三乙醇胺月桂酸单酯的合成、表面活性及防雾性能

用等摩尔比的月桂酸和三乙醇胺为原材料合成了三乙醇胺月桂酸单酯,并对其酯化过程进行了优化,利用红外和核磁共振氢谱对其酯化产物进行了分析和表征．结果表明,三乙醇胺月桂酸单酯的产率高达69%,其在水溶液中的临界胶束浓度及表面张力分别为0.91 μg/mL和22.1 mN/m,其在低密度聚乙烯薄膜上的第一滴流滴时间和十滴流滴时间分别为257和86 s,高温持续期超150 h．     

丙烯酰氯改性木质素模型物制备丙烯酸单体及聚合活性分析

以木质素模型化合物二氢丁香酚(DH)为原料,利用丙烯酰氯(AC)进行接枝改性制备丙烯酸二氢丁香酚酯(DH-AC)。采用傅里叶变换红外光谱(FTIR)、气相色谱-质谱联用仪(GC-MS)、核磁共振氢谱(1H-NMR)和凝胶色谱(GPC)等分析手段研究了丙烯酸二氢丁香酚酯的结构以及聚合活性。FTIR结果表明二氢丁香酚经过丙烯酰氯改性后,3 495 cm-1为酚羟基伸缩振动吸收峰完全消失,在1 762 cm-1处有新的酯基峰生成,同时在1 631和981 cm-1出现CC的特征吸收峰,表明丙烯酸酯官能团已成功接枝到二氢丁香酚上。1H-NMR分析结果显示DH-AC在δ=5.6的酚羟基质子峰完全消失,同时在δ=6.0,6.4和6.7出现了三个不同的质子峰,这主要是由于乙烯基CHCH₂结构的引入,该结果进一步证明目标产物丙烯酸二氢丁香酚酯结构的正确性。GC-MS结果表明目标产物丙烯酸二氢丁香酚酯的纯度为98.63%。GPC结果显示DH-AC在偶氮二异丁氰(AIBN)作为引发剂的存在下,DH-AC可以发生聚合反应,均聚物相对分子质量结果为：Mw(37400),Mn(23400),Mw/Mn=1.60,表明丙烯酸二氢丁香酚酯单体具有高的聚合活性。丙烯酸二氢丁香酚酯(DH-AC)的制备和性能研究为开发新型木质素基高分子材料奠定了理论基础。     

FTIR跟踪研究不饱和氯代阻燃聚醚多元醇与亚磷酸酯阻燃剂的反应

采用FTIR技术跟踪研究了由乙二醇和环氧氯丙烷以及烯丙基缩水甘油醚共聚而成的不饱和氯代聚醚多元醇,与亚磷酸三甲酯发生酯交换反应和酯交换聚合反应以及Arbuzov重排反应过程,合成反应型聚醚多元醇亚磷酸酯阻燃剂的方法。实验考察了物质量配比、反应温度、投料方式等对上述反应进程的影响。分析结果表明反应温度是决定上述反应进程的关键因素,同时适当条件下合成的反应产物,可以用作一种光固化的兼有抗老化和增塑功能新型有机磷酸酯阻燃剂。     

乙酸2-辛基十二烷醇酯的合成及其谱学研究

本文以乙酸和2－辛基十二烷醇为原料，以磷钨酸为催化剂，合成了乙酸2－辛基十二烷醇酯，酯化率为92.0%，对产物进行了红外光谱分析及核磁共振波谱分析。     

新药阿德福韦酯的核磁共振研究

采用2D NMR技术对阿德福韦酯的氢谱和碳谱进行了全归属。对其结构进行确定，用于质量标准研究。     

FTIR研究半预聚物法聚氨酯脲密封材料固化过程的表观动力学及氢键化作用

采用原位FTIR技术跟踪了半预聚物法聚醚型聚氯酯脲的固化过程,研究了其固化过程的宏观动力学.原位FTIR的光谱数据表明,随着反应时间的增加.脲键羰基的吸收逐渐增强,脲羰基的波数位置呈阶跃式向低波数方向移动.脲键羰基的氢键化作用逐渐增强.不含催化剂时,硬段优先形成,不利于NCO与OH的反应.氨酯羰基的峰高增加缓慢.脲键的生成对NCO/OH反应生成氨酯键无催化作用.     

