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2014年, 第44卷, 第7期　刊出日期：2014-07-22 上一期    下一期

基础研究

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双金属氢氧化物与改性海藻酸钠协同稳定液体石蜡/水乳液 Liquid paraffin/water emulsion stabilized by synergistic action of bi-metal hydroxide and modified sodium alginate 刘若林, 李嘉诚, 颜慧琼, 李晓璇, 程春风, 林强 2014 (7):  361-365.  doi: 10.13218/j.cnki.csdc.2014.07.080 摘要 ( 319 )   PDF(1768KB) ( 430 )   采用非稳态共沉淀法合成了Mg/Al双金属氢氧化物(LDH)。通过偶联酯化反应将疏水性的胆固醇(Chol)基接枝到海藻酸钠(Alg)上,制备了两亲性的改性海藻酸钠(Alg-Chol)。以Alg-Chol和LDH作为复合乳化剂,两者协同作用稳定液体石蜡/水乳液。采用傅里叶红外光谱(FTIR)、核磁共振氢谱(1HNMR)、透射电镜(TEM)、激光粒度仪(DLS)、接触角测量仪和光学显微镜等,分别对LDH,Alg-Chol和LDH/Alg-Chol水分散体系以及液体石蜡/水乳液的性能进行了表征。TEM和DLS结果显示LDH的平均粒径为159 nm,分散系数(PDI)为0.267。FTIR和1HNMR结果表明疏水性Chol基成功地接枝到Alg的侧链上。不同NaCl浓度下,LDH/Alg-Chol水分散体系在石蜡板上的接触角接近90°,说明LDH/Alg-Chol的润湿性较好,有利于增加乳液的稳定性。随着NaCl浓度的提高,乳液的粒径先由101.7 μm增大到121.8 μm,后来逐渐减小到58.1 μm。这是由于LDH/Alg-Chol在乳液液滴的表面自组装成为一层界面膜,并且LDH/Alg-Chol在油/水界面吸附量的变化影响乳液的粒径大小。 Mg/Al bi-metal hydroxide (LDH) was prepared via unsteady co-precipitation method.Hydrophobic cholesterol (Chol) was grafted onto sodium alginate (Alg) via coupling esterification to form an amphiphilic modified sodium alginate (Alg-Chol).Then the Alg-Chol and LDH was blended to be an emulsifier for synergistic stabilization of liquid paraffin/water emulsion.The LDH,Alg-Chol,LDH/Alg-Chol water dispersion,as well as liquid paraffin/water emulsion were characterized by FTIR,1HNMR,TEM,DLS,contact angle measurement and optical microscope et al.Results from TEM and DLS showed that the average size of LDH is 159 nm,and the dispersion coefficient is 0.267.Results from FTIR and 1HNMR showed that the hydrophobic Chol group has been successfully grafted onto the side chain of Alg.With different NaCl concentration,the contact angle of LDH/Alg-Chol water dispersion system on paraffin plate is near to 90°,which denotes that the wetting power of LDH/Alg-Chol is quite high and is beneficial to upgrade the stability of the emulsion.As the concentration of NaCl increases,the particle size increases from 101.7 μm to 121.8 μm,then gradually drops to 58.1 μm.This is due to the LDH/Alg-Chol self-assembles to form an interface film on the surface of the liquid particles of the emulsion and the particle size of the emulsion is affected by the change of amount of LDH/Alg-Chol adsorbed on the oil/water interface. 参考文献 | 相关文章 | 计量指标

