Microstructure and mechanical properties of polypropylene/polystyrene blend filled with as-synthesized MCM-41 prepared by melt-compounding

Nano-sized as-synthesized MCM-41 particle, whose pore channels and outer surface full of organic CTAB template, was used as compatibilizers for immiscible polypropylene (PP)/polystyrene (PS) blends. In this paper, the solid structure SiO₂ was selected to compare with as-synthesized MCM-41 in properties of PP/PS blend. The mechanical results showed that tensile strength of the blend was increased by 32% and the impact strength was increased by 41.1% by addition low content of as-synthesized MCM-41 compared to pure PP/PS. The presence of SiO₂ in the blend cannot improve the mechanical properties obviously. SEM indicated that incorporation of as-synthesized MCM-41 into PP/PS blend can act as compatibilizer, which resulted in a decreased particle size of dispersion phase together with morphological evidence of interfacial adhesion. However, with the presence of SiO₂, 1%, 3%, in the blend, the interface did not show clear change compared with the PP/PS blend.     

Preparation and characterization of epoxy composites filled with functionalized nano-sized MCM-41 particles

Mono-dispersed nano-sized MCM-41 (M (with template)) particles were synthesized by sol–gel reaction. The effect of interface modification on the properties of epoxy composites was investigated. Modifications were carried out either by substituting silanol groups on the surface or in the mesopore channels into amine (M-NH₂), calcinating mixture template in the mesopore channels (M(without template)), or recalcinating them at higher temperature to remove silanol groups (–OH) in the mesopore channels or on the surface (CM). Transmission electron micrograph results showed that the dispersing of MCM-41 nanoparticles was not influenced by the modification, while –NH₂ group indeed modified the mesopore channels or the surface of MCM-41 particle by using IR, XRD, and N₂ adsorption–desorption. In addition, tensile tests suggested that M-NH₂ nanoparticles could simultaneously provide epoxy matrix with strengthening and toughening effects. However, due to the different interfacial structures between the fillers and the matrix, the mechanical properties of the composites filled by M-NH₂ were much better than those of composites filled by MCM-41 (without template), MCM-41 (with mixture template), and CM.     

Incorporation of nano-sized mesoporous MCM-41 material used as fillers in natural rubber composite

The nano-sized mesoporous MCM-41 (without template), and the modification of MCM-41 (without template) were used to prepare natural rubber (NR) composites. The effects of coupling agents γ-aminopropyltriethoxysilane (KH-550), γ-methacryloxypropyltrimethoxysilane (KH-570), bis-(γ-triethoxysilylpropyl)-tetrasulfide (Si-69), isopropyl tri-(dioctylpyrophosphate)titanate (NDZ-201) on the mechanical properties of the composites were also investigated. The results showed that the tensile properties of Natural rubber/mesoporous MCM-41 nanocomposite were improved as compared with those of NR compound. KH-570 had good effect on enhancing the overall properties of the composites. Scanning electron microscopy (SEM) observations revealed that the modified nano-sized MCM-41 material was well dispersed in the polymer matrix and the enhancement of the interface between the matrix and fillers was obtained.     

Influence of mesoporous silica and hydroxyapatite nanoparticles on the mechanical and morphological properties of polypropylene

This paper presents the effect of different types of additives on the morphology and mechanical performance of polypropylene (PP). Three different types of nanoparticles, containing mesoporous silica (MCM-41), Hydroxyapatite (HA) and the composite of MCM-41 and HA (MH) were used. Nanocomposites containing PP, 3 wt.% of maleic anhydride grafted polypropylene (PP-g-MA) and 3 wt.% of different nanoparticles were prepared using the melt-compounding technique in a twin-screw extruder. The bulk mechanical response of the nanocomposites such as tensile, flexural and Izod impact properties were studied. The results of mechanical tests show that at the same nanomaterial content, all the nanofillers cause better tensile, flexural and impact strength than neat PP. The MH nanoparticle improves the mechanical properties of PP, better than the other nanoparticles because this nanofiller contains good properties of both MCM-41 and HA nanoparticles in itself. In order to investigate the effect of foam agent on the mechanical properties of neat PP and nanocomposites based on PP, inorganic azodicarboxamide was added to the aforementioned mixtures as chemical blowing agent and the foamed specimens were resulted using the melt-compounding technique. The results reveal that addition of foam agent to mixtures, leads to increase the flexural characteristics of samples, but the tensile properties and impact strength decrease. Scanning electron microscopy (SEM) was used to assess the fracture surface morphology and the dispersion of the nanoparticles. X ray diffractometry (XRD) was used to examine the intercalation effect on the nanocomposites. The observations show that the nanomaterials were well dispersed in the polymer matrix and the enhancement of the interface between the matrix and fillers was obtained by the incorporation of MH, MCM-41 and HA nanoparticles into PP matrix.     

