:
the preparation method of the polyester/cotton blended fabric with the durable and expanded carbon flame-retardant coating has the advantage that the polyvinyl alcohol is 1788 type or 1799 type.
According to the preparation method of the polyester/cotton blended fabric with the carbon flame-retardant coating, which is formed by persistent expansion, the content of polyvinyl alcohol in the flame-retardant finishing liquid is 60-80 g/L.
According to the preparation method of the polyester/cotton blended fabric with the carbon flame-retardant coating, which is formed by persistent expansion, the content of ammonium phytate in the flame-retardant finishing liquid is 150-200 g/L; ammonium phytate is prepared by the method described in reference 3 (phosphorus/nitrogen flame retardant finish for polyester/cotton blend fabrics [ J ]. Textile journal, 2022,43 (6): 94 99, 106).
The preparation method of the polyester/cotton blended fabric with the durable and expanded carbon flame-retardant coating comprises the steps that dicyandiamide is used as a catalyst for esterification reaction between ammonium phosphate and hydroxyl, and sodium hypophosphite is used as a catalyst for esterification reaction between hydroxyl and carboxyl; the content of dicyandiamide in the flame-retardant finishing liquid is 40-60 g/L, and the content of sodium hypophosphite is 30-50 g/L.
The preparation method of the polyester/cotton blended fabric with the durable and expanded carbon flame-retardant coating comprises the following process parameters: the rolling residual rate is 90-110 percent (the higher the rolling residual rate is, the higher the liquid carrying amount of the polyester/cotton blended fabric and the amount of the flame retardant are, the better the flame retardant effect is, but the too high flame retardant effect is easy to cause non-uniformity); the pre-baking temperature is 75-85 ℃, and the pre-baking time is 4-7 min; the baking temperature is 160-180 ℃ and the baking time is 3-5 min; the polyvinyl alcohol has good film forming property under baking condition and has higher adhesiveness with polyester/cotton blended fabrics; the ammonium phytate is rich in active ammonium phosphate groups, and can be subjected to esterification reaction with hydroxyl groups of cotton fibers, polyvinyl alcohol and pentaerythritol under baking conditions, so that polyvinyl alcohol and phosphorus-containing flame retardant groups are grafted on the polyester/cotton blended fabric, the ammonium phytate is high in consumption, good in flame retardant effect and waste due to overhigh flame retardant effect.
The preparation method of the polyester/cotton blended fabric with the durable and expanded carbon flame-retardant coating comprises the steps of 80/20, 65/35 or 50/50 of the polyester/cotton blended fabric.
According to the preparation method of the durable expansion carbon-flame-retardant coating polyester/cotton blended fabric, the limiting oxygen index of the durable expansion carbon-flame-retardant coating polyester/cotton blended fabric is not lower than 32.5%, the damage length is not higher than 11.5cm, the damage length after 50 times of water washing is not higher than 14.3cm (the damage length of the polyester/cotton blended fabric before treatment is 30cm, and the limiting oxygen index is 18.5%).
The principle of the invention:
the ammonium phytate can generate covalent bond grafting with cotton fibers under the action of a catalyst and high temperature, however, polyester/cotton blended fabrics mainly comprise polyester components, the polyester components and a flame retardant cannot generate grafting, and the flame retardant modification of the polyester/cotton blended fabrics is more difficult than the flame retardance of cotton and polyester fabrics. It is difficult to graft a sufficient amount of flame retardant on polyester/cotton blend fabrics, especially fabrics based on polyester components, by covalent bond grafting, so flame retardant modification and durable flame retardant modification are particularly difficult.
In the prior art, the flame retardant is singly grafted on the surface of the polyester/cotton blended fabric, so that excellent flame retardant durability cannot be provided for the flame retardant coating, because ester bonds formed by the flame retardant and the fabric are gradually hydrolyzed in the water washing process, and the flame retardant is removed through the water washing; the polyvinyl alcohol can form a film on the surface of the polyester/cotton blended fabric, and has certain adhesiveness to the polyester/cotton blended fabric; however, the improvement degree of the washability of the flame-retardant coating is limited only by the adhesion performance of the polyvinyl alcohol to the fabric; the flame retardant is singly grafted on the polyvinyl alcohol film, the polyvinyl alcohol film and the polyester/cotton blended fabric are physically adhered, and excellent flame retardant durability cannot be provided for the flame retardant coating, because ester bonds formed by the polyvinyl alcohol of the flame retardant can be gradually hydrolyzed in the water washing process and removed through the water washing, and the polyvinyl alcohol film can be swelled and shed in the water washing process, so that the flame retardant effect is poor.
