当期目录

2015年, 第45卷, 第11期　刊出日期：2015-11-22 上一期    下一期

基础研究

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乙二醇葡糖苷的合成及其动力学研究 Synthesis of glycol polyglucoside and its kinetics 张海红, 张然, 李晓元, 郑学明, 尚会建 2015 (11):  601-605.  doi: 10.13218/j.cnki.csdc.2015.11.001 摘要 ( 259 )   PDF(931KB) ( 306 )   以新型、绿色强酸性阳离子交换树脂CT169为催化剂,葡萄糖和乙二醇为原料合成乙二醇葡糖苷。考察了催化剂用量、醇糖摩尔比和反应温度对葡萄糖转化率的影响,探讨了该反应的反应机理,并建立了反应的动力学模型,求取了模型的相关参数。结果表明,较佳反应条件为:n(乙二醇)∶n(葡萄糖)=7∶1,强酸性阳离子交换树脂CT169用量为葡萄糖物质的量的35%,反应温度为100 ℃,反应时间为5 h,在此条件下葡萄糖转化率达99.33%。催化剂重复使用7次,葡萄糖转化率基本不变,具有较好的重复使用性能。该过程为拟一级可逆反应,表观活化能Ea+=41.572 kJ/mol,指前因子k0=7.716×103 min-1。 Synthesis of glycol polyglucoside from glucose and glycol with a kind of new green strong-acid cation exchange resin as catalyst was studied.Factors affecting the reaction such as catalyst dosage,mole ratio of glycol to glucose and reaction temperature were investigated.Based on experimental data,the reaction mechanism of preparation process was proposed.The reaction kinetics model was established,and parameters of the kinetics equation were decided.The optimum reaction conditions were obtained as:n(glycol)∶n(glucose)=7∶1;dosage of the strong-acid cation exchange resin catalyst,35% of the mole of glucose;reaction temperature,100 ℃ for 5 h.Under such conditions,conversion of glucose can reach 99.33%.When the catalyst was reused for seven times,conversion of glucose is basically unchanged,indicating a rather good reusing performance.The experiment results showed that the reaction can be considered as a quasi first order reversible reaction.The apparent activation energy is 41.572 kJ/mol,and the pre-exponential factor is 7.716×103 min-1. 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(Ⅹ ⅩⅢ) ——表面活性剂在农药中的应用 Performance and applications of surfactants (Ⅹ ⅩⅢ) Application of surfactants in pesticides 周雅文, 贾美娟, 刘金凤, 张华清, 马建业, 徐宝财 2015 (11):  606-610.  doi: 10.13218/j.cnki.csdc.2015.11.002 摘要 ( 299 )   PDF(845KB) ( 451 )   详细介绍了表面活性剂在乳油、可湿性粉剂、悬浮剂、水乳剂和微乳剂等多种农药剂型中的应用。在农药中,表面活性剂的加入可增添剂型种类、增强稳定性、提高药效与使用寿命、减少其实际用量以及拓展用途等。最后对表面活性剂在农药领域的应用进行了简单的展望,提出农药用表面活性剂的研发应朝高效多品种、绿色环保方向发展。 Applications of surfactants in many kinds of pesticide formulation,such as emulsifiable concentrate,wettable powder,suspending agent,aqueous emulsion,microemulsion,and so on,were reviewed.The addition of surfactant in the pesticides can increase the dosage forms,enhance their stability,improve the efficacy and service life,reduce the actual dosage and expand their applications.At last,the outlook for application of surfactant in pesticide field was prospected,and the research work of surfactant used in pesticide should be developed towards more efficient varieties and green environmental protection. 参考文献 | 相关文章 | 计量指标

