Higher Char Residue Research Articles

Effect of intercalation of layered double hydroxides with sulfonate-containing calix[4]arenes on the flame retardancy of castor oil-based flexible polyurethane foams

Abstract In this research, a series of castor oil-based flexible polyurethane nanocomposite foams incorporated with unmodified LDH and two kinds of sulfonate-containing calix[4]arenes (SC4A and SuBC4A macrocycles) intercalated LDHs were prepared. Structural, thermal, and morphological inspection of prepared LDHs nanosheets confirmed their successful preparation. The dispersion quality of nanosheets strongly dependent on the type of nanosheets. The SEM images of the prepared foams exhibited that the intercalation of LDH nanosheets with SuBC4A macrocycle could drastically overcome the agglomeration problem of unmodified LDH within the PUF matrices. According to TGA and DMTA results, the PUF/SuBC4A-LDH nanocomposite foam exhibited the highest char yield and also the highest storage modulus values, respectively. Furthermore, cone calorimeter tests (CCT) revealed that the PUF/SuBC4A-LDH foam has the best flame retardancy and smoke suppression properties with the highest char residue and lowest peak heat release rate (pHRR), total heat release (THR), and total smoke production (TSP) values.

Thermal stability and flame retardancy of an epoxy resin modified with phosphoric triamide and glycidyl POSS

Phosphoric triamide (PTA) and glycidyl polyhedral oligomeric silsesquioxane (POSS) were simultaneously incorporated into the cured network of a bisphenol F epoxy resin and 4,4′-diaminodiphenyl methane (DDM) to improve the thermal stability and flame retardancy. PTA was synthesized by triethyl phosphate and DDM, and its chemical structure was confirmed by 1H nuclear magnetic resonance (NMR) and Fourier transform infrared (FTIR). The differential scanning calorimetric (DSC) results showed that the introduction of PTA and POSS slightly increased the glass transition temperature of the epoxy resin. The thermogravimetric analysis results indicated that compared with the pure, phosphoric, and silicic epoxy resins, the modified epoxy resin possessed the lowest weight loss rate and highest char residue. Its limiting oxygen index value was as high as 30.5, and the UL-94 grade reached V-1. A decomposition test was carried out to obtain sufficient char residue and investigate the condensed mechanism. The scanning electron microscopic images demonstrated that the char residue of the modified epoxy resin had a compact structure. The energy dispersive X-ray and FTIR analyses verified the synergistic effect of the phosphorus and silicon in the PTA and POSS, respectively, on the epoxy resin.

Properties of polyurethane coatings based on linseed oil phosphate ester polyols and expandable graphite

The effect of two grades of expandable graphite (EG 096 and EG 290) on the thermal decomposition and flammability of polyurethane (PU) coatings, based on two kinds of linseed oil phosphate ester polyols, was studied. Thermogravimetric analysis (TGA) and the cone calorimeter test at a heat flux of 35 kW/m2 were used for this purpose. The chemical structure of the synthesized polyols was identified by Fourier Transform Infrared (FTIR) and Nuclear Magnetic Resonance (31P NMR) spectroscopy. The content of EG was varied from 0 up to 25%. For all characteristics of PU coatings, the maximum effect was reached at 25% of EG. It was found that PU coatings filled with EG 096 had higher char residue at thermal decomposition under nitrogen. The flame retardancy of the PU coating filled with EG 290, which generated more blowing gases at thermal decomposition and therefore had a higher expansion volume, was higher than the flame retardancy of the coatings filled with EG 096. The best characteristics were shown by filled PU coatings based on the polyol, which was phosphorylated in the presence of isopropyl alcohol and which, besides phosphate mono- and diesters, had phosphate triester and pyrophosphate monoester.

The block combustion, high char residues and smoke restrain effect of nano-FeSnO(OH)5 on polyvinyl chloride

Nanoscale and cubic-shaped FeSnO(OH)5 (ITOH) flame retardant was synthesized by co-precipitation method and characterized by X-ray diffraction and transmission electron microscopy (TEM). The blank poly(vinyl chloride) (PVC0) and flexible PVC/ITOH composites were investigated by the limiting oxygen index (LOI), cone calorimetric test, tensile test and thermogravimetric analysis. The results showed that compared with PVC0, the LOI of PVC sample treated with 15 phr ITOH (PVC15) increases by 7.7%, and ITOH could more effectively promote the dehydrochlorination reaction of PVC. The flame of PVC15 disappeared for up to 165 s when it burned for 120 s, which significantly reduced the total heat release and total smoke production of PVC. This phenomenon not only can effectively prevent the proliferation of fire, but also facilitates the evacuation of people in the event of a fire. Lewis acid FeCl2 and FeOCl, assigned by the Fe2p spectra of char residue, could effectively catalyze the cross-linking of PVC into carbon.