In the invention, ammonium phosphate of ammonium phytate can be subjected to esterification reaction with hydroxyl of pentaerythritol under the conditions of a catalyst and high-temperature baking, and hydroxyl of pentaerythritol can be subjected to esterification reaction with carboxyl of ethylenediamine tetraacetic acid, so that linear or network structure intumescent flame retardant can be generated in situ by the three reactions; the ammonium phosphate radical and carboxyl in the flame retardant molecule can be subjected to esterification reaction with hydroxyl of cotton fiber and polyvinyl alcohol; wherein, because polyvinyl alcohol, ammonium phytate, ethylenediamine tetraacetic acid, pentaerythritol, dicyandiamide and sodium hypophosphite are dissolved in distilled water to prepare flame retardant finishing liquid, the flame retardant finishing liquid is entangled with polyvinyl alcohol macromolecules in the process of generating the linear or network structure expansion flame retardant, thereby firmly fixing the polyvinyl alcohol film and the linear or network structure expansion flame retardant; therefore, in the prepared durable intumescent flame-retardant coating polyester/cotton blended fabric, on one hand, the linear or network-shaped intumescent flame retardant is bridged on cotton fibers and the polyvinyl alcohol film through ester bonds (part of flame retardant is also singly combined with the outer surface of the polyvinyl alcohol film through ester bonds), and on the other hand, the polyvinyl alcohol film is entangled and fixed with the linear or network-shaped intumescent flame retardant, so that the polyvinyl alcohol film and the linear or network-shaped intumescent flame retardant are difficult to separate through hydrolysis, and the polyvinyl alcohol film can be used as a protective film to reduce moisture penetration and reduce ester bond hydrolysis between the fabric and the flame retardant; therefore, the flame-retardant coating polyester/cotton blended fabric has excellent water-washing resistance (50 times of water washing resistance);
the flame retardation of the polyester/cotton blended fabric is usually finished by adopting a polyester cyclic phosphate flame retardant and a cotton phosphorus flame retardant, and the flame retardation system has low flame retardation efficiency; the cyclic phosphate flame retardant mainly plays a role in flame retardance through a gas phase mechanism, and the phosphorus flame retardant for cotton plays a role through a solid phase flame retardance mechanism, but has weak solid phase catalytic char forming capability and high flame retardant consumption; the ammonium phytate flame retardant mainly plays a role in solid phase, can catalyze cotton fibers to form charcoal, and the cotton fibers participate in main carbonization, but the cotton fibers have poor charcoal forming capability. In the linear or network-shaped intumescent flame retardant, the phosphate radical of the ammonium phytate flame retardant is used as an acid source, the ammonium radical is used as an air source, the ethylenediamine tetraacetic acid is rich in nitrogen elements and carboxylic acid groups, the ammonium phytate flame retardant can be used as an air source and a char former, the pentaerythritol can be used as a char former, the polyvinyl alcohol can be used as a char former, and several flame retardant groups are organically combined to construct an intumescent flame retardant system, so that the flame retardant has good intumescent foaming performance in the combustion process and high flame retardant efficiency.
