CN112831863B - Flame-retardant polyester fiber and preparation process thereof - Google Patents
Flame-retardant polyester fiber and preparation process thereof Download PDFInfo
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- CN112831863B CN112831863B CN202110253948.8A CN202110253948A CN112831863B CN 112831863 B CN112831863 B CN 112831863B CN 202110253948 A CN202110253948 A CN 202110253948A CN 112831863 B CN112831863 B CN 112831863B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
Abstract
The invention relates to the technical field of fiber preparation, in particular to a flame-retardant polyester fiber and a preparation process thereof, wherein the flame-retardant polyester fiber is prepared from the following raw materials in parts by weight: 70-80 parts of terylene slice, 18-30 parts of flame-retardant master batch and 2.0-5.0 parts of anti-dripping agent; the flame-retardant master batch comprises the following raw materials in parts by weight: 14 to 18 parts of composite flame retardant, 4 to 6 parts of synergistic flame retardant, 3 to 7 parts of urea, 0.2 to 0.3 part of nano titanium dioxide, 0.25 to 0.4 part of nano bamboo charcoal powder, 1.5 to 2.0 parts of antioxidant, 0.3 to 0.5 part of calcium stearate, 3.0 to 3.6 parts of ethylene bis fatty acid amide, 0.15 to 0.25 part of isopropyl tri (dioctyl pyrophosphato acyloxy) titanate and 65 to 75 parts of polyester chips; compared with the flame-retardant polyester fiber prepared by the traditional process, the prepared flame-retardant polyester fiber has better flame-retardant property and better flame-retardant effect under the synergistic action of the composite flame retardant and the synergistic flame retardant.
Description
Technical Field
The invention relates to the technical field of fiber preparation, in particular to a flame-retardant polyester fiber and a preparation process thereof.
Background
The polyester fiber is a synthetic fiber composed of a polyester linear macromolecule produced by polycondensation of a diol and a dibasic acid or an omega-hydroxy acid. In recent years, polyester fibers have been widely studied, but they are not widely used in industrial applications. At present, the polyester fiber produced in large-scale industrialization is prepared by taking polyethylene terephthalate as a raw material, the polyester fiber can also be called PET fiber according to English abbreviation of the raw material, and the trade name of China is terylene. Polyester fibers are the latest but the fastest growing among the three major synthetic fibers (polyester, polyamide, polyacrylonitrile). Since 90% or more of polyester fibers are PET fibers, polyester fibers are mostly PET fibers.
Because the polyester fiber has the advantages of fastness, durability, wrinkle resistance, easy ironing and no hair sticking. Therefore, the fabric is mainly used for clothes and interior decoration, and has the greatest advantages of good crease resistance and shape retention, high strength and high elastic recovery capability.
Although the polyester fiber product prepared by the prior art has good crease resistance and elastic recovery capability, the flame retardant property of the polyester fiber product is relatively poor. Which in case of fire is likely to cause immeasurable damage to people's life and property. Therefore, it is an urgent technical problem to be solved by those skilled in the art to provide a flame retardant polyester fiber and a preparation process thereof.
Disclosure of Invention
Compared with the flame-retardant polyester fiber prepared by the traditional process, the flame-retardant polyester fiber prepared by the invention has better flame-retardant property and better flame-retardant effect under the synergistic action of the composite flame retardant and the synergistic flame retardant.
In order to achieve the purpose, the invention provides the following technical scheme:
the flame-retardant polyester fiber is prepared from the following raw materials in parts by weight: 70-80 parts of terylene slice, 18-30 parts of flame-retardant master batch and 2.0-5.0 parts of anti-dripping agent;
the flame-retardant master batch comprises the following raw materials in parts by weight: 14 to 18 parts of composite flame retardant, 4 to 6 parts of synergistic flame retardant, 3 to 7 parts of urea, 0.2 to 0.3 part of nano titanium dioxide, 0.25 to 0.4 part of nano bamboo charcoal powder, 1.5 to 2.0 parts of antioxidant, 0.3 to 0.5 part of calcium stearate, 3.0 to 3.6 parts of ethylene bis fatty acid amide, 0.15 to 0.25 part of isopropyl tri (dioctyl pyrophosphato acyloxy) titanate and 65 to 75 parts of polyester chips.
