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EN
The interfacial structure and binding forces of polytrimethylene terephthalate/polyethylene terephthalate filament were investigated through the methods of Carbon-13 nuclear magnetic resonance (13C-NMR), differential scanning calorimeter (DSC), scanning electron microscopy (SEM) and optical microscopy. When two molten polymers met during the spinning process, an interface layer between the PTT and PET components formed and played an important role in binding the two components together. When the blending time was sufficient, an ester-interchange reaction took place with the generation of the copolymer. The PET recrystallisation was observed in the DSC curve under the influence of entangled PTT molecular chains. The morphology of the cross-section and side view proved that the linear boundary line was short and weaker in binding without a chemical bond and molecular diffusion. Side-by-side bi-component fiber and split-type fiber was able to be controllably spun by adjusting the spinning parameters.
EN
In this article, we report the synthesis and characterization of silver dispersed poly(m-toluidine-co-2-bromoaniline) copolymer synthesized by chemical oxidative polymerization method. The synthesized copolymer composites were subjected to different analytical characterization methods, such as FT-IR, UV, XRD, SEM, photoluminescence and electrical conductivity studies. All the polymer samples are found to be soluble in common organic solvents. UV absorption spectra show a red shift when silver nanoparticles are dispersed in the copolymer. The characteristic peaks observed in FT-IR spectra confirm the formation of the copolymer. XRD pattern reveals the crystalline nature of the copolymer composites and sharp peaks in the spectra confirm the presence of silver particles. The silver nanoparticles change the surface morphology in the form of perfect encapsulation. The electrical conductivity of the polymer composites is found to vary from 10-4 S/cm to 10-6 S/cm. PL study reveals the charge transfer between the copolymer and the silver particles.
EN
A series of sampies of the poly(methyl methacrylate-co-isopropyl acrylate), PMMA/iPrA, of different composition was synthesized via free radical polymerization in solution. The copolymer composition was determined from 400 MHz 1H NMR spectra while the carbonyl region of 100 MHz 13C NMR spectra provided microstructural information on sequence distribution at the level of configurational-compositional triads and pentads. Incremental calculation of the chemical shifts of individual sequences can be performed for carbonyl signal and permit for spectral simulation and verification of the signal attribution to respective sequences.
PL
: Serię próbek kopolimeru metakrylanu metylu z akrylanem izopropylu (PMMA/iPrA) o zmiennym udziale komonomerów, zsyntezowano w wolnorodnikowej polimeryzacji w roztworze. Skład kopolimeru wyznaczono na podstawie 400 MHz widm 1H NMR, podczas gdy obszar karbonylowy 100 MHz 13C NMR widm dostarczył mikrostrukturalnych informacji o rozkładzie kompozycyjno-konfiguracyjnych sekwencji na poziomie triad i pentad. Metoda inkrementalnego obliczania przesunięć chemicznych indywidualnych sekwencji zastosowana do sygnału karbonylowego pozwala na symulację tej części widma i weryfikację przypisania poszczególnych linii odpowiednim sekwencjom.
EN
An energetic tri-block copolymer PCL-GAP-PCL (Mn = 1794) was synthesized by a ring-opening polymerization of ε-caprolactone with glycidyl azide polymer (GAP) of low molecular weight (Mn = 1006 g/mol) as initiator, in the presence of dibutyltin dilaurate (DBTDL) as catalyst, at 100 °C in the absence of solvent. The products obtained in high yield were characterized by FTIR, gel permeation chromatography (GPC), and 1H and 13C NMR spectroscopy. Thermogravimetric analysis (TG) and differential scanning calorimetry (DSC) were used to study the thermal behaviour of the polymers. An advanced isoconversional method has been applied for kinetic analysis. The activation energy, calculated by the Flynn-Wall-Ozawa (FWO) and Kissinger methods, and thermal analysis revealed that the tri-block copolymer has greater thermal stability than homopolymer GAP. The results of the activation energies from the Kissinger method for the first and second steps were 180.3 kJ·mol−1 and 209.8 kJ·mol−1, respectively. Furthermore, for the copolymer, the activation energy versus the level of conversion was calculated by the FWO method. The glass transition temperature (Tg) for GAP was influenced by the PCL blocks; as a result the copolymer (Tg = −64 °C) showed better thermal properties than homopolymer GAP (Tg = −48 °C).
