Synthesis and application of polyacrylate nanocapsules loaded with lilial

Polyacrylate nanocapsules loaded with lilial (PNLs) were prepared via miniemulsion polymerization. Then, the PNLs were applied directly to leather. The influence of the contents of the surfactant and lilial and the stirring speed on the mean size and fragrance loading capacity of the PNLs was investigated in detail. The microstructure of the PNLs was determined by dynamic light scattering (DLS), transmission electron nicroscopy (TEM), Fourier transform infrared (FTIR) spectrometry, and thermogravimetric analysis (TGA). The sustained release properties of the leather finished by PNLs were characterized by scanning electron microscopy (SEM) and gas chromatography with a flame ionization detector (GC‐FID). DLS showed that the mean size of the PNLs was 67.78 nm, and the polydispersity index was 0.076. TEM illustrated that the size of the spherical PNL varied in the range 30–80 nm. FTIR spectroscopy showed that lilial was encapsulated into the polyacrylate nanocapsules. TGA illustrated that the fragrance loading ratio of the nanocapsules reached 36.83%. SEM and GC‐FID indicated that the leather finished by the PNLs had better flexing endurance than that finished by lilial emulsion. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40182.     

Novel blend microspheres of poly(vinyl alcohol) and succinyl chitosan for controlled release of nifedipine

Water-soluble succinyl chitosan (SCS) was synthesized by reacting succinic anhydride with –OH and –NH₂ reactive groups of chitosan (CS). The blend hydrogel microspheres were prepared from SCS with poly(vinyl alcohol) (PVA) by water-in-oil (w/o) emulsion cross-linking using glutaraldehyde (GA) as the cross-linking agent. Nifedipine (NFD), an antihypertensive drug having a plasma half-life of 2 h, was encapsulated giving encapsulation efficiency up to 92 % and its release was extended up to 12 h. Scanning electron microscopy (SEM) confirmed the spherical nature and smooth surfaces of the microspheres, while Fourier transform infrared spectroscopy (FTIR) confirmed succinylation of CS and chemical stability of NFD in the matrix. Thermogravimetry (TGA) and differential scanning calorimetry (DSC) characterized the SCS and the blend hydrogel microspheres. X-ray diffraction (XRD) and DSC were also used to study the crystalline or amorphous nature of NFD. Swelling and in vitro release experiments performed in pH 1.2 and 7.4 buffer media showed a dependence of blend composition, extent of cross-linking and pH of the media. The mechanism of drug release as analyzed by an empirical equation, suggested non-Fickian trends.     

海藻酸钙/埃洛石载药微球的制备与缓释盐酸二甲双胍性能

缓释可提高药物利用率,降低其毒副作用。采用交联法制备了海藻酸钙/埃洛石载药微球,以载药微球对盐酸二甲双胍（MH）药物的包封率和缓释效果为考察对象,研究了载药微球的制备工艺和缓释性能,并通过SEM、FTIR和TGA对其结构进行了表征。结果表明：在交联温度为0℃、海藻酸钠用量为1g、埃洛石添加量为2g时,能得到较优的载药微球包封率（79.23%）。上述条件下制得的复合载药微球在pH=6.8的磷酸盐缓冲液中能有效缓释,且720min后缓释度可达85.83%,说明其具有较好的pH敏感性和缓释效果。SEM表明海藻酸钙颗粒与埃洛石在载药微球内部形成复合结构,FTIR表明MH主要以物理包埋的形式于载药微球中,TGA表明添加埃洛石可以提高复合材料在200℃以上的热稳定性。     

丝素-羟丙基壳聚糖微球的结构和释药性能

以胰岛素为目标药物,以丝素(SF)和羟丙基壳聚糖(HPCS)为包药材料,复凝聚法制备SF-HPCS载药微球。采用红外光谱(FTIR)、扫描电镜(SEM)、X射线衍射(XRD)、热重分析(TGA)等对载药微球的结构、外部形貌及热性能等进行了表征。结果表明,所制备的载药微球表面密实,平均粒径22.4μm,呈正态分布;载药微球对胰岛素的包埋率达73.6%,大于HPCS载药微球(64.3%)及壳聚糖(CS)载药微球(57.1%);SF-HPCS载药微球在人工胃液中4h内累计释药率为21.3%,在人工肠液中24h内累计释药率达81.2%,48h累计释药率为92.2%,释放过程平稳、缓慢。     