The beneficial effects are that:
(1) According to the preparation method of the polyester/cotton blended fabric with the durable-swelling carbon-forming flame-retardant coating, esterification reaction can be carried out between ammonium phytate, pentaerythritol and ethylenediamine tetraacetic acid in the baking process, and a linear or network-like swelling flame retardant is generated in situ; the ammonium phosphate and the carboxylate in the linear or network-shaped expansion type flame retardant react with the hydroxyl of the cotton fiber and the polyvinyl alcohol in an esterification way, so that the flame retardant group and the polyvinyl alcohol film are firmly fixed on the polyester/cotton blended fabric, the durability of the flame retardant on the fabric is improved, and the flame retardant coating polyester/cotton blended fabric has excellent washing resistance;
(2) According to the preparation method of the durable intumescent flame-retardant coating polyester/cotton blended fabric, phosphate of the ammonium phytate flame retardant is used as an acid source, ammonium is used as an air source, ethylenediamine tetraacetic acid is rich in nitrogen and carboxylic acid groups, the ammonium can be used as an air source and a char forming agent, pentaerythritol can be used as the char forming agent, a plurality of flame-retardant groups are organically combined to construct an intumescent flame-retardant system, and the intumescent flame-retardant coating polyester/cotton blended fabric has good intumescent foaming performance and high flame-retardant efficiency in a combustion process.
Drawings
FIG. 1 is a schematic cross-linking mechanism of a flame retardant coating of the present invention with a polyester/cotton blend fabric;
FIG. 2 is a surface topography of an uncoated polyester/cotton blend fabric of example 1 (i.e., the polyester/cotton blend fabric of example 1) and a coated polyester/cotton blend fabric of the present invention;
FIG. 3 is a surface topography of an uncoated polyester/cotton blend fabric of example 1 (i.e., the polyester/cotton blend fabric of example 1) and coated polyester/cotton blend fabric carbon residue of the present invention;
fig. 4 is an infrared spectrum of carbon residue of the polyester/cotton blend fabric and the flame retardant coating polyester/cotton blend fabric of example 1 of the present invention.
Detailed Description
The invention is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
The test method related by the invention comprises the following steps:
limiting oxygen index: the limiting oxygen index of the polyester/cotton blended fabric of the carbon flame-retardant coating which is formed by persistent expansion is tested by GB/T5454-1997 "oxygen index method of textile combustion performance experiment";
damage length: the GB/T5455-2014 test of the damage length smoldering in the vertical direction of the combustion performance of the textile and the measurement of the continuous combustion time is adopted to test the damage length of the polyester/cotton blended fabric which is expanded into the carbon flame retardant coating for a long time;
damage length after 50 times of water washing: according to the invention, washing is carried out on the durable-expansion charcoal-resistant flame-retardant coating polyester/cotton blended fabric according to an AATCC 61-2013 accelerated test of household and commercial washing fastness, and the GB/T5455-2014 test of the damage length smoldering and continuous burning time in the vertical direction of the burning performance of the textile is adopted to test the damage length of the durable-expansion charcoal-resistant flame-retardant coating polyester/cotton blended fabric.
Example 1
A preparation method of a polyester/cotton blended fabric with a durable and expanded carbon flame-retardant coating is shown in figure 1, and comprises the following specific steps:
(1) Dissolving 1788 type polyvinyl alcohol, ammonium phytate, ethylenediamine tetraacetic acid, pentaerythritol, dicyandiamide and sodium hypophosphite in distilled water preheated to 80 ℃ to prepare flame-retardant finishing liquid;
wherein, the mol ratio of the ammonium phytate, the pentaerythritol and the ethylenediamine tetraacetic acid is 1:2.2:1.5; the content of polyvinyl alcohol in the flame-retardant finishing liquid is 60g/L, the content of ammonium phytate is 150g/L, the content of dicyandiamide is 40g/L, and the content of sodium hypophosphite is 30g/L;
(2) The 65/35 polyester/cotton blended fabric is treated by padding-baking method, and the polyester/cotton blended fabric which is expanded into the carbon flame-retardant coating for a long time is prepared;
the padding-baking process parameters are as follows: the rolling surplus rate is 90%; the pre-baking temperature is 75 ℃, and the pre-baking time is 7min; baking temperature is 160 ℃, and baking time is 5min.
The limiting oxygen index of the finally prepared polyester/cotton blended fabric with the durable and expanded flame-retardant carbon coating is 32.5%, the damage length is 11.5cm, and the damage length after 50 times of water washing is 14.3cm.
As shown in fig. 2, the surface of the uncoated polyester/cotton blend fabric was smoother, while the surface of the coated polyester/cotton blend fabric deposited a large amount of flame retardant.