Still further, the preparation method of the composite flame retardant comprises the following steps:
1. preparing a porous nano material;
adding a proper amount of nano-scale sodium-based montmorillonite into a water glass solution with the mass of 8-12 times and the concentration of 15-35%, then adding 5-8% of sodium bicarbonate into the water glass solution, mechanically stirring for 80-100 min, and raising the temperature of the obtained mixed components to 55-65 ℃; dispersing for 1-2 h by ultrasonic, stirring at the speed of 30-50 r/min, and slowly adding dilute hydrochloric acid solution to naturally precipitate the obtained mixture under the conditions that the pH value is 4.8-5.5 and the temperature is 55-65 ℃; when no flocculent precipitate or bubbles are generated, filtering the obtained mixture, drying the obtained filter material in vacuum to constant weight, and sieving by a grinder to obtain a finished product of the porous nano material;
2. modification of porous nano materials;
weighing a proper amount of 60-75% aqueous solution of ethanol, respectively adding 0.8-1.5% by mass of sodium dodecyl benzene sulfonate and 15-18% by mass of nano zinc borate into the aqueous solution, ultrasonically dispersing for 10-15 min, then adding 8-12% by mass of porous nano material and 20-30% by mass of 3-aminopropyltriethoxysilane into the aqueous solution of ethanol, ultrasonically dispersing for 20-30 min, and heating, stirring and mixing for 8-15 h under the protection of nitrogen; after the reaction is finished, the obtained reaction product is subjected to suction filtration and drying treatment, then is extracted for 32-45 h by using absolute ethyl alcohol, and then is subjected to vacuum drying, so that the modification of the porous nano material is finished.
Furthermore, the preparation method of the nano zinc borate comprises the following steps: mixing zinc sulfate solution with the concentration of 1.2-2.0 mol/L and sodium hydroxide solution with the concentration of 2.5-4.0 mol/L in equal volume, and ultrasonically stirring the obtained mixed solution at the temperature of 45-60 ℃ for 30-45 min; after the reaction is finished, weighing a proper amount of treated reaction liquid, respectively adding 3.5-5.0% by mass of boric acid and 0.3-0.5% by mass of Span80 into the reaction liquid, and performing ultrasonic stirring for 30-40 min at the constant temperature of 50-60 ℃; after the reaction is finished, centrifuging, collecting the obtained precipitate, washing the precipitate for 2 to 4 times by using deionized water, and drying the precipitate to obtain the finished product of the nano zinc borate.
Furthermore, the reaction solution treatment method comprises the following steps: and adding a proper amount of deionized water into the reaction liquid obtained after the reaction is finished so as to adjust the content of the zinc hydroxide in the reaction liquid to be 0.4-0.6 mol/L.
Further, the preparation method of the synergistic flame retardant comprises the following steps: respectively adding 5-8 wt% of nano antimony trioxide and 0.8-1.5 wt% of fatty glyceride into a proper amount of microcrystalline cellulose solution, and ultrasonically mixing for 10-20 min; and then carrying out electrostatic spraying on the obtained suspension to obtain the solid microspheres, namely the finished product of the synergistic flame retardant.
Further, the preparation method of the microcrystalline cellulose solution comprises the following steps: at the temperature of 65-80 ℃, adding a proper amount of microcrystalline cellulose into chlorinated 1-methyl 3-butylimidazolium salt ionic liquid with the mass of 10-20 times of that of the microcrystalline cellulose, and performing ultrasonic dissolution to obtain a finished product of a microcrystalline cellulose solution.
Furthermore, the anti-dropping agent is triallyl isocyanurate with the average grain diameter of 2-4 mu m.
Furthermore, the antioxidant is any one of antioxidant B215, antioxidant 1010 and antioxidant 168.
A preparation process of flame-retardant polyester fibers comprises the following steps:
s1, weighing a proper amount of polyester chips and flame-retardant master batches according to the formula amount; then respectively placing the weighed terylene slices and the flame-retardant master batch into a vacuum drying oven for drying treatment; drying the flame-retardant master batch until the water content is less than or equal to 180ppm, drying the terylene slices until the water content is less than or equal to 40ppm, and storing the dried terylene slices and the flame-retardant master batch for later use;
s2, putting the dried terylene slices and the flame-retardant master batches into a high-speed stirrer, slowly adding an anti-dropping agent into the mixture, and fully mixing the mixture in the high-speed stirrer; then feeding the obtained mixed material into a screw extruder for melt extrusion;
s3, spinning and forming the melt extruded by the screw extruder through a spinneret plate of a spinning assembly at a spinning speed of 220-240 m/min and a winding speed of 720-950 m/min, and performing heat setting at the temperature of 170-190 ℃ to obtain a flame-retardant polyester fiber crude product;
s4, carrying out irradiation treatment on the obtained flame-retardant polyester fiber crude product on a high-energy electron accelerator of 2.5-10 MeV; and obtaining the durable halogen-free flame-retardant anti-dripping polyester fiber after the treatment.
