CN103409844B - A kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres - Google Patents
A kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres, comprise: by dried recycled polyester, phosphorus flame retardant and nano material, under 30-180 DEG C of condition, stir and evenly mix, then under 240-300 DEG C of condition, extruding pelletization, the fire-retardant recycled polyester composite that is enhanced is cut into slices; Drying is carried out in fire-retardant for enhancing recycled polyester composite section, and be then cooled to 40-90 DEG C, add dispersant, obtain spinning material, carry out spinning, drawing-off is processed, and to obtain final product.Enhancing provided by the invention fire-retardant recycled polyester slice spinning forming, fiber quality is excellent; The nano material adopted can produce with phosphorus flame retardant and act synergistically, and effectively can reduce the consumption of fire retardant, thus reduce costs, can play humidification in addition, effectively can improve fibrous mechanical property.
Description
Technical field
The invention belongs to the preparation field of Regenerated Polyester Fibres, particularly a kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres.
Background technology
Recycled polyester is after polyester bottle slice is removed bottle cap, label and additive, uses physics or chemical method to carry out processing to bottle sheet and obtains.At present due to Physical have that process equipment is few, technique simple, low cost and other advantages and become main machining method.Compared with PET, recycled polyester section has own characteristic, as many in impurity content, molecular weight distribution is wide, range of viscosities is large, makes its spinning comparatively difficult, overcomes the Regenerated Polyester Fibres tool that its shortcoming obtains function admirable and has very important significance.In addition, polyester fiber belongs to melting Flammable fibers, carries out flame-retarded process to Regenerated Polyester Fibres, and the harmfulness reducing its initiation fire seems very necessary and urgent.
The method of polyester flame-retardant modification mainly contains the several methods such as copolymerization, blended, Final finishing, wherein blending method because of operation simple, advantages such as good endurance, and being widely used.But the membership that adds of addition type phosphorus flame retardant affects Regenerated Polyester Fibres mechanical property, become in fire-retardant recycled polyester spinning the major issue needing to solve.The Preparing Organic-inorganic Nano Hybrid Material that the eighties in 20th century rises provides thinking for solving the problem, the organic-inorganic nano collaboration system of one of nano flame retardant system, the not only good characteristic of comprehensive nano particle and organic material, also possesses the advantage that it is special: as eliminated greatly polymer and the unmatched problem of nano particle thermal coefficient of expansion by nano particle interface, the viscosity of nano material increases rheological property etc. like effect and composite and matrix phase, its maximum advantage is the heat endurance that few additive can significantly improve material, anti-flammability, resistance to molten drop and mechanical property.These advantages make inorganic nano-particle work in coordination with phosphorous flame-retardant Regenerated Polyester Fibres while realizing excellent fireproof performance, can improve the mechanical property of fiber.
The clay of organic silicon surfactant and epoxy resin intercalation is used in PET resin by patent CN1844239, gives the barrier properties for gases of its excellence, and makes composite have the advantage of high heat-resisting and high strength; Patent CN1287188A take waste polyester plastic as raw material, adds unsaturated polyester (UP), o-phthalic acid dibutyl ester etc. and filters through extrusion molten, and then the differential Regenerated Polyester Fibres of spinning regeneration; Patent CN101845205A take waste PET bottle chips as raw material, having prepared halogen-free fire-resistant engineering plastics, realizing halogen-free flameproof and higher CTI value by adding phosphorus system, nitrogenated flame retardant and nano clay.In a word, the research at present for nanometer reinforced polyester and recycled polyester composite and recycled polyester spinning is more, but rarely has report to the patent strengthening fire-retardant Regenerated Polyester Fibres relevant.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres, the enhancing that the method provides fire-retardant recycled polyester slice spinning forming, and fiber quality is excellent; The nano material adopted can produce with phosphorus flame retardant and act synergistically, and effectively can reduce the consumption of fire retardant, thus reduce costs, can play humidification in addition, effectively can improve fibrous mechanical property.
A kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres of the present invention, comprising:
(1) by dried recycled polyester (Shanghai Defulun Chemical Fiber Co., Ltd., SC600), phosphorus flame retardant and nano material, under 30-180 DEG C of condition, stir and evenly mix, then under 240-300 DEG C of condition, extruding pelletization, the fire-retardant recycled polyester composite that is enhanced is cut into slices; Wherein phosphorus flame retardant addition is the 3-10wt% of recycled polyester, and nano material addition is the 0.1-5wt% of recycled polyester;
(2) drying is carried out in fire-retardant for above-mentioned enhancing recycled polyester composite section, be then cooled to 40-90 DEG C, add dispersant, obtain spinning material, carry out spinning, drawing-off is processed, must strengthen fire-retardant Regenerated Polyester Fibres, wherein the addition of dispersant is the 0.1-2wt% of spinning material.
In described step (1), the drying means of recycled polyester is: 80-140 DEG C, forced air drying 1-5h, then at 100-170 DEG C, and vacuumize 12-60h.
In described step (1), phosphorus flame retardant baking temperature is 90-150 DEG C, and drying time is 5-48h; Nano material baking temperature is 80-150 DEG C, and drying time is 5-48h.
In described step (1), phosphorus flame retardant is triphenyl phosphate, gathers one or more in diphenyl sulphone (DPS) phenyl phosphate ester, phosphinic acids aluminium, phosphinic acids zinc, and particle diameter is 0.2-5.0 μm.
In described step (1), nano material is the one in sodium-based montmorillonite, amino silane modified imvite, quaternary alkylphosphonium salt intercalated montmorillonite, sial nanotube, expanded graphite, polyhedral oligomeric silsesquioxane, and particle diameter is 0.1-0.8 μm.
In described step (1), stir speed (S.S.) is 40-400rpm.
In described step (1), extruding pelletization is double screw extruder extruding pelletization.
In described step (2), the fire-retardant recycled polyester composite dicing method of dry enhancing is: forced air drying 1-5h at 80-140 DEG C, then puts it into 110-170 DEG C of dry 12-60h in vacuum drying chamber.
In described step (2), dispersant is one or both in pentaerythritol stearate, ethylene bis stearic acid amide.
In described step (2), spinning technology parameter is: composite spinning machine carries out spinning, spinning temperature 240-300 DEG C, and spinning silk winding speed is 600-3000m/min.
In described step (2), drawing-off machined parameters is drafting multiple 1-3.5 times, temperature of heat plate 50-90 DEG C, hot plate temperature 120-200 DEG C.
beneficial effect
(1) enhancing provided by the invention fire-retardant recycled polyester slice spinning forming, fiber quality is excellent;
(2) strengthening fire retardant used in fire-retardant Regenerated Polyester Fibres material in the present invention is halogen-free flame retardants, and use and safety non-toxic in combustion process, this fiber is a kind of green material;
(3) nano material that the present invention adopts can produce with phosphorus flame retardant and act synergistically, and effectively can reduce the consumption of fire retardant, thus reduce costs, can play humidification in addition, effectively can improve fibrous mechanical property.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) by particle diameter be the poly-sodium-based montmorillonite to diphenyl sulphone (DPS) phenyl phosphate ester powder and 0.3 μm of 3 μm, at 100 DEG C dry 24 hours;
(2) by recycled polyester (Shanghai Defulun Chemical Fiber Co., Ltd., SC600) forced air drying 2 hours at 120 DEG C, after to put it in vacuum drying chamber 135 DEG C of dryings 48 hours, then the fire retardant powder of gained in itself and step (1) and sodium-based montmorillonite are mixed under the mixing speed of the temperature of 60 DEG C and 300rpm, the addition of described fire retardant powder is 5% of recycled polyester section, the addition of nano material is 1% of recycled polyester section, the mixture of gained is injected double screw extruder extruding pelletization and make the section of fire-retardant recycled polyester, the screw rod processing temperature of double screw extruder is 260 DEG C,
(3) by the fire-retardant recycled polyester section that obtains in step (2) forced air drying 2 hours at 110 DEG C, then 130 DEG C of dryings 48 hours are put it in vacuum drying chamber, be cooled to 60 DEG C, add ethylene bis stearic acid amide and obtain spinning material, the addition of described ethylene bis stearic acid amide is the 0.4wt% of spinning material, spinning material joins in melt spinning machine and carries out spinning, spinning temperature 265 DEG C, spinning silk winding speed is 1000m/min, obtained nascent fire resistance fibre, Barmag drawing machine carries out first break draft processing, obtain fire-retardant Regenerated Polyester Fibres, wherein drafting multiple 2.7 times, temperature of heat plate 60 DEG C, hot plate temperature 140 DEG C.