Exceptional flame-retardant cellulosic foams modified with phosphorus-hybridized graphene nanosheets

Lightweight bio-based foams from renewable cellulose nanofibers (CNF) and phosphorus-hybridized graphene nanosheets (PGN) were prepared by means of a simple freeze-drying process. By comparison, the CNF–Graphite, CNF–chemically reduced graphene nanosheets (CRG), CNF–red phosphorus (RP) composite foams were also fabricated. The CNF–PGN composite foam showed porous structures and the PGNs were uniformly distributed in the pore wall of the cellulose foams. The resultant CNF composite foams exhibited a thermal conductivity in the range of 0.0299–0.0310 W/(m K). The CNF–PGN composite foam exhibited a high char residue (25.6 wt%) at 800 °C, which was 205% higher than the calculated value, suggesting the excellent char formation ability. In the vertical burning tests, the CNF foam burnt out with rapid flame propagation, while the CNF–Graphite, CNF-RP and CNF–CRG composite foams cannot stop the smoldering behaviors. In contrast to these composite foams, the CNF–PGN composite foam displayed self-extinguishing behaviours and the flame spread was suppressed completely. Cone calorimeter measurements further manifested excellent fire retardancy of the CNF–PGN composite foam, which showed that the peak heat release rate was reduced to 14.6 kW/m2, lower than most of the reported by state-of-the-art flame retardant polymeric foams.

The effects of polybenzimidazole and polyacrylic acid modified carbon black on the anti-UV-weathering and thermal properties of polyvinyl chloride composites

In this study, the effects of polybenzimidazole (PBI) and polyacrylic acid (PAA) modified carbon black (MCB) on the anti-UV-weathering and thermal properties of PVC composites were investigated. The optimal mass ratios of PBI and MCB to PVC are 0.1 wt% and 0.2 wt%, respectively, and the resultant 1PBI/2MCB/PVC composite membrane with a thickness of about 60 μm can block over 99% of UV light below 380 nm. The UV absorption mechanism was investigated by the optional band gap (Eg) and the fluorescence spectroscopy. The incorporation of PBI and MCB results in a decrease in Eg, from 4.96 eV for PVC membrane to 2.90 eV for 1PBI/2MCB/PVC composite membrane, and MCB can quench the fluorescence of PBI by photon-induced electron transfer to further protect PVC. The results of accelerated UV-weathering experiment indicate that the incorporation of PBI and MCB can improve the anti-UV-weathering property of PVC. The thermal degradation behaviors of PVC and its composite membranes in air and N2 atmosphere were also investigated. The highest char residue (13.7 wt%) is obtained in 1PBI/2MCB/PVC composite membrane at 800 °C in N2 atmosphere, with an increase of 73.4% compared with that of PVC membrane, which may be because PBI and MCB can synergistically accelerate the carbonization of PVC molecules to rapidly form stable char residue.

Preparation and characterisation of flame retardant encapsulated with functionalised silica-based shell

Intumescent fire retardant (IFR) coatings are nowadays considered as the most effective flame retardant (FR) treatment. Nevertheless, the principal compound in an IFR system, ammonium polyphosphate (APP), is highly sensitive to moisture and IFR coating effectiveness decreases quickly. The main objective of this study is to encapsulate APP in a hybrid silica-based membrane by sol-gel process using alkoxysilane tetraethoxysilane (TEOS) and methyltriethoxysilane (MTES) precursor. The morphology and structure of APP and microencapsulated ammonium polyphosphate (MAPP) were assessed by scanning electron microscopy and Fourier transforms infrared spectroscopy (FTIR). X-ray photoelectron spectroscopy (XPS) results revealed that APP was well encapsulated inside the polysiloxane shells. The thermal degradation of APP and MAPP was evaluated by thermogravimetric analysis. At 800 °C, the MAPP had higher char residue (70.49 wt%) than APP (3.06 wt%). The hydrophobicity of MAPP increased significantly with the water contact angles up to 98°, in comparison to 20° for APP.

