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1.
A novel synthesis path for the monotelechelic polydimethylsiloxane with a diol‐end group, α‐butyl‐omega‐{3‐[2‐hydroxy‐3‐(N‐methyl‐N‐hydroxyethylamino)propoxy]propyl}polydimethylsiloxane, is described in this article. The preparation included three steps, which were anionic ring‐opening polymerization, hydrosilylation, and epoxy addition. The structure and polydispersity index of the products were analyzed and confirmed by FTIR, 1H NMR, 13C NMR, H? H, and C? H. Correlated Spectroscopy and gel permeation chromatography. The results demonstrated that each step was successfully carried out and the targeted products were accessed in all cases. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010  相似文献   

2.
2‐Mercapto‐5‐methylpyridine‐N‐oxide (MMPNO) and its sodium salt (NaMMPNO) were synthesized. The reaction of the latter with Fe3+ generates Fe(MMPNO)3 chelate. The thermolysis of this chelate at 350 °C yielded highly pure reddish‐brown γ‐Fe2O3 nanocrystallites with an average particle size of 6.2 nm, a particle size range of 4.2 to 14.8 nm, and a specific surface area of 51.5 m2g–1. The thermolysis process was optimized using the 22 fractional design. Quantitative tests and characterization of products were carried out by UV‐vis spectroscopy, XRD, LLS, SEM, TGA, BET, TEM, FT‐IR, elemental microanalysis, and classical analytical measurements.  相似文献   

3.
A novel, asymmetric diamine, 3‐(4‐aminophenylthio)‐N‐aminophthalimide, was prepared from 3‐chloro‐N‐aminophthalimide and 4‐aminobenzenethiol. The structure of the diamine was determined via IR and 1H‐NMR spectroscopy and elemental analysis. A series of polyimides were synthesized from 3‐(4‐aminophenylthio)‐N‐aminophthalimide and aromatic dianhydrides by a conventional two‐step method in N,N‐dimethylacetamide and by a one‐step method in phenols. These polyimides showed good solubility in 1‐methyl‐2‐pyrrolidinone, m‐cresol, and p‐chlorophenol, except polyimide from pyromellitic dianhydride, which was only soluble in p‐chlorophenol. The 5% weight loss temperatures of these polyimides ranged from 460 to 498°C in air. Dynamic mechanical thermal analysis indicated that the glass‐transition temperatures of the polyimides were in the range 278–395°C. The tensile strengths at break, moduli, and elongations of these polyimides were 146–178 MPa, 1.95–2.58 GPa, and 9.1–13.3%, respectively. Compared with corresponding polyimides from 4,4′‐diamiodiphenyl ether, these polymers showed enhanced solubility and higher glass‐transition temperatures. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008  相似文献   

4.
The graft copolymerization of butyl acrylate (BA) onto chitosan was tried via a new protection‐graft‐deprotection procedure. About 6‐O‐maleoyl‐N‐phthaloyl‐chitosan was synthesized and characterized by Fourier transform infrared spectra analysis (FT‐IR) and 1H‐NMR. Because the intermediate 6‐O‐maleoyl‐N‐phthaloyl‐chitosan was soluble in organic solvents, the graft copolymerization was carried out in a homogeneous system. Grafting was initiated by γ‐irradiation. The graft extent was dependent on the irradiation dose and the concentration of BA monomer, and copolymers with grafting above 100% were readily prepared. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 489–493, 2006  相似文献   

5.
In this work, 2‐(3‐p‐bromophenyl‐3‐methylcyclobutyl)‐2‐hydroxyethylmethacrylate (BPHEMA) [monomer] was synthesized by the addition of methacrylic acid to 1‐epoxyethyl‐3‐bromophenyl‐3‐methyl cyclobutane. The monomer and poly(BPHEMA) were characterized by FT‐IR and [1H] and [13C]NMR. Average molecular weight, glass transition temperature, solubility parameter, and density of the polymer were also determined. Thermal degradation of poly[BPHEMA] was studied by thermogravimetry (TG), FT‐IR. Programmed heating was carried out at 10 °C min−1 from room temperature to 500 °C. The partially degraded polymer was examined by FT‐IR spectroscopy. The degradation products were identified by using FT‐IR, [1H] and [13C]NMR and GC‐MS techniques. Depolymerization is the main reaction in thermal degradation of the polymer up to about 300 °C. Percentage of the monomer in CRF (Cold Ring Fraction) was estimated at 33% in the peak area of the GC curve. Intramolecular cyclization and cyclic anhydride type structures were observed at temperatures above 300 °C. The liquid products of the degradation, formation of anhydride ring structures and mechanism of degradation are discussed. © 1999 Society of Chemical Industry  相似文献   