As shown in fig. 3, the carbon residue of the uncoated polyester/cotton blend fabric is smooth and porous, because the polyester/cotton blend fabric burns rapidly and has poor char formation performance, while the carbon residue of the coated polyester/cotton blend fabric finds more expansion structure, which indicates that the flame retardant mechanism of the coated polyester/cotton blend fabric is an expansion flame retardant mechanism.
As shown in FIG. 4, 1242cm of infrared spectrum of the flame retardant coated polyester/cotton blend fabric is compared with the uncoated polyester/cotton blend fabric -1 A new absorption peak appears at 1078cm -1 The absorption peak at the position is obviously changed, which is caused by the structures of P=O and P-O of phosphorus-containing groups in the flame-retardant coating; in addition, 1715cm of infrared spectrum of the flame-retardant coating polyester/cotton blended fabric -1 The absorption peak intensity at this point is significantly increased because a new carboxylate structure is formed in the flame retardant coating, which indicates that the flame retardant coating was successfully deposited on the polyester/cotton blend fabric.
Comparative example 1
A method for preparing a coated polyester/cotton blend fabric, which is basically the same as in example 1, and is different in that: in the step (1), the dicyandiamide and sodium hypophosphite are replaced by equal volume of water, and the baking temperature in the step (2) is 130 ℃.
The limiting oxygen index of the prepared coating polyester/cotton blended fabric is 32.4%, the damage length is 11.6cm, and the coating polyester/cotton blended fabric can only resist 15 times of water washing.
Comparing example 1 with comparative example 1, it can be found that comparative example 1 has good flame retardant property but poor water washing resistance, because polyvinyl alcohol can form a film better under the condition, but covalent bond crosslinking reaction cannot occur, and the degree of improvement of the water washing resistance of the flame retardant coating is limited only by the adhesion property of the polyvinyl alcohol to the fabric.
Comparative example 2
A method for preparing a coated polyester/cotton blend fabric, which is basically the same as in example 1, except that the polyvinyl alcohol is replaced by an equal volume of water in step (1).
The limiting oxygen index of the prepared coating polyester/cotton blended fabric is 32.7%, the damage length is 11.3cm, and the coating polyester/cotton blended fabric can only resist 10 times of water washing.
Comparing example 1 with comparative example 2, it can be found that the coated polyester/cotton blend fabric of comparative example 2 has better flame retardant properties but has poor water washing resistance because the flame retardant alone is grafted on the surface of the polyester/cotton blend fabric, and cannot provide excellent flame retardant durability to the flame retardant coating because the ester bond formed by the flame retardant and the fabric is gradually hydrolyzed during washing and removed by washing.
Example 2
A preparation method of a polyester/cotton blended fabric with a durable and expanded carbon flame-retardant coating comprises the following specific steps:
(1) Dissolving 1788 type polyvinyl alcohol, ammonium phytate, ethylenediamine tetraacetic acid, pentaerythritol, dicyandiamide and sodium hypophosphite in distilled water preheated to 82 ℃ to prepare flame-retardant finishing liquid;
wherein, the mol ratio of the ammonium phytate, the pentaerythritol and the ethylenediamine tetraacetic acid is 1:2:1.3; the content of polyvinyl alcohol in the flame-retardant finishing liquid is 65g/L, the content of ammonium phytate is 160g/L, the content of dicyandiamide is 45g/L, and the content of sodium hypophosphite is 35g/L;
(2) 80/20 of the polyester/cotton blended fabric is treated by padding-baking method, and the polyester/cotton blended fabric which is expanded into the carbon flame-retardant coating for a long time is prepared;
the padding-baking process parameters are as follows: the rolling surplus rate is 95%; the pre-baking temperature is 77 ℃, and the pre-baking time is 6.5min; baking temperature is 165 ℃, and baking time is 4.5min.
The limiting oxygen index of the finally prepared polyester/cotton blended fabric with the durable and expanded flame-retardant coating is 33.2%, the damage length is 11cm, and the damage length after 50 times of water washing is 13.6cm.