EN
The acrylate monomer was synthesized by two step process. 2,4-dichloro-1-ene(4-hydroxyphenyl)phenone (DHP) was synthesized using 4-hydroxy benzaldehyde and 2,4-dichloro acetophenone. 4-[3-(2,4-dichloro-phenyl)3-oxoprop-1-en-1-yl]phenylacrylate (DCP) was prepared by reacting DHP with acryloyl chloride. The synthesized monomer was copolymerized with 2-hydroxyethyl acrylate and styrene using solution polymerization technique. Monomer and polymers were characterized by IR, NMR and UV techniques. The average molecular weight of the polymer was around 4000 g/mol. First and second decomposition temperature of the polymers was around 320 °C and 430 °C, respectively. The reactivity ratio of the polymers was calculated by Fineman-Ross, Kelen-Tudos and extended Kelen-Tudos methods. The synthesized monomer has been less reactive than the commercial monomer. The rate of photocrosslinking increased from 39 % to 99 % due to the using of copolymerization technique.
EN
In order to achieve extended life of asphalt pavement, one of key points is to achieve a good bonding between it’s components. This research paper presents findings on the topic of influence of polyethylene bitumen modification on the adhesion between bitumen and aggregate. A novel method of quantifying the bitumen coated area, based on computer image analysis, has been developed for this study. Two different methods of adhesion testing were employed, namely boiling water method and the rolling bottle method. Aggregates used in this study were granite and limestone. Based on 108 measurements, it was concluded that polyethylene modification has a negative impact on binder aggregate adhesion.
PL
W związku ze stale rosnącą wielkością ruchu drogowego, dla prawidłowego rozwoju gospodarki, niezbędna jest budowa trwałych nawierzchni drogowych. Jednym ze sposobów osiągnięcia tego celu jest zastosowanie wysokiej jakości mieszanek mineralno-asfaltowych (MMA). Mieszanki te są kompozytami kruszyw oraz lepiszczy asfaltowych. Tematyka adhezji pomiędzy lepiszczami a kruszywem była przedmiotem badań prezentowanych w wielu publikacjach, np. [6, 11, 18 and 20]. Stwierdzić należy, że stosunkowo mało uwagi zostało poświęcone tematyce wpływu modyfikacji lepiszczy asfaltowych polietylenami na ich adhezję do kruszyw [1]. Celem badań prezentowanych w artykule była oceny wpływu modyfikacji lepiszczy asfaltowych polietylenami na zjawisko adhezji pomiędzy kruszywem a lepiszczem.
EN
The copolymers containing carbazole unit and iridium complexes, such as (Ir(bpy)2Cl, Ir(mbpy)2Cl and Ir(Brbpy)2Cl, were synthesized via radical copolymerization of N-vinylcarbazole, methyl methacrylate and iridium complex. The synthesized copolymers were characterized by FT-IR, UV-Vis absorption spectroscopy and photoluminescence (PL) spectroscopy, respectively. According to the results, the copolymers (Ir(Brbpy)2Cl/PVK and Ir(mbpy)2Cl/PVK) exhibit yellow phosphorescence with an emission peak at around 553 nm under UV-visible light in the solid state. The results also reveal almost complete energy transfer from the host carbazole segments to the guest Ir complex in the copolymer film when the Ir content reaches 1.0 wt.%. The synthesized copolymers are good candidates as blue or yellow phosphorescent materials for PLED applications.
EN
Ullmann type polycondensations in the presence of CuI and a base were carried out to afford network type π-conjugated copolymers. Infrared absorption spectroscopy measurements and surface observation using a scanning electron microscopy are carried out. Electron spin resonance spectroscopy measurements revealed that the cross-linked copolymers thus obtained contain small amount of copper. This polymerization conveniently allows production of network π-conjugated polymers. The polymer can be expected to have thermo-resistance.
