Degree of crosslinking and mechanical properties of crosslinked poly(vinyl alcohol) beads for use in solid-phase organic synthesis

The limited swellability in polar media of the commonly used polystyrene/divinylbenzene (PS-DVB) support materials for solid-phase organic synthesis has led to the development of novel, highly swellable hydrophilic gels designed for use in aqueous or polar media. Poly(vinyl alcohol) beads crosslinked with epichlorohydrin (PVA-EP) were prepared by a two-step inverse-suspension polymerization method. While it is known that the morphology of the resulting beads can be controlled by the ratio of EP versus PVA as well as by the pre-crosslinking time, the actual degree of crosslinking of the beads and their mechanical properties remain unknown. It is therefore the purpose of this study to evaluate the actual degree of crosslinking of beads prepared with different quantities of crosslinker in the feed by spectroscopic (Raman, nuclear magnetic resonance) and chemical (functional group loading) methods. The mechanical properties of these swollen PVA-EP beads will be evaluated by single-bead unconfined compression in solvents such as water, N,N-dimethylformamide (DMF), and tetrahydrofuran (THF) and compared to model PS-DVB beads commonly used for solid phase synthesis.     

窑炉用热电阻、热电偶智能温度测量板的设计

温度是影响陶瓷烧成质量的关键因素,介绍了一种适用于测量各种窑炉不同部位温度的智能温度测量板,由于该系统在不同的测温部位分别采用了热电阻和热电偶,克服了一般测温系统在连接不同的测温传感器需要更换不同的测温模板、成本高、使用不方便等不足,并具有适用性强、测温精度高等优点。     

利用ADCP回波强度估算河流悬移质含沙量的应用研究

通过简要介绍利用声学多普勒水流剖面仪(ADCP)回波强度估算悬移质含沙量的基本原理,结合梧州水文站的应用实例,利用ADCP的回波强度数据和现场采集的水样含沙量建立相关关系,根据相关关系由回波强度反演估算的水体悬移质含沙量验证了利用ADCP的回波强度估算悬移质含沙量的可行性。应用于梧州水文站的实践表明,左河道推算的系统误差为-0.1%,右河道推算的系统误差为1.5%。这种方法具有不扰动流场、测量剖面同步性较好、数据空间分辨率较高的优点,与传统的取样过滤称量法相比,计算效率显著提高。     

PMMA‐modified divinylester/styrene resins: Phase diagrams and morphologies

Binary and ternary experimental cloud‐point curves (CPCs) for systems formulated with a low molar mass synthesized divinylester (DVE) resin, styrene (St), and poly(methyl methacrylate) (PMMA) were determined. The CPCs results were analyzed with the Flory–Huggins (F‐H) thermodynamic model taking into account the polydispersity of the DVE and PMMA components, to calculate the different binary interaction parameters and their temperature dependences. The St‐DVE system is miscible in all the composition range and down to the crystallization temperature of the St; therefore, the interaction parameter expression reported for a higher molar mass DVE was adapted. The interaction parameters obtained were used to calculate the phase diagrams of the St‐PMMA and the DVE‐PMMA binary systems and that of the St‐DVE‐PMMA ternary system at three different temperatures. Quasiternary phase diagrams show liquid–liquid partial miscibility of the St‐PMMA and DVE‐PMMA pairs. At room temperature, the St‐DVE‐PMMA system is miscible at all compositions. Final morphologies of PMMA‐modified cured St‐DVE materials were generated by polymerization‐induced phase separation (PIPS) mechanism from initial homogeneous mixtures. SEM and TEM micrographs were obtained to analyze the generated final morphologies, which showed a direct correlation with the initial miscibility of the system. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 4539–4549, 2006     

相转移催化法合成多聚乙二醇二环氧甘油醚

以多聚乙二醇和环氧氯丙烷为原料合成了多聚乙二醇二环氧甘油醚。NaOH为催化剂,季铵盐为相转移催化剂。结论为:作为催化剂NaOH固体效果优于NaOH溶液;四正丁基硫酸氢铵(TBAS)催化醚化反应效果最佳,GC监测表明,二醚的选择性达98％以上;n(多聚乙二醇):n(环氧氯丙烷):n(NaOH):n(TBAS)= 1:10:7:0．08;反应温度55-60℃;反应时间1．5 h;产率83％。     

Proposal of a uniform color scale for virgin olive oils

A new color scale was developed from a broad data set of 1700 virgin olive oil samples over four crop seasons, which can be considered highly representative of the whole color range of virgin olive oils available in Spain. This color scale provides a new set of 60 color standards, improving the results achieved by the old 60-color standards proposed by the bromthymol blue method. Seeking the greatest possibility of including a near match between colors of virgin olive oils and proposed standards, we developed our new color scale using a recent uniform color space, with standards placed in a regular rhombohedral lattice like the one employed by the Uniform Color Scales of the Optical Society of America. The average color difference between each of the 1700 virgin olive oils and its nearest standard is reduced from 8.17 CIELAB units, using the bromthymol blue standards, to 3.99 CIELAB units using the new standards. Within a color tolerance of 7.0 CIELAB units, 93.2% of our virgin olive oils can be classified with the new standards, but only 59.1% with the bromthymol blue ones. In the interest of future adoption, the performance of the new color standards should be tested by industry and researchers.     

美国能源部的浆态床F－T合成技术

浆态床Ｆ－Ｔ合成技术是美国能源部Ｆ－Ｔ合成技术的主要开发项目。本文就浆态相Ｆ－Ｔ合成催化剂的开发、中试示范实验和浆态反应器的化工基础研究作一扼要的介绍。     

Liquid-phase stereoselective thymol hydrogenation over supported nickel catalysts

The stereoselective hydrogenation of thymol was studied in liquid phase over several nickel catalysts, modified by coimpregnation of inorganic compounds containing chlorine. The total activity of all catalysts studied was decreased and was on the same order of magnitude, indicating that chlorine even after reduction remains on the surface and is responsible for the poisoning effects. Such blocking of accessible sites results in similar reaction rates for the catalysts studied. Selectivity and stereoselectivity to menthols and menthones changed significantly. The modifiers could influence the rate of keto-enol transformations, which is thought to be the key selectivity and stereoselectivity governing step.     

Preparations and properties of thermosensitive terpolymers of N‐isopropylacrylamide,sodium 2‐acrylamido‐2‐methyl‐propanesuphonate,and N‐tert‐butylacrylamide

Terpolymers based on N‐isopropylacrylamide, sodium 2‐acrylamido‐2‐methyl‐propanesulfonate, and N‐tert‐butylacrylamide were synthesized by free‐radical copolymerization with 2,2′‐azobisisobutyronitrile as an initiator. The lower critical solution temperatures (LCSTs) of the linear polymer aqueous solutions were determined by the measurement of the transmittance on UV at different temperatures. The influence of the polymer concentration, polymer composition, and ionic strength on the LCSTs of the linear polymers was investigated. The LCST decreased with increases in the hydrophobic monomer N‐tert‐butylacrylamide, polymer concentration, and ionic strength. The phase transition became sharp when the polymer concentration and ionic strength increased. Meanwhile, the crosslinked hydrogels were prepared with the same recipe used for the linear terpolymers, but a crosslinker was added to the reaction system. The swelling ratios of the hydrogels at various temperatures and salt solutions were determined. The hydrogels possessed both high swelling ratios and thermosensitivity. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007