2,4-D/CMC接枝物纳米粒子的制备与缓释性能研究

以羧甲基纤维素钠（CMC）为基材，甲基丙烯酸甲酯（MMA）和二甲基二烯丙基氯化铵（DMDAAC）为改性单体，通过乳液聚合制备了CMC-g-P(MMA-DMDAAC)共聚物，采用自组装方法负载2,4-二氯苯氧乙酸（2,4-D）得到2,4-D/CMC-g-P(MMA-DMDAAC)纳米药物缓释体系。利用傅里叶红外光谱（FTIR）、差示扫描量热法（DSC）、热重分析（TGA）、扫描电镜（SEM）、粒度分析仪对其结构和形貌进行表征，并探究其载药性能和缓释性能。结果表明，2,4-D/CMC-g-P(MMA-DMDAAC)载药粒子呈笼状结构，粒度分布为160～425 nm；其载药率随着CMC∶MMA∶DMDAAC的摩尔比增大而提高，最高可达40.8%；其药物累计释放率随CMC∶MMA∶DMDAAC的摩尔比增大而降低，其释放行为符合Weibull模型，遵循Fick扩散机理。     

Preparation and characterization of polyaniline coated microspheres for potential application in anisotropic conductive film

Monodispersed polyaniline-coated (PANi) microspheres with a mean diameter of 5.174 μm and a 3.53% coefficient of variation were successfully prepared through an in-situ chemical oxidation polymerization of aniline on the surface of high-crosslinked polystyrene-divinylbenzene (PSDVB) particles with the mass ratio of 1: 0.12 between PSDVB particles and aniline. The microspheres were characterized by the scanning electron microscopy (SEM), FTIR and elemental analysis. A very thin layer of polyaniline, about 10.5% in weight, was found to evenly cover on the PSDVB, The microspheres were demonstrated to be thermal stable below 450 °C by thermogravimetric analysis (TGA) measurements and have a bulk conductivity of 6.67 × 10^-3 S.cm^-1 by AC impedance method. The good thermal stability suggested that PANi/PSDVB microspheres could be a promising material to replace the conventional metallic anisotropic conductive film (ACF) particles if the conductivity could be further improved in the future.     

Fabrication and characterization of colon specific eudragit coated graphene oxide microsphere for sustained delivery of tramadol hydrochloride

ABSTRACT

Present investigation reports a straight forward method for synthesis of graphene oxide (GO) followed by fabrication of graphene oxide microsphere (GMS) using water in oil (w/o) emulsification technique. For colon specific drug delivery, enteric coating is desirable, which was done using Eudragit S100 and characterized by Fourier transform Infrared Spectroscopy (FTIR). The surface morphology of fabricated microsphere was confirmed using scanning electron microscopy (SEM). Drug loaded microspheres demonstrated a high payload capacity for model drug tramadol hydrochloride (TmH). The comparative In-vitro drug release showed around 72.37% release from uncoated microspheres, whereas eudragit coated microspheres retarded the drug release upto 10 h.     

RAFT与点击化学结合合成SiO2/PNIPAm杂化微球

利用可逆加成-断裂链转移(RAFT)聚合与点击化学相结合的方法,将大分子链末端含巯基的聚(N-异丙基丙烯酰胺)(PNIPAm-SH)接枝到SiO2纳米粒子上制备了温度响应的SiO2为核、PNIPAm为壳的核-壳结构的SiO2/PNIPAm纳米杂化微球。采用FTIR、热重分析(TGA)、透射电镜(TEM)和动态光散射(DLS)对SiO2/PNIPAm杂化微球进行了表征。结果表明,SiO2/PNIPAm杂化微球粒径约为286 nm,尺寸均一。热重分析表明,PNIPAm接枝率为87%(质量分数),PNIPAm分子链在SiO2粒子上的接枝密度为0.4分子链/nm2。杂化微球表现出明显的温度响应性,温度从25℃升至35℃时,杂化微球粒径从286 nm减小至268 nm,PNIPAm壳层的厚度从16 nm减小至7 nm。     

Properties of osmanthus fragrance‐loaded chitosan–sodium tripolyphosphate nanoparticles delivered through cotton fabrics

Osmanthus fragrance‐loaded chitosan nanoparticles (OF‐NPs) were prepared via complex coacervation successfully. Then, the OF‐NPs were applied in the cotton fabrics directly. The microstructures of OF‐NPs were characterized by dynamic light scattering (DLS), transmission electron microscopy (TEM), Fourier transformation infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). The sustained property of the cotton fabrics treated with OF‐NPs was investigated with scanning electron microscopy (SEM) and gas chromatography‐mass spectrometry (GC‐MS). The common OF was also treated on fabrics for the parallel comparison. TEM and DLS displayed that the spherical OF‐NPs kept about 130 nm and dispersed evenly. FTIR confirmed that OF had been interacted with chitosan via the hydrogen bonds. TGA demonstrated that the thermal stability of OF‐NPs had been improved in contrast to OF and the loading content of OF was as high as 12.05%. SEM and GC‐MS displayed that the cotton fabrics treated by OF‐NPs had an excellent washing resistance. Overall, nanoencapsulation with CS‐TPP will provide an excellent method for releasing fragrance. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Synthesis of fluorine-containing latexes with core–shell structure by UV-initiated microemulsion polymerization

