双十二烷基对苯二甲酰胺丙酸钠的合成与性能研究

以十二胺、丙烯酸甲酯、对苯二甲酰氯等为主要原料经加成、酰胺化、皂化等反应合成了酰胺型羧酸盐Gemini表面活性剂——N,N′-双十二烷基对苯二甲酰胺丙酸钠(SDPA-12)。经单因素考察酰胺化反应得出最佳工艺条件为:n(N-十二烷基-β-氨基丙酸甲酯)∶n(对苯二甲酰氯)=2.2∶1,35℃回流反应8h,收率68.7%;经红外光谱、元素分析和核磁共振波谱对产物结构进行了确认。性能测定表明,25℃时SDPA-12的表面张力为27.09mN/m,临界胶束浓度为1.83×10-5mol/L。     

双十八烷基二羟乙基溴化铵的微波合成及性能

以十八烷基二乙醇胺和溴代十八烷通过微波合成技术制备了双十八烷基二羟基溴化铵季铵盐（DODAB）。确定最佳合成工艺条件为：反应物浓度为2.17 mol·L^-1、反应时间为158.61 min、微波功率为626.06 W，在此条件下转化率的预测值为93.71%。产品由IR和¹H NMR进行表征。测定产品的表面活性为：CMC=0.501 g·L^-1，表面张力为30.27 mN·m^-1，优于阳离子表面活性剂D1821。测定产品应用于织物的柔软性能，结果显示：DODAB的柔软效果与D1821相当，随着处理的次数增多，DODAB处理后的柔软效果虽比D1821稍微弱一些，但其手感上会更为自然，更为舒适。同时，DODAB较D1821有着更好的维持织物白度性能的效果，具有较好的抗黄变能力。     

甲基萘双十四烷基磺酸钠双子表面活性剂的合成研究

在“Berger法”基础上,提出合成甲基萘双十四烷基磺酸钠双子表面活性剂工艺路线———“一步法”,详细研究了反应时间、温度和催化剂对合成反应的影响。将甲基萘和α-十四烯烃磺酸按摩尔比为1∶2加入反应器中,在搅拌下,迅速升至150℃并保温4 h得甲基萘双十四烷基磺酸钠,经分析产品中双子表面活性剂质量分数达82%。此外,还研究了甲基萘双十四烷基磺酸钠的表面化学性能,它的cmc与pC20值分别是2.0×10-5mol/L和5.66。     

N—烷基—1,3—丙撑二胺的合成及应用

本文介绍了Ｎ－烷基－１,３－丙撑二胺的反应原理,生产工艺及其应用。     

磺基琥珀酸双十八油脂钠的合成

磺基琥珀酸酯钠盐系列表面活性剂在水中能电离成阴离子，属于阴离子表面活性剂。最早的工业产品之一是磺基琥珀酸二辛酯钠，为性能优异的工业用渗透剂和分散剂。磺基琥珀酸双十八油脂钠盐是磺基琥珀酸双酯钠盐系列产品的一种。是重要的双酯类表面活性剂，有极好的润湿性。不仅可用于纺织工业，而且通过在有机溶剂中形成胶束。在分离提取蛋白质领域展现了较好的应用前景。     

二步法合成烷基多苷工艺研究

在用二步法合成烷基多苷工艺过程中,影响烷基多苷组成的主要因素是Ｃ１２醇和葡萄糖的摩尔比以及反应温度;而催化剂和正丁醇的用量对烷基多苷的组成影响不大,正丁醇在整个反应体系中起相当于一种相转移催化剂的作用。     

二烷基磷酸酯铝的合成

二烷基磷酸酯铝是制备油基压裂液的主要成分。研究了反应温度、时间、反应物加量及带水剂对合成产率及其稳定性的影响，得到合成二烷基磷酸酯铝的最佳反应条件是：在常压，120℃下，将100g二烷基磷酸酯、42g硫酸铝及25mL带水剂混合并反应5h，产率为95％，w(二烷基磷酸酯铝）＝97．7％。用IR表征了其结构。     

双十四烷基双磺基甜菜碱表面活性剂合成

磺基甜菜碱分子结构中具有强酸根基团,是典型阴离子性和阳离子性极性集于一身季胺内盐型两性表面活性剂。磺基甜菜碱具有耐酸碱、钙皂分散性强、毒性低,化学稳定性好等优点;因而日益受到人们的重视,在日用化工及其它行业中的应用前景看好。本文主要介绍一种新型表面活性剂—双十四烷基双磺基甜菜碱的合成工艺条件。考察反应时间、温度等工艺条件对反应产物收率的影响。并通过红外光谱图验证了产物结构。通过优化工艺条件,在125℃反应16h甜菜碱的收率达到95.8%。     

