核壳型聚苯乙烯/聚甲基丙烯酸甲酯复合乳液的制备

以过硫酸铵(APS)为引发剂,用种子乳液聚合方法,合成出以聚苯乙烯(PSt)为核, 聚甲基丙烯酸甲酯(PMMA)为壳的复合乳液。透射电子显微镜观察了核壳复合乳胶粒的形态,光散射粒径分布仪(PCS)测量胶乳粒径大小及其分布。最终成功地制得了核壳型PS/PMMA复合乳液,所得复合乳胶粒粒径大小在60～90nm左右,且单分散性较好。     

Production of Methyl Oleate in Reactive‐Separation Systems

The esterification of oleic acid and methanol using sulfuric acid as a homogeneous catalyst is studied in reactive‐separation systems. The conversion of the free fatty acid was investigated in two different experiments with the molar ratio of methanol/oleic acid, amount of catalyst, temperature, and reaction time as variables. The conversion of the free fatty acid was found to depend strongly on the molar ratio of methanol/oleic acid. The reaction time had a direct effect on the conversion of the free fatty acid, and this conversion decreased with higher temperature. These results were valuable for a preliminary study on biodiesel production, using an acid homogeneous catalyst in a reactive dividing‐wall distillation column.     

Dependence of morphological changes of polymer particles on hydrophobic/hydrophilic additives

Fairly uniform microspheres of poly(styrene‐co‐methyl methacrylate) were prepared by employing a microporous glass membrane [Shirasu porous glass (SPG)]. The single‐step SPG emulsification, the emulsion composed mainly of monomers, hydrophobic additives, and an oil‐soluble initiator, suspended in the aqueous phase containing a stabilizer and inhibitor, was then transferred to a reactor, and subsequent suspension polymerization followed. The droplets obtained were polymerized at 75°C under a nitrogen atmosphere for 24 h. The uniform poly(styrene‐co‐methyl methacrylate) microspheres with diameters ranging from 7 to 14 μm and a narrow particle‐size distribution with a coefficient of variation close to 10% were prepared by using SPG membrane with a pore size of 1.42 μm. The effects of the crosslinking agent and hydrophobic additives on the particle size, particle‐size distribution, and morphologies were investigated. It was found that the particle size decreased with a narrower size distribution when the additives were changed from long‐chain alkanes to long‐chain alcohols and long‐chain esters, respectively. Various microspheres with different morphologies were obtained, depending on the composition of the oil phase. The spherical poly(styrene‐co‐methyl methacrylate) particles without phase separation were obtained when using an adequate amount of the crosslinking agent and methyl palmitate as an additive. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 1013–1028, 2000     

直接酯化法合成维生素C棕榈酸酯的工艺改进

维生素C棕榈酸酯是一种新型、脂溶性、无毒无害多功能的营养性抗氧化剂,近几年被国际上认可为一种新型食品添加剂.研究表明它的抗氧化效果明显比常用的抗氧化剂BHA、BHT、TBHQ等效果要好,还能与VE等抗氧化剂作用产生增效作用,仅仅需要加入少量,即可对食品起到保鲜作用,而且能延长食品贮存时间,增加食品的营养,安全可靠.因而广泛地应用于油脂、含油食品、医药、保健品化妆品等领域.实验以维生素C和棕榈酸为原料,硫酸为催化剂,直接酯化法合成维生素C棕榈酸酯.研究了反应时间、反应温度、维生素C与棕榈酸物质量的比、催化剂用量等工艺条件对产品收率的影响.工艺条件优化基础上,研究不同抗氧化增效剂对产品收率的影响.产品最终收率达到74.52％,产品质量符合GB16314-1996标准.     

超声酶促合成维生素A棕榈酸酯

研究了超声辐照下,在有机溶剂中以固定化脂肪酶Novozym435催化合成维生素A棕榈酸酯。考察了影响合成维生素A棕榈酸酯反应的诸因素(溶剂、底物摩尔比、底物浓度、反应时间、酶量和超声功率),并优化了反应条件:在10mL的正己烷溶剂中,0.164g维生素A醋酸酯和0.32g棕榈酸,在酶与维生素A醋酸酯的质量比为1∶4的固定化脂肪酶Novozym435催化下,超声功率为90W,反应6h,酯化率可达82%。     

Synthesis and characterization of novel hybrid polyoxazoline‐grafted multiwalled carbon nanotubes

The novel hybrid polyoxazoline‐grafted multiwalled carbon nanotubes (POZO‐grafted MWNTs) were synthesized by the reaction of partially hydrolyzed polyoxazolines (Hydrolyzed‐POZO) and MWNTs having carboxylic acid groups (MWNT‐COOH) in the presence of DCC as a condensing agent. Hydrolyzed‐POZO (degree of hydrolysis, 20.2 mol % by ¹H‐NMR) were produced from the hydrolysis of polyoxazolines in an aqueous NaOH solution at reflux for 72 h. MWNT‐COOH were prepared by acid treatment of pristine MWNTs. The composition, structure, thermal property, and surface morphology of the novel hybrid POZO‐grafted MWNTs were fully characterized by FT‐IR, Raman, ¹H‐NMR, DSC, TGA, SEM, and TEM. The obtained POZO‐grafted MWNTs are well soluble in various organic solvents and water. It was observed that the glass transition temperature (T_g) of POZO‐grafted MWNTs was lower than that of Hydrolyzed‐POZO due to the absence of hydrogen bonding interactions between Hydrolyzed‐POZO itself caused by the incorporation with MWNTs. It was also found that Hydrolyzed‐POZO was homogeneously attached to the surfaces of MWNTs through the “grafting‐to” method. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Influence of calcination temperature on the photocatalytic performance of the hierarchical TiO2 pinecone-like structure decorated with CdS nanoparticles

