Search

In this study, a salt-resistant hydrophobic association polymer (PZDY) is synthesized by acrylamide, octadecyl dimethylallyl ammonium chloride and decane polyoxyethylene ether acrylate by aqueous polymerization. The infrared spectroscopy, fluorescence spectroscopy, scanning electron microscopy and other characterization methods were used to study its properties, and the rheological properties of PZDY solution is analyzed. The results showed that when concentration of NaCl is less than 5 wt% and CaCl2 is less than 1 wt%, the viscosity of 0.4 wt% PZDY increases with the increase of salt concentration. When the salt concentration continued to increase, the PZDY viscosity gradually decreased. Investigation of the rheological behavior showed that 0.6 wt% PZDY in 5 wt% NaCl and 1 wt% CaCl2 solution, could withstand a temperature up to 180 °C, after being sheared for 2500 s at 170 s−1, and its viscosity was greater than 50 mPa·s. Moreover, the viscosity of 0.6 wt% PZDY in 5 wt% NaCl increased from 104 to 205 mPa·s and the viscosity of 0.6 wt% PZDY in 1 wt% CaCl2 increased from 110 to 157 mPa·s, when at a shear rate of 170 s-1, at 180 ° C and the shear time was less than 500 s. Meanwhile, SEM results showed that salt addition enhanced the quasi-spatial network structure, with closer clustering of PZDY molecules in NaCl solution than in CaCl2 solution. The storage modulus (G′) and loss modulus (G") increased with the increase of PZDY concentration. Therefore, PZDY can be used to improve the heat and shear resistance of fracturing fluids and enhance oil recovery.

Aims Vicagrel, a novel antiplatelet prodrug to overcome the residual high platelet reactivity of clopidogrel induced by inactive metabolism and cytochrome P450 (CYP) 2C19 polymorphisms, provides favourable antiplatelet inhibition in healthy volunteers. However, its antiplatelet effect and safety in patients with coronary artery disease (CAD) are unclear. Methods and results This was a multicentre, randomized, double-blind, triple-dummy, dose-exploring phase II trial comparing the antiplatelet activity and safety of vicagrel at different doses vs. those of clopidogrel in patients with CAD undergoing percutaneous coronary intervention (PCI). The primary endpoint was inhibition of adenosine diphosphate (ADP)-induced platelet aggregation (%IPA) after loading and maintenance doses (LD/MD) at 28 days. Safety endpoints included adverse events (AEs) and Bleeding Academic Research Consortium-defined any bleeding. Pharmacokinetic (PK) profiles and the influence of CYP2C19 polymorphisms were explored in subgroup analysis. Two hundred and seventy-nine patients diagnosed with stable CAD (51.97%), unstable angina (40.86%), and myocardial infarction (7.17%) were randomized to receive vicagrel 20/5 mg (LD/MD), 24/6 mg, or 30/7.5 mg or clopidogrel 300/75 mg in combination with aspirin. %IPAs on Day 28 were 30.19%, 35.02%, 45.61%, and 32.55% for vicagrel 20/5, 24/6, and 30/7.5 mg and clopidogrel, respectively, and were comparable across all groups (P = 0.0694). The plasma concentration of the vicagrel active metabolite M15-2 had a similar area under curve and Tmax to those of clopidogrel. There were no significant differences in AEs (4.35%, 0%, 1.45%, and 5.56% for vicagrel 20/5, 24/6, and 30/7.5 mg and clopidogrel, P = 0.6667) or any bleeding (13.04%, 14.06%, 11.59%, and 11.11% for vicagrel 20/5, 24/6, and 30/7.5 mg and clopidogrel, respectively, P = 0.95) across four groups. %IPAs and PK profiles of vicagrel did not vary significantly among different CYP2C19 metabolizers. Conclusion Vicagrel had comparable antiplatelet effect and safety to clopidogrel in patients with CAD undergoing PCI.

