CN102653890B - Preparation method of highly-spinnable halogen-free flame-retardant nylon fiber - Google Patents
Preparation method of highly-spinnable halogen-free flame-retardant nylon fiber Download PDFInfo
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Abstract
The invention relates to a preparation method of highly-spinnable halogen-free flame-retardant nylon fibers, which comprises the following steps: performing blending and granulation of nylon slices, cyclic phosphates, melamine compounds, nanometer inorganic substances, and antioxidants in a double screw extruder to obtain a halogen-free flame-retardant nylon master batch, spinning the halogen-free flame-retardant nylon master batch with nylon slices into halogen-free flame-retardant nylon fibers through a melt spinning method. Compared with the prior art, the invention improves the dispersibility of the fire retardants and the compatibility of the polymers, and thus the product has good flame retardance; the spinnability of the nylon fibers is improved to a great extent; the invention has low cost, is industrialized; both halogen-free flame-retardant nylon aircraft seat covers and aviation carpet lines spun by the method of the invention pass FAR 25.853 cabin internal material flammability tests.
Description
Technical field
The present invention relates to a kind of preparation method of fiber, especially relate to a kind of preparation method of high spinnability halogen-free flameproof nylon fibre.
Background technology
Nylon fibre is the synthetic fiber of realizing the earliest in the world suitability for industrialized production.Although it does not include flammable fiber (limited oxygen index LOI=22～24), when its burning, the existence of melting dropping very easily causes spreading of fire, very unfavorable to fire control and disaster rescue.Due to textiles catch fire or textiles not fire-retardant spread the fire causing account for China in recent years fire incident 20%, textiles fire-retardant become fire-retardantization of macromolecular material progress one of field the most rapidly in recent years.
The production of flame-retardant textile has two kinds of methods, and the one, fabric is carried out to flame-proof treatment and fire retardant is combined with fabric reach fire-retardant object by rolling the means such as baking process, rubbing method, spray-on process.Because the reactivity of nylon is low, fire retarding treating liquid is difficult to infiltrate fabric, and its flame retardant effect is along with the increase of service life and washing times reduces gradually, and the feel of fabric is poor, weightening finish is larger.
Another kind is weave cotton cloth and have permanent fire retardant with fire resistance fibre direct spinning.The flame-retardant modified research of nylon fibre starts relatively early, two kinds of point copolymerization method and blending methods.Utilize copolymerization method, by introduce aromatic ring or fragrant heterocycle in the macromolecular chain of fiber-forming polymer, thereby improved heat endurance.Adopt in this way, du pont company and Japanese You Nijika company have successfully developed respectively the aromatic series nylon fibre of commodity " Nomex " and " Apyil " by name, its heat resistance is very good, limited oxygen index reaches 30～32, but because cost is high, therefore only for the special dimension such as military project, aerospace.Blending method adds fire retardant in the melt of fiber-forming polymer or spinning solution, method is simple, but fire retardant dispersed and can affect the spinnability of fiber with the compatibility of polymer, and for polyamide fibre, high temperature during due to hard to bear its fibers melt spinning of fire retardant causes nylon fibre tensile strength to reduce, be difficult to spinning continuously, thereby make the application of this method still in lab scale and pilot scale stage, be JP2010018906 at application number, JP2007308838, JP2007056392, JP2000328363, 200710046218.0 in these patents, adopt different fire retardants to obtain fire-retardant nylon fibre, but all do not realize real high spinnability, without industrialized mass production.
Because halogen-free flameproof nylon fibre cannot suitability for industrialized production, China produces and uses still take FLAME RETARDANT FINISH FABRIC as main at present.Therefore inevitably there is above-mentioned various negative issue.
Summary of the invention
Object of the present invention is exactly that a kind of preparation method that can realize industrialization, economical and practical high spinnability halogen-free flameproof nylon fibre is provided in order to overcome the defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions:
A preparation method for high spinnability halogen-free flameproof nylon fibre, is characterized in that, the method comprises the following steps:
(1) by the blend granulation in double screw extruder of slices of caprone, annular phosphate, melamine compounds, nano-inorganic substance, antioxidant, obtain halogen-free flameproof chinlon master batch;
(2) halogen-free flameproof chinlon master batch and slices of caprone are adopted and melt spin processes and be spun into halogen-free flameproof nylon fibre.
