CN113774512A - Preparation method of flame-retardant color-spun polyester filament yarn special for high-speed rail - Google Patents
Preparation method of flame-retardant color-spun polyester filament yarn special for high-speed rail Download PDFInfo
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- CN113774512A CN113774512A CN202111076273.0A CN202111076273A CN113774512A CN 113774512 A CN113774512 A CN 113774512A CN 202111076273 A CN202111076273 A CN 202111076273A CN 113774512 A CN113774512 A CN 113774512A
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- polyester filament
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 239000003063 flame retardant Substances 0.000 title claims abstract description 129
- 229920000728 polyester Polymers 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229920001634 Copolyester Polymers 0.000 claims abstract description 42
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 42
- 239000011574 phosphorus Substances 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 37
- 238000003756 stirring Methods 0.000 claims abstract description 32
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 25
- 239000000835 fiber Substances 0.000 claims abstract description 22
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000007493 shaping process Methods 0.000 claims abstract description 18
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims abstract description 17
- 235000013539 calcium stearate Nutrition 0.000 claims abstract description 17
- 239000008116 calcium stearate Substances 0.000 claims abstract description 17
- 238000002844 melting Methods 0.000 claims abstract description 17
- 230000008018 melting Effects 0.000 claims abstract description 17
- 238000002074 melt spinning Methods 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 238000004804 winding Methods 0.000 claims abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 82
- 239000004408 titanium dioxide Substances 0.000 claims description 41
- 239000000843 powder Substances 0.000 claims description 25
- 238000009998 heat setting Methods 0.000 claims description 24
- BTKXSYWWRGMQHR-UHFFFAOYSA-N [amino(diethoxy)silyl]oxyethane Chemical compound CCO[Si](N)(OCC)OCC BTKXSYWWRGMQHR-UHFFFAOYSA-N 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 claims description 2
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 42
- 238000005507 spraying Methods 0.000 description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 28
- 239000007788 liquid Substances 0.000 description 25
- 229910052757 nitrogen Inorganic materials 0.000 description 21
- 239000002002 slurry Substances 0.000 description 20
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 19
- 239000007921 spray Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 12
- 235000019441 ethanol Nutrition 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 9
- 239000010936 titanium Substances 0.000 description 9
- 229910052719 titanium Inorganic materials 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 239000004005 microsphere Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000007664 blowing Methods 0.000 description 7
- 230000008021 deposition Effects 0.000 description 7
- 238000005868 electrolysis reaction Methods 0.000 description 6
- 239000004753 textile Substances 0.000 description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000011268 mixed slurry Substances 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 239000004744 fabric Substances 0.000 description 3
- 229920004933 Terylene® Polymers 0.000 description 2
- 238000004887 air purification Methods 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000003385 bacteriostatic effect Effects 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000008520 organization Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 206010000369 Accident Diseases 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002345 surface coating layer Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
Classifications
-
- 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
-
- 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
- D01F1/04—Pigments
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Developing Agents For Electrophotography (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of a special flame-retardant color-spun polyester filament yarn for high-speed rail, which comprises the following steps: step 1, pretreatment of environment-friendly toner: stirring the environment-friendly toner and a silane coupling agent at constant temperature until the environment-friendly toner and the silane coupling agent are completely mixed to obtain prefabricated environment-friendly toner; step 2, preparing the flame-retardant master batch: adding the phosphorus flame-retardant copolyester component and the nano calcium stearate into the prefabricated environment-friendly toner, mixing and stirring, extruding and melting by a screw extruder, cooling, granulating, sieving, mixing and drying to obtain flame-retardant master batch; step 3, preparing the flame-retardant color-spun polyester filament: and mixing and drying the phosphorus flame-retardant copolyester chips and the flame-retardant master batches, extruding, melt spinning by using a screw extruder, shaping by using a heat shaping box, cooling, winding and barreling to obtain the flame-retardant polyester fiber precursor. The invention solves the problem of poor flame resistance of the existing polyester fiber, and utilizes the premixing of the environment-friendly color paste and the silane coupling agent to realize the flame resistance and the thermal stability of the environment-friendly color paste and greatly improve the stability of the filament.
Description
Technical Field
The invention belongs to the field of fabrics, and particularly relates to a preparation method of flame-retardant color-spun polyester filament yarns special for high-speed rails.