Thermal degradation and pyrolysis analysis of zinc borate reinforced intumescent fire retardant coatings

This work aims at evaluating the potential of nano-sized zinc borate as substitution of boric acid for thermal degradation and gaseous products in expandable graphite based intumescent fire retardant coating IFRC systems. The thermal degradation and pyrolysis of intumescent flame retardant coatings was characterized by bunsen burner fire test, thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), energy dispersive spectrometry (EDX), X-ray diffraction (XRD), fourier transformed infra-red analysis (FTIR), X-ray photoelectron spectroscopy (XPS) and gaseous emission analysis (Py-GC). Bunsen burner fire test reveals that the partial substitution of zinc borate (6.61 mass%) imparts a substantial improvement in thermal stability and reduces steel substrate temperature to 124 °C. From thermogravimetric analysis results, it was shown that this composition increases char residual mass from 39 to 46.14 mass%. The morphological structures of char residue were investigated by FESEM and it indicates that zinc borate promotes more continuous and compact char layers that hinder the heat diffusion and oxygen transmission effectively. XRD and FTIR results show that zinc borate develops a zinc-based glassy intumescent shield i.e. zinc bis (hydroxyanthrapyrimidine) dehydrate (C30H14N4O4Zn·2H2O) that strengthens the char. The new chemical species enhances the thermal stability of the freshly formed char at high temperature and provides an enhanced fire protection. XPS analysis shows the higher carbon contents in formulation IF-5 (6.6 mass%) and endorses high char residue. The Py-GC analysis confirms release of less toxic gaseous products in IF-5 formulation, considering their type and concentration, as compared to control formulation, and is considered as an environmentally safe intumescent formulation.

Synthesis and Application of Polyurethane-Modified Silicone as Finishing Agent for Cotton Fabric

The polyurethane modified organic silicone (PU-SA) was successfully synthesized via step-by-step polymerization with isophorone diisocyanate (IPDI) and polypropylene glycol (PPG) used as monomers, dibutyltindilaurate (DBTDL) as the catalyst, trimethylolpropane (TMP) and N-methyldiethanolamine (MDEA) as the chain extender, and amino-terminated siloxane (SA) as the blocking agent. The chemical structure of PU-SA was characterized by Fourier transform infrared spectroscopy (FT-IR). X-ray photoelectron spectroscopy (XPS) and scanning electron microscope (SEM) showed that PUSA had been successfully finished on the surface. Additionally, the thermogravimetric analysis (TGA) demonstrated that the PU-SA treated fabrics showed low decomposition temperature and slightly high char residue. As a finishing agent, the effect of PU-SA on the handle of cotton fabrics was also studied by using a Kawabata Evaluation System for Fabrics (KES-F). The experimental results found that PU-SA had a significant improvement on the bending properties, surface properties, and compressional properties. Moreover, the mechanical and anti-wrinkle properties of the cotton fabrics were also enhanced.

Incorporation of graphene oxide nanolayers into thermally stable hybrid composites of thermosetting resins by combination of curing and sol–gel reactions

Three different hybrid composites with high thermal stability and char residue were prepared from incorporation of tetraethyl orthosilicate (TEOS)-modified epoxy resin (MER), (3-glycidyloxypropyl) trimethoxysilane (GPTMS)-modified novolac resin (MNR), epoxidized novolac resin (ENR), and also furfuryl alcohol- and (3-aminopropyl) trimethoxysilane (APTMS)-modified graphene oxide (GFS) into silica/siloxane network by a sol–gel reaction. The first hybrid was composed from ENR, MNR, and GFS. The second type was prepared from MER, MNR, and GFS. The third type was prepared from MER, novolac resin, and GFS in the presence of triphenylphosphine (TPP). Results of FT-IR and XPS confirmed successful modification of epoxy and novolac resins and also functionalization of GO with furfuryl alcohol and APTMS. Results of TGA showed that GFS reaches to char residue of 37.3% at 600 °C. Char residues of 44.4, 44.0, and 34.2% were obtained for the first, second, and third hybrid composites without GFS loading. Addition of 1 wt% of GFS into the hybrid networks results in increase of char residues to 56.3, 50.0, and 34.7%, respectively. So, the first hybrid composite reaches to the highest char residue at 600 °C. These hybrid composites showed degradation temperature of 416.4, 434.5, and 424.8 °C.