两种核-壳结构复合微球对聚丙烯的改性研究

以吸附自组装和共缩聚法制备的PS/MCM-41-g-MPS和P(St-MPS)/MCM-41两种具有不同界面作用的"核-壳"结构复合微球为填料,对聚丙烯(Polypropylene, PP)进行改性,研究了复合微球种类及用量对PP力学与结晶性能的影响.结果表明:两种复合微球的添加均可以显著提高PP的力学性能,在复合微球...     

Ultrasonic-assisted synthesis and magnetic studies of iron oxide/MCM-41 nanocomposite

Iron oxide nanoparticles were stabilized within the pores of mesoporous silica MCM-41 amino-functionalized by a sonochemical method. Formation of iron oxide nanoparticles inside the mesoporous channels of amino-functionalized MCM-41 was realized by wet impregnation using iron nitrate, followed by calcinations at 550 °C in air. The effect of functionalization level on structural and magnetic properties of obtained nanocomposites was studied. The resulting materials were characterized by powder X-ray diffraction (XRD), high-resolution transmission electron microscopy and selected area electron diffraction (HRTEM and SAED), vibrating sample and superconducting quantum interface magnetometers (VSM and SQUID) and nitrogen adsorption–desorption isotherms measurements. The HRTEM images reveal that the most of the iron oxide nanoparticles were dispersed inside the mesopores of silica matrix and the pore diameter of the amino-functionalized MCM-41 matrix dictates the particle size of iron oxide nanoparticles. The obtained material possesses mesoporous structure and interesting magnetic properties. Saturation magnetization value of magnetic iron oxide nanopatricles stabilized in MCM-41 amino-functionalized by in situ sonochemical synthesis was 1.84 emu g⁻¹. An important finding is that obtained magnetic nanocomposite materials exhibit enhanced magnetic properties than those of iron oxide/MCM-41 nanocomposite obtained by conventional method. The described method is providing a rather short preparation time and a narrow size distribution of iron oxide nanoparticles.     

A comparative study of the effect of different rigid fillers on the fracture and failure behavior of polypropylene based composites

Polypropylene (PP) composites with 5 wt% of different rigid particles (Al₂O₃ nanoparticles, SiO₂ nanoparticles, Clay (Cloisite 20A) nanoparticles or CaCO₃ microparticles) were obtained by melt mixing. Composites with different CaCO₃ content were also prepared. The effect of fillers, filler content and addition of maleic anhydride grafted PP (MAPP) on the composites fracture and failure behavior was investigated. For PP/CaCO₃ composites, an increasing trend of stiffness with filler loading was found while a decreasing trend of strength, ductility and fracture toughness was observed. The addition of MAPP was beneficial and detrimental to strength and ductility, respectively mainly as a result of improved interfacial adhesion. For the composites with 5 wt% of CaCO₃ or Al₂O₃, no significant changes in tensile properties were found due to the presence of agglomerated particles. However, the PP/CaCO₃ composite exhibited the best tensile behavior: the highest ductility while keeping the strength and stiffness of neat PP. In general, the composites with SiO₂ or Clay, on the other hand, displayed worse tensile strength and ductility. These behaviors could be probably related to the filler ability as nucleating agent. In addition, although the incorporation of MAPP led to improved filler dispersion, it was damaging to the material fracture behavior for the composites with CaCO₃, Al₂O₃ or Clay, as a result of a higher interfacial adhesion, the retardant effect of MAPP on PP nucleation and the lower molecular weight of the PP/MAPP blend. The PP/MAPP/SiO₂ composite, on the other hand, showed slightly increased toughness respect to the composite without MAPP due to the beneficial concomitant effects of the presence of some amount of the β crystalline phase of PP and the better filler dispersion promoted by the coupling agent which favor multiple crazing. From modeling of strength, the effect of MAPP on filler dispersion and interfacial adhesion in the PP/CaCO₃ composites was confirmed.     