Background
Along with the continuous improvement of the living standard of people, the requirements on textiles are higher and higher, the application fields are wider and wider, and the fire caused by the textiles frequently causes serious personal casualty accidents and economic huge loss accidents, so that the flame retardance of the textiles is improved, and the textile has important effects on ensuring the property life safety and reducing the occurrence of fire accidents. The application and standardization of flame retardant articles in public places is always a concern for the industry. The application of the qualified flame-retardant product in public places can reduce the fire load of the product, reduce the fire hazard and improve the fire safety level. A great deal of research work is done in this respect in many domestic research units and colleges and universities, and related enterprises also produce various flame-retardant products. Hundreds of national standards related to flame retardance have been established in the industries of fire fighting, textile, plastics, building materials and the like. The development and application of flame retardant technology and products are also one of technical measures for improving the fire safety conditions of buildings including public places in developed countries in the western world, and a plurality of standards related to flame retardant performance tests and evaluations are issued by the international organization for standardization (ISO), the european organization for standardization (EN), the UL and NFPA in the united states, and the like.
Polyester is one of three main fibers of synthetic fiber, and is widely applied to the field of clothing fabric and non-clothing fabric due to excellent physical and chemical properties. Along with the increasing requirements of people on living environment, the requirements of terylene on the aspects of environmental protection, flame retardance and the like are increased, so that the application range of the terylene is greatly reduced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a flame-retardant color-spun polyester filament yarn special for a high-speed rail, which solves the problem of poor flame retardance of the existing polyester fiber, and realizes flame retardance and thermal stability of environment-friendly color paste by premixing the environment-friendly color paste and a silane coupling agent, thereby greatly improving the stability of the filament yarn.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of the flame-retardant color-spun polyester filament yarn special for the high-speed rail comprises the following steps:
step 1, pretreatment of environment-friendly toner: stirring the environment-friendly toner and a silane coupling agent at constant temperature until the environment-friendly toner and the silane coupling agent are completely mixed to obtain prefabricated environment-friendly toner; the mass ratio of the environment-friendly toner to the silane coupling agent is 3-6:2, the constant-temperature stirring temperature is 125-128 ℃, and the mixing time is 45-50 min;
step 2, preparing the flame-retardant master batch: adding the phosphorus flame-retardant copolyester component and the nano calcium stearate into the prefabricated environment-friendly toner, mixing and stirring, extruding and melting by a screw extruder, cooling, granulating, sieving, mixing and drying to obtain flame-retardant master batch; the addition amount of the phosphorus flame-retardant copolyester powder is 2.3-3.0 times of the mass of the prefabricated environment-friendly toner, and the addition amount of the nano calcium stearate is 0.001% of the mass of the phosphorus flame-retardant copolyester powder;
step 3, preparing the flame-retardant color-spun polyester filament: mixing and drying the phosphorus flame-retardant copolyester chips and the flame-retardant master batches, extruding and melt spinning by using a screw extruder, then shaping by using a heat shaping box, cooling, winding and barreling to obtain flame-retardant polyester fiber precursor; the adding amount of the phosphorus flame-retardant copolyester chips is 7-49 times of the mass of the flame-retardant master batch, the melting temperature is 275-285 ℃, the heat setting box adopts double heat setting, and the temperature of the heat setting box is 245-255 ℃ and 215-225 ℃ in sequence; the linear density of the flame-retardant polyester fiber protofilament is 3.0-8.0 dtex.
Further, the environment-friendly toner is one of titanium dioxide, carbon black, iron blue, cobalt blue, iron red, titanium nickel yellow or cobalt green.
The silane coupling agent adopts amino triethoxysilane.
Still further, the environment-friendly toner is titanium dioxide-based titanium dioxide.
