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杨氏模量最大值英语The Yang's modulus, also known as the tangential modulus or the shear modulus, is a measure of the stiffness of a material when subjected to shear stress. It is a fundamental property of materials and plays a crucial role in various engineering applications. The Yang's modulus is defined as the ratio of shear stress to the corresponding shear strain within the proportional limit of a material. In other words, it quantifies how much force is required to deform a material in shear.The Yang's modulus is particularly important in the study of elasticity and plasticity of materials. It characterizes the material's behavior under shear deformation and is essential for designing structures and components that are subject to shear forces. Understanding the Yang's modulus of a material is crucial for predicting how it will deform undervarious loading conditions and for ensuring that it will perform as expected in real-world applications.The Yang's modulus is most commonly used for materials that are subject to torsional or bending loads, such as metals, composite materials, and certain types of polymers. It is an important parameter for designing components such as shafts, beams, and other structural members that must resist shear forces. By knowing the Yang's modulus of a material, engineers can predict how it will deform under these types of loading and design structures that will not fail under normal operating conditions.The Yang's modulus is typically determined through experimental testing, such as shear testing or torsion testing, where the material is subjected to controlled shear stress and the resulting deformation is measured. These tests allow engineers to calculate the Yang's modulus for aspecific material and to understand how it will behave under different loading conditions.In addition to its importance in structural design, the Yang's modulus also plays a crucial role in materialselection and development. Different materials have different Yang's moduli, and selecting the right material for aspecific application requires understanding how it will behave under shear loading. For example, a material with a high Yang's modulus is desirable for applications where stiffness is important, such as in aerospace or automotive components. Conversely, a material with a lower Yang's modulus may be more suitable for applications that require some degree of flexibility, such as in certain types of packaging or consumer products.In the field of materials science and engineering, researchers are constantly striving to develop new materials with improved mechanical properties, including higher Yang'smoduli. This involves understanding the underlying factors that influence a material's shear response and developing new manufacturing methods and material compositions to achieve the desired properties.One example of this is the development of advanced composite materials, which are made by combining different types of fibers with a matrix material. These materials can be engineered to have specific Yang's moduli and other mechanical properties, making them ideal for a wide range of applications. By tailoring the composition and microstructure of these composites, researchers can create materials that exhibit exceptional stiffness and strength under shear loading, opening up new possibilities for lightweight and high-performance structures.In conclusion, the Yang's modulus is a fundamental property of materials that is essential for understanding their behavior under shear loading. It plays a crucial rolein structural design, material selection, and the development of new high-performance materials. By understanding and controlling the Yang's modulus of materials, engineers and researchers can continue to push the boundaries of what is possible in fields ranging from aerospace and automotive engineering to consumer products and beyond.。
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS 2017年第36卷第2期·672·化工进展生物基芳香平台化合物2,5-呋喃二甲酸的合成研究进展王静刚，刘小青，朱锦（中国科学院宁波材料技术与工程研究所，浙江宁波 315201）摘要：生物基芳香平台化合物2,5-呋喃二甲酸（2,5-FDCA）有望替代现有的石油基单体对苯二甲酸用于高性能高分子材料的合成。
如何通过高效、廉价的路线制备2,5-FDCA已经成为近几十年的研究热点。
本文系统地介绍了从5-羟甲基糠醛（HMF）、糠酸、呋喃、二甘醇酸或己糖二酸制备2,5-FDCA的各种方法，并重点介绍了HMF 的直接氧化法、贵金属氧化法、非贵金属氧化法和生物酶氧化法合成2,5-FDCA。
在比较了现有各种路线优缺点的基础上，认为HMF路线是2,5-FDCA规模化制备最有希望的路线，长远发展应朝着以纤维素为起始原料的方向，打通纤维素到糖的关键制备技术。
关键词：2,5-呋喃二甲酸；生物基；平台化合物；合成；进展中图分类号：O63 文献标志码：A 文章编号：1000–6613（2017）02–0672–11DOI：10.16085/j.issn.1000-6613.2017.02.038Research progress on the synthesis of bio-based aromatic platformchemical 2,5-furandicarboxylic acidWANG Jinggang，LIU Xiaoqing，ZHU Jin（Ningbo Institute of Materials Technology and Engineering，Chinese Academy of Sciences，Ningbo 315201，Zhejiang，China）Abstract：2,5-Furandicarboxylic acid（2,5-FDCA） is a promising bio-based aromatic platform chemical for the synthesis of high performance polymers and has been regarded as the most suitable alternative to the petroleum-derived terephthalic acid. The synthesis of 2,5-FDCA through efficient and low cost route has been a hot subject since last decade. In this review article，the popular starting materials，including 5-hydroxymethyl furfural（HMF），furoic acid，furan，diglycolic acid，and hexaric acid，for the fabrication of 2,5-FDCA，are introduced in detail. Perspectives are given based on the comparison of different synthetic routes. The most popular synthetic route is based on HMF by either directly oxidation，noble metal oxidation，non-noble metal oxidation or enzyme catalysis oxidation.This method is considered as the most promising one to achieve large scale preparation of 2,5-FDCA.More importantly，development of novel technology for the conversion of cellulose to glucose is critical to produce large amount of low cost HMF.Key words：2,5-furandicarboxylic acid；bio-based；platform chemical；synthesis；progress当前，随着经济的快速发展和石油储备量的下降，人们已经越来越重视可再生资源的开发和利用[1-4]。
全球材料类S C I收录期刊影响因子排名投稿必备Standardization of sany group #QS8QHH-HHGX8Q8-GNHHJ8-HHMHGN#全球材料类SCI收录期刊影响因子排名期刊英文名中文名影响因子Nature自然Science科学Nature Material自然（材料）Nature Nanotechnology自然（纳米技术）Progress in Materials Science材料科学进展Nature Physics自然（物理）Progress in Polymer Science聚合物科学进展Surface Science Reports表面科学报告Materials Science & Engineering R-reports材料科学与工程报告Angewandte Chemie-International Edition应用化学国际版Nano Letters纳米快报Advanced Materials先进材料Journal of the American Chemical Society美国化学会志Annual Review of Materials Research材料研究年度评论Physical Review Letters物理评论快报Advanced Functional Materials先进功能材料Advances in Polymer Science聚合物科学发展Biomaterials生物材料Small微观？Progress in Surface Science表面科学进展Chemical Communications化学通信MRS Bulletin材料研究学会（美国）公告Chemistry of Materials材料化学Advances in Catalysis先进催化Journal of Materials Chemistry材料化学杂志Carbon碳Crystal Growth & Design晶体生长与设计Electrochemistry Communications电化学通讯The Journal of Physical Chemistry B物理化学杂志，B辑：材料、表面、界面与生物物理Inorganic Chemistry有机化学Langmuir朗缪尔Physical Chemistry Chemical Physics物理化学International Journal of Plasticity塑性国际杂志Acta Materialia材料学报Applied Physics Letters应用物理快报Journal of power sources电源技术Journal of the Mechanics and Physics of Solids固体力学与固体物理学杂志International Materials Reviews国际材料评论Nanotechnology纳米技术Journal of Applied Crystallography应用结晶学Microscopy and MicroanalysisCurrent Opinion in Solid State & Materials Science固态和材料科学的动态Scripta Materialia材料快报The Journal of Physical Chemistry A物理化学杂志，A辑Biometals生物金属Ultramicroscopy超显微术Microporous and Mesoporous Materials多孔和类孔材料Composites Science and Technology复合材料科学与技术Current Nanoscience当代纳米科学Journal of the Electrochemical Society电化学界Solid State Ionics固体离子IEEE Journal of Quantum ElectronicsIEEE量子电子学杂志Mechanics of Materials材料力学Journal of nanoparticle research纳米颗粒研究CORROSION SCIENCE腐蚀科学Journal of Applied Physics应用物理杂志Journal of Biomaterials Science-Polymer Edition生物材料科学—聚合物版IEEE Transactions on NanotechnologyIEEE 纳米学报Progress in Crystal Growth and Characterization of Materials晶体生长和材料表征进展Journal of Physics D-Applied Physics物理杂志D——应用物理Journal of the American Ceramic Society美国陶瓷学会杂志Diamond and Related Materials金刚石及相关材料Journal of Chemical & Engineering