CN116289201B - Intumescent flame retardant flame-retardant polyester/cotton blended fabric and preparation method thereof - Google Patents
Intumescent flame retardant flame-retardant polyester/cotton blended fabric and preparation method thereofInfo
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- CN116289201B CN116289201B CN202310134854.8A CN202310134854A CN116289201B CN 116289201 B CN116289201 B CN 116289201B CN 202310134854 A CN202310134854 A CN 202310134854A CN 116289201 B CN116289201 B CN 116289201B
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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
- 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
- D06M13/322—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 nitrogen
- D06M13/44—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 nitrogen containing nitrogen and phosphorus
- D06M13/453—Phosphates or phosphites containing nitrogen atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6515—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having three nitrogen atoms as the only ring hetero atoms
- C07F9/6521—Six-membered rings
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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
- D06M13/322—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 nitrogen
- D06M13/35—Heterocyclic compounds
- D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
- D06M13/358—Triazines
- D06M13/364—Cyanuric acid; Isocyanuric acid; Derivatives thereof
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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
- 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
- D06M2101/06—Vegetal fibres cellulosic
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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
- 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
- D06M2101/32—Polyesters
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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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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Abstract
The invention relates to a polyester/cotton blended fabric with an intumescent flame retardant and a preparation method thereof, wherein the surface of the polyester/cotton blended fabric with the intumescent flame retardant is provided with a network flame retardant film, the network flame retardant film and the polyester/cotton blended fabric are bridged by covalent bonds, the network flame retardant film is formed by connecting the intumescent flame retardant on the surface of the polyester/cotton blended fabric by the action of a cross-linking agent, and the structural formula of the intumescent flame retardant is thatThe preparation method comprises the steps of dissolving an intumescent flame retardant, tris (epoxypropyl) isocyanurate, sodium thiosulfate and dicyandiamide in a mixed solution of water and acetone, regulating the pH value of the solution to 6-7 by adopting ammonia water to obtain a flame-retardant finishing liquid, immersing a polyester/cotton blended fabric in the flame-retardant finishing liquid, and treating the polyester/cotton blended fabric by a padding-baking method to obtain the flame-retardant polyester/cotton blended fabric of the intumescent flame retardant. The intumescent flame retardant flame-retardant polyester/cotton blended fabric has excellent flame retardant effect and better flame retardant durability.
Description
Technical Field
The invention belongs to the technical field of flame-retardant modification of polyester/cotton blended fabrics, and relates to an intumescent flame retardant flame-retardant polyester/cotton blended fabric and a preparation method thereof.
Background
With the development of society, the living standard of people is continuously improved, the awareness of safety protection is gradually enhanced, and the social requirement of textile materials with flame-retardant protection function is gradually expanded. The polyester/cotton blended fabric has the characteristics of stiffness, smoothness, quick drying, wear resistance and the like, and has a great deal of application in civil and industrial fields such as indoor and vehicle interior decoration, protective clothing and the like. However, the polyester/cotton blended fabric has a special 'candlewick effect' in the combustion process, and the flame retardant property of the polyester/cotton blended fabric is different from that of the polyester and cotton fabrics, so that the flame retardant property of the polyester/cotton blended fabric is poor, and the requirements of the harsh flame retardant standards of textiles are difficult to meet. Therefore, the flame retardant modification of the polyester/cotton blended fabric is beneficial to improving the safety protection performance of the polyester/cotton blended fabric and expanding the application field of the polyester/cotton blended fabric.
Compared with the traditional halogen flame retardant, the intumescent flame retardant has the characteristics of low smoke, no toxicity, high efficiency, molten drop prevention and the like, and becomes an important development direction of flame retardant material science. Chinese patent No. 106436285A discloses a preparation method and application of an intumescent flame retardant system doped silica sol, wherein an acid source, a carbon source and an air source are mixed to form an intumescent flame retardant system, and then the intumescent flame retardant system is doped with the silica sol to improve the flame retardant property of terylene, cotton or polyester cotton blended fabrics. However, the intumescent flame retardant system has complex components, and the intumescent flame retardant coating and the polyester/cotton blended fabric cannot generate firm chemical bonding, so that the durability of the flame retardant polyester/cotton blended fabric is poor.
Chinese patent No. 104846639A discloses a flame-retardant finishing method of reactive intumescent flame retardant on cotton fabrics, wherein chlorine-containing s-triazine active groups and hydroxyl groups of cotton fibers undergo a crosslinking reaction in the baking process, however, the flame retardant has poor water solubility, a mixed system of ethanol and water is adopted as a solvent, and the reactive intumescent flame retardant is easier to react with the hydroxyl groups of ethanol, so that the reactive intumescent flame retardant loses activity, and the finished cotton fabrics have poor durability.