The titanium dioxide-based titanium dioxide takes porous titanium dioxide as a carrier and titanium dioxide as a surface coating layer, and further, the preparation method of the titanium dioxide-based titanium dioxide comprises the following steps: step a, mixing tetrabutyl titanate and polyvinylpyrrolidone powderMixing to form mixed slurry, adding absolute ethyl alcohol for dilution, uniformly stirring to form viscous slurry, spraying the viscous slurry into a reaction kettle to form particles, and standing for 20-50min to obtain particle microspheres; wherein the mass ratio of the n-butyl titanate to the polyvinylpyrrolidone powder is 2-4:1, the addition amount of the absolute ethyl alcohol is 50-80% of the volume of the n-butyl titanate, the spraying diameter is 8-10cm, the spraying speed is 3-5mL/min, the spraying temperature is 80-90 ℃, and the volume of the water vapor accounts for 5-8% in a standing environment; blowing tail by adopting nitrogen before standing, wherein the temperature of the nitrogen is 80-90 ℃, and the tail blowing speed is 4-6 mL/min; b, putting the particle microspheres into an electrolytic bath for electrolysis for 10-20min to obtain the porous titanium dioxide carrier, wherein the electrolyte in the electrolytic bath is sodium sulfate, the concentration is 0.1-0.3mol/L, the electrolysis voltage is 12-20V, and the current density is 20-30mA/cm2The temperature is 20-30 min; step c, evenly coating titanium alcohol solution on the surface of the porous titanium dioxide carrier to form an even liquid film, standing for 20-30min, and heating for 30-60min to obtain titanium dioxide-based titanium dioxide, wherein the titanium alcohol solution is 40-90g/L n-butyl titanate ethanol solution, and the concentration of n-butyl titanate in the liquid film is 0.1-0.5g/cm2In a standing environment, the temperature is 80-90 ℃, the volume concentration of the water vapor is 3-7%, and the temperature of the temperature raising treatment is 100-150 ℃.
Further, the environmental-friendly toner pretreatment comprises the following specific steps:
step i, stirring the environment-friendly toner and a silane coupling agent at constant temperature to form viscous slurry, wherein the mass ratio of the environment-friendly toner to the silane coupling agent is 3-6:2, and the stirring temperature is 125-;
step ii, injecting the viscous slurry into a spray pipe of a spraying device, heating liquid nitrogen, and introducing the heated liquid nitrogen into a spray branch pipe of the spray pipe to form a spray mixture, wherein the volume ratio of the viscous slurry to the liquid nitrogen is 3:1, and the liquid nitrogen can be replaced by nitrogen or inert gas with the same amount;
and step iii, spraying the spraying mixture into a constant-temperature reaction kettle, and performing constant-temperature deposition to obtain the prefabricated environment-friendly toner, wherein the spraying diameter is 10cm, the spraying amount is 2-5mL/min, the temperature in the constant-temperature reaction kettle is 100-.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of poor flame resistance of the existing polyester fiber, and utilizes the premixing of the environment-friendly color paste and the silane coupling agent to realize the flame resistance and the thermal stability of the environment-friendly color paste and greatly improve the stability of the filament.
2. The titanium dioxide-based titanium dioxide is used as the environment-friendly color paste, so that the stability of the pigment is greatly improved, and the titanium dioxide has good air purification, antibacterial and bacteriostatic effects.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A preparation method of the flame-retardant color-spun polyester filament yarn special for the high-speed rail comprises the following steps:
step 1, pretreatment of environment-friendly toner: stirring titanium dioxide and amino triethoxysilane at constant temperature until the titanium dioxide and the amino triethoxysilane are completely mixed to obtain prefabricated environment-friendly toner; the mass ratio of the environment-friendly toner to the silane coupling agent is 3:2, the constant-temperature stirring temperature is 125 ℃, and the mixing time is 45 min;
step 2, preparing the flame-retardant master batch: adding the phosphorus flame-retardant copolyester component and the nano calcium stearate into the prefabricated environment-friendly toner, mixing and stirring, extruding and melting by a screw extruder, cooling, granulating, sieving, mixing and drying to obtain flame-retardant master batch; the addition amount of the phosphorus flame-retardant copolyester powder is 2.3 times of the mass of the prefabricated environment-friendly toner, and the addition amount of the nano calcium stearate is 0.001 percent of the mass of the phosphorus flame-retardant copolyester powder;
step 3, preparing the flame-retardant color-spun polyester filament: mixing and drying the phosphorus flame-retardant copolyester chips and the flame-retardant master batches, extruding and melt spinning by using a screw extruder, then shaping by using a heat shaping box, cooling, winding and barreling to obtain flame-retardant polyester fiber precursor; the addition amount of the phosphorus flame-retardant copolyester chips is 7 times of the mass of the flame-retardant master batches, the melting temperature is 275 ℃, the heat setting box adopts double heat setting, and the temperature of the heat setting box is 245 ℃ and 215 ℃ in sequence; the linear density of the flame-retardant polyester fiber protofilament is 8.0 dtex.
