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茂金属催化剂催化烯烃聚合反应的研究 ——聚合物的聚集行为和热性能 Letter

吴长江, Minqiao Ren, Liping Hou, Shuzhang Qu, Xinwei Li, Cui Zheng, Jian Chen, 王伟

《工程（英文）》 2023年第30卷第11期页码 93-99 doi: 10.1016/j.eng.2023.07.001

摘要：

Olefin solution polymerization can be used to obtain high-performance polyolefin materials that cannot be obtained via other polymerization processes. Polyolefin elastomers (POE) are a typical example. Due to cost, only a few linear α-olefins (e.g., 1-butene, 1-hexene, and 1-octene) are used as comonomers in solution polymerization in industry. However, α-olefin comonomers with other structures may have different effects on polymerization in comparison with common linear ones. Moreover, the properties of the corresponding materials may differ significantly. In this work, copolymers of ethylene with linear and end-cyclized α-olefins are synthesized using a metallocene catalyst. The copolymerization of ethylene with linear α-olefins results in a higher turn-over frequency (TOF) and lower incorporation than copolymerization with end-cyclized α-olefins, which may indicate that end-cyclized α-olefins have a higher coordination probability and lower insertion rate. In this reaction, the comonomer is distributed randomly in the polymer chain and efficiently destroys crystallization. End-cyclized α-olefins exhibit a much stronger crystallization destructive capacity (CDC) in the copolymer than linear α-olefins, possibly because linear α-olefins act mainly in the radial direction of the main chain of the polymer, while end-cyclized α-olefins act mainly in the axial direction of the main chain.

关键词： Metallocene catalyst Ethylene copolymerization Comonomer distribution Crystallization destructive capacity

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Destructive and non-destructive evaluation of concrete for optimum sand to aggregate volume ratio

《结构与土木工程前沿（英文）》 2021年第15卷第6期页码 1400-1414 doi: 10.1007/s11709-021-0779-8

摘要： Aggregates are the biggest contributor to concrete volume and are a crucial parameter in dictating its mechanical properties. As such, a detailed experimental investigation was carried out to evaluate the effect of sand-to-aggregate volume ratio (s/a) on the mechanical properties of concrete utilizing both destructive and non-destructive testing (employing UPV (ultrasonic pulse velocity) measurements). For investigation, standard cylindrical concrete samples were made with different s/a (0.36, 0.40, 0.44, 0.48, 0.52, and 0.56), cement content (340 and 450 kg/m³), water-to-cement ratio (0.45 and 0.50), and maximum aggregate size (12 and 19 mm). The effect of these design parameters on the 7, 14, and 28 d compressive strength, tensile strength, elastic modulus, and UPV of concrete were assessed. The careful analysis demonstrates that aggregate proportions and size need to be optimized for formulating mix designs; optimum ratios of s/a were found to be 0.40 and 0.44 for the maximum aggregate size of 12 and 19 mm, respectively, irrespective of the W/C (water-to-cement) and cement content.

关键词： aggregates non-destructive testing sand-to-aggregate volume ratio (s/a) maximum aggregate size (MAS)

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声学综合无损检测技术

陈积懋

《中国工程科学》 2000年第2卷第4期页码 64-69

摘要：

论述了检测复合材料和胶接结构不连续（缺陷）的新型多模综合无损检测技术。该技术以声与超声检测技术为基础，包含五种不同检测模式，用以检测复合材料与胶接结构的失粘、脱粘、分层、疏松、夹芯压皱及其他缺陷。它适用于复合材料与构件的制造、维修和使用现场。它的适用对象范围广泛，几乎覆盖了现有常用的复合材料和胶接结构。它的检测可靠性高，重复精度好。文章还讨论了组成多膜声学综合胶接检测仪的五种不同检测模式的原理，并从我们和国内外同行的大量实践经验出发，说明了综合无损检测技术的巨大发展前景。

关键词：声学综合检测综合无损检测复合材料无损检测机械阻抗分析振动分析共振检测

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Synthesis and characterization of macromolecular surface modifier PP--PEG for polypropylene