Silica materials recovered from photonic industrial waste powder: its extraction, modification, characterization and application

This study explored the possibility of recovering waste powder from photonic industry into two useful resources, sodium fluoride (NaF) and the silica precursor solution. An alkali fusion process was utilized to effectively separate silicate supernatant and the sediment. The obtained sediment contains purified NaF (>90%), which provides further reuse possibility since NaF is widely applied in chemical industry. The supernatant is a valuable silicate source for synthesizing mesoporous silica material such as MCM-41. The MCM-41 produced from the photonic waste powder (PWP), namely MCM-41(PWP), possessed high specific surface areas (1082 m²/g), narrow pore size distributions (2.95 nm) and large pore volumes (0.99 cm³/g). The amine-modified MCM-41(PWP) was further applied as an adsorbent for the capture of CO₂ greenhouse gas. Breakthrough experiments demonstrated that the tetraethylenepentamine (TEPA) functionalized MCM-41(PWP) exhibited an adsorption capacity (82 mg CO₂/g adsorbent) of only slightly less than that of the TEPA/MCM-41 manufactured from pure chemical (97 mg CO₂/g adsorbent), and its capacity is higher than that of TEPA/ZSM-5 zeolite (43 mg CO₂/g adsorbent). The results revealed both the high potential of resource recovery from the photonic solid waste and the cost-effective application of waste-derived mesoporous adsorbent for environmental protection.     

Influence of pH on the sorption behaviour of uranyl ions in mesoporous MCM-41 and MCM-48 molecular sieves

The sorption of uranyl ions in mesoporous MCM-41 and MCM-48 was accomplished with the help of a direct-template-exchange route, and the progress was monitored as a function of pH of the precursor uranyl nitrate solution. Under identical conditions of synthesis, around one and a half times larger amount of uranium was found to be sorbed in MCM-48 (∼12.5 wt.%) as compared to MCM-41 (∼9.5 wt.%). Further, the powder X-ray diffraction (XRD) data revealed that the expansion of unit cell parameters and broadening of reflections of the uranium containing samples depended on the pH of the precursor uranyl solution. Likewise, the Fourier transform infrared spectroscopy (FT-IR) studies showed a progressive decrease in the frequency of the axial OUO asymmetric stretching vibrational band, ν_a(UO) of the anchored uranyl groups with the increase of pH of the exchanging uranyl solution. The presence of two bands at ∼920 and 879 cm⁻¹ for uranyl exchanged samples prepared at pH > 5 indicated the presence of trinuclear (UO₂)₃⁺₅(OH) species. The occlusion of uranium thus depends upon the pore structure of the host material and the nature and dimension of the hydrolysis species formed at a particular pH of uranyl solution. Furthermore, the template-exchange of hexavalent uranium in MCM-41 and MCM-48 not only results in the formation of bulky hydrolysis species in the mesovoids, but also substitutes (isomorphously) in the silicate matrix resulting in the formation of UMCM-41 and UMCM-48.     

Steam-assisted crystallization of TPA+-exchanged MCM-41 type mesoporous materials with thick pore walls

Hierarchical MCM-41/MFI composites were synthesized through ion-exchange of as-made MCM-41 type mesoporous materials with tetrapropylammonium bromide and subsequent steam-assisted recrystallization. The obtained samples were characterized by powder X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis, FT-IR, ¹H–¹³C CP/MAS and nitrogen adsorption–desorption. The XRD patterns show that the MCM-41/MFI composite possesses both ordered MCM-41 phase and zeolite MFI phase. SEM and TEM images indicate that the recrystallized materials retained the mesoporous characteristics and the morphology of as-made mesoporous materials without the formation of bulky zeolite, quite different from the mechanical mixture of MCM-41 and MFI structured zeolite. Among others, lower recrystallization temperature and the introduction of the titanium to the parent materials are beneficial to preserve the mesoporous structure during the recrystallization process.     