Example 3
A preparation method of a polyester/cotton blended fabric with a durable and expanded carbon flame-retardant coating comprises the following specific steps:
(1) Dissolving 1788 type polyvinyl alcohol, ammonium phytate, ethylenediamine tetraacetic acid, pentaerythritol, dicyandiamide and sodium hypophosphite in distilled water preheated to 84 ℃ to prepare flame-retardant finishing liquid;
wherein, the mol ratio of the ammonium phytate, the pentaerythritol and the ethylenediamine tetraacetic acid is 1:2.1:1.4; the content of polyvinyl alcohol in the flame-retardant finishing liquid is 70g/L, the content of ammonium phytate is 170g/L, the content of dicyandiamide is 50g/L, and the content of sodium hypophosphite is 40g/L;
(2) The 65/35 polyester/cotton blended fabric is treated by padding-baking method, and the polyester/cotton blended fabric which is expanded into the carbon flame-retardant coating for a long time is prepared;
the padding-baking process parameters are as follows: the rolling surplus rate is 100 percent; the pre-baking temperature is 79 ℃ and the pre-baking time is 6min; baking temperature is 170 ℃ and baking time is 4min.
The limiting oxygen index of the finally prepared polyester/cotton blended fabric with the durable and expanded flame-retardant carbon coating is 33.6%, the damage length is 10.6cm, and the damage length after 50 times of water washing is 13.1cm.
Example 4
A preparation method of a polyester/cotton blended fabric with a durable and expanded carbon flame-retardant coating comprises the following specific steps:
(1) Dissolving 1799 type polyvinyl alcohol, ammonium phytate, ethylenediamine tetraacetic acid, pentaerythritol, dicyandiamide and sodium hypophosphite in distilled water preheated to 86 ℃ to prepare flame-retardant finishing liquid;
wherein, the mol ratio of the ammonium phytate, the pentaerythritol and the ethylenediamine tetraacetic acid is 1:2.2:1.5; the content of polyvinyl alcohol in the flame-retardant finishing liquid is 75g/L, the content of ammonium phytate is 180g/L, the content of dicyandiamide is 55g/L, and the content of sodium hypophosphite is 45g/L;
(2) 80/20 of the polyester/cotton blended fabric is treated by padding-baking method, and the polyester/cotton blended fabric which is expanded into the carbon flame-retardant coating for a long time is prepared;
the padding-baking process parameters are as follows: the rolling surplus rate is 105%; the pre-baking temperature is 81 ℃, and the pre-baking time is 5.5min; baking temperature is 175 ℃ and baking time is 3.5min.
The limiting oxygen index of the finally prepared polyester/cotton blended fabric with the durable and expanded flame-retardant coating is 34%, the damage length is 10.3cm, and the damage length after 50 times of water washing is 12.7cm.
Example 5
A preparation method of a polyester/cotton blended fabric with a durable and expanded carbon flame-retardant coating comprises the following specific steps:
(1) Dissolving 1799 type polyvinyl alcohol, ammonium phytate, ethylenediamine tetraacetic acid, pentaerythritol, dicyandiamide and sodium hypophosphite in distilled water preheated to 88 ℃ to prepare flame-retardant finishing liquid;
wherein, the mol ratio of the ammonium phytate, the pentaerythritol and the ethylenediamine tetraacetic acid is 1:2:1.3; the content of polyvinyl alcohol in the flame-retardant finishing liquid is 80g/L, the content of ammonium phytate is 190g/L, the content of dicyandiamide is 60g/L, and the content of sodium hypophosphite is 50g/L;
(2) The 65/35 polyester/cotton blended fabric is treated by padding-baking method, and the polyester/cotton blended fabric which is expanded into the carbon flame-retardant coating for a long time is prepared;
the padding-baking process parameters are as follows: the rolling surplus rate is 108%; pre-baking temperature is 83 ℃, and pre-baking time is 5min; baking temperature is 178 ℃ and baking time is 3min.
The limiting oxygen index of the finally prepared polyester/cotton blended fabric with the durable and expanded flame-retardant carbon coating is 34.3%, the damage length is 9.9cm, and the damage length after 50 times of water washing is 12.5cm.