A core–shell structure of fluorine-containing polyacrylate latex was synthesized by UV-initiated two-stage microemulsion polymerization from styrene (St) and hexafluorobutyl acrylate (HFA) in the presence of Irgacure 2959 as hydrophilic photoinitiator at room temperature. The first polymerization stage took 12 min and the second stage took 10 min. The conversions of the first and the second polymerization stages were about 60 and 85 %, respectively. Fourier transform infrared (FTIR) spectra, transmission electron microscopy (TEM), dynamic light scattering (DLS), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and contact angle analysis were used to characterize the properties of latexes and their films. The DLS analysis results indicated that the size of the fluorine-containing nanoparticle is about 20 nm. The TEM photos showed that the particles have core–shell structure and some of the cores are located in the center and the others deviate from the center of particles. From the FTIR and XPS results, we can infer that the fluorine monomer could be introduced into the copolymer and the fluorine-containing polyacrylate mainly occupies the shell part. The TGA results indicated that the fluorine-containing polyacrylate copolymers exhibited higher thermal stability than that of the fluorine-free one. The contact angle analysis results showed that fluorine monomers make the film surface more hydrophobic.     

Preparation and characterization of fluorescent polymer magnetic particles

Magnetic iron oxide (maghemite, Fe₃O₄) particles were encapsulated with fluorescent polymer phase. The resulting fluorescent magnetic polymer particles were characterized by Fourier transform infrared spectroscopy (FTIR), thermal gravimeter analysis (TGA), reflection optical microscopy, differential scanning calorimeter (DSC), Fritsch particle sizer, scanning electron microscopy (SEM), powder X‐ray diffractometer (XRD), and vibrating sample magnetometer (VSM) measurements. FTIR and XRD confirmed the presence of iron oxide in polymer phase. The TGA and DSC measurements indicated that the magnetic polymer particles have more than 50% iron oxide content and high thermal stability. SEM and reflection optical microscopy under UV light revealed that all maghemite particles were embedded in the polymer spheres and have fluorescent characteristics. The size‐distribution analysis of prepared magnetic particles was shown that the means diameter of the particles slightly increased. According to our magnetometry data, shape of the loops evidences the ferromagnetic character of the material and no evidence of superparamagnetism was seen. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Vermiculite/polyacrylamide copolymers microspheres for profile control in oilfields

Polyacrylamide copolymers (PAMVT) microspheres were prepared through inverse emulsion polymerization by using acrylic acid (AA), 2‐acrylamido‐2‐methylpropane sulfonic acid (AMPS) as functional monomers, N,N′‐methylene bis‐acrylamide (MBA) as crosslinker and modified vermiculite (MVMT) with the single‐factor experiments. The initial and swelled particle sizes were tested through the dynamic light scattering (DLS). The swelled particle size under the optimum conditions could be 1.98 μm. The structure was characterized through Fourier transform infrared (FTIR), which indicated that vermiculite has successfully modified and the polymerization reaction was completed. The scanning electron microscopy (SEM) shows that MVMT was evenly filled with PAM copolymers. The water absorption capacity can be up to 80.2%. The recovery efficiency of the water flooding was increased from 69.33% to 77.56%. All these results indicated that the microspheres emulsions could be used as profile control agent to enhance the recovery efficiency. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44918.     

Application of poly (amide-<Emphasis Type="Italic">b</Emphasis>-ethylene oxide)/zeolitic imidazolate framework nanocomposite membrane in gas separation

