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2015年, 第45卷, 第8期　刊出日期：2015-08-22 上一期    下一期

基础研究

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两性双子表面活性剂的合成及性能研究 Synthesis and properties of amphoteric Gemini surfactant 谢郢, 赖璐 2015 (8):  421-424.  doi: 10.13218/j.cnki.csdc.2015.08.001 摘要 ( 264 )   PDF(865KB) ( 381 )   以二乙胺盐酸盐、十二烷基二甲基叔胺、环氧氯丙烷和丙磺酸内酯等为原料,合成了一种两性型双子(Gemini)表面活性剂,并采用红外光谱和元素分析对合成产物进行结构表征;采用滴体积法测定合成产物的表面张力曲线;采用电导率法测定并计算了合成产物的胶束化热力学参数。结果表明,合成产物的临界胶束浓度(cmc)和cmc时的表面张力分别为8×10-5 mol/L和38.57 mN/m,且随着温度的升高,产物溶液的cmc升高。胶束化过程的ΔHmθ为负值,说明胶束化过程是一个放热过程;胶束化过程的ΔSmθ为正值,说明胶束化过程是一个熵驱动过程。 A kind of amphoteric Gemini surfactant was synthesized with diethylamine hydrochloride,epichlorohydrin,dodecyl dimethylamine and propanesultone as starting materials.The chemical structure of the synthesis product was characterized by IR and elemental analysis.The surface activity vs.concentration plot of the synthesis product was investigated by drop volume method,and the thermodynamic parameters were calculated based upon measurement of electrical conductivity of the synthesis product.Results showed that the critical micelle concentration (cmc) of the synthesis product is 8×10-5 mol/L,and the surface tension at cmc minimizes to 38.57 mN/m.Moreover,with the increasing of temperature,the cmc of the synthesis product increases.The ΔHmθ of micellization process is negative,indicating that the process is an exothermic process.The ΔSmθ is positive,which suggests that the micellization process is an entropy-driven process. 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(ⅩⅩ)——表面活性剂在制革工业中的应用 Performance and applications of surfactants (ⅩⅩ) Applications of surfactants in leather industry 武丽丽, 张利丹, 马帅帅 2015 (8):  425-428.  doi: 10.13218/j.cnki.csdc.2015.08.002 摘要 ( 242 )   PDF(788KB) ( 676 )   分别介绍了表面活性剂在制革工业准备工序、鞣制工序以及整理工序中的作用与功能及适用类型,表面活性剂在制革工业各工序中的应用,在很大程度上影响着成革的品质和性能。同时,提出了皮革用表面活性剂的发展方向,能赋予皮革特殊性能的专用皮革助剂(如含氟和含硅表面活性剂)将是未来皮革用表面活性剂研发的重要品种之一。 Actions and functions as well as applicable types of surfactants in preparation step,tanning step and finishing step of leather making technological process were described.Application of surfactants influences the quality and performances of finished leather products to a large extent.Trend of development of applications of surfactants in leather industry was put forward.The specific leather auxiliaries for providing special performance of leather products,such as fluorinated surfactant and silicone surfactant,will be the important orientation for research and development work in this field in near future. 参考文献 | 相关文章 | 计量指标