Furthermore, during the irradiation treatment, the irradiation dose is 80-200 kGy, and the irradiation time is 20-30 min.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes nano-scale sodium-based montmorillonite, water glass solution, sodium bicarbonate and the like as raw materials, fully disperses all the raw materials through ultrasonic dispersion, and then carries out treatment of various working procedures such as natural precipitation and the like to finally prepare the porous nano material which is composed of the nano-scale sodium-based montmorillonite and silicon dioxide and has larger specific surface area. Then soaking the prepared empty nano material in ethanol solution containing nano zinc borate and sodium dodecyl benzene sulfonate, and enabling the nano zinc borate to be effectively filled in a porous structure on the surface of the porous nano material through ultrasonic dispersion treatment. And finally, adding 3-aminopropyltriethoxysilane into the ethanol solution, performing ultrasonic dispersion treatment on the ethanol solution to enable related functional groups in the 3-aminopropyltriethoxysilane to chemically react with hydroxyl radicals on the surface of the porous nano material to form bonds, and effectively fixing the nano zinc borate through a three-dimensional network structure formed by the 3-aminopropyltriethoxysilane on the surface and in holes of the porous nano material. The finally prepared composite flame retardant not only has the flame retardant performance of the nano zinc borate, but also has the flame retardant effect of the sodium montmorillonite, so that the composite flame retardant has better flame retardant performance compared with the traditional flame retardant. Meanwhile, the paint also has certain water resistance and durability. In addition, the silane coupling agent is used, so that the compatibility between the prepared composite flame retardant and the terylene is further enhanced.
In addition, the microcrystalline cellulose solution, the nano antimony trioxide and the fatty glyceride are used as raw materials for preparing the synergistic flame retardant, and the solid microspheres taking the nano antimony trioxide as the core and the microcrystalline cellulose as the shell are finally prepared through processes such as ultrasonic mixing, electrostatic spraying and the like, namely the synergistic flame retardant. And the microcrystalline cellulose has a porous structure, and is used as a carbon source to easily form an expanded carbon layer, so that the effective range of isolation and flame retardance is enlarged. The flame retardant property of the prepared synergistic flame retardant is further improved under the synergistic action of the nano antimony trioxide and the microcrystalline cellulose.
In conclusion, under the synergistic action of the composite flame retardant and the synergistic flame retardant, the flame-retardant polyester fiber prepared by the invention has more excellent flame-retardant performance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The flame-retardant polyester fiber is prepared from the following raw materials in parts by weight: 70 parts of polyester chips, 18 parts of flame-retardant master batches and 2.0 parts of anti-dripping agents;
the flame-retardant master batch comprises the following raw materials in parts by weight: 14 parts of composite flame retardant, 4 parts of synergistic flame retardant, 3 parts of urea, 0.2 part of nano titanium dioxide, 0.25 part of nano bamboo charcoal powder, 1.5 parts of antioxidant, 0.3 part of calcium stearate, 3.0 parts of ethylene bis fatty acid amide, 0.15 part of isopropyl tri (dioctyl pyrophosphato acyloxy) titanate and 65 parts of polyester chips.