Borax-PVA hydrogels with excellent mechanical properties are prepared by simple physical mixing of polyvinyl alcohol (PVA, thickener) and borax (cross-linking agent) at room temperature. The resulting hydrogel is a three-dimensional structure composed of boric ester bonds as physical crosslinking points. Thus, the spatial structure, swelling properties, viscoelastic properties, tensile properties, and self-healing properties of hydrogels with different ratios of borax and PVA are studied. XRD confirmed that the hydrogels have similar structures near 2θ values of 10 and 20. The microstructure of the hydrogel is confirmed by SEM and TEM. With an increase of borax mass fraction, the pore structure and morphology of hydrogel are more ordered, with substantial quantities of water immobilized within their three-dimensional structure. The viscoelastic properties and tensile properties showed that when the mass fraction of borax is 5%, the storage modulus and compressive stress of the hydrogel are the highest, reaching 100 Pa and 5.6 kPa, respectively. In addition, through physical and chemical stimulation (heating and varying pH, respectively), the hydrogels also showed reversible gel–sol conversion characteristics, indicating that the boric ester bonds have self-healing properties.

A novel fracturing fluid system with wettability was prepared. XRD and TGA of the polymer were measured. Rheology and SEM experiments showed that the fracturing fluid had a dense network structure. The microstructures of the gel breaking fluid were obtained using SEM and TEM tests, which demonstrated more obvious crosslinking. Contact angle and wetting function of the gel breaking fluid were evaluated on sandstone. The NFW fracturing fluid showed excellent rheological properties at 90 °C. The surface tension of the gel breaking fluid was relatively low, being 20 mN m−1. The WA, BET data and zeta potential of the NFW gel breaking fluid suggested that the material was absorbed on the sandstone surface and a bilayer was formed. Meanwhile, CT and AFM studies indicated that the imbibition effect of the gel breaking fluid could obviously be observed on the sandstone. The contact angle increased to 146° when the sandstone was immersed in solution, which suggested that the wettability of the rock was changed. The imbibition efficiency of NFW is higher than that of water. Thus, this fracturing fluid with wettability could be an alternative for development in tight oil reservoirs.

Vicagrel is a novel antiplatelet drug used to mitigate clopidogrel resistance due to CYP2C19 polymorphism. This study aimed to develop a semi-mechanistic population pharmacokinetic (PopPK) model to characterize the pharmacokinetic (PK) profile of M15-2, the active metabolite of vicagrel and clopidogrel, and to evaluate the influence of CYP2C19 polymorphisms and other covariates in healthy subjects and patients with acute coronary syndrome (ACS) after oral administration.The analysis utilized data from 213 subjects, including 178 healthy subjects and 35 patients, from five clinical trials. PopPK modeling and simulation were used to estimate PopPK parameters and evaluate the impact of covariates.The M15-2 PK profiles were well characterized by a model incorporating transit compartments, two-compartment parent models and two-compartment M15-2 models for both vicagrel and clopidogrel. The parameter estimates indicated the dose fraction of vicagrel that formed M15-2 was approximately 20-fold that of clopidogrel. Covariate analysis identified a significant effect of CYP2C19 on M15-2 apparent clearance (CL/F) and apparent volume of distribution (V3/F) for clopidogrel but only CL/F for vicagrel. The analysis suggested that the nonlinear PK of M15-2 for clopidogrel was due the first-step bioactivation of clopidogrel to 2-oxoclopidogrel.The model illustrated the bioactivation of vicagrel is more efficient and less dependent on CYP2C19 than that of clopidogrel. M15-2 is formed in a linear process from vicagrel, versus a nonlinear and less predictable process from clopidogrel. Advantages in both PK and pharmacogenetics suggest that vicagrel may reduce the complexity of currently recommended CYP2C19-based dosage adjustment for clopidogrel.

A series of betaine-type Gemini surfactants (Cs-BGS, where C is the methylene part of the spacer, s = 2, 4, 6) were synthesized from sodium 3-chloro-2-hydroxypropanesulfonate, oleamidopropyl dimethylamine and bromoalkane. The chemical structure of the prepared compounds was confirmed by 1H NMR, 13C NMR, IR spectra, and elemental analysis. Their critical micelle formation concentrations (CMC) in the aqueous solution at 25 °C were determined by measuring the surface tension and the electrical conductivity. As the length of the spacer increased, the values of their CMC and γcmc also increased. The surface tension measurements of C2-BGS revealed that the surfactant possesses a low CMC, is very efficient in reducing the surface tension, and is very strongly adsorbed at the air-water interface. In addition, the adsorption and micellization behavior of Cs-BGS was estimated from the efficiency of surface tension reduction (pC20), minimum average surface area per surfactant molecule (Amin), and standard free energies of micellization and adsorption. These properties are significantly affected by the spacers and the adsorption is more favored than the micellization.