Adopt the fire-retardant Regenerated Polyester Fibres filament number that the method is obtained: 1.5 ~ 2.5dtex, fracture strength >=3.5CN/dtex, elongation at break >=15%, line density deviation ratio ± 6.0; By obtained fiber woven into fabric, the LOI recording this fire-retardant Regenerated Polyester Fibres material according to GB/T5454-1997 " textile combustion performance test oxygen index method " is 29%.
Embodiment 2
(1) be that two component fire retardants of 1.0 μm are poly-to diphenyl sulphone (DPS) phenyl phosphate ester and phosphinic acids aluminium (mass ratio is 2:1) powder by particle diameter, and the quaternary alkylphosphonium salt intercalated montmorillonite of 0.3 μm, at 110 DEG C dry 24 hours;
(2) by recycled polyester (Shanghai Defulun Chemical Fiber Co., Ltd., SC600) forced air drying 3 hours at 115 DEG C, after to put it in vacuum drying chamber 135 DEG C of dryings 48 hours, then the fire retardant powder of gained in itself and step (1) and quaternary alkylphosphonium salt intercalated montmorillonite are mixed under the mixing speed of the temperature of 80 DEG C and 250rpm, the addition of described fire retardant powder is 4% of recycled polyester section, the addition of quaternary alkylphosphonium salt intercalated montmorillonite is 0.6% of recycled polyester section, the mixture of gained is injected double screw extruder extruding pelletization and make the fire-retardant recycled polyester section of enhancing, the screw rod processing temperature of double screw extruder is 260 DEG C,
(3) by the fire-retardant recycled polyester section that obtains in step (2) forced air drying 2 hours at 110 DEG C, then 135 DEG C of dryings 48 hours are put it in vacuum drying chamber, be cooled to 50 DEG C, add pentaerythritol stearate and obtain spinning material, the addition of described pentaerythritol stearate is the 0.6wt% of spinning material, spinning material joins in melt spinning machine and carries out spinning, spinning temperature 270 DEG C, spinning silk winding speed is 800m/min, obtained nascent fire resistance fibre, Barmag drawing machine carries out first break draft processing, obtain fire-retardant Regenerated Polyester Fibres, wherein drafting multiple 3.0 times, temperature of heat plate 70 DEG C, hot plate temperature 150 DEG C.
Adopt the fire-retardant Regenerated Polyester Fibres filament number that the method is obtained: 1 ~ 3dtex, fracture strength >=3.0CN/dtex, elongation at break >=15%, line density deviation ratio ± 5.0; By obtained fiber woven into fabric, the LOI recording this fire-retardant Regenerated Polyester Fibres material according to GB/T5454-1997 " textile combustion performance test oxygen index method " is 30%.