Data化学和工程资料杂志Intermetallics金属间化合物Electrochemical and Solid State Letters固体电化学快报Synthetic Metals合成金属Composites Part A-Applied Science and Manufacturing复合材料 A应用科学与制备Journal of Nanoscience and Nanotechnology纳米科学和纳米技术Journal of Solid State Chemistry固体化学Journal of Physics: Condensed Matter物理学学报：凝聚态物质Urnal of Bioactive and Compatible Polymer生物活性与兼容性聚合物杂志International Journal of Heat and Mass Transfer传热与传质Applied Physics A-Materials Science & Processing应用物理A－材料科学和进展Thin Solid Films固体薄膜Surface & Coatings Technology表面与涂层技术Materials Science & Engineering C-Biomimetic and Supramolecular Systems材料科学与工程C—仿生与超分子系统Materials Research Bulletin材料研究公告International Journal of Solids and Structures固体与结构Materials Science and Engineering A-Structural Materials Properties Microst材料科学和工程A—结构材料的性能、组织与加工Materials Chemistry and Physics材料化学与物理Powder Technology粉末技术Materials Letters材料快报Journal of Materials Research材料研究杂志Smart Materials & Structures智能材料与结构Solid State Sciences固体科学Polymer Testing聚合物测试Nanoscale Research Letters纳米研究快报Surface Science表面科学Optical Materials光学材料International Journal of Thermal Sciences热科学Thermochimica Acta热化学学报Journal of Biomaterials Applications生物材料应用杂志Journal of Thermal Analysis andJournal of Solid State Electrochemistry固体电化学杂志Journal of the European Ceramic Society欧洲陶瓷学会杂志Materials Science and Engineering B-Solid State Materials for Advanced Tech材料科学与工程B—先进技术用固体材料Applied Surface Science应用表面科学European Physical Journal B欧洲物理杂志Solid State Communications固体物理通信International Journal of Fatigue疲劳国际杂志Computational Materials Science计算材料科学Cement and Concrete Research水泥与混凝土研究Philosophical Magazine Letters哲学杂志（包括材料）Current Applied Physics当代应用物理Journal of Alloys and Compounds合金和化合物杂志Wear磨损Journal of Materials Science-Materials in Medicine材料科学杂志—医用材料Advanced Engineering Materials先进工程材料Journal of Nuclear Materials核材料杂志International Journal of Applied Ceramic Technology应用陶瓷技术Chemical Vapor Deposition化学气相沉积COMPOSITES PART B-ENGINEERING复合材料B工程Composite Structures复合材料结构Journal of Non-crystalline Solids非晶固体杂志Journal of Vacuum Science & Technology B真空科学与技术杂志Semiconductor Science and Technology半导体科学与技术Journal of SOL-GEL Science and TEchnology溶胶凝胶科学与技术杂志Science and Technology of Welding and Joining焊接科学与技术Metallurgical and Materials Transactions A-Physical Metallurgy and Material冶金与材料会刊A——物理冶金和材料Modelling and Simulation in Materials Science and Engineering材料科学与工程中的建模与模拟Philosophical Magazine A-Physics of Condensed Matter Structure Defects and Mechanical Properties哲学杂志A凝聚态物质结构缺陷和机械性能物理Philosophical Magazine哲学杂志Ceamics International国际陶瓷Oxidation of Metals材料氧化Modern Physics Letters A现代物理快报Cement & Concrete Composites水泥与混凝土复合材料Journal of Intelligent Material Systems and Structures智能材料系统与结构Journal of Magnetism and Magnetic Materials磁学与磁性材料杂志Journal of Electronic Materials电子材料杂志Surface and Interface Analysis表面与界面分析Science and Technology of AdvancedJournal of Computational and Theoretical Nanoscience计算与理论纳米科学IEEE TRANSACTIONS ON ADVANCED PACKAGINGIEEE高级封装会刊Materials Characterization材料表征International Journal of Refractory Metals & Hard Materials耐火金属和硬质材料国际杂志Physica Status solidi A-Applied Research固态物理A——应用研究PHASE TRANSITIONS相变Journal of Thermal Spray Technology热喷涂技术杂志International Journal of Nanotechnology纳米工程Journal of Materials Science材料科学杂志Journal of Vacuum Science & Technology A-VACUUM Surfaces and Films真空科学与技术A真空表面和薄膜PHYSICA STATUS SOLIDI B-BASIC RESEARCH固态物理B—基础研究MATERIALS SCIENCE IN SEMICONDUCTOR PROCESSING半导体加工的材料科学International Journal of Fracture断裂学报Journal of Materials Processing Technology材料加工技术杂志Metals and Materials International国际金属及材料IEEE TRANSACTIONS ON MAGNETICSIEEE磁学会刊Vacuum真空Journal of Applied Electrochemistry应用电化学Materials & Design材料与设计JOURNAL OF PHYSICS AND CHEMISTRY OF SOLIDS固体物理与化学杂志Journal of Experimental Nanoscience实验纳米科学POLYMER COMPOSITES聚合物复合材料Journal of Materials Science-Materials in Electronics材料科学杂志—电子材料Journal of Composite Materials复合材料杂志Journal of the Ceramic Society of Japan日本陶瓷学会杂志JOURNAL OF ELECTROCERAMICS电子陶瓷杂志ADVANCES IN POLYMER TECHNOLOGY聚合物技术发展IEEE TRANSACTIONS ON COMPONENTS AND PACKAGING TECHNOLOGIESIEEE元件及封装技术会刊Journal of Porous Materials多孔材料IEEE TRANSACTIONS ON SEMICONDUCTOR MANUFACTURINGIEEE半导体制造会刊CONSTRUCTION AND BUILDING MATERIALS结构与建筑材料Journal of Engineering Materials and Technology-Transactions of The ASME工程材料与技术杂志—美国机械工程师学会会刊FATIGUE & FRACTURE OF ENGINEERING MATERIALS & STRUCTURES工程材料与结构的疲劳与断裂IEEE TRANSACTIONS ON APPLIED SUPERCONDUCTIVITYIEEE应用超导性会刊ACI STRUCTURAL JOURNAL美国混凝土学会结构杂志Materials Science and Technology材料科学与技术Materials and Structures材料与结构Reviews on Advanced Materials Science先进材料科学评论International Journal of Thermophysics热物理学国际杂志JOURNAL OF ADHESION SCIENCE AND TECHNOLOGY粘着科学与技术杂志Journal of Materials Science & Technology材料科学与技术杂志High Performance Polymers高性能聚合物BULLETIN OF MATERIALS SCIENCE材料科学公告Mechanics of Advanced Materials and Structures先进材料结构和力学PHYSICA B物理EUROPEAN PHYSICAL JOURNAL-APPLIED PHYSICS欧洲物理杂志—应用物理CORROSION腐蚀International Journal of Materials Research材料研究杂志JOURNAL OF NONDESTRUCTIVE EVALUATION无损检测杂志METALLURGICAL AND MATERIALS TRANSACTIONS B-PROCESS METALLURGY ANDMATERIALS冶金和材料会刊B—制备冶金和材料制备科学Materials Transactions材料会刊Aerospace Science and Technology航空科学技术Journal of Energetic Materials金属学杂志Advanced Powder Technology先进粉末技术Applied Composite Materials应用复合材料Advances in Applied Ceramics先进应用陶瓷Materials and Manufacturing Processes材料与制造工艺Composite Interfaces复合材料界面JOURNAL OF ADHESION粘着杂志INTERNATIONAL JOURNAL OF THEORETICAL PHYSICS理论物理国际杂志JOURNAL OF NEW MATERIALS FOR ELECTROCHEMICAL SYSTEMS电化学系统新材料杂志Journal of Thermophysics and Heat Transfer热物理与热传递Materials and Corrosion-Werkstoffe Und Korrosion材料与腐蚀RESEARCH IN NONDESTRUCTIVE EVALUATION无损检测研究JOURNAL OF COMPUTER-AIDED MATERIALS DESIGN计算机辅助材料设计杂志JOURNAL OF REINFORCED PLASTICS AND COMPOSITES增强塑料和复合材料杂志ACI MATERIALS JOURNAL美国混凝土学会材料杂志SEMICONDUCTORS半导体FERROELECTRICS铁电材料INTERNATIONAL JOURNAL OF MODERN PHYSICS B现代物理国际杂志MATERIALS RESEARCH INNOVATIONS材料研究创新GLASS TECHNOLOGY -PART A玻璃技术JOURNAL OF MATERIALS IN CIVIL ENGINEERING土木工程材料杂志NEW DIAMOND AND FRONTIER CARBON TECHNOLOGY新型金刚石和前沿碳技术SCIENCE IN CHINA SERIES E-TECHNOLOGICAL SCIENCES中国科学E技术科学ATOMIZATION AND SPRAYS雾化和喷涂SYNTHESE合成HIGH TEMPERATURE高温Journal of Phase Equilibria and Diffusion相平衡与扩散INORGANIC MATERIALS无机材料MECHANICS OF COMPOSITE MATERIALS复合材料力学BIO-MEDICAL MATERIALS AND ENGINEERING生物医用材料与工程PHYSICS AND CHEMISTRY OF GLASSES玻璃物理与化学JOURNAL OF WUHAN UNIVERSITY OF TECHNOLOGY-MATERIALS SCIENCE EDITION 武汉理工大学学报-材料科学版ADVANCED COMPOSITE MATERIALS先进复合材料Journal of Materials Engineering and Performance材料工程与性能杂志Solid State Technology固体物理技术FERROELECTRICS LETTERS SECTION铁电材料快报JOURNAL OF POLYMER MATERIALS聚合物材料杂志JOURNAL OF INORGANIC MATERIALS无机材料杂志GLASS SCIENCE AND TECHNOLOGY-GLASTECHNISCHE BERICHTE玻璃科学与技术POLYMERS & POLYMER COMPOSITES聚合物与聚合物复合材料Surface Engineering表面工程RARE METALS稀有金属HIGH TEMPERATURE MATERIAL PROCESSES高温材料加工JOURNAL OF TESTING AND EVALUATION测试及评价杂志AMERICAN CERAMIC SOCIETY BULLETIN美国陶瓷学会公告MATERIALS AT HIGH TEMPERATURES高温材料MAGAZINE OF CONCRETE RESEARCH混凝土研究杂志SURFACE REVIEW AND LETTERS表面评论与快报Journal of Ceramic Processing Research陶瓷处理研究JSME INTERNATIONAL JOURNAL SERIES A-SOLID MECHANICS AND MATERIAL ENGINEERIN日本机械工程学会国际杂志系列A－固体力学与材料工程MATERIALS TECHNOLOGY材料技术ADVANCED COMPOSITES LETTERS先进复合材料快报HIGH TEMPERATURE MATERIALS AND PROCESSES高温材料和加工INTEGRATED FERROELECTRICS集成铁电材料MATERIALS SCIENCE材料科学MATERIALS EVALUATION材料评价POWDER METALLURGY AND METAL CERAMICS粉末冶金及金属陶瓷RARE METAL MATERIALS AND ENGINEERING稀有金属材料与工程INTERNATIONAL JOURNAL OF MATERIALS & PRODUCT TECHNOLOGY材料与生产技术国际杂志METAL SCIENCE AND HEAT TREATMENT金属科学及热处理JOURNAL OF ADVANCED MATERIALS先进材料杂志ADVANCED MATERIALS & PROCESSES先进材料及工艺MATERIALS WORLD材料世界SCIENCE AND ENGINEERING OF COMPOSITE MATERIALS复合材料科学与工程MATERIALS PERFORMANCE材料性能。
无机非金属材料一级学科二级学科1.无机非金属材料包括陶瓷材料和高分子材料。
Inorganic non-metallic materials include ceramics and polymers.2.陶瓷材料是一种具有高硬度和高耐热性的材料。
Ceramic materials are materials with high hardness and high heat resistance.3.高分子材料是由许多重复单元组成的大分子化合物。
Polymer materials are large molecular compounds composed of many repeated units.4.无机非金属材料学科涉及材料的合成、性能和应用。