CHEN Hanjia, SHI Xuhua, ZHU Yafei, ZHANG Yi, XU Jiarui

《化学科学与工程前沿（英文）》 2008年第2卷第1期页码 102-108 doi: 10.1007/s11705-008-0018-z

摘要： A novel macromolecular surface modifier, polypropylene-grafted-poly(ethylene glycol) copolymer (PP--PEG), was synthesized by coupling polypropylene containing maleic anhydride with monohydroxyl-terminated poly(ethylene glycol). The effects of the reaction condition on the graft reactions were studied. The copolymers were characterized by IR, H NMR, thermogravimetry (TG) and differential scanning calorimetry (DSC). The results indicated that the graft reactions were hindered by increasing the molecular weight of PP or PEG. The graft copolymer was found to have a higher initial thermal degradation temperature and lower crystallization capacity as compared with pure PP, and the side chain of PEG hindered the PP chain from forming a perfect ? crystal. The thermal stability of PP--PEG decreased with the increasing content or molecular weight of PEG. The copolymers were blended with polypropylene to modify the surface hydrophilicity of the products. The results of attenuated total reflectance FTIR spectroscopy (ATR-FTIR) showed that PP--PEG could diffuse preferably onto the surface of the blends and be suitable as an effectual macromolecular surface modifier for PP.

关键词： polypropylene crystallization capacity attenuated hydrophilicity reflectance

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Separation of gibberellic acid (GA3) by macroporous adsorption resins

WANG Ruifang, YANG Jialing, SHI Zuoqing, OU Lailiang

《化学科学与工程前沿（英文）》 2008年第2卷第2期页码 171-175 doi: 10.1007/s11705-008-0025-0

摘要： The adsorption effects of several macroporous adsorption resins for gibberellic acid (GA3) were investigated. The dynamic adsorption capacity is 58.38 mg/g dry beads for resin R4 and 96.46 mg/g dry beads for resin R5 which is consistent with the surface area. Aqueous methanol (50%, V/V) is a good eluent and the yield of GA3 is above 95%. The concentration of GA3 could increase five-fold after an adsorption-elution cycle and this is important when considering further crystallization of GA3 in an industrial process.

关键词： industrial gibberellic adsorption capacity crystallization consistent

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破坏性地震是可以预测的——孕震物理模型及临震信号

孙威

《中国工程科学》 2007年第9卷第7期页码 7-17

摘要：

讨论地震前兆有它自已的孕震物理模型，地震孕育全过程分为加载、相持、卸载、短临和临震５个阶段；多次震例证明，破坏性地震的孕震物理模型是会重复和再现的；提出了追踪地震前兆信息，循序渐进预报地震的分析方法，对地震预报的阶段性进行了实用性的划分，有希望实现对破坏性地震的预报。

关键词：破坏性地震孕震物理模型临震信号地震前兆

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Progress in membrane distillation crystallization: Process models, crystallization control and innovative

Xiaobin Jiang, Linghan Tuo, Dapeng Lu, Baohong Hou, Wei Chen, Gaohong He

《化学科学与工程前沿（英文）》 2017年第11卷第4期页码 647-662 doi: 10.1007/s11705-017-1649-8

摘要： Membrane distillation crystallization (MDC) is a promising hybrid separation process that has been applied to seawater desalination, brine treatment and wastewater recovery. In recent years, great progress has been made in MDC technologies including the promotion of nucleation and better control of crystallization and crystal size distribution. These advances are useful for the accurate control of the degree of supersaturation and for the control of the nucleation kinetic processes. This review focuses on the development of MDC process models and on crystallization control strategies. In addition, the most important innovative applications of MDC in the last five years in crystal engineering and pharmaceutical manufacturing are summarized.

关键词： membrane distillation crystallization mathematics model nucleation separation hybrid process

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Effects of a structurally related substance on the crystallization of paracetamol

Ali SALEEMI, I.I. ONYEMELUKWE, Zoltan NAGY

《化学科学与工程前沿（英文）》 2013年第7卷第1期页码 79-87 doi: 10.1007/s11705-013-1308-7

摘要： Paracetamol (PCM) was crystallized from an isopropanol (IPA) solution containing various small amounts of metacetamol as an additive. The effect on the nucleation kinetics was studied by measuring the induction time to nucleation and the metastable zone width using focused beam reflectance measurements (FBRM) and attenuated total reflectance (ATR-UV/Vis) spectroscopy. Both the induction time and the metastable zone width were expressed as functions of the additive concentration. Small amounts of metacetamol (1–4 mol-%) were found to cause significant inhibition to the nucleation by extending both the induction time and the metastable zone width. A progressive change in the morphology of the paracetamol crystals from tabular to columnar habit was observed with increasing metacetamol concentration. The solvent also had a significant effect on the size of the paracetamol crystals as smaller crystals were obtained in IPA than in aqueous solution. The dissolution rate of paracetamol was improved by the incorporation of metacetamol with 4 mol-% having the most effect. A supersaturation control (SSC) approach was implemented for the PCM-IPA system with and without metacetamol in an attempt to control and obtain larger metacetamol-doped paracetamol crystals.