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甲醇柴油乳液稳定性研究 Stability of methanol-diesel emulsions 李静, 焦纬洲, 刘有智, 刘文丽, 许承骋, 郭亮 2014 (7):  366-369.  doi: 10.13218/j.cnki.csdc.2014.07.081 摘要 ( 288 )   PDF(1016KB) ( 564 )   在20 ℃下,研究了复配乳化剂及助乳化剂的含量、HLB值、甲醇含量、乳化时间及转速等对甲醇柴油乳液稳定性的影响规律。研究结果表明,随着复配乳化剂及助乳化剂的含量、HLB值和转速的增大,乳液的稳定性呈现先升高后降低的趋势。随着乳化时间的延长,稳定性先升高后趋于基本稳定。随着甲醇含量的增大,乳液的稳定性逐渐降低。实验得到的适宜操作参数:乳化时间为2 min、转速为5×2 800 r·min-1、HLB值为4.5、乳化剂及助乳化剂质量分数均为3%、甲醇质量分数为15%。测得Sauter平均直径D=13 μm。 Effect of methanol content,different kinds and contents of emulsifying agent and co-emulsifying agent,HLB value,emulsifying time and stirring speed on the stability of methanol-diesel emulsions was investigated under 20 ℃.Experimental results showed that the stability of the emulsion firstly increases and then decreases with the increase of content of blend emulsifying agent and co-emulsifying agent,as well as HLB value and stirring speed.As the extension of emulsifying time,the stability of the emulsion increases firstly and then gradually reached a plateau.The stability of the emulsion decreases with the augment of the methanol content.Based upon the experimental results the suitable operating parameters were identified as:emulsifying time,2 min;stirring speed,5×2 800 r·min-1;HLB value,4.5;content of both the emulsifying agent and co-emulsifying agent,3% for each;methanol content,15%.Sauter mean diameter of the emulsion particles was measured as 13 μm. 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(Ⅶ)——表面活性剂微乳状液及其应用 Performance and applications of surfactants (Ⅶ) Surfactant micro-emulsion and its applications 张崴, 赵莉, 韩富, 徐宝财 2014 (7):  370-374.  doi: 10.13218/j.cnki.csdc.2014.07.082 摘要 ( 317 )   PDF(916KB) ( 618 )   首先介绍了表面活性剂微乳状液的3种类型及鉴别参数,对比了与乳状液性质的差异。然后对微乳状液的形成及相关理论进行了阐述。综述了微乳状液技术在化妆品、医药和采油相关设备3个方面的应用,最后对这3个方面的发展趋势进行了展望。 The classification and its parameters for discrimination of surfactant micro-emulsion were introduced.Differences of properties with conventional emulsion were compared.Formation and concerning theoretical conceptions of the surfactant micro-emulsion were described.Applications of the surfactant micro-emulsion in the fields of cosmetics,medicament and oil extraction equipment were summarized.Finally,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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驱油用磺化聚丙烯酰胺的制备及溶液性能研究 Synthesis of oil-displacing agent sulfonated polyacrylamide and performance of its aqueous solutions 杨雪, 王江红, 卢琼 2014 (7):  375-378.  doi: 10.13218/j.cnki.csdc.2014.07.083 摘要 ( 240 )   PDF(814KB) ( 309 )   采用NaHSO3-K2S2O8和偶氮二异丁脒盐酸盐(AIBA)复合引发剂体系及高低温分段引发法合成了丙烯酰胺/2-丙烯酰胺基-2-甲基丙磺酸(AM/AMPS)共聚物,通过单因素实验与正交试验考察了单体质量分数、引发剂质量分数、引发温度、pH、单体配比、引发剂配比等因素对共聚物表观黏度的影响,筛选出共聚物的最佳制备条件,即单体质量分数为25%,引发剂质量分数为0.015%,引发温度为10 ℃,pH=7,m(AM):m(AMPS)=5:1,m(K2S2O8):m(NaHSO3)=2:1,m(NaHSO3-K2S2O8):m(AIBA)=1:1,引发时间为1.5 h。耐温抗盐及热稳定性评价实验结果表明AM/AMPS共聚物的综合耐温抗盐性较好。 Copolymer acrylamide/2-acrylamide-2-methyl propylsulfonate was synthesized by using acrylamide (AM) and 2-acrylamide-2-methylpropane sulfonic acid (AMPS) as starting materials,and adopting high/low temperature two-step initiating method,with a complex initiator system which composed of NaHSO3-K2S2O8 and azo diisobutyl amidine hydrochloride (AIBA).Factors that affect the apparent viscosity of the product,such as mass fraction of reacting monomers,mass fraction of initiator,temperature,pH,ratio of monomers,ratio of initiator et al were studied by single factor experiment and orthogonal designed experiment.The optimal preparation conditions of polymers were screened as:monomer mass fraction,25%;initiator mass fraction,0.015%;initiation temperature,10 ℃;pH,7;m(AM):m(AMPS)=5:1;m(K2S2O8):m(NaHSO3)=2:1;m(NaHSO3-K2S2O8):m(AIBA)=1:1;initiating time,1.5 h.Temperature tolerance,salt resistance and thermal stability evaluation experiment results showed that the AM/AMPS copolymer product acts good comprehensive performance. 参考文献 | 相关文章 | 计量指标