The discipline of inorganic non-metallic materials involves the synthesis, properties, and applications of materials.5.该学科与化学、材料科学和工程学等领域紧密相关。
This discipline is closely related to fields such as chemistry, materials science, and engineering.6.研究无机非金属材料的二级学科包括陶瓷工程、高分子工程等。
Secondary disciplines that study inorganic non-metallic materials include ceramic engineering, polymer engineering, and so on.7.陶瓷工程主要研究陶瓷材料的制备及应用。
Ceramic engineering mainly studies the preparation and application of ceramic materials.8.高分子工程研究涉及塑料、橡胶和纤维等高分子材料的开发。
双马来酰亚胺树脂固化技术及反应机理研究进展任荣;熊需海;刘思扬;陈平【摘要】双马来酰亚胺树脂是一种高性能热固性树脂，在尖端技术领域有着广泛的应用。
本文综述了双马来酰亚胺树脂（ BMI）在热、微波辐射、电子束辐射和紫外光等作用下固化成型技术及固化机理等方面的研究进展。
%Bismaleimide is a class of high-performance thermosetting resin and widely applied in high-tech fields.This paper discusses the progress in curing technology and reaction mechanism of bismaleimide resin under the conditions of thermal activation,microwave radiation,electron beam and UV-irradiation.【期刊名称】《纤维复合材料》【年(卷),期】2014(000)002【总页数】5页(P10-14)【关键词】双马来酰亚胺( BMI);固化成型技术;固化机理【作者】任荣;熊需海;刘思扬;陈平【作者单位】沈阳航空航天大学航空航天工程学院辽宁省高性能聚合物基复合材料重点实验室，沈阳110136;沈阳航空航天大学航空航天工程学院辽宁省高性能聚合物基复合材料重点实验室，沈阳110136;沈阳航空航天大学航空航天工程学院辽宁省高性能聚合物基复合材料重点实验室，沈阳110136;沈阳航空航天大学航空航天工程学院辽宁省高性能聚合物基复合材料重点实验室，沈阳110136; 大连理工大学化工学院精细化工国家重点实验室，辽宁大连116024【正文语种】中文双马来酰亚胺树脂(下称双马或BMI)是一种典型的耐热型热固性树脂。
其优越性能如加工性能、粘结性、电绝缘性、耐疲劳性、高强度以及耐湿热能力使之作为基体树脂或粘胶剂广泛应用于先进复合材料领域、多层印刷电路板以及电绝缘器件等电子电器行业[1]。
全球SCI收录材料期刊影响因子排名Nature自然31。
434Science科学28。
103Nature Material自然（材料）23。
132Nature Nanotechnology自然（纳米技术）20。
571Progress in Materials Science材料科学进展18。
132Nature Physics自然（物理）16.821Progress in Polymer Science聚合物科学进展16.819Surface Science Reports表面科学报告12。
808Materials Science & Engineering R—reports材料科学与工程报告12。
619 Angewandte Chemie—International Edition应用化学国际版10.879Nano Letters纳米快报10。
371Advanced Materials先进材料8。
191Journal of the American Chemical Society美国化学会志8.091Annual Review of Materials Research材料研究年度评论7。
947Physical Review Letters物理评论快报7。
180Advanced Functional Materials先进功能材料6.808Advances in Polymer Science聚合物科学发展6。
802Biomaterials生物材料6.646Small微观？6.525Progress in Surface Science表面科学进展5。
429Chemical Communications化学通信5。
34MRS Bulletin材料研究学会（美国）公告5.290Chemistry of Materials材料化学5。
046Advances in Catalysis先进催化4.812Journal of Materials Chemistry材料化学杂志4。
化工进展Chemical Industry and Engineering Progress2024 年第 43 卷第 3 期水驱油藏聚乙烯亚胺交联聚合物凝胶体系研究进展王凯1，罗明良1，李明忠1，黄飞飞2，蒲春生1，蒲景阳3，樊乔1（1 中国石油大学（华东）石油工程学院，山东 青岛 266580；2 延安大学石油工程与环境工程学院，陕西 延安716000；3 中国石油大学（北京）碳中和示范性能源学院，北京 102249）摘要：聚乙烯亚胺（PEI ）是一种低毒性环保材料，它与聚合物交联的凝胶体系具有适用温度范围广、成胶时间可控、成胶后强度大、高温稳定时间长、几乎不受储层岩石矿物影响等优点。
本文回顾了以PEI 作为交联剂的各类凝胶体系的研究动态，阐明了PEI 与各类聚合物的交联反应机理及其凝胶体系特点，分析了各类因素对凝胶性能的影响，并列举了改善凝胶性能的方法和成功的矿场应用实例，重点分析了提高凝胶体系交联活性的方法研究。
最后，提出聚丙烯酰胺（PAM ）/PEI 凝胶体系作为环保型调驱体系在中低温油藏深部调控方面具有非常大的应用前景，应继续深入研究提高PAM/PEI 凝胶体系交联效率的方法及其作用机理，以降低聚合物与交联剂用量，为这一体系的推广应用提供理论依据与实验基础。
关键词：聚合物；凝胶；聚乙烯亚胺；交联剂；黏度；调剖堵水中图分类号：TE39 文献标志码：A 文章编号：1000-6613（2024）03-1506-18Research progress of polyethyleneimine crosslinked polymer gel systemin water-drive reservoirsWANG Kai 1，LUO Mingliang 1，LI Mingzhong 1，HUANG Feifei 2，PU Chunsheng 1，PU Jingyang 3，FAN Qiao 1(1 College of Petroleum Engineering, China University of Petroleum (East China), Qingdao 266580, Shandong, China;2School of Petroleum Engineering and Environmental Engineering, Yan ’an University, Yan ’an 716000, Shaanxi, China;3College of Carbon Neutral Energy, China University of Petroleum (Beijing), Beijing 102249, China)Abstract: Polyethyleneimine (PEI) is an environment-friendly and low toxic material. PEI and polymer crosslinked gel system has the advantages of controllable gelation time, high strength of mature gel, high-temperature resistance, long-time stability, and almost unaffected by minerals of reservoir. This paper reviewed the research of various polymer gel systems with PEI as crosslinker. The crosslinking mechanism and the characteristics of those gel systems were clarified. The influence of various factors on the gel system was analyzed. And, the methods to improve the gel performance and successful filed trial were listed, the methods to improve the crosslinking activity of gel system were emphatically analyzed. Finally, it was pointed out that polyacrylamide(PAM)/PEI gel system, as an environment-friendly system, had great application prospects in conformance control and water shutoff of medium and low temperature reservoirs, and it was suggested that the method and the corresponding mechanism of improving theDOI ：10.16085/j.issn.1000-6613.2023-0376收稿日期：2023-03-13；修改稿日期：2023-04-12。
Original ArticleSynthesis and properties of a novelhigh-temperature diphenylsulfone-based phthalonitrile polymerXuegang Peng1,Haitong Sheng1,Hui Guo1,Kimiyoshi Naito2,Xiaoyan Yu1,Huili Ding1,Xiongwei Qu1and Qingxin Zhang1AbstractA novel high-temperature diphenyl sulfone-based phthalonitrile polymer is prepared from bis-[4-(3,4-dicyanophenoxy)-phenyl]sulfone(BDS)monomer synthesized with high yield by a simple nucleophilic displacement of a nitro-substituent from4-nitrophthalonitrile(NPN).The structure of BDS polymer is investigated by Fourier transform infrared spectro-scopy and wide-angle X-ray diffraction.Curing behavior of BDS monomer with1,3-bis(4-aminophenoxy)benzene(APB) is recorded by differential scanning calorimetry.The properties of BDS polymer are evaluated by thermogravimetric anal-ysis,dynamic mechanical analysis,and tensile test.The results reveal that the BDS polymer exhibits excellent thermal and thermo-oxidative stabilities,high glass temperature(T g¼337 C),and outstanding mechanical properties(Young’s mod-ulus:4.02GPa and tensile strength:64.16MPa).Additionally,the BDS polymer exhibits high flame retardance and low water uptake.KeywordsPhthalonitrile polymer,high glass transition temperature,thermal stability,mechanical propertyIntroductionPhthalonitrile polymers,as a new family of high-temperature and high-performance polymers proposed by Keller and Griffith,1have drawn great attention for their superior ther-mal and thermo-oxidative stabilities and various other prop-erties.The interest in high-performance polymers versus metallic materials arises from the need for a reduction in weight and an enhancement in performance.2For advanced composites,the upper limit application temperature is largely determined by the glass transition temperature(T g) and the thermal decomposition temperature of the polymer matrix;thus the polymer matrix plays a vital role to achieve the best performance.The key to the development of high-temperature poly-mers is the incorporation of thermally stable structural units such as aromatic or heteroaromatic rings within the back-bone of a polymeric system,2and heterocyclic polymers have been proved to possess high thermal stability.3–7 Nowadays,aromatic polyimides are mainly used in high-temperature materials because of their high thermal stability and excellent mechanical properties.8–10How-ever,volatile by-products,such as water,inevitably yield during imidization reaction leading to the formation of void-filled fabricated components thereby consequently affecting their mechanical pared with aro-matic polyimides,the addition cure mechanism of phtha-lonitrile polymers ensures that little or no volatiles are evolved during the polymerization producing highly cross-linked,void-free network polymers with the desired structure and properties.Thermosetting phthalonitrile polymers are a unique class of high-temperature materials having a number of excellent properties such as high T g s, outstanding thermal and thermo-oxidative stabilities, excellent mechanical properties,good moisture resis-tance,and superior fire resistance.2,11–18It is reported that 1Institute of Polymer Science and Engineering,School of Chemical Engineering and Technology,Hebei University of Technology,Tianjin, China2Hybrid Materials Center,National Institute for Materials Science, Tsukuba,JapanCorresponding author:Xiaoyan Yu,Institute of Polymer Science and Engineering,School of Chemical Engineering and Technology,Hebei University of