醇钠法合成一缩二丙二醇的工艺过程控制

介绍了一缩二丙二醇的用途及合成方法,重点阐述了以乙醇钠为催化剂,用丙二醇和环氧丙烷在一定温度和压力条件下合成一缩二丙二醇的反应原理和工艺流程,从反应温度、压力、精馏方式、催化剂回收等方面对生产工艺过程控制进行了探讨,总结出一种效率高,成本低,质量好的一缩二丙二醇的生产工艺条件。     

双子表面活性剂N,N'-双十二烷基对苯二甲胺丙酸的合成及性能研究

以十二胺、丙烯酸甲酯和对二氯苄为原料,三氯甲烷为溶剂,合成了双子表面活性剂N,N'-双十二烷基对苯二甲胺丙酸。采用~1H NMR和~(13)C NMR对其结构进行了表征。(25±1)℃时pH对产物表面活性的影响研究结果表明:pH分别为8,10和12时,cmc分别为1.6×10~(-5),3.3×10~(-5)和2.1×10~(-5)mol/L;γ_(cmc)分别为32.39,33.24和36.94 mN/m;pc_(20)分别为2.56,2.14和2.09;Γ_(max)分别为3.45×10~(-6),3.97×10~(-6)和4.34×10~(-6)mol/m~2;A_(min)分别为0.48,0.42和0.38 nm~2。当pH=12时,随溶液温度升高,pc_(20)和A_(min)增大,Γ_(max)减小。     

水热合成氧化钼纳米纤维及其表征

以新型二钼酸铵[(NH4)2Mo2O7]饱和溶液和硝酸为原料,经过酸化处理后,利用水热反应法制备了纤维直径在50～200 nm,纤维长度在20 μm左右的三氧化钼纳米纤维材料.通过高分辨电子显微镜和场发射电子扫描显微镜以及XRD等手段对所合成的三氧化钼纳米纤维进行了表征.所合成的三氧化钼纳米纤维微观尺寸均匀、纤维表面光滑、具有良好的分散性,在催化剂、阻燃抑烟剂、钼深加工制品等领域具有广泛的潜在应用市场.     

Synthesis of phase- and shape-controlled TiO2 nanoparticles via hydrothermal process

The TiO₂ nanoparticles with anatase (5.7–12.7 nm), rutile (5.4–8.8 nm), mixed (4.4–8.6 nm) phase were individually prepared using the hydrothermal method. The structure and shape of the particles could be controlled by careful alterations of the hydrothermal conditions. Herein, the TiO₂ nanoparticles were successfully synthesized by employing Ti-isopropoxide as the titanium source into hydrochloric acid solution at mild conditions. The crystal structures such as anatase, rutile and mixed phase of TiO₂ nanoparticles were determined by means of concentration of hydrochloride. Especially, we observed that the rutile TiO₂ crystallites were grown into one-dimensional nanostructures, especially, nanowires, with increasing reaction time. The mechanism of the crystallization of the nanoparticles and the growth habit of TiO₂-rutile structure were discussed.     

高能机械球磨法制备高质量纳米β-SiC粉体

使用高能机械球磨法,首次以单质硅和石墨的混合粉体为初始原料,制备出了高质量的β-SiC纳米粉体.对球磨产物进行了XRD和TEM等表征,结果表明:球磨10h后,石墨粉完全非晶化,大部分硅粉也已经非晶化,而且已经有β-SiC纳米粉生成;球磨20h后,硅粉和石墨粉完全反应生成了单相的β-SiC纳米粉,平均晶粒尺寸约为20nm,但是团聚比较明显;球磨40h后的样品,平均晶粒尺寸约为12nm,而且样品分散性较好,为均匀的球形颗粒;继续增加球磨时间,虽然样品晶粒尺寸稍有减小,但是团聚又逐渐变明显,而且样品中混入铁的量逐渐增加.     

Synthesis of micro-and nanosized PbS with different morphologies by the hydrothermal process

PbS micro- and nanostructures with different morphologies and particle sizes were obtained via a simple hydrothermal reaction between lead oxalate, Pb(C₂O₄)₂, and thioglycolic acid (TGA) as Pb²⁺ and the sulfur source and the capping agent, respectively. Products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), ultraviolet–visible (UV–vis) spectroscopy and Fourier transform infrared (FT-IR) spectra. The effects of temperature, reaction time and the type of Pb²⁺ source on the morphology and particle sizes of products were investigated.     