开发与应用

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酯基有机硅季铵盐合成工艺的响应面优化及表面性能 Synthesis and surface activity of silicone based esterquat by response surface methodology 郑成, 黄武欢, 毛桃嫣, 陈鹏, 林璟, 虞启明 2015 (8):  429-433.  doi: 10.13218/j.cnki.csdc.2015.08.003 摘要 ( 217 )   PDF(1216KB) ( 332 )   以自制硬脂酸甲基二乙醇胺双酯和γ-氯丙基甲基二甲氧基硅烷为原料,制备了酯基有机硅季铵盐(Si-QAS)。通过傅里叶红外光谱和核磁共振氢谱对产物的结构进行了表征。采用响应面分析法通过建立硬脂酸甲基二乙醇胺双酯的转化率与各因素之间的Central-Composite数学模型,对Si-QAS的合成工艺进行了优化。Si-QAS的最优制备工艺条件为:反应时间和微波功率分别为20.89 min和600 W,溶剂二甲基亚砜用量占体系总质量的33.1%。通过表面张力法测得25 ℃下产物水溶液的临界胶束浓度(cmc)为2.36×10-4 mol/L,相应的表面张力(γcmc)为24.25 mN/m,胶束化标准自由能为-30.7 kJ/mol,吸附化标准自由能为-56.0 kJ/mol。 A silicone based esterquat (Si-QAS) was prepared from γ-chloropropyl methyl dimethoxysilane and distearic ester of methyldiethanolamine as starting materials,which were prepared by the authors in the laboratory.The structure of the Si-QAS was characterized with Fourier transform infrared spectrum and 1H nuclear magnetic resonance spectrum.Meanwhile,a mathematical model for relationship between the conversion rate of distearic ester of methyldiethanolamine and its affecting factors was established to optimize the synthesis process conditions for the Si-QAS.The optimized synthesis conditions are as follows:reaction time,20.89 min;microwave power,600 W;and solvent dosage,33.1%.Physical-chemical properties were investigated and the results showed that the critical micelle concentration (cmc) of the Si-QAS is 2.36×10-4 mol/L and the corresponding γcmc is 24.25 mN/m.The standard free energy of formation for micellization and the standard adsorption free energy are -30.7 and -56.0 kJ/mol respectively. 参考文献 | 相关文章 | 计量指标

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二烯丙基甲基烷基溴化铵的合成及性能研究 Synthesis and properties of diallylmethylalkylammonium bromide 陶贤平, 张跃军, 夏胜利 2015 (8):  434-438.  doi: 10.13218/j.cnki.csdc.2015.08.004 摘要 ( 227 )   PDF(904KB) ( 350 )   以二烯丙基甲胺(DAM)和不同碳链的1-溴代烷为主要原料,合成了4种二烯丙基甲基烷基(n=4,6,8,10)溴化铵(分别标记为C4,C6,C8和C10),用IR,1HNMR和元素分析对产物结构进行了表征,并通过测定其表面活性、水溶性和絮凝性能,考察产物结构对其性能的影响。结果表明:C4~C10较佳的合成工艺条件为以丙酮为溶剂,DAM与1-溴代烷的摩尔比为1∶1.1,反应时间为64~72 h,反应温度为50~60 ℃,所得产物的收率分别为86.16%,78.02%,75.46%和68.10%。结构表征表明合成的产物为目标产物。性能测定表明随烷基链长度的增加,二烯丙基甲基烷基溴化铵的临界胶束浓度和相应的表面张力依次减小,分别为3.2×10-2,2.1×10-2,1.7×10-2和9.0×10-3 mol/L以及40.3,38.5,34.3和33.1 mN/m;水溶性好,Krafft点均小于0 ℃;对高岭土和硅藻土絮凝能力的强弱次序为C10>C8>C6>C4。 Four kinds of diallylmethylalkyl (n=4,6,8,10) quaternary ammonium salt (refers to as C4,C6,C8 and C10) were synthesized by using diallylmethylamine (DAM) and 1-bromo alkane with separate chain length as raw materials.The chemical structure of the products was characterized by IR,1HNMR and elemental analysis.Meanwhile,their surface activity,water solubility and flocculation property were examined.Results showed that the recommended better process conditions are:acetone as the solvent;molar ratio of DAM to 1-bromo alkane,1∶1.1;reaction time,64~72 h at 50~60 ℃.The product yields achieve 86.16%,78.02%,75.46% and 68.10% respectively.With the increase of the alkyl chain length,their critical micelle concentration decreases as 3.2×10-2,2.1×10-2,1.7×10-2 and 9.0×10-3 mol/L respectively;as well as their corresponding surface tension decreases as 40.3,38.5,34.3 and 33.1 mN/m respectively.All of them show good water solubility,and their Krafft points are all less than 0 ℃.Their flocculation capacity to kaolin and diatomite are in the order of C10>C8>C6>C4. 参考文献 | 相关文章 | 计量指标

