Preparation and characterizations of flame retardant melamine cyanurate/polyamide 6 composite fibers via in situ polymerization

2016 ◽  
Vol 87 (5) ◽  
pp. 561-569 ◽  
Author(s):  
Yuanyuan Li ◽  
Yunzhi Lin ◽  
Kai Sha ◽  
Ru Xiao

To improve the flame retardancy of polyamide 6 (PA6) fibers, melamine cyanurate (MCA)/PA6 composites were synthesized via in situ polymerization of ɛ-caprolactam in the presence of adipic acid-melamine salt and cyanuric acid-hexane diamine salt. The flame retardant MCA/PA6 composite fibers were prepared by melt spinning. The structure and properties of MCA/PA6 composites and MCA/PA6 composite fibers were studied by Fourier transform infrared spectra, X-ray diffraction, differential scanning calorimetry, thermogravimetric analysis, scanning electron microscopy, tensile tests, vertical burning tests (UL94) and limiting oxygen index (LOI) tests. Experimental results indicated that the MCA/PA6 composites loaded with 8 wt% of additives can achieve UL94 V-0 rating with an LOI value of 29.3%. The tenacity at break of PA6 fiber decreased from 4.85 to 3.11 cN·dtex–1 for MCA/PA6-8 composite fiber. However, the MCA/PA6 composite fibers can effectively suppress the propagation of flame in fabric. This means that the in situ polymerization approach paves the way for the preparation of MCA/PA6 composites that have good spinnability and flame retardancy.

Polymers ◽  
2020 ◽  
Vol 12 (8) ◽  
pp. 1787
Author(s):  
Jelena Vasiljević ◽  
Andrej Demšar ◽  
Mirjam Leskovšek ◽  
Barbara Simončič ◽  
Nataša Čelan Korošin ◽  
...  

Studies of the production of fiber-forming polyamide 6 (PA6)/graphene composite material and melt-spun textile fibers are scarce, but research to date reveals that achieving the high dispersion state of graphene is the main challenge to nanocomposite production. Considering the significant progress made in the industrial mass production of graphene nanoplatelets (GnPs), this study explored the feasibility of production of PA6/GnPs composite fibers using the commercially available few-layer GnPs. To this aim, the GnPs were pre-dispersed in molten ε-caprolactam at concentrations equal to 1 and 2 wt %, and incorporated into the PA6 matrix by the in situ water-catalyzed ring-opening polymerization of ε-caprolactam, which was followed by melt spinning. The results showed that the incorporated GnPs did not markedly influence the melting temperature of PA6 but affected the crystallization temperature, fiber bulk structure, crystallinity, and mechanical properties. Furthermore, GnPs increased the PA6 complex viscosity, which resulted in the need to adjust the parameters of melt spinning to enable continuous filament production. Although the incorporation of GnPs did not provide a reinforcing effect of PA6 fibers and reduced fiber tensile properties, the thermal stability of the PA6 fiber increased. The increased melt viscosity and graphene anti-dripping properties postponed melt dripping in the vertical flame spread test, which consequently prolonged burning within the samples.


2016 ◽  
Vol 16 (9) ◽  
pp. 9919-9924 ◽  
Author(s):  
Shanshan Wei ◽  
Leyu Wang ◽  
Ce Liu ◽  
Mulin Yu ◽  
Xianhong Chen ◽  
...  

Polymers ◽  
2020 ◽  
Vol 12 (3) ◽  
pp. 657 ◽  
Author(s):  
Jelena Vasiljević ◽  
Marija Čolović ◽  
Nataša Čelan Korošin ◽  
Matic Šobak ◽  
Žiga Štirn ◽  
...  

The production of sustainable and effective flame retardant (FR) polyamide 6 (PA6) fibrous materials requires the establishment of a novel approach for the production of polyamide 6/FR nanodispersed systems. This research work explores the influence of three different flame-retardant bridged 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) derivatives on the comprehensive properties of in situ produced PA6/FR systems. To this end, in situ water-catalyzed ring-opening polymerization of ε-caprolactam was conducted in the presence of three different bridged DOPO derivatives, e.g., one P−N bond phosphonamidate derivative and two P−C bond phosphinate derivatives. The selected bridged DOPO derivatives mainly act in the gas phase at the temperatures that relatively match the PA6 pyrolysis specifics. The effects of the FRs on the dispersion state, morphological, molecular, structural, melt-rheological, and thermal properties of the in situ synthesized PA6 were evaluated. The specific advantage of this approach is one-step production of PA6 with uniformly distributed nanodispersed FR, which was obtained in the case of all three applied FRs. However, the applied FRs differently interacted with monomer and polymer during the polymerization, which was reflected in the length of PA6 chains, crystalline structure, and melt-rheological properties. The applied FRs provided a comparable effect on the thermal stability of PA6 and stabilization of the PA6/FR systems above 450 °C in the oxygen-assisted pyrolysis. However, only with the specifically designed FR molecule were the comprehensive properties of the fiber-forming PA6 satisfied for the continuous conduction of the melt-spinning process.


