Study of different effect on foaming process of biodegradable bionolle in supercritical carbon dioxide

Microcellular foaming of biodegradable Bionolle in supercritical CO₂ has been produced. The effects of a series of variable factors, such as saturation temperature, saturation pressure, and depressurization time and step on the foam structures and density, were studied through measurement of density and SEM observation. The experimental results show that higher saturation temperatures lead to an increase in bulk densities; and different depressurization time and step result in different product cell morphology. In addition, at some saturation temperature, the orientation of the cells can be found in the product morphology. XRD experimental results show that the foaming treatment with SC CO₂ increased the crystallinity of Bionolle. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 2901–2906, 2006     

Generation of microcellular biodegradable polycaprolactone foams in supercritical carbon dioxide

Microcellular foaming of low‐T_g biodegradable and biocompatible polycaprolactone (PCL) in supercritical CO₂ has been studied. The purpose is to apply microcellular materials to drug containers and medical materials for artificial skin or bone. Effects of a series of variable factors on the foam structures, such as saturation temperature, saturation pressure, saturation time, and depressurization time were studied. The experimental results indicate that, while keeping other variables unchanged, higher saturation temperature leads to reduced bulk densities and different saturation pressures result in different nucleation processes. In addition, saturation time has a profound effect on the structure of the product. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 94: 593–597, 2004     

超临界二氧化碳釜压发泡法制备生物可降解PBAT发泡颗粒

通过超临界二氧化碳釜压发泡技术制备了生物可降解聚对苯二甲酸丁二醇酯?co?聚己二酸丁二醇酯（PBAT）发泡颗粒,采用核磁共振光谱仪（¹H?NMR）、凝胶渗透色谱仪（GPC）、差示扫描量热仪（DSC）对PBAT的化学组分及热性能进行了表征,并研究了渗透条件对PBAT发泡性能的影响。结果表明,PBAT中己二酸丁二醇（BA）和对苯二甲酸丁二醇（BT）链节含量分别为53 %和47 %（摩尔分数）;PBAT的玻璃化转变温度、最大熔融温度和结晶度分别是-33、122 ℃ 和13.16 %,其分解温度为280 ℃;当渗透温度从76 ℃增加到90 ℃时,PBAT发泡颗粒密度逐渐降低、发泡倍率逐渐增大,且该条件下制备的PBAT发泡颗粒放置1 d后密度增加、发泡倍率降低,继续延长放置时间至7 d时,其密度和发泡倍率保持不变;当渗透时间从0.5 h延长到2 h时,PBAT发泡颗粒密度逐渐降低、发泡倍率逐渐增加;当渗透时间从2 h延长到3 h时,其密度和发泡倍率保持不变;当渗透压力从10 MPa增加到12 MPa时,PBAT发泡颗粒密度逐渐降低、发泡倍率逐渐增加;当渗透压力从12 MPa增加到14 MPa时,其密度和发泡倍率保持不变。     

Microcellular foaming of poly(phenylene sulfide)/poly(ether sulfones) blends using supercritical carbon dioxide

Microcellular foaming of poly(phenylene sulfide)/poly(ether sulfones) (PPS/PES) blends presents a promising approach to produce high‐performance cellular materials with tailored microstructures and enhanced properties. This study investigated the effects of multiphase blend composition and process conditions on the foaming behaviors and final cellular morphology, as well as the dynamic mechanical properties of the solid and microcellular foamed PPS/PES blends. The microcellular materials were prepared via a batch‐foam processing, using the environment‐friendly supercritical CO₂ (scCO₂) as a blowing agent. The saturation and desorption behaviors of CO₂ in PPS/PES blends for various blend ratios (10 : 0, 8 : 2, 6 : 4, 5 : 5, 4 : 6, 2 : 8, and 0 : 10) were also elaborately discussed. The experimental results indicated that the foaming behaviors of PPS/PES blends are closely related to the blend morphology, crystallinity, and the mass‐transfer rate of the CO₂ in each polymer phase. The mechanisms for the foaming behaviors of PPS/PES blends have been illustrated by establishing theoretical models. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42634.     