Background and objectives Vicagrel, a novel thienopyridine antiplatelet agent, is an analogue of clopidogrel in development for the treatment of acute coronary syndromes. This study investigated the pharmacokinetic properties of vicagrel after single oral dosing with a direct comparison with clopidogrel in healthy Chinese subjects in the first two phase I clinical studies. The relationship between the exposure to the active metabolite and the platelet reactivity was also assessed for vicagrel. Methods Study A was a single-ascending-dose study of vicagrel (5–75 mg) compared with clopidogrel (75 mg) in 67 healthy volunteers. Study B was a randomized, two-period, crossover, loading-dose study of vicagrel 20 mg compared with clopidogrel 300 mg in 12 healthy subjects. Plasma concentrations of three common metabolites of vicagrel and clopidogrel, the active thiol metabolite H4, the inactive thiol metabolite H3, and the S-methylated form of H3 (SM3, the major metabolite of vicagrel), were determined using a validated UHPLC–MS/MS method. The relationship between the AUC0−t of active H4 and the P2Y12 reaction units at 4 h after administration of vicagrel was investigated. Blood concentrations of vicagrel were determined after a single oral administration of vicagrel 25 mg to two healthy Chinese subjects. Results In the single-ascending-dose study, vicagrel was metabolized rapidly with the median tmax for the three metabolites, namely, H4, H3, and SM3, ranging from 0.25–1.75 h. The pharmacokinetics of the three metabolites for vicagrel were linear across the dose range of 5–75 mg, with the mean Cmax and AUCs for H4 and H3 increasing in an approximately 1:1 dose-proportional manner and for SM3 increasing in a Conclusions Vicagrel was rapidly and extensively metabolized, and the levels of the parent drug in circulation were very low. The pharmacokinetics of the three metabolites of vicagrel were linear and predictable across the dose range of 5–75 mg. The AUC of active H4 was apparently associated with the P2Y12 reaction units for vicagrel. For active H4, vicagrel 5 mg produced similar exposure (AUC) with more rapid appearance compared with clopidogrel 75 mg, and vicagrel 20 mg produced even slightly higher exposure (AUC) with more rapid appearance compared with clopidogrel 300 mg in humans. Trial Registration: CTR20150346, CTR20160379.

Herein, a novel ultra-high salt hydrophobic associated polymer, UUCPAM, was prepared using acrylamide, acrylic acid, 2-acrylamide-2-methyl propane sulfonic acid and the hydrophobic monomer UUC. Polymerization exothermic test results indicated that the increase in the hydrophobic monomer content led to an increase in the exothermic time, which is considerably conducive to the formation of hydrophobic structures. The scanning electron microscopy and transmission electron microscopy studies showed that the polymer had complex network structures and that this phenomenon was considerably obvious in NaCl solution. The fluorescence probe experiment verified that the critical association concentration of this polymer decreased with an increase in the hydrophobic monomer. Rheology studies indicated that the polymer had good temperature and shear resistance in NaCl solution. Moreover, the apparent viscosity of the polymer remained above 80 mPa s when 0.3 wt% UUCPAM was added at 170 s−1 in 20 000 mg L−1 NaCl solution at 90 °C. The storage modulus that indicated strong elasticity increased with an increase in the polymer concentration. Meanwhile, the number of hydrophobic micro-zones increased, thus forming dense network structures. Therefore, the polymer was found to have excellent salt resistance and extensive application prospects.

AIMS: We investigated the impacts of CYP2C19 polymorphisms on pharmacokinetics and pharmacodynamics of vicagrel in healthy Chinese subjects. METHODS: CYP2C19 extensive metabolizers (EMs), intermediate metabolizers (IMs) and poor metabolizers (PMs; 16 subjects/group) participated in a randomized, open‐label, 2‐period cross‐over study. Each study period lasted 7 days, with a loading dose of 24 mg of vicagrel or 300 mg of clopidogrel on day 1, and maintenance doses of 6 mg of vicagrel or 75 mg of clopidogrel daily from day 2 to day 7. The pharmacokinetics and pharmacodynamics were assessed on day 1 and day 7. RESULTS: After a loading dose, the AUC(0‐t) of the active metabolite H4 by vicagrel was slightly lower in IMs and PMs (decreased by 21 and 27%, respectively) compared to EMs. Similar results were found after maintenance doses. In EMs, the AUC(0‐t) of H4 by vicagrel was somewhat higher than clopidogrel after the loading dose, and comparable with clopidogrel (90% confidence interval 0.94, 1.21) after the maintenance doses. However, it was much higher than clopidogrel in PMs, with a 1.28‐fold (loading dose) and a 73% (maintenance doses) increases compared to clopidogrel (P < 0.001). Consequently, the inhibition of platelet aggregation by vicagrel was greater than clopidogrel after both loading dose (28.2 vs 12.4% at 4 hours, P < 0.01) and maintenance doses (42.8 vs 24.6% at 4 hours, P < 0.001) in PMs. CONCLUSIONS: CYP2C19 polymorphisms have less impact on vicagrel as compared to clopidogrel. Drug exposure and response to vicagrel in PMs were even higher than to clopidogrel in IMs.