6.
A new monomer 1,1‐bis(4‐amino‐3‐mercaptophenyl)‐4‐tert‐butylcyclohexane dihydrochloride, bearing the bulky pendant 4‐tert‐butylcyclohexylidene group, was synthesized from 4‐tert‐butylcyclohexanone in three steps. Its chemical structure was characterized by 1H NMR, 13C NMR, MS, FTIR, and EA. Aromatic poly(bisbenzothiazole)s (PBTs V) were prepared from the new monomer and five aromatic dicarboxylic acids by direct polycondensation. The inherent viscosities were in the range of 0.63–2.17 dL/g. These polymers exhibited good solubility and thermal stability. Most of the prepared PBTs V were soluble in various polar solvents. Thermogravimetric analysis showed the decomposition temperatures at 10% weight loss that were in the range of 495–534°C in nitrogen. All the PBTs V, characterized by X‐ray diffraction, were amorphous. The UV absorption spectra of PBTs V showed a range of λmax from 334 to 394 nm. All the PBTs V prepared had evident fluorescence emission peaks, ranging from 423 to 475 nm with different intensity. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 2000–2008, 2006  相似文献   

7.
The energetic material, 3‐nitro‐1,5‐bis(4,4′‐dimethyl azide)‐1,2,3‐triazolyl‐3‐azapentane (NDTAP), was firstly synthesized by means of Click Chemistry using 1,5‐diazido‐3‐nitrazapentane as main material. The structure of NDTAP was confirmed by IR, 1H NMR, and 13C NMR spectroscopy; mass spectrometry, and elemental analysis. The crystal structure of NDTAP was determined by X‐ray diffraction. It belongs to monoclinic system, space group C2/c with crystal parameters a=1.7285(8) nm, b=0.6061(3) nm, c=1.6712(8) nm, β=104.846(8)°, V=1.6924(13) nm3, Z=8, μ=0.109 mm−1, F(000)=752, and Dc=1.422 g cm−3. The thermal behavior and non‐isothermal decomposition kinetics of NDTAP were studied with DSC and TG‐DTG methods. The self‐accelerating decomposition temperature and critical temperature of thermal explosion are 195.5 and 208.2 °C, respectively. NDTAP presents good thermal stability and is insensitive.  相似文献   

8.
4,5‐Bis(5‐tetrazolyl)‐1,2,3‐triazole (BTT) was synthesized by a new method. Its structure was characterized by IR and 13C NMR spectroscopy and elemental analysis (EA). The thermal stability of BTT was investigated by TG‐DSC technique. The kinetic parameters including activation energy and pro‐exponential factor were calculated by Kissinger equation. The combustion heat, detonation products, hygroscopicity, impact, and friction sensitivity were also measured. The formation heat, detonation pressure, and detonation velocity of BTT were calculated. BTT has high detonation pressure and detonation velocity (P=35.36 GPa, D=8.971 km s−1). BTT has potential application prospect as environmentally friendly gas generant, insensitive explosive and solid propellant.  相似文献   

9.
Novel polyesters, poly[(ε‐caprolactone)‐co‐(N‐trityl‐L ‐serine‐β‐lactone)]s, were prepared by copolymerizing ε‐caprolactone (CL) with N‐trityl‐L ‐serine‐β‐lactone (TSL) using ZnEt2 as the catalyst. The number‐average molecular weights were determined which ranged from 2.7 × 104 to 4.9 × 104 Da with dispersity values ranging from 1.6 to 1.8. The structures of the copolymers were investigated by means of 1H NMR, 13C NMR and infrared spectroscopies, thermogravimetric analysis and differential scanning calorimetry. The results indicated that CL and TSL monomer units were randomly distributed within the copolymer backbone structures and the ratios of TSL to CL in the copolymers were close to those in the feeds. After removal of the trityl group under mild condition, a new polyester with side amino groups provided by serine units was obtained. L929 cell culturing test indicated good biocompatibility of the polyester with or without protective groups. © 2012 Society of Chemical Industry  相似文献   