Preparation of poly(propylene carbonate)/nano calcium carbonate composites and their supercritical carbon dioxide foaming behavior

Biodegradable polymer foams are attracting extensive attention in both academic and industrial fields. In this study, an emerging biodegradable polymer, poly(propylene carbonate) (PPC), was compounded with nano calcium carbonate (nano‐CaCO₃) and foamed via supercritical carbon dioxide for the first time. Four concentrations of nano‐CaCO₃, 1, 3, 5, and 10 wt %, were used and the thermal properties of PPC/nano‐CaCO₃ composites were investigated. The glass‐transition temperature and thermal decomposition temperature of the PPC/nano‐CaCO₃ composites increased with the addition of nano‐CaCO₃. The morphologies of the PPC/nano‐CaCO₃ composites and the rheological results showed that homogeneous dispersions of nano‐CaCO₃ and percolated nano‐CaCO₃ networks were achieved at a nano‐CaCO₃ content of 3 wt %. Therefore, the finest cell diameter (3.13 μm) and highest cell density (6.02 × 10⁹ cells/cm³) were obtained at the same nano‐CaCO₃ content. The cell structure dependences of PPC and PPC with a nano‐CaCO₃ content of 3 wt % (PPC‐3) foams on the foaming pressure and temperature were investigated as well. The results suggested that the cell structure of PPC‐3 was more stable at different foaming conditions due to the networks of nano‐CaCO₃. Moreover, the change in pressure was more influential on the cell structure than the temperature. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42248.     

超临界CO2萃取大豆卵磷脂工艺条件的研究

本文通过对萃取压力、萃取温度、萃取时间等条件的实验,获得了最佳的工艺参数。实验结果表明,超临界萃取法具有工艺简单、操作安全、产品质量好、萃取效率高等优点。     

Synthesis of montmorillonite/polystyrene nanocomposites in supercritical carbon dioxide

Monomer styrene and initiator N,N′‐azobis(isobutyronitrile) were impregnated into montmorillonite (MMT) galleries using supercritical CO₂ at 35°C and 12.0 MPa, after thermal polymerization of monomer at 65°C, resulting in MMT/polystyrene nanocomposites. The morphology and structure of the products were characterized by FTIR, powder X‐ray diffraction, transmission electron microscopy, differential scanning calorimetry, and thermogravimetric analysis. The results indicate that MMT is dispersed in the composite with intercalated and exfoliated structures, enhancing the thermal stability of nanocomposites. Changing the soaking time and the content of MMT in the supercritical solution during the impregnating process can control the exfoliated extent of MMT. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 94: 1194–1197, 2004     

Application of supercritical carbon dioxide in the preparation of biodegradable polylactide membranes

The application of supercritical carbon dioxide (SCCO₂) has been attracting more and more attention, especially in the formation of polymer membranes. The membrane formation using SCCO₂ is analogous to conventional immersion precipitation process by using organic nonsolvent. Polylactide (PLA) membranes were prepared by phase separation with SCCO₂ as nonsolvent. Two kinds of solvents were used to study the effect of the solvent on the cross‐section structure of the PLA membrane and the compatibility between the solvent and SCCO₂ was studied. The effect of the solvent and the preconditioning on the morphology of the PLA membrane was also investigated through scanning electron microscope, wide‐angle X‐ray diffraction, and polarizing microscopy. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 94: 2158–2163, 2004     

Mechanical and biodegradation properties of bamboo fiber-reinforced starch/polypropylene biodegradable composites

Bamboo fiber (BF)-reinforced starch/polypropylene (PP) composites were prepared by extrusion and injection molding methods. The mechanical and thermal properties and water absorption were evaluated by different methods. Moreover, composite samples were subjected to biodegradation through soil burial test and microbes medium degradation. Different stages of biodegradation were investigated by weight loss, attenuated total reflection Fourier transformed infrared spectroscopy, differential scanning calorimeter, and scanning electron microscope. It was found that contents of BF and starch resin had a significant influence on the properties of the composites. With more content of BF, the composite exhibited a better flexural property and biodegradation. A distinct decrease of weight loss and mechanical properties indicated the degradation caused by the microbes. After biodegradation, thermal stability of the composites decreased while the crystallinity of PP increased. The results prove that the composites more easily tend to be degraded and assimilated by microbes. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 137, 48694.     