Example 2
A preparation method of the flame-retardant color-spun polyester filament yarn special for the high-speed rail comprises the following steps:
step 1, pretreatment of environment-friendly toner: stirring carbon black and amino triethoxysilane at constant temperature until the carbon black and the amino triethoxysilane are completely mixed to obtain the prefabricated environment-friendly toner; the mass ratio of the environment-friendly toner to the silane coupling agent is 3:1, the constant-temperature stirring temperature is 128 ℃, and the mixing time is 50 min;
step 2, preparing the flame-retardant master batch: adding the phosphorus flame-retardant copolyester component and the nano calcium stearate into the prefabricated environment-friendly toner, mixing and stirring, extruding and melting by a screw extruder, cooling, granulating, sieving, mixing and drying to obtain flame-retardant master batch; the addition amount of the phosphorus flame-retardant copolyester powder is 3.0 times of the mass of the prefabricated environment-friendly toner, and the addition amount of the nano calcium stearate is 0.001 percent of the mass of the phosphorus flame-retardant copolyester powder;
step 3, preparing the flame-retardant color-spun polyester filament: mixing and drying the phosphorus flame-retardant copolyester chips and the flame-retardant master batches, extruding and melt spinning by using a screw extruder, then shaping by using a heat shaping box, cooling, winding and barreling to obtain flame-retardant polyester fiber precursor; the adding amount of the phosphorus flame-retardant copolyester chips is 49 times of the mass of the flame-retardant master batches, the melting temperature is 285 ℃, the heat setting box adopts double heat setting, and the temperature of the heat setting box is 255 ℃ and-225 ℃ in sequence; the linear density of the flame-retardant polyester fiber protofilament is 3.0 dtex.
Example 3
A preparation method of the flame-retardant color-spun polyester filament yarn special for the high-speed rail comprises the following steps:
step 1, pretreatment of environment-friendly toner: stirring iron blue and amino triethoxysilane at constant temperature until completely mixing to obtain a prefabricated environment-friendly toner; the mass ratio of the environment-friendly toner to the silane coupling agent is 2:1, the constant-temperature stirring temperature is 127 ℃, and the mixing time is 48 min;
step 2, preparing the flame-retardant master batch: adding the phosphorus flame-retardant copolyester component and the nano calcium stearate into the prefabricated environment-friendly toner, mixing and stirring, extruding and melting by a screw extruder, cooling, granulating, sieving, mixing and drying to obtain flame-retardant master batch; the addition amount of the phosphorus flame-retardant copolyester powder is 2.8 times of the mass of the prefabricated environment-friendly toner, and the addition amount of the nano calcium stearate is 0.001 percent of the mass of the phosphorus flame-retardant copolyester powder;
step 3, preparing the flame-retardant color-spun polyester filament: mixing and drying the phosphorus flame-retardant copolyester chips and the flame-retardant master batches, extruding and melt spinning by using a screw extruder, then shaping by using a heat shaping box, cooling, winding and barreling to obtain flame-retardant polyester fiber precursor; the addition amount of the phosphorus flame-retardant copolyester chips is 25 times of the mass of the flame-retardant master batches, the melting temperature is 280 ℃, the heat setting box adopts double heat setting, and the temperature of the heat setting box is 250 ℃ and 220 ℃ in sequence; the linear density of the flame-retardant polyester fiber protofilament is 5.0 dtex.
Example 4
A preparation method of the flame-retardant color-spun polyester filament yarn special for the high-speed rail comprises the following steps:
step 1, preparing environment-friendly toner: the preparation method of the titanium dioxide-based titanium dioxide comprises the following steps: step a, mixing n-butyl titanate and polyvinylpyrrolidone powder to form mixed slurry, then adding absolute ethyl alcohol to dilute, uniformly stirring to form viscous slurry, spraying the viscous slurry into a reaction kettle to form particles, and standing for 20min to obtain particle microspheres; wherein the mass ratio of the n-butyl titanate to the polyvinylpyrrolidone powder is 2:1, the addition amount of the absolute ethyl alcohol is 50% of the volume of the n-butyl titanate, the spraying diameter is 8cm, the spraying speed is 3mL/min, the spraying temperature is 80 ℃, and the volume of the water vapor accounts for 5% in a standing environment; blowing tail by adopting nitrogen before standing, wherein the temperature of the nitrogen is 80 ℃, and the tail blowing speed is 4 mL/min; b, putting the particle microspheres into an electrolytic bath for electrolysis for 10min to obtain the porous titanium dioxide carrier, wherein the electrolyte in the electrolytic bath is sodium sulfate, the concentration is 0.1mol/L, the electrolysis voltage is 12V, and the current density is 20mA/cm2At the temperature of 20 min; step c, evenly coating titanium alcohol solution on the porous titanium dioxideForming a uniform liquid film on the surface of the carrier, standing for 20min, and heating for 30min to obtain titanium dioxide-based titanium dioxide, wherein the titanium alcohol solution is a 40g/L n-butyl titanate ethanol solution, and the concentration of n-butyl titanate in the liquid film is 0.1g/cm2In a standing environment, the temperature is 80 ℃, the volume concentration of water vapor is 3%, and the temperature of the temperature rise treatment is 100 ℃.