开发与应用

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一种阳离子型氟表面活性剂的合成及性能研究 Synthesis and performance of a cationic fluorinated surfactant 肖子冰, 邢航, 肖进新 2015 (11):  611-615.  doi: 10.13218/j.cnki.csdc.2015.11.003 摘要 ( 295 )   PDF(958KB) ( 476 )   以全氟辛基碘乙烷(C8F17CH2CH2I)为原料,通过格氏反应,得到全氟辛基丙酸(C8F17CH2CH2COOH),进而通过酰氯化、酰胺化和季铵化等多步反应得到一种阳离子型氟表面活性剂C8F17(CH2)2CONH(CH2)3N+(CH3)3I-,用IR,1HNMR和19FNMR对其结构进行了表征。测试了其水溶液及其0.1 mol/L NaCl水溶液的表面张力、在石蜡表面的接触角以及泡沫性能。结果表明,该氟表面活性剂在室温下具有极高的表面活性,且其泡沫性能及润湿性与传统碳氢阳离子表面活性剂C12H25N+(CH3)3Cl-相比,均更为优异。 A cationic fluorinated surfactant,C8F17(CH2)2CONH(CH2)3N+(CH3)3I- (FTAI),was synthesized with perfluorooctyliodoethane (C8F17CH2CH2I) as starting material through a series of reactions,including Grignard reaction,acylchlorination,amidation and quaterization.Structure of the FTAI was characterized by IR,1HNMR and 19FNMR.The surface tension,the contact angle on paraffin wax surface and the foaming power of FTAI aqueous solution and FTAI aqueous solution with 0.1 mol/L NaCl were measured.The results showed that this fluorinated surfactant exhibits excellent surface activity at room temperature.Its foaming power and wetting power were much higher than that of conventional cationic surfactant C12H25N+(CH3)3Cl-. 参考文献 | 相关文章 | 计量指标

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烯丙基二甲基烷基溴化铵的合成与性能研究 Synthesis and performance of allyldimethylalkylammonium bromide 陶贤平, 张跃军 2015 (11):  616-620.  doi: 10.13218/j.cnki.csdc.2015.11.004 摘要 ( 199 )   PDF(888KB) ( 345 )   以烯丙基二甲基胺(ADMA)和1-溴代直链烷为原料,合成了2种不同碳链长度(n=16,18)的烯丙基二甲基烷基溴化铵(C16和C18),得到较佳的合成工艺条件为以丙酮作溶剂,ADMA与溴代烷的摩尔比为1∶1.1~1.2,65 ℃下反应60 h,所得产品的收率分别为68.20%和66.05%。用IR,1HNMR和元素分析对产品结构进行了表征,并测定了产品的表面活性、水溶性、泡沫性能、乳化性及絮凝性。结果表明,C16和C18的临界胶束浓度分别为5.5×10-4和1.8×10-4 mol/L,相应的表面张力分别为33.5和32.4 mN/m,产品具有良好的表面活性;C16和C18的Krafft点分别为8和21 ℃;与十二烷基硫酸钠(SDS)相比,产品的乳化能力较弱;C16的发泡能力以及对高岭土的絮凝能力明显强于C18。 Two kinds of allyldimethylalkylammonium bromide (C16 and C18) with different carbon chain length (n=16,18) were synthesized by using allyldimethylamine (ADMA) and 1-bromo linear alkanes as starting materials.The better synthetic conditions are as follows:acetone as the solvent;reaction temperature,65 ℃;reaction time,60 h;molar ratio of ADMA to 1-bromo alkane,1∶1.1~1.2.Yield of the product are 68.20% and 66.05% respectively.Their structures were characterized by IR,1HNMR and elemental analysis.Their performance was measured,such as surface activity,water solubility and foaming,emulsifying and flocculating performance.Results showed that critical micelle concentration of the products (C16 and C18) is 5.5×10-4 and 1.8×10-4 mol/L respectively.Their corresponding surface tension is 33.5 and 32.4 mN/m respectively.The products display good surface properties.Krafft point is 8 and 21 ℃ respectively.The products display lower emulsifying power than that of sodium dodecyl sulfonate (SDS).The product C16 displays significantly stronger foaming power and stronger flocculating capacity to kaolin than that of the product C18. 参考文献 | 相关文章 | 计量指标

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磺基琥珀酸双酯钠盐的合成与表/界面性能 Preparation and surface/interfacial performance of sodium dialkyl sulfosuccinates 王红庄, 蔡红岩, 周朝辉, 张群, 田茂章, 李建国 2015 (11):  621-624.  doi: 10.13218/j.cnki.csdc.2015.11.005 摘要 ( 301 )   PDF(980KB) ( 343 )   以顺丁烯二酸酐分别与正辛醇、异辛醇、正癸醇和异癸醇在对甲苯磺酸的催化作用下进行酯化反应,然后再与亚硫酸氢钠发生磺化反应,合成出一系列磺基琥珀酸双酯钠盐(SS)表面活性剂SSN8,SSI8,SSN10和SSI10。采用红外光谱对目标产物进行结构表征确定了化合物结构。评价了SS表面活性剂的表面性能和与直链烷烃间的界面性能。结果表明,SS系列表面活性剂的临界胶束浓度在10-6~10-3 mol/L数量级,对应的表面张力在24.90~30.00 mN/m;界面性能评价表明,支链磺基琥珀酸双酯钠盐比相应的直链磺基琥珀酸双酯钠盐适合碳数更高的油相。 A series of surfactant sodium dialkyl sulfosuccinates,SSN8,SSI8,SSN10 and SSI10 were prepared through two steps.For the first step, cis-butenedioic anhydride reacted with n-octanol,iso-octanol,n-decanol,and iso-decanol separately to obtain diesters.Then,the diesters were sulfonated by sodium bisulfite to produce the sulfosuccinates.The structure of the target products was characterized by FTIR.Surface performance of aqueous solution of the target products as well as interfacial performance between aqueous solution of the target products and normal alkanes was evaluated.The cmc of these surfactants is in the range of 10-6-10-3 mol/L magnitude.The corresponding surface tensions are in the range of 24.90-30.00 mN/m.According to the results of interfacial tension measurement,the sulfosuccinates with branched carbon chain are more suitable for oil phase with higher carbon numbers than the sulfosuccinates with straight carbon chain. 参考文献 | 相关文章 | 计量指标

