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    2014年, 第44卷, 第3期 刊出日期:2014-03-22 上一期    下一期
    基础研究
    含羟基-磺酸基不对称表面活性剂的合成及表面活性
    Synthesis and surface activity of dissymmetric surfactants containing a sulfonic and a hydroxyl group
    侯璐, 胡志勇, 姜欣欣, 菅丰田
    2014 (3):  121-125.  doi: 10.13218/j.cnki.csdc.2014.03.028
    摘要 ( 266 )   PDF(924KB) ( 382 )  
    以三聚氯氰、氨基乙磺酸、乙醇胺和二正己胺、二正辛胺以及二异辛胺为原料合成出3种疏水结构不同的含羟基-磺酸基不对称表面活性剂(XSOHC6,XSOHC8和XSOHEC8),并用1HNMR,ESI-MS和元素分析对终产品进行了结构表征,结果与目标结构一致。采用吊片法测定目标产物的表面活性,运用稳态荧光探针法测定3种表面活性剂的临界胶束聚集数(Nm)。30 ℃下,XSOHC6,XSOHC8和XSOHEC8的cmc依次为8.1×10-4,2.1×10-6和8.5×10-5 mol·L-1cmc分别为33.0,27.6和28.2 mN·m-1,Nm分别为18,11和18。结果表明此类表面活性剂均具有较好的表面活性。 Three dissymmetric surfactants containing a sulfonic and a hydroxyl group with different length of carbon chain (XSOHC6,XSOHC8 and XSOHEC8) were synthesized with cyanuric chloride,three different kinds of fatty amine,taurine and ethanolamine as starting materials.Structure of the targeted products was characterized by 1HNMR,ESI-MS and elemental analysis.Surface activity of the surfactants was measured by Wilhelmy plate method.The critical aggregation number of micelle (Nm) was determined by steady-state fluorescence probe method.The cmc of XSOHC6,XSOHC8 and XSOHEC8 is 8.1×10-4,2.1×10-6 and 8.5×10-5 mol·L-1cmc of them is 33.0,27.6 and 28.2 mN·m-1,and Nm of them is 18,11 and 18 respectively.The results of the study showed that such dissymmetric surfactants have rather good surface activity.
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    半胱氨酸盐酸盐改性膨润土对铀的吸附研究
    Study on adsorption of uranium onto bentonite modified by cysteine hydrochloride
    王光辉, 胡苏杭, 韩晨
    2014 (3):  126-130.  doi: 10.13218/j.cnki.csdc.2014.03.029
    摘要 ( 264 )   PDF(793KB) ( 397 )  
    以钠基膨润土为原料,通过与半胱氨酸盐酸盐的离子交换反应制得改性膨润土。研究改性后的膨润土对铀的吸附行为,以及初始质量浓度和pH对吸附的影响,探讨改性后的膨润土对铀的吸附等温线、吸附热力学规律和吸附动力学规律。结果表明,改性后的膨润土对铀的吸附性能明显提高,吸附规律较好地符合Langmuir吸附等温式,最大吸附量为39.06 mg·g-1;该吸附反应为吸热反应,升高温度有利于吸附反应的进行;吸附动力学模型可用准二级反应动力学方程来描述,其二级反应速率常数为0.017 90 g·mg-1·min-1。 Using bentonite as raw material,the modified bentonite was prepared by ion exchange reaction of bentonite with cysteine hydrochloride.Uranium adsorption behavior of the modified bentonite,as well as effect of initial mass concentration and pH on the adsorption were investigated and described.Adsorption isotherms,adsorption thermodynamics and adsorption kinetics of uranium onto modified bentonite were also studied.The results showed that the adsorption capacity of the modified bentonite for uranium is significantly higher than that of unmodified bentonite.The adsorption pattern of uranium onto the modified bentonite follows the Langmuir model very well,and the maximum adsorption capacity of the modified bentonite is 39.06 mg·g-1.The adsorption process is an endothermic reaction and higher temperature is favorable for adsorption of uranium.The pseudo-second-order kinetics model was used to describe the adsorption process,and the adsorption kinetics constant was found to be 0.017 90 g·mg-1·min-1.
