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MOLECULES · 2023 ·Vol. 28 ·期 5 ·2246 · IF 4.6

Grafting of Maleic Anhydride onto Poly(vinylidene fluoride) Using Reactive Extrusion

Cuichuan Zhang,Zhiqiang Lu,Bin Wu,Shu-Dong Jiang,Jiasheng Qian

Poly(vinylidene fluoride) was grafted with maleic anhydride through reactive extrusion by using diisopropyl benzene peroxide as an initiator and 9-vinyl anthracene as a stabilizer. Effects of various parameters on grafting degree were investigated including the amounts of monomer, initiator and stabilizer. The maximum extent of grafting achieved was 0.74%. The graft polymers were characterized using FTIR, water contact angle, thermal, mechanical and XRD studies. Improved hydrophilic and mechanical properties were observed for graft polymers.Keywords:PVDF;MAH;stem grafting;melt extrusion

研究领域: 材料科学 · 化学工程
✓ 已验证 产品关联 DOI PubMed 高影响因子
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MOLECULES · 2021 ·Vol. 26 ·期 16 ·4982 · IF 4.412

Sustained-Release Solid Dispersion of High-Melting-Point and Insoluble Resveratrol Prepared through Hot Melt Extrusion to Improve Its Solubility and Bioavailability

Wenjing Zhu,Wenling Fan,Xiaotong Zhang,Meiqi Gao

This study aimed to prepare a sustained-release solid dispersion of poorly water-soluble resveratrol (RES) with high melting point in a single hot melt extrusion step. A hydrophobic–hydrophilic polymeric blend (Eudragit RS and PEG6000) was used to control the release of RES. With the dispersive mixing and high shear forces of hot melt extrusion, the thermodynamic properties and dispersion of RES were changed to improve its solubility. The effects of the formulation were investigated through univariate analysis to optimize the preparation of the sustained-release solid dispersion. In vitro and in vivo studies were performed to evaluate the prepared RES/RS/PEG6000 sustained-release solid dispersion. The physical state of the solid dispersion was characterized using differential scanning calorimetry and X-ray diffraction. Surface properties of the dispersion were visualized using scanning electron microscopy, and the chemical interaction between RES and excipients was detected through Fourier-transform infrared spectroscopy. Results suggested that the optimized sustained-release solid dispersion was obtained when the mass ratio of RES-polymeric blend was 1:5, the ratio of PEG6000 was 35%, the barrel temperature was 170 °C, and the screw speed was 80 rpm. In vitro studies demonstrated that the solid dispersion showed a good sustained release effect. The cumulative release of RES reached 82.42% until 12 h and was fit by the Weibull model. In addition, the saturated solubility was 2.28 times higher than that of the bulk RES. In vitro studies demonstrated that the half-life increased from 3.78 to 7.09 h, and the bioavailability improved to 140.38%. The crystalline RES was transformed into the amorphous one, and RES was highly dispersed in the polymeric blend matrix.Keywords:solid dispersion;resveratrol;hot melt extrusion;dissolution;sustained-release

研究领域: 药剂学 · 生物制药
✓ 已验证 DOI PubMed 高影响因子
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INTERNATIONAL JOURNAL OF PHARMACEUTICS · 2021 · IF 5.875

Improving chemical stability of resveratrol in hot melt extrusion based on formation of eutectic with nicotinamide

Huanyue Zhou,Yu Wang,Shuting Li,Ming Lu

Hot melt extrusion (HME) is a technique applied in the preparation of pharmaceutical amorphous solid dispersions (ASD). Notably it is important to prevent thermal degradation of heat-sensitive drugs during HME. In this study, we present a new strategy to improve chemical stability of pharmaceutical compounds during HME through the formation of eutectics with small molecules. Resveratrol (RES) was selected as the model compound because it is a heat-liable natural product with a very high melting point of 267 °C. When heated at its melting point for 3 min, it degrades by 40%. RES can co-crystallize with nicotinamide (NIC) in solution, however, it can only form a eutectic with NIC during heating. HPMCAS was selected as the polymer matrix and the drug loading of RES was fixed as 20% (weight ratio). The lowest extrusion temperature that can result to RES-HPMCAS ASD is 215 °C. At this temperature, RES shows 7.36% degradation during extrusion. Replacement of 21.4% HPMCAS with NIC decreased the melting temperature of NIC and thus lowered the minimal extrusion temperature to 155 °C. This effectively prevented thermal degradation of RES without negatively affecting non-sink dissolution. The only extra cost for this method is stricter storage conditions (low temperature and low humidity) due to the low glass transition temperature of NIC. Similar strategy may be applied to other heat-liable drugs in similar ways. This study demonstrates the use of eutectic formation for preventing thermal degradation of drug during extrusion of ASD.