The preparation method of the composite flame retardant comprises the following steps:
1. preparing a porous nano material;
adding a proper amount of nano-scale sodium-based montmorillonite into a water glass solution with the mass of 8 times and the concentration of 15%, then adding sodium bicarbonate with the mass of 5% into the water glass solution, mechanically stirring for 80min, and raising the temperature of the obtained mixed components to 55 ℃; dispersing for 1h by ultrasonic, stirring at 30r/min, and slowly adding dilute hydrochloric acid solution to obtain mixture, and naturally precipitating at 55 deg.C and pH of 4.8; when no flocculent precipitate or bubbles are generated, filtering the obtained mixture, drying the obtained filter material in vacuum to constant weight, and sieving by a grinder to obtain a finished product of the porous nano material;
2. modification of porous nano materials;
weighing a proper amount of 60% ethanol water solution, respectively adding 0.8% sodium dodecyl benzene sulfonate and 15% nano zinc borate by mass into the ethanol water solution, ultrasonically dispersing for 10min, then adding 8% porous nano material and 20% 3-aminopropyltriethoxysilane by mass into the ethanol water solution, ultrasonically dispersing for 20min, and heating, stirring and mixing for 8h under the protection of nitrogen; after the reaction is finished, the obtained reaction product is subjected to suction filtration and drying treatment, then is extracted for 32 hours by using absolute ethyl alcohol, and then is subjected to vacuum drying, so that the modification of the porous nano material is finished.
The preparation method of the nano zinc borate comprises the following steps: mixing zinc sulfate solution with concentration of 1.2mol/L and sodium hydroxide solution with concentration of 2.5mol/L in equal volume, and ultrasonically stirring the obtained mixed solution at the temperature of 45 ℃ for 30min; after the reaction is finished, weighing a proper amount of treated reaction liquid, respectively adding 3.5% by mass of boric acid and 0.3% by mass of Span80 into the reaction liquid, and ultrasonically stirring the mixture for 30min at a constant temperature of 50 ℃; after the reaction is finished, centrifuging, collecting the obtained precipitate, washing the precipitate for 2 times by using deionized water, and drying the precipitate to obtain the finished product of the nano zinc borate.
The reaction solution treatment method comprises the following steps: and adding a proper amount of deionized water into the reaction liquid obtained after the reaction is finished so as to adjust the content of the zinc hydroxide in the reaction liquid to 0.4mol/L.
The preparation method of the synergistic flame retardant comprises the following steps: respectively adding 5wt% of nano antimony trioxide and 0.8 wt% of fatty glyceride into a proper amount of microcrystalline cellulose solution, and ultrasonically mixing for 10 min; and then carrying out electrostatic spraying on the obtained suspension to obtain the solid microspheres, namely the finished product of the synergistic flame retardant.
The preparation method of the microcrystalline cellulose solution comprises the following steps: at the temperature of 65 ℃, adding a proper amount of microcrystalline cellulose into 10 times of chlorinated 1-methyl 3-butylimidazolium salt ionic liquid, and carrying out ultrasonic dissolution to obtain a finished product of a microcrystalline cellulose solution.
The anti-dripping agent is triallyl isocyanurate with an average particle size of 2 mu m.
The antioxidant is antioxidant B215.
A preparation process of flame-retardant polyester fibers comprises the following steps:
s1, weighing a proper amount of polyester chips and flame-retardant master batches according to the formula amount; then respectively placing the weighed terylene slices and the flame-retardant master batch into a vacuum drying oven for drying treatment; drying the flame-retardant master batch until the water content is 180ppm, drying the terylene slices until the water content is 40ppm, and storing the dried terylene slices and the flame-retardant master batch for later use;
s2, putting the dried polyester chips and the flame-retardant master batches into a high-speed stirrer, slowly adding an anti-dripping agent into the high-speed stirrer, and fully mixing the anti-dripping agent and the flame-retardant master batches in the high-speed stirrer; then feeding the obtained mixed material into a screw extruder for melt extrusion;
s3, spinning and forming the melt extruded by the screw extruder through a spinneret plate of a spinning assembly at a spinning speed of 220m/min and a winding speed of 720m/min, and performing heat setting at 170 ℃ to obtain a flame-retardant polyester fiber crude product;
s4, carrying out irradiation treatment on the obtained flame-retardant polyester fiber crude product on a 2.5MeV high-energy electron accelerator; and after the treatment is finished, obtaining the durable halogen-free flame-retardant anti-dripping polyester fiber.
During irradiation treatment, the irradiation dose is 80kGy, and the irradiation time is 20min.
Example 2
The flame-retardant polyester fiber is prepared from the following raw materials in parts by weight: 75 parts of polyester chips, 25 parts of flame-retardant master batch and 3.5 parts of anti-dripping agent;
the flame-retardant master batch comprises the following raw materials in parts by weight: 16 parts of composite flame retardant, 5 parts of synergistic flame retardant, 4 parts of urea, 0.25 part of nano titanium dioxide, 0.35 part of nano bamboo charcoal powder, 1.8 parts of antioxidant, 0.4 part of calcium stearate, 3.3 parts of ethylene bis fatty acid amide, 0.20 part of isopropyl tri (dioctyl pyrophosphato acyloxy) titanate and 70 parts of polyester chip.
