含环三硅氮烷的星形聚硅氧烷的合成——环硅氮阴离子引发环硅氧烷开环聚合

以环三硅氮锂盐（ＤＮＬｉ３）为引发剂，成功地引发了环硅氧烷开环聚合．通过含氮量测定，利用１Ｈ、２９ＳｉＮＭＲ和ＩＲ谱以及分子量测定（ＧＰＣ）和特性粘度测试，并与模型化合物进行比较，证明所得聚合物是含环三硅氮烷的星形聚硅氧烷．研究了六甲基环三硅氮锂盐引发八甲基环四硅氧烷（Ｄ４）开环聚合的动力学，结果表明该聚合反应相对于Ｄ４为一级反应，同时也比较了不同促进剂对聚合速率的影响，ＤＭＦ对聚合速率的促进作用比ｄｉｇｌｙｍｅ大     

含硅芳香二胺的合成及其聚酰亚胺硅氧烷的热性能

从ｐ－或ｍ－氯苯胺出发，经三步反应合咸位置弄构的四甲基［双（苯胺）］二硅氧烷和六甲基［双（苯胺）］三硅二氧烷，总产率为２５％．与芳香二胺和芳香四酸二酐共聚得聚酰亚胶硅氧烷．研究了共聚物在玻璃化转变区的热松弛行为．对位异构体的共聚物，其分子链段的构象熵大，运动较易．     

气相色谱法测定油脂中棕榈酸单甘油酯与油酸单甘油酯含量

建立了一种利用气相色谱法测定油脂中棕榈酸单甘油酯与油酸单甘油酯含量的方法。样品中加入六甲基二硅氨烷,于９５℃水浴中完成硅烷化反应。样品的平均加标回收率分别为９６．３０％与９７．８２％,ＲＳＤ分别为１．８％与２．１％。最低检出限分别为０．０１μｇ／ｇ与０．１μｇ／ｇ。     

邻苯二甲醛柱前衍生反相高效液相色谱法测定人和小鼠血浆中的游 …

以邻苯二甲醛（ＯＰＡ）３－巯基丙酸（３－ＭＰＡ）为衍生试剂，手动柱前衍生，ＯＤＳ（十八基哇烷）柱分离；以磷酸盐缓冲液（ＰＨ７．２）配制流动相，二元一级性梯度洗脱，紫外３４０ｎｍ检测，在４０ｍｉｎ内分离测定了人和小鼠血浆中２１种游离氨基酸的含量。方法准确可靠。２１种氨基酸保留时间和峰面积的相对标准偏差分别为０．０９－０．３８％和１．５－４．９％，氨基酸的进样量为０．１－１．６ｎｍｏｌ时，峰面积与进样     

气相色谱法分析聚酯中多元醇

用气相色谱法分析聚酯中多元醇,通常是用正丁胺降解聚酯,使生成的多元醇转变为乙酸酯或三甲基硅醚的衍生物后,再进行色谱分析。最近,Mlejnek和Cveckova提出用水合肼降解聚酯,以六甲基二硅胺烷和三氟醋酸为硅烷化试剂,将多元醇转变为硅烷化衍生物,但未给出定量结果。我们参照此法,用六甲基二硅胺烷和三甲基氯硅烷为硅烷化试剂对聚酯中多元醇进行定量分析,并将其扩大应用于聚酯聚氨酯中多元醇的分析。     

6—硫杂—13—氮杂二环（9.3.0）—3,8—二炔十四烷的合成及核磁共振鉴定

以３，４－二（４′－甲磺酰氧－２′－丁炔基）四氢呋喃或６－硫杂－３，８－二炔－１，１１－二羟甲基环十一烷为原料合成了二环化合物６－硫杂－１３－氧杂二环（９．３．０）－３，８－二炔十四烷，通过＾１ＨＮＭＲ＾１３ＣＮＭＲ，ＩＲ及ＭＳ进行结构鉴定。     

1-酰氧(胺)-2,8,9-三氧杂-5-氮杂-1-锡杂三环[3.3.3.01.5]十一烷的合成和结构研究

合成了１４个新化合物：１－酰氧（胺）基－２，８，９－三氧杂－５－氮杂－１－锡杂三环［３．３．３．０１．５］十一烷．由ＩＲ、１ＨＮＭＲ、１３ＣＮＭＲ和１１９ＳｎＮＭＲ及元素分析确定其结构．该类化合物在ＣＤＣｌ３中可能形成六配位化合物，而在ＤＭＳＯ中，溶剂分子参与Ｓｎ原子配位，聚合体解聚为六配位化合物．     

气相色谱法同时测定初烤烟叶中的4种水溶性糖

建立了一种用三甲基氯硅烷及六甲基二硅胺烷衍生化,气相色谱-氢火焰离子化检测器同时测定初烤烟叶中4种水溶性糖的检测方法。烟叶样品用50%(V/V)的乙腈溶液振荡提取,无需净化,直接用三甲基氯硅烷及六甲基二硅胺烷衍生化,产物通过微型液-液萃取净化后用气相色谱检测。通过优化前处理条件和讨论基质效应,果糖、葡萄糖、蔗糖和麦芽糖的含量均与其峰面积呈良好的线性关系(相关系数为0.9991～0.9999),添加回收率为98.14%～102.45%,重复性较好(RSD<2.2%),该方法适用于初烤烟叶中果糖、葡萄糖、蔗糖和麦芽糖的同时测定。     