Embodiment 3
(1) be the sial nanotube of 0.3 μm at 120 DEG C dry 24 hours by particle diameter, and select triphenyl phosphate to be fire retardant;
(2) by recycled polyester (Shanghai Defulun Chemical Fiber Co., Ltd., SC600) forced air drying 24 hours at 110 DEG C, after to put it in vacuum drying chamber 135 DEG C of dryings 48 hours, then the fire retardant powder of gained in itself and step (1) and sial nanotube are mixed under the mixing speed of the temperature of 40 DEG C and 200rpm, the addition of described fire retardant powder is 5% of recycled polyester section, the addition of sial nanotube is 0.5% of recycled polyester section, the mixture of gained is injected double screw extruder extruding pelletization and make the section of fire-retardant recycled polyester, the screw rod processing temperature of double screw extruder is 258 DEG C,
(3) by the fire-retardant recycled polyester section that obtains in step (2) forced air drying 2 hours at 100 DEG C, then 125 DEG C of dryings 48 hours are put it in vacuum drying chamber, be cooled to 40 DEG C, add ethylene bis stearic acid amide and obtain spinning material, the addition of described ethylene bis stearic acid amide is the 0.8wt% of spinning material, spinning material joins in melt spinning machine and carries out spinning, spinning temperature 265 DEG C, spinning silk winding speed is 800m/min, obtained nascent fire resistance fibre, Barmag drawing machine carries out first break draft processing, obtain fire-retardant Regenerated Polyester Fibres, wherein drafting multiple 3 times, temperature of heat plate 60 DEG C, hot plate temperature 140 DEG C.
Adopt the fire-retardant Regenerated Polyester Fibres filament number that the method is obtained: 1.5 ~ 3.0dtex, fracture strength >=3.0CN/dtex, elongation at break >=20%, line density deviation ratio ± 8.0; By obtained fiber woven into fabric, the LOI recording this fire-retardant Regenerated Polyester Fibres material according to GB/T5454-1997 " textile combustion performance test oxygen index method " is 29%.
Embodiment 4
(1) be the expanded graphite of 0.2 μm at 120 DEG C dry 24 hours by particle diameter, and to select poly-be fire retardant to diphenyl sulphone (DPS) phenyl phosphate ester and triphenyl phosphate (mass ratio 4:1);
(2) by recycled polyester (Shanghai Defulun Chemical Fiber Co., Ltd., SC600) forced air drying 3 hours at 115 DEG C, after to put it in vacuum drying chamber 135 DEG C of dryings 48 hours, then the fire retardant powder of gained in itself and step (1) and quaternary alkylphosphonium salt intercalated montmorillonite are mixed under the mixing speed of the temperature of 50 DEG C and 200rpm, the addition of described fire retardant powder is 5% of recycled polyester section, the addition of expanded graphite is 0.5% of recycled polyester section, the mixture of gained is injected double screw extruder extruding pelletization and make the fire-retardant recycled polyester section of enhancing, the screw rod processing temperature of double screw extruder is 265 DEG C,
(3) by the fire-retardant recycled polyester section that obtains in step (2) forced air drying 3 hours at 105 DEG C, then 130 DEG C of dryings 48 hours are put it in vacuum drying chamber, be cooled to 50 DEG C, add ethylene bis stearic acid amide and obtain spinning material, the addition of described ethylene bis stearic acid amide is the 0.5wt% of spinning material, spinning material joins in melt spinning machine and carries out spinning, spinning temperature 278 DEG C, spinning silk winding speed is 1000m/min, obtained nascent fire resistance fibre, Barmag drawing machine carries out first break draft processing, obtain fire-retardant Regenerated Polyester Fibres, wherein drafting multiple 3 times, temperature of heat plate 70 DEG C, hot plate temperature 150 DEG C.
Adopt the fire-retardant Regenerated Polyester Fibres filament number that the method is obtained: 1.5 ~ 2.5dtex, fracture strength >=3.5CN/dtex, elongation at break >=15%, line density deviation ratio ± 7.0; By obtained fiber woven into fabric, the LOI recording this fire-retardant Regenerated Polyester Fibres material according to GB/T5454-1997 " textile combustion performance test oxygen index method " is 30%.
