干态大孔强酸树脂孔结构影响因素的研究

以二乙烯苯为交联剂,以甲苯、200#汽油和异丁醇为致孔剂,通过悬浮聚合法制备大孔聚苯乙烯白球,再经磺化反应合成大孔强酸阳离子树脂。采用比表面积测定仪对大孔白球和干态大孔阳离子树脂的孔结构进行了表征。考察了交联度、致孔剂用量和致孔剂种类对干态大孔强酸阳离子树脂孔结构的影响。     

致孔剂溶胀法制备多孔结构的乳胶粒

以苯乙烯、二乙烯基苯为单体 ,在传统乳液聚合阶段引入甲苯和庚烷作为单体的混合溶剂 (致孔剂 ) ,使溶剂在聚合中进入乳胶粒子内部 ,聚合完成后 ,通过水蒸气蒸馏的方法将致孔剂带出 ,以形成多孔结构乳胶粒。本文考察了单体和致孔剂比例、致孔剂中甲苯和庚烷的比例对反应速率、单体转化率及多孔结构乳胶粒的影响 ,结果表明 :单体和致孔剂比例为 2∶1、致孔剂中甲苯和庚烷的比例为 2∶1时 ,能够得到清晰结构多孔乳胶粒。     

多元致孔剂合成吸附树脂及吸附性能研究

以苯乙烯为单体,二乙烯苯为交联剂,甲苯和聚乙二醇为混合致孔剂,采用悬浮聚合的方法合成吸附树脂,研究树脂对苯酚的静态吸附。结果表明,当交联度50%,致孔剂:单体=1.5,甲苯:聚乙二醇400=1:1时,树脂对苯酚的吸附容量最大,达到85.16 mg/g,最佳吸附平衡时间为2 h;对树脂吸附容量影响最大的是致孔剂与单体的配比,其次依次是混合致孔剂中单体的配比和交联度。     

致孔剂用量对苯乙烯悬浮聚合微球粒径和密度的影响

以苯乙烯(St)为单体,正庚烷为致孔剂,偶氮二异丁腈(AIBN)为引发剂,聚乙烯醇(PVA)为分散剂,用悬浮聚合法制备聚合物微球,在转速和分散剂一定的条件下,研究致孔剂用量对聚苯乙烯微球粒径和密度的影响。结果表明,微球的粒径和密度均受致孔剂含量的影响。致孔剂含量影响初始液滴大小、致孔剂均匀分布、液滴中致孔剂和聚苯乙烯比例、相分离难易和微球的溶胀度等方面,这些因素共同影响微球粒径和密度。在实验条件范围内,V(致孔剂)∶V(St)=0.40时制备的微球粒径最大,平均粒径1.6mm;V(致孔剂)∶V(St)=0.80时微球密度最低,为0.899 8g/cm3,漂浮率最高,为96.29%。     

吸附树脂的合成及性能研究

采用悬浮聚合的方法,分别以甲苯和环己烷为致孔剂,在不同转速下合成聚苯乙烯-二乙烯苯共聚物大孔吸附树脂,用氮气吸附仪及热分析仪考察了其物理性能,并测定了对苯酚的静态吸附性能。结果表明,在交联度为30%时,吸附树脂的比表面积随着转速的增大而逐渐减小,对苯酚具有较好的吸附性能。相同实验条件下用甲苯作为致孔剂合成树脂的吸附性能优于用环己烷作为致孔剂所合成的树脂吸附性能,其最大吸附率可以达到68%。     

多孔性聚苯乙烯磁性微球的制备

以磁流体颗粒为核,采用乳液聚合法合成了聚苯乙烯磁性微球.用该微球作为种子,采用分散聚合法,以乙二醇/水为分散介质,聚乙二醇为分散剂,甲苯为制孔剂,进行二乙烯苯-丙烯酸-苯乙烯三元共聚物的合成,最终合成了粒径大小均匀、具有强磁响应性的多孔聚苯乙烯磁性微球.     