Technology, Tianjin300130,China.Email:yuxycnn@High Performance Polymers2014,Vol.26(7)837–845ªThe Author(s)2014Reprints and permission:/journalsPermissions.navDOI:10.1177/0954008314532479phthalonitrile polymer-based composites meet the Navy specification(MIL-STD-2031)for their usage as a poly-meric composite in the interior of a submarine.19–21 In this article,a rigid,thermotolerant and oxidation-resistant diphenyl sulfone unit was introduced into the molecular skeleton of phthalonitrile polymers in order to further improve the mechanical properties and thermal and thermo-oxidative stabilities.The diphenyl sulfone-based phthalonitrile polymer exhibits superior thermal stability, outstanding mechanical properties,high T g,and excellent flame-retardant property,and thus it is a qualified candi-date for applications in the field of heat-resistant and high-performance materials.Experimental sectionMaterials4-Nitrophthalonitrile(NPN;98.0%),bis-(4-hydroxyphe-nyl)sulfone(BHPS;þ98.0%),and1,3-bis-(4-aminophe-noxy)benzene(APB;þ97.0%)were supplied by Wako Chemical Industries(Japan).Pulverized anhydrous potas-sium carbonate(99%)and dehydrated dimethyl sulfoxide (DMSO)were provided by Alfa Aesar(Ward hill,Massa-chusetts,USA)and Wako,respectively.All the chemicals were used without any pretreatment.Synthesis of BDS monomerTo a500-mL three-necked flask was added BHPS(37.51g, 0.15mol),NPN(51.92g,0.30mol),pulverized anhydrous potassium carbonate(62.10g,0.45mol),and200mL of dry DMSO.Then,the mixture was kept at80–90 C for5h under nitrogen(N2)atmosphere with continuous stirring.After cooling,the product mixture was slowly poured into hydrochloric acid solution(600mL,2M) and brown bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone (BDS)monomer deposited consequently.The BDS mono-mer was collected by suction filtration and washed with plenty of distilled water until the filtrate became neutral. The filtered BDS cake was dried at80 C for24h with a yield of64.76g(86%).Preparation of BDS prepolymer and polymerBDS prepolymer was synthesized in a500-mL reaction ket-tle equipped with a mechanical stirrer.First,BDS monomer (30.00g,0.0597mol)was melted followed by the addition of APB(1.02g,0.0035mol)with continuous stirring at 250 C for5min,and then the BDS prepolymer was formed with a black block.The prepolymer was pulverized and fur-ther cured,namely,postcured,in an autoclave under0.70 MPa pressure with a high degree of vacuum(À0.10MPa) by a heating procedure:200 C for4h,260 C for4h,315 C for4h,and343 C for4h.The prepared BDS polymer was machined into rectangular specimens(55.00Â10.00Â2.00 mm3)for dynamic mechanical analysis(DMA)experiments. CharacterizationThe proton nuclear magnetic resonance(1H NMR)spec-trum of BDS monomer was recorded on a Bruker300MHz NMR spectrometer(Germany)with deuterated chloroform (CDCl3)as the solvent and tetramethylsilane as the internal reference.Elemental analysis for C,H,N,and S were car-ried out on a Thermo Flash EA1112analyzer(Thermo Fisher Scientific,Waltham,Massachusetts,USA).Fourier transform infrared(FTIR)spectra were recorded using a Nicolet Nexus670FTIR spectrometer(Madison,Wisconsin, USA)in potassium bromide mode for BDS monomer and attenuated total reflectance mode for BDS prepolymer and polymer.Wide-angle X-ray diffraction(WAXD)was con-ducted with a Rigaku diffractometer(model RINT2500; Rigaku Co.,Tokyo,Japan)operating at40kV and300mA with nickel-filtered copper K a radiation(l¼0.15406 nm)in reflection mode.The2y scan data were collected from2 to60 with an interval of0.02 at a scanning speed of4 minÀ1.Thermogram of the BDS monomer with APB was recorded using a TA Q10differential scanning calori-meter(New Castle,Delaware,USA)at a heating rate of 10 C minÀ1.Scanning electron microscopy(SEM)images were acquired using a JEOL6500field emission scanning electron microscope(Tokyo,Japan).The specimen was coated with gold prior to observation.Thermogravimetric analysis(TGA)was performed on solid samples and pow-der samples using a TA Q50instrument at a heating rate of 20 C minÀ1under N2and in air atmospheres,respectively. The T d,5%and T d,max are defined as the temperatures at which5%weight loss occurs and the peak of the deriva-tive thermogravimetric analysis curve,respectively. Tensile tests were performed according to ASTM D-638 standard using a universal testing machine(Table top-type tester EZ-Test;Shimadzu,Tokyo,Japan)with a crosshead speed of1mm minÀ1.The rectangular speci-men was stored in a test tube filled with distilled water for more than2months at room temperature,dried with paper towel,and weighed using a balance to determine the water uptake.DMA was performed on a2980dynamic mechanical analyzer(TA Instruments)in dual cantilever mode at a frequency of1Hz and an amplitude of10m m over the temperature range of50–450 C with a heating rate of5 C minÀ1.Results and discussionSynthesisIt is reported that a class of phthalonitrile monomers were prepared by a simple nucleophilic displacement of a nitro substituent.1In our research,the diphenyl sulfone-based838High Performance Polymers26(7)phthalonitrile monomer,BDS,was synthesized with high yield by the nucleophilic displacement of a labile nitro sub-stituent from NPN.The typical procedure of synthesis of BDS monomer,prepolymer,and polymer is illustrated in Figure 1.The BDS polymer was prepared via two steps.The first is the preparation of BDS prepolymer by addition of amine into BDS monomer melt at 250 C,while the second step is the conversion of prepolymer into highlycross-linked BDS polymer by postcuring at elevated temperatures.FTIR spectroscopy was employed to characterize the BDS monomer,and the overlaid FTIR spectra of BHPS and BDS monomers are shown in Figure 2.The absorption peak at 3365cm À1of BHPS is due to the stretching vibration of phenolic hydroxyl (Ar–OH),while BDS monomer shows no absorption signal around 3365cm À1indicating that nucleophilic displacement reaction has taken place and all the –OH groups have been replaced by NPN.Aromatic C–H bending absorptions appear at 3097and 3043cm À1,and the out-of-plane bending absorptions are observed at 900–700cm À1.A strong absorption peak appears around 2237cm À1corresponding to the characteristic stretching of nitrile groups (–CN)of BDS.The absorption bands within 1600–1400cm À1could be attributed to the stretching of phe-nyl rings.It is noticed that a strong absorption peak centered at 1251cm À1appears,which is ascribed to the stretching of C–O of BDS,and absorption range within 1300–1100cm À1should be assigned to sulfone group (–SO 2–)stretching.While FTIR spectra provide information about charac-teristic groups of molecules to further confirm the structure of BDS monomer,NMR spectroscopy is employed and 1H NMR spectrum of the BDS monomer is presented in Figure 3.All signals have been assigned to protons as follows:1H NMR (300MHz,CDCl 3,d ):8.06(d,J ¼8.6Hz,4H,H1),7.80(d,J ¼8.4Hz,2H,H4),7.35(d,2J ¼2.4Hz,2H,H5),7.32(dd,1J ¼8.3Hz,2J ¼2.4Hz,2H,H3),and 7.21(d,J ¼8.6Hz,4H,H2).Moreover,the signal integrations sup-port the formulation.Calculated values for BDS monomer (C 28H 14N 4SO 4):C,66.93;H, 2.79;N,11.16;S, 6.37.Found:C,66.68;H,2.71;N,11.03;S,6.19.Elemental analysis and 1H NMR results are consistent with the FTIR spectroscopy analysis proving that the BDS monomer was successfully synthesized.The WAXD spectrum of BDS monomer is presented in Figure 4.The cell parameters of the monomer were deter-mined by a trial and error method,and the result was further refined by a least squares procedure.The experimental and calculated cell parameters are listed in Table 1,and theunitFigure 1.Synthesis of BDS monomer,prepolymer,and polymer.BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Figure 2.FTIR spectra of BHPS and BDS monomer.FTIR:Fourier transform infrared spectroscopy;BHPS:bis-(4-hydroxyphenyl)sul-fone;BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Figure 3.1H NMR spectrum of BDS monomer.1H NMR:proton nuclear magnetic resonance;BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Peng et