Step 2, pretreatment of the environment-friendly toner: step i, stirring the environment-friendly toner and a silane coupling agent at constant temperature to form viscous slurry, wherein the mass ratio of the environment-friendly toner to the silane coupling agent is 3:2, and the stirring temperature is 125 ℃; step ii, injecting the viscous slurry into a spray pipe of a spraying device, heating liquid nitrogen, and introducing the heated liquid nitrogen into a spray branch pipe of the spray pipe to form a spray mixture, wherein the volume ratio of the viscous slurry to the liquid nitrogen is 3: 1; step iii, spraying the spraying mixture into a constant-temperature reaction kettle, and performing constant-temperature deposition to obtain the prefabricated environment-friendly toner, wherein the spraying diameter is 10cm, the spraying amount is 2mL/min, the temperature in the constant-temperature reaction kettle is 100 ℃, water vapor accounts for 10% of the volume of air, and the constant-temperature deposition temperature is 120 ℃;
step 3, preparing the flame-retardant master batch: adding the phosphorus flame-retardant copolyester component and the nano calcium stearate into the prefabricated environment-friendly toner, mixing and stirring, extruding and melting by a screw extruder, cooling, granulating, sieving, mixing and drying to obtain flame-retardant master batch; the addition amount of the phosphorus flame-retardant copolyester powder is 2.3 times of the mass of the prefabricated environment-friendly toner, and the addition amount of the nano calcium stearate is 0.001 percent of the mass of the phosphorus flame-retardant copolyester powder;
step 4, preparing the flame-retardant color-spun polyester filament: mixing and drying the phosphorus flame-retardant copolyester chips and the flame-retardant master batches, extruding and melt spinning by using a screw extruder, then shaping by using a heat shaping box, cooling, winding and barreling to obtain flame-retardant polyester fiber precursor; the addition amount of the phosphorus flame-retardant copolyester chips is 7 times of the mass of the flame-retardant master batches, the melting temperature is 275 ℃, the heat setting box adopts double heat setting, and the temperature of the heat setting box is 245 ℃ and 215 ℃ in sequence; the linear density of the flame-retardant polyester fiber protofilament is 8.0 dtex.
Example 5
A preparation method of the flame-retardant color-spun polyester filament yarn special for the high-speed rail comprises the following steps:
step 1, preparing environment-friendly toner: the preparation method of the titanium dioxide-based titanium dioxide powder comprises the following steps: step a, mixing n-butyl titanate and polyvinylpyrrolidone powder to form mixed slurry, then adding absolute ethyl alcohol to dilute, uniformly stirring to form viscous slurry, spraying the viscous slurry into a reaction kettle to form particles, and standing for 50min to obtain particle microspheres; wherein the mass ratio of the n-butyl titanate to the polyvinylpyrrolidone powder is 4:1, the addition amount of the absolute ethyl alcohol is 80% of the volume of the n-butyl titanate, the spraying diameter is 10cm, the spraying speed is 5mL/min, the spraying temperature is 90 ℃, and the volume of the water vapor accounts for 8% in a standing environment; before standing, blowing tail by adopting nitrogen, wherein the temperature of the nitrogen is 90 ℃, and the tail blowing speed is 6 mL/min; b, putting the particle microspheres into an electrolytic bath for electrolytic treatment for 20min to obtain the porous titanium dioxide carrier, wherein the electrolyte in the electrolytic bath is sodium sulfate, the concentration is 0.3mol/L, the electrolytic voltage is 20V, and the current density is 30mA/cm2The temperature is 30 min; step c, uniformly placing titanium alcohol liquid on the surface of the porous titanium dioxide carrier to form a uniform liquid film, standing for 30min, and heating for 60min to obtain titanium dioxide-based titanium dioxide, wherein the titanium alcohol liquid is 90g/L n-butyl titanate ethanol solution, and the concentration of n-butyl titanate in the liquid film is 0.5g/cm2In a standing environment, the temperature is 90 ℃, the volume concentration of water vapor is 7%, and the temperature of the temperature rise treatment is 150 ℃;