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    科技讲座
    表面活性剂的性能与应用(Ⅲ)——表面活性剂的相转移催化作用及其应用
    Performance and applications of surfactants (Ⅲ) Phase transfer catalytic action of surfactants and its applications
    王楠, 赵莉, 徐宝财, 周雅文
    2014 (3):  131-134.  doi: 10.13218/j.cnki.csdc.2014.03.030
    摘要 ( 366 )   PDF(778KB) ( 471 )  
    按照反应系统分类,分别介绍了液-液相转移催化剂、固-液相转移催化剂、三相相转移催化剂和反相相转移催化剂的催化机理、常用的表面活性剂类型,并给出了一些应用实例。最后提出了目前存在的问题并对其应用前景进行了展望。 Mechanism for action of phase transfer catalyst (PTC),including liquid-liquid PTC,solid-liquid PTC,three-phase PTC and reverse phase PTC as well as types of commonly used surfactant were reviewed with some practical application examples presented.Currently existing problems and outlooks for applications in this field were prospected.
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    开发与应用
    N,N′-双十二烷基乙脒基碳酸氢盐的合成及性能研究
    Synthesis and properties of N,N′-didodecylacetamidinium bicarbonate
    张婷, 代利, 蒋建中, 崔正刚
    2014 (3):  135-138.  doi: 10.13218/j.cnki.csdc.2014.03.031
    摘要 ( 213 )   PDF(778KB) ( 381 )  
    在N2保护下,以原乙酸三乙酯和十二胺为原料合成了N,N′-双十二烷基乙脒,然后在少量水存在下,向含N,N′-双十二烷基乙脒的乙醚中通入CO2生成了开关型表面活性剂N,N′-双十二烷基乙脒基碳酸氢盐,其结构经IR,MS和1HNMR表征。通过吊环法测得其在水中的cmc为7.08×10-5 mol·L-1cmc为28.96 mN·m-1,可以大幅度降低水的表面张力,具有良好的表面活性,并利用电导率测试证实了它的开关性能。 Under the atmosphere of nitrogen,N,N′-didodecylacetamidine was synthesized by reacting triethyl orthoacetate with dodecylamine,followed by bubbling CO2 through ether with existence of small amount of water,the switchable surfactant N,N′-didodecylacetamidinium bicarbonate was produced.IR,MS and 1HNMR were used to characterize its structure.The critical micelle concentration tested in water by ring method is 7.08×10-5 mol·L-1 and γcmc is 28.96 mN·m-1.It shows a good performance in reducing the surface tension of water.Switching performance was tested and confirmed by conductivity.
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    碱性蛋白酶在液体洗涤剂中的稳定性
    Stability of alkaline protease in liquid laundry detergent
    康林霞, 张剑, 秦洁, 张晟
    2014 (3):  139-142.  doi: 10.13218/j.cnki.csdc.2014.03.032
    摘要 ( 300 )   PDF(3206KB) ( 340 )  
    研究了利用α-环糊精(α-CD)与聚乙二醇-聚丙二醇-聚乙二醇(F108)之间的主客体识别作用构筑一种空心微球,此微球在水溶液中有碱性蛋白酶存在时,能够将其包裹在内腔中,起到保护作用,提高了其稳定性。结果表明,包裹后的碱性蛋白酶在液体洗涤剂中保存7 d时,酶活力是包裹前的2倍。 Based upon the host-guest recognition between α-cyclodextrin (α-CD) and poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (F108),a kind of self-assembly hollow nanospheres that can encapsulate alkaline protease in aqueous solution for improving stability of the enzyme was prepared.Test results showed that,after storing of 7 d,activity of the encapsulated enzyme formulated in the liquid laundry detergent is twice of that without the encapsulation.