Preparation of Furfuryl Alcohol‐Functionalized Carbon Nanotube and Epoxidized Novolac Resin Composites with High Char Yield

Epoxidized novolac resin (ENR) composites with high thermal stability and char residue were prepared by incorporation of furfuryl alcohol‐modified carbon nanotubes (CNTFA). Modification of oxidized carbon nanotubes (CNTs) with furfuryl alcohol resulted in their improved dispersion in the resin matrix. After curing of ENR in the presence of CNTFA with ethylenediamine, thermally stable composites were obtained. Successful modification of CNTs with furfuryl alcohol was confirmed using Fourier‐transform infrared spectroscopy and thermogravimetric analysis (TGA). TGA results showed that degradation temperature and char residue of cured ENR were considerably increased by incorporation of CNTFA. CNTFA reached to char residue of 91.5% at 600°C, which shows that about 3.3 wt% of CNTFA is composed of furfuryl alcohol. Addition of 2 and 4 wt% of CNTFA into the ENR matrix results in increase of char content from 44.7% for to 45.4 and 49.4%, respectively. X‐ray diffraction showed that CNTFA was uniquely dispersed in the ENR matrix. Scanning electron microscopy and transmission electron microscopy images showed tubular and entangled structure of CNTFA. Finally, these results show that this approach can be considered in production of thermal‐resistant composites. POLYM. COMPOS., 39:E1231–E1236, 2018. © 2018 Society of Plastics Engineers

Preparation of hybrid composites based on epoxy, novolac, and epoxidized novolac resins and silica nanoparticles with high char residue by sol‐gel method

A facile method was developed for preparation of three hybrid composites by using tetraethyl orthosilicate oligomer‐modified epoxy resin (MER), (3‐glycidyloxypropyl) trimethoxysilane‐modified novolac resin (MNR), epoxidized novolac resin (ENR), and silica nanoparticles (SiO2). Accordingly, the first class of composites was prepared from MER and SiO2. The second class of composites was prepared from MER, MNR, and SiO2. And the third class of composites was prepared from silica MNR, ENR, and nanoparticles. All the modified resins and their composites were characterized by Fourier‐transform infrared spectroscopy and their thermal behavior was investigated by thermo gravimetric analysis. The obtained thermograms showed that thermal stability of hybrid composites were controlled by the amount of SiO2 and type of resins. Char yield of epoxy resin was increased significantly by formation of hybrid composites. The second class of composites showed higher char yields in comparison with the first class (52.1 compared with 23.2% for 8 wt% of SiO2). Incorporation of ENR instead of MER in the third class composites resulted in much more char residues of 60.2 and 60.6% for 4 and 8 wt% of SiO2. Therefore, third class composite with 8 wt% of SiO2 exhibited the highest char yield. Scanning electron and transmission electron microscopies were used to study the morphology and dimension of SiO2. POLYM. COMPOS., 39:E2316–E2323, 2018. © 2017 Society of Plastics Engineers

Thermal Stability and Fire Retardant Properties of Polyamide 11 Microcomposites Containing Different Lignins

This study investigates the influence of various lignins and their content on the thermal stability and fire retardancy of biobased polyamide 11 (PA). Microcomposites based on PA and containing 5, 10, 15, and 20 wt % different lignins were prepared with a twin-screw extruder. Morphological analysis showed good interfacial interaction and uniform distribution of lignin particles within the resulting microcomposites. Further, thermogravimetric analyses carried out in inert atmosphere indicated that, unlike kraft lignin, which is able to give rise to the formation of lower char residue (41–48 wt % at 600 °C), the sulfonated counterpart provides a higher thermal stability as well as a higher char residue (55–58 wt %). Furthermore, vertical flame spread tests clearly showed that 15 wt % is the optimum of kraft or sulfonated lignin loading to achieve improved flame retardant properties and a V1 rating. In addition, a cone calorimeter was exploited to study forced combustion behavior; in particular the microcomp...

A novel Schiff-base polyphosphate ester: Highly-efficient flame retardant for polyurethane elastomer

A novel Schiff-base polyphosphate ester (SPE) flame retardant was synthesized through melt polycondensation, and used to flame retard thermoplastic polyurethane elastomer (TPU). The SPE possessed high thermal stability and rich char residue under high temperature according to the thermogravimetric (TG) analysis. In combustion tests, the flame-retarded TPU passed the UL-94 V-0 rating, and had a limited oxygen index (LOI) of 29% when the content of SPE was only 5 wt%, meanwhile, the amount of dripping remarkably reduced. In cone calorimetry test, the peak of heat release rate (pHRR), average mass loss rate (AMLR), and maximum average rate of heat emission (MARHE) of the flame-retarded TPU with 5 wt% SPE were respectively decreased by 61.7%, 41.8%, and 30.2% compared with the corresponding value of neat TPU. All these results demonstrated that the SPE simultaneously improved the flame retardancy and dripping behavior of TPU. Thermogravimetric-Fourier transform infrared spectra (TG-FTIR), pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and laser Raman spectroscopy (LRS) illustrated that SPE simultaneously played a flame-retardant role in both condensed phase and gas phase.