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反应性高分子灭菌剂的合成和对大肠杆菌的杀灭性能 Synthesis and performance for sterilization of colon bacillus of reactive polymeric sterilants 鹿桂乾, 张利萍, 黄亮, 符若文 2015 (8):  439-442.  doi: 10.13218/j.cnki.csdc.2015.08.005 摘要 ( 245 )   PDF(780KB) ( 400 )   通过甲基丙烯酰氧乙基二甲基十二烷基溴化铵(DMAEMA-DB)、丙烯酰胺(AAm)和马来酸酐(MAn)三元共聚,将马来酸酐活性基团和长链烷基季铵盐基团同时引入大分子链中,制备了一系列的反应性高分子灭菌剂Poly(DMAEMA-DB/AAm/MAn)。用FTIR和1HNMR等表征了其结构,用JIS法测定了其阳离子度;用平板活菌计数法对各种反应性高分子灭菌剂的灭菌活性分别进行了表征,并研究了灭菌单体用量、接触时间和高分子灭菌剂的质量浓度对灭菌活性的影响。结果表明:当马来酸酐的投料摩尔分数为15%,灭菌单体DMAEMA-DB的投料摩尔分数为7%~20%时,聚合物表现出较好的灭菌活性;0.5 g/L的Poly(DMAEMA-DB/AAm/MAn) (单体摩尔比为20/65/15)表现出了快速的灭菌能力。 A series of reactive polymeric sterilants,Poly(DMAEMA-DB/AAm/MAn) were synthesized by copolymerizing dimethylaminoethyl methacrylate dodecyl ammonium bromide (DMAEMA-DB),acrylamide (AAm) and maleic anhydride (MAn) to introduce reactive maleic anhydride groups and long alkyl quaternary ammonium salt groups into macromolecules.Their structures were characterized by FTIR and 1HNMR.The cation density was determined by JIS method.The sterilizing activities of the various reactive polymeric sterilants were measured by viable cell counting method.The effects of the dosage of sterilant monomer in feed,the contact time and the mass concentration of the polymeric sterilant on sterilizing activity were investigated.Results showed that the Poly(DMAEMA-DB/AAm/Man) exhibit rather high sterilizing activity when the mole fraction of MAn is 15% in the feed and the mole fraction of DMAEMA-DB is 7%~20% in the feed;Poly(DMAEMA-DB/AAm/MAn) with mass concentration of 0.5 g/L exhibits good sterilizing activity when mass ratio of the monomers DMAEMA-DB/AAm/MAn in the feed is at 20/65/15. 参考文献 | 相关文章 | 计量指标

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基于Retinex图像增强算法的面部皮肤光泽度评价研究 Research on gloss evaluation of facial skin based on Retinex algorithm 焦志鑫, 王瑜, 王小艺, 董银卯, 孟宏, 赵华 2015 (8):  443-446.  doi: 10.13218/j.cnki.csdc.2015.08.006 摘要 ( 272 )   PDF(3494KB) ( 359 )   研究基于Retinex图像增强算法的皮肤光泽度评价方法。通过对196名志愿者进行仿真实验,构建面部皮肤图库,利用单尺度Retinex算法将读入的人脸皮肤图像S(x,y)转换成反射图像R(x,y),计算出R(x,y)的像素均值和方差值,将其与使用光泽度测试仪测出的光泽度值分别归一化,并利用相对平方误差法进行误差分析。结果表明,R(x,y)像素均值法对面部皮肤光泽度评价效果理想,误差在0.13以内。 Based on Retinex theory,an evaluation model for measuring gloss of people's facial skin was established.Via the simulation experiments on samples of 196 volunteers,a library of people's facial skin images was built,which was accessed by means of single scale Retinex algorithm to transform the readings of people facial skin images S(x,y) into reflectance images R(x,y).By this way,the mean and variance of pixels of R(x,y),which were processed in normalizing with the gloss reading given by gloss meter and the error analysis was conducted by use of relative square error method.The experimental results indicated that the evaluation on facial skin gloss by R(x,y) pixel mean method agrees with that measured by the gloss meter with an error ratio of less than 0.13.Therefore,the method can be deemed as a suitable,simple and effective way to evaluate people's facial skin gloss. 参考文献 | 相关文章 | 计量指标

