2-甲基-4-羟基-6-苯基嘧啶和2-甲基-4-羟基-5-溴-6-苯基嘧啶的高效液相色谱法分离测定

采用ODS-C18色谱柱和紫外检测器,对2-甲基-4-羟基-6-苯基嘧啶和2-甲基-4-羟基-5-溴-6-苯基嘧啶的含量进行HPLC分离测定.以甲醇水=4555为流动相,紫外检测波长为237 nm,样品线性范围为0.001～0.1 mg/mL.2-甲基-4-羟基-6-苯基嘧啶的RSD为0.5%;2-甲基-4-羟基-5-溴-6-苯基嘧啶的RSD为1.0%.     

2-甲氧基-3-氟-4-碘吡啶的合成

2-甲氧基-3-氟-4-碘吡啶是一个重要的医药化工中间体,其合成路线未见文献报道。以2-甲氧基-3-氟-5-氯吡啶为起始原料,经氢解和碘代两步反应合成标题化合物,总收率62.8%,其结构经¹H NMR, ¹³C NMR和MS确证。     

稳定烯醇结构3-氯-2-羟基-4-羰基-4-对甲苯基-2-丁烯酸乙酯的合成

以甲苯为起始原料,通过傅克-酰基化、Aldol反应合成了具有稳定烯醇结构的3-氯-2-羟基-4-羰基-4-对甲苯基-2-丁烯酸乙酯,反应过程生成了中间体3,3-二氯-2-羟基-4-羰基-4-对甲苯基丁酸乙酯,采用红外、核磁共振谱、HRMS产品进行了测定和结构表征。对反应机理进行了初步探讨。     

卤代-2-(3-甲基-5-取代-4H-1,2,4-三唑-4-基)-苯甲酸的合成

邻氮基苯甲酸;缩合反应;卤代-2-(3-甲基-5-取代-4H-1;2;4-三唑-4-基)-苯甲酸的合成     

1-(2-吡啶基)-2-氮杂-1,3-丁二烯的合成与应用

以2-吡啶甲醛为起始原料制备1-(2-吡啶基)-2-氮杂-1,3-丁二烯(2),然后与烯烃、炔烃发生Diels-Alder反应分别得到6-(2-吡啶基)-2-哌啶酮和6-(2-吡啶基)-二氢-2-吡啶酮.用2,3-二氯-5,6-二氰基-1,4-苯醌(DDQ)氧化6-(2-吡啶基)-二氢-2-吡啶酮得到6-(2-吡啶基)-2-吡啶酮,最后用三氯氧磷处理得到联吡啶类化合物.     

2-烷基氨基-3-芳基-5-苄基-1-咪唑啉-4-酮的合成及杀菌活性

咪唑啉酮衍生物;反应;2-烷基氨基-3-芳基-5-苄基-1-咪唑啉-4-酮的合成及杀菌活性     

4-甲基-苯磺酸-2-氧-2-[3-(5-芳基-[1,3,4]噁二唑-2-基)-硫脲]-乙基酯的合成及生物活性研究

合成了12个未见文献报道的4-甲基-苯磺酸2-氧-2-[3-(5-芳基-[1,3,4]噁二唑-2-基)-硫脲]-乙基酯, 其结构经元素分析、¹H NMR和IR确证. 初步活性测试结果表明: 部分化合物有较好的杀菌活性.     

1,5-二-(3-硝基苯基)-1,4-戊二烯-3-酮的超声合成

1;5-二-(3-硝基苯基)-1;4-戊二烯-3-酮的超声合成;二-（硝基苯基）-戊二烯-酮;合成;超声;催化     

3-甲基-2-戊烯-4-炔醛的合成新方法

化合物3-甲基-2-戊烯-4-炔-1-醛两端均为活性官能团,在分子连接及成环反应中能够起到非常重要的作用,是合成轮烯酮[1-7],脱落酸[8]和二苯基二苯并环辛烯[9]等的重要中间体.     