The literature (phosphorus/nitrogen flame retardant to the flame retardant finish [ J ]. Textile science report, 2022,43 (6): 94-99,106) adopts phytic acid and urea to synthesize phytic acid ammonium salt, through rolling-baking process to carry out formaldehyde-free flame retardant finish to the terylene/cotton blended fabric, phytic acid ammonium can produce covalent bond crosslinking with cotton fiber under the catalysis of dicyandiamide, however in the process of baking at high temperature, ammonium phosphate group is easy to produce and decompose to generate phosphate radical and ammonia gas, resulting in unable to construct phosphorus/nitrogen synergistic flame retardant effect, flame retardant efficiency of the flame retardant is reduced, water-fast washing performance of the finished terylene/cotton blended fabric is poor, and flame retardant effect is lost after water washing.
Therefore, it is necessary to develop an intumescent flame retardant integrating an acid source, a carbon source and a gas source and graft the intumescent flame retardant on a polyester/cotton blend fabric through a covalent bond, thereby providing a flame retardant function with high efficiency and durability.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides an intumescent flame retardant polyester/cotton blended fabric and a preparation method thereof. The invention synthesizes an intumescent flame retardant which contains an acid source, an air source and a carbon source, and can effectively construct the intumescent flame retardant by combining the acid source, the air source and the carbon source, solve the problem of nitrogen loss in the high-temperature baking process, and has higher flame retardant performance.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the surface of the intumescent flame retardant flame-retardant polyester/cotton blended fabric is provided with a network flame-retardant film, and the network flame-retardant film and the polyester/cotton blended fabric are bridged through covalent bonds to generate stable bonding with the polyester/cotton blended fabric, so that the polyester/cotton blended fabric is endowed with high-efficiency and durable flame-retardant functions;
The network flame-retardant film is formed by connecting an intumescent flame retardant on the surface of a polyester/cotton blended fabric through a cross-linking agent tri (epoxypropyl) isocyanurate;
the structural formula of the intumescent flame retardant is
As a preferable technical scheme:
The flame retardant performance of the intumescent flame retardant polyester/cotton blended fabric is that Limiting Oxygen Index (LOI) is 29.8% -33.5%, damage length is 11.9-8.3 cm, no molten drops are generated, maximum heat release rate is 121.3-139.2W/g (LOI of unmodified polyester/cotton blended fabric is 17.3%, damage length is 30cm, maximum heat release rate is 213.5W/g), and damage length after 30 times of washing is not higher than 14.6cm, so that the modified polyester/cotton blended fabric has high-efficiency durable flame retardant function.
The invention also provides a preparation method of the intumescent flame retardant polyester/cotton blended fabric, which comprises the steps of immersing the polyester/cotton blended fabric into flame retardant finishing liquid, and treating the polyester/cotton blended fabric by a padding-baking method to prepare the intumescent flame retardant polyester/cotton blended fabric;
The flame-retardant finishing liquid is prepared by dissolving an intumescent flame retardant, tris (epoxypropyl) isocyanurate, sodium thiosulfate and dicyandiamide in a mixed liquid of water and acetone, regulating the pH value of the solution to 6-7 by adopting ammonia water, and converting phosphate groups into ammonium phosphate groups under the pH condition, so that covalent bond crosslinking with cotton fibers is facilitated.
As a preferable technical scheme:
According to the preparation method of the intumescent flame retardant flame-retardant polyester/cotton blended fabric, the concentration of the intumescent flame retardant in the flame retardant finishing liquid is 100-200 g/L, the increase of the flame retardant dosage is beneficial to improving the flame retardant property of the polyester/cotton blended fabric, but the content of the flame retardant on the polyester/cotton blended fabric is saturated, and excessive flame retardant is wasted.
According to the preparation method of the polyester/cotton blended fabric with the intumescent flame retardant, the tri (epoxypropyl) isocyanurate serves as a network crosslinking agent, three epoxy groups of the tri (epoxypropyl) isocyanurate can generate crosslinking reaction with phosphate groups and hydroxyl groups of the intumescent flame retardant, so that the intumescent flame retardant is mutually connected on the surface of the polyester/cotton blended fabric to form a network structure, the tri (epoxypropyl) isocyanurate can also react with the hydroxyl groups on the surface of the fabric and serve as a crosslinking agent between the flame retardant and the polyester/cotton blended fabric, and the flame retardant network coating is grafted on the surface of the polyester/cotton blended fabric through covalent bonds, so that the efficient and durable flame retardant function is provided. The molar ratio of the tri (epoxypropyl) isocyanurate to the intumescent flame retardant is 2-3:1, the usage amount of the tri (epoxypropyl) isocyanurate is increased to facilitate the formation of a network structure and the grafting of the flame retardant on the fabric, but the excessive usage is wasteful, the acetone is a solvent of the tri (epoxypropyl) isocyanurate, the acetone accounts for 20% -30% of the total volume of water and the acetone, sodium thiosulfate is used as a catalyst to promote the epoxy group of the tri (epoxypropyl) isocyanurate to react with hydroxyl groups of cotton fibers and the intumescent flame retardant, the mass of the sodium thiosulfate is 3-5% of that of the tri (epoxypropyl) isocyanurate, the ammonium phosphate group of the intumescent flame retardant can react with the hydroxyl groups of the cotton fibers in an esterification crosslinking way under the catalysis of dicyandiamide, and the mass of the dicyandiamide is 5-7% of that of the intumescent flame retardant.