The preparation method of the composite flame retardant comprises the following steps:
1. preparing a porous nano material;
adding a proper amount of nano-scale sodium-based montmorillonite into a water glass solution with the mass being 10 times that of the nano-scale sodium-based montmorillonite and the concentration being 25%, then adding sodium bicarbonate with the mass being 6% of that of the nano-scale sodium-based montmorillonite into the water glass solution, mechanically stirring for 90min, and then raising the temperature of the obtained mixed components to 60 ℃; dispersing for 1.5h by ultrasonic, stirring at 40r/min, and slowly adding dilute hydrochloric acid solution to obtain mixture, and naturally precipitating at 60 deg.C and pH of 5.2; when no flocculent precipitate or bubbles are generated, filtering the obtained mixture, drying the obtained filter material in vacuum to constant weight, and sieving by a grinder to obtain a finished product of the porous nano material;
2. modification of porous nano materials;
weighing a proper amount of ethanol water solution with the concentration of 70%, respectively adding 1.2% by mass of sodium dodecyl benzene sulfonate and 16% by mass of nano zinc borate into the ethanol water solution, performing ultrasonic dispersion for 10min, then adding 10% by mass of porous nano material and 25% by mass of 3-aminopropyltriethoxysilane into the ethanol water solution, performing ultrasonic dispersion for 25min, and heating, stirring and mixing for 10h under the protection of nitrogen; after the reaction is finished, the obtained reaction product is subjected to suction filtration and drying treatment, then is extracted for 40 hours by using absolute ethyl alcohol, and then is subjected to vacuum drying, so that the modification of the porous nano material is completed.
The preparation method of the nano zinc borate comprises the following steps: mixing zinc sulfate solution with concentration of 1.6mol/L and sodium hydroxide solution with concentration of 3.2mol/L in equal volume, and performing ultrasonic stirring on the obtained mixed solution at the temperature of 55 ℃ for 40min; after the reaction is finished, weighing a proper amount of treated reaction liquid, respectively adding 4.0% by mass of boric acid and 0.4% by mass of Span80 into the reaction liquid, and ultrasonically stirring the mixture for 35min at the constant temperature of 55 ℃; after the reaction is finished, centrifuging, collecting the obtained precipitate, washing the precipitate for 3 times by using deionized water, and drying the precipitate to obtain the finished product of the nano zinc borate.
The reaction solution treatment method comprises the following steps: and adding a proper amount of deionized water into the reaction liquid obtained after the reaction is finished so as to adjust the content of the zinc hydroxide in the reaction liquid to 0.5mol/L.
The preparation method of the synergistic flame retardant comprises the following steps: respectively adding 6wt% of nano antimony trioxide and 1.2 wt% of fatty glyceride into a proper amount of microcrystalline cellulose solution, and ultrasonically mixing for 15 min; and then carrying out electrostatic spraying on the obtained suspension to obtain the solid microspheres, namely the finished product of the synergistic flame retardant.
The preparation method of the microcrystalline cellulose solution comprises the following steps: at the temperature of 75 ℃, adding a proper amount of microcrystalline cellulose into a chlorinated 1-methyl 3-butylimidazolium salt ionic liquid with the mass 15 times of that of the microcrystalline cellulose, and carrying out ultrasonic dissolution to obtain a finished product of a microcrystalline cellulose solution.
The anti-dripping agent is triallyl isocyanurate with an average particle size of 3 mu m.
The antioxidant is antioxidant 1010.
The preparation process of the flame-retardant polyester fiber is the same as that of example 1.
Example 3
The flame-retardant polyester fiber is prepared from the following raw materials in parts by weight: 80 parts of polyester chips, 30 parts of flame-retardant master batches and 5.0 parts of anti-dripping agents;
the flame-retardant master batch comprises the following raw materials in parts by weight: 18 parts of composite flame retardant, 6 parts of synergistic flame retardant, 7 parts of urea, 0.3 part of nano titanium dioxide, 0.4 part of nano bamboo charcoal powder, 2.0 parts of antioxidant, 0.5 part of calcium stearate, 3.6 parts of ethylene bis fatty acid amide, 0.25 part of isopropyl tri (dioctyl pyrophosphato acyloxy) titanate and 75 parts of polyester chip.