10.
The ring‐opening polymerization of γ‐benzyl‐L ‐glutamate N‐carboxyanhydride (BLG‐NCA) was initiated by n‐hexylamine in N,N‐dimethyformamide under normal pressure at 0 °C. The products were characterizated by gel permeation chromatography, matrix‐assisted laser desorption/ionization time of flight mass spectroscopy (MALDI‐TOF MS), nuclear magnetic resonance etc. MALDI‐TOF MS gave direct evidence that the side reactions during the polymerization of BLG‐NCA could be greatly reduced by decreasing the reaction temperature, e.g. from room temperature to 0 °C. As a result, over 90% of the products were amino‐terminated poly(γ‐benzyl‐L ‐glutamate) (PBLG) with low polydispersity index when the polymerization was carried out at 0 °C, which could be used to re‐initiate the polymerization of other NCAs. Then several well‐defined PBLG‐containing block copolypeptides were successfully synthesized in a convenient way. Copyright © 2012 Society of Chemical Industry  相似文献   

11.
Poly‐α,β‐(3‐hydroxypropyl)‐DL ‐aspartamide (PHPA) was synthesized by the ring‐open reaction of polysuccinimide (PSI) and 3‐hydroxypropylamine. The polymer was characterized by 1H‐NMR, 13C‐NMR, FTIR, and GPC. Mark–Houwink coefficients were obtained from viscometry and GPC measurements, K = 5.53 × 10−3 and α = 0.78 in water. The acute toxicity of PHPA was examined and it revealed no death in ICR mice up to the dose treated of 15.3 kg/kg, and hematological parameters showed no significant difference between treated and control animals. The potential use of PHPA as a drug carrier was also investigated. In a typical case, a contraceptive drug, norethindrone (NET), was bonded to PHPA, and the drug sustained released as long as 120 days an in vitro test. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 2411–2417, 2000  相似文献   

12.
A novel π‐conjugated poly[di(p‐phenyleneethynylene)‐alt‐(p‐phenylenecyanovinylene)] having n‐octyloxy side chains (PPE‐C8PPE‐PPV) was prepared by polymerization of the monomer DEDB with BCN. Chemical structure of the polymer obtained was confirmed by 1H NMR, FTIR, and EA. PPE‐C8PPE‐PPV had a molecular weight enough to fabricate the electroluminescent (EL) device, and showed a good organosolubility, excellent thermal stability, and film‐forming property. In UV absorption and PL spectra in film it showed a maximum at 430 and 543 nm, respectively, which appeared 5 and 41 nm longer wavelengths than that of the solution, respectively. HOMO, LUMO energy levels and band gap were determined to be ?5.70, ?3.29, and 2.41 eV, respectively. Two EL devices with low‐work function cathodes were fabricated with the structures of ITO/PEDOT/PPE‐C8PPE‐PPV/cathodes (LiF/Al and Mg:Ag/Ag). The both devices exhibited a bright green light emission at 545 nm and the maximum luminescence of 197 cd/cm2 (LiF/Al) and 158 cd/cm2 (Mg:Ag/Ag). © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008  相似文献   

13.
3,3′‐Bisazidomethyl oxetane‐3‐azidomethyl‐3′‐methyl oxetane (BAMO‐AMMO) tri‐block copolymer was successfully synthesized by azidation of a polymeric substrate containing bromo leaving groups, and an alternative block energetic thermoplastic elastomer (ETPE) was prepared by chain extension reaction. The tri‐block copolymer was characterized by Fourier transform infrared (FTIR), 1H NMR, and 13C NMR spectroscopy, X‐ray diffraction (XRD), and thermogravimetric analysis (TGA). It was found that the composition of the copolymer is nearly 1 : 1; crystallinity of the copolymer (71.81 %) is less than that of PBAMO (78.30 %). This is due to a partly mixture between soft and hard segments. Kinetic result shows that a crosslinking network is formed after the decomposition of azide group. Tensile strength of alternative block ETPE is 150 % of traditionally synthesized BAMO‐AMMO ETPE.  相似文献   