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多壁碳纳米管表面苯酚印迹聚合物的制备及性能研究 Preparation and properties of phenol imprinted polymers based on multi-walled carbon nanotubes 龚超, 王翠, 刘文慧, 成斌, 范济民, 赵志换 2015 (8):  447-451.  doi: 10.13218/j.cnki.csdc.2015.08.007 摘要 ( 235 )   PDF(1274KB) ( 441 )   以聚乙二醇改性的多壁碳纳米管为基质,苯酚为模板分子,α-甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,乙腈为溶剂,偶氮二异丁腈为引发剂,结合表面分子印迹技术在碳纳米管表面合成了苯酚分子印迹聚合物。利用红外光谱和扫描电镜表征合成材料的形貌特征,结果表明,碳纳米管表面成功接枝了印迹材料。研究了印迹材料的吸附性能,此印迹材料对苯酚有特异性吸附和选择性吸附性能,印迹因子最大达到3.64,选择因子最大达到2.78,最大吸附量为44.30 mg/g,能较好的用于痕量苯酚的分离。 Phenol molecular imprinted polymer was synthesized with polyethylene glycol-modified multi-walled carbon nanotubes as the substrate,phenol as a template molecule,α-methacrylic acid as functional monomer,ethylene glycol dimethacylate as cross-linking agent and azobisisobutyronitrile as initiator in acetonitrile solution.FTIR and SEM were used to characterize the synthesis product.Results showed that the molecular imprinting polymer has been grafted to the surface of multi-walled carbon nanotubes successfully.The adsorption performance of imprinted material were examined,and results showed that the imprinted material displays specific and selective adsorption performance;the maximum imprinting factor for the template is 3.64;the maximum selectivity is 2.78 and the adsorption capacity is 44.30 mg/g.The imprinted materials can be applied for the separation of trace amount of phenol. 参考文献 | 相关文章 | 计量指标

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乳状液长期物理稳定性的评价与预测研究 Prediction and rapid evaluation of long-term physical stability of emulsions 甘亮, 张晨, 张玲, 牛玉莲, 张志伟 2015 (8):  452-456.  doi: 10.13218/j.cnki.csdc.2015.08.008 摘要 ( 291 )   PDF(1444KB) ( 488 )   对比分析了离心结合近红外和冷热循环这2种分析方法对乳剂化妆品长期物理稳定性的评价与预测,研究结果表明:离心不能加速所有不稳定过程,不同配方体系的样品,所发生的不稳定过程不同;离心结合近红外的方法可以相对准确地预判相似配方体系的样品稳定性,对于配方开发阶段的原料筛选、配方优化以及生产时的质量控制具有重要意义;而对于配方体系完全不同的样品,不能用单一的离心结合近红外测试结果来判断样品的稳定性。 Two ways for assessment and prediction of long-term physical stability of emulsion cosmetics,centrifugation in combination with near infrared irradiation and cold-hot cycling,were conducted and compared.Results showed that the unstablization process of samples generated from separate formulation systems is different and the centrifugation method cannot accelerate all kinds of the unstablization process.The centrifugation in combination with near infrared irradiation method can rather accurately predict the stability of samples with similar formulation system and makes important sense in the raw material screening and selection period and the formulation development period as well as for the quality-control in production.However,for samples of completely different formulation system,the simple centrifugation in combination with near infrared irradiation method is not sufficient to predict and judge the stability of the product. 参考文献 | 相关文章 | 计量指标

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纤维素酶活力测定条件研究及其在洗涤剂中的应用 Studies on conditions for determination of cellulase activity and its adoption for determination in cellulase formulated detergent products 于跃, 张剑, 何德志 2015 (8):  457-461.  doi: 10.13218/j.cnki.csdc.2015.08.009 摘要 ( 275 )   PDF(858KB) ( 433 )   采用纤维素酶羧甲基纤维素(CMC)酶活的测定方法,研究了温度、pH、波长及吸光度等条件对纤维素酶活力测定的影响。结果表明,在温度为50 ℃,pH=6,吸收波长为530 nm及吸光度为0.2~0.4的条件下,测得的纤维素酶活力数值较为稳定。在上述优选条件下添加液体洗涤剂和洗衣粉背景,考察该方法能否用于液体洗涤剂和洗衣粉中纤维素酶活力的测定。研究结果显示,此方法适用于液体洗涤剂和洗衣粉中纤维素酶活力的测定,但需严格控制洗涤剂或洗衣粉溶液的温度和pH。 Determination of enzymatic activity of cellulase formulated with carboxymethylcellulose (CMC) was conducted.Effect of determination conditions including enzymatic reaction temperature,pH value,wavelength and absorbance on the analysis results were studied.Results showed that under conditions for determination of cellulase activity as temperature 50 ℃,pH value 6,wavelength 530 nm and absorbance 0.2~0.4,stable analysis results can be obtained.Further studying on the cellulase formulated in laundry liquid detergent and laundry powder showed that this method is suitable for measuring cellulase activity in laundry liquid detergent and laundry powder.However,the operating temperature and pH value should be strictly controlled. 参考文献 | 相关文章 | 计量指标