CAS / MDL: 10102-40-6
研究领域: 药学 · 材料科学
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JOURNAL OF APPLIED POLYMER SCIENCE · 2024 · IF 2.7

Unlocking the Potential of Polylactic Acid: Exploring Its Thermal and Mechanical Properties for Vitrimerization via Double Reactive Extrusion and Transesterification

Linda Yahia Cherif,Nacira Naar,Ahmed Mekki,Amina Ouadah,Rania Ahmed Hamada,Djalal Trache

Polylactic acid (PLA) is a biosourced thermoplastic polymer widely used in various fields such as biomedical, packaging, and prototyping. Enhancing PLA thermal and mechanical properties has been a research focus, by transforming it into a vitrimer, a new polymer class. This study demonstrated the effectiveness of a dual reactive extrusion process followed by vacuum compression molding to improve a thermoplastic's properties with vitrimer tendency, using PLA as the main component, diglycidyl ether bisphenol A (DGEBA) as an additive, and zinc acetate as a catalyst. Several characterizations were carried out to assess the thermal, morphological, and mechanical properties of the developed PLA mixtures. Moreover, a kinetic study using three iterative isoconversional integral models (iterative Kissinger–Akahira–Sunose (it-KAS), iterative Flynn–Wall–Ozawa (it-FWO), and Trache–Abdelaziz–Siwani) was employed to analyze the effects of the catalyst and DGEBA on the cross-linking reaction kinetics after the process employed in this work. Results demonstrated the presence of a cross-linked structure in addition to a promising polymer behavior characterized by enhancements in toughness, ductility, and cross-linking density by 290%, 127.5%, and 80.5%, respectively. Finally, the optimal composition exhibited almost 96% self-healing of its surface, demonstrating significant potential for advanced material applications.

CAS / MDL: 1675-54-3
研究领域: 材料科学 · 聚合物化学 · 生物医学工程
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Metals · 2025 ·Vol. 15 ·期 3 ·337 · IF 2.5

Effect of Extrusion Temperature on the Microstructure and Properties of Biomedical Mg-1Zn-0.4Ca-1MgO Composite

Shuaipeng Gao,Shaoyuan Lyu,Qian Zhao,Minfang Chen

The effects of extrusion temperatures on the microstructure, mechanical properties, and corrosion performance of biomedical Mg-1Zn-0.4Ca-1MgO composites were systematically investigated. The results indicated that lower extrusion temperatures notably refined the grain size and promoted the formation of numerous nano-scaled secondary phase particles. The grain sizes were 0.8 μm, 1.7 μm, and 3.4 μm for the materials extruded at 280 °C, 310 °C, and 330 °C, which were named ET280, ET310, and ET330. The finest grain size and abundant precipitates enhanced the mechanical properties of the composite with a microhardness of 86.9 HV, a yield strength of 305 MPa, and a fracture elongation of 15.2%. Moreover, the ET280 alloy with ultra-fine grains exhibited the optimal corrosion resistance among these three composites, and its annual corrosion after immersion in Hank’s solution for 14 days was only 0.17 mm/y. The excellent performance in vitro immersion was mainly attributed to the formation of the uniformly dense Ca-P layer on its surface and the contiguous compact Mg(OH)2layer, which could effectively weaken the contact between the corrosive solution and the Mg matrix.

研究领域: 材料科学 · 生物医学工程
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2022 · IF 5.895

Efficient Retention and Complexation of Exogenous Ferulic Acid in Starch: Could Controllable Bioextrusion Be the Answer?

Shuohan Ma,Qingqing Zhu,Siyu Yao,Ruihao Niu,Yu Liu,Yu Qin,Yuxue Zheng,Jinhu Tian,Dandan Li,Wenjun Wang,Donghong Liu,Enbo Xu

The starch–phenolics complexes are widely fabricated as functional foods but with low phenolics retention limited by traditional liquid reaction and washing systems. In this study, ferulic acid (FA, 5%) was exogenously used in the crystalline form, and it reacted with starch in a high-solid extrusion environment, which was simultaneously controlled by thermostable α-amylase (0–252 U/g). Moderate enzymolysis (21 or 63 U/g) decreased the degree of the starch double helix and significantly increased the FA retention rate (>80%) with good melting and distribution. Although there were no significantly strong chemical bonds (with only 0.17–2.39% FA bound to starch hydrolysate), the noncovalent interactions, mainly hydrogen bonds, van der Waals forces, and electrostatic interactions, were determined by 1H NMR and molecular dynamics simulation analyses. The phased release of total FA (>50% in the stomach and ∼100% in the intestines) from bioextrudate under in vitro digestion conditions was promoted, which gives a perspective for handing large loads of FA and other phenolics based on starch carrier.