14.
BACKGROUND: Biodegradable block copolymers have attracted particular attention in both fundamental and applied research because of their unique chain architecture, biodegradability and biocompatibility. Hence, biodegradable poly[((R )‐3 ‐hydroxybutyrate)‐block‐(D ,L ‐lactide)‐block‐(ε‐caprolactone)] (PHB‐PLA‐PCL) triblock copolymers were synthesized, characterized and evaluated for their biocompatibility. RESULTS: The results from nuclear magnetic resonance spectroscopy, gel permeation chromatography and thermogravimetric analysis showed that the novel triblock copolymers were successfully synthesized. Differential scanning calorimetry and wide‐angle X‐ray diffraction showed that the crystallinity of PHB in the copolymers decreased compared with methyl‐PHB (LMPHB) oligomer precursor. Blood compatibility experiments showed that the blood coagulation time became longer accompanied by a reduced number of platelets adhering to films of the copolymers with decreasing PHB content in the triblocks. Murine osteoblast MC3T3‐E1 cells cultured on the triblock copolymer films spread and proliferated significantly better compared with their growth on homopolymers of PHB, PLA and PCL, respectively. CONCLUSION: For the first time, PHB‐PLA‐PCL triblock copolymers were synthesized using low molecular weight LMPHB oligomer as the macroinitiator through ring‐opening polymerization with D ,L ‐lactide and ε‐caprolactone. The triblock copolymers exhibited flexible properties with good biocompatibility; they could be developed into promising biomedical materials for in vivo applications. Copyright © 2008 Society of Chemical Industry  相似文献   

15.
Summary: VP and co‐monomers DMAAm and ST were successfully grafted onto a PP fabric in an emulsion copolymerization process initiated by γ‐radiation. The radiation dose, concentration of VP, the ratio of VP/DMAAm and VP/ST in the reaction solution, and the reaction temperature dependent graft copolymerization were investigated. The order of dependence of the initial rate of grafting on the radiation dose was found to be in the range of 1.2 to 0.93 for VP; 0.84 to 0.70 for VP/DMAAm and for VP/ST was in the range of 0.59 to 0.41. The activation energy of the graft copolymer reaction was determined to be 40.18 J · mol?1 for 0.464 mol · L?1 VP. In the case of co‐monomer mixtures (VP/DMAAm: 0.464/0.5) the energy of activation was noticeably higher at 49.71 J · mol?1 while for VP/ST (0.464/0.436) the activation energy was same as that of VP. XRD results showed that overall crystallinity significantly decreased with the increase of graft weight with a noticeable change in the chemical structure of the PP, indicating that the graft copolymer reaction was taking place both in the amorphous and crystalline regions of PP. A similar characteristic behavior was also obtained by DSC, which revealed the presence of an endotherm process in the range of 25 to 130 °C depending on the degree of grafting, attributed to the grafted chains of the monomer/co‐monomers. In order to determine the graft copolymer reaction of VP, DMAAm and ST onto the backbone of PP, the reaction products were characterized by FTIR spectroscopy. A good correlation was found between changes of crystallinity and level of graft copolymerization as determined by WAXRD and DSC.

Typical XRD traces of as‐received PP fabric (PPF) and grafted with VP (PPF‐g‐VP).  相似文献   


16.
Isomers of 4‐amino‐1,3‐dinitrotriazol‐5‐one‐2‐oxide (ADNTONO) are of interest in the contest of insensitive explosives and were found to have true local energy minima at the DFT‐B3LYP/aug‐cc‐pVDZ level. The optimized structures, vibrational frequencies and thermodynamic values for triazol‐5‐one N‐oxides were obtained in their ground state. Kamlet‐Jacob equations were used to evaluate the performance properties. The detonation properties of ADNTONO (D=10.15 to 10.46 km s−1, P=50.86 to 54.25 GPa) are higher compared with those of 1,1‐diamino‐2,2‐dinitroethylene (D=8.87 km s−1, P=32.75 GPa), 5‐nitro‐1,2,4‐triazol‐3‐one (D=8.56 km s−1, P=31.12 GPa), 1,2,4,5‐tetrazine‐3,6‐diamine‐1,4‐dioxide (D=8.78 km s−1, P=31.0 GPa), 1‐amino‐3,4,5‐trinitropyrazole (D=9.31 km s−1, P=40.13 GPa), 4,4′‐dinitro‐3,3′‐bifurazan (D=8.80 km s−1, P=35.60 GPa) and 3,4‐bis(3‐nitrofurazan‐4‐yl)furoxan (D=9.25 km s−1, P=39.54 GPa). The  NH2 group(s) appears to be particularly promising area for investigation since it may lead to two desirable consequences of higher stability (insensitivity), higher density, and thus detonation velocity and pressure.  相似文献   