Novel bio-based epoxidized cardanol/cenosphere syntactic foams

Cenosphere-filled epoxidized cardanol syntactic foams were fabricated using stir-casting technique: 10–40 wt% of cenosphere was mixed gradually in several steps in order to avoid any damage of the cenosphere. The syntactic foams were cured at room temperature for a day followed by postcure for 3 h at 100°C. Completion of the cure reaction was ascertained using differential scanning calorimetry of the fresh sample and postcured sample. Homogeneous distribution of cenosphere was confirmed with the scanning electron microscopic (SEM) images. The fracture mechanism was also analysed using SEM image of the compression failed sample. Thermal, hygrothermal and compressive properties of the syntactic foams were studied. Epoxidized cardanol-based syntactic foams were found to have lower density, good thermal stability and higher char residue as revealed from the thermogravimetric analysis result. The yield strength decreased with the increase in cenosphere. The specific modulus was optimum for 30% loading of cenosphere and it increased by 42% in comparison to the neat sample. Hygrothermal studies conducted using deionized water and sea water at room and high temperature conditions revealed stability and lower water absorption. The bio-based syntactic foams derived from cardanol promised sustainable path for the preparation of light-weight foam core materials.

Preparation of a Crosslinked Chitosan Coated Calcium Sulfate Whisker and Its Reinforcement in Polyvinyl Chloride

A calcium sulfate whisker (CSW) coated with glutaraldehyde crosslinked chitosan (GACS) was prepared to reinforce polyvinyl chloride (PVC) in this study. The results show that the optimum concentration of both chitosan (CS) and glutaraldehyde (GA) is 0.05 wt%. The tensile strength, impact strength, flexural modulus and vicat softening temperature of the PVC composite with 12 wt% of modified CSW are increased by 17.5%, 40.4%, 0.8% and 3.8% compared with those of the PVC composite with 12 wt% of unmodified CSW, and by 2.9%, 42.4%, 27.1% and 6.8% compared with those of pure PVC, respectively. The dynamic mechanical analysis results indicate that the modified CSW/PVC composite exhibits much higher storage modulus and glass transition temperature than those of unmodified CSW/PVC composite and pure PVC. In addition, the modified CSW/PVC composite also demonstrates good thermal properties with a high rapidest decomposition temperature (Trpd) and char residue. The scanning electron microscopy images of tensile-fractured surfaces show that the modified CSW has a strong interfacial adhesion with PVC matrix.

Sizing and Thermal Stability of Prepared Tetraaminophthalocyaninatocopper(II) Derivatives-grafted Polymers

Different polymers were prepared by condensation polymerization of sebacic anhydride and adipic anhydride with ethylene glycol and poly(ethylene glycol). Their number average molecular weights were determined by end group analysis. Then, they were grafted on the prepared phthalocyaninatocopper(II) compounds with the general formula (NH2)4PcCu(II) having amino groups of 3,3',3'',3'''- or 4,4',4'',4'''- positions. All prepared polymers, compounds, and phthalocyaninatocopper(II)-grafted polymers were characterized by FTIR. The sizing measurements were carried out in 3,3',3'',3'''- (NH2)4PcCu(II) and 4,4',4'',4'''- (NH2)4PcCu(II) compounds with and without grafting polymers. The results showed that the grafting process led to decreasing in particle size and increasing in surface area. The grafting process was reflected positively on the thermal degradation of 3,3',3'',3'''- (NH2)4PcCu(II) and 4,4',4'',4'''- (NH2)4PcCu(II) grafted polymers. They had higher thermal stability accompanied with higher char residue and T50% weight loss with 3,3',3'',3'''-(NH2)4PcCu(II) and their grafted polymers being the best.

Pyrolysis characteristics and kinetics of lignin derived from enzymatic hydrolysis residue of bamboo pretreated with white-rot fungus.