step 2, pretreatment of the environment-friendly toner: step i, stirring the environment-friendly toner and a silane coupling agent at constant temperature to form viscous slurry, wherein the mass ratio of the environment-friendly toner to the silane coupling agent is 3:1, and the stirring temperature is 128 ℃; step ii, injecting the viscous slurry into a spray pipe of a spraying device, heating liquid nitrogen, and introducing the heated liquid nitrogen into a spray branch pipe of the spray pipe to form a spray mixture, wherein the volume ratio of the viscous slurry to the liquid nitrogen is 3: 1; step iii, spraying the spraying mixture into a constant-temperature reaction kettle, and performing constant-temperature deposition to obtain the prefabricated environment-friendly toner, wherein the spraying diameter is 10cm, the spraying amount is 5mL/min, the temperature in the constant-temperature reaction kettle is 110 ℃, the water vapor accounts for 20% of the volume of the air, and the constant-temperature deposition temperature is 150 ℃;
step 3, preparing the flame-retardant master batch: adding the phosphorus flame-retardant copolyester component and the nano calcium stearate into the prefabricated environment-friendly toner, mixing and stirring, extruding and melting by a screw extruder, cooling, granulating, sieving, mixing and drying to obtain flame-retardant master batch; the addition amount of the phosphorus flame-retardant copolyester powder is 3.0 times of the mass of the prefabricated environment-friendly toner, and the addition amount of the nano calcium stearate is 0.001 percent of the mass of the phosphorus flame-retardant copolyester powder;
step 4, preparing the flame-retardant color-spun polyester filament: mixing and drying the phosphorus flame-retardant copolyester chips and the flame-retardant master batches, extruding and melt spinning by using a screw extruder, then shaping by using a heat shaping box, cooling, winding and barreling to obtain flame-retardant polyester fiber precursor; the adding amount of the phosphorus flame-retardant copolyester chips is 49 times of the mass of the flame-retardant master batches, the melting temperature is 285 ℃, the heat setting box adopts double heat setting, and the temperature of the heat setting box is 255 ℃ and-225 ℃ in sequence; the linear density of the flame-retardant polyester fiber protofilament is 3.0 dtex.
Example 6
A preparation method of the flame-retardant color-spun polyester filament yarn special for the high-speed rail comprises the following steps:
step 1, preparing environment-friendly toner: the preparation method of the titanium dioxide-based titanium dioxide powder comprises the following steps: step a, mixing n-butyl titanate and polyvinylpyrrolidone powder to form mixed slurry, then adding absolute ethyl alcohol to dilute, uniformly stirring to form viscous slurry, spraying the viscous slurry into a reaction kettle to form particles, and standing for 40min to obtain particle microspheres; wherein the mass ratio of the n-butyl titanate to the polyvinylpyrrolidone powder is 3:1, the addition amount of the absolute ethyl alcohol is 70% of the volume of the n-butyl titanate, the spraying diameter is 9cm, the spraying speed is 4mL/min, the spraying temperature is 85 ℃, and the volume of the water vapor accounts for 7% in a standing environment; blowing tail with nitrogen at 85 deg.C before standingThe tail speed is 5 mL/min; b, putting the particle microspheres into an electrolytic bath for electrolysis for 15min to obtain the porous titanium dioxide carrier, wherein the electrolyte in the electrolytic bath is sodium sulfate, the concentration is 0.2mol/L, the electrolysis voltage is 16V, and the current density is 25mA/cm2At a temperature of 25 min; step c, uniformly placing titanium alcohol liquid on the surface of the porous titanium dioxide carrier to form a uniform liquid film, standing for 25min, and heating for 30-60min to obtain titanium dioxide-based titanium dioxide, wherein the titanium alcohol liquid is a 40-90g/L (per liter) n-butyl titanate ethanol solution, and the concentration of n-butyl titanate in the liquid film is 0.4g/cm2In a standing environment, the temperature is 85 ℃, the volume concentration of water vapor is 5%, and the temperature of the temperature rise treatment is 130 ℃;
step 2, pretreatment of the environment-friendly toner: step i, stirring the environment-friendly toner and a silane coupling agent at constant temperature to form viscous slurry, wherein the mass ratio of the environment-friendly toner to the silane coupling agent is 5:2, and the stirring temperature is 126 ℃; step ii, injecting the viscous slurry into a spray pipe of a spraying device, heating liquid nitrogen, and introducing the heated liquid nitrogen into a spray branch pipe of the spray pipe to form a spray mixture, wherein the volume ratio of the viscous slurry to the liquid nitrogen is 3: 1; step iii, spraying the spraying mixture into a constant-temperature reaction kettle, and performing constant-temperature deposition to obtain the prefabricated environment-friendly toner, wherein the spraying diameter is 10cm, the spraying amount is 4mL/min, the temperature in the constant-temperature reaction kettle is 105 ℃, the water vapor accounts for 15% of the volume of the air, and the constant-temperature deposition temperature is 140 ℃;
