Improving properties of natural rubber/polyamide 12 blends through grafting of diacetone acrylamide functional group

The aim of the present study was to improve the compatibility in blends of natural rubber (NR) and polyamide 12 (PA12) by grafting NR with hydrophilic monomer, diacetone acrylamide (DAAM), via seeded emulsion polymerization. The increase in polarity of NR after grafting modification was confirmed by a considerable increase in the polar component of its surface energy. Blends of graft copolymers of NR and poly(diacetone acrylamide) prepared using 10 wt% of DAAM (NR‐g‐PDAAM10) and PA12 were prepared at a 60/40 blend ratio (wt%) using simple blend and dynamic vulcanization techniques. The mechanical and rheological properties of the resulting blends were subsequently investigated and compared with those of the corresponding blends based on unmodified NR. The results show that dynamic vulcanization led to a significant increase in both mechanical and rheological properties of the blends. It was also observed that the dynamically cured NR‐g‐PDAAM10/PA12 blend had smaller particle size of vulcanized rubber dispersed in the PA12 matrix than observed for the dynamically cured NR/PA12 blend. This is due to the compatibilizing effect of DAAM groups present in NR‐g‐PDAAM10 molecule, which decreases the interfacial tension between the two polymeric phases. Therefore, it can be stated that the interfacial adhesion between NR and PA12 was improved by the presence of DAAM groups in NR molecule. This was reflected in the higher tensile properties observed in the dynamically cured NR‐g‐PDAAM10/PA12 blend. Copyright © 2017 John Wiley & Sons, Ltd.     

水溶性负性光致抗蚀剂的研制

以自制丙烯酰胺-双丙酮丙烯酰胺共聚物和聚乙烯吡咯烷酮(PVP)为成膜基体物质,芳香族叠氮化合物为感光剂,研制出水溶性负性光致抗蚀剂配方.通过正交试验确定了最优配方.即共聚物中AM与DAAM质量比为1:1;P(AM-DAAM)与PVP质量比为1:2;感光剂用量为占成膜基体物质质量的1/6;偶联剂用量占成膜基体物质质量的1/60;表面活性剂G-18用量占成膜基体物质质量的1/40.在该配方下配制的光致抗蚀剂达到商品规格要求.通过与国外同类商品的比较得出自制光致抗蚀剂具有同国外商品相当的感光性能.     

A Novel Category of Ionic Liquids Based on Diacetone Acrylamide Cation and Their Use as Esterification Catalysts

A novel category of salts based on diacetone acrylamide cation （DA^＋） and the anions such as acetate （Ac^-）, trifluoroacetate （TF^-）, tetrafluoroborate （BF^-）, hexafluorophosphate （PF^-）, sulfate （SO^-） and chloride （Cl^-） were synthesized by usual neutralization of acids and bases at room temperature and characterized by IR, ^1H NMR and elemental analysis （EA）. The results show that these compounds possess the characteristic of ionic liquids. In addition, four of them, DABF, DACl, DASO and DAPF, were efficient catalysts for esterication of acetic acid with C1-C6 alcohols and octanol.     

含糖基水溶性紫外吸收剂的合成与表征

以三聚氯氰(TCT)、2,4-二羟基二苯甲酮(UV-0)、双丙酮葡萄糖为原料,经三步反应合成一种具有反应性基团的水溶性紫外吸收剂3-(2-(2-羟基苯基苯甲酮-4-氧基)-4-氯-1,3,5-三嗪-6-氧基)-1,2-异丙叉-α-D-葡萄糖(UV-DTM),产物的结构经IR、NMR和MS表征。探讨了每一步反应的条件对反应产率的影响。合成3-(4,6-二氯-1,3,5-三嗪-2-氧基)-1,2,5,6-双异丙叉-α-D-葡萄糖(DTDT)的优化反应条件为:n(三聚氯氰)∶n(双丙酮葡萄糖)∶n(Na OH)=0.9∶1∶1.7,在丙酮和水的混合体系中0℃下反应8h,产率73%。合成3-(2-(2-羟基苯基苯甲酮-4-氧基)-4-氯-1,3,5-三嗪-6-氧基)-1,2,5,6双异丙叉-α-D-葡萄糖(UV-DT)的优化条件为:n(DTDT)∶n(UV-0)∶n(Na OH)=1∶1.1∶1,在丙酮和水的混合体系中30℃下反应2h,产率74%。合成UV-DTM的优化条件为:每1mmol UV-DT与0.5m L盐酸(36%)在THF体系中25℃下反应5h,产率74%。UV-DTM的紫外吸收性能在240~400 nm内表现良好,水溶性得到大幅改善。     

