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2016年, 第46卷, 第6期　刊出日期：2016-06-22 上一期    下一期

基础研究

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GSS362/TX-100复配体系在水中的溶液行为研究 Behavior of blend of GSS362/TX-100 in aqueous solution 喻红梅, 刘骏峰, 华平, 李建华, 朱成龙, 王灵光 2016 (6):  305-308.  doi: 10.13218/j.cnki.csdc.2016.06.001 摘要 ( 350 )   PDF(816KB) ( 405 )   研究了1,3-丙二醇双子琥珀酸二异辛酯磺酸钠(GSS362)和辛基酚聚氧乙烯醚(TX-100)复配物在水中的表面性质和胶束化行为,并对理想混合临界胶束浓度以及混合体系中各组分在表面吸附层和胶束中的组成、相互作用参数和热力学参数进行分析计算。结果表明,复配物在水溶液中不存在协同效应,但是TX-100的加入明显降低了GSS362的临界胶束浓度,混合胶束的形成为自发过程,胶束中GSS362与TX-100分子具有较弱的相互作用,胶束中富含非离子表面活性剂TX-100。 The surface properties and micellization behavior of blend of 1,3-propanediol Gemini sodium bis-isooctyl succinyl ester sulfonate (GSS362) and octylphenol ethoxylate (TX-100) in aqueous solution were investigated.The cmc of ideal mixed surfactants and the composition as well as the interaction parameters and thermodynamic parameters of separate components in the surface adsorption layer as well as in the micelles were also examined and calculated.Results showed that:no synergistic effect of the blend surfactants is found in the aqueous solution;however,with the addition of TX-100,the cmc of the blend surfactants decreases apparently as comparing to that of GSS362 alone;the formation of mixed micelle is spontaneous and the molecular interaction between GSS362 and TX-100 is weak;TX-100 is enriched in the micelles of the blend surfactants. 参考文献 | 相关文章 | 计量指标

科技讲座

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氟表面活性剂和氟聚合物(Ⅵ)——“弱位点”氟表面活性剂的合成 Fluorinated surfactants and fluoropolymers (Ⅵ) Synthesis of fluorinated surfactants with weak point 邢航, 陈现涛, 肖进新 2016 (6):  309-313.  doi: 10.13218/j.cnki.csdc.2016.06.002 摘要 ( 314 )   PDF(870KB) ( 380 )   重点综述了具有潜在非生物累积性的氟表面活性剂的近期合成策略,包括:CF3-X-(CH2)n-SO3Na (X=O,C6H4O或N(CF3),n=8~12)的制备;通过六氟环氧丙烷(HFPO)寡聚或氟化氧杂环丁烷的开环阳离子寡聚合成含氟聚醚;偏氟乙烯(VDF)与全氟烷基碘发生调聚反应生成CnF2n+1-(VDF)2-CH2COOR (n=2或4,R=H或NH4);3,3,3-三氟丙烯(TFP)与全氟烷基碘进行自由基调聚反应制备相应的表面活性剂;VDF与TFP在全氟烷基碘存在下的自由基共调聚,或它们在氟化黄原酸酯存在下的可控自由基共聚。进一步综述了这些含弱位点氟烷基醚物质的降解性和安全性以及作为PFOS和PFOA替代品的问题。 Recent strategies for synthesis of fluorosurfactants that may be potentially non-bioaccumulable were reviewed.These routes are devoted on:(ⅰ) preparation of CF3-X-(CH2)n-SO3Na [with X=O,C6H4O or N(CF3) and n=8-12];(ⅱ) synthesis of fluorinated polyethers either by oligomerization of hexafluoropropylene oxide (HFPO) or by ring opening cationic oligomerization of fluorinated trimethylene oxide;(ⅲ) telomerization of vinylidene fluoride (VDF) with 1-iodoperfluoroalkanes to produce CnF2n+1-(VDF)2-CH2COOR (n=2 or 4,R=H or NH4);(ⅳ) free radical telomerization of 3,3,3-trifluoro-propene (TFP) and 1-iodoperfluoroalkanes to prepare corresponding surfactants;(ⅴ) free radical co-telomerization of VDF and TFP in presence of 1-iodoperfluoroalkanes,or their controlled free radical co-polymerization in presence of fluorinated xanthate.The degradability and safety of these fluorinated ethers with weak point and their problems for being used as replacing products for PFOS and PFOA were summarized. 参考文献 | 相关文章 | 计量指标