种子溶胀法制备聚甲基丙烯酸酯类微球

以分散聚合法制得的单分散聚苯乙烯微球为种球,采用改进的两步种子溶胀法制备了粒度均一、高交联、多孔的聚甲基丙烯酸缩水甘油酯-乙二醇二甲基丙烯酸酯微球,并系统探索了稳定剂种类和浓度、活化剂用量、溶胀倍数、致孔剂的种类及比例对微球形态和粒径分布的影响,同时用光学显微镜、扫描电镜、红外光谱及高效液相色谱对微球进行了表征。结果表明,以2μm和4μm的聚苯乙烯微球为种球,当活化剂与种球质量比为4,溶胀倍数为20~40倍,致孔剂为体积比为6∶4的环己醇和甲苯混合溶剂,以质量分数0.2%的羟丙甲基纤维素(以整个体系质量计,下同)为稳定剂时可制得粒径5μm和10μm的单分散高交联多孔的聚甲基丙烯酸酯类微球。     

单分散多孔聚合物微球的制备及其反相色谱应用

用分散聚合的方法制得单分散微米级聚苯乙烯微球(PS),以此聚苯乙烯微球作为种子,以邻苯二甲酸二丁酯为溶胀剂,苯乙烯为单体,二乙烯基苯为交联剂,甲苯为致孔剂,采用种子溶胀聚合的方法制得粒径分布较窄的多孔高交联的聚苯乙烯-二乙烯基苯微球(PS-DVB)。研究了交联剂与致孔剂的加入量对微球形貌、粒径及孔结构参数的影响。结果表明,所得多孔微球球形圆整,库尔特测得平均粒径为5.067~5.520μm,粒径分布窄,D90/D10为1.23~1.56,孔结构可控,并以此多孔微球作为反相色谱填料基质,理论塔板数每米可达6 000~15 000,可以用作高效液相色谱(HPLC)填料。     

K_2SO_4辅助混合模板剂制备大孔-中孔SiO_2微球

采用三嵌段聚合物F127、聚乙二醇和甲基纤维素为混合模板剂,以正硅酸乙酯为原料,无机盐K_2SO_4为添加剂,利用液-液微分散技术制备SiO_2微球。用透射电镜、扫描电镜、N_2吸附-脱附、X射线衍射及红外光谱对微球进行了表征。研究了混合模板剂的质量比、水解时间及K_2SO_4的量对于微球结构的影响。结果表明:无机盐的加入可有效调节微球的孔结构,得到的微球球形度和单分散性好,具有大孔-中孔孔结构,孔容可以达到4mL/g。     

HCl用量对介孔二氧化硅形貌的影响

以十六烷基三甲基溴化铵为模板剂、甲酰胺为共溶剂、正硅酸乙酯为硅源,室温下在HCl介质中合成了纤维状、圆盘状和花卉状等多种混合形貌的介孔二氧化硅.采用XRD、SEM、TEM等方法对样品进行表征,探讨了HCl用量对产物形貌的影响.结果表明,增加HCl用量会导致孔间距减小,但有助于提高介孔结构有序性和纤维状形貌的产率;过低的HCl用量条件下介孔二氧化硅不能形成规则外形.     

NKC-9型树脂催化合成单新戊二醇缩1,4-环己二酮

以阳离子交换树脂为固体酸催化剂,新戊二醇与1,4-环己二酮在二氯甲烷溶剂中脱水缩合合成了单新戊二醇缩1,4-环己二酮(单缩酮).实验考察了不同类型阳离子交换树脂的催化效果,结果表明,NKC-9型树脂具有良好的催化作用.通过单因素分析及正交试验,获得了该催化剂催化合成单新戊二醇缩1,4-环己二酮的最佳条件:在二氯甲烷溶液中,于25℃和反应液浓度为1.3mol˙L-1,催化剂用量为反应物总质量的15.40%,反应110 min,新戊二醇的转化率达94%,所得目标产物单缩酮收率达74.8%,气相色谱测定其纯度为96%.通过红外光谱分析、核磁共振谱图分析验证了所合成的产物为目标产物单缩酮.与传统酸性催化剂相比,采用树脂NKC-9作为反应催化剂不仅提高了反应收率,简化了反应工艺流程,无酸腐蚀和污染问题,且催化剂无需处理可重复使用多次.     