EN
We report on the synthesis, characterization and aqueous dispersion properties of well-defined double hydrophilic copolymer with pH- and thermo-responsive segments via atom transfer radical polymerization (ATRP). Poly(N-isopropylacrylamide-co-Diethylaminoethylmeth-acrylate), P(NIPAAm-co-DEAEMA), was prepared by ATRP using methyl-4-bromomethyl benzoate initiator. The product was characterized by proton-nuclear magnetic resonance (1H NMR) and attenuated total reflectance infrared (ATR-IR) spectroscopy. The multi-responsive switching between unimer and two types of micellar aggregates were characterized by temperature-dependent dynamic light scattering (DLS). Self-assembles into two types spherical aggregates in 1 mg/mL (0.0315 mM) aqueous solution, depending on solution pH and temperatures were widely investigated. The result shows two types of aggregate with large (280 nm) aggregate and variable sizes of small (17 nm, 25 nm, 45 nm) aggregates depending on temperature ranges from 26 to 40 °C at pH 4.
10
Content available remote Synteza, badania NMR i DSC kopolimeru metakrylanu metylu z akrylanem n-propylu
PL
Próbki polimerów: poli(akrylanu n-propylu), poli(metakrylanu metylu) i poli(metakrylanu metylu-co-akrylanu n-propylu) otrzymano w wolnorodnikowej polimeryzacji w roztworze, uzyskując łańcuch o dominacji struktur syndiotaktycznych. Widma 400 MHz ¹H NMR i 100 MHz ¹³C NMR zsyntezowanych polimerów zarejestrowano w deuterowanym benzenie. Przypisano sygnały rezonansowe protonom i węglom z łańcucha polimerowego. Dla otrzymanych próbek wykonano pomiary temperatury zeszklenia, Tg, przy użyciu skaningowej kalorymetrii różnicowej, DSC.
EN
Poly(n-propyl acrylate), poly(methyl methacrylate) and poly(methyl acrylate-co-n-propyl acrylate), were synthesized by free radical polymerization in solution, obtaining samples containing predominantly syndiotactic structure. The 400 MHz ¹H NMR and 100 MHz ¹³C NMR spectra of these polymers were recorded in deutereted benzene. The resonance signals were assigned to protons and carbons from polymer chain. The polymer samples were also analyzed using differential scanning calorimetry, DSC, determining their glass transition temperatures, Tg.
EN
Cu(I)-catalyzed Huisgen click reactions between lipophilic polymer (tri-arm azidofunctionalized polystyrene) and hydrophilic polymer (copolymer of styrene sulfonate sodium and propargyl methacrylate) were investigated and hollow capsules, consisting of composite polymer nanofilms were obtained in chloroform-water biphasic solution. Since the lipophilic polymer, or hydrophilic polymer and copper catalyst were present in the oil or aqueous phase, respectively, the cross-linking reaction proceeded only at the phase interface. The combination of lipophilic and hydrophilic polymers produced hollow capsules consisting of nanofilms with lipophilic core and hydrophilic shell.
EN
Microstructure of copolymers of two methacrylate monomers are difficult to analyze by 13C NMR spectroscopy since the region of the carbonyl signals, usually utilized for this purpose, is relatively narrow and the lines split due to different sequences are strongly superimposed. The spectra of the two respective homopolymers indicate that both monomers introduce configurational effects, hence the copolymer microstructure should be described in terms of distribution of configurational-compositional sequences. It was shown that for the investigated copolymer of n-butyl methacrylate and methyl methacrylate such analysis can be performed at the triad level.
13
Content available remote Poli(oksyetyleno-b-tereftalan trimetylenu) : synteza, struktura, degradacja
PL
Otrzymano poli(estro-b-etery) składające się z poli(tereftalanu trimetylenu) (PTT) jako bloku sztywnego oraz poli(oksyetyleno)diolu (PEG) jako bloku giętkiego. Metodami 1H NMR oraz FTIR potwierdzono zakładaną strukturę kopolimerów. Metodami DSC i DMTA zdefiniowano właściwości termiczne i rozdział fazowy otrzymanych układów. Materiały poddano testom podatności na degradację hydrolityczną w roztworach o pH=4,9; 7; 8,5 oraz na degradację w glebie. Degradację polimerów po 8 tygodniach oceniono mierząc zmianę lepkości istotnej.