Vicagrel is a new antiplatelet pro-drug based on clopidogrel sulfur lactone metabolites. The purpose of the study was to evaluate the safety, tolerability, and pharmacodynamics (PD) of vicagrel in healthy Chinese subjects. This study was designed as a single-center, randomized, double-blind, placebo-controlled, single oral ascending dose study. Fifty nine subjects were assigned to 6 vicagrel dose cohorts (5, 10, 20, 40, 60, and 75 mg), and 8 subjects were assigned to 75 mg clopidogrel. Within each vicagrel dose cohort, the 10 subjects (9 in the 75 mg cohort) were randomized 4:1 to receive vicagrel or placebo. Platelet function was assessed using VerifyNowTM P2Y12. ΔP2Y12 reaction units (ΔPRU) and percent inhibition platelet aggregation (%IPA) were used to evaluate the PD of vicagrel. Although the number of adverse events (AEs) increased with vicagrel dose, none were considered serious, suggesting that vicagrel is safe and well-tolerated. The ΔPRU and %IPA patterns suggest that inhibition of ADP-induced platelet aggregation increased in a dose-dependent manner across the 10 to 40 mg dose range. The inhibitory effect was nearly complete at 4 hours (mean %IPA 87.9%–93.0%, mean ΔPRU 206.6–240.0) for doses of 40 to 75 mg of vicagrel. In contrast, for 5 mg vicagrel and 75 mg clopidogrel, there were no measurable effects on platelet aggregation throughout the study. The results suggest that vicagrel at 40 to 75 mg inhibits ADP-induced platelet aggregation, with a fast onset of action and significantly greater potency than clopidogrel. These findings indicate that vicagrel may be a highly effective and well-tolerated antiplatelet agent.

A novel betaine Gemini surfactant (B18-4-18) was synthesized by two-step reaction with N,N-dimethyl oleoaminde-propylamine, sodium 2-hydroxy-3-chloro propanesulfate and 1,4-dibromobutane as main raw materials. The structure of the synthesized betaine Gemini surfactant was characterized by Fourier transform infrared spectroscopy (FTIR) and 1H nuclear magnetic resonance spectrum (1HNMR), the surface tension curve and related parameters were obtained by surface tension measurements. The surface tension of oleamide hydroxypropyl betaine (B18) and the Gemini surfactant (B18-4-18) at different concentrations was measured. The experimental results showed that the structure of the synthesized compounds was in conformity with the expected structure of the surfactants. The critical micelle concentration of B18 was 6.1 × 10−6 mol/L, the corresponding surface tension was 34.27 mN/m. The critical micelle concentration of B18-4-18 was 5.0 × 10−6 mol/L, the corresponding surface tension was 31.67 mN/m at 25°C. The liquid carrying rate of B18 and B18-4-18 can reach 87% and 92% in water respectively. The liquid carrying rate of B18 and B18-4-18 can reach 82% and 84% in 150 000 mg/L mineralized water. The liquid carrying rate of B18 and B18-4-18 can reach 64% and 67% respectively at 10% condensate oil.