关键词： acetaminophen metacetamol crystallization metastable zone width induction time supersaturation control

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Interfacial induction and regulation for microscale crystallization process: a critical review

《化学科学与工程前沿（英文）》 2022年第16卷第6期页码 838-853 doi: 10.1007/s11705-021-2129-8

摘要： Microscale crystallization is at the frontier of chemical engineering, material science, and biochemical research and is affected by many factors. The precise regulation and control of microscale crystal processes is still a major challenge. In the heterogeneous induced nucleation process, the chemical and micro/nanostructural characteristics of the interface play a dominant role. Ideal crystal products can be obtained by modifying the interface characteristics, which has been proven to be a promising strategy. This review illustrates the application of interface properties, including chemical characteristics (hydrophobicity and functional groups) and the morphology of micro/nanostructures (rough structure and cavities, pore shape and pore size, surface porosity, channels), in various microscale crystallization controls and process intensification. Finally, possible future research and development directions are outlined to emphasize the importance of interfacial crystallization control and regulation for crystal engineering.

关键词： interfacial crystallization heterogeneous nucleation supersaturation micro/nanostructure process control and intensification

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The feasibility of coating by cooling crystallization on ibuprofen naked tablets

Fatima Mameri, Ouahiba Koutchoukali, Mohamed Bouhelassa, Anne Hartwig, Leila Nemdili, Joachim Ulrich

《化学科学与工程前沿（英文）》 2017年第11卷第2期页码 211-219 doi: 10.1007/s11705-017-1619-1

摘要： Sugar spray coating is a frequently used process in the pharmaceutical industry. However, this process presents the disadvantage to form an amorphous coating around the active ingredient. A crystalline coating formed on the surface of a tablet is highly desirable. Recently, a new process of coating by cooling crystallization has been developed and applied on bisacodyl pastilles obtained by melt crystallization. In this work, we investigated the feasibility of coating by cooling crystallization on ibuprofen “naked tablets” manufactured by compression. In the first part of this work, the solubility and the metastable zone width have been determined experimentally for the coating solution because they are essential factors for any crystallization process. In the second part, the coating process is investigated on the operating conditions that affect the surface morphology and the crystal growth rate. These experimental conditions include concentration of the coating solution, degree of sub-cooling, agitation speed, retention time, and surface properties of the naked ibuprofen tablets. The results show that naked tablet coating by cooling crystallization is feasible and can be applied in the pharmaceutical industry.

关键词： coating solution crystallization ibuprofen tablets sucrose

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Utilizing melt crystallization fundamentals in the development of a new tabletting technology

Ahmed ABOUZEID,Sandra PETERSEN,Joachim ULRICH

《化学科学与工程前沿（英文）》 2014年第8卷第3期页码 346-352 doi: 10.1007/s11705-014-1443-9

摘要： Increasing production effeciency and lowering costs are some of the many advantages melt crystallization technology offers over the conventional methodology of tabletting. A normal tablet consists of a pure shell or a coat and a separate core constituting the pharmaceutical active ingredient. Great emphasis is put on the purity of the shell since its purpose is to solely protect and deliver the active ingredient to its target. Melt crystallization is a purification (separation) process. It is discussed here for its ability to produce coated tablets, by separating the “coating” material from the “to be coated” material coming from one molten mixture. Molten drops of lutrol-ibuprofen mixture are produced using the drop forming technique. The subsequent analysis involves proving and quantifying the phase separation (coat purity). The mechanism of a crystallizing drop is shown as direct evidence of the ongoing process. Moreover, solidified tablet batches are analyzed for the purity of their coating by measuring the ibuprofen concentration. This optimization process is carried out through multiple stages of development and condition enhancements in order to produce the most pure tablet coating. As a result, a trial showing an almost purely coated tablet is presented here.