2008 ◽  
Vol 19 (2) ◽  
pp. 241-244 ◽  
Author(s):  
Zhi Yong Wu ◽  
Wei Xu ◽  
Jin Kui Xia ◽  
Yao Chi Liu ◽  
Qian Xin Wu ◽  
...  

2014 ◽  
Vol 789 ◽  
pp. 169-173 ◽  
Author(s):  
Li Li Li ◽  
Zhi Hao Wu ◽  
Shuai Shuai Jiang ◽  
Tian Ze Wu ◽  
Shou Yang Lu ◽  
...  

Different dimensional siliciferous particles including silica (0D), halloysite nanotubes (HNTs,1D) and montmorillonite (MMT,2D) were melt blending with certain amount of melamine cyanurate and polyamide 6(PA6) by a twin-screw extruder. Characterization of the PA6 composites has been investigated using scan electron microscopy (SEM), thermal gravimetric analyzer (TGA), universal testing machine and limiting oxygen index instrument. SEM images indicate that the nanoparticles were uniformly dispersed in the PA6 but there was some aggregation of MCA in the composites. The incorporation of silica exerted a negative effect on the flame retardancy of PA6/MCA composite, whereas adding HNTs and MMT lead to the improvements of LOI value of 30.4 and 30.9 respectively. TGA results show that PA6/MCA/silica, PA6/MCA/HNTs and PA6/MCA/OMMT exhibit two degradation stages. Higher Tmax1 and Tmax2 appeared comparing with PA6/MCA. Char residue of PA6/MCA/OMMT at 600°C were elevated most. HNTs and OMMT can increase the tensile strength and elongation of PA6/MCA by universal testing machine results, even higher than pure PA6, showing enhanced effects of these 1D and 2D fillers. These could enhance strength of the char and finally increase the flame retardancy of PA6.


2019 ◽  
Vol 166 ◽  
pp. 50-59 ◽  
Author(s):  
Jelena Vasiljević ◽  
Marija Čolović ◽  
Ivan Jerman ◽  
Barbara Simončič ◽  
Andrej Demšar ◽  
...  

Materials ◽  
2020 ◽  
Vol 13 (21) ◽  
pp. 4826
Author(s):  
Simon König ◽  
Philipp Kreis ◽  
Christian Herbert ◽  
Andreas Wego ◽  
Mark Steinmann ◽  
...  

Poly(acrylonitrile) (PAN) fibers have two essential drawbacks: they are usually processed by solution-spinning, which is inferior to melt spinning in terms of productivity and costs, and they are flammable in air. Here, we report on the synthesis and melt-spinning of an intrinsically flame-retardant PAN-copolymer with phosphorus-containing dimethylphosphonomethyl acrylate (DPA) as primary comonomer. Furthermore, the copolymerization parameters of the aqueous suspension polymerization of acrylonitrile (AN) and DPA were determined applying both the Fineman and Ross and Kelen and Tüdõs methods. For flame retardancy and melt-spinning tests, multiple PAN copolymers with different amounts of DPA and, in some cases, methyl acrylate (MA) have been synthesized. One of the synthesized PAN-copolymers has been melt-spun with propylene carbonate (PC) as plasticizer; the resulting PAN-fibers had a tenacity of 195 ± 40 MPa and a Young’s modulus of 5.2 ± 0.7 GPa. The flame-retardant properties have been determined by Limiting Oxygen Index (LOI) flame tests. The LOI value of the melt-spinnable PAN was 25.1; it therefore meets the flame retardancy criteria for many applications. In short, the reported method shows that the disadvantage of high comonomer content necessary for flame retardation can be turned into an advantage by enabling melt spinning.


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