Claims (6)
1. strengthen a preparation method for fire-retardant Regenerated Polyester Fibres, comprising:
(1) by dried recycled polyester, phosphorus flame retardant and nano material, under 30-180 DEG C of condition, stir and evenly mix, then under 240-300 DEG C of condition, extruding pelletization, the fire-retardant recycled polyester composite that is enhanced is cut into slices; Wherein phosphorus flame retardant addition is the 3-10wt% of recycled polyester, and nano material addition is the 0.1-5wt% of recycled polyester; Wherein the drying means of recycled polyester is: 80-140 DEG C, forced air drying 1-5h, then at 100-170 DEG C, and vacuumize 12-60h; Phosphorus flame retardant is triphenyl phosphate, gathers one or more in diphenyl sulphone (DPS) phenyl phosphate ester, phosphinic acids aluminium, phosphinic acids zinc, and particle diameter is 0.2-5.0 μm; Nano material is the one in sodium-based montmorillonite, amino silane modified imvite, quaternary alkylphosphonium salt intercalated montmorillonite, sial nanotube, expanded graphite, polyhedral oligomeric silsesquioxane, and particle diameter is 0.1-0.8 μm;
(2) drying is carried out in fire-retardant for above-mentioned enhancing recycled polyester composite section, be then cooled to 40-90 DEG C, add dispersant, obtain spinning material, carry out spinning, drawing-off is processed, must strengthen fire-retardant Regenerated Polyester Fibres, wherein the addition of dispersant is the 0.1-2wt% of spinning material; Wherein dispersant is one or both in pentaerythritol stearate, ethylene bis stearic acid amide.
2. a kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres according to claim 1, is characterized in that: in described step (1), phosphorus flame retardant baking temperature is 90-150 DEG C, and drying time is 5-48h; Nano material baking temperature is 80-150 DEG C, and drying time is 5-48h.
3. a kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres according to claim 1, is characterized in that: in described step (1), extruding pelletization is double screw extruder extruding pelletization.
4. a kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres according to claim 1, it is characterized in that: in described step (2), the fire-retardant recycled polyester composite dicing method of dry enhancing is: forced air drying 1-5h at 80-140 DEG C, then puts it into 110-170 DEG C of dry 12-60h in vacuum drying chamber.
5. a kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres according to claim 1, it is characterized in that: in described step (2), spinning technology parameter is: composite spinning machine carries out spinning, spinning temperature 240-300 DEG C, spinning silk winding speed is 600-3000m/min.
6. a kind of preparation method strengthening fire-retardant Regenerated Polyester Fibres according to claim 1, is characterized in that: in described step (2), drawing-off machined parameters is drafting multiple 1-3.5 times, temperature of heat plate 50-90 DEG C, hot plate temperature 120-200 DEG C.
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| CN103741250A (en) * | 2013-12-04 | 2014-04-23 | 太仓荣文合成纤维有限公司 | Inorganic/organic hybrid composite fire retardation agent and application of the same in PET fibers |
| CN104017195B (en) * | 2014-05-30 | 2016-01-20 | 浙江金汇特材料有限公司 | The production method of a kind of flame-retarding phosphorus copolymerized recycled polyester section and industrial yarn thereof |
| CN105442079A (en) * | 2015-12-28 | 2016-03-30 | 常熟市翔鹰特纤有限公司 | Environment-friendly high-strength polyester fibers |
| CN105603560B (en) * | 2016-01-25 | 2017-12-05 | 晋江市亿泰隆化纤制造有限公司 | Filling mattress flame-proof antibiotic polyester fiber and preparation method thereof |
| CN105970341A (en) * | 2016-06-29 | 2016-09-28 | 马海燕 | Flame-retardant polyester monofilament and method for producing same |
| CN107641845A (en) * | 2017-11-09 | 2018-01-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Polyester-base nano hydridization is fire-retardant/preparation method of antibiotic multifunction fiber and products thereof and application |
| TWI715381B (en) * | 2019-12-27 | 2021-01-01 | 穩得實業股份有限公司 | Fiber-grade conductive polymer composition and multifilament fiber yarn |
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