Ring‐opening graft polymerization of L‐lactide onto starch granules in an ionic liquid

A room temperature ionic liquid 1‐allyl‐3‐methylimidazolium chloride ([AMIM]Cl) was a promising direct solvent for starch and nonderivitizing solvent for starch‐effective dissolution, in which the ring‐opening graft polymerization (ROGP) of L ‐lactide (L ‐LA) onto starch chains was carried out homogeneously. The obtained starch grafted poly(L ‐lactide) (starch‐g‐PLLA) was characterized by FTIR, ¹³C NMR, DSC, and WAXD, and the good adhesion between the two components was evidenced by SEM observations although the chains of grafted PLLA were not long. The grafting efficiency of PLLA reached 30% when the ROGP proceeded at 100°C for 10 h with L ‐LA/starch 0.5 : 1 (wt/wt) and stannous octoate (Sn(Oct)₂) as a catalyst, which was calculated according to a standard curve newly created by FTIR method. The homopolymerization of L ‐LA and the disconnection of grafted PLLA from starch‐g‐PLLA were the main competition reactions. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Grafting of poly(vinyl chloride) and polypropylene with styrene in a supercritical CO2 solvent medium: Synthesis and characterization

Graft copolymerization of styrene onto poly(vinyl chloride) (PVC) and polypropylene (PP) was carried out in a supercritical CO₂ medium using AIBN as a free radical initiator. The supercritical CO₂ medium served as a reaction medium in addition to being a solvent for the styrene monomer and the free radical initiator. The reaction temperature and pressure were kept above the critical points of the solvent‐monomer mixture to form a homogeneous single‐phase medium. The resulting graft copolymers were characterized using Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and nuclear magnetic resonance (NMR) techniques. The weight percent of grafting was determined using IR absorbance ratio technique. TGA results showed that the thermal stabilily of grafted copolymer of PVC was better than that of PVC, while grafted copolymer of PP had poorer thermal stability than PP. DSC results showed that glass transition temperatures (T_g's) of the grafted copolymers were higher than those of the starting polymers PVC and PP. The presence of polystyrene attached to the backbone polymer was confirmed by ¹H NMR and ¹³C NMR analyses.     

Effect of amphoteric grafting branch on the adhesion of starch to textile fibers

Starch-g-poly(2-methacryloyloxyethyl trimethyl ammonium chloride-co-acrylic acid) (starch-g-P(DMC/AA)) with different zeta potentials was prepared via the graft copolymerization of acid-thinned cornstarch (ATS) with 2-methacryloyloxyethyl trimethyl ammonium chloride (DMC) and acrylic acid (AA) in aqueous medium using Fe²⁺–H₂O₂ initiator. The investigation was carried out to reveal the influence of amphoteric branches grafted onto starch chains upon the adhesion of starch to textile fibers. Zeta potential of starch-g-P(DMC/AA) was adjusted by altering the mole ratio of DMC to AA charged into the copolymerization system. The adhesion was evaluated in terms of bonding strength and specific bonding strength of slightly sized roving based on a legal method (FZ/T 15001-2008) through the comparison of the amphoteric branch-grafted starch with ATS, starch-g-PAA, and starch-g-PDMC for warp sizing. It was found that the charged branches grafted onto starch chains were able to significantly enhance the adhesion. Zeta potential, depending on the mole ratio of DMC to AA units in the grafting branches, showed evident effect on the adhesion and desizability of the grafted starch. Increase in the potential favored to improve the adhesion, but disfavored the removal of the starch from sized warps. Alkali-oxidant agent desizing test confirmed that the starch-g-P(DMC/AA) with neutral potential was desizable. The amphoteric branch-grafted starch exhibited potential application as size base materials in warp sizing operation if its zeta potential was neutral.     