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α-长链烷基甜菜碱在皂类产品中的应用性能研究 Study of application performances of α-long-chain betaine in soap products 王泽云 2014 (7):  379-382.  doi: 10.13218/j.cnki.csdc.2014.07.084 摘要 ( 261 )   PDF(800KB) ( 516 )   研究了两性表面活性剂α-长链烷基(C10,C14)甜菜碱在皂类产品中的应用性能。结果表明,皂产品中复配α-长链烷基甜菜碱后,产品的润湿力和抗硬水性能明显改善,对皮肤的刺激性显著降低,但对皂的泡沫性能无明显影响。 The application performances of α-long-chain (C10,C14) betaine in soap products were studied.Results indicated that,wetting power and resistance to hard water of soap products which blended with α-long-chain (C10,C14) betaine are improved significantly,and skin irritation is obviously reduced,but the foaming power acts no significant change. 参考文献 | 相关文章 | 计量指标

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环路反应器制备聚甘油的研究 Preparation of polyglycerol with loop reactor 耿二欢, 孙永强, 孙晋源, 张勇, Martino Di Serio 2014 (7):  383-386.  doi: 10.13218/j.cnki.csdc.2014.07.085 摘要 ( 249 )   PDF(870KB) ( 419 )   以工业甘油和自制催化剂为原料在环路反应器上制备聚甘油,通过监测反应过程中游离甘油含量和羟值的变化以确定甘油转化率和产物的平均聚合度。研究了反应温度、催化剂用量和反应器压力对甘油转化率及产品平均聚合度的影响。结果表明,环路反应器制备聚甘油的优化工艺条件为:反应温度240 ℃,催化剂用量2.0%,反应器压力0.2～0.3 MPa;此条件下甘油转化率可以达到99%以上,产品的平均聚合度能达到20以上。 Polyglycerol was prepared in a loop reactor with industrial grade glycerol as starting material and catalyst self-made in laboratory.The free glycerol content and hydroxyl value of the product were measured to determine the conversion of glycerol and the average degree of polymerization,respectively.The effects of reaction temperature,dosage of catalyst and the operating pressure on glycerol conversion and degree of polymerization were investigated.The optimal process conditions were identified as:reaction temperature,240 ℃;dosage of catalyst,2.0%;operating pressure,0.2-0.3 MPa.The conversion of glycerol could reach 99% and the polymerization degree of the product obtained is higher than 20. 参考文献 | 相关文章 | 计量指标

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无钠法合成EU-1分子筛及其催化性能 Synthesis of EU-1 zeolite without use of sodium hydroxide and its catalytic performance 张燕挺, 李晓峰, 贾妙娟, 景超, 孙晓涛, 窦涛 2014 (7):  387-389.  doi: 10.13218/j.cnki.csdc.2014.07.086 摘要 ( 283 )   PDF(1462KB) ( 450 )   分别以四甲基氢氧化铵(TMAOH)、四乙基氢氧化铵(TEAOH)和氢氧化钠(NaOH)为碱源合成了EU-1分子筛,采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、氨气程序升温脱附(NH3-TPD)和低温N2吸附等对合成样品进行了表征,并以二甲苯异构化反应表征其催化性能。结果表明:与以NaOH为碱源相比,采用TMAOH和TEAOH可一步合成铵型EU-1分子筛,以TEAOH为碱源合成样品的粒径在200~500 nm之间,比表面积高达390.2 m2·g-1。 EU-1 zeolites were successfully synthesized with three different alkali sources[tetramethylammonium hydroxide (TMAOH),tetraethylammonium hydroxide (TEAOH) and sodium hydroxide (NaOH)].Structure of the product samples obtained were characterized by XRD,SEM,NH3-TPD and BET methods.Their catalytic performance was evaluated through xylene isomerization reaction.The results showed that as comparing with the process that adopting NaOH as alkali source,the process adopting TMAOH or TEAOH can produce ammonium type EU-1 zeolite in one step.Particle size of the product obtained from the process adopting TEAOH as alkali source is in range of 200-500 nm,and its specific surface area achieves as high as 390.2 m2·g-1. 参考文献 | 相关文章 | 计量指标