Halogen-free flameproof chinlon master batch described in step (1) comprises following component and weight percent content:
Slices of caprone 45-60%;
Annular phosphate 5-8%;
Melamine compounds 30-45%;
Nano-inorganic substance 0.1-5%;
Antioxidant 1-2%.
Described slices of caprone uses the spinning-grade slices of caprone that viscosity is 2.8-3.4dl/g.
The ANTIBLAZE 1045 of the preferred AIBRIGHT & of described annular phosphate WILSON company.
Described melamine compounds is selected from melamine, melamine polyphosphate, melamine cyanurate or melamine hydrobromate, preferably melamine cyanurate.
Described melamine compounds carries out surface treatment through ethylene bis stearic acid amide (EBS) or glycerin monostearate (GMS), 90% melamine compounds particle diameter is less than 5 microns, and wherein 50% melamine compounds particle diameter is 1-2 micron.
The particle diameter of described nano-inorganic substance is 10nm-100nm.
Described nano-inorganic substance is calcium carbonate, barium sulfate, glass microballoon, kaolin, wollastonite, talcum powder, mica, imvite, aluminium hydroxide, magnesium hydroxide, diatomite or silica.
Described antioxidant is antioxidant 1098, antioxidant 1076 or antioxidant SEED.
The preferred antioxidant SEED of described antioxidant.
Halogen-free flameproof chinlon master batch described in step (2) and slices of caprone adopt the mode of Weightlessness balance to add by following percentage by weight:
Slices of caprone 14-20%,
Halogen-free flameproof chinlon master batch 80-86%,
Described slices of caprone is that viscosity is the spinning-grade slices of caprone of 2.8-3.4dl/g.
The temperature Wei Yi district 230-240 ℃ of the melt spinning that melts spin processes described in step (2), two district 240-245 ℃, three district 240-245 ℃, four 245 ℃, districts, spinning speed is 800-1200m/min, and drafting multiple is 3-4 times, and draft speed is 500m/min.
The halogen-free flameproof nylon fibre preparing can be in aircraft seat cover, the application of aviation carpet line field.
Compared with prior art, the invention has the advantages that: owing to improving the dispersed of fire retardant and the compatibility with polymer, not only there is good anti-flammability, and improve to a great extent the spinnability of nylon fibre, and cost is low, realize industrialization, with this technique can continuous spinning 100 hours fracture of wires not above, spinnable halogen-free flameproof nylon fibre specification is 8D, 15D, 20D, 30D, limited oxygen index LOI is 31-32, the halogen-free flameproof polyamide fibre aircraft seat cover and the aviation carpet line that obtain of spinning, all pass through the flammable test of FAR 25.853 engine room inside materials, average char length < 203mm after vertical combustion, remove the average flame combustion time < 15s after burning things which may cause a fire disaster, dropping < 5s average time that glows.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
The preparation of high spinnability halogen-free flameproof nylon fibre, wherein first step halogen-free flameproof chinlon master batch, each weight percentages of components is: slices of caprone (M2800, Xin Hui Meida Company produces, viscosity 2.8dl/g) 60%, annular phosphate (ANTIBLAZE 1045) 6%, melamine cyanurate (through EBS surface treatment) 30%, wherein, 90% melamine cyanurate particle diameter is less than 5 microns, wherein 50% melamine cyanurate particle diameter is 1-2 micron, nano diatomite (particle diameter is 10nm) 2%, antioxidant SEED 2%.Said components joins parallel dual-screw extruding machine extruding pelletization after mixing, and with the pelletizing of tie rod water-cooled rear haulage, the each district of double screw extruder Temperature Setting is respectively 200 ℃-220 ℃-220 ℃-230 ℃-230 ℃-230 ℃-240 ℃-230 ℃.Cooling water temperature is controlled at 70 ℃, through melt extruding granulation the cooling halogen-free flameproof chinlon master batch that obtains.
The preparation of second step halogen-free flameproof nylon fibre, adopt the mode of Weightlessness balance to add by following percentage by weight halogen-free flameproof chinlon master batch and slices of caprone: slices of caprone (M2800, Xin Hui Meida Company produces, viscosity 3.2dl/g) 14%, halogen-free flameproof chinlon master batch 86%.The temperature Wei Yi district 230-240 ℃ of its melt spinning, two district 240-245 ℃, three district 240-245 ℃, four 245 ℃, districts, spinning speed is 1000m/min, and drafting multiple is 3 times, and draft speed is 500m/min; Spinnable halogen-free flameproof nylon fibre specification is 8D, 15D, 20D, 30D, limited oxygen index LOI is 31.2, through the flammable test of standard FAR 25.853 engine room inside materials, after 12s vertical combustion, average char length is 187mm, remove the average flame combustion time 11s after burning things which may cause a fire disaster, dropping 4.3s average time that glows.This halogen-free flameproof nylon fibre is for the non-halogen project of Boeing jumbo carpet, and Italian Aquafil company small lot is used.