Graft copolymerization of water‐soluble monomers containing quaternary ammonium group on poly(vinyl alcohol) using ceric ions

Graft copolymerization of water‐soluble monomers containing quaternary ammonium onto PVA was studied in an aqueous medium using ceric ammonium nitrate‐nitric acid as the redox initiator. To optimize the reaction conditions for obtaining a maximum percent of grafting, the concentrations of methacryloxyethyl trimethylammonium chloride (DMC) monomer, ceric ammonium nitrate, and temperature were varied, and the effects on the grafting copolymerization were discussed. Under optimum conditions, a series of water‐soluble monomers containing quaternary ammonium, such as methacryloxyethyl trimethylammonium chloride (DMC), DMAEMA^˙C₂H₅Br, DMAEMA^˙C₄H₉Br, DMAEMA^˙C₁₆H₃₃Br, and DMAEMA^˙C₇H₇Cl, were successfully grafted onto PVA. The resulting grafted PVA were characterized with IR, NMR, and viscosity measurements. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 2186–2191, 2005     

Synthesis and characterization of polyacrylonitrile pregelled starch graft copolymers using ferrous sulfate‐hydrogen peroxide redox initiation system as surface sizing agent

A graft copolymer was synthesized by graft copolymerization of starch with styrene (St) and butyl acrylate (BA), using ferrous sulfate‐hydrogen peroxide redox initiation system. The starch was pregelled in the presence of acrylonitrile (AN) in aqueous alkali at high temperature before graft polymerization. Major factors affecting the polymerization reaction were investigated. It was found that a graft copolymer with higher percentage conversion (PC), graft efficiency (GE) and graft percentage (GP) was obtained by controlling the initiator concentration, concentration, and ratio of monomers and polymerization temperature. The optimum conditions were as follows: H₂O₂ concentration, 12%; monomer concentration, 120%; St/BA ratio, 1 : 1; polymerization temperature, 65°C. Fourier transform infrared spectroscopy and NMR analyses were used to gain information on the structure of the products. It was demonstrated that St, BA, and AN had been successfully grafted onto starch and ? CN had been saponified into ? CONH₂ and ? COO^? to a certain degree when pregelling. Scanning electron microscope micrographs showed the coarse structure and broad network. The graft polymerization took place on the surface of starch granule and led to amorphization of the starch structure. Graft polymer had better thermal stability and was endowed with pseudo‐plasticity. It was observed that the starch graft copolymer offers good properties such as water resistance as surface‐sizing agent. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Poly(ethylene glycol) grafted polystyrene dendrimer resins: Novel class of supports for solid phase peptide synthesis

Poly(propyleneglycol)dimethacrylate cross-linked support using monomers Styrene and 4-chloromethyl styrene (PS-PPGDMA-VBC resin) was prepared by suspension polymerization method. Dendritic templates were synthesized from Schiff base and trimesic acid molecules and assembled independently on PS-PPGDMA-VBC support to the second generation. N,N-bischloro ethyl amine dendrimer was generated from Schiff base units and introduced to the chloromethyl groups uniquely through secondary amine. It was followed by acidolytic cleavage, diazotization and thionyl chloride reactions leading to first generation dendrimer. O-benzyl ether dendrimer was created using 1,3,5-tris(hydroxyl methyl)benzene unit which was produced by the LiAlH₄ reduction of carbonyl groups of trimesic acid molecule. The hydroxyl methyl groups formed were converted to chloro methyl groups by adding thionyl chloride that leads to first generation dendrimer. Similar synthetic routes were followed to produce second generation dendrimers too. Poly(ethylene glycol), M_n ≈ 1500) has been grafted to chlorine termini of both dendrimers and used to check various physical and chemical properties of different peptide synthetic conditions. Reactions were qualitatively analyzed by FTIR, ¹³C NMR, SEM and quantitatively analyzed by UV measurements and CHN analysis. Classically difficult ACP sequence was synthesized on both PEGylated dendrimer supports and compared to Tenta Gel. Biologically significant disulfide bonded endothelin class of peptides were also synthesized using novel supports using various literature reported methods.     

Synthesis and characterization of fullerene functionalized poly(vinyl chloride) (PVC) and dehydrochlorinated PVC using atom Transfer Radical Addition and AIBN based fullerenation