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阳离子田菁胶的合成及性能研究 Synthesis and performance of cationic sesbania gum 李东虎, 曹光群, 董伟 2014 (7):  390-393.  doi: 10.13218/j.cnki.csdc.2014.07.087 摘要 ( 281 )   PDF(892KB) ( 325 )   以田菁胶(SG)为原料,3-氯-2-羟丙基三甲基氯化铵(CHPAC)为醚化剂,氢氧化钠为催化剂,异丙醇水溶液为分散剂,合成阳离子田菁胶。讨论了影响阳离子田菁胶取代度的主要因素,得出较优的合成条件为:n(NaOH)/n(SG)=0.4,n(CHPAC)/n(SG)=0.5,碱化温度20 ℃,碱化时间50 min,醚化温度50 ℃,醚化时间4 h,制得阳离子田菁胶的取代度为0.45。将阳离子田菁胶添加到洗发水中进行梳理性测试,结果表明其具有较好的调理性能。 Cationic sesbania gum (CSG) was synthesized by sesbania gum (SG) and 3-chloro-2-hydroxypropyltrimethylammonium chloride (CHPAC) as starting materials with sodium hydroxide as catalyst.The reaction was performed in isopropyl alcohol aqueous solution.Main factors that affect the substitution degree of CSG were investigated.The optimum reaction conditions are as follows:n(NaOH)/n(SG),0.4;n(CHPAC)/n(SG),0.5;alkalization temperature,20 ℃;alkalization time,50 min;etherification temperature,50 ℃;etherification time,4 h.Under these conditions the substitution degree of CSG achieves 0.45.CSG product was formulated into shampoo and the test results show excellent combing performance. 参考文献 | 相关文章 | 计量指标

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丝胶蛋白酶解产物的保湿与美白作用研究 Moisturizing performance and whitening efficacy of sericin enzymatic hydrolysis product 靳春平, 杨明英, 朱良均 2014 (7):  394-397.  doi: 10.13218/j.cnki.csdc.2014.07.088 摘要 ( 307 )   PDF(906KB) ( 443 )   以蚕茧层中提取的丝胶蛋白及其酶解产物(丝胶蛋白肽)为研究对象,测定不同分子质量丝胶蛋白肽的保湿性能和对皮肤的美白作用等。结果表明,0～14 h内,质量分数为5%的丝胶蛋白肽保湿性能优于甘油,且质量分数为10%和15%的丝胶蛋白肽的保湿性均在80%以上;丝胶蛋白肽对皮肤具有一定的美白效用。 Functions of sericin and its enzymatic hydrolysis product (sericin peptide) were studied as the object.Moisturizing performance of sericin peptides with different molecular weight as well as their skin whitening efficacy was measured and determined.Results showed that moisturizing performance of sericin peptide with mass fraction of 5% is better than that of glycerol within time period of 0-14 h;while moisturizing performance of sericin peptide with mass fraction of 10% and 15% can achieve an extent higher than 80%.Further,test result showed that the sericin peptide displays certain skin whitening efficacy. 参考文献 | 相关文章 | 计量指标