Vicagrel, an analog of clopidogrel, is a novel thienopyridine P2Y12 antagonist in clinical development in China for the treatment of acute coronary syndromes. Vicagrel and clopidogrel are prodrugs requiring metabolic activation to produce a pharmacologically active thiol metabolite (H4) in vivo. The formation of H4 from vicagrel in humans is promising more efficient and consistent than that from clopidogrel. After oral dosing of vicagrel or clopidogrel to humans, the active thiol metabolite H4 and two inactive metabolites closely related to H4 formation (the thiol metabolite H3 and the S-methylated metabolite SM3) were observed in plasma; SM3 was the most abundant drug-related component of vicagrel in circulation. In this study, a sensitive, rapid, and reliable UHPLC-MS/MS method was developed for the simultaneous determination of derivatized H3 (MP-H3), derivatized H4 (MP-H4), and SM3 in human plasma to investigate the pharmacokinetics of vicagrel in healthy subjects compared with clopidogrel. After extracted from 50μL of plasma by simple protein precipitation, the analytes and stable isotope-labeled internal standards were separated on an Acquity UPLC BEH C18 column (100mm×2.1mm, 1.7μm). The mobile phase was acetonitrile-water-formic acid (45:55:0.0275, v/v/v) delivered at a flow rate of 0.45mL/min under isocratic elution. The total chromatographic run time was 6min. MP-H3, MP-H4, and SM3 were separated from their corresponding isomers under the chromatographic conditions. Mass spectrometric detection was conducted in multiple reaction monitoring mode on an AB Sciex Qtrap 5500 System using a positive electrospray ionization interface. The calibration curves were linear in the following ranges: 0.100-200ng/mL for MP-H3 and MP-H4 and 1.00-1000ng/mL for SM3. The intra- and inter-day accuracy and precision for each analyte at all concentrations were within acceptable limits (±15%). The validated method was successfully applied to compare the pharmacokinetics of vicagrel and clopidogrel after a single oral administration to healthy subjects in the first-in-human study of vicagrel.

Background: Vicagrel is a novel anti-platelet drug and hydrolyzed to the same intermediate as clopidogrel via esterase, instead of CYP2C19. Here we report the first clinical trial on the tolerability, pharmacokinetics and pharmacodynamics of different doses of vicagrel, and comparison with clopidogrel in healthy Chinese volunteers. Methods: This study was conducted in two parts. Study I was a dose-escalating (5–15 mg) study. For each dose, 15 participants were randomized into three groups (total n = 45); nine participants were given vicagrel, three were given clopidogrel, and three were given a placebo. Study II was conducted to assess interactions between vicagrel and aspirin in 15 healthy participants. The plasma concentrations of the metabolites of vicagrel and clopidogrel were determined using a LC-MS/MS method. Platelet aggregation was assessed using the VerifyNow-P2Y12 assay. Results: Vicagrel (5–15 mg per day) dosing for 10 days or addition of aspirin was well tolerated in healthy volunteers. The exposure of the active metabolite increased proportionally across the dose range and was higher (~10-fold) than clopidogrel. The levels of IPA dosing 75 mg clopidogrel were between the responses of 5 mg and 10 mg vicagrel. After a single loading dose of vicagrel (30 mg) and a once-daily maintenance dose (7.5 mg) for 8 days, the maximum inhibition of platelet aggregation was similar to that seen with the combined use of vicagrel and aspirin (100 mg/day). Conclusion: Oral vicagrel demonstrated a favorable safety profile and excellent anti-platelet activity, which could be a promising P2Y12 antagonist as anti-platelet drug and can be further developed in phase II/III studies, and marketing for the unmet medical needs of cardiovascular diseases. The study was registered at http://www.chictr.org.cn (ChiCTR-IIR-16009260).

Vicagrel, a novel thienopyridine antiplatelet agent, is an analogue of clopidogrel in development for the treatment of acute coronary syndromes. This study investigated the pharmacokinetic properties of vicagrel after single oral dosing with a direct comparison with clopidogrel in healthy Chinese subjects in the first two phase I clinical studies. The relationship between the exposure to the active metabolite and the platelet reactivity was also assessed for vicagrel.Study A was a single-ascending-dose study of vicagrel (5-75 mg) compared with clopidogrel (75 mg) in 67 healthy volunteers. Study B was a randomized, two-period, crossover, loading-dose study of vicagrel 20 mg compared with clopidogrel 300 mg in 12 healthy subjects. Plasma concentrations of three common metabolites of vicagrel and clopidogrel, the active thiol metabolite H4, the inactive thiol metabolite H3, and the S-methylated form of H3 (SM3, the major metabolite of vicagrel), were determined using a validated UHPLC-MS/MS method. The relationship between the AUCIn the single-ascending-dose study, vicagrel was metabolized rapidly with the median tVicagrel was rapidly and extensively metabolized, and the levels of the parent drug in circulation were very low. The pharmacokinetics of the three metabolites of vicagrel were linear and predictable across the dose range of 5-75 mg. The AUC of active H4 was apparently associated with the P2YCTR20150346, CTR20160379.