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Guerbet十六醇磺基琥珀酸单酯二钠盐的性能研究 Performance of disodium Guerbet hexadecyl sulfosuccinate 李云哲, 李运玲, 宋永波, 李俊 2015 (11):  625-628.  doi: 10.13218/j.cnki.csdc.2015.11.006 摘要 ( 303 )   PDF(891KB) ( 393 )   以Guerbet十六醇为原料,通过与顺丁烯二酸酐进行酯化反应再与亚硫酸钠发生磺化反应,制备了Guerbet十六醇磺基琥珀酸单酯二钠盐(HDSS),采用FTIR和1HNMR对其结构进行表征,并对其性能进行考察。HDSS的γcmc为27.7 mN/m,3.0 g/L的HDSS溶液中帆布润湿时间为10 s,2.0 g/L的HDSS溶液在0.5和30 min时的泡沫体积分别为445和235 mL。上述结果表明HDSS具有优良的表面活性、润湿性和泡沫性能。 Disodium Guerbet hexadecyl sulfosuccinate (HDSS) was synthesized through esterification of C16 Guerbet alcohol (2-hexyl-1-decanol) with maleic anhydride and sulfonation of the mono ester with Na2SO3.Structure of the HDSS was characterized by FTIR and 1HNMR,and its performance was investigated.The γcmc of the HDSS is 27.7 mN/m,the wetting time of canvas in the HDSS aqueous solution (3.0 g/L) is 10 s,and the foam volume of HDSS (2.0 g/L) is 445 mL at 0.5 min and 235 mL at 30 min.The results indicated that the HDSS has good surface activity,wetting power and foaming performance. 参考文献 | 相关文章 | 计量指标

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聚六亚甲基胍盐酸盐的合成研究 Study on synthesis of polyhexamethylene guanidine hydrochloride 曾平, 谢维跃, 蒋健, 魏盼中, 许筠 2015 (11):  629-631.  doi: 10.13218/j.cnki.csdc.2015.11.007 摘要 ( 471 )   PDF(963KB) ( 466 )   以盐酸胍和1,6-己二胺为主要原料,聚乙二醇400为溶剂,经高温热缩聚反应合成聚六亚甲基胍盐酸盐。考察了聚合工艺中反应温度、反应时间、投料比和溶剂用量等对产物数均分子量Mn和重均分子量Mw的影响,得到了较佳聚合反应条件。在较佳条件下合成的产品分子具有良好的线性分布,抗菌性能良好。 Polyhexamethylene guanidine hydrochloride was synthesized through high-temperature thermal condensation with guanidine hydrochloride and 1,6-hexanediamine as the main starting materials and polyethylene glycol-400 as solvent.The impact of the reaction conditions such as reaction temperature and time as well as molar ratio of the reactants and dosage of the solvent on the number average molecular weight Mn and the weight average molecular weight Mw of the product was studied,and the optimal polymerization process conditions were obtained.The product synthesized under the optimal process shows good molecular linear distribution and good antibacterial performance. 参考文献 | 相关文章 | 计量指标