al.839cell was determined to be orthorhombic with unit cell dimen-sions:a ¼26.1289A˚,b ¼12.3071A ˚,and c ¼4.1142A ˚,with a volume of 1323.01A˚3.Microstructure of BDS polymerThe differential scanning calorimetry (DSC)scan of theBDS monomer with ABP (5.8mol %)is shown in Figure 5.To obtain a homogeneous mixture,BDS monomer and ABP were thoroughly mixed by stirring prior to DSC tests.As observed,APB gives a small endothermic melting peak at 114.9 C,while the synthesized BDS monomer shows a sharp melting peak at 221.6 C indicating the high purity of BDS monomer.An exotherm peak at 259.5 C after the melting peak of BDS monomer is attributed to the reaction of the diamine with BDS,which manifests that the process-ing window is nearly 38 C as defined by the temperature difference between the melting point of the monomer and the exothermic curing temperature.17WAXD spectra of the BDS prepolymer and polymer are presented in Figure 6.The BDS prepolymer exhibits no sharp diffraction peak in addition to a noncrystalline diffraction hump centered at 20.1 ,implying that the BDS monomers have been con-verted into prepolymer indicated by the complete disap-pearance of the diffraction peaks of monomers.Similarly,the BDS polymer shows a noncrystalline diffraction at 20.7 .This noncrystalline hump indicates the frequent occurrence of a particular interatomic distance (R )of a polymer in a largely disordered substance and could be determined by the following expression:22R ¼54Âl 2sin y¼1:25d Bragg ð1Þwhere l is the wavelength of X-ray and 2y is the diffraction angle.This equation means that the interatomic distance (R )responsible for a strong maximum in the diffractionpattern at angle y is equal to 1.25times the d -spacing cal-culated with the aid of the well-known Bragg’s equation.This equation was used to assess the most intense diffrac-tion for noncrystalline materials.As a result,the intera-tomic distance was determined to be 0.536nm for the BDS polymer.FTIR spectra of the BDS prepolymer and polymer are given in Figure 7.As observed,FTIR spectrum of BDS prepolymer shows medium absorption bands within 1600–1100cm À1because of the formation of BDS oligo-mer in the first stage.However,the characteristic peak of nitrile groups at 2230cm À1becomes weak in the prepoly-mer compared with that of BDS monomer,and it is much weaker in the BDS polymer,indicating that most of the nitrile groups have been polymerized during postcuring process.It has been reported that phthalonitrile monomers might polymerize into polytriazine structures and polyisoindole structures.13,23,24A new absorption of BDS polymer at 1358cm À1is attributed to the formation of triazine rings,indicating that polytriazine structure might generate during polymerization.13In addition,there is still a weak absorp-tion of –CN groups at 2230cm À1for BDS polymer because only half of the –CN groups participate in polytriazine ring structures due to high steric hindrance.On the other hand,the FTIR spectroscopy of the BDS polymer exhibits other two new absorptions at 1720cm À1(–C ¼N–)and 1528cm À1(pyrrole ring)implying that the polyisoindole struc-ture might form in the BDS polymer.23,24Based on the above analysis,it is reasonable to conclude that both the polyisoindole structure and the polytriazine structure coex-ist in BDS polymer as illustrated in Figure 8.Polyimides,as one of the most important high-temperature and high-performance polymer families,have been mainly used for high-tech applications where void-free property is particularly important.However,polyi-mides are extremely tedious to process and liberate volatile by-products such as water during the imidizing polymeriza-tion reaction leading to void-filled fabricated components.Although various methods have been tried to solve the void problems,microvoids have been a critical issue for broad high-temperature applications.SEM photographs of frac-ture surfaces of the BDS polymer are shown in Figure 9.As seen,no voids can be observed for the BDS polymer at low (1,000Â)and high (10,000Â)magnifications due to the absence of solvents and the addition polymerization mechanism of BDS monomer,which proves the void-free structure of BDS polymer,and it also guarantees the out-standing thermal and mechanical properties.Thermal and thermo-oxidative stabilitiesThe thermal and thermo-oxidative properties of BDS poly-mer were investigated between 25and 1000 C by TGA under N 2and in air atmospheres,respectively,asshownFigure 4.WAXD of BDS monomer.WAXD:wide-angle X-ray diffraction;BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.840High Performance Polymers 26(7)in Figure 10,and the thermal parameters are listed in Table 2.As observed,the weight of BDS polymer in N 2exhibits only 5%loss with temperature growing up to 418 C (solid sample)and 436 C (powder sample),and it shows a rapid decrease upon further heating and reaches a maximum rate at T d,max of 476 C (solid sample)and 493 C (powder sam-ple),which indicates high thermal stabilities of BDS poly-mer.The BDS polymer retains 59wt %(solid sample)and 57wt %(powder sample)at 1000 C.While the T d,5%of BDS polymer solid sample appears at 450 C in air,and maximum decomposition takes place at three temperature ranges of 486,655,and 725 C,respectively.Analogously,the T d,5%of BDS polymer powder sample appears at 441 C in air,and maximum decomposition takes place at three temperature ranges of 492,658,and 740 C,respectively,which demonstrates the outstanding thermo-oxidative stabi-lity of BDS polymer.Based on the above analysis,the effect of type of sample on thermal and thermo-oxidative prop-erties is little in the same atmosphere for the BDS poly-mer.It is reported that for most of the thermosetting resins,thermo-oxidation process starts around 500 C and at 600 C char yield (CR)equals zero,7but the BDS polymer still exhibits significant char retention of 72%(solid sample)and 69%(powder sample)by weight at 600 C in air.Generally,predominant factors that contribute to thermal stability in polymers are primary bond strength,rigid intra-chain structure,the degree of cross-linking,and so on.1,12,25The C–O (bond dissociation energy is 332kJ mol À1)and C–S (bond dissociation energy is 328kJ mol À1)among BDS polymer molecular chains are relatively weak;26as a result,Table 1.Experimental and calculated cell parameters of BDS monomer.h k l d (A ˚)Experimental 2 (deg)Calculated 2 (deg)Experimentalsin 2 Calculated sin 2 Experimental sin 2 –calculated sin 220013.06 6.76 6.760.0034760.003474 2.1Â10À63008.8010.0410.140.0076570.007816 1.6Â10À4400 6.4713.6613.540.0141430.013900 2.4Â10À4120 5.9314.9214.770.0168570.016525 3.3Â10À4410 5.7715.3415.340.0178140.017809 4.6Â10À6320 5.2216.9817.620.0217970.023470 1.7Â10À3420 4.4919.7419.790.0293830.029550 1.7Â10À4101 4.0821.7821.840.0356920.035895 2.0Â10À4130 3.9822.3021.900.0373950.036100 1.3Â10À3201 3.9222.6422.630.0385290.038494 3.5Â10À5211 3.7423.7423.760.0423090.0423958.6Â10À5311 3.5724.9024.970.0464780.046742 2.6Â10À4021 3.4126.0826.020.0509090.050670 2.4Â10À4321 3.2427.5227.990.0565750.058501 1.9Â10À33312.7532.4632.450.0781170.0780645.2Â10À5BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Figure 5.DSC thermogram of BDS monomer with 5.8mol%of APB.DSC:differential scanning calorimetry;BDS:bis-[4-(3,4-dicya-nophenoxy)phenyl]sulfone;APB:1,3-bis(4-aminophenoxy)benzene.Figure 6.WAXD of BDS prepolymer and polymer.WAXD:wide-angle X-ray diffraction;BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Peng et al.841these single bonds rupture firstly with increasing temperature,which could be responsible for the maximum rate at T d,max of 476 C (solid sample)and 493 C (powder sample).The ther-mal decomposition in air involves several steps associating with oxidation reactions differing from those under N 2.Ortho H atoms on substituted benzene become active due to electron-donating effects of –O–groups,which results in the first T d,max of 486 C (solid sample)and 492 C (powder sam-ple)in addition to dissociation of C–O and C–S bonds at ele-vated temperature