近红外光谱法测定不同产地独活中蛇床子素和二氢欧山芹醇当归酸酯含量

应用近红外光谱技术建立对独活中蛇床子素和二氢欧山芹醇当归酸酯的快速检测方法。自不同产地采集97批样品,通过高效液相色谱法测定指标成分含量,并测定样品的近红外光谱图,由于光谱图间差异较小,需要进行光谱预处理,通过比较不同预处理方法的结果,选择最优模型参数,结合偏最小二乘法分别建立独活中蛇床子素和二氢欧山芹醇当归酸酯的定量分析模型。结果显示,预处理方法为一阶导数时,蛇床子素的模型处于最优化性能,模型的相关系数为0.941 3,RMSEP值为0.141;校正集相关系数为0.923 3,RMSEC值为0.163。不经预处理的二氢欧山芹醇当归酸酯模型处于最优化性能,模型的相关系数为0.857 4,RMSEP值为0.103;校正集相关系数为0.831 5,RMSEC值为0.112。研究表明,近红外光谱技术结合偏最小二乘法操作简便,测定方法快速、高效、无损,可以实现对独活中蛇床子素和二氢欧山芹醇当归酸酯的含量进行定量分析,为中药材的质量控制研究和含量测定提供了一种科学有效的方法,同时为近红外光谱技术发展中药实时分析开辟了一个新方法,对保证中药材质量稳定可控有重要意义。     

植物甾醇乙酰化过程中高效液相色谱法的测定

应用高效液相色谱法对混合植物甾醇乙酰化过程的产物进行了测定。实验采用的色谱柱为 HypersilODS反相柱 (4 .6× 15 0 mm,5 μm) ,流动相为甲醇 ,紫外检测波长为 2 10 nm,恒溶剂洗脱的操作条件。实验结果表明 ,混合植物甾醇及其乙酸酯的响应时间小于 2 5 min,且各种甾醇及其酯的分离效果较好。采用该方法能够快速、准确地对植物甾醇酯化反应进行的程度及酯化产物含量进行测定。     

RAFT聚合制备聚丙烯酸钠

合成了RAFT试剂苄基三硫代碳酸酯基丙酸,并在其存在下,采用水溶液聚合法,对丙烯酸钠进行了RAFT聚合。通过核磁氢谱对苄基三硫代碳酸酯基丙酸的结构进行了鉴定,并采用GPC测定了聚丙烯酸钠分子量和分子量分布。     

β-(4-硝基酞酰亚胺基)丙酸酯的合成及其IR和1H-NMR研究

采用相转移催化法，以Michael加成反应合成了β-(4-硝基酞酰亚胺基)丙酸酯，并对产物进行了红外光谱及核磁共振氢谱分析。     

近红外光谱法检测聚醚多元醇伯羟基与仲羟基的相对含量

文章利用近红外光谱法,采用多元线性回归检测了聚醚多元醇的伯羟基与仲羟基的相对含量,得到了较好的预测结果,对工业在线检测具有重要的参考价值。     

Improvement in dispersion and ionic conductivity of polyether/freeze-dried clay composites using supercritical carbon dioxide as treatment medium