CAS / MDL: 1135-24-6
研究领域: 食品科学 · 生物化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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CERAMICS INTERNATIONAL · 2023 · IF 5.2

Effect of the slurry composition on the piezoelectric properties of PZT ceramics fabricated via materials extrusion 3D printing

Kai Liu,Yuhang Xia,Qingqing Zhang,Yanying Du,Yusheng Shi,Sanjay Joshi,Chunze Yan,Yanjiao Wu,Shangyu Huang,Huajun Sun

Herein, the effect of the binder content in lead zirconate titanate (PZT) slurry has been systematically studied to improve the piezoelectric properties of PZT ceramics prepared via material extrusion 3D printing . For smooth printing, a slurry with a binder concentration ranging from 6 to 12 wt% was proposed. The porosity of the green body first decreased and then increased with an increase in the binder concentration, and the minimum porosity was obtained when the binder concentration reached 10 wt%. Samples with increased density were obtained after debinding and lead-rich atmosphere sintering. PZT piezoceramics fabricated using a binder content of 10 wt% exhibit the maximum relative density (96.9%), largest piezoelectric constant (342.6 pC/N) and dielectric constant (1621). Based on the above process, the wood pile structure and helical twentytetrahedral structural components were successfully fabricated using the material extrusion process. This research lays the foundation for the engineering application of 3D printing to fabricate high-performance piezoceramics with complex shapes.

CAS / MDL: 7732-18-5
研究领域: 材料科学 · 电子工程
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CARBOHYDRATE POLYMERS · 2024 · IF 10.7

Variations in the effects of extrusion treatments and ferulic acid addition on starch digestibility with different botanical backgrounds

Xianglong Zhou,Tao Huang,Shulin Deng,Hongsheng Liu,Wenwen Yu

In the current study, the effects of extrusion using a haake rheometer with a twin-roll mixer, with and without FA addition, on the structures and in vitro digestibility of starches from different sources were investigated. After extruding for 15 min at 90 °C with a moisture content of 40 %, no matter FA was added or not, lager Ap molecules were preferentially debranched, while Am with longer CL were depolymerized simultaneously, resulting to reduced averaged molecular size of Ap and shortened Am chains. Of all starches, regardless of their botanical backgrounds, although synergic effects were found between extrusion and FA addition on reducing their relative crystallinity and the ordered structures, distinctly different effects on the in vitro digestibility of these starches have also been observed especially regarding the digestion of starch branches with DP > 10 Particularly, the Am chains with DP 10–1000 was remaining undigested when FA was added. This study provides important information concerning how to adjust starch digestibility into a healthy range through altering the starch structures using extrusion technique with the addition of phytochemicals or not.

CAS / MDL: 1135-24-6
研究领域: 食品科学 · 生物化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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SCIENCE OF THE TOTAL ENVIRONMENT · 2020 · IF 6.551

Preparation of porous antibacterial polyamide 6 (PA6) membrane with zinc oxide (ZnO) nanoparticles selectively localized at the pore walls via reactive extrusion

Qi Tang,Kang Wang,Xiaoming Ren,Qunchao Zhang,Weiwei Lei,Tao Jiang,Dean Shi

Antibacterial polymer membranes have been widely used in many fields of our daily life. In this study, porous PA6 membrane with ZnO nanoparticles attaching on to the surface of inner pore walls is prepared. Firstly, SMA (styrene maleic anhydride copolymer) is used to graft onto the surface of ZnO nanoparticle in DMF (dimethylformamide). Then the pre-treated ZnO nanoparticles (ZnO-SMA) are added into SEBS (Styrene-ethylene-butylene-styrene copolymer)/PA6 (60/40 wt/wt) blends with co-continuous morphology. The effects of SMA molecular structure (molecular weight and maleic anhydride content) used for ZnO-SMA nanoparticles on their dispersion states in SEBS/PA6/ZnO-SMA nanocomposites are investigated. When SMA3 (MAH = 8 wt%, Mn = 250,000 g mol −1 ), which has relatively higher molecular weight and lower MAH content, is used as the pre-treating agent, ZnO-SMA3 nanoparticles tend to be dispersed at the phase interface in SEBS/PA6/ZnO-SMA nanocomposites. However, when SMA2 (MAH = 23 wt%, Mn = 110,000 g mol −1 ) with relatively lower molecular weight and higher MAH content is used, no ZnO-SMA2 nanoparticles locate at the interface but stay within PA6 phase. Porous PA6 membranes are obtained by selectively etching SEBS phase out with xylene. It can be found that porous PA6 membrane containing ZnO-SMA3 nanoparticles still exhibits much better antibacterial property (R = 3.76) toward S. aureus even at a very low ZnO content (0.5 wt%). This result should be ascribed to almost all the ZnO-SMA3 nanoparticles being exposed to the surface of inner pore walls of PA6 membrane. This work proposes an effective method to prepare porous polymer membrane with functional nanoparticles selectively located at the inner pore walls.