step 3, preparing the flame-retardant master batch: adding the phosphorus flame-retardant copolyester component and the nano calcium stearate into the prefabricated environment-friendly toner, mixing and stirring, extruding and melting by a screw extruder, cooling, granulating, sieving, mixing and drying to obtain flame-retardant master batch; the addition amount of the phosphorus flame-retardant copolyester powder is 2.8 times of the mass of the prefabricated environment-friendly toner, and the addition amount of the nano calcium stearate is 0.001 percent of the mass of the phosphorus flame-retardant copolyester powder;
step 4, preparing the flame-retardant color-spun polyester filament: mixing and drying the phosphorus flame-retardant copolyester chips and the flame-retardant master batches, extruding and melt spinning by using a screw extruder, then shaping by using a heat shaping box, cooling, winding and barreling to obtain flame-retardant polyester fiber precursor; the addition amount of the phosphorus flame-retardant copolyester chips is 25 times of the mass of the flame-retardant master batches, the melting temperature is 280 ℃, the heat setting box adopts double heat setting, and the temperature of the heat setting box is 250 ℃ and 220 ℃ in sequence; the linear density of the flame-retardant polyester fiber protofilament is 5.0 dtex.
The results of examples 1 to 6, which are tested by the national standard method for grading the combustion performance of building materials and products, are as follows:
the evaluation criteria were:
the detection conditions were as follows:
| 1 | 2 | 3 | 4 | |
| example 1 | 50 | 7.4 | 545 | ZA3 |
| Example 2 | 59 | 7.9 | 556 | ZA3 |
| Example 3 | 55 | 7.7 | 549 | ZA3 |
| Example 4 | 53 | 7.5 | 547 | ZA3 |
| Example 5 | 62 | 8.1 | 558 | ZA3 |
| Example 6 | 58 | 7.9 | 549 | ZA3 |
In summary, the invention has the following advantages:
1. the invention solves the problem of poor flame resistance of the existing polyester fiber, and utilizes the premixing of the environment-friendly color paste and the silane coupling agent to realize the flame resistance and the thermal stability of the environment-friendly color paste and greatly improve the stability of the filament.
2. The titanium dioxide-based titanium dioxide is used as the environment-friendly color paste, so that the stability of the pigment is greatly improved, and the titanium dioxide has good air purification, antibacterial and bacteriostatic effects.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (9)
1. A preparation method of flame-retardant color-spun polyester filament yarn special for high-speed rails is characterized by comprising the following steps: the method comprises the following steps:
step 1, pretreatment of environment-friendly toner: stirring the environment-friendly toner and a silane coupling agent at constant temperature until the environment-friendly toner and the silane coupling agent are completely mixed to obtain prefabricated environment-friendly toner;
step 2, preparing the flame-retardant master batch: adding the phosphorus flame-retardant copolyester component and the nano calcium stearate into the prefabricated environment-friendly toner, mixing and stirring, extruding and melting by a screw extruder, cooling, granulating, sieving, mixing and drying to obtain flame-retardant master batch;
step 3, preparing the flame-retardant color-spun polyester filament: and mixing and drying the phosphorus flame-retardant copolyester chips and the flame-retardant master batches, extruding, melt spinning by using a screw extruder, shaping by using a heat shaping box, cooling, winding and barreling to obtain the flame-retardant polyester fiber precursor.
2. The preparation method of the special flame-retardant color-spun polyester filament yarn for the high-speed rail according to claim 1, which is characterized by comprising the following steps of: the mass ratio of the environment-friendly toner to the silane coupling agent in the step 1 is 3-6:2, the constant-temperature stirring temperature is 125-128 ℃, and the mixing time is 45-50 min.