The research presented details chemical modifications of poly(vinyl chloride) (PVC) and its derivative, dehydrochlorinated PVC (DH‐PVC) through the use of two grafting techniques, namely a normal fullerenation, using AIBN (2,2′‐Azoisobutyronitrile), and the atom transfer radical addition (ATRA). The products were characterized and the presence of new FTIR peaks at 528 and 577 cm^?1 along with new ¹H‐NMR signal at 3.9 ppm, suggested that fullerenes has been grafted to the polymer molecules. Percentage of C₆₀ in the fullerene grated products determined by UV/Visible spectroscopy initially increased with the amount of fullerene used to a maximum value (～5.66 % wt) before decreasing again. It was also determined that the C₆₀ content of the fullerene grafted PVC product prepared by using ATRA, was notably greater than that obtained using the normal fullerenation approach, regardless of the amount of C₆₀ used. When the dehydrochlorinated PVC was used as the starting polymer for fullerenation, the fullerene grafted DH‐PVC using ATRA, was markedly insoluble in many common solvents (THF and dichlorobenzene). This was not the cases for the fullerene grafted DHPVC prepared via an AIBN based fullerenation. Furthermore, the electrical conductivity values of the modified PVC products determined by using a four‐point probe method were found to increase linearly with the amount of C₆₀ present. Overall our data suggest that the suitable and efficient techniques for grafting C₆₀ onto PVC and DHPVC chains are ATRA and AIBN‐based fullerenation, respectively. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 130: 2410–2421, 2013     

Chitosan-<Emphasis Type="Italic">g</Emphasis>-poly(4-acrylamidobenzenesulfonamide) copolymers: synthesis,characterization, and bioactivity

The monomer, 4-acrylamidobenzenesulfonamide (ABS), was synthesized via reaction of acryloyl chloride with 4-aminobenzenesulfonamide in acetone at 0 °C. This monomer was then grafted onto chitosan using solution containing 2% acetic acid and mixture of K₂S₂O₈ and Na₂SO₃ as the redox promoter. An optimal G% of 150% was obtained when the process is conducted at 60 °C for 3 h employing 3.0 × 10^?3 M K₂S₂O₈ and 1.5 × 10^?3 M Na₂SO₃. The graft copolymers, chitosan-g-poly(4-acrylamidobenzenesulfonamide), were characterized by using FTIR, XRD, and SEM. The results were shown that the crystallinity of chitosan is enhanced by increasing the monomer content through the grafting process. Potential Antimicrobial activities of the permethyl ammonium salt forms of chitosan and its grafted copolymers against selected microorganisms were evaluated. The results show that the graft copolymers display better inhibitory effects on the growth of bacteria and some fungi than does chitosan.     

One simple and stable coating of mixed‐charge copolymers on poly(vinyl chloride) films to improve antifouling efficiency

An antifouling surface is highly desirable for many biomedical applications. In this study, poly(vinyl chloride) (PVC) films were endowed with the improved properties of resisting nonspecific protein adsorption and platelet adhesion simply through being coated with a kind of mixed‐charge zwitterionic polymer, poly(3‐sulfopropyl methacrylate–methacrylatoethyl trimethyl ammonium chloride–glycidyl methacrylate) (PSTG), with random moieties of negatively charged 3‐sulfopropyl methacrylate potassium, positively charged [2‐(methacryloyloxy)‐ethyl] trimethylammonium chloride, and glycidyl methacrylate. The PSTG‐grafted PVC films were formed by the simple immersion of an amino‐functionalized PVC film into a PSTG solution. A grafting density of 220.84 µg/cm² of PSTG4‐grafted PVC film was successfully obtained. The PSTG4‐grafted PVC film showed a lower contact angle (37.5 °) than the ungrafted PVC film (98.3 °). The in vitro protein adsorption results show that the bovine serum albumin adsorption amount decreased 6.72 µg/cm² in the case of the PSTG4‐grafted PVC film, whereas that on the ungrafted PVC film was 28.54 µg/cm². So, PSTG‐grafted PVC films could be promising materials for medical devices. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44632.     

Study on preparation and properties of gel polymer electrolytes based on comb-like copolymer matrix of poly(ethylene glycol) monomethylether grafted carboxylated butadiene-acrylonitrile rubber

A novel kind of gel polymer electrolytes (GPE) based on comb-like copolymers of poly(ethylene glycol) monomethylether (mPEG) grafted carboxylated butadiene-acrylonitrile rubber (XNBR) were prepared by introducing ionic liquids and LiClO₄ into polymer framework. FTIR spectra confirmed the grafting of mPEG to XNBR as side chains, and the content of grafted mPEG were calculated from the integral area of related peaks in ¹ H NMR spectra. Such grafted copolymer based GPE with ionic liquids as solvent showed higher ionic conductivity and reached a maximum ionic conductivity of 1.64?×?10^?3?S/cm (30?°C) in the experimental range, because the copolymers performed better polymer chain flexibility, which could be concluded from the decrease of T _g and crystallinity through DSC analysis. The generated GPE exhibited high electrochemical stability and the unit cell of LiFePO₄/GPE/Li could be cycled at room temperature.     