Polyurethane/polyacrylate (PUA) composite emulsions were synthesized based on the presence of preformed polyurethane chains. Glycidyl methacrylate (GMA), an acrylate monomer, was introduced into the system. Surface tension measurements assured the surface activities of the polyurethane emulsion. Dynamic light scattering (DLS) result showed that the average diameters and polydispersity were increased with the increment of GMA content. X-ray photoelectron spectroscopy (XPS) result indicated that the upper surface was rich in PU phase. The peak deconvolution results of XPS also confirmed the formation of PUA. The crosslinking degree and tensile strength were both enhanced due to the reaction between the carboxyl groups and the epoxide groups. Thermo gravimetric analysis (TGA) of the membranes showed that the thermal stability enhanced and the decomposition temperature was much higher than the pure PU membrane. X-ray diffraction (XRD) analysis, together with differential scanning calorimetry (DSC) results, demonstrated the amorphous nature of the PU matrix. Atomic force microscopy (AFM) observation performed the extremely flat membrane.

In the paper, the hydrophobic associating polymer ACS-210 was prepared by solution polymerization of acrylamide, acrylic acid, salt-resisting monomer and hydrophobic monomer. Chemical structure and properties of the polymer was characterized by FTIR, TGA and XRD. The rheological property of ACS-210 solution was investigated by rheometer. The frictional resistance of the ACS-210 solutions at different application condition was examined using friction testing system. Results showed that the thermal stability of polymer ACS-210 increases and crystallinity of ACS-210 declines after incorporating of hydrophobic monomer. The viscosity of ACS-210 solution of different concentration decreased with prolonging the shearing time and the retention rate of viscosity is relatively high after long shearing time. The relation curve between the viscosity of polymer solution and shear rate followed the power law model. When the concentration of ACS-210 aqueous solution was less than the critical associating concentrations, storage modulus G’ is less than loss modulus G”, the association was weaker between the molecular chains, and the effective spatial structure did not form. After increasing the concentration of the polymer solution, G’ is more than G”, the degree of association of polymer is stronger. The synthesized polymer has favorable drag reduction effect. The molecular weight is not the only factor to determine drag reduction efficiency. The hydrophobic association can also improve the drag reduction efficiency.

The waterborne fluorinated polyurethane–acrylate hybrid emulsion (WFPUA) was prepared by two steps, including the preparation of the fluorinated alcohol blocked polyurethanes (FBPU) in the mixtures of vinyl monomers and fluorinated monomers and then the free radical polymerization after the pre-emulsification of the said system. The effects of hydrophilic monomer (MDEA) on the surfactivity and the emulsifiability of the FBPU were firstly reported. Then, the particle size (d), zeta potential (ζ), and viscosity (η) of the WFPUA hybrid emulsion were characterized, respectively. At the same time, the surface properties and the mechanical properties of the films were investigated. The results show that the increase of MDEA is good for the emulsifiability and the lower surface tension of the FBPU. This increase improves the stability, the ζ and η, yet decreases the d of the WFPUA emulsion. However, it has disadvantages to the hydrophobic performance of the WFPUA films. When the content of the MDEA in the WFPUA is increased from 4.67 to 14.89 %, the surface free energies are increased from 22.22 to 27.28 mJ m−2 and the attenuation rate of the contact angle–time curve is increased from 0.3051° to 0.6290°/min. Also, with the increase of MDEA, the tensile strength and the shore hardness of the film are increased, but its elongation at break is decreased. The storage moduli of the film are enhanced remarkably. Meanwhile, the glass transition temperature of the soft segment [Tg(s)] is reduced and that of the hard segment [Tg(h)] is raised.

Hydroxyl-terminated polyurethane (EPPU) modified by epoxy resin was synthesized. The structure of polyurethane (PU) was characterized by Attenuated total reflection Fourier transform infrared spectrometer (ATR-FTIR) and transmission electron microscope (TEM). The effect of w(E-44) on thermal stability and mechanical properties of the membranes were also measured. ATR-FTIR and TEM indicates that epoxy resin has been successfully incorporated into the copolymer's main chain, and the thermal stability has improved. It was found that greater mechanical properties of PU were obtained when chemical networks were formed between PU and epoxy resin. The maximum tensile strength is up to 6.99 MPa.