BackgroundThe lignocellulose biorefinery based on the sugar platform usually focuses on polysaccharide bioconversion, while lignin is only burned for energy recovery. Pyrolysis can provide a novel route for the efficient utilization of residual lignin obtained from the enzymatic hydrolysis of lignocellulose. The pyrolysis characteristics of residual lignin are usually significantly affected by the pretreatment process because of structural alteration of lignin during pretreatment. In recent years, biological pretreatment using white-rot fungi has attracted extensive attention, but there are only few reports on thermal conversion of lignin derived from enzymatic hydrolysis residue (EHRL) of the bio-pretreated lignocellulose. Therefore, the study investigated the pyrolysis characteristics and kinetics of EHRL obtained from bamboo pretreated with Echinodontium taxodii in order to evaluate the potential of thermal conversion processes of EHRL.ResultsFourier transform infrared spectroscopy spectra showed that EHRL of bamboo treated with E. taxodii had the typical lignin structure, but aromatic skeletal carbon and side chain of lignin were partially altered by the fungus. Thermogravimetric analysis indicated that EHRL pyrolysis at different heating rates could be divided into two depolymerization stages and covered a wide temperature range from 500 to 900 K. The thermal decomposition reaction can be well described by two third-order reactions. The kinetics study indicated that the EHRL of bamboo treated with white-rot fungus had lower apparent activation energies, lower peak temperatures of pyrolysis reaction, and higher char residue than the EHRL of raw bamboo. Pyrolysis–gas chromatography–mass spectrometry (Py–GC/MS) was applied to characterize the fast pyrolysis products of EHRL at 600 ℃. The ratios of guaiacyl-type to syringyl-type derivatives yield (G/S) and guaiacyl-type to p-hydroxy-phenylpropane-type derivatives yield (G/H) for the treated sample were increased by 33.18 and 25.30 % in comparison with the raw bamboo, respectively.ConclusionsThe structural alterations of lignin during pretreatment can decrease the thermal stability of EHRL from the bio-treated bamboo and concentrate the guaiacyl-type derivatives in the fast pyrolysis products. Thus, the pyrolysis can be a promising route for effective utilization of the enzymatic hydrolysis residue from bio-pretreated lignocellulose.

A Simple Way to Achieve Legible and Local Controllable Patterning for Polymers Based on a Near-Infrared Pulsed Laser.

This study developed a simple way to achieve legible and local controllable patterning for polymers based on a near-infrared (NIR) pulsed laser. The polycarbonate-coated nano antimony-doped tin oxide (nano ATO) was designed as a core-shell structure that was tailored to be responsive to a 1064 nm NIR laser. The globular morphology of polycarbonate-coated nano ATO with a diameter of around 2-3 μm was observed by scanning electron microscopy and transmission electron microscopy. This core-shell structure combined the excellent photothermal conversion efficiency of nano ATO and the high char (carbon) residue of polycarbonate. The X-ray photoelectron spectroscopy results of a polymer-patterning plate after laser irradiation demonstrated that, through local controlled photochromism, the well-defined legible patterns can be fabricated on the polymer surfaces contribute to the synergistic effect consisting of polycarbonate carbonization and nano ATO photothermal conversion. Furthermore, polymers doped with a minimal content of polycarbonate-coated nano ATO can achieve a remarkable patterning effect. This novel laser-patterning approach will have wide promising applications in the field of polymer NIR pulsed-laser patterning.

Sizing and Thermal Stability of Prepared Tetraaminophthalocyaninatocopper(II) Derivatives-grafted Polymers

Different polymers were prepared by condensation polymerization of sebacic anhydride and adipic anhydride with ethylene glycol and poly(ethylene glycol). Their number average molecular weights were determined by end group analysis. Then, they were grafted on the prepared phthalocyaninatocopper(II) compounds with the general formula (NH2)4PcCu(II) having amino groups of 3,3',3'',3'''- or 4,4',4'',4'''- positions. All prepared polymers, compounds, and phthalocyaninatocopper(II)-grafted polymers were characterized by FTIR. The sizing measurements were carried out in 3,3',3'',3'''- (NH2)4PcCu(II) and 4,4',4'',4'''- (NH2)4PcCu(II) compounds with and without grafting polymers. The results showed that the grafting process led to decreasing in particle size and increasing in surface area. The grafting process was reflected positively on the thermal degradation of 3,3',3'',3'''- (NH2)4PcCu(II) and 4,4',4'',4'''- (NH2)4PcCu(II) grafted polymers. They had higher thermal stability accompanied with higher char residue and T50% weight loss with 3,3',3'',3'''-(NH2)4PcCu(II) and their grafted polymers being the best.