Hydrophilic methacrylate monoliths as platforms for protein microarray

Hydrophilic macroporous monolithic materials based on a copolymer of 2-hydroxyethyl methacrylate with glycerol dimethacrylate was synthesized by photo-initiated free-radical polymerization of monomers in a presence of the low molecular mass porogens, such as cyclohexanol, dodecanol, toluene and heptane, as well as the solutions of hydrophobic polymers, namely, polystyrene of different molecular weights and concentrations in toluene, and poly(dimethyl siloxane) in heptane. The Hildebrand solubility parameters were used to predict the diluent-polymer compatibility. Pore size distribution and surface area characterization have been assessed by mercury intrusion porosimetry; scanning electron microscopy was used to evaluate the differences in macroporous morphology obtained with different porogenic agents. The monolithic materials were covalently attached to a glass surface directly at polymerization step. Monolithic layers were applied as platforms for microarrays to accomplish highly sensitive solid-phase protein analysis. The efficiency of developed microarrays was demonstrated using mouse IgG and goat anti-mouse IgG as a model affinity pair.     

红霉素在大孔树脂上的吸附动力学研究

采用液膜及孔内扩散模型,模拟不同温度和不同红霉素(EM)初始浓度条件下,大孔吸附树脂HZ816及XAD16吸附红霉素的动态吸附曲线,并获得液膜传质及孔内扩散系数;考察了温度及溶质浓度对红霉素在两种树脂中吸附动力学的影响.结果表明,在实验范围内,红霉素在HZ816和XAD16两种树脂上的吸附平衡数据满足Langmuir吸附等温线方程,液膜及孔内扩散模型能较好地描述红霉素在两种树脂上的吸附动力学,同时,模型拟合得到的液膜传质系数随着温度的升高而增大,随着初始浓度的增大而增大,孔内扩散系数随着温度的升高而增大,随着初始浓度的增大而减小.     

Synthesis and characterization of a novel hydroxyl-terminated polydimethylsiloxane for application in the silicone-modified acrylic-grafted polyester resins

Monoallyl-end-capped polypropylene glycol (MPG) was successfully synthesized by the reaction of polypropylene glycol and allyl chloride. Also, hydrogen-terminated polydimethylsiloxane (H-PDMS) was prepared by the reaction of dichlorodimethylsilane and chlorodimethylsilane (CDMS). Then, MPG and H-PDMS were reacted to produce hydroxyl-terminated polydimethylsiloxane (OH-PDMS) as silicone which is used to prepare automotive pre-painted or coil-coated metals (PCM). This pre-coated metal PCM system was investigated to remove the wet-coating process, such as pre-treatment and spray coating for environmental regulations. However, automotive pre-coated metal must have high flexibility and stiffness to overcome the harsh conditions such as those encountered in the cutting, pressing, and stamping process. For these reasons, a series of silicone-modified acrylic-grafted polyester (SAGP) resins (e.g. SAGP-0–SAGP-10) were designed to satisfy both the hardness and the flexibility for an automotive PCM. The OH-PDMS (silicone) was characterized by Fourier transform-infrared (FT-IR), ¹H-NMR, and ¹³C-NMR spectroscopic techniques. The results showed that the targeted product was successfully carried out. The structural elucidation of the synthesized SAGP was carried out by FT-IR spectroscopic technique. Thermal properties of the resins were studied using thermogravimetric analysis and differential scanning calorimetry. The flexibility of the resins was measured by tensile test. The contact angle measurement can be measured by the water repellence of the coating surface, which is a standard method to evaluate cleanable characteristics. The surface free energy was calculated by the contact angle measurement.     

液液萃取和大孔吸附树脂纯化银杏外种皮黄酮类化合物的比较研究

选取5种弱极性有机溶剂和3种弱极性大孔吸附树脂,就液液萃取法和大孔吸附树脂法对银杏外种皮黄酮类化合物的纯化效果进行比较.结果表明,以芦丁为对照,液液萃取法在产品质量和黄酮类化合物含量方面均低于大孔吸附树脂法,其中DM-130大孔吸附树脂对银杏外种皮黄酮类化合物的纯化效果最好,产品中黄酮类化合物含量达25.92％.     