6-硫杂-13-氧杂二环[9.3.0]-3,8-二炔十四烷的合成及核磁共振鉴定

以３，４－二（４′－甲磺酰氧－２′－丁炔基）四氢呋喃或６－硫杂－３，８－二炔－１，１１－二羟甲基环十一烷为原料合成了二环化合物６－硫杂－１３－氧杂二环［９．３．０］－３，８－二炔十四烷。通过１ＨＮＭＲ，１３ＣＮＭＲ，ＩＲ及ＭＳ进行了结构鉴定。     

用~（31）P－NMR和IR谱研究MoDTP合成产物组分及反应机理

用~（３１）Ｐ核磁共振（ＮＭＲ）谱和红外（ＩＲ）光谱研究了二硫代磷酸钼（ＭｏＤＴＰ）合成产物组分含量、分子结构及其合成反应机理。结果表明，ＭｏＤＴＰ合成产物是由３７．２％的有机五价钼络合物、３５．１％的有机Ｐ＝Ｓ化合物和２７．７％的有机Ｐ＝Ｏ化合物等１４种成分组成，所含副产物或由原料带入，或因ＭｏＤＴＰ合成反应过程原料本身副反应伴随产生。     

基于自组装溶胶凝胶法无机Janus纳米片的制备及其乳化性能研究

论文首先采用水解苯乙烯-马来酸酐共聚物为乳化剂,正硅酸乙酯、亲油性硅烷偶联剂和亲水性硅烷偶联剂三种前驱体溶于石蜡做为油相(分散相),水为连续相,乳化分散后通过溶胶凝胶法,制备得到了表面亲水/内部亲油的核壳实心微球;然后超声清洗除去石蜡后得到了表面亲水/内部亲油的二氧化硅空心球,将其破碎后即得到了无机Janus纳米片.实...     

Synthesis and characterization of quinoline-derivated fluorescent sol–gel-imprinted polymer as a chemosensor for sensing of uranyl ion

Journal of Sol-Gel Science and Technology - In this work, chemosensor that contains 3-aminoquinoline derivative of silane coupling agent grafted to the sol–gel polymer has been synthesized...     

MORPHOLOGY AND PROPERTIES OF LINEAR LOW-DENSITY POLYETHYLENE HIGHLY LOADED WITH ALUMINUM HYDROXIDE

An experimental study was carried out to investigate the effects of isopropoxy tri(dioctyl pyrophosphoryl) titanatecoupling agent on the mechanical performance, rheological property and microstructures of polyethylene highly loaded withaluminum hydroxide (Al(OH)_3) composite. It was found that the addition of coupling agent results in reduced tensile strengthand increased percentage elongation of the filled systems. Silane crosslinkable polyethylene substituting for polyethylene asmatrix improves the tensile strength of the composite, while the percentage elongation of the composite still remains at adesired level. Melt viscosity of the composite will be improved by addition of titanate coupling agent. Microstructures of thecomposites were also studied by means of the scanning electron microscopy (SEM) technique. SEM micrographs reveal thatfiner dispersion of Al(OH)_3 will be obtained upon treatment of titanate and a transition from brittle to tough fracture takesplace before and after silane crosslinking structure is introduced into polyethylene highly filled with Al(OH)_3 composite.     

Synthesis and lectin-binding activity of luminescent silica particles peripherally functionalized with lactose

A novel O-protected lactose (Galβ1→4Glcβ1-) derivative bearing trimethoxysilyl group at the aglycon was developed as a silane coupling agent. Reaction of the coupling agent with tris(2,2′-bipyridine)ruthenium (II) dichloride (Rubpy) doped silica particle gave a Rubpy-doped silica particle peripherally functionalized with O-protected lactose derivative. De-O-protection of the particle with aqueous ammonia provided lactose-coating Rubpy-doped silica particles, combining luminophor encapsulated in silica matrix and carbohydrate having lectin-recognition ability. Specific adhesion of fluorescein isothiocyanate-labeled peanut agglutinin (FITC-PNA) to the lactose-coating Rubpy-doped silica particles was confirmed by fluorescence microscopic analysis.     

Effect of different preparation methods on mechanical behaviors of carbon fiber-reinforced PEEK-Titanium hybrid laminates

This paper aims to investigate the mechanical behaviors of carbon fiber-reinforced PEEK-Titanium hybrid laminates (TiGr) prepared by different surface treatment conditions using silane coupling agent. In order to improve the bonding performance between the titanium sheets and PEEK, the titanium layers were subjected to sandblasting roughening and silanization treatment, the curing process was explored by setting different concentrations of silane coupling agent, curing temperatures and curing times. The optimum parameters of the process were determined by analyzing the mechanical properties of the laminates, which are 10% of SCA concentration, 130 °C of curing temperature and 1 h of curing time, and the corresponding tensile, bending and inter-laminar shearing strengths are 837, 1071 and 75 MPa, respectively. The surface composition, structures and chemical bonding of the modified titanium sheet were analyzed through Scanning Electronic Microscope (SEM), Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). It was evidenced that the optimal process could produce a relatively complete and uniformed silane film compared to other cases. In addition, the results show that the Si–O–Ti covalent bonds were formed, which demonstrated that the preparation of the laminates through silane coupling agent is reliable.     

