阳离子型水性聚氨酯制备和应用

阳离子型水性聚氨酯制备和应用台会文，王农跃，张留成（河北工学院化工系天津３００１３０）关键词聚氨酯，乳液，织物整理剂水性聚氨酯能赋予织物柔软、丰满的手感，改善织物耐磨性、抗皱性、防缩性、回弹性、通透性等。它还能与多种乳液树脂及助剂配合使用，是一类很有...     

超高效液相色谱法测定纺织品中的甲醛

纺织品中甲醛的来源概括起来主要有以下几个途径:纺织纤维在生产过程中进行醛化或增白处理后残余的甲醛;在对纺织品进行特殊处理如防皱、防水、阻燃、柔软等过程中的一些整理剂会释放甲醛;纺织品在印染过程中一些助剂会释放甲醛.织物上的甲醛不仅会刺激呼吸道黏膜和皮肤,而且会诱发癌症.服装在穿着和使用过程中,甲醛会释放出来,对人体造成伤害.     

可再生甲壳素吸附铬（Ⅵ）的特性研究

可再生甲壳素吸附铬（Ⅵ）的特性研究陈炳稔＊汤又文李国明万春华（华南师范大学化学系广州５１０６３１）关键词可再生甲壳素，制备，铬（Ⅵ），吸附１９９７－０８－１９收稿，１９９７－１２－２３修回广东省科委及高教厅资助课题利用甲壳素作为铬（Ⅵ）的捕集剂已有报...     

有机硅在抗菌整理剂中的应用

有机硅作为最常用的织物后整理剂之一,能赋予织物柔滑弹挺等多种功能。近年来,由于高致病菌的滋生蔓延,织物的抗菌整理受到广泛关注,抗菌整理剂也被认为是最有前途的整理剂之一。本文介绍了有机硅季铵盐、有机硅卤胺以及纳米金属杂化有机硅等抗菌整理剂的制备方法、抗菌效果和应用范围。从三个方面简单讨论了抗菌整理剂的作用机制,即作用于微生物细胞壁、细胞膜,以及破坏或抑制微生物核酸和蛋白质的生物合成。最后,在分析抗菌整理剂现状的基础上,提出了理想抗菌整理剂应具备的特征,并对抗菌整理剂的开发和应用前景进行展望。     

高效液相色谱-串联质谱法测定泡沫灭火材料及其他材料中的全氟辛烷磺酸及其盐

建立了一种高效液相色谱-串联质谱(HPLC-MS/MS)测定泡沫灭火材料、洗涤剂以及织物整理剂中全氟辛烷磺酸及其盐(PFOS)的方法。对应产品中的PFOS用水超声提取后,经固相萃取柱淋洗萃取,萃取液以乙腈-10 mmol/L乙酸铵溶液(80:20, v/v)为流动相进行HPLC分离,在负离子模式和多级反应监测(MRM)方式下进行测定。用两个子离子的相对丰度定性,外标法定量。PFOS的测定在0.002~0.1 mg/L范围内线性关系良好(r2=0.998);泡沫灭火材料、洗涤剂以及织物整理剂中PFOS的加标回收率分别为93.4%～103%, 93.2%～102%和91.8%～102%,精密度(以相对标准偏差(RSD)计)分别为0.48%～3.52%, 0.78%～1.79%和0.47%～3.47%;方法的检出限均为2 mg/kg(0.0002%)(信噪比（S/N）≥10),满足欧盟法规对泡沫灭火材料、洗涤剂以及织物整理剂中PFOS的限量检测要求。该方法准确度和灵敏度高,前处理简单,可用于泡沫灭火材料、洗涤剂以及织物整理剂中PFOS的检测。     

草菇菌丝体中氨基酸和甲壳素的提取及鉴定

草菇菌丝体中氨基酸和甲壳素的提取及鉴定刘佳铭（漳州师范学院化学系３６３０００）甲壳素（Ｃｈｉｔｉｎ）是自然界中含量仅次于纤维素的天然多糖［１］。国内外多数从虾、蟹、蛤等外壳提取甲壳素［２］。作者从草菇菌丝体中提取及鉴定氨基酸与甲壳素，结果令人满意。１...     

羧甲基甲壳素水溶液等电点的测定

羧甲基甲壳素水溶液等电点的测定陈炳稔汤又文陈文森（华南师范大学化学系广州５１０６３１）自然界每年生物合成的甲壳素估计数十亿吨，是仅次于纤维素的天然高分子化合物，壳聚糖是由甲壳素经过脱乙酰化反应而得到的一种生物高分子［１，２］。与甲壳素相比，壳聚糖的溶...     

纳米抗静电织物整理剂的制备和应用

研究了涤纶用抗静电剂－纳米锑掺杂二氧化锡（ATO）在整理剂中的稳定分散技术，探讨了分散剂的类型，添加量，pH值以及球磨工艺对分散的影响。用分散剂BN，粒子呈单分散状态，直径为20nm，可基本解决ATO在水相团聚现象，当分散剂KH560用量为ATO粉体质量的1％，pH值为9左右，球磨40h时，ATO的分散效果最好。用该抗静电整理剂处理涤纶织物，织的表面电阻从未处理的＞10^12Ω的数量级降低到＜10^10Ω的数量级，洗涤50次，抗静电效果基本不变。     

基体辅助激光解吸—电离飞行时间质谱法分析衍生化的寡链糖

以２，５－二羟基苯甲酸（ＤＨＢ）＋间硝基苄醇（ＮＢＡ）混合基体辅助激光解吸电离飞行时间质谱法（ＭＡＬＤＩ）分析甲壳素降解并衍生化的寡链糖，获得了满意的结果。对比其它基体，如：芥子酸（ＳＡ）、α－氰基－４－羟基肉桂酸等（α＿ＣＨＣＡ），２，５＿ＤＨＢ＋ＮＢＡ混合基体解吸电离效果最好：信号强、信噪比高。甲壳素降解产物的质谱分析至今未见报道。     

天然高分子甲壳素／壳聚糖在生物和医药方面的应用

天然高分子甲壳素／壳聚糖在生物和医药方面的应用徐健，金鑫荣（上海华东理工大学化学系上海２００２３７）甲壳素又称甲壳质、几丁质、壳蛋白、蟹壳素、壳聚糖等，广泛存在于低等动物，特别是节肢动物（如昆虫、蜘蛛、甲壳类）的外壳，以及低等动物（如真菌、藻类、酵母...     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Microwave-assisted copper-catalyzed stereoselective ring expansion of three-membered heterocycles with α-diazo-β-dicarbonyl compounds

Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular S_N2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.