EN
New poly(ester-b-ether) multiblock elastomers containing poly(trimethylene terephthalate) hard segments and polyoxyethylene soft segment were prepared and studied by 1H NMR and FTIR methods to confirme their assumed chemical structures and by DSC and DMTA methods to define the phase separation and thermal properties. Materials were subjected to hydrolytic degradation in solutions of pH: 4,9; 7; 8,5; and degradation in soil. The degradation after a period of 8 weeks was measured by the change of intrinsic viscosity of the polymers.
PL
W artykule przedstawiono wpływ wybranych parametrów termoformowania próżniowego na rozkład grubości ścianki wyrobu. Na podstawie założonych parametrów procesu przeprowadzono analizę porównawczą. Wykonano obliczenia rozkładu grubości ścianki modelowego wyrobu dla wybranych materiałów polimerowych, które zweryfikowano eksperymentalnie.
EN
The article presents the influence of selected parameters of vacuum thermoforming on wall thickness distribution of the product. On the basis of assumed parameters of the process, the comparative analysis was conducted. The calculations of the wall thickness were performed for selected polymer materials, which were experimentally verified.
EN
A chelating resin based on Salicylic acid-Formaldehyde copolymer, containing Orcinol (SFO), has been synthesized and characterized on the basis of Elemental Analysis, Particle Size Distribution, FT-IR Analysis, XRD, SEM and Optical Photographs. The Physico-Chemical properties have been studied. This resin is highly stable in acidic and alkaline solutions and has been studied as a chelating sorbent for heavy metal ions and transition metal ions. The Exchange capacity order is Ni(II) > Cu(II) > Zn(II) > Cd(II) > Pb(II). The effect of nature and concentration of different electrolytes on distribution coefficient (Kd) for metal ions have been investigated. Separation of synthetic mixtures containing Cu(II)-Pb(II), Ni(II)-Cd(II) and Brass constituents has been carried out using a column prepared from the synthesized chelating resin. The developed procedure was also tested for the removal of Cd(II) and Pb(II) from natural water of Purna River near by Navsari, Gujarat, India. Keywords
EN
This paper presents the results of synthesis copolymers based on 2-(9-carbazolyl)ethyl methacrylate (CEM) and 7- (diethylamino)coumarin-3-carboxylic acid 2-(methacryloyloxy) ethyl ester (MK) using ATRP technique. The reactions were carried out both under conventional and microwave conditions. Various activations system with organic ligand 1,10-phenanthroline monohydrate were tested. Obtained polymers were characterized by GPC and UV-VIS techniques.
PL
W artykule przedstawiono wyniki reakcji kopolimeryzacji monomerów: metakrylanu 2-(9-karbazolilo) etylu (CEM) i 7-(dietyloamino)-3-(metakroilooksyetoksy)karbonylokumaryny. (MK). Syntezę kopolimerów przeprowadzono techniką ATRP w warunkach ogrzewania konwencjonalnego jak również pod wpływem promieniowania mikrofalowego. Testowano różne układy inicjujące z monohydratem 1,10-fenantroliny, stanowiącym ligand organiczny. Dla uzyskanych kopolimerów wykonano analizę GPC i UV-VIS.
17
Content available remote Crosslinking polymerization of polyfunctional monomers by free radical mechanism
EN
The crosslinked architectures based on diallyl maleate (DAM) obtained by suspension polymerization techniques have been studied. The influence of synthesis parameters on the structure of poly(diallyl maleate) [poly(DAM)] and copolymers of DAM with methyl methacrylate (MM) [poly(DAM-co-MM)] was also investigated. The effect of the diluents (n-butyl acetate or cyclohexanole) on the inner macroporous structure (apparent and skeletal density, pore volume, total porosity, cyclohexane uptake) has been studied. The experimental results showed that the values of the solvent uptake are strongly influenced by the diluent quantity as well as its solubility parameter.
PL
Przedmiotem badań był proces sieciowania na drodze polimeryzacji suspensyjnej maleinianu diallilu (DAM) i jego kopolimeru z metakrylanem metylu (MM). Określono wpływ warunków prowadzenia reakcji na strukturę otrzymanych poli(maleinianu diallilu) [poly(DAM)] i poli(maleinianu diallilu-ko-metakrylanu metylu) [poly(DAM-co-MM)]. Badano także wpływ rodzaju rozcieńczalnika (octan n-butylu lub cykloheksanol) i jego ilości na makroporowatą strukturę produktów. W tym celu wyznaczano gęstość pozorną, gęstość szkieletową, objętość porów, porowatość całkowitą i absorpcję cykloheksanu. Wyniki badań pokazują, że wielkość absorpcji rozpuszczalnika silnie zależy od ilości jak i parametru rozpuszczalności rozcieńczalnika.
