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2014年, 第44卷, 第1期　刊出日期：2014-01-22    下一期

基础研究

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十六烷基三甲基水杨酸铵水溶液的电导和流变性能研究 Study of conductivity and rheological behaviors of cetyltrimethylammonium salicylate in aqueous solution 邱召民, 平阿丽, 魏西莲 2014 (1):  1-5.  doi: 10.13218/j.cnki.csdc.2014.01.001 摘要 ( 326 )   PDF(1205KB) ( 344 )   研究了十六烷基三甲基水杨酸铵水溶液在稀溶液和亚浓溶液范围的电导和流变行为。体系的电导率-浓度曲线显示2个转折点:第一个转折点对应临界胶束浓度(cmc),第二个对应体系开始形成棒状胶束的浓度。计算了胶束化的热力学函数变化,证实胶束化过程主要来自于焓驱动。流变实验表明:所有体系均显示剪切稀化行为;溶液质量摩尔浓度高于119 mmol·kg-1时,体系符合Maxwell流体行为,具有单一结构弛豫时间;体系的高黏度来自于短棒状胶束之间的链接而不是缠结的蠕虫状胶束。 The conductivity and rheological behaviors of aqueous solution of cetyltrimetylammonium salicylate in dilute and semidilute range were studied.Profile of plot of conductivity vs.concentration of the system shows two inflection points.The first inflection point corresponds to the critical micelle concentration (cmc),while the second corresponds to the concentration that the rodlike micelles begin to form.The changes of thermodynamic functions of micellization were calculated and the results showed that the micellization is an enthalpy-driven process.The steady-state rheological experiment showed that all systems exhibit shear thinning behavior.When the mass mole concentration of the system is higher than 119 mmol·kg-1,its rheological behavior is in line with Maxwell fluid behavior with a single stress relaxation time.The high viscosity behavior is caused by the linkages between short rodlike micelles rather than entangled wormlike micelles. 参考文献 | 相关文章 | 计量指标

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长链酰胺基磺酸盐型双子表面活性剂的合成及性能研究 Synthesis and properties of long-chain amido sulfonate type gemini surfactants 秦文龙, 刘旋, 肖曾利, 杨江, 杨珍 2014 (1):  6-9.  doi: 10.13218/j.cnki.csdc.2014.01.002 摘要 ( 287 )   PDF(858KB) ( 334 )   以二聚酸和N-甲基牛磺酸钠为原料,经酰氯化和Schotten-Baumann缩合反应合成了一种磺酸盐型双子表面活性剂,并对其相关性能进行了表征。结果表明,通过正交试验获得的磺酸盐型双子表面活性剂C34H66(CON(CH3)CH2CH2SO3Na)2的优化合成条件为:反应温度15 ℃,反应时间5 h,碱质量分数40%,n(N-甲基牛磺酸钠)∶n(二聚酸酰氯)=2.3∶1。合成的C34H66(CON(CH3)CH2CH2SO3Na)2具有更高的表面活性,其γcmc和cmc分别为30.4 mN·m-1和3.55×10-4 mol·L-1。泡沫性能分析表明其具有良好的起泡性和稳泡性,水溶液的泡沫高度和半衰期分别是传统表面活性剂的1.3～3.2倍和12～33倍。 A kind of sulfonate type gemini surfactant was synthesized with dimmer acid and sodium N-methyl-β-amino ethyl sulfonate as starting materials via acylation and Schotten-Baumann condensation;and its relevant properties were characterized.Based upon orthogonal designed experiments,the optimum reaction conditions were obtained as:reaction temperature,15 ℃;reaction time,5 h;mass fraction of NaOH,40%;molar ratio of sodium N-methyl-β-amino ethyl sulfonate to dimmer acyl chloride,2.3∶1.The product displays higher surface activities as compared with the conventional surfactants.Its γcmc and cmc were determined as 30.4 mN·m-1 and 3.55×10-4 mol·L-1,respectively.In addition,its foaming power and foam stability is good,with foam height and foam half life 1.3-3.2 times and 12-33 times as compared with that of the conventional surfactants respectively. 参考文献 | 相关文章 | 计量指标