Example 6
A preparation method of a polyester/cotton blended fabric with a durable and expanded carbon flame-retardant coating comprises the following specific steps:
(1) Dissolving 1799 type polyvinyl alcohol, ammonium phytate, ethylenediamine tetraacetic acid, pentaerythritol, dicyandiamide and sodium hypophosphite in distilled water preheated to 90 ℃ to prepare flame-retardant finishing liquid;
wherein, the mol ratio of the ammonium phytate, the pentaerythritol and the ethylenediamine tetraacetic acid is 1:2.1:1.4; the content of polyvinyl alcohol in the flame-retardant finishing liquid is 80g/L, the content of ammonium phytate is 200g/L, the content of dicyandiamide is 60g/L, and the content of sodium hypophosphite is 50g/L;
(2) The 65/35 polyester/cotton blended fabric is treated by padding-baking method, and the polyester/cotton blended fabric which is expanded into the carbon flame-retardant coating for a long time is prepared;
the padding-baking process parameters are as follows: the rolling surplus rate is 110%; pre-baking temperature is 85 ℃, and pre-baking time is 4min; baking temperature is 180 ℃ and baking time is 3min.
The limiting oxygen index of the finally prepared polyester/cotton blended fabric with the durable and expanded flame-retardant carbon coating is 34.5%, the damage length is 9.6cm, and the damage length after 50 times of water washing is 12.2cm.

Claims (8)

1. A preparation method of a polyester/cotton blended fabric with a durable and expanded carbon flame-retardant coating is characterized by comprising the following steps: after polyvinyl alcohol, ammonium phytate, ethylenediamine tetraacetic acid, pentaerythritol, dicyandiamide and sodium hypophosphite are dissolved in distilled water to prepare flame-retardant finishing liquid, the polyester/cotton blended fabric is treated by a padding-baking method, and the durable-expansion carbon-coated flame-retardant polyester/cotton blended fabric is prepared;
the molar ratio of the ammonium phytate, the pentaerythritol and the ethylenediamine tetraacetic acid is 1:2-2.2:1.3-1.5.
2. The method for preparing a polyester/cotton blend fabric with a durable and flame retardant carbon-expanded coating according to claim 1, wherein the polyvinyl alcohol is 1788 type or 1799 type.
3. The method for preparing the polyester/cotton blended fabric with the durable-swelling-carbon-forming flame-retardant coating, which is disclosed in claim 1, is characterized in that the content of polyvinyl alcohol in the flame-retardant finishing liquid is 60-80 g/L.
4. The method for preparing the polyester/cotton blended fabric with the durable-swelling-carbon-forming flame-retardant coating, which is disclosed in claim 1, is characterized in that the content of ammonium phytate in the flame-retardant finishing liquid is 150-200 g/L.
5. The preparation method of the durable and intumescent flame-retardant coating polyester/cotton blended fabric according to claim 1, wherein the content of dicyandiamide in the flame-retardant finishing liquid is 40-60 g/L, and the content of sodium hypophosphite is 30-50 g/L.
6. The method for preparing the durable and intumescent flame retardant coating polyester/cotton blended fabric according to claim 1, wherein the padding-baking process parameters are as follows: the rolling surplus rate is 90-110%; the pre-baking temperature is 75-85 ℃, and the pre-baking time is 4-7 min; the baking temperature is 160-180 ℃ and the baking time is 3-5 min.
7. The method for preparing the polyester/cotton blend fabric with the durable and expanded carbon flame retardant coating according to claim 1, wherein the polyester/cotton blend fabric is 80/20, 65/35 or 50/50 polyester/cotton blend fabric.
8. The method for preparing the polyester/cotton blended fabric with the durable and expanded flame-retardant coating, as claimed in claim 7, wherein the limiting oxygen index of the polyester/cotton blended fabric with the durable and expanded flame-retardant coating is not lower than 32.5%, the damage length is not higher than 11.5cm, and the damage length after 50 times of water washing is not higher than 14.3cm.
CN202311640433.9A 2023-12-04 2023-12-04 Preparation method of polyester/cotton blended fabric with durable and expanded carbon flame-retardant coating Active CN117364488B (en)

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