The preparation method of the polyester/cotton blended fabric with the flame retardant by the intumescent flame retardant comprises the following technological parameters of padding-baking, namely, padding residual rate of 100-110%, pre-baking temperature of 70-80 ℃, pre-baking time of 2-4 min, baking temperature of 160-170 ℃ and baking time of 5-8 min. The higher the rolling surplus rate is, the higher the liquid carrying amount of the polyester/cotton blended fabric is, which is favorable for improving the flame retardant performance, but the content of the flame retardant on the fabric is saturated to cause waste, and the higher the baking temperature is, the reaction of the tri (epoxypropyl) isocyanurate, the intumescent flame retardant and the polyester/cotton blended fabric is promoted, but the higher the baking temperature is, the waste is, and the physical performance of the fabric is easily damaged.
The preparation method of the polyester/cotton blended fabric with the flame retardant of the intumescent flame retardant comprises the steps that the polyester/cotton blended fabric is 35/65, 40/60 or 45/55.
The preparation method of the intumescent flame retardant flame-retardant polyester/cotton blended fabric comprises the steps of heating tris (epoxypropyl) isocyanurate to 140-150 ℃, adding pentaerythritol to react for 3-4 hours (140-150 ℃ higher than the melting point of the tris (epoxypropyl) isocyanurate, enabling the tris (epoxypropyl) isocyanurate to be in a liquid state under the temperature condition, facilitating the reaction, enabling the reaction time to be 3-4 hours, enabling the rising of the reaction temperature and the prolonging of the reaction time to facilitate the synthesis reaction, wasting the reaction time to be too high), adding phosphoric acid, continuing the reaction at 105-115 ℃ for 3-4 hours (enabling the rising of the reaction temperature and the prolonging of the reaction time to facilitate the synthesis reaction, wasting the reaction time to be too high), and drying and purifying to obtain the intumescent flame retardant.
According to the preparation method of the intumescent flame retardant flame-retardant polyester/cotton blended fabric, the molar ratio of the tri (epoxypropyl) isocyanurate to the pentaerythritol is 2-2.2:1, epoxy groups of two moles of the tri (epoxypropyl) isocyanurate and two hydroxyl groups of the pentaerythritol are subjected to epoxy ring-opening addition reaction, the molar ratio of the phosphoric acid to the tri (epoxypropyl) isocyanurate is 2-2.3:1, and the residual two epoxy groups and phosphate groups of the tri (epoxypropyl) isocyanurate can be subjected to epoxy ring-opening addition reaction, so that the reaction efficiency is improved due to the fact that the phosphoric acid is slightly excessive, but is wasted due to excessive phosphoric acid.
According to the preparation method of the polyester/cotton blended fabric with the flame retardant of the intumescent flame retardant, after the reaction is finished, the product is dried in vacuum to remove water, then methanol and toluene are used for purification, and the yield of the intumescent flame retardant is 75-79%.
The principle of the invention is as follows:
The invention synthesizes an intumescent flame retardant which contains an acid source, an air source and a carbon source, and the combination of the acid source, the air source and the carbon source can effectively construct the intumescent flame retardant, can solve the problem of nitrogen loss in the high-temperature baking process, and has higher flame retardant property. The tri (epoxypropyl) isocyanurate can be used as a network cross-linking agent, and can be used for generating cross-linking reaction with phosphate radical and hydroxyl radical of the intumescent flame retardant in the baking process, so that the intumescent flame retardant is mutually connected on the surface of the polyester/cotton blended fabric to form a network film structure, the tri (epoxypropyl) isocyanurate can also be used for reacting with hydroxyl radical of cotton fiber, and can be used as a cross-linking agent between the flame retardant and the polyester/cotton blended fabric, so that the network structure of the flame retardant is grafted on the surface of the polyester/cotton blended fabric through covalent bond, and in addition, the ammonium phosphate radical of the intumescent flame retardant is esterified with the hydroxyl radical of the cotton fiber under the action of dicyandiamide catalyst and high temperature. Therefore, the invention constructs a network structure on the surface of the fabric and is fixed on the surface of the polyester/cotton blended fabric through various crosslinking modes, thereby providing high-efficiency durable flame-retardant function.