科技讲座

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表面活性剂的性能与应用(Ⅰ)——表面活性剂的胶束及其应用 Performance and applications of surfactants (Ⅰ) Surfactant micelles and their applications 刘静伟, 刘红芹, 赵莉, 邓奥, 徐宝财 2014 (1):  10-14.  doi: 10.13218/j.cnki.csdc.2014.01.003 摘要 ( 526 )   PDF(945KB) ( 625 )   介绍了表面活性剂胶束的形成、结构及增溶作用。综述了胶束强化超滤技术的原理、主要影响因素及在废水处理领域中的应用,同时阐述了胶束催化的原理及其在有机反应中的应用研究进展。最后对胶束强化超滤技术和胶束催化的发展趋势进行了展望。 Formation,structure and solubilization effect of surfactant micelles were introduced.Technical principle and affecting factors of micelle-enhanced ultrafiltration (MEUF),as well as its application in field of waste water treatment were summarized.Meanwhile,mechanism of micellar catalysis and its applications in organic synthesis were described.Their development outlooks were prospected. 参考文献 | 相关文章 | 计量指标

开发与应用

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微波辅助法合成季鏻盐 Synthesis of quaternary phosphonium salts under assistance of microwave irradiation 尹晓刚, 赵正容, 肖维军, 陈卓, 于杰 2014 (1):  15-18.  doi: 10.13218/j.cnki.csdc.2014.01.004 摘要 ( 284 )   PDF(863KB) ( 304 )   以三苯基膦和卤代烃为原料,采用微波法合成了7种季鏻盐。考察了反应温度、反应时间、溶剂种类、溶剂用量及原料摩尔比对产物产率的影响,确定了微波辅助法合成季鏻盐的较优条件:以DMF,乙腈或甲苯为溶剂、反应时间为20 min、反应温度为120 ℃、三苯基膦与卤代烃的摩尔比为1.1∶1、三苯基膦在反应体系中的浓度为2.86 mol·L-1。在此条件下,苄基三苯基溴化鏻产率可达93.5%,其他季鏻盐产率也较为理想。使用熔点仪和核磁共振波谱仪对合成的季鏻盐进行了表征。在较优条件下,微波法合成季鏻盐所需时间仅为传统加热法的2.8%以下。 Seven kinds of quaternary phosphonium salt were synthesized with halogenated hydrocarbons and triphenylphosphine as starting materials under assistance of microwave irradiation.Effects of reaction temperature,time,kind of solvent,solvent dosage and the molar ratio were studied,and the optimal conditions of the reaction were determined as:adopting DMF,acetonitrile or toluene as the solvent;reaction time,20 min;reaction temperature,120 ℃;molar ratio of triphenylphosphine and halogenated hydrocarbon,1.1∶1;concentration (measured by moles of triphenylphosphine),2.86 mol·L-1.Under the above mentioned conditions,yield of benzyltriphenylphosphonium bromide product can achieve 93.5%;while yield of other kinds of the quaternary phosphonium salt are also satisfactory.The products were characterized by 1HNMR and melting point.Under optimal conditions,the time needed for completion of the reaction is no more than 2.8% of that of conventional heating methods. 参考文献 | 相关文章 | 计量指标