超临界CO2萃取辣椒红色素工艺条件的研究

本文通过对萃取压力、萃取温度、萃取时间等条件的探索,获得了最佳的工艺参数。实验结果表明,超临界萃取法具有工艺简单、操作安全、产品质量好、萃取效率高等优点。     

超临界二氧化碳中季铵盐插层改性蒙脱土的制备和结构调控

为了改善蒙脱土的层间结构、分散状态和表面形貌,在以超临界二氧化碳为媒介的环境下,利用十四烷基三甲基溴化铵对钠基蒙土进行有机插层改性,并考察了反应压强和洗涤方式对插层效果的影响。利用热重分析仪(TGA)、X射线衍射仪(XRD)、扫描电镜(SEM)和比表面积仪(BET)对样品进行分析和表征。结果表明,当温度和试剂用量一定,反应压强为20 MPa,并且采用先蒸馏水洗涤再乙醇洗涤的后处理方式时,插层效果较好。在此条件下,季铵盐成功插层到蒙脱土片层,间距由1.31 nm增加到1.70 nm,样品中仍然存在一些聚集体结构,但是颗粒粒径减小,颗粒形貌变得蓬松。     

超临界二氧化碳微乳液的研究进展

系统地阐述了超临界二氧化碳微乳液的形成机理和概念,讨论了能形成超临界二氧化碳微乳液的表面活性剂和助表面活性剂的结构设计和选择。介绍了傅立叶红外光谱(FTIR)、电子顺磁共振(EPR)、核磁共振(NMR)、紫外可见光谱(UV-VIS)、X射线小角散射(SAXA)、中子小角散射(SANS)和动态光散射(DLS)等近代测试方法在超临界二氧化碳微乳液结构特性研究中的应用,并对超临界二氧化碳微乳液的研究应用进行了展望。     

Effect of different experimental conditions on biodegradable polylactide membranes prepared with supercritical CO2 as nonsolvent

There is increasing interest in the application of supercritical CO₂ (SCCO₂) in the preparation of polymer membranes. Membrane formation with SCCO₂ as a nonsolvent is analogous to the conventional immersion precipitation process using an organic nonsolvent. Polylactide membranes were prepared with SCCO₂ as the nonsolvent under different experimental conditions such as different polymer concentrations, different depressurization rates, and different nonsolvent compositions. The effects of these conditions on the cross‐sectional structure were investigated through scanning electron microscopy. In addition, solvent‐induced crystallization and CO₂‐induced crystallization were studied. The crystallinity of PLA membranes prepared with different solvents or at different pressures was characterized by wide‐angle X‐ray diffraction and differential scanning calorimetry. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 831–837, 2005     

A dynamic supercritical carbon dioxide foaming method for fabricating wrinkled surface to enhance triboelectric nanogenerator performance

Triboelectric nanogenerator (TENG) is a promising energy harvester to overcome the energy depletion issue. The surface structure has been considered as an effective way to enhance the triboelectric performance. Herein, a dynamic supercritical carbon dioxide (scCO₂) foaming method, which introduced a scCO₂ flow field during scCO₂ saturation, was proposed to fabricate thermoplastic polyurethane (TPU) foams with surface wrinkly structures. The size of the surface wrinkles could be regulated in the range of 1.8–10 μm by varying the foaming pressure. The surface wrinkled TPU film with wrinkle wave length of 2.4 μm demonstrated an excellent enhancement in output voltage (130%), current (180%), and maximum transfer charge (130%) when paired with surface structured polydimethylsiloxane film in a TENG. Due to the excellent durability and flexibility of the composing materials, the developed TENG showed outstanding stability in long-term continuous operation. With a high power density of 0.5 W/m² achieved on a 10⁷ Ω external load, the flexible TENG could be used to charge capacitors, power light-emitting-diodes, and served as a self-powered sensor to detect various human movement behaviors. This work provides a new path for the fabrication of surface wrinkled films for the sustainable development of high performance TENGs.     