Synthesis and characterization of macromolecular surface modifier PP-g-PEG for polypropylene

A novel macromolecular surface modifier, polypropylene-grafted-poly(ethylene glycol) copolymer (PP-g-PEG), was synthesized by coupling polypropylene containing maleic anhydride with monohydroxyl-terminated poly(ethylene glycol). The effects of the reaction condition on the graft reactions were studied. The copolymers were characterized by IR, ¹H NMR, thermogravimetry (TG) and differential scanning calorimetry (DSC). The results indicated that the graft reactions were hindered by increasing the molecular weight of PP or PEG. The graft copolymer was found to have a higher initial thermal degradation temperature and lower crystallization capacity as compared with pure PP, and the side chain of PEG hindered the PP chain from forming a perfect β crystal. The thermal stability of PP-g-PEG decreased with the increasing content or molecular weight of PEG. The copolymers were blended with polypropylene to modify the surface hydrophilicity of the products. The results of attenuated total reflectance FTIR spectroscopy (ATR-FTIR) showed that PP-g-PEG could diffuse preferably onto the surface of the blends and be suitable as an effectual macromolecular surface modifier for PP. __________ Translated from Acta Polymerica Sinica, 2007, (2): 203–208 [译自:高分子学报]     

水热法合成叶片状氧化铜及其生长过程研究

以氯化铜和氢氧化钠为原料,在无表面活性剂条件下采用水热法合成出由纳米棒组装成的叶片状氧化铜粉体。探究了在不同水热时间下产物的相结构及微观形貌的变化,进而探索产物的形成过程。利用X射线衍射（XRD）、扫描电子显微镜（SEM）和高分辨率透射电子显微镜（HRTEM）对产物的相结构及微观形貌进行分析。研究结果表明,随着水热时间的延长,产物经历了由短棒状氢氧化铜到长纤维状氢氧化铜和氧化铜混相结构再到叶片状氧化铜结构的转变。对叶片状结构中位错及堆垛层错的形成分析,证明了该微观形貌的产生可归因于不完全定向依附生长机制。     

Synthesis and characterization of macromolecular surface modifier PP--PEG for polypropylene

A novel macromolecular surface modifier, polypropylene-grafted-poly(ethylene glycol) copolymer (PP-g-PEG), was synthesized by coupling polypropylene containing maleic anhydride with monohydroxyl-terminated poly(ethylene glycol). The effects of the reaction condition on the graft reactions were studied. The copolymers were characterized by IR, ¹H NMR, thermogravimetry (TG) and differential scanning calorimetry (DSC). The results indicated that the graft reactions were hindered by increasing the molecular weight of PP or PEG. The graft copolymer was found to have a higher initial thermal degradation temperature and lower crystallization capacity as compared with pure PP, and the side chain of PEG hindered the PP chain from forming a perfect ? crystal. The thermal stability of PP-g-PEG decreased with the increasing content or molecular weight of PEG. The copolymers were blended with polypropylene to modify the surface hydrophilicity of the products. The results of attenuated total reflectance FTIR spectroscopy (ATR-FTIR) showed that PP-g-PEG could diffuse preferably onto the surface of the blends and be suitable as an effectual macromolecular surface modifier for PP.     

Synthesis and characterization of a macromolecular surface modifier for polypropylene

A novel macromolecular surface modifier, a polypropylene‐graft‐poly(butyl methylacrylate) copolymer, was synthesized through the coupling of polypropylene containing maleic anhydride with monohydroxyl‐terminated poly(butyl methylacrylate). The effects of the raw ratio, reaction temperature, and molecular weight of the branches on the graft reaction were studied. The graft copolymers were characterized with IR, ¹H‐NMR, thermogravimetry, and differential scanning calorimetry. The results of attenuated total reflection/Fourier transform infrared and contact‐angle measurements indicated that polypropylene‐graft‐poly(butyl methylacrylate) could diffuse preferably onto the surface and be used as a surface modifier for polypropylene. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102:3413–3419, 2006     

硫化钠还原制备邻氨基苯甲酸的研究

以邻硝基苯甲酸为原料,硫化钠还原制备邻氨基苯甲酸,研究并获得了反应的较佳工艺参数:邻硝基苯甲酸、硫化钠的摩尔比分别为1∶2.0,反应时间2.0h,反应温度80℃。在该工艺条件下,产物的收率为78%,产品的纯度为97%。