专论与综述

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染发剂中禁限用染料检测方法的研究现状 Status of research work field with respect to test methods for banned and restricted dyes in hair dyes 陈梦, 周明昊 2015 (8):  462-467.  doi: 10.13218/j.cnki.csdc.2015.08.010 摘要 ( 287 )   PDF(830KB) ( 556 )   简要介绍了染发剂的分类及氧化型染发剂的作用过程和安全性问题;比较了我国与欧盟对染发剂的监管措施;重点介绍了氧化型染发剂的主要检测方法,各检测方法检测的染料种类及优缺点。 The classification as well as action process and safety issues of oxidation type hair dyes were briefed.The regulations for supervision and administration of hair dyes executed in China and the European Union were compared.The main test methods,kinds of hair dye to be detected,as well as advantages and disadvantages of the test methods for the oxidation type hair dyes were emphatically described. 参考文献 | 相关文章 | 计量指标

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荧光增白剂及其在洗涤剂和化妆品中的应用和检测研究进展 Applications of fluorescent brightener in detergent and cosmetics as well as progress in research work field for its detection technique 顾宇翔, 周泽琳, 王丁林 2015 (8):  468-473.  doi: 10.13218/j.cnki.csdc.2015.08.011 摘要 ( 323 )   PDF(1000KB) ( 665 )   综述了荧光增白剂的分类、特性、代表品种及其在洗涤剂和化妆品中的应用;概述了国内外对荧光增白剂安全性的评价;介绍了荧光增白剂在洗涤剂和化妆品中的作用、使用情况及其检验技术的研究进展;重点阐述了不同检测方法所采用的技术和注意事项;最后展望了荧光增白剂的发展趋势。 The classification,characteristics,representative varieties and applications of different types of fluorescent brightener were presented.The safety evaluation of fluorescent brightener at home and abroad was briefed.An overview of fluorescent whitening about actions and status of applications of fluorescent brighteners as well as progress in research work field for detection technique in detergents and cosmetics were reviewed.Finally,the outlook for development fluorescent brighteners was prospected. 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-四极杆飞行时间串联质谱法对α-烯烃磺酸盐的分析 Analysis of alpha olefin sulfonate by ultra-high performance liquid chromatography-quadrupole time of flight mass spectrometry 段建军, 祝愿, 滕伟林, 李晓芳 2015 (8):  474-476.  doi: 10.13218/j.cnki.csdc.2015.08.012 摘要 ( 350 )   PDF(884KB) ( 337 )   建立了阴离子表面活性剂α-烯烃磺酸盐(AOS)中多种组分(C14~18烯烃磺酸盐、C14~18羟烷基磺酸盐和少量二磺酸盐)的超高效液相色谱-四极杆飞行时间串联质谱(UPLC-Q-TOF-MS)分析方法。样品用超纯水超声溶解,过0.22 μm微孔滤膜,经Waters ACQUITY UPLC HSS C18色谱柱(150 mm×2.1 mm×1.7 μm)分离,采用电喷雾离子源(ESI)负离子模式对AOS进行四极杆飞行时间串联质谱分析,分析时间为16 min,各组分基本完全分离,可实现对AOS中多组分的定性定量分析。 An analysis method for determination of various components in anionic surfactant alpha olefin sulfonate (AOS) product (C14~18 olefin sulfonates,C14~18 hydroxyalkyl sulfonates and few disulfonate) adopting ultra-high performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-Q-TOF-MS) was established.The sample was dissolved in ultra purified water under assistance of ultrasonic irradiation and filtered with 0.22 μm micropore membrane.The filtrate was separated by Waters ACQUITY UPLC HSS C18 column (150 mm×2.1 mm×1.7 μm),and further analyzed by quadrupole time of flight mass spectrometry using electrospray ionization (ESI) negative ion mode.Analysis time is 16 min.The various components in the sample can be substantially completely separated.Via the analysis method,the content of the components with separate carbon chain length of the sample can be identified and examined. 参考文献 | 相关文章 | 计量指标