The preparation method of the composite flame retardant comprises the following steps:
1. preparing a porous nano material;
adding a proper amount of nano-scale sodium-based montmorillonite into a water glass solution with the mass being 12 times that of the nano-scale sodium-based montmorillonite and the concentration being 35%, then adding sodium bicarbonate with the mass being 8% of that of the nano-scale sodium-based montmorillonite into the water glass solution, mechanically stirring for 100min, and then raising the temperature of the obtained mixed components to 65 ℃; dispersing for 2h by ultrasonic, stirring at 50r/min, and slowly adding dilute hydrochloric acid solution to obtain mixture, and naturally precipitating at 65 deg.C and pH of 5.5; when no flocculent precipitate or bubbles are generated, filtering the obtained mixture, drying the obtained filter material in vacuum to constant weight, and sieving by a grinder to obtain a finished product of the porous nano material;
2. modification of porous nano materials;
weighing a proper amount of 75% ethanol aqueous solution, respectively adding 1.5% sodium dodecyl benzene sulfonate and 18% nano zinc borate by mass into the ethanol aqueous solution, ultrasonically dispersing for 15min, then adding 12% porous nano material and 30% 3-aminopropyltriethoxysilane by mass into the ethanol aqueous solution, ultrasonically dispersing for 30min, and heating, stirring and mixing for 15h under the protection of nitrogen; after the reaction is finished, the obtained reaction product is subjected to suction filtration and drying treatment, then is extracted for 45 hours by using absolute ethyl alcohol, and then is subjected to vacuum drying, so that the modification of the porous nano material is finished.
The preparation method of the nano zinc borate comprises the following steps: mixing a zinc sulfate solution with the concentration of 2.0mol/L and a sodium hydroxide solution with the concentration of 4.0mol/L in equal volume, and ultrasonically stirring the obtained mixed solution at the temperature of 60 ℃ for 45min; after the reaction is finished, weighing a proper amount of treated reaction liquid, respectively adding 5.0% by mass of boric acid and 0.5% by mass of Span80 into the reaction liquid, and ultrasonically stirring the mixture for 40min at a constant temperature of 60 ℃; after the reaction is finished, centrifuging, collecting the obtained precipitate, washing the precipitate for 4 times by using deionized water, and drying the precipitate to obtain the finished product of the nano zinc borate.
The reaction solution treatment method comprises the following steps: and adding a proper amount of deionized water into the reaction liquid obtained after the reaction is finished so as to adjust the content of the zinc hydroxide to 0.6mol/L.
The preparation method of the synergistic flame retardant comprises the following steps: respectively adding 8wt% of nano antimony trioxide and 1.5 wt% of fatty glyceride into a proper amount of microcrystalline cellulose solution, and ultrasonically mixing for 20 min; and then carrying out electrostatic spraying on the obtained suspension to obtain the solid microspheres, namely the finished product of the synergistic flame retardant.
The preparation method of the microcrystalline cellulose solution comprises the following steps: at the temperature of 80 ℃, adding a proper amount of microcrystalline cellulose into chlorinated 1-methyl 3-butylimidazolium salt ionic liquid with the mass being 20 times of that of the microcrystalline cellulose, and carrying out ultrasonic dissolution to obtain a finished product of a microcrystalline cellulose solution.
The anti-dripping agent is triallyl isocyanurate with an average particle size of 4 mu m.
Antioxidant 168 is selected as antioxidant.
The preparation process of the flame-retardant polyester fiber is the same as that of example 1.