Macroporous chelating resins incorporating heterocyclic functional groups via hydrophilic PEG spacer arms. I. Synthesis and characterization

A series of novel chelating resins were synthesized by incorporating heterocyclic functional groups such as 2‐aminopyridine (AP), 2‐amino‐5‐methylthio‐1,3,4‐thiadizole (AMTZ), 2‐amino‐5‐ethyl‐1,3,4‐thiadizole (AETZ), and 2‐mercaptobenzothiazole (MBZ) into macroporous crosslinked polystyrene via a hydrophilic spacer arm of polyethylene glycol containing sulfur. Structures of the above‐mentioned resins were characterized by elemental analysis, Fourier transform‐infrared spectra (FTIR), ASAP‐2020 surface area and porosity analyzer, and scanning electron microscopy (SEM). © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 3220–3227, 2007     

Importance of Surface Area and Pore Size Distribution of Resin for Organic Toxicants Adsorption

Adsorption of benzoic acid and reactive brilliant blue 4 (RBB4) by hypercrosslinked resins and macroporous resins was examined. Micropore areas were much higher in the hypercrosslinked resins than macroporous resins while the pore volume and average pore diameter of macroporous resins were superior to the hypercrosslinked resins. The investigation showed that the pore size distributions of the resins significantly influenced the adsorption capacity of adsorbents. Adsorption of benzoic acid was dominated by BET surface area and the micropore area while the adsorption of RBB4 shifted to a pore-size-dominant process. The maximum mol adsorption capacities of benzoic acid were all higher than those of RBB4 by the resins, showing the influence of the molecular dimension on adsorption. The adsorption thermodynamic parameters were calculated and it revealed that the adsorption was an exothermic, spontaneous, and more ordered process. Adsorption kinetics and elution processes were also investigated for establishing the appropriate adsorption conditions for purifying wastewater containing benzoic acid or RBB4.     

大孔吸附树脂对芦丁的吸附实验探索

以芦丁为吸附质,考察不同种类的大孔吸附树脂对芦丁水溶液的吸附、树脂活化处理方法、吸附实验的实施方法和树脂的最佳用量。结果表明,最佳操作条件如下:树脂活化时间5 d,吸附前用95%乙醇浸泡会明显增加吸附量,吸附实验增重物确定为玻璃珠子,树脂适宜用量约为1.20000 g。并做了6种大孔树脂在芦丁水溶液中的吸附等温线,得出大孔树脂在芦丁中的吸附,会发生毛细下降效应,通过对大孔树脂的物化参数分析,发现大孔树脂的比表面积并不是决定吸附量的最主要因素,而由大孔树脂的物化参数以及溶剂的性质等协同作用决定。     

Solvent impregnated resins for MTBE removal from aqueous environments

MTBE removal from groundwater is difficult. State-of-the-art processes such as air stripping or adsorption can have significant drawbacks, like high energy consumption, low capacity and low selectivity. This is why the alternative technology of solvent impregnated resins is investigated. The extractant used is 3-iodophenol diluted with propylbenzene. From solids screening and impregnation experiments macroporous polypropylene (MPP) particles appear as a suitable solid support. The MTBE capacity of impregnated MPP is lower than that of a carbonaceous resin, but the selectivity of the SIR between MTBE and humic acid is significantly higher. Solvent impregnated resin (SIR) regeneration can be easily achieved with hot gas.     

Unsaturated Polyester Resins Obtained from Glycolysis Products of Waste PET

Abstract

Waste polyethylene terephthalate (PET) flakes were depolymerized by using ethylene glycol (EG), propylene glycol (PG), diethylene glycol (DEG), and triethylene glycol (TEG) in the presence of zinc acetate as catalyst. All glycolysis products were reacted with maleic anhydride and mixed with styrene monomer to get unsaturated polyester (UP) resins. Molecular weights of all synthesized UP resins were determined by end-group analysis. The curing characteristics such as gel time and maximum curing temperatures, and mechanical properties such as hardness, tensile strength, and elastic module of these resins were investigated. The waste PET resins were compared with the reference resins prepared with the same glycols and the properties of the resins were found to be compatible with the properties of the reference resins.