Self-crosslinkable polyurethane emulsion containing active carbonyl group was obtained using dihydroxyketon N-[(1,1-dimethyl-2-acetyl)ethyl]-β-dihydroxyethylamino propanamide(DDP) and 1,4-butanediol as chain extenders, isophorone diisocyanate (IPDI), polyether polyol (PTMG1000), dimethylol propionic acid (DMPA) and trimethylol propane (TMP) as main materials, γ-aminopropyltriethoxysilane (APTES) as end capping agent. Then adipic dihydrazide was added into the emulsion. The structure and composition of DDP and the films were confirmed by means of FTIR and 1H nuclear magnetic resonance (1H-NMR) spectrometer, the test results indicated that the reaction between ketone carbonyl and hydrazine has happened during the film curing. The effects of n(NH2NH-)/n(C=O) and DDP content on the properties of the films were studied. The results show that water absorption of the films decreases from 39.3% to 18.9%, crosslinking degree increases from 51.5% to 90.2%, tensile strength increases from 20.1 MPa to 28.3 MPa and pencil hardness is 2H when the DDP content increases from 0% to 6.13%. TGA analysis indicates that the Ketone-Hydrazide crosslinking structure can improve thermal stability of the films.

The polyurethane prepolymer was synthesized, and hydrophilic nano-sized silica (A200) was added to the prepolymer with KH550 as a coupling agent, then a waterborne polyurethane/nanosilica hybrid material (WPUNS) was obtained by a sol-gel process. The structure and performance of the WPUNS films were studied by FTIR, TG, DSC and physical mechanical testing. The particle size and distribution of WPUNS hybrid emulsion was analyzed by a dynamic light scatter (DLS). The morphology of emulsion and films were observed by Transmission Electron Microscope (TEM) and Atomic Force Microscope (AFM), respectively. FTIR analysis indicates the formation of chemical bond between WPU and A200. TEM images display that A200 particles were encapsulated by PU macromolecules and formed a composite particles structure. As the mass fraction of A200 increased from 0 to 2%, the particle size increased from 79.9 nm to 139.9 nm, the tensile strength of the films increased from 6.32 MPa to 20.46 MPa, water absorption decreased from 28...

Polyurethane/silica hybrid emulsion (PUSi) was synthesized by the reaction of isophorone isocyanate, polyether polyol, hydrophilic nanosilica (A200), dimethylol propionic acid, trimethylol propane, and 3-aminopropyltriethoxysilane (KH550). The films of the waterborne polyurethane (WPU) were prepared. The structure of the polyurethane was characterized by Fourier transform infrared spectrometer (FTIR), thermogravimetry (TG), and differential scanning calorimetry (DSC). The particle size distribution and morphology of emulsion were examined. Influence of nanosilica content on the mechanical properties and solvent absorption of the cast films were also measured quantificationally. FTIR indicates that NH2 of KH550 reacted with NCO of polyurethane. TG analysis indicates that nanosilica can improve thermal stability of polyurethane. There is no clear effect of nanosilica on the glass transition of soft segments. It was found that greater mechanical properties of WPU were obtained when chemical networks were formed by sol-gel process. As the nanosilica content increases, water absorption and ethanol absorption decreased. The particle size increases with increase of A200 content. PUSi hybrid emulsions are endowed with pseudoplasticity. The apparent viscosity of emulsions increased and then decreased with addition of A200. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011

Waterborne polyurethane prepolymer was prepared by the reaction of isophorone isocyanate(IPDI), polyether polyol(PTMG), dimethylol propionic acid(DMPA) and trimethylol propane(TMP), which was modified by silicane coupling agent(APTES) to form highly crosslinked polyurethane emulsion. The films of the waterborne polyurethane were prepared. The structure of the polyurethane was characterized by Fourier transform infared spectrometer (FTIR), X-ray diffraction (XRD) and differential scanning calorimeter (DSC). The mechanical properties and water absorption of the films were measured. FT-IR indicates that APTES reacted with -NCO of polyurethane. XRD and DSC shows that crystallinity of polyurethane decreased with the increase of w(APTES). Tensile strength increases as the NCO/OH ratio increases. Tensile strength of films increases with increase of w(DMPA) and elongation at break decreases. The water absorption decreases with the increase of w(TMP) when w(TMP) is lower than 1.8%. As the mass fraction of APTES increases from 0% to 10%, the tensile strength of PU films increased from 18 MPa to 28 MPa, water absorption and ethanol absorption decreased.