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芥酸酰胺丙基羟基磺基甜菜碱的合成及性能研究 Synthesis and properties of erucoylamidopropyl hydroxysulfobetaine 于洪江, 刘玉, 肖志海 2014 (1):  19-22.  doi: 10.13218/j.cnki.csdc.2014.01.005 摘要 ( 355 )   PDF(853KB) ( 462 )   以芥酸和N,N-二甲基-1,3-丙二胺为原料经缩合反应生成芥酸酰胺丙基二甲基胺,再与亚硫酸氢钠和环氧氯丙烷反应生成的3-氯-2-羟基丙磺酸钠进行季铵化反应,合成出芥酸酰胺丙基羟基磺基甜菜碱。研究了合成的优化工艺条件,用红外光谱法对产品进行表征,并对其性能进行了评价。结果表明,缩合反应的优化工艺条件为:n(芥酸)∶n(N,N-二甲基-1,3-丙二胺)=1∶1.1,反应温度为160 ℃,反应时间为10 h,催化剂用量为1.5%,此条件下产率为82.7%;季铵化反应的优化工艺条件为:n(芥酸酰胺丙基二甲基胺)∶n(3-氯-2-羟基丙磺酸钠)=1∶1.1,反应温度为85 ℃,反应时间为8 h,此条件下产率为88.1%。产物溶液的cmc为1.78×10-5 mol·L-1,30 ℃时γcmc为40.1 mN·m-1,60 ℃时γcmc为30.6 mN·m-1;对Ca2+的容忍度达8 g·L-1;质量分数为2%时溶液表观黏度可达204 mPa·s。 Erucic acid and N,N-dimethyl-1,3-propane diamine were used as starting materials for preparation of erucoylamidopropyl dimethylamine via condensation.The latter was further quaterized with sodium 3-chloro-2-hydroxy propane sulfonate,which was formed by reaction between sodium hydrosulfite and epichlorihydrin,for synthesis of the targeted product erucoylamidopropyl hydroxysulfobetaine.Optimization of the synthesis conditions was studied.The targeted product was characterized by IR,and its performance was evaluated.Experimental results showed that the optimum conditions for the condensation are as follows:n(erucic acid)∶n(N,N-dimethyl-1,3-propane diamine)=1∶1.1,reaction temperature 160 ℃,reaction time 10 h,catalyst dosage 1.5%.Under the above mentioned conditions the yield can achieve 82.7%.The optimum conditions for the quaterization are:n(erucoylamidopropyl dimethylamine)∶n(sodium 3-chloro-2-hydroxy propane sulfonate)=1∶1.1,reaction temperature 85 ℃,reaction time 8 h.Under these conditions the yield of the quarterization can achieve 88.1%.The cmc of the targeted product is 1.78×10-5 mol·L-1.The γcmc achieves 40.1 mN·m-1 at 30 ℃,and 30.6 mN·m-1 at 60 ℃.Tolerance to Ca2+ achieves 8 g·L-1.Apparent viscosity of a solution of the targeted product with mass fraction of 2% achieves 204 mPa·s. 参考文献 | 相关文章 | 计量指标

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椰油酰胺丙基甜菜碱的合成与表征 Synthesis and characterization of cocamidopropyl betaine 吴海龙, 黄建帮, 罗啸秋 2014 (1):  23-25.  doi: 10.13218/j.cnki.csdc.2014.01.006 摘要 ( 1170 )   PDF(998KB) ( 852 )   以椰油酸甲酯、N,N-二甲基-1,3-丙二胺、氯乙酸和NaOH为原料,KOH为催化剂合成椰油酰胺丙基甜菜碱。考察了N,N-二甲基-1,3-丙二胺与椰油酸甲酯的投料比、催化剂用量、反应温度和反应时间对主反应椰油酰胺丙基二甲胺合成的影响。结果表明,较佳工艺条件为:n(N,N-二甲基-1,3-丙二胺)∶n(椰油酸甲酯)=1.15∶1,w(催化剂)=3.0%,反应温度为210 ℃,反应时间为25 min,此条件下椰油酸甲酯的转化率达到99.70%。采用红外光谱、质谱和高效液相色谱对目标产物结构进行了确认。 Cocamidopropyl betaine was synthesized using coconut fatty acid methyl ester,N,N-dimethyl propylene diamine,chloroacetic acid and NaOH as starting materials,and KOH as catalyst.Effect of factors such as molar ratio of N,N-dimethyl propylene diamine to coconut fatty acid methyl ester,dosage of catalyst,reaction temperature and reaction time et al on main reaction (synthesis of cocamidopropyl dimethylamine) was examined.Results showed that optimum conditions were screened out as follows:n(N,N-dimethyl propylene diamine)∶n(coconut fatty acid methyl ester)=1.15∶1;w(catalyst)=3.0%;reaction temperature 210 ℃;reaction time 25 min.Yield of the coconut fatty acid methyl ester achieves 99.70%.The structure of the targeted product was characterized with FTIR,MS and HPLC. 参考文献 | 相关文章 | 计量指标