because active H atoms are oxidized easily leading to thermal degradation.12,27The other two maximums at 655and 725 C for the solid sample and 658and 740 C for the powder sample might be attributed to the oxidation of degraded polyisoindole and polytriazine because of their aro-matic structure and absence of active H atoms.Obviously,the rigid aromatic and heterocyclic molecu-lar skeleton and high cross-linked network together ensure excellent thermal stability of BDS polymer.Meanwhile,the low level of active H atoms on molecular structure ben-efits the excellent oxidation stability of the BDS polymer.CR can be used as a criterion for evaluating limiting oxygen index (LOI)of the polymers according to van Krevelen,28and LOI test is a commonly used method for evaluation of flame retardancy of polymeric materials.There is a linear relationship between LOI and CR for halogen-free polymers:LOI ¼17:5þ0:4CR ðÞð2ÞFrom this equation,a higher CR will improve flame retardancy,and BDS polymer has an LOI value of 40.3calculated according to the CR at 1000 C under N 2atmo-sphere for powder sample.On the basis of this LOI value,BDS polymer can be classified as self-extinguishing material indicating excellent fire retardance.29Mechanical and dynamic mechanical propertiesYoung’s modulus,tensile strength,and elongation at break of BDS polymer are displayed in Table 3.The BDS polymer fractures without any yield during tensile test implying a stiff and brittle tensile behavior.The BDS polymer exhibits high Young’s modulus (4.02GPa),high tensile strength (64.16MPa),and low elongation at break (1.77%)which are attributed to its rigid aromatic structure and cross-linked structure.Figure 11displays DMA spectra of BDS polymer.The storage modulus exhibits a value of 3.36GPa at 25 C,and such high modulus is ascribed to the aromatic and cross-linked microstructure.The loss tangent (tan d )is the ratio of loss modulus to storage modulus,and the temperature cor-responding to a maximum of tan d curve is taken as T g ,which is vital for high-temperature polymers because it lim-its the maximum application temperature.As seen in Figure 11,T g of BDS polymer is 337 C,which is much higher than most polyimides,which are around 200–300 C.30Another important merit of phthalonitrile thermosets is their low water absorption capability.14,15Figure 12showsFigure 7.FTIR spectra of BDS prepolymer and polymer.FTIR:Fourier transform infrared spectroscopy;BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Figure 8.Schematic structure of BDS polymer.BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.842High Performance Polymers 26(7)a plot of the water absorption versus time for BDS polymer soaked in distilled water.The maximum amount of water uptake is approximately 3.3wt %after 69days.The water absorption reaches a plateau after 30days.For the use in a high humidity or aqueous environment,the BDS polymer is close to some polyimides but superior to many high-performance polymers such as polyamide 46(12.4%).31Besides high degree of cross-linking of BDS polymer,the absence of hydrophilic groups on molecular chain contri-butes to its low wateruptake.Figure 9.Fracture surfaces of the BDS polymer:(a)Â1000and (b)Â10,000magnification.BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Figure 10.TGA curves of BDS polymer solid sample under N 2(a),solid sample in air (b),powder sample under N 2(c),and powder sample in air (d)atmospheres.TGA:thermogravimetric analysis;BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Peng et al.843Figure 13shows the DMA spectra of the water-absorbed BDS polymer,and its T g reduces by 15 C compared with that of dry BDS polymer;meanwhile,there is a b -relaxa-tion peak at 112 C in addition to the a -relaxation (T g ),both of them are ascribed to the absorbed moisture which acts as a plasticizer in polymer matrix and prefers to reduce inter-molecular forces resulting in the growth of molecular chain mobility.25However,the impact of water uptake on storage modulus is very little for the BDS polymer.ConclusionA novel high-temperature diphenyl sulfone-based phthalo-nitrile polymer is prepared from BDS monomer.Polytria-zine and polyisoindole structures might form during BDS polymerization as revealed by FTIR.BDS polymer exhibits good thermal and thermo-oxidative stabilities,outstanding mechanical properties,high T g ,and excellent flame-retardant property.Based on all of the above superiorproperties,the BDS polymer is a competent candidate for applications in the field of heat-resistant and high-performance materials.AcknowledgementProf.Y.Kagawa at the University of Tokyo,Japan,and Prof.F.X.Yin at the National Institute of Materials Science (NIMS),Ibaraki,Japan,are greatly acknowledged for their help.Table 2.Thermal parameters of BDS polymer.T d,5%( C)T d,max ( C)CR at 1000 C (%)LOI at 1000 CN 2Solid sample 4184765941.1Powder sample 4364935740.3AirSolid sample 450486,655,7250–Powder sample441492,658,740–BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone;CR:char yield;LOI:limiting oxygen index;N 2:nitrogen;T d,5%:5%weight loss temperature;T d,max :maximum decomposition temperature.Table 3.Mechanical properties of BDS polymer.Young’s modulus (GPa)Tensile strength(MPa)Elongation at break (%)4.0264.161.77BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Figure 11.DMA plots for BDS polymer versus temperature.DMA:dynamic mechanical analysis;BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Figure 12.Plot of water uptake over time for BDS polymer.BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.Figure 13.DMA plots of BDS polymer with 3.3wt%water uptake.DMA:dynamic mechanical analysis;BDS:bis-[4-(3,4-dicyanophenoxy)phenyl]sulfone.844High Performance Polymers 26(7)FundingThis work was supported by the National Natural Science Foundation of China(grant no.51073049and21001039),the Youth Foundation of Hebei Educational Committee(grant no. QN20131037),Natural Science Foundation of Hebei Province (grant no.E2014202033),the Scientific Research Foundation for the Returned Overseas Scholars,Hebei Personnel Commit-tee(grant no.CG2013003003),and the Scientific Research Foundation for the Returned Overseas Chinese Scholars,State Education Ministry.References1.Keller TM and Griffith JR.Resins for aerospace:ACS Sympo-sium Series.Washington,DC:American Chemical Society, 1980,pp.25–34.skoski M,Dominguez DD and Keller TM.Synthesis andproperties of a bisphenol a based phthalonitrile resin.J Polym Sci A:Polym Chem2005;43:4136–4143.3.Gaymans RJ,Hodd KA and Holmes-Walker WA.Studies ofheterocyclic polymers:part1.The synthesis and structure of macrocyclic polymers.Polymer1971;12:400–408.4.Gaymans RJ,Hodd KA and Holmes-Walker WA.Studies inheterocyclic polymers:part2.The thermal degradation of some macrocyclic polymers.Polymer1971;12:602–615.5.Hodd KA and Holmes-Walker WA.Studies in heterocyclicpolymers.III.A comparison of the thermal 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PBO纤维增强树脂基复合材料的制备及性能研究的开题报告一、研究背景和意义纤维增强树脂基复合材料 (Fiber Reinforced Polymer Composites, FRP Composites) 具有高强度、高刚度、耐疲劳、耐腐蚀、轻量化等优异性能，因而在航空航天、汽车、建筑、民用、军事等领域得到广泛应用。
纤维增强树脂基复合材料的研制是一种重要的新材料开发方向。
PBO (Poly(p-phenylene benzobisoxazole)) 纤维是最具有强度和模量的材料之一，也是目前市场上最先进的高强度、高模量技术纤维。
PBO纤维具有高强度、高模量、阻燃、耐热性好、耐腐蚀、抗紫外线、耐疲劳等卓越性能，已被广泛应用于高温、高强度和防护等领域。
PBO纤维与树脂基体复合材料中，能够发挥纤维增强和增加复合材料的强度、模量、热稳定性等优异性能。
本文旨在研制 PBO纤维增强树脂基复合材料，研究其制备工艺，评估其力学性能和热稳定性能，以期为广大使用者提供一种新型高性能材料。
二、研究内容和方法本文将采用热固性树脂为基体，PBO纤维为增强体，采用手层叠工艺制备 PBO纤维增强树脂基复合材料，研究不同PBO纤维含量下的复合材料的制备工艺优化和力学性能表现，探讨纤维含量和力学性能之间的关系。
同时，利用热重分析、差热分析和红外光谱等手段对复合材料的热稳定性能进行评估，研究不同温度下的热性能表现和热分解动力学机理。
三、预期研究结果本研究将研究 PBO纤维增强树脂基复合材料的制备工艺及其力学性能和热稳定性能，预计得到以下几方面的研究结果：1. 研究不同PBO纤维含量下的复合材料的制备工艺优化，确定最佳纤维含量和制备工艺。
2. 评估 PBO纤维增强树脂基复合材料的力学性能，研究纤维含量和力学性能之间的关系，探讨其在高强度和高刚度方面的应用潜力。
3. 评估 PBO纤维增强树脂基复合材料的热稳定性能，研究不同温度下的热性能表现和热分解动力学机理，探讨其在高温环境下的应用潜力。