Herein, a novel hierarchical TiO₂ pinecone-like structure (TPS) has been successfully fabricated for the first time by self-assembling anodic oxidation methods on the Ti plate. Then it was constructed that a series of CdS-TPS nanocomposites with different cycles CdS modifying by a successive ionic layer adsorption and reaction (SILAR) after different temperature annealing in air. The structures and properties of the CdS-TPS were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Current-voltage (I-V), ultraviolet-visible (UV–vis/DRS). The results shown that the optical properties of the CdS-TPS could be rationally tailored by adjusting the CdS-modified cycles and annealing temperature, which significantly enhanced photocatalytic activity. To be used in photocatalytic organic pollutant removal after optimizing both the CdS modification cycles and annealing temperature. The 15-CdS-TPS-500?°C exhibited significantly improved photocatalytic activities of methyl orange (MO) degradation under simulated sunlight irradiation. With 180?min, 85% of the MO (0.05?mM/L, 5?mL) was photodegraded and its kinetic constant reached to 0.0104?min^?1, which is the 3.0 times and 3.6 times quicker than that of 5-CdS-TPS-500?°C and 15-CdS-TPS-0?°C, respectively. This could be ascribed to the result of the synergy effects of the suitable quantity of CdS nanoparticles modifier, the special surface structure, excellent crystallinity, higher electrical conductivity, and band structure matching. The possible photocatalytic mechanism of the CdS-TPS sample is investigated as well.     

Enzymatic Synthesis and Antioxidant Activity of 1‐Caffeoylglycerol Prepared from Alkyl Caffeates and Glycerol

Caffeic acid (CA) as a strong antioxidant has lower solubility in nonpolar media, which limits its application in the food industry. To increase the lipophilicity of CA, 1‐caffeoylglycerol (1‐CG) was synthesized by lipase‐catalyzed transesterification of alkyl caffeates in solvent‐free system and its antioxidant capacity was investigated. Methyl caffeate was screened as the appropriate substrate from tested alkyl caffeates with a yield of 90.63%. Ethyl acetate was used for extracting 1‐CG from enzymatic reactants and could be easily recycled. The produced 1‐CG had 2.5‐ and 10‐fold lower values of half maximal inhibitory concentration (IC₅₀) (10.86 and 3.99 μM) than butylated hydroxyanisole by 1,1‐diphenyl‐2‐picrylhydrazyl radical scavenging and β‐carotene‐linoleic acid assays, respectively. Thus, 1‐CG is an excellent antioxidant for application in the functional food industry. Using alkyl caffeates and glycerol as substrates to produce 1‐CG catalyzed by immobilized lipase in a solvent‐free system is a simple, selective, and safe bioprocess that can readily be achieved in the food industry, and the product 1‐CG could be widely applied in food, nutraceutical, and biotechnological products.     

Photocatalytic activity of nanocrystalline mesoporous-assembled TiO2 photocatalyst for degradation of methyl orange monoazo dye in aqueous wastewater

In this work, nanocrystalline mesoporous-assembled TiO₂ photocatalyst was synthesized by a sol–gel process with the aid of a structure-directing surfactant and employed for the photocatalytic degradation of methyl orange azo dye (monoazo dye), as compared to various commercially available non-mesoporous-assembled TiO₂ powders. The experimental results showed that the synthesized mesoporous-assembled TiO₂ nanocrystal calcined at 500 °C provided superior decolorization and degradation performance to the non-mesoporous-assembled commercial TiO₂ powders. In addition, several operational parameters affecting the decolorization and degradation of methyl orange, namely photocatalyst dosage, initial dye concentration, H₂O₂ concentration, and initial solution pH, were systematically investigated, using the mesoporous-assembled TiO₂ nanocrystal. The optimum conditions were a photocatalyst dosage of 7 g/l, an initial dye concentration of 5 mg/l, a H₂O₂ concentration of 0.5 M, and an initial solution pH of 4.7, exhibiting the highest decolorization rate of methyl orange.     

超浓乳液聚合苯乙烯—甲基丙烯酸的乳胶粒径及羧基分布

以苯乙烯、甲基丙烯酸为主要原料进行超浓乳液聚合 ,制备了含功能基的单分散性复合物。考察了乳化剂浓度、内相比、聚合程度对乳胶粒大小及分布的影响。同时 ,用电导滴定法测定了乳胶粒表面羧基的含量 ,探讨了乳化剂浓度、羧酸含量及内相比对羧基分布的影响。结果表明 ,随乳化剂浓度减小、内相比增加、聚合时间延长、乳胶粒径增大 ,随乳化剂浓度减小、内相比增加、粒子表面羧基减少 ,而羧酸含量对羧基分布的影响不太明显