Comparative example 1: the flame-retardant polyester fiber prepared by the preparation process provided by the embodiment 1 of the invention is different in that: the raw materials do not contain a composite flame retardant;
comparative example 2: the flame-retardant polyester fiber prepared by the preparation process provided by the embodiment 1 of the invention is different in that: the raw materials do not contain a synergistic flame retardant;
comparative example 3: the flame-retardant polyester fiber prepared by the preparation process provided by the embodiment 1 of the invention is different in that: only the common flame retardant (coated red phosphorus is selected in the embodiment) sold in the market is used in the raw materials;
performance testing
The flame-retardant polyester fibers prepared in examples 1 to 3 of the present invention were respectively prepared into fabrics, which were respectively designated as experimental examples 1 to 3; the flame-retardant polyester fibers prepared in the comparative examples 1 to 3 are prepared into fiber fabrics which are respectively marked as the comparative examples 1 to 3; the fabrics prepared in examples 1 to 3 and comparative examples 1 to 3 were then subjected to performance tests, the results of which are reported in table 1:
TABLE 1
| Smoke Density Rating (SDR) | Limiting Oxygen Index (LOI)/% | 45 degree direction flame spread/breakage length (cm) | Smoke generating toxicity/grade | |
| Example 1 | 32 | 36.6 | No/3.2 | AQ2 grade |
| Example 2 | 35 | 37.2 | NO/2.8 | AQ2 grade |
| Example 3 | 39 | 36.9 | NO/2.5 | AQ2 stage |
| Comparative example 1 | 45 | 31.8 | No/4.8 | AQ2 stage |
| Comparative example 2 | 36 | 34.5 | NO/3.7 | ZA1 stage |
| Comparative example 3 | 65 | 28.6 | No/5.8 | ZA2 stage |
| Basis of test | GB/T 8627-2007 | GB/T 2406.2-2009 | GB/T 8333-2008 | GB20285-2006 |
As can be seen from the relevant data in Table 1, under the synergistic action of the composite flame retardant and the synergistic flame retardant, the flame-retardant polyester fiber prepared by the method has more excellent flame retardant property. And the toxic smoke generated during combustion is relatively less, and the smoke density grade is relatively lower. Therefore, the fiber fabric prepared by the method has wider market prospect and is more suitable for popularization.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (9)
1. The flame-retardant polyester fiber is characterized by being prepared from the following raw materials in parts by weight: 70-80 parts of terylene slice, 18-30 parts of flame-retardant master batch and 2.0-5.0 parts of anti-dripping agent;
the flame-retardant master batch comprises the following raw materials in parts by weight: 14 to 18 parts of composite flame retardant, 4 to 6 parts of synergistic flame retardant, 3 to 7 parts of urea, 0.2 to 0.3 part of nano titanium dioxide, 0.25 to 0.4 part of nano bamboo charcoal powder, 1.5 to 2.0 parts of antioxidant, 0.3 to 0.5 part of calcium stearate, 3.0 to 3.6 parts of ethylene bis fatty acid amide, 0.15 to 0.25 part of isopropyl tri (dioctyl pyrophosphoryl) titanate and 65 to 75 parts of terylene slice;
the preparation method of the composite flame retardant comprises the following steps:
1. preparing a porous nano material;
adding a proper amount of nano-sodium montmorillonite into a water glass solution with the mass of 8-12 times and the concentration of 15-35%, then adding 5-8% of sodium bicarbonate into the water glass solution, mechanically stirring for 80-100 min, and raising the temperature of the obtained mixed components to 55-65 ℃; dispersing for 1-2 h by ultrasonic, stirring at the speed of 30-50 r/min, and slowly adding dilute hydrochloric acid solution to naturally precipitate the obtained mixture under the conditions that the pH value is 4.8-5.5 and the temperature is 55-65 ℃; when no flocculent precipitate or bubbles are generated, filtering the obtained mixture, drying the obtained filter material in vacuum to constant weight, and sieving by a grinder to obtain a finished product of the porous nano material;
2. modification of porous nano materials;
weighing a proper amount of 60-75% aqueous solution of ethanol, respectively adding 0.8-1.5% by mass of sodium dodecyl benzene sulfonate and 15-18% by mass of nano zinc borate into the aqueous solution, ultrasonically dispersing for 10-15 min, then adding 8-12% by mass of porous nano material and 20-30% by mass of 3-aminopropyltriethoxysilane into the aqueous solution of ethanol, ultrasonically dispersing for 20-30 min, and heating, stirring and mixing for 8-15 h under the protection of nitrogen; after the reaction is finished, the obtained reaction product is subjected to suction filtration and drying treatment, then is extracted for 32-45 h by using absolute ethyl alcohol, and then is subjected to vacuum drying, so that the modification of the porous nano material is finished.