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    化妆品用原花青素脂质体的制备及应用性能研究
    Preparation and application performance of proanthocyanidin liposome for cosmetics
    郭芳, 胡国胜, 奚朝晖, 王一宇, 林苗
    2014 (3):  143-146.  doi: 10.13218/j.cnki.csdc.2014.03.033
    摘要 ( 356 )   PDF(1090KB) ( 500 )  
    采用逆相蒸发法制备了化妆品用的原花青素脂质体,考察了原花青素与卵磷脂的质量比(药脂比)、聚乙二醇(PEG 1500)的用量对脂质体稳定性和包封率的影响。实验发现,随着药脂比或PEG 1500用量的增加,脂质体的包封率均呈先增加后降低的趋势。在m(原花青素)∶m(卵磷脂)=1∶20,m(卵磷脂)∶m(PEG 1500)=3∶1的较优条件下,得到的原花青素脂质体的包封率为77.28%,平均粒径为144.9 nm,透射电镜下观察其外观为球形或椭球形。同时研究了最优条件下原花青素脂质体的保湿性能,实验证明原花青素脂质体的保湿性能明显优于游离的原花青素溶液。 Proanthocyanidin liposome for cosmetics was prepared by reverse phase evaporation method.Effect of mass ratio of proanthocyanidin to lecithin and dosage of PEG 1500 on stability and extent of the encapsulation of the liposome product were examined.Results showed that the extent of encapsulation increases firstly and then decreases later as the increase of both mass ratio of proanthocyanidin to lecithin and the dosage of PEG 1500.Under conditions of m(proanthocyanidin)∶m(lecithin)=1∶20 and m(lecithin)∶m(PEG 1500)=3∶1,the extent of encapsulation achieves 77.28%,with an average value of particle size of 144.9 nm.The morphology of the liposome particle is spherical or ellipsoidal as observed by transmission electron microscope.In addition,the moisturizing performance of the liposome under optimal conditions was also studied.The results proved that the moisture retention performance of proanthocyanidin liposome is significantly better than that of proanthocyanidin solution without encapsulation of the liposome.
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    薄荷基甲酸薄荷酯的合成研究
    Synthesis of menthyl menthylformate
    岳海波, 梁娅, 陈义坤, 戴莉, 郭春生, 张峻松
    2014 (3):  147-150.  doi: 10.13218/j.cnki.csdc.2014.03.034
    摘要 ( 292 )   PDF(751KB) ( 399 )  
    首先以薄荷基甲酸与亚硫酰氯为原料,制得薄荷基甲酰氯;然后以薄荷基甲酰氯和L-薄荷醇进行反应,用无水吡啶为溶剂和缚酸剂,一锅法制得薄荷基甲酸薄荷酯。通过单因素实验和正交试验设计确定优化条件为:n(L-薄荷醇)∶n(薄荷基甲酸)=1∶1.5,n(L-薄荷醇)∶n(无水吡啶)=1∶6,反应温度为60 ℃,搅拌反应3 h,平均收率达83.91%。得到的目标产物经过IR,1HNMR及MS对其结构进行确认,通过感官评价可知薄荷基甲酸薄荷酯具有较好生理凉感,味觉凉感阈值为1.5 mg·L-1,100 mg·L-1的薄荷基甲酸薄荷酯溶液浸渍的滤纸条能在口中维持凉感的持续时间约为20 min。 Firstly,menthyl formic acid and thionyl chloride were used as starting materials to prepare menthyl formyl chloride and then menthyl menthylformate was prepared via the reaction of the menthyl formyl chloride and menthol,with anhydrous pyridine as solvent as well as acid absorbing agent.Single factor tests as well as orthogonal designed tests were carried out and the optimal reaction conditions were identified as:mole ratio of the chemical reagents,n(menthol)∶n(menthyl formic acid)=1∶1.5,n(menthol)∶n(pyridine)=1∶6;reaction temperature,60 ℃ for 3 h.Under such conditions,the average yield achieves 83.91%.Structure of the targeted product was characterized by IR,1HNMR and MS.Via sensory evaluation,the targeted product shows good cool feeling and its threshold value achieves 1.5 mg·L-1.A filter paper strip impregnated with 100 mg·L-1 solution of the targeted product can maintain cool feeling in mouth for 20 min.
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    专论与综述
    光敏表面活性剂胶束体系的研究进展
    Progress in research work with respect to photosensitive surfactant micelle system
    郁丽程, 陈洁, 方波, 吕婷阳, 王进爽, 金浩
    2014 (3):  151-154.  doi: 10.13218/j.cnki.csdc.2014.03.035
    摘要 ( 344 )   PDF(751KB) ( 578 )  
    综述了近年来光敏流变胶束体系的研究进展,包括光稀化体系、光凝胶体系和光流变可逆胶束体系及其流变特性。介绍了光敏胶束体系的形成原理。进一步对光敏胶束体系的相关研究和应用前景提出了建议和展望。 Progress in research work with respect to photorheological micelles,including photothinning fluids,photogelling fluids and reversible photorheological micelle system was reviewed.Mechanism for formation of photosensitive micelle system was described.Further concerning research work and applications in this field were prospected.