Analysis of thermolabile residual solvents in a spray dried dispersion using static headspace gas chromatography

In this study, we discuss the development of a static headspace gas chromatography method for the analysis of residual acetone as well as its enriched impurities including mesityl oxide and diacetone alcohol, in a spray dried dispersion. The major challenges include the instability of mesityl oxide and diacetone alcohol at high temperature and peak tailing of diacetone alcohol. It was found that the headspace oven temperature has to be controlled to 150°C or below to prevent degradation beyond an acceptable level (< 1%). The peak tailing of diacetone alcohol was attributed to the “Phase Soaking” effect due to excessive diluent, which may condense and temporarily modify the stationary phase. The peak shape of diacetone alcohol is dependent on the column loading capacity and the peak area of N‐methyl pyrrolidone, the solvent that elutes after diacetone alcohol. The headspace oven temperature was set at 140°C, where the highest response ratio of diacetone alcohol/N‐methyl pyrrolidone at 1.46 and thus the best sensitivity was obtained. The calculated quantitation limits were 1 ppm for acetone, 3 ppm for mesityl oxide and 31 ppm for diacetone alcohol. The method successfully passed validation criteria for specificity, linearity, accuracy, and precision.     

Preparation and Characterization of New Type Ionic Liquids

A new type of ionic liquids containing cation of diacetone acrylamide [or N-(1,1-bismethyl-3-oxo-butyl)acrylamide]and anions such as CH3COO^-(Ac),CF3COO^-(TF),BF4^-(BF),PF6^-(PF),HSO4^-(SO) and Cl^-(Cl) were prepared by normal neutralization.The obtained ionic liquids were identified by FT-IR and ^1H NMR spectroscopy.However,their properties such as meliting point,conductivity,viscosity etc,were determined.     

二丙酮丙烯酰胺共聚物膜用于渗透汽化法分离乙醇—水混合物

为将稀薄的乙醇水溶液浓缩,传统的蒸馏方法不能避免乙醇-水的共沸,能耗也很大。渗透汽化法克服了蒸馏法的这两个缺点,有希望成为分离乙醇水溶液的较为理想的方法。 作为水优先透过膜材料,有聚乙烯醇、磺化聚苯乙烯、聚丙烯腈、醋酸纤维素、聚乙烯亚胺、阴、阳离子交换膜阴、阳离子性多糖类、聚丙烯酸等及各种共聚物和共混     

An emulsifier‐free core–shell polyacrylate/diacetone acrylamide emulsion with nano‐SiO2 for room temperature curable waterborne coatings

An emulsifier‐free core–shell polyacrylate emulsion, containing nano‐SiO₂ nanoparticles in the core and diacetone acrylamide (DAAM) in the shell, has been successfully prepared by emulsifier‐free seeded emulsion polymerization. The effects of reaction temperature, dropping time, nano‐SiO₂ and initiator contents, and variation of the composition of core monomers on the amount of coagulum, particle size, and monomer conversion have been investigated. The particle morphology and the distribution of emulsion particles have been measured by transmission electron microscopy (TEM) and dynamic light scattering. The keto‐carbonyl groups on the surface of the polyacrylate emulsion nanoparticles reacted with adipic dihydrazide (ADH) to form a film with a cross‐linked network structure at room temperature. Therefore, the emulsifier‐free core–shell emulsion could be used as a two‐component room temperature curable waterborne coating. It was also found that the properties of the coating were clearly superior after using the cross‐linker. Copyright © 2009 John Wiley & Sons, Ltd.     

Synthesis of Novel Pyran β-Amino Acid and 5,6-Dihydro-2H-pyran β-aminoxy Acid from Carbohydrate Derivatives

Synthesis of two new amino acids, containing pyran rings, is reported from carbohydrate derivatives. The cis-3-amino-pyran-2-carboxylic acid (cis-APyC) was prepared from (R)-glyceraldehyde derivative, using nucleophilic substitution reaction for pyran ring formation. Similarly, the trans-3-aminoxy-5,6-dihydro-2H-pyran-2-carboxylic acid (trans-AmPyC) was prepared from diacetone glucose (DAG), using ring closing metathesis (RCM) reaction for the ring formation.     

二丙酮果糖的氧化及其支链糖的合成

本文报道了两种新的氧化剂体系:(1)三氧化铬-乙醚-二氯甲烷/硅藻土,(2)重铬酸吡啶(Pyri-dinium dichromate)-三氟乙酸酐在酮粮合成中的应用。并通过酮糖3与RLi(R=Me,Ph)经亲核加成,合成得到了支链单糖4,5,由元素分析及IR、~1H、~(13)C-NMR数据证实了其结构。