2. The flame-retardant polyester fiber according to claim 1, wherein the preparation method of the nano zinc borate comprises the following steps: mixing zinc sulfate solution with the concentration of 1.2-2.0 mol/L and sodium hydroxide solution with the concentration of 2.5-4.0 mol/L in equal volume, and ultrasonically stirring the obtained mixed solution at the temperature of 45-60 ℃ for 30-45 min; after the reaction is finished, weighing a proper amount of treated reaction liquid, respectively adding 3.5-5.0% by mass of boric acid and 0.3-0.5% by mass of Span80 into the reaction liquid, and performing ultrasonic stirring for 30-40 min at the constant temperature of 50-60 ℃; after the reaction is finished, centrifuging, collecting the obtained precipitate, washing the precipitate for 2 to 4 times by using deionized water, and drying the precipitate to obtain the finished product of the nano zinc borate.
3. The flame-retardant polyester fiber according to claim 2, wherein the reaction solution treatment method comprises: and adding a proper amount of deionized water into the reaction liquid obtained after the reaction is finished so as to adjust the content of the zinc hydroxide in the reaction liquid to be 0.4-0.6 mol/L.
4. The flame-retardant polyester fiber according to claim 1, wherein the preparation method of the synergistic flame retardant comprises the following steps: respectively adding 5-8 wt% of nano antimony trioxide and 0.8-1.5 wt% of fatty glyceride into a proper amount of microcrystalline cellulose solution, and ultrasonically mixing for 10-20 min; and then carrying out electrostatic spraying on the obtained suspension to obtain the solid microspheres, namely the finished product of the synergistic flame retardant.
5. The flame-retardant polyester fiber according to claim 4, wherein the microcrystalline cellulose solution is prepared by a method comprising the following steps: at the temperature of 65-80 ℃, adding a proper amount of microcrystalline cellulose into chlorinated 1-methyl 3-butylimidazolium salt ionic liquid with the mass of 10-20 times of that of the microcrystalline cellulose, and performing ultrasonic dissolution to obtain a finished product of a microcrystalline cellulose solution.
6. The flame-retardant polyester fiber according to claim 1, wherein: the anti-dripping agent is triallyl isocyanurate with the average grain diameter of 2-4 mu m.
7. The flame-retardant polyester fiber according to claim 1, wherein: the antioxidant is any one of antioxidant B215, antioxidant 1010 and antioxidant 168.
8. The preparation process of the flame-retardant polyester fiber according to any one of claims 1 to 7, characterized by comprising the following steps:
s1, weighing a proper amount of polyester chips and flame-retardant master batches according to the formula amount; then respectively placing the weighed polyester chips and the flame-retardant master batches into a vacuum drying oven for drying treatment; drying the flame-retardant master batch until the water content is less than or equal to 180ppm, drying the terylene slices until the water content is less than or equal to 40ppm, and storing the dried terylene slices and the flame-retardant master batch for later use;
s2, putting the dried polyester chips and the flame-retardant master batches into a high-speed stirrer, slowly adding an anti-dripping agent into the high-speed stirrer, and fully mixing the anti-dripping agent and the flame-retardant master batches in the high-speed stirrer; then feeding the obtained mixed material into a screw extruder for melt extrusion;
s3, spinning and forming the melt extruded by the screw extruder through a spinneret plate of a spinning assembly at a spinning speed of 220-240 m/min and a winding speed of 720-950 m/min, and performing heat setting at 170-190 ℃ to obtain a flame-retardant polyester fiber crude product;
s4, performing irradiation treatment on the obtained flame-retardant polyester fiber crude product on a high-energy electron accelerator of 2.5-10 MeV; and obtaining the durable halogen-free flame-retardant anti-dripping polyester fiber after the treatment.
9. The preparation process of the flame-retardant polyester fiber according to claim 8, wherein the preparation process comprises the following steps: during the irradiation treatment, the irradiation dose is 80-200 kGy, and the irradiation time is 20-30 min.
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| CN114808190B (en) * | 2022-05-13 | 2023-12-22 | 杭州晨昊纺织整理有限公司 | High-elastic flame-retardant polyester fabric and preparation method thereof |
| CN114914022B (en) * | 2022-06-13 | 2023-02-28 | 广州市孖宝电缆有限公司 | Anti-electromagnetic and flame-retardant cable |
| CN115652467A (en) * | 2022-10-10 | 2023-01-31 | 南通强生石墨烯科技有限公司 | Heat-resistant flame-retardant functional fiber and preparation method thereof |
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