Original ArticleSynthesis of polystyrene nanolatexes viaemulsion polymerization using sodiumdodecyl sulfonate as the emulsifierLiyan Yang and Yangchuan KeAbstractPolystyrene(PS)nanolatexes were successfully prepared via emulsion polymerization using sodium dodecyl sulfonate as the emulsifier.The effects of emulsifier concentration,initiator concentration,polymerization reaction time,and polymerization reaction temperature on particle size and size distribution of PS colloidal spheres were investigated,respectively.The particle size of the diluted polymer emulsion was about20nm,as determined by laser scattering.These obtained PS particles were also characterized using Fourier transform infrared spectroscopy and scanning electron microscopy.KeywordsPolystyrene nanolatexes,emulsion polymerization,sodium dodecyl sulfonateIntroductionPolymer nanoparticles(PNPs)have attracted much atten-tion over recent decades in the field of material and colloi-dal science.During the past decades,PNPs are widely used in many fields,such as electronics,paint coatings,optics,cata-lysis,diagnostics,therapeutics,and so on.1–6These particles can be made from large numbers of materials,such as metals, metal oxides,inorganic materials,polymeric materials,and so on.7–10The diameter of these particles can range from sev-eral to several hundreds of nanometers.Among these parti-cles,polystyrene(PS)nanolatexes are one of the most promising materials due to their monodispersity,strong adsorption ability,uniform particle size,large specific surface area,11–14and so on.More and more attention has been paid to the study of PS in many countries.Several methods for production of the PS nanolatexes have been developed,such as emulsion polymerization, suspension polymerization,microemulsion polymeriza-tion,cationic polymerization,and dispersion polymeriza-tion.15–19In general,dispersion polymerization technique has been widely used to produce monodisperse micron-sized polymer particles directly in the size range of approx-imately0.5–20m m.Hou et al.20synthesized five kinds of PS microspheres of approximately4–6m m in diameter bearing different surface functional groups by dispersion copolymerization of styrene and various vinyl comono-mers.Although this method is simple and practicable,the average particle diameter of the copolymer is large.Suspension polymerization is a kind of precipitation poly-merization.Kim et al16synthesized PS particles by the reverse iodine transfer polymerization-suspension polymer-ization ranging approximately from100nm–200m m with broad size distribution.Although this system uses water as polymerization medium which is nonflammable and non-toxic,the average particle diameter and the size distribution of PS particles are large,broad,and polydisperse.Microe-mulsion polymerization is a new and effective approach for preparing nanoscaled polymer particles and has attracted significant attention.However,the commercial use of this process has been limited because typical polymer formula-tions are diluted and require a large ratio of surfactant com-pared with monomer.The surfactant concentrations usually exceed the amount required for polymer stability.21 To overcome the disadvantages as mentioned previ-ously,emulsion polymerization is generally used to prepare PS nanoparticles.15Over the past decades,emulsion poly-merization has been used for the production of polymers. To date,it is employed for the polymerization of a variety State Key Laboratory of Heavy Oil Processing,College of Science,China University of Petroleum,Beijing,ChinaCorresponding author:Yangchuan Ke,State Key Laboratory of Heavy Oil Processing,College of Science,China University of Petroleum,Beijing102249,China. Email:kyc01@High Performance Polymers1–6ªThe Author(s)2014Reprints and permission:/journalsPermissions.navDOI:10.1177/0954008314533979of monomers such as styrene,graphene,methyl metacry-late,isoprene,butadiene,and so on.22–24Emulsion poly-merization is the most successful industrial methods. Regarding the most commonly used organic solvent-based systems,water as polymerization medium exhibits unique properties such as high heat capability and high polarity.25Generally,high-molecular-weight polymers and narrow size distribution particles are easy to be obtained in emulsion polymerization.26,27Recently,the micro-sized PS nanoparticles were successfully prepared by emulsion polymerization and the average diameter is60nm.15Kim et al.28synthesized unmodified and modified PS nanoparti-cles with hydrophilic end group on surface by emulsion polymerization for adsorption of a protein(immunoglobu-lin G,IgG).The presence of formed IgG-PS particle com-plex was confirmed by dynamic light scattering measurement which shows the increased size of particle (approximately178and220nm)after IgG immobilization. Therefore,emulsion polymerization has been widely applied in the design and preparation of functional polymer materials with special function,such as block copolymers, surface-modified emulsion,and responsive particles,or with fancy morphologies such as core–shell structure parti-cles and natural material-coated emulsions.29–32 In this study,small-sized PS nanolatexes with uniform distribution via emulsion polymerization using sodium dodecyl sulfonate(SDSN)as the surfactant have been suc-cessfully prepared.The effects of emulsifier concentration, initiator concentration,polymerization reaction time,and polymerization reaction temperature on particle size and size distribution of PS colloidal spheres were investigated, respectively.The particle size of the diluted polymer emul-sion was about20nm,as determined by laser scattering. These obtained PS particles were also characterized by Fourier transform infrared spectroscopy(FTIR)and scan-ning electron microscopy(SEM).ExperimentalMaterialsStyrene(St)from Tianjin Guangfu Chemical Reagents Company(China)was vacuum distilled to remove trace inhibitor prior to use.Divinylbenzene(DVB),SDSN,and potassium peroxydisulfate(KPS)from Beijing Chemical Reagents Company(China)were used as received. Synthesis of the PS nanospheresPS nanolatexes were successfully prepared via emulsion polymerization.A typical emulsion recipe,consisting of 0.1wt%SDSN,0.01wt%KPS,0.01wt%DVB,20mL St,and100mL water,was employed.It was performed in a three-necked flask immersed in an oil bath controlled at70 C.KPS was selected as a water-soluble initiator.Typically,the emulsifier was dissolved in deionized water in a250-mL flask and agitated at around400r minÀ1with a magnetic stirrer for15min.A condenser pipe was used to prevent evaporation during polymerization.After homoge-nization,the solution was purged with nitrogen(N2)for45 min to remove the dissolved oxygen;meanwhile,the reac-tor temperature was brought to70 C.St monomer,DVB, and KPS were added into the reaction system under N2 protection.Afterward,the system was obturated,and the solution was stirred for16h.Then,the solution was natu-rally cooled and demulsified by the addition of alcohol; finally,the PS nanospheres were collected and washed three times with deionized water and then dried at50 C in the oven for24h.PS spheres of different particle sizes were synthesized by changing the experiment conditions. The emulsion polymerization mechanism follows Harkins theory.33The chemical reaction and the chemical struc-ture of the emulsifier is shown in Figure1. CharacterizationThe PS particle size and size distribution were determined by laser scattering using a Malvern Mastersizer2000 (Malvern Instruments,Malvern,UK)at25 C.Before analysis,the latexes were diluted with deonized water to minimize the particle–particle interactions.The determina-tion of PS size and size distribution is derived from Eshuis et al.34The number-average,volume-average,and weight-average diameters(i.e.,D n,D v,and D w,respectively)are defined as usual.35If one were to assume a single-sized pop-ulation following a Gaussian distribution,then the polydis-persity index(PDI)related to the standard deviation( )of the hypothetical Gaussian distribution is shown below:D n¼PN i D iPN ið1ÞD v¼PN i D3iPN i1=3ð2ÞD w¼PN i D6iPN i Di1=3ð3ÞCH CH2Figure1.Chemical reaction and the chemical structure of the emulsifier.2High Performance PolymersPDI ¼ 2Z