The beneficial effects are that:
(1) According to the preparation method of the polyester/cotton blended fabric with the flame retardant of the intumescent flame retardant, the phosphorus-containing flame retardant group, the nitrogen-containing heterocycle and the polyol group are combined through covalent bonds to synthesize the flame retardant with three groups as a whole, so that nitrogen loss caused by baking is avoided; in the combustion process, the intumescent flame retardant is favorable for forming intumescent carbon residue on the surface of the polyester/cotton blended fabric, has the effects of isolating heat, oxygen and combustible gas, and has excellent flame retardant property;
(2) According to the preparation method of the polyester/cotton blended fabric with the flame retardant by the intumescent flame retardant, a network structure is constructed on the surface of the fabric and is fixed on the surface of the polyester/cotton blended fabric in a plurality of crosslinking modes, so that the high-efficiency durable flame retardant function is provided;
(3) The polyester/cotton blended fabric with the flame retardant of the intumescent flame retardant has excellent flame retardant effect and better flame retardant durability.
Drawings
FIG. 1 is a 13 C nuclear magnetic resonance spectrum of the intumescent flame retardant of example 1;
FIG. 2 is a schematic diagram of the crosslinking mechanism of intumescent flame retardant on a polyester/cotton blend Fabric, where IFR represents intumescent flame retardant and Fabric represents polyester/cotton blend Fabric.
Detailed Description
The application is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The invention refers to AATCC 61-2006 accelerated test of washing fastness for household and commercial use, which washes the intumescent flame retardant polyester/cotton blended fabric.
The test method adopted by the invention is as follows:
(1) Limiting oxygen index is measured according to GB/T5454-1997 standard of oxygen index method for experimental combustion Performance of textiles;
(2) The damage length is measured according to GB/T5455-2014 standard of measurement of smoldering and continuous burning time of damage length of vertical direction of burning property of textile;
(3) Maximum heat release rate test was performed with reference to ASTM D7309-21 a.
Example 1
A preparation method of a polyester/cotton blended fabric with an intumescent flame retardant comprises the following steps:
(1) Heating tris (epoxypropyl) isocyanurate to 140 ℃ according to the mol ratio of 2:1 of the tris (epoxypropyl) isocyanurate to react with pentaerythritol for 4 hours, adding phosphoric acid according to the mol ratio of 2:1 of the phosphoric acid to the tris (epoxypropyl) isocyanurate, continuing to react for 3 hours at 110 ℃, removing water from the product after the reaction is finished by vacuum drying, and purifying by adopting methanol and toluene to prepare the intumescent flame retardant, wherein the yield of the intumescent flame retardant is 75 percent, and the structural formula is as follows
(2) According to the molar ratio of the tris (epoxypropyl) isocyanurate to the intumescent flame retardant being 2.3:1, the mass of the sodium thiosulfate being 3% of the tris (epoxypropyl) isocyanurate and the mass of the dicyandiamide being 6% of the intumescent flame retardant, dissolving the intumescent flame retardant obtained in the step (1), the tris (epoxypropyl) isocyanurate, the sodium thiosulfate and the dicyandiamide in a mixed solution of water and acetone (the acetone accounts for 25% of the total volume of the water and the acetone), and adjusting the pH value of the solution to 6 by adopting ammonia water to obtain a flame retardant finishing liquid, wherein the concentration of the intumescent flame retardant in the flame retardant finishing liquid is 100g/L;
(3) Immersing the 35/65 polyester/cotton blended fabric into the flame retardant finishing liquid obtained in the step (2) (the crosslinking mechanism is shown in figure 2), and treating the polyester/cotton blended fabric by a padding-baking method, wherein the padding residual rate is controlled to be 100%, the pre-baking temperature is controlled to be 80 ℃, the pre-baking time is controlled to be 2min, the baking temperature is controlled to be 170 ℃ and the baking time is controlled to be 5min, so that the intumescent flame retardant polyester/cotton blended fabric is prepared.
The surface of the prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric is provided with a network flame-retardant film, the network flame-retardant film is formed by connecting an intumescent flame retardant on the surface of the polyester/cotton blended fabric through tri (epoxypropyl) isocyanurate, and the network flame-retardant film and the polyester/cotton blended fabric are bridged through covalent bonds;
The flame retardant performance of the polyester/cotton blended fabric of the intumescent flame retardant is that the limiting oxygen index is 29.8%, the damage length is 11.9cm, no molten drops are generated, the maximum heat release rate is 139.2W/g, and the damage length is 14.6cm after 30 times of washing.