Graft copolymerization onto starch. II. Grafting of acrylonitrile to granular native potato starch by manganic pyrophosphate initiation. Effect of reaction conditions on grafting parameters

The effect of reaction conditions on the composition of native potato starch–polyacrylonitrile graft copolymers initiated by manganic pyrophosphate onto starch slurries at 30°C has been examined. In general, when the Mn³⁺ ion concentration was increased from 0.15 × 10^?3M to 3.0 × 10^?3M (other conditions kept constant), an increase in conversion of monomer to polymer and % add-on was observed, whereas frequency of grafts (anhydroglucose units, AGU, per grafted chain) decreased. Also, the average molecular weights of grafts showed a decrease from 2.2 × 10⁵ to 1.5 × 10⁵. Increasing the concentration ratio of starch to monomer during polymerization by a factor of 3 produced an increase in the conversion of monomer to polymer, whereas an increase in frequency of grafts (AGU/chain) was obtained. Values of % add-on and average molecular weights of the grafts showed, however, a decreasing tendency. It was observed that grafting onto starch took place readily even at acid additions as low as 10 × 10^?3M H₂SO₄ (pH ?1.8). Selective solvent extraction of homopolymer and extremely low conversions of monomer to polymer (0.1%–1.5%) in duplicate runs without addition of starch indicated that grafting efficiencies were high in all cases. An attempt has been made to interpret the results in terms of variations in factors such as initial ratio of (Mn³⁺)/(AGU), termination rate of acrylonitrile chain radicals by oxidation by Mn³⁺ ions, oxidation rate of radicals formed on anhydroglucose units by Mn³⁺ ions, and physical factors such as diffusion rate of Mn³⁺ ions through the polyacrylonitrile-grafted starch granules for terminating the radicals.     

Amine-terminated aromatic and semi-aromatic hyperbranched polyamides: synthesis and characterization

A facile synthetic approach to aromatic and semiaromatic amine-terminated hyperbranched polyamides via direct polymerization of triamine (B₃) with different diacid chlorides (A₂) was explored. An aromatic triamine, 1,3,5-tris(4′-aminophenylcarbamoyl)benzene (TAPCB), was synthesized and monomers were characterized by elemental analysis, FTIR, ¹H and ¹³C NMR spectroscopy. Finally, the polycondensation reaction of TAPCB with terephthaloyl chloride (TPC), isophthaloyl chloride (IPC), sebacoyl chloride (SC) and adipoyl chloride (AC) resulted in the preparation of four hyperbranched polyamides i.e., HBPA 1, 2, 3 and 4, respectively. FTIR and ¹H NMR analyses confirmed the structures of the ensuing polymers and DB was found between 0.51–0.55. These thermally stable amorphous HBPAs were soluble in polar aprotic solvents at room temperature having glass transition temperatures (T_g) between 138–198 °C. Inherent viscosities (η_inh) and weight average molecular weights (M_w) were in the range of 0.27–0.35 dL/g and 1.3 × 10⁴–2.7 × 10⁴, respectively. Future prospects are envisaged.     

Cationic starch iodophores

Cross‐linked cationic starches N‐(2‐hydroxyl)propyl‐3‐trimethyl ammonium starch chloride (CQS chloride), N‐(2‐hydroxyl)propyl‐3‐trimethyl ammonium starch iodide (CQS iodide), and N‐(2‐hydroxyl)propyl‐3‐trimethyl ammonium starch iodide–iodine (CQS triiodide) with the degree of substitution (DS) according to cationic groups from 0.04 to 0.62, as well as cross‐linked starch–iodine complexes were synthesized and tested as potential antibacterial agents. Cationic starch iodine derivatives were obtained during ion exchange reaction between CQS chloride and iodide or iodide–iodine anions in aqueous solutions. CQS_DS≤0.3 chloride can form several types of iodine complexes, such as the blue amylose–iodine inclusion complex and ionic CQS⁺I^?·(I₂)_m complex (m ≥ 1). The antibacterial activity of modified starches–iodine samples against different pathogenic bacterial cultures and contaminated water microorganisms was evaluated. CQS chloride and CQS iodide were found to be bacteriostatic. A strong antibacterial activity was characteristic of CQS triiodides in which molecular iodine is present in both ionic and inclusion complexes. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Thermodynamic and Surface Properties of Aqueous 1-Dodecyl-3-Methylimidazolium Chloride [C12mim][Cl] Solution in the Presence of a Series of Inorganic Salts