Crosslinked starch microspheres (CSMs) were prepared in an inverse suspension system. Scanning electron microscopy observation indicated that the CSMs were uniform in granularity with a smooth spherical particulate surface. The particle size analysis revealed that the average diameter was 18.2 μm and that 85.8% of the microspheres were of a diameter below 30 μm. The structural characteristics of the carbonyl group and the second acrylamide by Fourier transform infrared spectroscopy of the CSMs showed that the soluble starch obviously crosslinked with N,N′-methylene bisacrylamide. The physical properties of the CSMs were analyzed by way of X-ray diffraction, differential scanning calorimetry, and thermogravimetric analysis. The results show that the crosslinking resulted in an increase in thermal stability and a decrease in crystallinity of the CSMs compared with soluble starch. The adsorption capacity of the CSMs increased with increasing concentration of methylene blue. The lower temperature was in favor of the adsorption capacity of the CSMs. The adsorption mode of methylene blue by the CSMs agreed more with the Langmuir isothermal equation. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008

Novel polyurethane/polyacrylate (PUA) composite emulsions were synthesized by soap-free emulsion polymerization method from methyl methacrylate (MMA), butyl acrylate (BA), and 2-Hydroxyethyl acrylate (HEA) in the presence of PU as seeds and a polymerizable emulsifier-Allyloxy hvdroxyl propanesulfonic salt (AHPS). Effects of the AHPS content on the properties of the emulsions and films were studied. Dynamic light scattering (DLS) result showed that the average diameters and polydispersity were decreased with the increment of AHPS content. Fourier transform infrared spectroscopy (FT-IR) result shows that AHPS was introduced into the PUAS chains. Their thermal stability and Tg of the films increased gradually with augment of AHPS amount in polymer. X-ray photoelectron spectroscopy (XPS) analysis showed that sodium was preferably enriched on the surface of latex particles. Atomic force microscopy (AFM) observation performed the extremely flat membrane.

Self-crosslinkable aqueous polyurethane (PU)/polyacrylate (PA) composite emulsion was obtained by radical copolymerization. Fourier transform infrared spectroscopy (FT-IR) result shows that the cross-linking reaction between the carbonyl group and the hydrazine group has happened. The influence of the hydrazide-carbonyl molar ratio and the PA content on the properties of the composite emulsions and their films were investigated. The results show that, under the optimal hydrazide-carbonyl molar ratio (n (hydrazine group)/n (carbonyl group) =1:1), the water absorption is 10.56 %, and the mechanical properties and thermal stabilities are both improved. As the PA content increases from 0 wt% to 15 wt%, the tensile strength increases from 5.7 MPa to 7.3 MPa and the gel content increases from 70.3 % to 87 %.

Cationic blocked waterborne polyurethane (CBWPU) as paper strength agent was prepared by the reaction of N-[(1,1-dimethyl-2-acetyl)ethyl]-β-dihydroxyethylamino propanamide(DDP), isophorone diisocyanate(IPDI), polycaprolactone glycol(PCL) and bisphenol A, with imidazole as blocking agent and N-methyldiethanolamine as hydrophilic chain-extending agent. Effects of the blocked ratio and the dosage of CBWPU on the physical properties of the treated paper were studied. The chemical structure of CBWPU and the surface morphology of the paper surface are characterized by Fourier transform infared spectrometer(FT-IR) spectra and scanning electron microscopy(SEM). The results show that the paper strength, especially the wet tensile index and the wet strength of paper can be obviously improved with the increasing of the blocked ratio and the dosage of CBWPU. FT-IR result shows that structures of tertiary amine group, imidazole ring and urethane group are found in CBWPU molecular structure. SEM obsevation of the treated paper reveals that the exiestence of a lot of filamentous materials and films, which can improve the crosslinking between fibers.

According to the characteristic of polyhydroxy alcohol fracturing fluid system, the regeneration of the system was investigated for the first time. A stable organic boron crosslinking poly(vinyl alcohol) regenerable polyhydroxy alcohol fracturing fluid system was prepared, and the rheological property of the polyhydroxy alcohol fracturing fluid system with different regenerable times was researched. The effect of regenerable times on the rheological property of the system was studied. The results showed that the aims of gel breaking and regeneration can be achieved by regulating its pH value and controlling its crosslinking degree. With the increment of the regenerable times, both the temperature resistance and shearing resistance performances were decreased, and the viscoelasticity of the gel was also reduced.