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氨基有机硅表面活性剂的合成及性能研究 Synthesis and performance of amino silicone surfactant 谢妃军, 成晓玲, 余林, 余培荣, 张兆宏 2014 (1):  26-30.  doi: 10.13218/j.cnki.csdc.2014.01.007 摘要 ( 364 )   PDF(1019KB) ( 357 )   采用八甲基环四硅氧烷与四甲基二氢基二硅氧烷在浓硫酸作用下合成含氢硅油,然后以氯铂酸为催化剂,烯丙基缩水甘油醚与含氢硅油发生硅氢加成合成环氧改性有机硅,最后通过二乙醇胺对环氧改性有机硅进行开环反应得到氨基有机硅。采用FTIR和1HNMR对产物结构进行表征,研究氨基有机硅的润湿性能,测定得到其临界胶束浓度为0.102 g·L-1,并与嵌段硅油9906和共聚改性嵌段硅油进行比较研究。结果表明,润湿力随氨基有机硅含量的增加而增强,相同含量下,氨基有机硅的氨值越大,其对帆布的润湿力越强,所合成氨基有机硅微乳液的稳定性、整理后织物的亲水性和柔软手感均比嵌段硅油9906和共聚改性嵌段硅油好。 Hydrogen containing silicone fluid was synthesized by using octamethylcyclotetrasiloxane and 1,1,3,3-tetramethyldisiloxane as starting materials under the action of concentrated sulfuric acid.Then hydrosilylation between allyl glycidyl ether and the hydrogen containing silicone fluid was carried out with chloroplatinic acid as catalyst to produce epoxy modified silicone.Finally,ring opening reaction of the epoxy modified silicone was processed with diethanolamine to obtain amino silicone surfactant as the product.Structure of the product was characterized by FTIR and 1HNMR.Wetting power of the amino silicone product was investigated,and its cmc was determined as 0.102 g·L-1.Performance of the product was compared with that of block silicone oil 9906 and co-modified block silicone oil.Results showed that wetting power increases with the increase of content of amino silicone.Under the same content of amino silicone,the higher ammonia value of the amino silicone,the stronger wetting power to canvas sample.All the performance in application of the amino silicone surfactant such as stability of microemulsion prepared by amino silicone,hydrophilicity and hand feeling softness of cotton fabrics finished with amino silicone are better than that of block silicone oil 9906 and co-modified block silicone oil. 参考文献 | 相关文章 | 计量指标

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生物防晒剂活酵母细胞衍生物制备中酶解条件的优化 Optimization of enzymolysis conditions in preparation of biological sunscreen live yeast cell derivative 陈玲林, 代彦, 赵华 2014 (1):  31-34.  doi: 10.13218/j.cnki.csdc.2014.01.008 摘要 ( 333 )   PDF(850KB) ( 374 )   研究了紫外照射培养后蛋白酶添加量、酶解温度、酶解时间及pH等酵母菌酶解条件对酵母水解液的紫外吸收性能的影响,并将活酵母细胞衍生物应用于防晒护肤品中。实验结果表明,活酵母细胞衍生物的优化制备条件为:质量分数10%酵母菌液中添加2%的蛋白酶,1%的纤维素酶,pH=6,52 ℃酶解26 h。所制得的活酵母细胞衍生物作为防晒护肤品添加剂,使其SPF值最大可提高128.2%。 Effects of yeast enzymolysis conditions,such as dosage of UV irradiation cultivated protease,temperature,pH and time of the enzymolysis on the UV absorption performance of the yeast enzymolysis product solution were studied.Further,the live yeast cell derivative was applied in sun screening skin care cosmetic product.Experimental results showed that the optimum conditions for preparation of live yeast cell derivative are:addition of 2% of protease and 1% of cellulase into 10% (mass fraction) yeast solution,pH=6,temperature 52 ℃ and enzymolysis time of 26 h.The live yeast cell derivative can be used as additive in sun screening skin care cosmetics so as to increase maximum sun protection factor of the cosmetics by 128.2%. 参考文献 | 相关文章 | 计量指标