1-(4-取代苯基)-4-苯基-5-(2-羟基苄基)氨基-1,2,3-三唑类衍生物的合成及抑菌活性

将邻羟苯基引入1,2,3-三唑结构中, 设计合成了10个1-(4-取代苯基)-4-苯基-5-取代-1,2,3-三唑类衍生物. 首先, 以对位取代的芳胺为原料, 经重氮化、叠氮化、闭环和缩合反应制得1-(4-取代苯基)-4-苯基-5-水杨醛亚胺-1,2,3-三唑类衍生物(3a~3e), 再用硼氢化钠还原制得1-(4-取代苯基)-4-苯基-5-(2-羟基苄基)氨基-1,2,3-三唑类衍生物(4a~4e). 目标化合物的结构经核磁、IR及元素分析确认. 抑菌活性测试表明, 当质量浓度为0.1 mg/L时, 除化合物3e和4e外, 所有化合物对白色念球菌的抑菌率均达95%以上, 对大肠杆菌的抑菌率达85%以上, 具有强抑菌活性, 表明该类化合物在抗菌药物开发方面有重要应用价值.     

Synthesis of Fullerene-Acrylamide Copolymer Nanoball and Its Lubrication Properties

A novel fuUerene-acrylamide copolymer was synthesized via radical polymerization. It is soluble in polar solvents such as water, dimethyl sulfoxide etc. The product was characterized by FTIR, UV-Vis and GPC. TEM analysis shows that the average particle diameter is about 46 nm. Four-ball tests show that the addition of a certain concentration of the fullerene copolymer to base stock (2 wt% triethanolamine and 0.5 wt% OPZ aqueous solution) can effectively raise the load-carrying capacity (PB value) and the antiwear ability. SEM analysis shows that the addition results in reducing diameter of wear scar and decreasing wear.     

富勒烯-苯乙烯-顺丁烯二酸酐三元共聚物的摩擦学行为

水溶性;纳米微球;摩擦学性能;富勒烯-苯乙烯-顺丁烯二酸酐三元共聚物的摩擦学行为     

C60-丙烯酸月桂酯共聚物的合成及其摩擦学行为

合成了一种新颖的油溶性C60-丙烯酸月桂酯共聚物,采用四球摩擦磨损试验机、扫描电子电镜研究了其作为液体石蜡润滑添加剂的摩擦学特性,结果表明,C60-丙烯酸月桂酯共聚物可提高石蜡基础液的抗磨性能,改善微观磨损状态.     

PDEA和P(DEA-co-NHMAA)稀水溶液相分离行为研究

运用紫外-可见分光光度法分别考察了聚N,N-二乙基丙烯酰胺(PDEA)和N-羟甲基丙烯酰胺(NHMAA)与DEA的共聚物P(DEA-co-NHMAA)稀水溶液相分离行为. 结果发现，当P(DEA-co-NHMAA)中NHMAA的质量分数小于5.25%时, 随着NHMAA含量的增加， 其最低临界溶解温度(TLCS)下降；当NHMAA的含量大于5.25%时，随着NHMAA含量的增加，其TLCS上升；与PDEA相比P(DEA-co-NHMAA)相分离行为的浓度依赖性减弱；PDEA和P(DEA-co-NHMAA)从无规线团(coil)到蜷曲球(globular)的突然转变与从globular到coil的逐渐转变机理不同. 据此提出了P(DEA-co-NHMAA)在稀水溶液中相变的分子机理.     

Self-assembly of mixtures of block copolymers of poly(styrene-b-acrylic acid) with random copolymers of poly(styrene-co-methacrylic acid)

The effects of the addition of random copolymers of poly(styrene-co-methacrylic acid) [P(S-co-MAA)] on the self-assembly of block copolymers of poly(styrene-b-acrylic acid) (PS-b-PAA) are described. The effects of variation of five factors, including the MAA content, the weight fraction and molar mass of the P(S-co-MAA), the initial concentration of the mixture, and the length of the PAA segment in the block copolymer, were investigated. With increasing MAA content, the localization of the random copolymer in the aggregate changed from the core to the interface, which led to a morphological transition from spheres to vesicles. Vesicles, mixtures of vesicles and large spheres, and large spheres alone were formed with increasing weight fraction of the random copolymer. When the molar mass of the random copolymer was high, both rods and vesicles were observed at low water contents; otherwise, only vesicles were observed. The vesicle size increased (from 100 to 140 nm) with increasing initial polymer concentration, whereas the vesicle membrane thickness remained constant. The size of the vesicles prepared from the mixtures increased with water content but decreased with the length of PAA in the diblock.     