The micellization behavior of amphiphiles is a well-analyzed physicochemical phenomenon, which can be easily influenced by various parameters such as pressure, temperature, and the presence of different additives. Inorganic salts are able to affect the thermodynamic and surface properties of amphiphiles significantly. The effect of a series of salts as additives namely lithium chloride (LiCl), potassium chloride (KCl), sodium chloride (NaCl), sodium bromide (NaBr), and sodium iodide (NaI) on interfacial chemical characteristics of the surface-active ionic liquid (SAIL) 1-dodecyl-3-methylimidazolium chloride [C₁₂mim][Cl] in aqueous solution were examined through conductance, surface tension, fluorescence, ¹H NMR, and dynamic light scattering measurements. The interfacial and thermodynamic parameters of all investigated SAIL-salt systems were evaluated from surface tension and conductance measurements, respectively. A detailed analysis of the microenvironment of the micelles and the size of the micelles was done using ¹H NMR and dynamic light scattering measurements.     

Starch‐g‐polycaprolactone copolymerization using diisocyanate intermediates and thermal characteristics of the copolymers

Starch‐g‐polycaprolactone copolymers were prepared by two‐step reactions. The diisocyanate‐terminated polycaprolactone (NCO–PCL) was prepared by introducing NCO on both hydroxyl ends of PCL using diisocyanates (DI) at a molar ratio between PCL and DI of 2:3. Then, the NCO–PCL was grafted onto corn starch at a weight ratio between starch and NCO–PCL of 2:1. The chemical structure of NCO–PCL and the starch‐g‐PCL copolymers were confirmed by using FTIR and ¹³C‐NMR spectrometers, and then the thermal characteristics of the copolymers were investigated by DSC and TGA. By introducing NCO to PCL (M_n : 1250), the melting temperature (T_m ) was reduced from 58 to 45°C. In addition, by grafting the NCO–PCL (35–38%) prepared with 2,4‐tolylene diisocyanate (TDI) or 4,4‐diphenylmethane diisocyanate (MDI) onto starch, the glass transition temperatures (T_g 's) of the copolymers were both 238°C. With hexamethylene diisocyanate (HDI), however, T_g was found to be 195°C. The initial thermal degradation temperature of the starch‐g‐PCL copolymers were higher than that of unreacted starch (320 versus 290°C) when MDI was used, whereas the copolymers prepared with TDI or HDI underwent little change. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 78: 986–993, 2000     

Graft copolymerization of methyl acrylate onto sago starch using ceric ammonium nitrate as an initiator

The graft copolymerization of methyl acrylate onto sago starch was carried out by a free radical initiating process. The free radicals were produced by the chemical initiation method in which ceric ammonium nitrate was used as an initiator. It was found that the percentages of grafting, grafting efficiency, and rate of grafting were all dependent on the concentration of ceric ammonium nitrate (CAN), methyl acrylate (MA), sago starch (AGU), mineral acid (H₂SO₄), and reaction temperature and period. The variables affecting the graft copolymerization were thoroughly examined. The optimum yield of grafting was obtained when the concentration of CAN, MA, AGU, and H₂SO₄ were used at 8.77 × 10⁻³, 0.803, 0.135, and 0.175 mol L⁻¹, respectively. The optimum reaction temperature and period were 50°C and 60 min, respectively. The rate of graft polymerization was explored on the basis of experimental results and reaction mechanism. The evidence of grafted copolymers was investigated by using FTIR spectroscopy, TG, and DSC analysis. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 76: 516–523, 2000     

Antifouling performance of poly(acrylonitrile)-based membranes: From green synthesis to application

