Combination of nuclear magnetic resonance spectroscopy and nonlinear methods to analyze the copolymerization of phosphonic acid derivatives

We demonstrate in this study that the combination of modern inline monitoring methods [here: inline nuclear magnetic resonance (NMR)] with simulations gains more exact and profound kinetic results than previously used methods like linearization without that combination. The ¹H-NMR spectroscopic data (more than 100 data points) are used to construct the copolymerization diagram. The reactivity ratios are obtained applying the van Herks nonlinear least square method. The examination of the radical copolymerization of 2-hydroxyethyl methacrylate (HEMA) with (2-{[2-(ethoxycarbonyl)prop-2-en-1-yl]oxy}ethyl) phosphonic acid (ECPPA) as important adhesive monomer used in dentistry yields reactivity ratios of r_HEMA = 1.83; r_ECPPA = 0.42. The copolymerization diagram reflects nonideal, non-azeotropic copolymerization. The sequence distribution of the obtained by Monte Carlo simulation indicates the generation of statistical copolymers. As an important finding, it is demonstrated that the repeating units responsible for etching and adhesion are arranged over the whole polymer chain, which is necessary to achieve proper functionality. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 48256.     

Aqueous One-pot Synthesis of Glycopolymers by Glycosidase-catalyzed Glycomonomer Synthesis Using 4,6-Dimetoxy Triazinyl Glycoside Followed by Radical Polymerization

Glycopolymers have attracted increased attention as functional polymeric materials, and simple methods for synthesizing glycopolymers remain needed. This paper reports the aqueous one-pot and chemoenzymatic synthesis of four types of glycopolymers via two reactions: the β-galactosidase-catalyzed glycomonomer synthesis using 4,6-dimetoxy triazinyl β-D-galactopyranoside and hydroxy group-containing (meth)acrylamide and (meth)acrylate derivatives as the activated glycosyl donor substrate and as the glycomonomer precursors, respectively, followed by radical copolymerization of the resulting glycomonomer and excess glycomonomer precursor without isolating the glycomonomers. The resulting glycopolymers bearing galactose moieties exhibited specific and strong interactions with the lectin peanut agglutinin as glycoclusters.     

从7-ADCA生产过程中环境友好的回收苯乙酸

采用新工艺回收7-氨基-3-脱乙酰氧基头孢烷酸(7-ADCA)生产中产生的苯乙酸,并对苯乙酸回收过程中产生的废硫酸进行处理。采用硫酸(9 8%)洗涤二氯甲烷,硫酸与二氯甲烷适宜的体积比为1∶50,洗涤好的二氯甲烷中含苯乙酸4%。蒸馏出二氯甲烷,趁热向熔融苯乙酸中加入母液,降温析出苯乙酸。晾干的苯乙酸为白色鳞片状,含量大于99%,苯乙酸母液补充部分清水套用到下一批析出苯乙酸。废浓硫酸用芬顿试剂氧化,控制80℃氧化4h,双氧水和七水硫酸亚铁重量比为6∶1,废浓硫酸COD下降85%以上。氧化结束后向废硫酸中加入铁粉和双氧水,制得聚合硫酸铁。     

含锌离子的聚硅硫酸铝的合成及性能研究

采用一步法制备聚硅硫酸铝絮凝剂合成了含锌离子的聚硅硫酸铝并研究了其性能.含锌离子絮凝剂是一种无毒高效的絮凝剂,且絮凝效果优良,锌离子含量对絮凝剂性能影响很大.     

草酸钙在硫酸软骨素自组装膜上周期沉淀的研究

利用硫酸软骨素(chondroitin sulfate，CS)在云母基底上通过浇铸法制备的自组装膜为基底，诱导草酸钙在其上的凝集生长。发现当硫酸软骨素的浓度为1．Omg／ml时在该膜体系中可形成规整的周期性草酸钙环状沉淀。这种有序的环状结构可能是耗散结构的一种具体表现形式。利用原子力显微镜(atomic forcemicroscope，AFM)和傅立叶红外光谱仪对这种结构进行了表征，实验结果显示合适浓度下形成的CS膜在一定程度上可以抑制草酸钙的凝集结晶，表明高分子基质与无机离子间强烈的相互作用对无机盐的成核结晶有显著影响，为探讨结石的形成与抑制提供了一定的实验依据。     