Embodiment 2
The preparation of high spinnability halogen-free flameproof nylon fibre, wherein first step halogen-free flameproof chinlon master batch, each weight percentages of components is: slices of caprone (M3200, Xin Hui Meida Company produces, viscosity 3.2dl/g) 45%, annular phosphate (ANTIBLAZE 1045) 5%, melamine cyanurate 45%, wherein, 90% melamine cyanurate particle diameter is less than 5 microns, and wherein 50% melamine cyanurate particle diameter is 1-2 micron, and nano imvite is (through EBS surface treatment, particle diameter is 50nm) 4%, antioxidant SEED 1%.Said components joins parallel dual-screw extruding machine extruding pelletization after mixing, and with the pelletizing of tie rod water-cooled rear haulage, the each district of double screw extruder Temperature Setting is respectively 200 ℃-220 ℃-220 ℃-230 ℃-230 ℃-230 ℃-240 ℃-230 ℃.Cooling water temperature is controlled at 70 ℃, through melt extruding granulation the cooling halogen-free flameproof chinlon master batch that obtains.
The preparation of second step halogen-free flameproof nylon fibre, adopt the mode of Weightlessness balance to add by following percentage by weight halogen-free flameproof chinlon master batch and slices of caprone: slices of caprone (M2800, Xin Hui Meida Company produces, viscosity 3.4dl/g) 20%, halogen-free flameproof chinlon master batch 80%.The temperature Wei Yi district 230-240 ℃ of its melt spinning, two district 240-245 ℃, three district 240-245 ℃, four 245 ℃, districts, spinning speed is 800m/min, and drafting multiple is 3.2 times, and draft speed is 500m/min; Spinnable halogen-free flameproof nylon fibre specification is 8D, 15D, 20D, 30D, limited oxygen index LOI is 31.9, through the flammable test of standard FAR 25.853 engine room inside materials, after 12s vertical combustion, average char length is 156mm, remove the average flame combustion time 5s after burning things which may cause a fire disaster, dropping 3.2s average time that glows.
Embodiment 3
The preparation of high spinnability halogen-free flameproof nylon fibre, wherein first step halogen-free flameproof chinlon master batch, each weight percentages of components is: slices of caprone (M3200, Xin Hui Meida Company produces, viscosity 3.2dl/g) 48%, annular phosphate (ANTIBLAZE 1045) 7%, melamine cyanurate (through GMS surface treatment) 42.9%, wherein, 90% melamine cyanurate particle diameter is less than 5 microns, wherein 50% melamine cyanurate particle diameter is 1-2 micron, nano-glass microballon (particle diameter is 100nm) 0.1%, antioxidant SEED2%.Said components joins parallel dual-screw extruding machine extruding pelletization after mixing, and with the pelletizing of tie rod water-cooled rear haulage, the each district of double screw extruder Temperature Setting is respectively 200 ℃-220 ℃-220 ℃-230 ℃-230 ℃-230 ℃-240 ℃-230 ℃.Cooling water temperature is controlled at 80 ℃, through melt extruding granulation the cooling halogen-free flameproof chinlon master batch that obtains.
The preparation of second step halogen-free flameproof nylon fibre, adopt the mode of Weightlessness balance to add by following percentage by weight halogen-free flameproof chinlon master batch and slices of caprone: slices of caprone (M2800, Xin Hui Meida Company produces, viscosity 3.0dl/g) 18%, halogen-free flameproof chinlon master batch 82%.The temperature Wei Yi district 230-240 ℃ of its melt spinning, two district 240-245 ℃, three district 240-245 ℃, four 245 ℃, districts, spinning speed is 1200m/min, and drafting multiple is 3.6 times, and draft speed is 500m/min; Spinnable halogen-free flameproof nylon fibre specification is 8D, 15D, 20D, 30D, limited oxygen index LOI is 31.5, through the flammable test of standard FAR 25.853 engine room inside materials, after 12s vertical combustion, average char length is 167mm, remove the average flame combustion time 6s after burning things which may cause a fire disaster, dropping 3.5s average time that glows.