研究领域: 材料科学 · 生物医学工程
✓ 已验证 DOI PubMed 高影响因子
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PHARMACEUTICAL DEVELOPMENT AND TECHNOLOGY · 2015 · IF 1.202

Application of quality by design (QbD) to formulation and processing of naproxen pellets by extrusion–spheronization

Junlin Wang,Shuling Kan,Tong Chen,Jianping Liu

The aim of this research was to apply quality by design (QbD) to the development of naproxen loaded core pellets which can be used as the potential core for colon-specific pellets. In the early stages of this study, prior knowledge and preliminary studies were systematically incorporated into the risk assessment using failure mode and effect analysis (FMEA) and fishbone diagram. Then Plackett–Burman design was used to screen eight potential high risk factors (spheronization speed, spheronization time, extrusion speed, drying method, CCMC-Na concentration, lactose concentration, water concentration and Tween 80 concentration) obtained from the above risk assessment. It was discovered that out of the eight potential high risk factors only three factors (spheronization speed, extrusion speed and CCMC-Na concentration) had significant effects on the quality of the pellets. This allowed the use of Box–Behnken design (BBD) to fully elucidate the relationship between the variables and critical quality attribute (CQA). Finally, the final control space was established within which the quality of the pellets can meet the requirement of colon-specific drug delivery system. This study demonstrated that naproxen loaded core pellets were successfully designed using QbD principle.

CAS / MDL: 77-93-0
研究领域: 药剂学 · 制药工程
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF FOOD PROCESS ENGINEERING · 2022 ·Vol. 46 ·期 2 ·e14221 · IF 2.889

Clarifying the effect of rheological parameters of starch fluid on tensile properties of final extrudate in twin-screw extrusion by numerical simulation

Qiannan Liu,Wei Liu,Chao Bi,Xiaojia Hu,Tingting Zhang,Liang Zhang,Honghai Hu

The distribution of the flow field, the input energy of the twin-screw, and the dissipated energy on the fluid during the twin-screw extrusion process were calculated by the POLYFLOW software to establish the relationship between the rheological parameters of starch fluid and tensile properties of the final extrudate. The results demonstrated that the pressure difference, the input energy of the twin-screw, and the dissipated energy on the fluid were directly proportional to the zero-shear viscosity ( η 0 ), reduced with the raise of the relaxation time constant ( λ ) and raised with the raise of the power-law index ( n ). When the moisture content of starch fluid raised, the η 0 value reduced, whereas the λ value and n value increased. The pressure difference, the input energy of the twin-screw, and the dissipated energy on the fluid decreased, reducing the maximum tensile force of the final extrudate. Through numerical simulation and experimental verification, it was found that the changes of η 0 value, λ value, and n value restricted each other on the tensile properties of final extrudate. Based on the numerical simulation, the tensile properties of the final extrudate could be predicted through rheological parameters of starch fluid. Practical Applications A method was established to predict the final extrudate properties based on rheological parameters and numerical simulation in this study. Based on the numerical simulation, the tensile properties of the final extrudate could be predicted through rheological parameters of starch fluid. This research will provide insight into the mechanism of twin-screw extrusion of starch-based materials.

CAS / MDL: 9005-25-8
研究领域: 食品科学与工程 · 材料科学
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CHINESE JOURNAL OF POLYMER SCIENCE · 2020 ·Vol. 39 ·期 5 ·566-572 · IF 3.154

Foam/Film Alternating Multilayer Structure with High Toughness and Low Thermal Conductivity Prepared via Microlayer Coextrusion

Luo Qi,Pu Hong-Ting,Zhang Zhi-Hua,Zhang Xiong,Yu Cheng-Long

Multilayer membranes prepared via microlayer coextrusion have attracted wide attention due to their unique properties and broad applications. In present study, the foam/film alternating multilayer sheets based on ethylene-vinyl acetate copolymer (EVA) and high-density polyethylene are successfully prepared via microlayer coextrusion. The cells in the sheets are single-cell-array along the foamed EVA layers with uniform cell size. In addition, the effects of layer number and foam relative thickness on morphology, mechanical properties, damping and heat insulation properties are investigated. The cell size decreases significantly with increasing layer number due to the enhanced confine effects. The tensile strength, elongation at break, and heat insulation also increase significantly. However, the mechanical damping properties change little in the observed frequency. Meanwhile, with higher relative thickness of EVA foam, the sheets have lower tensile strength and lower thermal conductivity, while the damping properties are enhanced in a specific frequency scope. The elongation at break of the optimized sample comes to 800% and the thermal conductivity decreases to 61 mW·m −1 ·K −1 , which shows high toughness and low thermal conductivity, indicating a possible method for preparing materials with high toughness and heat-insulating properties.

CAS / MDL: 471-34-1
研究领域: 材料科学 · 高分子科学
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