Mixed matrix membranes (MMMs) are gaining increasing interest in academic and industrial research due to their combined, desirable properties of both polymers and organic/inorganic filler as important materials. In this work, synthesized zeolitic imidazolate framework (ZIF-8) suspension (10–50 wt%) was directly incorporated into a [poly (amide-b-ethylene oxide) Pebax^® 1657] matrix in order to improve the gas separation performance of the membrane. Dynamic light scattering (DLS) analysis showed an average diameter of 77.4 nm for the prepared nanoparticles. The transparent membranes were characterized by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Fourier transform infrared (FTIR) spectroscopy, and X-ray diffractometry (XRD). These indicated excellent dispersion of nanoparticles, which was achieved by ultrasonication before casting the solution. Incorporation of ZIF-8 as filler in the polymer matrix led to improved thermal and mechanical stability of the membranes. This was confirmed by TGA and tensile analyses, indicating good contacts provided at the polymer/filler interfaces. The effect of ZIF-8 loading (up to 50 wt%) on membrane performance was investigated and it showed an optimum loading of 30 %. Single gas (CO₂, N₂ and CH₄) permeation tests revealed rapid, enhanced permeability of the nanocomposite membranes without significant changes in selectivity (compared to those of the pristine polymeric membrane). The permeability increases for CO₂, CH₄ and N₂ in the optimum Pebax^® 1657/ZIF-8 (30 wt%) membrane were found in the stated order as 111, 88 and 99 %. The study revealed that Pebax^® 1657/ZIF-8 membranes displayed better gas permeation properties compared to those of Pebax^® 1657.     

阿维菌素凝胶微球制备及其缓释性能研究

以壳聚糖(CS)和海藻酸钠(ALG)为包封材料,以阿维菌素(AVM)为芯材,采用锐孔法制备了阿维菌素-海藻酸钠-壳聚糖微球,考察了海藻酸钠质量分数、壳聚糖质量分数、氯化钙质量分数和芯壁体积比(质量分数1%的阿维菌素乳液与质量分数3%海藻酸钠溶液的体积比)对微球形态及包埋率的影响,利用SEM、FTIR等对微球结构及性质进行了表征,并考察了其在土壤中的缓释性能和释药机制。结果表明,经优化的制备条件为:海藻酸钠、壳聚糖及氯化钙的质量分数分别为3%、0.6%及5%,芯壁体积比为1∶2,制备的载药微球形状规整,成球性良好,粒径约0.7 mm,载药量31.65%,包埋率83.81%;红外光谱分析显示,芯壁材料之间除氢键外,没有发生化学作用。所制备的阿维菌素微球在土壤中具有缓释特性,42 h累积释药率达到82.06%,之后药物释放减缓。药物释放特性符合Riger-Peppas模型,释放机理为Fick扩散。     

Facile and green preparation of thermal and ph sensitive hydrogel microspheres based on spray drying and the diels–alder reaction

Thermal and pH dual‐sensitive hydrogel microspheres were fabricated using spray drying. During the spray drying, chemical crosslinks were formed in situ via the Diels–Alder reaction without the involvement of any catalysts or organic solvents. The structures and morphologies of the products were characterized by Fourier Transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), Raman spectroscopy, scanning electron microscopy (SEM), X‐ray diffraction (XRD), and thermogravimetric analysis (TGA). A general weighing method was applied to study the swelling behavior of the microspheres at different temperatures and pHs. Using urea as a model molecule, the ability of the microspheres to control the release of urea was explored by spectrophotometry and calculated from the calibration curve obtained from the reaction of urea and diaminobenzaldehyde. The as‐prepared microspheres show a reversible and reproducible volume change with varying pH or temperature, and their swelling ratios increase with increasing temperature or pH. Furthermore, the urea release rates can be tuned by changing the pH or the temperature. Since spray drying can easily produce microspheres on a large scale, the strategy demonstrated here has the potential for applications in the green preparation of hydrogel microspheres. POLYM. ENG. SCI., 59:1999–2007, 2019. © 2019 Society of Plastics Engineers     

Magnetic field responsive methylcellulose-polycaprolactone nanocomposite gels for targeted and controlled release of 5-fluorouracil

5-Fluorouracil loaded magnetic field sensitive methylcellulose and polycaprolactone gels were prepared and characterized by FTIR, XRD, TGA, SEM, and VSM. Swelling analysis supplied important information on drug diffusion properties. The release profile of gels was investigated in different buffer solutions and the highest release values were observed at pH = 7.2. Release kinetic was analyzed using an empirical equation to clarify the transport properties of drug. The effects of nanoparticle concentration and applying external magnetic field were investigated on release profile. The results indicated that the drug release decreased by both, applying external magnetic field and increasing the concentration of Fe₃O₄ nanoparticles.     