关键词： phase separation melt crystallization tablets process optimization

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Nucleic acid crystallization and X-ray crystallography facilitated by single selenium atom

Wen Zhang,Jack W. Szostak,Zhen Huang

《化学科学与工程前沿（英文）》 2016年第10卷第2期页码 196-202 doi: 10.1007/s11705-016-1565-3

摘要： X-ray crystallography is a powerful strategy for 3-D structure determination of macromolecules, such as nucleic acids and protein-nucleic acid complexes. However, the crystallization and phase determination are the major bottle-neck problems in crystallography. Recently we have successfully developed synthesis and strategy of selenium-derivatized nucleic acids (SeNA) for nucleic acid crystallography. SeNA might not only provide the rational strategies to solve the phase determination problem, but also offer a potential strategy to explore crystallization solutions.

关键词： selenium DNA RNA nucleic acid crystallization

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Preparation and crystallization kinetics of micron-sized Mg(OH)

Xingfu SONG, Kefeng TONG, Shuying SUN, Ze SUN, Jianguo YU

《化学科学与工程前沿（英文）》 2013年第7卷第2期页码 130-138 doi: 10.1007/s11705-013-1332-7

摘要： Magnesium hydroxide is an important chemical, and is usually obtained from seawater or brine via precipitation process. The particle size distribution of magnesium hydroxide has great effects on the subsequent filtration and drying processes. In this paper, micron-sized magnesium hydroxide with high purity, large particle size and low water content in filter cake was synthesized via simple wet precipitation in a mixed suspension mixed product removal (MSMPR) crystallizer. The effects of reactant concentration, residence time and impurities on the properties of magnesium hydroxide were investigated by X-Ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Malvern laser particle size analyzer. The results show that NaOH concentration and residence time have great effects on the water content and particle size of Mg(OH) . The spherical Mg(OH) with uniform diameter of about 30 μm was obtained with purity higher than 99% and water content less than 31%. Furthermore, the crystallization kinetics based on the population balance theory was studied to provide the theoretical data for industrial enlargement, and the simulation coefficients ( ) based on ASL model and C-R model are 0.9962 and 0.9972, respectively, indicating that the crystal growth rate of magnesium hydroxide can be well simulated by the size-dependent growth models.

关键词： magnesium hydroxide precipitation micron-sized crystallization kinetics

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Applications of the crystallization process in the pharmaceutical industry

Sohrab ROHANI

《化学科学与工程前沿（英文）》 2010年第4卷第1期页码 2-9 doi: 10.1007/s11705-009-0297-z

摘要： The applications of the crystallization technique in the pharmaceutical industry as a purification and separation process for the isolation and synthesis of pure active pharmaceutical ingredients (API), co-crystals, controlled release pulmonary drug delivery, and separation of chiral isomers are briefly discussed using a few case studies. The effect of process variables and solvent on the polymorphism and morphology of stavudine is discussed. The implementation of external control in the form of feedback and real-time optimal control using cooling and antisolvent crystallization of paracetamol in water-isopropyl alcohol is introduced. Two methods to prepare micron-sized drug particles, namely, micro-crystallization and polymer-coated API-loaded magnetic nanoparticles for pulmonary drug delivery, are discussed. The significance of co-crystals in drug administration is highlighted using the theophylline-nicotinamide co-crystal system. Resolution of chloromandelic acid derivatives, a racemic compound, is achieved using direct crystallization and diastereomeric salts crystallization. The crystal structures of diastereomeric salts of chloromandelic acid and phenylethylamine are determined. The structure comparison between the less soluble and more soluble salts shows that weak interactions such as CH/π interactions and van der Waals forces contribute to chiral recognition when the hydrogen bonding patterns are similar.

关键词： feedback morphology pulmonary paracetamol recognition

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Importance of emulsions in crystallization—applications for fat crystallization

Sandra PETERSEN, K. CHALEEPA, Joachim ULRICH

《化学科学与工程前沿（英文）》 2013年第7卷第1期页码 43-48 doi: 10.1007/s11705-013-1309-6

摘要： Emulsions and crystallization are two independent research topics which normally do not overlap although a combination of the two could be applicable to many areas. Here, the importance of emulsions in the field of fat crystallization is described. Three applications with industrial relevance were chosen for investigation: fat fractionation, the solidification of phase change materials and solid lipid nanoparticles. For fat fractionation and phase change materials, emulsification can be applied as a tool to improve the fat crystallization process, and thus the product quality of the crystallized fat. Furthermore, the use of emulsification creates new application fields such as solid lipid nanoparticles in the area of fat crystallization.

关键词： emulsion fat crystallization phase change material emulsion fractionation emulsion solidification