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一种出水型色彩调控霜的制备 Preparation of a moisture releasing color control cream 孟潇, 陈庆生, 赵金虎, 龚盛昭 2014 (1):  35-38.  doi: 10.13218/j.cnki.csdc.2014.01.009 摘要 ( 340 )   PDF(806KB) ( 721 )   制备了一种出水型色彩调控霜。通过对W/Si乳化体系出水技术的研究,探讨了配方中乳化剂的种类及用量、水相与油相质量比、成膜剂用量、乳化温度及均质乳化速率等影响水分释放效果的主要因素,得出较优的工艺参数:乳化剂为环五聚二甲基硅氧烷、二硬脂二甲铵锂蒙脱石及PEG-10聚二甲基硅氧烷的复配物,其质量分数为1.40%,水相与油相质量比大于13∶7(即水相质量分数大于65.0%),成膜剂黄原胶质量分数不超过0.05%,乳化温度为25 ℃,均质乳化速率为3 000 r·min-1。 A kind of moisture releasing color control cream was prepared.Via the study on moisture releasing technology of W/Si emulsification system,effects of main factors such as emulsifier type and its dosage,mass ratio of water phase to oil phase,dosage of film-forming agent,emulsification temperature as well as the speed of homogeneous emulsification on the moisture releasing result of the prepared product were investigated.The optimal process parameters were as follows:the emulsifier is a blend of cyclopentasiloxane,disteardimonium hectorite and PEG-10 polydimethylsiloxane with mass fraction 1.40%;mass ratio of water phase to oil phase is higher than 13∶7 (mass fraction of water phase is higher than 65.0%);mass fraction of xanthan gum as film-forming agent is less than 0.05%;emulsification temperature is 25 ℃;speed of homogeneous emulsification is 3 000 r·min-1. 参考文献 | 相关文章 | 计量指标

专论与综述

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化妆品及其原料中有毒残留物检测方法研究进展 Progress on detection methods for toxic residues in cosmetics and their ingredients 黄荣, 叶峻, 傅小红 2014 (1):  39-44.  doi: 10.13218/j.cnki.csdc.2014.01.010 摘要 ( 398 )   PDF(1102KB) ( 564 )   介绍了化妆品及其原料中有毒物质带来的安全性问题,对有毒物质的检验现状进行了总结;综述了化妆品和原料中有毒残留物邻苯二甲酸酯类化合物、二恶烷、亚硝胺化合物、双酚类和烷基酚类化合物、丙烯酰胺、残留溶剂的危害和检测方法;并讨论了国内近几年对上述有毒残留物常用的分析方法,主要有气相色谱法、高效液相色谱法、气相色谱-质谱法、液相色谱-质谱法;最后提出了在检测方面存在的问题和发展方向。 Security problems caused by toxic substances in cosmetics and their ingredients were introduced,as well as the present situation of detection for toxic substances were described.The harmfulness and detection method of toxic residues in cosmetics and their ingredients,such as phthalate esters,dioxane,nitrosamines,bisphenols,alkyl phenols,acrylamide and residual solvents,were summarized.The conventionally used detection methods for toxic residues in China recent years were discussed,including gas chromatography,high performance liquid chromatography,gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry.Finally,existing problems in detection methods and development trend were put forward. 参考文献 | 相关文章 | 计量指标

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植物精油在皮肤美白领域中的研究进展 Progress in research work on skin-whitening effect of essential oils 余汉谋, 姜兴涛, 李庆廷, 肖海鸿 2014 (1):  45-49.  doi: 10.13218/j.cnki.csdc.2014.01.011 摘要 ( 411 )   PDF(913KB) ( 647 )   简要介绍了传统皮肤美白剂的应用缺陷;重点综述了不同种类植物精油在皮肤美白领域的研究工作,包括体外酪氨酸酶抑制实验、黑色素细胞生长存活实验、黑色素生成实验及胞内酪氨酸酶活性测定实验;并从与熊果苷、曲酸的比较中分析了植物精油在皮肤美白领域中的应用潜力;最后提出了植物精油目前在皮肤美白领域研究中存在的问题、发展方向和应用前景等。 The defects in application of conventional skin-whitening agents were introduced.Research work in the field of skin-whitening effect of various plant essential oils,such as in-vitro test for inhibition of tyrosinase activity,test for survival and growing of melanin cells,test for formation of melanin as well as determination of intracellular tyrosinase activity were focused.Potential applications of the plant essential oils in the skin-whitening field were prospected by comparison of the results obtained in the above mentioned tests with that of arbutin or kojic acid.Current existing problems,development trends and application outlooks of the essential oils in the skin-whitening field were put forward. 参考文献 | 相关文章 | 计量指标