The 13 C nuclear magnetic resonance spectrum of the intumescent flame retardant is shown in FIG. 1. As can be seen from FIG. 1, the chemical shifts at 150.6ppm are due to the carbon atom of the C=O structure on the nitrogen heterocycle, the chemical shifts at 59.2 and 46.2ppm are due to the carbon atom of the C-OH structure of pentaerythritol and the central carbon atom, the chemical shifts at 45.7 and 45.2ppm are due to the carbon atom of the C-N structure attached to the epoxy group, and the chemical shifts at 67.0ppm and 63.9ppm are due to the carbon atoms of the C-O-P and C-OH structures generated after the reaction of the epoxy group in the intumescent flame retardant structure, indicating that the epoxy group is reacted with the phosphate. The chemical shifts at 74.8 and 69.7ppm are caused by the ring-opened carbon atom of the epoxy group in the C-O structure and the pentaerythritol carbon atom, respectively, after the epoxy group has reacted with the pentaerythritol hydroxyl group. The above results indicate that intumescent flame retardants were successfully synthesized.
Comparative example 1
The preparation method of the intumescent flame retardant polyester/cotton blended fabric is basically the same as the embodiment, and is characterized in that the flame retardant solution in the step (2) is prepared by dissolving the intumescent flame retardant obtained in the step (1), sodium thiosulfate and dicyandiamide in a mixed solution of water and acetone (the acetone accounts for 25% of the total volume of the water and the acetone), regulating the pH value of the solution to 6 by adopting ammonia water, and the dosage proportion relation among the intumescent flame retardant, the sodium thiosulfate and the dicyandiamide, the proportion relation between the water and the acetone and the concentration of the flame retardant solution are the same as the embodiment 1. The final flame retardant performance of the intumescent flame retardant polyester/cotton blended fabric is that the limiting oxygen index is 29.3%, the damage length is 12.1cm, no molten drops are generated, the maximum heat release rate is 142.3W/g, and the damage length is 30cm after 5 times of washing.
As can be seen from comparing example 1 with comparative example 1, the flame retardant performance of the flame retardant polyester/cotton blend fabric prepared in comparative example 1 is slightly lower than that of the flame retardant polyester/cotton blend fabric prepared in example 1, while the water washing resistance of the flame retardant polyester/cotton blend fabric prepared in comparative example 1 is remarkably poor, because the intumescent flame retardant in comparative example 1 is simply deposited on the polyester/cotton blend fabric, cannot generate covalent bond with the fabric, cannot be combined with each other on the surface of the polyester/cotton blend fabric to form a network flame retardant film, and is easily washed out in the water washing process, thereby losing the flame retardant effect.
Example 2
A preparation method of a polyester/cotton blended fabric with an intumescent flame retardant comprises the following steps:
(1) Heating tris (epoxypropyl) isocyanurate to 145 ℃ according to the mole ratio of 2.1:1 of the tris (epoxypropyl) isocyanurate to pentaerythritol, adding pentaerythritol for reaction for 3 hours, adding phosphoric acid according to the mole ratio of 2.1:1 of phosphoric acid to the tris (epoxypropyl) isocyanurate, continuing to react for 3 hours at 115 ℃, removing water from the product after the reaction, and purifying by adopting methanol and toluene to obtain the intumescent flame retardant, wherein the yield of the intumescent flame retardant is 76 percent, and the structural formula is as follows
(2) According to the molar ratio of the tris (epoxypropyl) isocyanurate to the intumescent flame retardant being 3:1, the mass of the sodium thiosulfate being 3.5% of the tris (epoxypropyl) isocyanurate and the mass of the dicyandiamide being 7% of the intumescent flame retardant, dissolving the intumescent flame retardant obtained in the step (1), the tris (epoxypropyl) isocyanurate, the sodium thiosulfate and the dicyandiamide in a mixed solution of water and acetone (the acetone accounts for 30% of the total volume of the water and the acetone), and regulating the pH value of the solution to 6.2 by adopting ammonia water to obtain a flame retardant finishing liquid, wherein the concentration of the intumescent flame retardant in the flame retardant finishing liquid is 200g/L;
(3) Immersing 40/60 of the polyester/cotton blended fabric into the flame-retardant finishing liquid obtained in the step (2), and treating the polyester/cotton blended fabric by a padding-baking method, wherein the padding surplus rate is controlled to be 110%, the pre-baking temperature is controlled to be 78 ℃, the pre-baking time is controlled to be 3min, the baking temperature is controlled to be 160 ℃, and the baking time is controlled to be 8min, so that the intumescent flame retardant flame-retardant polyester/cotton blended fabric is prepared.