Microcalorimetric Investigation on the lower critical solution temperature behavior of N-isopropycrylamide-co-acrylic acid copolymer in aqueous solution

The lower critical solution temperature (LCST) behaviors of random and segmented copolymers of N-isopropylacrylamide (NIPAM) and acrylic acid (AA) prepared in dioxane and water have been investigated by using ultrasensitive microcalorimetry (US-DSC). The introduction of AA increases the LCST of the former but slightly affects that of the latter. When the molar fraction of AA is low (approximately 2 mol %), the LCST of the segmented copolymer shifts to a higher temperature with increasing pH, while the LCST of the corresponding random copolymer slightly changes. Below the boiling point of water, the random copolymer and segmented copolymer with the molar fraction of AA about 15 mol % no longer exhibit an LCST at pH > 5. The addition of calcium ions leads the LCST of both the segmented copolymer and random copolymer to decrease. Our results suggest that the LCST behavior of the copolymers is determined by the clustering of poly(N-isopropylacrylamide) segments.     

纳米氮化硅在提高PS版耐磨性中的应用研究

测试了纳米氮化硅可以使阳图PS版耐磨性提高30%,对感光度和分辨率没有影响.将<20nm氮化硅(0.0%—2.0%质量分数)超声波分散在混合溶剂中,再依次投入成膜树脂和光敏剂配制成感光胶,经离心涂布在(砂目Ra=0.65)铝版基上干燥后,晒版,显影,磨版.由反射密度的损失量评定印版耐磨性,由扫描电镜观察氮化硅纳米粒子在版面的状态.氮化硅质量分数为0.15%时耐印效果最好,大于2.0%时由SEM观察到团聚现象,印刷力下降.     

PABA疏水缔合水溶性共聚物溶液的合成与性能研究

本文根据高分子的分子设计原理，合成了带苯基的疏水单体N－苯基对正丁基丙烯酰胺（BBAM）。采用自由基胶束共聚的方法制备了水溶性丙烯胺／N－苯基对正丁基丙烯酰胺（BBAM）疏水缔合型共聚物（PABA）。研究了共聚物溶液的性能及影响因素。结果表明，随共聚物溶液浓度的增加，在临界缔合浓度以上，分子间缔合大量形成，水溶液表现粘度迅速增加，表现出明显的疏水缔合行为，与HPAM相比有优异的抗盐性。     

Effect of water content on the size and membrane thickness of polystyrene-block-poly(ethylene oxide) vesicles

The asymmetric amphiphilic block copolymer polystyrene962-block-poly(ethylene oxide)227(PS962-b-PEO227) canforms micelles with N, N-dimethylformamide(DMF) as co-solvent and water as selected solvent, and when the water content of the mixed solvent is higher than 4.5 wt%, the vesicle will be dominated. This work finds that once vesicles are formed in the DMF-water mixed solvent, the vesicle size and membrane thickness can be tuned by further increasing water content. As the water fraction elevated from 4.8 wt% to 13.0 wt%, the vesicle size dercreases from 246 nm to 150 nm, while the membrane thickness increases from 28 nm to 42 nm. In addition, the block copolymer packing and the free energy are analyzed as the vesicle size becomes small and the membrane becomes thick.     

钻井液用交联-接枝淀粉的制备及性能

以N,N′-亚甲基双丙烯酰胺为交联剂,过硫酸铵为引发剂,采用“溶剂法”工艺合成了高粘度抗剪切丙烯酸钠接枝淀粉(St),考察了单体、引发剂和交联剂用量、丙烯酸中和度、反应时间及反应温度对合成交联丙烯酸钠接枝淀粉糊液粘度的影响。 结果表明,其优化反应条件为：m(淀粉)∶m(丙烯酸）=1∶1.5,乙醇质量分数为80%,过硫酸铵的用量为单体总质量的1%,交联剂为单体总质量的0.6%,反应时间2.5 h,反应温度为55 ℃,丙烯酸中和度为70%。 该交联接枝淀粉糊液具有良好的触变性,在4%盐水泥浆中的添加量为14.0 g/L时,表观粘度为26.0 mPa·s,滤失量为7.2 mL;在饱和盐水泥浆中添加量为23.5 g/L时,表观粘度为54.5 mPa·s,滤失量为3.1 mL;在80 ℃高温下老化16 h其表观粘度及滤失量等性能基本保持不变,表现出良好的增粘、降失水作用和抗盐、抗老化性能。