分析与检测

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超高效液相色谱法测定染发剂中的非那西丁 Determination of phenacetin in hair dye by ultra-high performance liquid chromatography 刘春生, 陈立伟, 吴玉銮, 罗海英, 冼燕萍, 王莉 2014 (1):  50-53.  doi: 10.13218/j.cnki.csdc.2014.01.012 摘要 ( 320 )   PDF(864KB) ( 333 )   建立了一种测定染发剂中非那西丁的超高效液相色谱(UPLC)分析方法。染发剂样品经体积分数为70%的甲醇水溶液提取,再用正己烷进行反萃取后,采用BEH C18色谱柱,以乙腈-水为流动相进行梯度洗脱分离,结合保留时间和光谱图定性,以标准曲线定量。实验结果表明:非那西丁质量浓度在0.5～50.0 mg·L-1内与峰面积线性关系良好,相关系数大于0.999 3;方法检出限(S/N=3)为3.0 mg·kg-1;加标量为10,20和50 mg·kg-1时,平均回收率为85.6%～97.9%,相对标准偏差(RSD,n=6)为3.7%～5.3%。 An analysis method was established to determine phenacetin in hair dye by ultra-high performance liquid chromatography with a diode array detector (UPLC-PDA).The hair dye sample was extracted with 70% (volume fraction) methanol-water solution,reverse extracted with n-hexane,and analyzed by UPLC-PDA on a BEH C18 column,with acetonitrile-water as the mobile phase in gradient elution mode.The targets were qualitatively determined by retention time,confirmed by the ultraviolet spectrum,and quantified by standard graph.Test results indicated that in the phenacetin mass concentration range of 0.5-50.0 mg·L-1,the content shows a good linearity with the peak value with correlation coefficient (r) higher than 0.999 3.The detection limit of phenacetin is 3.0 mg·kg-1.When the spiking level is 10,20 and 50 mg·kg-1,the spiked recoveries of phenacetin are ranged within 85.6% and 97.9%,and the precision (RSD) ranges from 3.7% to 5.3% (n=6). 参考文献 | 相关文章 | 计量指标

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高效液相色谱法检测防脱、育发类化妆品中的非那雄胺 Determination of finasteride in anti-calvous hair cosmetics by high performance liquid chromatography 刘亚雄, 吴达萍, 孙婷婷 2014 (1):  54-56.  doi: 10.13218/j.cnki.csdc.2014.01.013 摘要 ( 293 )   PDF(967KB) ( 383 )   采用高效液相色谱法测定防脱、育发类化妆品中的非那雄胺,色谱条件为Zorbax Extend C18柱(250 mm×4.6 mm,5 μm),流动相为乙腈/10 mmol·L-1磷酸二氢钾梯度洗脱体系,流速为1.0 mL·min-1,检测波长为220 nm,柱温为30 ℃。实验结果表明,在此条件下非那雄胺在0.8～20 mg·L-1与相应的峰面积具有良好的线性关系(R2=0.999 0),回收率为90.3%～102.0%。 A reversed-phase high performance liquid chromatography for the determination of finasteride in anti-calvous hair cosmetics was established.The sample was analyzed on a Agilent Zorbax Extend C18 column (250 mm×4.6 mm,5 μm) with detecting wavelength of 220 nm at 30 ℃,and eluted by mobile phase composed of acetonitrile (CH3CN) and KH2PO4 (10 mmol·L-1) with a gradient model,at a flow rate 1.0 mL min-1.Results showed that as the mass concentration of finasteride is in the range of 0.8-20 mg·L-1,the relationship between the mass concentration and the corresponding peak area shows good linearity (R2=0.999 0).The recoveries of finasteride achieve 90.3%-102.0%. 参考文献 | 相关文章 | 计量指标