石膏转化制硫酸钾结晶动力学及结晶添加剂研究

研究了浓氨介质中石膏与氯化钾直接转化制硫酸钾的结晶动力学及结晶添加剂的作用效果。结果表明 ,硫酸钾在氨介质中的成核速率与晶体生长速率、悬浮密度、搅拌速率存在如下关联式 :B0 =5 .64 13×10 8G3.32 0 8Mt0 .0 559np0 .2 92 8。加入异丙醇、OP乳化剂及十二烷基苯磺酸钠等添加剂 ,可使硫酸钾结晶产品纯度提高 ,晶体形态整齐均匀     

碳黑对苯乙烯自由基聚合反应影响的研究

研究了碳黑对苯乙烯单体聚合物反应的影响，结果表明，用过氧化苯甲酰作引发剂，普通碳黑子对苯乙烯的聚合有强烈的阻聚作用，而用偶氮二异丁腈引发聚合物时，普通碳黑的阻聚性很小，当时碳黑进行接枝处理后，接枝碳黑对苯乙烯自由基聚合的影响程度与接枝方法有关，其中过氧化苯甲酰 自由基枝枝碳黑的聚性变化较大。     

十二酰胺丙基二甲基羟乙基氯化铵与十二烷基硫酸钠水溶液的表面吸附和胶束形成

利用十二酰胺丙基二甲胺和氯乙醇反应 ,合成了十二酰胺丙基二甲基羟乙基氯化铵 (DDHA)阳离子表面活性剂 ,将其与十二烷基硫酸钠 (SDS)以不同摩尔比进行混合 ,测定了混合系统的表面张力 ,计算了单一系统和混合系统的饱和吸附量、分子最小截面积 ,表面层和胶束中 DDHA的摩尔分率及分子间相互作用参数 ,目视观察了混合系统的浑浊情况。结果表明 :在降低γcmc和 cmc方面 ,DDHA SDS混合系统有协同效应 ,表面层和胶束的组成与二组分配比有关 ,但是非对称的 ,等物质的量混合物中 ,DDHA在胶束和表面层中具有较大的摩尔分数。DDHA与 SDS在实验测定的各混合系统中都不出现混浊     

用硫酸铁铵容量法测定钛精矿中二氧化钛含量

样品在过氧化钠熔融、水浸取及盐酸酸化后，在盐酸和硫酸介质中，隔绝空气，用金属铝将钛(Ⅳ)还原至钛(Ⅲ)，以硫氰酸盐为指示剂，用硫酸铁铵标准溶液滴定。     

High char‐yielding poly[acrylonitrile‐co‐(itaconic acid)‐co‐(methyl acrylate)]: synthesis and properties

Polyacrylonitrile terpolymers of various compositions consisting of acrylonitrile (AN), itaconic acid (IA) and methyl acrylate (MA) were synthesized by solution polymerization in dimethylsulfoxide. Increase in concentration of either IA or MA retarded the overall polymerization rate and the polymer molecular weight. The system consisting of AN + MA and varying IA concentration was more prone to retardation in comparison with the system composed of AN + IA with variable MA concentration. The retardation factors were quantified. Minor quantities of MA boost the reactivity of IA in the terpolymer system. The terpolymer was richer in MA vis‐à‐vis the feed. The thermal characteristics of the terpolymer were examined as a function of its composition. In contrast to the copolymer of AN and IA requiring 1–1.5 mol% IA, the terpolymer required an IA content of approximately 2.5 mol% for optimum thermal stability. The polymer with 90 mol% AN, 2.5 mol% IA and 7.5 mol% MA exhibited reasonably good char‐forming characteristics and thermal stability. The overall crystallinity and crystallite size of the polymers were found to decrease on incorporation of the comonomers. The ‘aromatization index’ of the copolymer increased with the temperature of pyrolysis through re‐organization of the tetrahydropyridine ladder structure. Copyright © 2005 Society of Chemical Industry