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包封维生素E脂质体的研究 Study on liposome for encapsulating VE 刘本娜, 许虎君, 李芳芳, 毛建明 2014 (7):  398-401.  doi: 10.13218/j.cnki.csdc.2014.07.089 摘要 ( 326 )   PDF(933KB) ( 331 )   采用超声法制备包封维生素E的脂质体,以包封率和粒径为衡量标准,通过单因素实验确定较优的实验条件为:m(大豆卵磷脂):m(维生素E):m(胆固醇):m(聚乙烯醇)=6:3:3:2,V(氯仿):V(水)=1:3,且体系中维生素E的质量分数为8.8%,超声2 min。此条件下包封率可达86.8%,平均粒径为62.9 nm;所得脂质体呈圆球状,储存在4 ℃下较适宜。 Preparation of liposome for encapsulating VE was conducted under assistance of ultrasonic wave.Extent of encapsulation and particle size were taken as evaluation criteria.Via single factor experiments,relatively better conditions were identified.Mass ratio of the ingredients is:m(soybean lecithin):m(VE):m(cholesterol):m(polyvinyl alcohol)=6:3:3:2.Volume ratio of solvents is:V(chloroform):V(water)=1:3.The mass fraction of VE is 8.8% in system.Ultrasonic treatment time is 2 min.Extent of encapsulation achieves 86.8% with particle size of 62.9 nm under above conditions,and the shape of the liposome product is round balls.Suitable temperature for storing the liposome product is recommended as 4 ℃. 参考文献 | 相关文章 | 计量指标

专论与综述

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化妆品用变性淀粉的研究进展 Progress in research work with respect to modified starch used for cosmetics 王文, 黄继红, 游倩倩, 冯军伟, 苏雪锋, 杨明乾 2014 (7):  402-405.  doi: 10.13218/j.cnki.csdc.2014.07.090 摘要 ( 394 )   PDF(813KB) ( 661 )   综述了化妆品用变性淀粉的研究进展。重点讨论了化妆品用变性淀粉的制备方法,阐述了变性淀粉的主要功能特性及其在化妆品中的应用优势,并对变性淀粉应用于化妆品的未来发展趋势进行了展望。 Progress in research work with respect to modified starch used for cosmetics was reviewed.Preparation methods for modified starch were focused.Main characteristics of modified starch and its benefits for application in cosmetics were described,and the future development trend of modified starch used in cosmetics was forecasted. 参考文献 | 相关文章 | 计量指标

分析与检测

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液相色谱-四极杆/离子阱串联质谱法测定牙膏中的绿原酸 Detection of chlorogenic acid in toothpaste by liquid chromatography coupled to quadrupole/linear ion trap tandem mass spectrometry 马晓斐, 宋炜, 梁天佐, 贾振国, 冯浩彬, 张岩 2014 (7):  406-409.  doi: 10.13218/j.cnki.csdc.2014.07.091 摘要 ( 246 )   PDF(830KB) ( 336 )   建立了液相色谱-四极杆/离子阱串联质谱(LC-QTRAP-MS/MS)测定牙膏中绿原酸的方法。试样经超声提取,Kinetex C18色谱柱(2.1 mm×100 mm,2.6 μm)分离,以甲醇-0.1%甲酸水溶液为流动相洗脱,采用多反应监测(MRM)-信息依赖性采集(IDA)-增强子离子扫描(EPI)模式检测,外标法定量。结果表明,绿原酸在质量浓度为1.0～100 μg·L-1范围内线性关系良好(r=0.999 6),方法检出限为10.0 μg·kg-1,在低、中、高3个添加水平时的平均回收率为85.6%~96.6%,相对标准偏差均不大于5.8%。 A comprehensive method for detection of chlorogenic acid in toothpaste was established with liquid chromatography coupled to quadrupole/linear ion trap tandem mass spectrometry (LC-QTRAP-MS/MS).The samples were extracted under ultrasonic assistance.The separation was carried out on a Kinetex C 18 column (2.1 mm×100 mm,2.6 μm) using mobile phases of methanol-0.1% formic acid solution as eluant.A multiple reaction monitoring (MRM) in negative mode as survey scan and an enhanced production (EPI) scan as dependent scan in an information-dependent acquisition (IDA) experiment was adopted in mass spectrometry acquisition.External standard was employed for the quantification.Test results showed that content of the chlorogenic acid displays good linearity within 1.0～100 μg·L-1 vs.the peak area of the chromatogram with a correlation coefficient (r) of 0.999 6.The limit of detection for the chlorogenic acid is 10.0 μg·kg-1.The mean recoveries at the three spiked levels are 85.6%~96.6%,and the relative standard deviations are not higher than 5.8%. 参考文献 | 相关文章 | 计量指标