PL
Kopolimer SBS już od kilkunastu lat jest standardowym materiałem stosowanym do modyfikacji asfaltu używanego do wyrobu różnego rodzaju budowlanych materiałów hydroizolacyjnych. Szybkie i w miarę dokładne określenie zawartości SBS w asfalcie stanowi spore wyzwanie.
EN
The aim of the study was to develop and verify, in laboratory conditions, the method of quick and easy assesment of SBS volume in the bitumen used for the manufacture of waterproofing materials. On the basis of the results of viscosity tests carried out in various temperatures (bitumen 160/220, 40/175 and 95/35) and their SBS modified variants, the so called reograms were developed. Analyzing the group composition and colloidal structure of the tested bitumens, it was noticed that the reograms are unique and characteristic for the given type of bitumen. The tests proved that they can be used to specify SBS content in bitumen on the basis of a single viscosity measurement.
PL
W pracy zaproponowano prostą syntezę mikro- i mikro-mezoporowatego węgla z wykorzystaniem koloidalnej krzemionki o wymiarach ok. 24 nm i kopolimeru chlorku winylidenu i chlorku winylu (Saranu) jako prekursora węglowego. W celach porównawczych z samego kopolimeru, bez dodatku koloidalnej krzemionki, otrzymano całkowicie mikroporowaty materiał węglowy. Otrzymany z udziałem krzemionki koloidalnej węgiel mikro-mezoporowaty miał powierzchnią właściwą ok. 850 m2/g, natomiast węgiel mikroporowaty - ok. 1000 m2/g. Udział objętości mikro- i mezoporów stanowił po 50% całkowitej objętości porów węgla mikro-mezoporowatego, matomiast w wypadku węgla mikroporowatego udział mikroporów stanowił blisko 100% całkowitej objętości porów. O ile wymiar mikroporów w obu węglach wynosił ok. 1 nm, o tyle duże, jednorodne, sferyczne mezopory w węglu mikro-mezoporowatym miały wymiar ok. 25 nm, zgodny z wymiarem krzemionki koloidalnej użytej w procesie syntezy tego materiału. Pomiary adsorpcji azotu wykazały, że mezopory były połączone ze sobą i w związku z tym dostępne w procesie adsorpcji tego gazu. Ponadto wykazano, że dobrze rozwinięta mikroporowatość węgla powstała podczas procesu karbonizacji w wyniku termicznego rozkładu kopolimeru (Saranu). Wydaje się, że zaproponowaną metodę można wykorzystać do produkcji mikro-mezoporowatych węgli na skalę techniczną.
EN
A simple strategy is proposed for the synthesis of microporous and micro-mesoporous carbons by using colloidal silica (approx. 24 nm in diameter; hard template) and the vinylidene and vinyl chloride copolymer (Saran) as a carbon precursor. For the purpose of comparison, microporous carbon was obtained from the copolymer alone, with no addition of colloidal silica. When colloidal silica was added, the micro-mesoporous carbon obtained via this route exhibited a specific surface area approaching 850 m2/g, whereas the microporous carbon had a surface area of approx. 1000 m2/g. The micropore and mesopore volumes accounted for about 50% each to the total pore volume of the micro-mesoporous carbon; as for the microporous carbon, the micropore volume was close to 100% of the total pore volume. In both the carbons, the size of micropores approached 1 nm. In the micro-mesoporous carbon the uniform and spherical mesopores were approx. 25 nm in size, which coincided with the size of the colloidal silica used for the synthesis of this material. Nitrogen adsorption measurements have shown that the mesopores were interconnected and accessible to the molecules of this gas in the course of the process. Moreover, it has been demonstrated that the well-developed microporosity was formed during carbonization due to the thermal decomposition of the copolymer (Saran). Apparently, the method proposed can be used for large-scale preparation of micro-mesoporous carbons.
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