The surface of the prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric is provided with a network flame-retardant film, the network flame-retardant film is formed by connecting an intumescent flame retardant on the surface of the polyester/cotton blended fabric through tri (epoxypropyl) isocyanurate, and the network flame-retardant film and the polyester/cotton blended fabric are bridged through covalent bonds;
the flame retardant performance of the polyester/cotton blended fabric of the intumescent flame retardant is that the limiting oxygen index is 33.5%, the damage length is 8.3cm, no molten drops are generated, the maximum heat release rate is 121.3W/g, and the damage length is 12.5cm after 30 times of washing.
Example 3
A preparation method of a polyester/cotton blended fabric with an intumescent flame retardant comprises the following steps:
(1) Heating tris (epoxypropyl) isocyanurate to 150 ℃ according to the mole ratio of 2.1:1 of the tris (epoxypropyl) isocyanurate to be added into pentaerythritol for reaction for 3.5 hours, adding phosphoric acid according to the mole ratio of 2.2:1 of phosphoric acid to the tris (epoxypropyl) isocyanurate, continuing to react for 4 hours at 105 ℃, removing water from the product after the reaction, and purifying by adopting methanol and toluene to prepare the intumescent flame retardant, wherein the yield of the intumescent flame retardant is 76 percent, and the structural formula is as follows
(2) According to the molar ratio of the tri (epoxypropyl) isocyanurate to the intumescent flame retardant being 2:1, the mass of the sodium thiosulfate being 4% of the tri (epoxypropyl) isocyanurate and the mass of the dicyandiamide being 5% of the intumescent flame retardant, dissolving the intumescent flame retardant obtained in the step (1), the tri (epoxypropyl) isocyanurate, the sodium thiosulfate and the dicyandiamide in a mixed solution of water and acetone (the acetone accounts for 20% of the total volume of the water and the acetone), and regulating the pH value of the solution to 6.5 by adopting ammonia water to obtain a flame retardant finishing liquid, wherein the concentration of the intumescent flame retardant in the flame retardant finishing liquid is 120g/L;
(3) Immersing 45/55 of the polyester/cotton blended fabric into the flame-retardant finishing liquid obtained in the step (2), and treating the polyester/cotton blended fabric by a padding-baking method, wherein the padding redundancy is controlled to be 105%, the pre-baking temperature is controlled to be 76 ℃, the pre-baking time is controlled to be 4min, the baking temperature is controlled to be 165 ℃, and the baking time is controlled to be 6min, so that the intumescent flame retardant flame-retardant polyester/cotton blended fabric is prepared.
The surface of the prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric is provided with a network flame-retardant film, the network flame-retardant film is formed by connecting an intumescent flame retardant on the surface of the polyester/cotton blended fabric through tri (epoxypropyl) isocyanurate, and the network flame-retardant film and the polyester/cotton blended fabric are bridged through covalent bonds;
The flame retardant performance of the polyester/cotton blended fabric of the intumescent flame retardant is that the limiting oxygen index is 30.5%, the damage length is 11.1cm, no molten drops are generated, the maximum heat release rate is 133W/g, and the damage length is 14cm after 30 times of washing.
Example 4
A preparation method of a polyester/cotton blended fabric with an intumescent flame retardant comprises the following steps:
(1) Heating tris (epoxypropyl) isocyanurate to 145 ℃ according to the mole ratio of 2.2:1 of the tris (epoxypropyl) isocyanurate to pentaerythritol, adding pentaerythritol to react for 3.5 hours, adding phosphoric acid according to the mole ratio of 2.2:1 of phosphoric acid to the tris (epoxypropyl) isocyanurate, continuing to react for 4 hours at 108 ℃, removing water from the product after the reaction, and purifying by adopting methanol and toluene to obtain the intumescent flame retardant, wherein the yield of the intumescent flame retardant is 76 percent, and the structural formula is
(2) According to the molar ratio of the tri (epoxypropyl) isocyanurate to the intumescent flame retardant being 2.8:1, the mass of the sodium thiosulfate being 4.5% of that of the tri (epoxypropyl) isocyanurate and the mass of the dicyandiamide being 5.5% of that of the intumescent flame retardant, the intumescent flame retardant obtained in the step (1), the tri (epoxypropyl) isocyanurate, the sodium thiosulfate and the dicyandiamide are dissolved in a mixed solution of water and acetone (the acetone occupies 22% of the total volume of the water and the acetone), ammonia water is adopted to adjust the pH value of the solution to 6.8, so that a flame retardant finishing liquid is obtained, and the concentration of the intumescent flame retardant in the flame retardant finishing liquid is 180g/L;
(3) Immersing the 35/65 polyester/cotton blended fabric into the flame-retardant finishing liquid obtained in the step (2), and treating the polyester/cotton blended fabric by a padding-baking method, wherein the padding surplus rate is controlled to be 105%, the pre-baking temperature is controlled to be 75 ℃, the pre-baking time is controlled to be 4min, the baking temperature is controlled to be 168 ℃, and the baking time is controlled to be 7min, so that the intumescent flame retardant flame-retardant polyester/cotton blended fabric is prepared.