The preparation and properties of polystyrene/functionalized graphene nanocomposite foams using supercritical carbon dioxide

In this work, polystyrene (PS)/functionalized graphene nanocomposite foams were prepared using supercritical carbon dioxide. Thermally reduced graphene oxide (TRG) and graphene oxide (GO) were incorporated into the PS. Subsequently, the nanocomposites were foamed with supercritical CO₂. The morphology and properties of the nanocomposites and the nucleation efficiency of functionalized graphene in foaming PS are discussed. Compared with GO, TRG exhibited a higher nucleation efficiency and more effective cell expansion inhibition thanks to its larger surface area and better exfoliated structure. It is suggested that the factors that have a significant influence on the nucleation efficiency of TRG and GO originate from the differences in surface properties and chemical structure. Furthermore, PS/TRG nanocomposites and their nanocomposite foams also possess good electrical properties which enable them to be used as lightweight functional materials.© 2012 Society of Chemical Industry     

Preparation of polystyrene/montmorillonite nanocomposites in supercritical carbon dioxide

The preparation of polystyrene (PS)/montmorillonite (MMT) composites in supercritical carbon dioxide (SC? CO₂) was studied. Lipophilic organically modified MMT can be produced through an ion‐exchange reaction between native hydrophilic MMT and an intercalating agent (alkyl ammonium). PS/clay composites were prepared by free‐radical precipitation polymerization of styrene containing dispersed clay. X‐ray diffraction and transmission electron microscopy indicated that intercalation of MMT was achieved. PS/clay composites have a higher thermal decomposition temperature and lower glass‐transition temperature than pure PS. The IR spectrum analysis showed that the solvent of SC? CO₂ did not change the structures of the PS molecules, but there were some chemical interactions between the PS and the clay in the composites. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 22–28, 2005     

超临界CO2流体中染料溶解度研究进展

综述了超临界CO2流体中染料溶解度的测试装置与方法。分析了超临界CO2流体工艺参数与染料化学结构对分散染料溶解度的影响规律；总结了国内外近二十年的分散染料在超临界CO2流体中溶解度数据，并介绍了分散染料在超临界CO2中的溶解度增溶技术。指出加强染料结构对其溶解性能作用原理及影响规律剖析，超临界CO2中染料溶解行为数据库构建，染料拼色与配色研究三方面为未来的研究重点。     

Physical properties and morphology of polycaprolactone/starch/pine‐leaf composites

Polycaprolactone (PCL)/starch and PCL/starch/pine‐leaf composites, which can be possibly applied as biodegradable food packaging materials with natural pine flavor, were prepared and characterized in this study. The effect of incorporating a silane coupling agent at different content levels on the physical properties and morphology of the composites was studied. To investigate the melting behavior of the composites, a differential scanning calorimetry was employed. A universal testing machine was used to investigate the tensile properties of the composites and the water absorption properties of the composites were also investigated. Scanning electron microscope was used to investigate the morphology of the composites. The physical properties and morphology of the PCL/starch and PCL/starch/pine‐leaf composites were largely affected by the composition, especially the content of the silane coupling agent. The silane coupling agent led to a much better interfacial compatibility between the PCL matrix and the fillers and resulted in better physical properties of the composites. The PCL/starch/pine‐leaf composite with the silane coupling agent showed a morphology, indicating a good interfacial adhesion between the PCL matrix and the fillers. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 928–934, 2007     

聚酯（PET）在超临界二氧化碳中溶胀玻璃化转变温度模型研究

在实验测得高压环境中PET玻璃化转变温度（您）的基础上，将所得实验数据与G—D，CHOW等理论模型计算的％值进行验算比较，发现两种模型均不能很好的描述高压条件下CO2对PET的溶胀行为。     

Investigation on the cell nucleation and cell growth in microcellular foaming by means of temperature quenching

The cell nucleation and real‐time cell growth with increasing cell growth time in microcellular foaming were investigated by means of temperature quenching in a supercritical CO₂ pressure‐quench process. Samples of uniform size and shape were saturated in a vessel under conditions of 100–180°C and 30 MPa, and then depressurized to the atmosphere in 10 s. After depressurization, these samples were removed from the vessel at prescribed intervals, and immediately immersed in an ice‐water slurry to obtain foamed samples with various cell growth times. It was found that the nucleation density is closely correlated to the gas absorption capacity of the polymer matrix, so that the final cell density should not be adopted as the nucleation density, as done commonly. The change of cell structure and mass density with increasing cell growth time was dominated by gas diffusion behavior, which was strongly influenced by the temperature. The final cell structure was mainly determined by the cell growth step, where gas diffusion played a key role. The final cell density was in direct proportion to the gas remaining in the substrate, which ranged from 6.0 × 10⁹ to 4.7 × 10⁶ cells/cm³. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 163–171, 2004