NMR analysis of the microstructure of poly(methyl acrylate-co-N-vinylcarbazole)

The microstructure of a series of high conversion copolymers of methyl acrylate (MA) and N-vinylcarbazole (NVC) was characterized by NMR. ¹H- and ¹³C-NMR spectra were assigned by comparison to the homopolymers and by using heteronuclear shift correlation spectroscopy. MA-centered triad distributions were obtained from the carbonyl carbon. Distributions of NVC sequences were determined from aromatic carbons 1 and 8a, and aromatic proton 1 These experimentally determined sequence distributions were compared to those calculated from reactivity ratios approximated from the copolymer compositions. Agreement was very good for low NVC content copolymers. Three signals were particularly useful in providing rapid assessment of the distribution of NVC units within low NVC content copolymers: proton 1 and carbon 1 of NVC and the carbonyl carbon of MA. © 1992 John Wiley & Sons, Inc.     

N-二茂铁甲酰基-N′-芳(烷)基硫脲的合成及光谱性质研究

合成了二茂铁甲耽墓异硫氛酸始，并可与各种胺类(取代苯胺类，a-茶胺，低分于1的脂肪按，六红毗咬)反应，合成了未见报道的21种含二茂铁甲耽基的硫膝衍生物.本法简便，产物易分离提纯，产率高.二茂铁甲耽基异硫氛酸脂也可在低温(一5一0℃)下与强城性的脂肪胺在水溶液中石应.产物为经牙资夺娇_红夕卜产.讲_牙定磁共版讲确宁了里去构.     

Radiation-induced polymerization of methyl methacrylate in microemulsion with high monomer content

γ-Ray-induced polymerization of methyl methacrylate was conducted in a microemulsion stabilized by a mixture of sodium of 12-acryloxy-9-octadecenoic acid (AOA) and sodium dodecyl sulfate (SDS) with various weight ratios at room temperature. The experimental data showed that the mixture of AOA and SDS with a weight ratio 2 was an efficient surfactant system for the microemulsion containing 38.6 wt% MMA and 5.5 wt% surfactant. The effects of MMA concentration and dose rate on the polymerization kinetics and particle size are discussed.     

甲基绿褪色分光光度法测定维生素K3

在pH8.7~9.5的弱碱性介质中,维生素K3(VK3)能使甲基绿发生褪色反应,其最大褪色波长为630nm,并在紫外区出现两个新的吸收峰,其褪色程度(ΔA)与VK3浓度在0·11~2·40mg/L的范围呈正比,可用于VK3的分光光度测定。方法具有很高的灵敏度,其表观摩尔吸光系数ε630=2·13×105L·mol-1·cm-1;对VK3的检出限(3σ)为32·0μg/L。方法有较好的选择性,可用于某些药物制剂及血药中VK3含量的测定。     

微波辐射法合成α-萘甲醚的研究

用微波辐射法合成α－萘甲醚，考察了不同条件对产率的影响，此法反应时间短，产率可达75％。     

Two-step preparation for catalyst-free biodiesel fuel production

Biodiesel fuel was prepared by a two-step reaction: hydrolysis and methyl esterification. Hydrolysis was carried out at a subcritical state of water to obtain fatty acids from triglycerides of rapeseed oil, while the methyl esterification of the hydrolyzed products of triglycerides was treated near the supercritical methanol condition to achieve fatty acid methyl esters. Consequently, the two-step preparation was found to convert rapessed oil to fatty acid methyl esters in considerably shorter reaction time and milder reaction condition than the direct supercritical methanol treatment. The optimum reaction condition in this two-step preparation was 270°C and 20 min for hydrolysis and methyl esterification, respectively. Variables affecting the yields in hydrolysis and methyl esterification are discussed.     