SiC-dopped MCM-41 materials with enhanced thermal and hydrothermal stabilities

SiC-dopped MCM-41 mesoporous materials were synthesized by the in situ hydrothermal synthesis, in which a small amount of SiC was added in the precursor solvent of molecular sieve before the hydrothermal treatment. The materials were characterized by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, N₂ physical adsorption and thermogravimetric analysis, respectively. The results show that the thermal and hydrothermal stabilities of MCM-41 materials can be improved obviously by incorporating a small amount of SiC. The structure collapse temperature of SiC-dopped MCM-41 materials is 100 °C higher than that of pure MCM-41 according to the differential scanning calorimetry analysis. Hydrothermal treatment experiments also show that the pure MCM-41 will losses it's ordered mesoporous structure in boiling water for 24 h while the SiC-dopped MCM-41 materials still keep partial porous structure.     

Room temperature synthesis of Si-MCM-41 using polymeric version of ethyl silicate as a source of silica

Synthesis of mesoporous MCM-41 materials at room temperature using less expensive polymeric version of ethyl silicate (40 wt% SiO₂) as a source of silica was established. The influence of crucial synthesis parameters such as molar ratios of H₂O/NH₄OH, NH₄OH/SiO₂ and CTMABr/SiO₂ in gel on the quality of the phase formed was investigated. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and low temperature N₂ adsorption-desorption isotherms have been employed to characterize the products. The magnitude of orderness, textural properties and thermal stability of the Si-MCM-41 samples prepared under identical judiciously pre-controlled synthesis conditions using ethyl silicate and conventional tetraethyl orthosilicate (TEOS) were assessed. Even though, ethyl silicate has proved to be suitable source for the preparation of MCM-41 at room temperature, there exists an optimum value of H₂O/NH₄OH for different NH₄OH/SiO₂ molar ratios in the gel. Changes in the morphology were observed when NH₄OH/SiO₂, H₂O/NH₄OH molar ratios in the gels were changed.     

A novel application of mesoporous silica material for extraction of pesticides

The mesoporous silica material MCM-41 was prepared by the sol-gel method and characterized using X-ray diffraction (XRD), N₂ adsorption-desorption and thermogravimetric analysis. The material was tested for extraction of trichlorfon, pyrimethanil, tetraconazole, thiabendazole, imazalil and tebuconazole from mango fruit, with analysis using gas chromatography-mass spectrometry (GC/MS). In experiments carried out in triplicate, at a 1.0 mg/kg concentration level, recoveries using the MCM-41 sorbent were in the range 73-103%. Comparison of MCM-41 with commercially available silica gel showed that MCM-41 was a similar extracting phase for the pesticides investigated with a significant cost advantage over this conventional material.     

Hollow MCM-41 microspheres derived from P(St-MMA)/MCM-41 core/shell composite particles

In soap-free latex media, poly(styrene-methyl methacrylate)/MCM-41 core/shell composite microspheres have been fabricated by adding silicate source in batches. In this process, silicate species and the surfactant micelles were self-assembled into 2-dimensional hexagonal arrangement on the surface of P(St-MMA) microspheres. Hollow MCM-41 microspheres were obtained via removing polymer core by solvent. XRD, TEM, IR and N₂ adsorption-desorption analysis were applied to characterize products. The results showed that average diameter and wall thickness of hollow MCM-41 microspheres is about 240 nm and 20 nm, respectively. Results of N₂ adsorption-desorption indicate that hollow MCM-41 microspheres possess a highly ordered mesoporous structure and a narrow pore distribution with a mean value of 2.34 nm.     