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伊利石美容面膜的研究 Study on the natural cosmetic mask of illite 王杨, 张莲姬, 金玉子 2015 (11):  632-634.  doi: 10.13218/j.cnki.csdc.2015.11.008 摘要 ( 324 )   PDF(998KB) ( 538 )   制备了一种伊利石面膜(IFM),IFM由基料(BM)、伊利石矿物粉(IMP)和稳定剂黄原胶组成。其中,BM中各组分的质量分数分别为:甘油56.0%、双碱基调和剂28.0%、去离子水15.0%和维生素E 1.0%。BM,IMP和黄原胶以质量分数20.0%,79.5%和0.5%混合,可以得到保湿率为72.5%,润滑性、耐热性、耐寒性和稳定性均良好的IFM。 A kind of illite facial mask (IFM) was prepared based on the character of illite.The IFM was made of basic material,illite mineral powder (IMP) and stabilizing agent xantham gum.Mass fraction composition of the basic material was glycerol of 56.0%,double base additive of 28.0%,deionized water of 15.0%,and vitamin E of 1.0%.The basic material,IMP and xantham gum with respective mass fraction of 20.0%,79.5% and 0.5% were mixed homogenously to form the product.Through various laboratory tests as well as application practice,the product displays moisture retention capacity of 72.5%,as well as good performance such as good slippery and smooth feeling,heat resisting,cold resisting and storing stability. 参考文献 | 相关文章 | 计量指标

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疏水性光子晶体薄膜的制备及性能研究 Fabrication and performance of hydrophobic photonic crystal films 李珩, 徐朝华, 周春健 2015 (11):  635-638.  doi: 10.13218/j.cnki.csdc.2015.11.009 摘要 ( 263 )   PDF(3601KB) ( 324 )   以一步乳液聚合法制备单分散的聚(苯乙烯-甲基丙烯酸甲酯-丙烯酸)乳胶微球,通过控制表面活性剂十二烷基苯磺酸钠用量来调控乳胶微球粒径的大小,采用竖直沉积法将乳胶微球组装成光子晶体薄膜,继而用疏水改性剂对光子晶体薄膜表面进行改性。利用扫描电镜、紫外-可见分光光谱仪和接触角测量仪对样品进行了表征。结果表明:合成的乳胶微球的单分散性优异;不同带隙的光子晶体薄膜的颜色可实现全可见光的覆盖;疏水性光子晶体薄膜的疏水性能良好,其接触角在130°以上。 The monodispersing poly(styrene-methyl methacrylate-acrylic acid) latex microspheres were prepared by one-step emulsion polymerization.Diameter of the latex microspheres can be controlled by the dosage of surfactant sodium dodecylbenzene sulfonate.By vertical deposition method,latex microspheres with different diameter were self-assembled to form photonic crystal (PC) films.Finally,the surface of PC films was modified by hydrophobic agent.The products were characterized by means of scanning electron microscopy,UV-Vis spectrophotometer and contact angle measurement.Experimental results showed that the latex microspheres possess excellent monodispersity.The color for the different band gaps of PC films covers that of whole visible light.The performance of hydrophobic PC films is outstanding;its contact angle is more than 130°. 参考文献 | 相关文章 | 计量指标

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化妆品用微生物源天然防腐剂的抑菌效能研究 Antimicrobial effectiveness evaluation of natural microorganism source preservatives used for cosmetic formulation 李馨恩, 何秋星, 区梓聪, 方电力, 关建云, 赵红 2015 (11):  639-642.  doi: 10.13218/j.cnki.csdc.2015.11.010 摘要 ( 319 )   PDF(866KB) ( 506 )   以微生物源的嗜热链球菌发酵产物和曲霉发酵产物作为研究对象,根据其抑菌作用进行复配研究,参考美国个人护理品委员会(PCPC)的抑菌效能测试方法对乳液配方进行微生物挑战试验。结果表明,在乳液配方中,质量分数为0.5%的嗜热链球菌发酵产物和0.3%曲霉发酵产物可以使配方中的微生物菌落数在第14天降到100 CFU/g以下,可通过微生物挑战试验。 Two kinds of new natural microorganism source preservatives nominated Streptococus thermophilus Ferment and Aspergillus Ferment were taken as the object for research work.Formulation study based upon the bacterial inhibition action of the aforesaid preservatives was carried out.With reference of the bacterial inhibition efficacy test method of the American Personal Care Product Committee (PCPC),microbial challenge tests for emulsion formulations were processed.The test results demonstrated that an emulsion consisting of Streptococus thermophilus Ferment at 0.5% of mass fraction and Aspergillus Ferment at 0.3% of mass fraction can reduce the amount of microbial to be lower than 100 CFU/g on the 14th day and can pass the microbial challenge test meanwhile. 参考文献 | 相关文章 | 计量指标