表面改性对片状锌粉分散稳定性的影响

采用物理化学法,将实验室自制锌粉分别添加钛酸酯偶联剂、硅烷偶联剂和十二烷基苯磺酸钠进行表面改性,利用沉降法测试高度研究改性前后锌粉的分散稳定性。 结果表明,不同种类、不同浓度的表面改性剂对锌粉的分散稳定性有较大的影响;其中,经1.0%钛酸酯偶联剂改性后锌粉的分散稳定性有了明显的改善,与进口粉的分散稳定性接近。     

硅烷偶联剂制备及对磷灰石-硅灰石生物玻璃陶瓷的表面改性

采用谷氨酸与硅烷偶联剂(KH-792)缩合反应,制备出一种含酰胺基的硅烷偶联剂,利用其与材料之间的化学结合,将谷氨酸共价固定至磷灰石-硅灰石生物玻璃陶瓷表面,实现表面改性。将改性后的磷灰石-硅灰石生物玻璃陶瓷与人骨肉瘤细胞MG63共培养,评价其体外细胞生物相容性。应用FTIR、SEM、XPS等测试技术分别对合成的偶联剂、改性后的陶瓷材料进行结构、表面形貌及细胞生长情况的表征,结果表明:谷氨酸与KH-792的反应产物有酰胺基生成;含酰胺基的硅烷偶联剂能对磷灰石-硅灰石生物玻璃陶瓷表面进行有效改性;共培养3 d后细胞在材料材料表面大量贴附,MTT实验也证明增殖良好,即含酰胺基的硅烷偶联剂能改善磷灰石-硅灰石生物玻璃陶瓷的体外细胞生物相容性。     

Effect of silane coupling agent on mechanical interfacial properties of glass fiber‐reinforced unsaturated polyester composites

A silane coupling agent, γ‐methacryloxypropyltrimethoxysilane, for the surface modification of glass fibers was varied between 0.1 and 0.8 wt %. To understand the role of interfacial adhesion of glass fiber/unsaturated polyester composites, contact angles of the silane‐treated glass fibers were measured by the wicking method on the basis of the modified Washburn equation with deionized water, diiodomethane, and ethylene glycol as testing liquids. As a result, silane‐treated glass fibers led to increased surface free energy, mainly because of their increased specific or polar component. The mechanical interfacial behaviors based on the interlaminar shear strength (ILSS) of the composites determined by short‐beam tests and the critical stress‐intensity factor (K_IC) were also improved in the case of silane‐treated composites. The surface free energy and the mechanical interfacial properties especially showed the maximum value in the presence of 0.4 wt % silane coupling agent. It revealed that the increase of a specific component of the surface free energy or hydrogen bonding between the glass fibers and the coupling agents plays an important role in improving the degree of adhesion at interfaces in a composite system. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 41: 55–62, 2003     

同时测定合成样中铜钴镍钒含量的分光光度法--主成分回归法和偏最小二乘法比较

研究了主成分回归和偏最小二乘方法在多组分分光光度法分析中的应用,以５－Ｂｒ－ＰＡＤＡＰ（２〔５－溴－２－吡啶）－偶氮〕５－二乙氨基苯酚）为显色剂,ＯＰ（聚乙二醇辛基苯基醚）作为增溶增稳剂,在ｐＨ＝３．６的条件下,用主成分回归及偏最小二乘分光光度法同时测定了合成样中的铜、钴、镍、钒４组分含量,测定相对误差在－６．００％～４．００％之间。实验证明,对于加和性不好的体系偏最小二乘分光光度法要优于主成分回     

硅烷偶联剂对SSBR/SiO_2混炼胶体系动态流变行为的影响

研究了高填充白炭黑(SiO2)补强溶液聚合丁苯橡胶(SSBR)混炼胶体系的动态流变特性,分别考察了在2个混炼温度(120℃、160℃)下添加3种不同偶联剂(TESPT、TESPD、NXT)对其体系中SiO2粒子表面改性的效果.结果表明,在较低混炼温度下添加偶联剂,不利于SiO2粒子表面改性.在较高混炼温度下,偶联剂TESPT、PESPD、NXT均对SiO2粒子表面有改性效果,但同时引起混炼胶不同程度的焦烧,其中以TESPT最明显.随SiO2粒子表面改性程度的提高,出现“Payne效应”的临界应变(γc)值以及低频率(ω)区域lgG′-lgω曲线的斜率值均增大,反映出偶联剂对SiO2与SSBR相互作用的促进以及SiO2粒子分散的改善.