Embodiment 4
The preparation of high spinnability halogen-free flameproof nylon fibre, wherein first step halogen-free flameproof chinlon master batch, each weight percentages of components is: slices of caprone (M3400, Xin Hui Meida Company produces, viscosity 3.4dl/g) 51%, annular phosphate (ANTIBLAZE 1045) 8%, melamine hydrobromate (through EBS surface treatment) 35%, wherein, 90% melamine hydrobromate particle diameter is less than 5 microns, wherein 50% melamine hydrobromate particle diameter is 1-2 micron, nano barium sulfate (particle diameter is 70nm) 5%, antioxidant SEED 1%.Said components joins parallel dual-screw extruding machine extruding pelletization after mixing, and with the pelletizing of tie rod water-cooled rear haulage, the each district of double screw extruder Temperature Setting is respectively 200 ℃-220 ℃-220 ℃-230 ℃-230 ℃-230 ℃-240 ℃-230 ℃.Cooling water temperature is controlled at 60 ℃, through melt extruding granulation the cooling halogen-free flameproof chinlon master batch that obtains.
The preparation of second step halogen-free flameproof nylon fibre, adopt the mode of Weightlessness balance to add by following percentage by weight halogen-free flameproof chinlon master batch and slices of caprone: slices of caprone (M2800, Xin Hui Meida Company produces, viscosity 2.8dl/g) 16%, halogen-free flameproof chinlon master batch 84%.The temperature Wei Yi district 230-240 ℃ of its melt spinning, two district 240-245 ℃, three district 240-245 ℃, four 245 ℃, districts, spinning speed is 1100m/min, and drafting multiple is 3.5 times, and draft speed is 500m/min; Spinnable halogen-free flameproof nylon fibre specification is 8D, 15D, 20D, 30D, limited oxygen index LOI is 31.2, through the flammable test of standard FAR 25.853 engine room inside materials, after 12s vertical combustion, average char length is 181mm, remove the average flame combustion time 8s after burning things which may cause a fire disaster, dropping 3.9s average time that glows.
Claims (8)
1. a preparation method for high spinnability halogen-free flameproof nylon fibre, is characterized in that, the method comprises the following steps:
(1) by the blend granulation in double screw extruder of slices of caprone, annular phosphate, melamine compounds, nano-inorganic substance, antioxidant, obtain halogen-free flameproof chinlon master batch;
(2) adopt melt spinning method to be spun into halogen-free flameproof nylon fibre halogen-free flameproof chinlon master batch and slices of caprone;
Halogen-free flameproof chinlon master batch described in step (1) comprises following component and weight percent content: slices of caprone 45-60%; Annular phosphate 5-8%; Melamine compounds 30-45%; Nano-inorganic substance 0.1-5%; Antioxidant 1-2%;
Halogen-free flameproof chinlon master batch described in step (2) and slices of caprone add by following percentage by weight: slices of caprone 14-20%, and halogen-free flameproof chinlon master batch 80-86%, wherein slices of caprone is that viscosity is the spinning-grade slices of caprone of 2.8-3.4d1/g;
Described melamine compounds carries out surface treatment through ethylene bis stearic acid amide or glycerin monostearate, and 90% melamine compounds particle diameter is less than 5 microns, and wherein 50% melamine compounds particle diameter is 1-2 micron.
2. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 1, is characterized in that, described annular phosphate is the ANTIBLAZE1045 of ALBRIGHT & WILSON company.
3. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 1, it is characterized in that, described melamine compounds is selected from melamine, melamine polyphosphate, melamine cyanurate or melamine hydrobromate.
4. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 1, is characterized in that, described melamine compounds is melamine cyanurate.
5. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 1, it is characterized in that, described nano-inorganic substance is calcium carbonate, barium sulfate, glass microballoon, kaolin, wollastonite, talcum powder, mica, imvite, aluminium hydroxide, magnesium hydroxide, diatomite or silica, and particle diameter is 10nm-100nm.
6. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 1, is characterized in that, described antioxidant is antioxidant 1098, antioxidant 1076 or antioxidant SEED.
7. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 1, is characterized in that, described antioxidant is antioxidant SEED.
8. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 1, it is characterized in that, the temperature Wei Yi district 230-240 ℃ of the melt spinning of the melt spinning method described in step (2), two district 240-245 ℃, three district 240-245 ℃, four 245 ℃, districts, spinning speed is 800-1200m/min, drafting multiple is 3-4 times, and draft speed is 500m/min.
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