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    反应型季铵盐表面活性剂的合成与应用研究进展
    Progress in research work on synthesis and application of reactive quaternary ammonium salt cationic surfactants
    黄颖虹, 郑成, 林璟, 毛桃嫣, 徐运欢, 陈瑞兰
    2014 (3):  155-162.  doi: 10.13218/j.cnki.csdc.2014.03.036
    摘要 ( 423 )   PDF(971KB) ( 420 )  
    系统综述了反应型季铵盐表面活性剂的合成路线和方法,并按照其不同的分子结构特点进行了分类比较,着重介绍了几种含有特定功能基团的反应型季铵盐表面活性剂(双键型、环氧型、羟基型以及酰胺型)的合成方法,并阐述了其作为缓蚀防垢剂、增溶增敏剂、可聚合乳化剂、粘土稳定剂、纸张柔软剂以及相转移催化剂等在工业上的应用。最后分析了反应型季铵盐表面活性剂目前存在的不足并对其发展趋势进行了展望。 Methods for synthesis of reactive quaternary ammonium salt surfactants were systematically summarized.According to the features of molecular structure,various types of reactive quaternary ammonium salt surfactant were classified and compared.Methods for synthesis of several types of reactive quaternary ammonium salt cationic surfactants with specific functional groups (double bond,epoxy,hydroxy and amide) were introduced.Industrial applications of the surfactants,such as corrosion inhibiting and anti-scaling agent,solubilizing and sensitizing agent,co-polymerizable emulsifier,clay stabilizer,sheet softener as well as phase transfer catalyst were expounded.Currently existing deficiencies of the reactive quaternary ammonium salt surfactants and the development trend was prospected.
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    人参美容护发功效研究现状
    Current status of research work with respect to effect of ginseng in make up and hair care cosmetics
    张瑞, 闫梅霞, 许世泉, 王英平
    2014 (3):  163-166.  doi: 10.13218/j.cnki.csdc.2014.03.037
    摘要 ( 474 )   PDF(748KB) ( 619 )  
    简要介绍了人参透皮吸收的研究成果,不同人参皂苷其透皮吸收具有差异;从人参抗皮肤衰老的作用机制、人参美白的作用途径、人参对头发和头皮的护理作用等方面进行了重点综述;最后对人参化妆品的进一步开发提出了建议。 Results from research work with respect to percutaneous absorption of ginseng were briefed.There are significant differences in view of percutaneous absorption action between various kinds of ginsenoside.Mechanism for anti-aging action and process of whitening action on skin,as well as care actions on hair and scalp of ginseng were emphatically summarized.Suggestions for further development of ginseng formulated cosmetics were put forward.
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    分析与检测
    由α-氯代酸制备α-癸基甜菜碱产物的全组分分析
    Total component analysis of α-capric betaine product prepared from α-chloro fatty acid
    梅杰, 张永民, 刘雪锋, 方云
    2014 (3):  167-170.  doi: 10.13218/j.cnki.csdc.2014.03.038
    摘要 ( 250 )   PDF(777KB) ( 353 )  
    针对α-氯代十二酸(CDA)与三甲胺反应制备α-癸基甜菜碱(CB)的工艺路线,采用HPLC-ELSD法分析合成产物中的CB含量,采用索氏抽提法萃取残留脂肪酸,并用气相色谱(GC)进一步分析残留脂肪酸中十二酸(DA)、CDA和α-羟基十二酸(HDA)的相对含量。以V(甲醇)∶V(水)=7∶1的混合溶液为流动相,HPLC-ELSD的峰信号分离度高,在质量浓度0.004~0.08 g·L-1内线性关系、精密度和准确性较好;以石油醚(60~90 ℃)为萃取溶剂可以将残留脂肪酸萃取完全,结合GC测试,可定量分析DA,CDA和HDA。 α-Capric betaine (CB) was prepared from α-chlorododecanoic acid (CDA) and trimethylamine (TMA) as starting materials.The content of CB in the product was analyzed adopting HPLC-ELSD method.The residual fatty acids containing in the product were extracted with Soxhlet extractor and then the relative content of dodecanoic acid (DA),CDA and α-hydroxydodecanoic acid (HDA) in the residual of fatty acid extract were further analyzed with gas chromatography (GC).Results showed that,using a solution composed of V(methanol)∶V(water)=7∶1 as the mobile phase of HPLC-ELSD,the linear relationship,the reproducibility and the accuracy were good and the signal separation is high in the mass concentration range of 0.004-0.08 g·L-1;the residual fatty acids can be completely extracted with petroleum ether (60-90 ℃) as the solvent of Soxhlet extraction,and the relative content of DA,CDA and HDA can be quantitatively analyzed using GC.