The surface of the prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric is provided with a network flame-retardant film, the network flame-retardant film is formed by connecting an intumescent flame retardant on the surface of the polyester/cotton blended fabric through tri (epoxypropyl) isocyanurate, and the network flame-retardant film and the polyester/cotton blended fabric are bridged through covalent bonds;
The flame retardant performance of the polyester/cotton blended fabric of the intumescent flame retardant is that the limiting oxygen index is 32.8%, the damage length is 8.9cm, no molten drops are generated, the maximum heat release rate is 124.1W/g, and the damage length is 12.8cm after 30 times of washing.
Example 5
A preparation method of a polyester/cotton blended fabric with an intumescent flame retardant comprises the following steps:
(1) Heating tris (epoxypropyl) isocyanurate to 145 ℃ according to the mole ratio of 2.2:1 of the tris (epoxypropyl) isocyanurate to pentaerythritol, adding pentaerythritol for reaction for 4 hours, adding phosphoric acid according to the mole ratio of 2.3:1 of phosphoric acid to the tris (epoxypropyl) isocyanurate, continuing to react for 3.5 hours at 110 ℃, removing water from the product after the reaction, and purifying by adopting methanol and toluene to obtain the intumescent flame retardant, wherein the yield of the intumescent flame retardant is 79%, and the structural formula is as follows
(2) According to the molar ratio of tris (epoxypropyl) isocyanurate to intumescent flame retardant being 2.6:1, the mass of sodium thiosulfate being 4.8% of tris (epoxypropyl) isocyanurate and the mass of dicyandiamide being 6% of intumescent flame retardant, dissolving the intumescent flame retardant obtained in the step (1), tris (epoxypropyl) isocyanurate, sodium thiosulfate and dicyandiamide in a mixed solution of water and acetone (the acetone accounts for 25% of the total volume of water and acetone), regulating the pH value of the solution to 6.6 by adopting ammonia water to obtain a flame retardant finishing solution, wherein the concentration of the intumescent flame retardant in the flame retardant finishing solution is 150g/L;
(3) Immersing 40/60 of the polyester/cotton blended fabric into the flame-retardant finishing liquid obtained in the step (2), and treating the polyester/cotton blended fabric by a padding-baking method, wherein the padding surplus rate is controlled to be 108%, the pre-baking temperature is controlled to be 72 ℃, the pre-baking time is controlled to be 2min, the baking temperature is controlled to be 165 ℃, and the baking time is controlled to be 6min, so that the intumescent flame retardant flame-retardant polyester/cotton blended fabric is prepared.
The surface of the prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric is provided with a network flame-retardant film, the network flame-retardant film is formed by connecting an intumescent flame retardant on the surface of the polyester/cotton blended fabric through tri (epoxypropyl) isocyanurate, and the network flame-retardant film and the polyester/cotton blended fabric are bridged through covalent bonds;
the flame retardant performance of the polyester/cotton blended fabric of the intumescent flame retardant is 31.4% of limiting oxygen index, 10.5cm of damage length, no generation of molten drops, 128.3W/g of maximum heat release rate and 13.2cm of damage length after 30 times of washing.
Example 6
A preparation method of a polyester/cotton blended fabric with an intumescent flame retardant comprises the following steps:
(1) Heating tris (epoxypropyl) isocyanurate to 145 ℃ according to the mole ratio of 2.2:1 of the tris (epoxypropyl) isocyanurate to pentaerythritol, adding pentaerythritol for reaction for 3 hours, adding phosphoric acid according to the mole ratio of 2.3:1 of phosphoric acid to the tris (epoxypropyl) isocyanurate, continuing to react for 3.5 hours at 112 ℃, removing water from the product after the reaction, and purifying by adopting methanol and toluene to obtain the intumescent flame retardant, wherein the yield of the intumescent flame retardant is 78%, and the structural formula is
(2) According to the molar ratio of the tris (epoxypropyl) isocyanurate to the intumescent flame retardant being 2.5:1, the mass of the sodium thiosulfate being 5% of that of the tris (epoxypropyl) isocyanurate and the mass of the dicyandiamide being 6.5% of that of the intumescent flame retardant, the intumescent flame retardant obtained in the step (1), the tris (epoxypropyl) isocyanurate, the sodium thiosulfate and the dicyandiamide are dissolved in a mixed solution of water and acetone (the acetone occupies 28% of the total volume of the water and the acetone), ammonia water is adopted to adjust the pH value of the solution to 7, so that a flame retardant finishing liquid is obtained, and the concentration of the intumescent flame retardant in the flame retardant finishing liquid is 160g/L;
(3) Immersing 45/55 polyester/cotton blended fabric into the flame retardant finishing liquid obtained in the step (2), and treating the polyester/cotton blended fabric by a padding-baking method, wherein the padding surplus rate is controlled to be 102%, the pre-baking temperature is controlled to be 70 ℃, the pre-baking time is controlled to be 3min, the baking temperature is controlled to be 162 ℃, and the baking time is controlled to be 6min, so that the intumescent flame retardant polyester/cotton blended fabric is prepared.