17.
Poly(2‐acrylamido glycolic acid‐co‐2‐acrylamido‐2‐methyl‐1‐propane sulfonic acid) [P(AGA‐co‐APSA)] was synthesized by radical polymerization in an aqueous solution. The water‐soluble polymer, containing secondary amide, hydroxyl, carboxylic, and sulfonic acid groups, was investigated, in view of their metal‐ion‐binding properties, as a polychelatogen with the liquid‐phase polymer‐based retention technique under different experimental conditions. The investigated metal ions were Ag+, Co2+, Ni2+, Cu2+, Zn2+, Cd2+, Pb2+, and Cr3+, and these were studied at pHs 3, 5, and 7. P(AGA‐co‐APSA) showed efficient retention of all metal ions at the pHs studied, with a minimum of 60% for Co(II) at pH 3 and a maximum close to 100% at pH 7 for all metal ions. The maximum retention capacity (n metal ion/n polymer) ranged from 0.22 for Cd2+ to 0.34 for Ag+. The antibacterial activity of Ag+, Cu2+, Zn2+, and Cd2+ polymer–metal complexes was studied, and P(AGA‐co‐APSA)–Cd2+ presented selective antibacterial activity for Staphylococcus aureus with a minimum inhibitory concentration of 2 μg/mL. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009  相似文献   

18.
Polyamides (PAs) containing fluorene, oxyether, and diphenyl‐silane moieties in the repeating unit were synthesized in > 85% yield by direct polycondesation between a diamine and four dicarboxylic acids. Alternatively, one PA was synthesized from an acid dichloride. The diamine 4‐[4‐[9‐[4‐(4‐aminophenoxy)‐3‐methyl‐phenyl]fluoren‐9‐yl]‐2‐methyl‐phenoxy]aniline ( 3 ) was obtained from the corresponding dinitro compound, which was synthesized by nucleophilic aromatic halogen displacement from p‐chloronitrobenzene and 9,9‐bis (4‐hydroxy‐3‐methyl‐phenyl)fluorene ( 1 ). Monomers and polymers were characterized by FTIR and 1H, 13C, and 29Si‐NMR spectroscopy and the results were in agreement with the proposed structures. PAs showed inherent viscosity values between 0.14 and 0.43 dL/g, indicative of low molecular weight species, probably of oligomeric nature. The glass transition temperature (Tg) values were observed in the 188–211°C range by DSC analysis. Thermal decomposition temperature (TDT10%) values were above 400°C due to the presence of the aromatic rings in the diamine. All PAs showed good transparency in the visible region (>88% at 400 nm) due to the incorporation of the fluorene moiety. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

19.
Radiation‐induced graft polymerization of low‐density polyethylene with N‐vinylpyrrolidone, LDPE‐g‐PNVP, was used as a starting material for the synthesis of polyfunctionally substituted heterocyclic products. Thus, LDPE‐g‐PNVP reacts with ylidenemalononitrile derivatives to give the Michael addition products. In multistep reaction, LDPE‐g‐PNVP reacts with N,N‐dimethylformamide dimethyl acetal (DMFDMA), hydrazine hydrate and malononitrile, respectively, to give a hydropyrrolopyridazine derivative. The latter could also be prepared via the reaction of LDPE‐g‐PNVP with DMFDMA, followed by treating with cyanoacetohydrazide. Also, LDPE‐g‐PNVP reacts with malononitrile to give an adduct product, dimer malononitrile derivative 13. The latter reacts with sulfur element to afford the thiophene derivative. Furthermore, this adduct reacts with hydrazine hydrate to isolate the original starting material, LDPE‐g‐PNVP, and aminopyridine derivative. The resulted films were characterized by infrared (IR) spectroscopy, 1H nuclear magnetic resonance (1H‐NMR) mass spectroscopy, elemental analysis, swelling behavior, and electron scanning microscope. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 74: 2963–2970, 1999  相似文献   

20.
A new polymerizable 1,1′‐bi‐2‐naphthol derivative for polymer‐supported catalytic asymmetric synthesis is presented. The synthesis is conducted within a single reaction step, which is a major advantage over other approaches presented in the literature. The ligand‐bearing polymer is prepared through copolymerization with N‐isopropylacrylamide. Preliminary experiments on the utility in catalytic asymmetric alkylation reactions reveal the accessibility and activity of the polymer‐attached catalysts. The stereoselectivity of the reaction is found to be somewhat lower than for reactions performed in the presence of free 1,1′‐bi‐2‐naphthol, and thus requires further optimization. The enantiomeric excess of the reaction products was determined via 1H NMR spectroscopy after chiral derivatization with (R)‐α‐methylbenzyl isocyanate. © 2015 Society of Chemical Industry  相似文献   

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