三组分体系相图教学实验——微乳的制备*

为了让三组分体系相图的教学紧跟学科发展前沿,设计了一个研究型综合性实验——微乳的制备。实验以油酸乙酯为油相、吐温-80和乙醇质量比为3∶1的混合体系为乳化剂相,蒸馏水为水相,采用水滴定和油滴定结合的方法绘制了拟三元相图。通过电导率法对微乳3种类型的转变点进行了初判,按照电导率实验结果制备了3种不同类型的微乳样品,并利用染色法、黏度法和光散射法对微乳的物理化学性状进行了表征。通过实验,可以使学生获得分散体系的前沿知识,有利于创新人才的培养。     

微乳液法合成白光LED NaLu(MO_4)_2:Eu~(3+)/Eu~(3+),Tb~(3+)(M=W,Mo)荧光粉

采用微乳液法制备Na Lu(WO4)2-x(Mo O4)x∶8%Eu3+(x=0,0.5,1.0,1.5,2.0)/y%Eu3+,5%Tb3+(y=1,3,5,7,9)系列荧光粉。通过X射线衍射(XRD)表征,所制样品的X射线衍射峰与标准卡片PDF#27-0729基本吻合,表明所制的样品为白钨矿结构,属于四方晶系。扫描电镜(SEM)显示制备的纳米粒子是梭子状的,粒径大约是110 nm。激发发射光谱显示,在Eu3+离子掺杂物质的量分数为8%时,Na Lu(WO4)(Mo O4)∶Eu3+发光强度最大。Na Lu(WO4)2-x(Mo O4)x∶8%Eu3+(x=0,0.5,1.0,1.5,2.0)荧光粉在nMo/nW比达到1∶1(x=1)时发光强度最大,强烈的红光发射表明该材料可用于白光LED材料。该荧光粉在268、394和466 nm波长光激发下分别发出橙红色、黄色和淡黄色光,可以满足不同光色需要。Na Lu(WO4)(Mo O4)∶y%Eu3+,5%Tb3+(y=1,3,5,7,9)荧光粉,随着y值增大,从绿光区(x=0.278,y=0.514)进入白光区(x=0.356,y=0.373),(x=0.278,y=0.313),同时观察到Tb3+到Eu3+有效能量传递。     

反相微乳液法制备尺寸可调的高荧光碳量子点(英文)

在反相微乳液体系中,以抗坏血酸作为碳源制备具有高强度荧光的碳量子点。实验中通过调整水和表面活性剂的量比实现对碳量子点尺寸大小的控制,利用十六烷基胺修饰碳量子点。当激发波长为360 nm时,碳量子点的量子产率最高为47%。当水和表面活性剂的量比从20增加到50时,碳量子点的尺寸也随之而增大。     

YVO_4∶Eu~(3+)@SiO_2核壳结构纳米复合材料的合成与表征

用沉淀法制备了尺寸约为8 nm的YVO4∶Eu3+纳米粒子,然后用反相微乳液法在YVO4∶Eu3+纳米粒子的表面包覆了一层Si O2壳。利用XRD、TEM、UV-Vis吸收光谱和光致发光光谱对合成的样品进行了表征。得到的复合物具有较好的核壳结构,通过改变硅酸四乙酯的用量可以改变Si O2壳的厚度。研究了Si O2壳对YVO4∶Eu3+发光性质的影响,结果表明:包覆和未包覆的样品在紫外光激发下都有Eu3+的特征发射;随着Si O2壳厚度的增加,发光强度和量子效率越来越低,Eu3+格位对称性越来越高。     

Photocatalytic Oxidation of HMF under Solar Irradiation: Coupling of Microemulsion and Lyophilization to Obtain Innovative TiO2-Based Materials

The photocatalytic oxidation of biomass-derived building blocks such as 5-hydroxymethylfurfural (HMF) is a promising reaction for obtaining valuable chemicals and the efficient long-term storage of solar radiation. In this work, we developed innovative TiO₂-based materials capable of base-free HMF photo-oxidation in water using simulated solar irradiation. The materials were prepared by combining microemulsion and spray-freeze drying (SFD), resulting in highly porous systems with a large surface area. The effect of titania/silica composition and the presence of gold-copper alloy nanoparticles on the properties of materials as well as photocatalytic performance were evaluated. Among the lab-synthesized photocatalysts, Ti₁₅Si₈₅ SFD and Au₃Cu₁/Ti₁₅Si₈₅ SFD achieved the higher conversions, while the best selectivity was observed for Au₃Cu₁/Ti₁₅Si₈₅ SFD. The tests with radical scavengers for both TiO₂-m and Au₃Cu₁/Ti₁₅Si₈₅ SFD suggested that primary species responsible for the selective photo-oxidation of HMF are photo-generated electrons and/or superoxide radicals.     