Addition of inorganic fillers to polyether-based electrolytes can lead to an increase in ionic conductivity, a reduction in the degree of crystallinity, and an increase in cation transport number. In order to enhance further conductivity of polyether/clay composites, a dispersion of ??nano-level?? clay in polyether is needed. In this study, we prepared polyether composite filled with freeze-dried clay, which may give a more dispersed state. In a previous study, we reported that supercritical carbon dioxide (scCO₂) treatment medium is an effective method for enhancing the conductivity of polyether/saponite (Sa) composites. Here, we prepared polyether/freeze-dried saponite (fSa) composites and treated them with scCO₂ and studied the effects of freeze-drying and scCO₂ treatment using wide-angle X-ray diffraction (WAXD), transmission electron microscopy (TEM), differential scanning calorimetry, and complex impedance measurements. The WAXD and TEM measurements revealed that the dispersion of Sa in polyether is caused by the freeze-drying pretreatment. Moreover, the combination of freeze-drying and scCO₂ treatment gave rise to homogeneous composites, leading to a significant increase in conductivity. The conductivity of the scCO₂-treated fSa composite was 100 times greater than that of the original Sa composite.     

红外光谱法测定聚醚硅油中含氢硅油的含量

以烷基酚聚氧乙烯醚(OP-10)和含氢硅油为原料,以辛酸亚锡为催化剂,甲苯作溶剂,采用溶液聚合的方法合成了一种新型聚醚硅油。用红外光谱法对合成样品中残留的含氢硅油进行定量分析,利用含氢硅油中Si—H键在2 167 cm-1处的吸收峰,选择司班-60作为内标物,以朗伯-比尔定律为理论依据,推导出样品和内标物的吸光度比(Y)与质量比(X)的线性关系式为Y=kX(k为常数),从而建立了直接红外光谱法测定聚醚硅油中含氢硅油含量的方法。实验测定内标工作曲线为Y=2.072 1X+0.296 3,相关系数r2=0.998 9,通过对方法重现性和回收率的测定,得到了较为满意的结果。该法是确定合成聚醚硅油产品的反应程度和控制产品质量的一种必要手段,同时为调整聚醚硅油的性能提供了依据;从而确定了最佳合成工艺路线及工艺条件。将合成的聚合物经处理后进行了应用实验,该聚合物对醇系和苯系化合物的萃取效果很好,具有广泛的应用前景。     

Crystallization Behavior of Modified Polyester with Varied Macromolecular Architecture

Several modified polyesters with varied macromolecular architecture, such as branched poly(ethylene terephthalate) (PET) based on glycerol (GL) from 0.004 to 0.05 mol ratio as a branching agent, blocked and branched poly(butylene terephthalate)‐polyether containing poly(tetramethylene oxide) (PTMO) as soft segment and GL as a branching unit, as well as segmented poly(ethylene terephthalate)‐polyether,were prepared. Their crystallization behavior was studied by differential scanning calorimetry (DSC), wide‐angle X‐ray diffraction (WAXD), and polarized optical microscopy (POM). It was found that a small extent of branching may enhance the crystallization of poly(ethylene terephthalate), while high degrees of branching (0.035–0.05) could block the development of crystallization. On the other hand, for even a small extent of incorporation of GL in the more flexible poly(butylene terephthalate)‐polyether chains, no enhanced crystallization was observed; blocking of crystallization from a branching defect may play the main role. The introduction of PTMO in poly(ethylene terephthalate) chains to a small degree facilitated the nucleation and speeded crystallization, but decreased the melting points of the polymers. A small number of nuclei and the greater induction time were found for branched PETs. The spherulities developed in branched PETs were larger and more perfect than those in PET due to less truncation of spherulites resulting from fewer nuclei, whereas the size of spherulities in poly(ethylene terephthalate)‐polyether became smaller with the increase of PTMO.     

Cu(Ⅱ)及Zn(Ⅱ)与直链醚席夫碱配合物的合成与表征

合成了两种直链醚席夫碱双水杨醛缩二甘醇二胺(SALDA)和双水杨醛缩四甘醇二胺(SALTTA)及其新配合物[Zn(SALDA)](NO₃)₂·4H₂O和[Cu₃(SALTTA)(NO₃)₄](NO₃)₂·3H₂O.并以IR谱、UV谱,特别是¹H和¹³C NMR谱等方法进行了表征,并详细地讨论了合成方法,IR谱表明SALTTA中醚氧并未全部配位.     