Nanostructured lanthanum cobaltate: oxidation and coordination states of Co atoms

Lanthanum cobaltate (LaCoO _x ) nanostructured inside the MCM-41 mesoporous molecular sieve as well as in the bulk LaCoO₃ perovskite were characterised by SAXS, ESR, UV–vis DRS, EXAFS and XPS techniques. The nanosized LaCoO _x particles stabilised within the mesopores of MCM-41 matrix containing Co atoms in rather low average oxidation state, which is not characteristic of bulk LaCoO₃ perovskites. Meanwhile, the coordination states of Co in both cases are quite similar. Also, the concentration of Co(II) cations in cobaltate nanoparticles was found to be twice as in bulk LaCoO₃ material. The supported cobaltate does not form short-range ordered species of LaCoO₃ in the MCM-41 matrix but presents as the highly disordered, oxygen-deficient Co oxide nanophase which is probably to be stabilised by La ions present.     

Preparation of high nickel-containing MCM-41-type mesoporous silica via a modified direct synthesis method

A method with modifying tetraethyl orthosilicate (TEOS) with nickel species has been developed for the synthesis of mesoporous silica with high nickel content (11.8 wt.% of Ni or even higher). With the method, MCM-41-type materials were obtained with high BET surface area reaching 868 m²/g and pore volume up to 0.73 cm³/g. The materials were characterized by means of X-ray powder diffraction, transmission electron microscopy, energy dispersive X-ray spectroscopy, N₂ adsorption, Fourier transform infrared and X-ray photoelectron spectroscopy. Nickel species were incorporated into the silica frameworks. The mesostructures still remain after activation using H₂ at 773 K.     

Synthesis of mesoporous silica materials (MCM-41) from iron ore tailings

Highly ordered mesoporous materials were successfully synthesized by using the iron ore tailings as the silica source and n-hexadecyltrimethyl ammonium bromide as the template. The samples were detail characterized by powder X-ray diffraction, scanning electron microscope, high-resolution transmission electron microscopy and N₂ physisorption. The as-synthesized materials had high surface area of 527 m² g⁻¹ and the mean pore diameter of 2.65 nm with a well-ordered two-dimensional hexagonal structure. It is feasible to prepare mesoporous MCM-41 materials using the iron ore tailings as precursor.     

Thermal stability of Si–MCM-41 in gaseous atmosphere

The thermal stability of Si–MCM-41 in different atmosphere (air, O₂, NH₃, N₂, and Ar) has been investigated in the present work; as-synthesized Si–MCM-41 was heat-treated at 800–1030 °C for 6–12 h in the selected atmosphere. Based on absorption–desorption isotherms and low-angle XRD measurement of the treated samples, it was found that the thermal stability varied greatly in different atmosphere. As-synthesized Si–MCM-41 retained mesoporous structure up to 1010 °C in NH₃, N₂, and Ar environment, but in air and O₂ environment, the highest thermal stable temperature of mesoporous structure in Si–MCM-41 was no more than 900 °C.     

Mechanical properties and toughening mechanisms of polypropylene/barium sulfate composites

The effect of interfacial interaction on the mechanical performance of a group of polypropylene (PP)/barium sulfate (BaSO₄) composites were studied. It was found that PP can be toughened with specially treated BaSO₄ particles. The interfacial modification contributes to the toughening in two aspects. The first is to provide a proper interfacial adhesion and control the interfacial debonding occurs at well-timed stages. This ensures the inorganic particles transfer the stress and stabilizes the cracks at the initial stage of the deformation, and satisfy the stress conditions for plastic deformation of matrix ligaments subsequently via debonding. The second is that the modified interface between PP matrix and filler particles increases the nucleating ability of the fillers and retards the motion of the PP chains. This leads to the formation of PP crystals with less perfection and smaller size in the matrix and promotes plastic deformation of the matrix after the debonding occurs.     

Investigation on the mechanism of the photoluminescence of MCM-41

Pure siliceous MCM-41 sample was synthesized in ethylenediamine (EDA) medium. MCM-41 sample calcined at 813 K showed the most strong photoluminescent (PL) effect, while those calcined at 1073 K and 1323 K only showed weak photoluminescence. The intensity of photoluminescence decreased as the calcined temperature increased. By nuclear magnetic resonance (NMR) spectroscopy and infrared (IR) investigation, it was demonstrated that both the Al-depleted defect sites and silanol contents were responsible for the strong PL effect of the investigated MCM-41 samples. It was also suggested that the mesoporous channel structure of MCM-41 influences the investigated PL effect.