Esterification of Octanoic Acid with Octanol in Microemulsion and Emulsion System

The esterification of octanoic acid with octanol in microemulsion and emulsion system is studied. In the presence of 5–10% dodecylbenzene-sulfonic acid (DBSA), which is a surfactant-type catalyst, high conversion of esterification can be given both in microemulsion and in emulsion system. Compared with emulsion system, single-phase microemulsion is a more effective reaction system for esterification, with the advantages of comparatively little influence by the amount of water, no need of hard stirring, and stable state when laid long. The esterification of other fatty acids and alcohols in this reaction system were also accomplished in favorable conversion.     

Micellar nucleation differential microemulsion polymerization

Polymer nanoparticles within the range of 2–5 nm with a solid content of more than 13 wt.% and a narrow molecular weight polydispersity (Mw/Mn ∼ 1.1) were for the first time prepared using a micellar nucleation differential microemulsion polymerization system emulsified by sodium dodecyl sulfate (SDS), with SDS/monomer (methyl methacrylate) and SDS/H₂O weight ratios of up to 1:16 and 1:100, respectively. It was found that for benzoyl peroxide (BPO), micellar nucleation is more favorable for the synthesis of smaller polymer nanoparticles than ammonium persulfate (APS) which gives rise to homogeneous nucleation and 2,2′-azobisisobutyronitrile (AIBN) which involves partially heterogeneous nucleation. In the polymerization process, there exists a critical stability concentration (CSC) of SDS, above which the size of the nanoparticles is to be minimized and stabilized. With an increase in the monomer addition rate, the polymerization system changes from a microemulsion system to an emulsion system. A mechanism was proposed to describe the micellar nucleation process of differential microemulsion polymerization. This study may contribute to the development of fine polymer nanoparticles for drug delivery systems.     

Comparison of Loading Efficiency between Hyperbranched Polymers and Cross‐Linked Nanogels at Various Branching Densities

The effect of branching point structures and densities is studied between azido‐containing hyperbranched polymers and cross‐linked nanogels on their loading efficiency of alkynyl‐containing dendron molecules. Hyperbranched polymers that contained “T”‐shaped branching linkage from which three chains radiated out and cross‐linked nanogels that contained “X”‐shaped branching linkage with four radiating chains are synthesized in microemulsion using either atom transfer radical polymerization (ATRP) or conventional radical polymerization (RP) technique. Both polymers have similar density of azido groups in the structure and exhibit similar hydrodynamic diameter in latexes before purification. Subsequent copper‐catalyzed azide–alkyne cycloaddition reactions between these polymers and alkynyl‐containing dendrons in various sizes (G1–G3) demonstrate an order of dendron loading efficiencies (i.e., final conversion of alkynyl‐containing dendron) as hyperbranched polymers > nanogels synthesized by ATRP > nanogels synthesized by RP. Decreasing the branching density or using smaller dendron molecules increases the click efficiency of both polymers. When G2 dendrons with a molecular weight of 627 Da are used to click with the hyperbranched polymers composed of 100% inimer, a maximum loading efficiency of G2 in the loaded hyperbranched polymer is 58% of G2 by weight. These results represent the first comparison between hyperbranched polymers and cross‐linked nanogels to explore the effect of branching structures on their loading efficiencies.

     

微乳液相色谱法对吴茱萸中辛弗林、吴茱萸碱与吴茱萸次碱含量的测定

构建了一种新的微乳体系,用于微乳液相色潜同时分析吴茱萸药材中的辛弗林、吴茱萸碱和吴茱萸次碱.用甲醇超声提取方法制备样品,通过对表面活性剂种类及浓度、酸度、添加剂等影响因素进行考察,得到最佳微乳体系的组成为:3.0%SDS-6.0%正丁醇-0.6%正辛烷-1.0%甲酸-1.2%乙腈-88.2%水.选择Diamonsil ...     

水/Triton X-100/正丁醇/环己烷反相微乳液体系中水结构的FT-IR研究

用FT-IR法研究了水/辛烷基苯酚聚氧乙烯醚（Triton X-100）/正丁醇/环己烷组成的反相微乳液体系水池中存在的束缚、结合和自由3种不同的水的状态.分别考察了水与表面活性剂物质的量之比（Rw）、水油比φ（水与环己烷的质量比）、助剂正丁醇的含量对3种状态水含量的影响.发现在φ=2.8、m正丁醇/mTriton X...