Studies on Preparation and Hydrogen Storage Properties of Dual-Metal Ferrocenyl Coordination Polymer Microspheres

A series of dual-metal ferrocenyl coordination polymer microspheres (M₁M₂-CPMs, M₁M₂ = CoMn, CoCu, MnCu) were synthesized by the reaction of 1,1′-ferrocene dicarboxylic acid with mixed metal salts via solvothermal method. From SEM and TEM images, it was found that all the as-synthesized coordination polymers showed microspheres structures. The products were also characterized by X-ray photoelectron spectroscopy (XPS), fourier transform infrared (FT-IR), powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA). The M₁M₂-CPMs showed good thermostability and remained stable up to 250 °C. These M₁M₂-CPMs exhibited hydrogen uptake capacity. More interestingly, through the comparison among three microspheres we found that the M₁M₂-CPMs with hollow structures showed better hydrogen uptake.     

Characterization and Application of Intercalated Montmorillonite with Verapamil and its Polymethyl Methacrylate Nanocomposite in Drug Delivery

This work examined two drug delivery systems: the first system studied the adsorption of Verapamil hydrochloride drug into montmorillonite clay (MMT) by intercalation process to prepare MMT-Verapamil hybrid at different intercalating time, temperatures, pH values and initial drug concentrations. The second system includes the preparation of MMT-Verapamil hybrid combined with polymethyl methacrylate via an emulsion polymerization process to produce a novel nanocomposite material to be used in drug delivery. The polymerization process was carried out using an ultrasonic technique to achieve a biologically safe drug delivery system. Best conditions for the intercalation of verapamil hydrochloride drug into the interlayer of MMT clay were found to be at 50°C and 1 hr using pH ranges of 4–6. The prepared MMT-Verapamil hybrid and the produced MMT-verapamil-MMA nanocomposite material were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and thermal gravimetric analysis (TGA). The in-vitro release profile of Verapamil in the case of a drug hybrid is faster than the release in the case of a drug nanocomposite in both gastric and intestinal fluids where, in the case of gastric fluid (pH 1.2), about 40% of the loaded drug was released from the drug hybrid in the first 4 h against only 37% in 5 h in the case of drug nanocomposite. Also in the intestinal fluid (pH 7.4), the verapamil release from drug hybrid reached 68% in 5 h against only 57% was released from drug nanocomposites in 7 h.     

Controlled biofertilizer release kinetics and moisture retention in gum xanthan-based IPN

A crosslinked interpenetrating network based on gum xanthan was produced in the presence of gamma radiation and its potential as controlled release fertilizer was evaluated. Different process parameters such as gamma radiation dose, solvent amount, crosslinker and monomer concentrations were optimized to determine the maximum fluid uptake capacity of the synthesized sample. The samples were characterized using FTIR, XRD and SEM. The thermal stability was investigated using TGA, DTG and DTA techniques. The biofertilizer extracted from vermicompost was used as model agro-chemical and the presence of essential macro- and micronutrients in the biofertilizer was confirmed by chemical analysis. The in vitro release kinetics was administered by Korsmeyer–Peppas model. Release exponents were found in the range of 0.8–0.9, signifying the non-Fickian mode of diffusion where the relaxation of polymer matrix also played an important role. Further, the impact of biofertilizer control release on Cicer arietinum plant growth was investigated and it was found that there was an increase in stem and root bio-mass. The synthesized candidate polymer was found to act as a mini-water reservoir in different soil types and prolonged soil moisture for more than 50 days. Therefore, the synthesized superabsorbent with controlled release of biofertilizer can protect the environment from adverse effects of carcinogenic synthetic fertilizer leaching, along with its functionality to act as water reservoir in the fields.     

Preparation of PAM/PVA blending films by solution-cast technique and its characterization: a spectroscopic study

Polyacrylamide (PAM) and poly(vinyl alcohol) (PVA) were blended with different weight percentages (70/30, 50/50, 30/70) using solution-cast technique. The prepared films were studied by different characterization techniques. The effect of PVA content on PAM blends was investigated by Fourier transform infrared (FTIR), ultra violet visible (UV–vis), thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). Different mechanical properties of blends were also studied. Significant changes were observed in FTIR, UV–vis, TGA, SEM and mechanical analysis which revealed interactions between the two polymers. FTIR spectra showed the presence of hydrogen bonding between PAM and PVA and hydrophilic nature of the blends. Different optical properties were studied by UV–vis spectroscopy. The weight loss, as a function of temperature of blends, was analyzed by TGA. The results obtained from different experimental techniques were supported by SEM image analysis. FTIR analysis confirmed the conclusion on the specific hydrogen bonding between –CONH₂ groups in PAM and –OH group in PVA. These results showed the change in the thermal stability and mechanical properties. FTIR analysis revealed that a blend ratio of 50/50 wt% had maximum intermolecular interaction between two polymers. It was finally concluded that blend films with the above ratio display higher thermal stability and improved mechanical properties. Due to changes in interactions, the optical parameters were also changed.