专论与综述

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表面活性剂检测方法综述 Review of various measurement methods for surfactants 吕鹏, 左清泉, 李奇, 吴晓燕, 王成胜, 张润芳 2015 (11):  643-647.  doi: 10.13218/j.cnki.csdc.2015.11.011 摘要 ( 286 )   PDF(857KB) ( 402 )   重点综述了分光光度法、两相滴定法、色谱法、薄层层析法、电化学法、共振散射法、毛细管电泳法和示波极谱法等常见的表面活性剂检测方法,对比了各种检测方法的适用条件、优点与缺点;提出表面活性剂检测方法的选择与表面活性剂的类型有关;最后展望了表面活性剂检测的发展方向。 Conventional measurement methods for surfactants,including spectrophotometry,two-phase titration method,chromatography,thin layer chromatography,electrochemical method,resonance scattering method,capillary electrophoresis method and oscilloscope polarography method were reviewed.The applicable conditions,the advantages/disadvantages of these different methods were discussed.The selection of measurement method for surfactant is closely related to the type of the surfactant.The trend of development of measurement methods for surfactant was also discussed. 参考文献 | 相关文章 | 计量指标

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化妆品用水杨酸酯类衍生物的制备及应用进展 Preparation and applications of salicylic acid esters used in cosmetics 季丹丹, 刘艳红, 祝钧 2015 (11):  648-652.  doi: 10.13218/j.cnki.csdc.2015.11.012 摘要 ( 415 )   PDF(868KB) ( 678 )   系统综述了化妆品用水杨酸酯类衍生物的合成方法,并按照类型的不同对其合成方法进行分类,着重介绍了固体酸催化法、酯交换法、相转移催化法及微波合成法等;并阐述了其作为防晒剂、定香剂、抑菌剂和抗氧化剂在化妆品中的应用;最后分析了化妆品中水杨酸酯类衍生物目前存在的不足并对其发展趋势进行了展望。 Methodsfor synthesis of salicylic acid esters used in cosmetics were systematically summarized and classified.Various methods for synthesis,including solid acid catalytic method,ester exchange method,phase-transfer catalytic method as well as microwave synthesis method were introduced.Cosmetic applications of salicylic acid esters,such as sun-screening agent,perfume fixing agent,antimicrobial agent as well as antioxidant were expounded.Currently existing deficiencies of salicylic acid esters used in cosmetics and the development trend were prospected. 参考文献 | 相关文章 | 计量指标

分析与检测

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气相色谱-质谱联用法同时测定除螨类化妆品中乐杀螨和克螨特 Simultaneous determination of binapacryl and propargite in acaricidal cosmetics by GC-MS 周静, 周泽琳, 顾宇翔, 冷桃花, 徐红斌, 周耀斌 2015 (11):  653-656.  doi: 10.13218/j.cnki.csdc.2015.11.013 摘要 ( 355 )   PDF(917KB) ( 325 )   建立了除螨类化妆品中乐杀螨和克螨特的气相色谱-质谱联用(GC-MS)分析方法。样品用乙腈提取,基体分散固相萃取净化,经弱极性毛细管柱(HP-5MS)分离,选择特征离子监测扫描模式(SIM)测定,采用基质匹配标准溶液外标法定量。结果表明,乐杀螨和克螨特在6.0~40.0 mg/kg的范围内方法线性关系良好,相关系数R2≥0.995;乐杀螨和克螨特的检出限均为2.0 mg/kg,定量限均为6.0 mg/kg;在6.0和40.0 mg/kg质量分数下,乐杀螨和克螨特的精密度和重复性相对标准偏差均小于5%;在添加量为6.0,20.0和40.0 mg/kg时,乐杀螨的加标回收率为76.2%~93.1%,克螨特的加标回收率为77.2%~95.0%。 An analysis method was established for the simultaneous determination of binapacryl and propargite in acaricidal cosmetics using gas chromatography-mass spectrometry (GC-MS).Samples were extracted by acetonitrile and purified with matrix solid-phase dispersion extraction (MSPD).The purified extracts were separated by weak polar capillary column (HP-5MS) and components were detected with selected ion monitoring (SIM) scanning mode.Quantification was carried out using matrix-matched standard curve calibration.The results showed that when the mass fraction of binapacryl and propargite is in the range of 6.0-40.0 mg/kg,the content data displays good linear relationship with the response of the instrument and the correlation coefficients (R2) are all more than 0.995.The limits of detection of binapacryl and propargite are all 2.0 mg/kg and the limits of quantification are all 6.0 mg/kg.Under condition of mass fraction of 6.0 and 40.0 mg/kg,all RSD of data of precisions and repeatability for binapacryl and propargite are less than 5%.Values of spiked recoveries tested with addition of binapacryl on the levels of 6.0,20.0 and 40.0 mg/kg are found to be from 76.2% to 93.1%.The spiked recoveries of propargite on the same levels are from 77.2% to 95.0%. 参考文献 | 相关文章 | 计量指标