Continuous acid-catalyzed esterification using a 3D printed rotor–stator hydrodynamic cavitation reactor reduces free fatty acid content in mixed crude palm oil

Free fatty acid (FFA) content in FFA-rich mixed crude palm oil (MCPO) was reduced through a continuous esterification process. The reaction conditions were optimized, the yield purified esterified oil was determined, and the average total electricity consumption of the entire process was evaluated. The key component of this study was the cost-effective, 3D-printed rotor that was installed in a continuous rotor–stator hydrodynamic reactor. The surface of the rotor was designed with spherical holes where the center-to-center distance between them was fixed. Response surface methodology (RSM) using central composite design (CCD) was employed to analyze the design of experiments (DOE) and optimize FFA-content reduction. The optimized conditions were 17.7 vol% methanol, 2.9 vol% sulfuric acid, a 3000 rpm rotor speed, and surface holes measuring 4 mm in diameter and 6 mm in depth. The experimental results showed that the FFA content in MCPO was reduced from 11.456 to 1.028 wt% upon esterification under these optimal conditions. The maximum yield of esterified oil from the phase separation step was 96.07 vol%, and that of the purified esterified oil was 91.27 vol%. The average total energy consumed by this hydrodynamic cavitation reactor to produce this esterified oil was 0.0264 kW h/L. This 3D printed rotor–stator reactor is a promising, novel reactor technology for producing biodiesel from FFA-rich oils.     

Morphology and protonic conductivity of the polyurethanes with acid groups in the flexible segment

Thermal transitions, morphology and electric conductivity of polyurethanes that contain acid (COOH) groups bound to their polyether (poly(tetramethylene oxide)) chains and hard urethane segments of various length have been studied by means of calorimetry, wide- and small-angle X-ray scattering and a.c. conductivity in wide range of frequencies (0.1 Hz–1 MHz) and temperature (−100 to 100°C). It was shown that the polyurethanes are basically microphase-separated systems whose polyether-rich matrix contain from 20 to 25% of the hard urethane fragments. The protonic conductivity of the materials decreases with decreasing the polyether phase in the system.     

A novel sulfonated dendritic polymer as the acidic component in proton conducting membranes

The present study involves the synthesis of sulfonated poly(3-ethyl-3-(hydroxymethyl)oxetane), sPTMPO, by end-capping the hydroxy-groups in the PTMPO with 1,4-butane sultone. A series of the polymer with different degrees of substitution was investigated. Furthermore, the subsequent use of the sulfonated PTMPO as the acidic component in proton conducting membranes was explored. The membranes were prepared by either a) mixing the partly sulfonated PTMPO with hexamethoxymethyl melamine (HMMM) to form cross-links by ether formation between the methylol groups on HMMM and the remaining hydroxyl groups on the hyperbranched polyether or b) using the sulfonated polyether in conjunction with a pyridine functionalised polysulfone, PSU-pyridine, to produce acid–base blend membranes. Membrane properties such as proton conductivity, water uptake and mechanical properties are discussed.     

Enhancing the properties of wood through chemical modification with palmitoyl chloride

Hevea brassiliensis (rubber wood) was esterified with palmitoyl chloride, prepared from the reaction of palmitic acid with thionyl chloride. The weight gain of the wood increased with increasing reaction time and temperature, the esterified wood were evaluated for their photostability and dimensional stability. Fourier transform infrared spectroscopy (FTIR), solid-state cross-polarization/magic angle spinning ¹³C nuclear magnetic resonance spectroscopy (CP/MAS ¹³C NMR) were used to elucidate the characteristics of wood after esterification. The dimensional stability and photostability of the wood was improved by esterification. This is an important observation since chemical modification of wood with fatty acid chlorides has been found to induce thermo-plasticity into wood.