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    己基葡萄糖苷的核磁共振氢谱分析
    Analysis of hexyl glucoside by 1HNMR
    付鹿, 王万绪, 杜志平, 王天壮, 刘晓英
    2014 (3):  171-173.  doi: 10.13218/j.cnki.csdc.2014.03.039
    摘要 ( 238 )   PDF(1635KB) ( 482 )  
    采用薄层色谱法分离己基葡萄糖苷(APG-06),并对分离的各组分进行核磁共振氢谱(1HNMR)鉴定。结果表明,以氯仿/无水乙醇/氨水(V(氯仿)∶V(无水乙醇)∶V(氨水)=19∶13∶1)混合溶液为展开剂可将APG-06在薄层板上分成5个区段;5个区段的组分分别为原料醇、单苷、二苷、三苷、四苷及以上与多聚糖的混合物。 The various components in hexyl glucoside (APG-06) product sample were separated by thin layer chromatography (TLC),and identified by 1HNMR.Results showed that when mobile phase consists of V(CHCl3)∶V(CH3CH2OH)∶V(NH3·H2O)=19∶13∶1,the APG-06 product can be separated into five parts:unreacted alcohol,monoglucoside,diglucoside,triglucoside and polyglucosides that are higher than tetraglucoside.
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    全二维气相色谱-飞行时间质谱法分析香水中的化学成分
    Analysis of components in perfumery by comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry
    姚林江, 王林, 陈玲, 李剑政
    2014 (3):  174-179.  doi: 10.13218/j.cnki.csdc.2014.03.040
    摘要 ( 266 )   PDF(4063KB) ( 419 )  
    采用一维气相色谱-飞行时间质谱法(1DGC TOF-MS)和全二维气相色谱-飞行时间质谱法(GC×GC TOF-MS)分析了香水的组成情况,对部分常见物质进行了定性分析。结果表明,对于同一香水样品,1DGC TOF-MS只鉴定出样品中匹配度大于750的共172种化合物,分别为萜烯类34种、醇类25种、酯类37种、醚类15种、酮类23种、醛类12种、酸和其他杂环烃类26种;GC×GC TOF-MS软件对经过数据自动处理,并结合标准谱图辅助定性和手动扣除,定性出匹配度大于750的共722种化合物,分别为萜烯类125种、醇类168种、酯类79种、醛类33种、酮类92种、其他杂环和饱和长链烃类等225种。 For analysis of composition of perfumery product,two detection technologies,one-dimensional gas chromatography+time-of-flight mass spectrometry (1DGC TOF-MS) and comprehensive two-dimensional gas chromatography+time-of-flight mass spectrometry (GC×GC TOF-MS) were applied.Conventional components in perfumery product were identified and classified.Results showed that 1DGC TOF-MS can identify 172 compounds with high matched results with MF>750 when matched with dedicated standard library.Among these compounds,they are constituted of 34 terpenes,25 alcohols,37 esters,15 ethers,23 ketones,12 aldehydes,26 acids and other heterocyclic compounds.While by the help of automatic processing of software and manually deduct background,GC×GC TOF-MS can identify 722 compounds with matched results MF>750,and those compounds are classified 125 terpenes,168 alcohols,79 esters,92 ketones,33 aldehydes,225 heterocyclic and alkane compounds.
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