The surface of the prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric is provided with a network flame-retardant film, the network flame-retardant film is formed by connecting an intumescent flame retardant on the surface of the polyester/cotton blended fabric through tri (epoxypropyl) isocyanurate, and the network flame-retardant film and the polyester/cotton blended fabric are bridged through covalent bonds;
The flame retardant performance of the polyester/cotton blended fabric of the intumescent flame retardant is 31.9% of limiting oxygen index, 9.9cm of damage length, no generation of molten drops, 126.8W/g of maximum heat release rate and 13.1cm of damage length after 30 times of washing.
Claims (10)
1. The intumescent flame retardant polyester/cotton blended fabric is characterized in that a network flame retardant film is arranged on the surface of the intumescent flame retardant polyester/cotton blended fabric, and the network flame retardant film and the polyester/cotton blended fabric are bridged through a covalent bond;
the network flame-retardant film is formed by connecting an intumescent flame retardant on the surface of a polyester/cotton blended fabric through tri (epoxypropyl) isocyanurate;
the structural formula of the intumescent flame retardant is
2. The intumescent flame retardant polyester/cotton blend fabric is characterized in that the flame retardant performance of the intumescent flame retardant polyester/cotton blend fabric is that the limiting oxygen index is 29.8% -33.5%, the damage length is 11.9-8.3 cm, no molten drops are generated, the maximum heat release rate is 121.3-139.2W/g, and the damage length is not higher than 14.6cm after 30 times of washing.
3. The preparation method of the intumescent flame retardant polyester/cotton blend fabric as claimed in claim 1 or 2, which is characterized in that the polyester/cotton blend fabric is immersed in flame retardant finishing liquid, and is treated by padding-baking method to prepare the intumescent flame retardant polyester/cotton blend fabric;
the flame-retardant finishing liquid is prepared by dissolving an intumescent flame retardant, tris (epoxypropyl) isocyanurate, sodium thiosulfate and dicyandiamide in a mixed liquid of water and acetone, and regulating the pH value of the solution to 6-7 by adopting ammonia water.
4. The method for preparing the intumescent flame retardant polyester/cotton blended fabric according to claim 3, wherein the concentration of the intumescent flame retardant in the flame retardant finishing liquid is 100-200 g/L.
5. The preparation method of the intumescent flame retardant polyester/cotton blended fabric is characterized in that the molar ratio of tri (epoxypropyl) isocyanurate to the intumescent flame retardant is 2-3:1, acetone accounts for 20% -30% of the total volume of water and acetone, sodium thiosulfate accounts for 3-5% of the mass of the tri (epoxypropyl) isocyanurate, and dicyandiamide accounts for 5-7% of the mass of the intumescent flame retardant.
6. The method for preparing the intumescent flame retardant polyester/cotton blend fabric as claimed in claim 5, characterized in that,
The padding-baking process parameters are that the padding residual rate is 100-110%, the pre-baking temperature is 70-80 ℃ and the pre-baking time is 2-4 min;
the baking temperature is 160-170 ℃ and the baking time is 5-8 min.
7. The method for preparing a polyester/cotton blend fabric flame retardant by an intumescent flame retardant as claimed in claim 6, wherein the polyester/cotton blend fabric is a polyester/cotton blend fabric of 35/65, 40/60 or 45/55.
8. The preparation method of the intumescent flame retardant polyester/cotton blended fabric according to claim 3 is characterized in that the intumescent flame retardant is prepared by heating tris (epoxypropyl) isocyanurate to 140-150 ℃, adding pentaerythritol to react for 3-4 hours, adding phosphoric acid, continuing to react for 3-4 hours at 105-115 ℃, drying and purifying.
9. The preparation method of the intumescent flame retardant polyester/cotton blended fabric is characterized in that the molar ratio of tri (epoxypropyl) isocyanurate to pentaerythritol is 2-2.2:1, and the molar ratio of phosphoric acid to tri (epoxypropyl) isocyanurate is 2-2.3:1.
10. The method for preparing the intumescent flame retardant polyester/cotton blended fabric according to claim 8, wherein the yield of the intumescent flame retardant is 75-79%.
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