Dð4Þwhere N i is the number of particles having diameter D i .FTIR spectra of PS nanolatexes were obtained using an FTS-3000spectrophotometer (Digilab Inc,Marlborough,MA,USA).FTIR spectra were obtained at wave numbers ranging from 4000cm À1to 400cm À1.The measured wafer was prepared by potassium bromide (KBr)pellet with a 1/100weight ratio of sample to KBr.The resolution was set at 2cm À1for all measurements.SEM analysis was measured using a field-emission scanning electron microscope Quanta 200F(FEI Corpora-tion,Hillsboro,Oregon,USA)with an accelerating voltage of 20kV.Results and discussionEffect of reaction conditions on particle size of PS nanolatexesEffect of SDSN concentration.As is well documented,particle size decreases with increasing emulsifier concentration.36Figure 2demonstrates the effect of SDSN concentration on D v of PS nanolatexes.Variation of SDSN concentration was found to be an effective method for obtaining average diameters in the range of approximately 10–30nm,while keeping constant initiator and total monomer concentration.D v of PS nanolatexes curve shows that with an increas-ing SDSN concentration,the volume-average particle size decreased.This can be attributed to variations in the num-ber of the loci.A higher concentration of surfactant gener-ated and stabilized larger number of PS nanolatexes;thespeed of reaction also accelerated.However,when the SDSN concentration was higher than 0.4wt %,reaction rate and viscosity of the system increased rapidly,some PS nanolatexes coalesced into larger particles,and the particle size did not decrease but rather increased slightly.Effect of KPS concentration.The effect of KPS concentration on D v of PS nanolatexes is shown in Figure 3.The curve shows that with an increasing concentration of KPS,from 0.01wt %to 0.04wt %,based on monomer weight,the D v of PS nanolatexes decreased.This result can be explained as follows:higher initiator concentration generated more free radicals and formed more activated micelles.More-over,the decomposition of initiator can play a part in in situ co-emulsifying effect.In addition,increasing the concen-tration of KPS enhanced the in situ co-emulsifying effect and stabilized the formed particles easily.However,when the KPS concentration was higher than 0.04%,D v of PS nanolatexes increased slightly.This is because the emulsi-fier in the system could not stabilize such more free radicals simultaneously generated by higher initiator concentration and increased the probability of aggregation.Thus,the par-ticle size increased.Effect of polymerization reaction time.Figure 4exhibits the effect of reaction time on D v of PS nanolatexes;mean-while,other parameters are fixed.Clearly,the particle size grows as the polymerization time increases.From Figure 4,the reaction can be divided into three stages.In the first stage,more polymer nuclei are rapidly produced,and the system becomes unstable.In the second stage,they gradually come together to form larger size par-ticles and increase to 20.62nm average within 6h.In the0.10.20.30.40.50.61520253035SDSN (wt%)D v (n m )Figure 2.Effect of SDSN concentration on volume–average particle diameter of polystyrene nanolatexes.A nonlineardecrease in particle size was observed with increasing concen-tration of SDSN,meanwhile,initiator concentration and volumes of styrene and of aqueous continuous phase were kept constant.SDSN:sodium dodecyl sulfonated.0.010.020.030.040.050.062021222324252627D v (n m )KPS (wt%)Figure 3.Effect of KPS concentration on volume–average parti-cle diameter of polystyrene nanolatexes.A nonlinear decrease in particle size was observed with increasing concentrations of KPS,meanwhile,surfactant concentration and volumes of styrene and aqueous continuous phase were kept constant.KPS:potassium peroxydisulfate.Yang and Ke3last stage,as the reaction time increases,the growth of the polymer sphere particle size almost never changes.Effect of polymerization reaction temperature.The relation between the particle sizes of PS nanolatexes and reaction temperature of the system is illustrated in Figure 5.It is clear that D v of PS decreases with the increasing tempera-ture at first and then increases when the temperature is higher than 70 C.The reason is that when the temperature was higher than 70 C,the decomposition rate of initiator increased,and the stability of PS nanolatexes decreased.Particles should gather together to improve the surface charge density so as to improve the stability of PS nanola-texes.The aggregation of PS nanolatexes generated more number of larger size particles.Thus,the optimal reaction temperature is 70 C.Particle size distribution of PS nanolatexes.The particle size distribution of PS nanolatexes was measured by Malvern Mastersizer 2000(Malvern Instruments).The particle size of PS nanolatexes via emulsion polymerization with differ-ent emulsifier concentration was measured and is listed in Table 1.From Table 1,it can be seen that D w /D n <1.05,indicating that PS nanolatexes are of narrow and small size distribution.FTIR analysis.Figure 6illustrates the IR absorption spectra of the PS spheres.Obviously,there are several absorption peaks within the involved wave number range.The absorp-tion bands at 3027.7and 2921.7cm À1correspond to aro-matic C–H stretching vibration absorption,and there are60657075801520253035D v (n m )T (°C)Figure 5.Effect of reaction temperature on volume–average particle diameter of polystyrene nanolatexes.5D v (n m )t (h)Figure 4.Effect of polymerization reaction time on volume–average particle diameter of polystyrene nanolatexes.Table 1.Average particle size of polystyrene nanolatexes via emulsion polymerization with different emulsifier concentration.Concentration (wt%)D n (nm)D w (nm)D w /D n PDI (Â10À1)0.1028.4227.59 1.030.720.2026.5326.01 1.020.570.3022.4721.61 1.040.390.4020.3920.19 1.010.250.5023.7223.25 1.020.460.6028.6727.841.030.83D n :number-average diameter;D w :weight-average diameter;PDI:polydispersity index.40003500300025002000150010005002844.5698.1752.11452.21492.71604.52921.7Wavenumber (cm –1)T r a n s m i t t a n c e (%)3027.73446.2Figure 6.FTIR spectra of the polystyrene spheres.FTIR:Fourier transform infrared.4High Performance Polymersthree absorption peaks at 1604.5,1492.7,and 1452.2cm À1that correspond to aromatic C ¼C stretching vibration absorption.These absorption peaks indicate the existence of benzene rings.The absorption peaks at 752.1and 698.1cm À1correspond to C–H out-of-plane bending vibra-tion absorption and indicate that there is only one substitu-ent in the benzene ring.Figure 6also shows the absorption peaks at 2921.7and 2844.5cm À1,corresponding to the existence of methylene.In addition,the absorption peaks at 3446.2cm À1correspond to O–H stretching vibration absorption indicating the existence of hydroxyl.These FTIR results have confirmed that the polymeriza-tion reaction of St has occurred.There is no absorption peak at approximately 1680–1620cm À1or 970–800cm À1corre-sponding to olefin C ¼C stretching vibration absorption or olefin hydrogen bending vibration,which is a further indica-tion that the polymerization reaction occurred.Obviously,FTIR characterization results of PS are in accord with the standard spectrum diagram indicating that the product is pure PS.SEM morphology.The SEM images of PS nanolatexes with different emulsifier concentration are shown in Figure 7.It is confirmed that PS nanolatexes with uniform size were successfully prepared via emulsion polymerization.In Figure 7(a),the nanospheres were perfect spheres with a very smooth surface and well dispersed.Figure 7(b)indi-cates that when the emulsifier concentration was 0.6wt %,higher than 0.4wt %,some PS particles aggregated to gen-erate larger particles,and the particle size distribution was not homogenous anymore.ConclusionsPS nanolatexes were successfully prepared via emulsion polymerization using SDSN as the emulsifier.The effects of emulsifier concentration,initiator 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