Helical poly(3-methyl-4-vinylpyridine)/amino acid complexes: preparation, characterization, and biocompatibility

Helical poly(3-methyl-4-vinylpyridine) (P3M4VP)/amino acid complexes have been prepared via acid-base reaction of the achiral polymer with D and L amino acids: alanine, leucine, valine, serine and phenylalanine. The circular dichroism (CD) spectra of P3M4VP/D- and L-alanine complexes in CH(3)OH/H(2)O show opposing (near mirror image) Cotton effect signals at 278.4, 274.8 and 270.8 nm, indicating the formation of enantiomeric secondary structures. The formation of the enantiomeric structures is supported by observed [alpha](D)(25) values of -3.0 and +3.0 for the P3M4VP/D-alanine and P3M4VP/L-alanine complexes, respectively. The preparation of helical P3M4VP/amino acid complexes has been carried out in CH(3)OH and H(2)O at pH 1.8 and 2.7. The intensities of the Cotton effect signals were good. For example, for the P3M4VP/L-alanine complexes in CH(3)OH/H(2)O and H(2)O (pH 1.8), the second Cotton effect signal around 275-277 nm show [theta;] values of 49 980 and 79 210 deg . cm(2) . dmol(-1), respectively. The formation of the helical secondary structure is rapid. The acid-base reaction between P3M4VP and L-alanine in CH(3)OH/H(2)O, in 10 min, show a CD spectrum with Cotton effect signals at 274 and 272 nm with [theta] values of 27,000 deg . cm(2) . dmol(-1) and -36,000 deg . cm(2) . dmol(-1), respectively. P3M4VP permits ready conformational reorientation on complexation with amino acids, but once the helical P3M4VP/amino acid complexes are formed, it is stable at room temperature. P3M4VP is not compatible with HeLa ovarian cancer cells, but the helical P3M4VP/amino acid complexes are compatible with HeLa cells. The complexes minimally interfere with the adhesion and growth of HeLa cells on complex surfaces. Helical poly(3-methyl-4-vinylpyridine)/D- and L-alanine complexes support the attachment and growth of HeLa cells. The micrographs shows HeLa cells after three days: left panel: on P3M4VP/L-alanine complex; right panel: on P3M4VP/D-alanine complex.     

Production of poly(methyl methacrylate) particles by dispersion polymerization with mercaptopropyl terminated poly(dimethylsiloxane) stabilizer in supercritical carbon dioxide

Poly(methyl methacrylate) (PMMA) particles were produced by dispersion polymerization of methyl methacrylate in the presence of mercaptopropyl terminated poly(dimethylsiloxane) (MP-PDMS) in supercritical carbon dioxide at about 30 MPa for 24 h at 65 °C. The particle diameter could be controlled in a size range of submicron to micron by varying MP-PDMS concentration. The MP-PDMS worked as not only a chain transfer agent but also a colloidal stabilizer, which was named tran stab.Part CCLI of the series Studies on suspension and emulsion     

Sulfonated polypropylene ionomers

Polypropylene ionomers have been prepared by sulfonation of copolymers of propene and 7 methyl, 1-6 octadiene, followed by neutralization to cesium salts. Both WAXS and SAXS were used to study the morphology of the samples, while their thermal properties were studied by DSC and their mechanical properties by DMTA. The sulfonation process is shown to cause a further drop in crystallinity in addition to the effect of comonomer incorporation. Ion clustering is observed when the extent of sulfonation is high enough, the limit being dependent on the copolymer composition. The ion pairs which are not incorporated into the cluster cause a small-angle upturn in the WAXS pattern. The mechanical properties are strongly affected by the drop in crystallinity, but may be partly recovered due to ion clustering. No disruption of the ion clusters is observed before thermal decomposition of the polymer.     

烷基硫酸钠对MMA种子乳液聚合的影响

研究了烷基硫酸钠纯度，烷基碳链分布对甲基丙烯酸甲酯种子乳液聚合反应的影响。结果表明，烷基硫酸钠中乙醇不溶物含量的增加，可提高ＭＭＡ乳液聚合反应速度，在采用Ｋ２Ｓ２Ｏ８－ＮａＨＳＯ３－Ｃｕ＾２＋三元氧化－还原引发体系的ＭＭＡ乳液聚合中，Ｆｅ＾２＋降低反应速率，而Ｆｅ＾３＋则提高聚合反应速率；