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离子色谱法测定牙膏中的亚硫酸盐含量 Determination of sulfite content in toothpaste by ion chromatography 郭长虹, 夏泽敏, 谭建华, 李慧勇, 席绍峰, 王继才, 熊小婷, 赵田甜 2014 (7):  410-412.  doi: 10.13218/j.cnki.csdc.2014.07.092 摘要 ( 232 )   PDF(796KB) ( 314 )   建立了离子色谱法检测牙膏中亚硫酸盐含量的方法。以甲醛溶液为SO2-3稳定剂,样品采用10 mmol·L-1 NaOH水溶液提取后,以Metrosep Supp 5-250为色谱柱,淋洗液为V(3.2 mmol·L-1 Na2CO3+1.0 mmol·L-1 NaHCO3):V(丙酮)=88:12的混合溶液,流速0.5 mL·min-1,进样体积 20 μL。结果表明,亚硫酸盐在0.10～10 mg·L-1内线性关系良好,相关系数为0.999 9,样品基质加标的回收率为84.7%～90.1%,相对标准偏差为1.06%～3.18%,样品中亚硫酸盐的检出限为5 mg·kg-1。 A method was established for the determination of sulfite content in toothpaste by ion chromatography.With formaldehyde solution as stabilizing agent of SO2-3,samples were extracted with 10 mmol·L-1 sodium hydroxide solution and were separated on a Metrosep Supp 5-250 chromatographic column using solution of V(3.2 mmol·L-1 Na2CO3+1.0 mmol·L-1 NaHCO3):V(acetone)=88:12 as the eluent.The flow rate was 0.5 mL·min-1 and the injection volume was 20 μL.With this method,range with good linearity for sulfite was 0.10~10 mg·L-1 with the correlation coefficient of 0.999 9.The recoveries,relative standard deviations and detection limits were 84.7%-90.1%,1.06%-3.18% and 5 mg·kg-1 respectively. 参考文献 | 相关文章 | 计量指标

生产与技术

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滚筒洗衣机与波轮洗衣机的洗涤性能比较 Comparison of laundry performance of front load washing machine and top load washing machine 王燕飞 2014 (7):  413-416.  doi: 10.13218/j.cnki.csdc.2014.07.093 摘要 ( 370 )   PDF(949KB) ( 458 )   以衣物洗涤剂的全规模洗涤评价方法为基础,对比了滚筒洗衣机和波轮洗衣机在多种消费者相关技术污布上的洗涤力差异。实验结果表明,滚筒洗衣机洗涤程序持续时间更长,且耗水量更少,为波轮洗衣机的1/3。在相同洗涤剂质量浓度及洗涤温度条件下,所有洗涤剂样品在滚筒洗衣机中的去污力表现明显高于在波轮洗衣机中的表现。滚筒洗衣机的主洗时间更长,能够使洗涤剂中各组分的功能发挥得更为充分。 Based upon results of full-scale washing test method for detergency evaluation,differences of detergency performance on technical stain swatches obtained from front load washing machine and top load washing machine were compared.The test results indicated that the front load washing machine takes a longer operating time duration while consumes less water about 1/3 of that of the top load washing machine.Under same conditions such as detergent mass concentration and operating temperature,the detergency displayed by the front load washing machine is significantly higher than that by the top load washing machine.Longer main washing cycle of the front load washing machine is beneficial to bring action of ingredients of the detergent into full play. 参考文献 | 相关文章 | 计量指标