3. The preparation method of the special flame-retardant color-spun polyester filament yarn for the high-speed rail according to claim 1, which is characterized by comprising the following steps of: the addition amount of the phosphorus flame-retardant copolyester powder in the step 2 is 2.3-3.0 times of the mass of the prefabricated environment-friendly toner, and the addition amount of the nano calcium stearate is 0.001% of the mass of the phosphorus flame-retardant copolyester powder.
4. The preparation method of the special flame-retardant color-spun polyester filament yarn for the high-speed rail according to claim 1, which is characterized by comprising the following steps of: the adding amount of the phosphorus flame-retardant copolyester chips in the step 3 is 7-49 times of the mass of the flame-retardant master batches, and the melting temperature is 275-285 ℃.
5. The preparation method of the special flame-retardant color-spun polyester filament yarn for the high-speed rail according to claim 1, which is characterized by comprising the following steps of: the heat setting box in the step 3 adopts double heat setting, and the temperature of the heat setting box is 245-255 ℃ and 215-225 ℃ in sequence.
6. The preparation method of the special flame-retardant color-spun polyester filament yarn for the high-speed rail according to claim 1, which is characterized by comprising the following steps of: the linear density of the flame-retardant polyester fiber protofilament obtained in the step 3 is 3.0-8.0 dtex.
7. The preparation method of the special flame-retardant color-spun polyester filament yarn for the high-speed rail according to claim 1, which is characterized by comprising the following steps of: the environment-friendly toner is one of titanium dioxide, carbon black, iron blue, cobalt blue, iron red, titanium-nickel yellow or cobalt green.
8. The preparation method of the special flame-retardant color-spun polyester filament yarn for the high-speed rail according to claim 7, which is characterized by comprising the following steps of: the environment-friendly toner is titanium dioxide-based titanium dioxide.
9. The preparation method of the special flame-retardant color-spun polyester filament yarn for the high-speed rail according to claim 1, which is characterized by comprising the following steps of: the silane coupling agent adopts amino triethoxysilane.
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| CN103409845A (en) * | 2013-08-20 | 2013-11-27 | 东华大学 | Preparation method for stoste coloring anti-flaming copolyester fibers |
| CN108251908A (en) * | 2017-12-01 | 2018-07-06 | 绍兴协力新材料科技有限公司 | A kind of flame retardant polyester fiber |
| CN108993558A (en) * | 2018-08-13 | 2018-12-14 | 蒋黎婷 | A kind of preparation method of high-performance titanium dioxide optical catalyst |
| CN109264778A (en) * | 2018-10-16 | 2019-01-25 | 张静娟 | A kind of preparation method of the nano-titanium dioxide of size tunable |
| CN109319834A (en) * | 2018-11-08 | 2019-02-12 | 绍兴文理学院 | A kind of preparation method of nano-titanium dioxide |
| CN109853073A (en) * | 2018-11-12 | 2019-06-07 | 上海德福伦化纤有限公司 | A kind of original liquid coloring flame-retardant water-repellent polyester fiber and preparation method thereof |
| CN110527287A (en) * | 2019-09-30 | 2019-12-03 | 华南理工大学 | A kind of polyamide Masterbatch and preparation method thereof |
-
2020
- 2020-11-13 CN CN202011269262.XA patent/CN112695405A/en not_active Withdrawn
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- 2021-09-14 CN CN202111076273.0A patent/CN113774512A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409845A (en) * | 2013-08-20 | 2013-11-27 | 东华大学 | Preparation method for stoste coloring anti-flaming copolyester fibers |
| CN108251908A (en) * | 2017-12-01 | 2018-07-06 | 绍兴协力新材料科技有限公司 | A kind of flame retardant polyester fiber |
| CN108993558A (en) * | 2018-08-13 | 2018-12-14 | 蒋黎婷 | A kind of preparation method of high-performance titanium dioxide optical catalyst |
| CN109264778A (en) * | 2018-10-16 | 2019-01-25 | 张静娟 | A kind of preparation method of the nano-titanium dioxide of size tunable |
| CN109319834A (en) * | 2018-11-08 | 2019-02-12 | 绍兴文理学院 | A kind of preparation method of nano-titanium dioxide |
| CN109853073A (en) * | 2018-11-12 | 2019-06-07 | 上海德福伦化纤有限公司 | A kind of original liquid coloring flame-retardant water-repellent polyester fiber and preparation method thereof |
| CN110527287A (en) * | 2019-09-30 | 2019-12-03 | 华南理工大学 | A kind of polyamide Masterbatch and preparation method thereof |
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