In order to develop clean ultrafiltration membranes able to prevent the fouling of biological compounds in filtration processes, poly(ethylene glycol) methyl ether acrylate (PEGA) was grafted to poly(acrylonitrile) (PAN) by free-radical polymerization in supercritical carbon dioxide (scCO₂) and the grafted copolymer was blended with PAN to fabricate porous membranes using scCO₂-induced phase inversion method. Fourier transform infrared (FT-IR) analysis, ¹H nuclear magnetic resonance (¹H NMR) and differential scanning calorimetry (DSC) confirmed that the poly(acrylonitrile)-graft-poly(ethylene oxide) (PAN-g-PEO) was successfully synthesized, for the first time, in scCO₂. The effect of increasing PEGA content on the initial monomer feed mixture on graft polymer morphology and average molecular weight was studied. Blended membranes with different PEGA contents were investigated by scanning electron microscopy (SEM), mercury porosimetry and dynamical mechanical analysis (DMA) to characterize their morphological, physico-chemical and mechanical properties. Moreover, water contact angle measurements, pure water permeability and filtration experiments were performed to evaluate membrane hydrophilicity and fouling resistance properties. Permeation experiments of model foulants, bovine serum albumin (BSA) and starch solutions were used to investigate antifouling character of blend membranes at different pHs. PAN:PAN-g-PEO (70:30) showed to be the ultrafiltration membrane with best performance. Furthermore, comparing with conventional technologies blended membranes of PAN:PAN-g-PEO prepared by a scCO₂-assisted process showed enhanced hydrophilicity, larger protein and starch solution permeabilities and good resistance to irreversible fouling, indicating that the technology is an efficient process to prepare fouling resistant membranes for biomacromolecule separations.     

碱性嫁接型离子液体催化二氧化碳环加成反应

采用后嫁接法将不同量的1-甲基-3-丙基(三乙氧基硅基)咪唑的氢氧化物(［Smim］OH)嫁接到介孔硅胶(SiO₂)上,采用傅里叶变换红外光谱、元素分析、硅核磁共振及热重分析等技术对所制备的材料进行表征。在无溶剂、温和的条件下,将碱性嫁接型离子液体用于CO₂与环氧丙烷(PO)合成碳酸丙烯酯(PC)的环加成反应来考察其催化活性。结果表明,离子液体［Smim］OH成功地以共价键嫁接到介孔硅胶上得到碱性嫁接型离子液体(GILs),但不同量的［Smim］OH嫁接程度有所不同;在优化条件下,PO的转化率为99.5%,选择性为100%。反应后催化剂经过滤即可分离回收利用,且多次使用仍保持较高的反应活性。     

Thermoreversible crosslinked thermoplastic starch

A novel furan‐modified thermoreversible crosslinked thermoplastic starch was synthesized. The crosslinking mechanism was based on a thermoreversible furan/maleimide adduct formed by the Diels ? Alder reaction. Thermoplastic starch (TPS) was first modified by forming a urethane linkage between the product of the reaction of furfuryl alcohol with 4,4‐methylene diphenyldiisocyanate and a starch hydroxyl group. Crosslinking was then achieved by the addition of 1,1′‐(methylene‐di‐4,1‐phenylene) bismaleimide to the furan‐grafted starch in solution (dimethylsulfoxide) and in the molten state during conventional extrusion. The materials were characterized by Fourier transform infrared and ¹H NMR spectroscopy. The thermoreversible reaction was assessed by viscosity measurement and ¹H NMR, for the system in dimethylsulfoxide, and by solubility tests, hot‐pressing experiments and dynamic mechanical analysis measurements for the extruded product. The crosslinked product showed a higher storage modulus and water resistance than its non‐crosslinked counterpart, opening novel opportunities to widen the range of TPS applications. © 2015 Society of Chemical Industry     

The preparation of multi-walled carbon nanotubes encapsulated by poly(3-acrylaminopropylsiloxane) with silica nanospheres on the polymer surface

A silica-polymer-carbon nanotube hybrid was prepared in which the nanotubes were encapsulated by poly(3-acrylaminopropylsiloxane) with silica nanospheres on the polymer surface. First, highly reactive poly(acryloyl chloride) (PAC) was grafted onto the nanotubes through the reaction of side acyl chloride groups with hydroxyl groups present on the surface of acid-oxidized nanotubes. Second, reacting 3-aminopropyltriethoxysilane with the grafted PAC through the reaction between amino and acyl chloride groups, siloxane-containing sub-grafts were introduced onto the primary PAC grafts. Third, silica nanospheres were covalently linked to the sub-grafts by condensation to form a nanotube-polymer-silica hybrid. Each intermediate structure was confirmed by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscopy (TEM). TEM observation revealed a nanostructure in which the nanotube was encapsulated with a polymer layer bearing silica nanospheres on its surface.