开发与应用

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响应面法优化咪唑啉硫酸酯盐的合成及性能研究 Optimization of synthesis of imidazoline sulfate salt by response surface method and study of its performance 郭睿,程敏,杨江月,李欢乐,刘爱玉 2016 (6):  314-319.  doi: 10.13218/j.cnki.csdc.2016.06.003 摘要 ( 256 )   PDF(2453KB) ( 345 )   以氨基磺酸为硫酸化试剂,月桂酸和羟乙基乙二胺为原料,尿素为催化剂,合成了咪唑啉硫酸酯盐。利用IR和1H NMR对合成产物的结构进行了表征。在单因素试验的基础上,利用响应面法优化硫酸酯盐的合成工艺条件,确定较佳工艺条件为:反应温度107 ℃、反应时间3.7 h、n(咪唑啉)∶n(氨基磺酸)=1∶1.09、催化剂用量为反应物总质量的2.93%,在此条件下咪唑啉硫酸酯盐的产率为75.20%。同时测定了咪唑啉硫酸酯盐的表面活性及泡沫性能,测试结果表明,合成的咪唑啉硫酸酯盐具有良好的表面活性和泡沫性能。 Under the catalysis of urea,a kind of imidazoline sulfate salt was synthesized with amino sulfonic acid as the sulfating reagent,lauric acid and N-hydroxyethyl-ethylenediamine as starting materials.The chemical structure of the target product was characterized by IR and 1H NMR.Based upon results obtained from single factor experiments and in combination with response surface method,the optimal synthesis conditions were determined as:n(imidazoline)∶n(amino sulfonic acid)=1∶1.09;reaction temperature,107 ℃;reaction time,3.7 h;dosage of the catalyst,2.93% of the total mass of the reactants.Under the above-mentioned conditions,the reaction yield achieves 75.20%.Surface activity and foaming performance of the product were measured.The results showed that imidazoline sulfate salt displays good surface activity and foaming performance. 参考文献 | 相关文章 | 计量指标

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泡沫复合驱用癸基糖苷磺酸盐的合成及性能研究 Synthesis and performance of decyl polyglycoside sulfonate for foam blended flooding agent 邹新源,罗文利,马德胜,周新宇,田茂章 2016 (6):  320-323.  doi: 10.13218/j.cnki.csdc.2016.06.004 摘要 ( 246 )   PDF(852KB) ( 347 )   以癸基葡萄糖苷(C10APG)和3-氯-2-羟基丙烷磺酸钠为原料反应制得癸基糖苷磺酸盐(C10APGS),用FT-IR和ESI-MS对产物进行了表征,并对其泡沫性能和吸附性进行了测定。结果表明:C10APGS表现出良好的发泡能力和泡沫稳定性,其发泡率和排液半衰期随C10APGS质量分数的增加而增加,当质量分数增加到0.4%后,发泡率和排液半衰期增速变缓;随着二价盐质量分数的增加,C10APGS的发泡率变化不大,但对泡沫稳定性产生明显的影响,当二价盐质量分数增加到8%时,C10APGS仍表现出良好的耐盐性能;相对于C10APG,C10APGS的饱和吸附损失量降低了14.4%,可作为较理想的发泡剂应用于高盐油藏的泡沫复合驱。 Decyl polyglycoside sulfonate (C10APGS) was prepared with decyl polyglycoside (C10APG) and sodium 3-chloro-2-hydroxypropanesulfonate as starting materials.Chemical structure of the product was characterized by FT-IR and ESI-MS,and the foam performance,adsorption capacity of the product were also investigated.Results showed that the foaming power and foam stability of C10APGS are very well,and the foaming power and the draining half-life period increase with the increase of C10APGS mass fraction,while as C10APGS mass fraction exceeds 0.4% the trend of the increment of the foaming power becomes slower.As the mass fraction of the divalent salts increases,the foaming power changes insignificantly,while the foam stability drops significantly.Even in case that the mass fraction of the divalent salts achieves up to 8%,C10APGS still displays good salt tolerance.The adsorption loss of C10APGS reduces by 14.4% as comparing with that of C10APG and can be used as a rather satisfiable component in foam blended flooding agent for application in high salinity crude oil mines. 参考文献 | 相关文章 | 计量指标

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烷基糖苷羟丙基磺酸盐和咪唑啉复配性能研究 Performance of blend systems based on alkyl hydroxypropyl polyglucoside sulfonates and imidazoline 董庆文,张威,樊伟,王丰收,董万田 2016 (6):  324-327.  doi: 10.13218/j.cnki.csdc.2016.06.005 摘要 ( 289 )   PDF(800KB) ( 376 )   研究了烷基糖苷羟丙基磺酸盐阴离子表面活性剂(APGHPS)和咪唑啉两性离子表面活性剂(IMD)复配体系的稳定性、表面活性、泡沫性能、润湿性能和耐硬水性能。结果表明:APGHPS和IMD复配体系稳定性好;复配体系表现出良好的协同增效作用,当n(APGHPS)∶n(IMD)=1∶1时,增效作用最为明显,此时临界胶束浓度cmc=8.81×10-5 mol/L,最低表面张力γcmc=26.2 mN/m,均低于单一组分;复配体系的泡沫性能、润湿性能和耐硬水性能都较单一组分表面活性剂有所提高。 Performance of blend systems composed of anionic surfactant alkyl hydroxypropyl polyglucoside sulfonates (APGHPS) and amphoteric surfactant imidazoline (IMD) such as stability,surface activity,foam performance,wetting power,and hard water endurance were investigated.It was found that the blend system of APGHPS and IMD has a good compatibility and a strong synergic effect.When the molar ratio between APGHPS and IMD is 1∶1,the blend system shows the strongest synergic effect.The minimum value of critical micelle concentration (cmc) and the surface tension at cmc (γcmc) of the blend system is 8.81×10-5 mol/L and 26.2 mN/m respectively,which is much lower than that of each single component in the blend system.The foam performance,wetting power and hard water endurance are also better than that of each single component in the blend system. 参考文献 | 相关文章 | 计量指标

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CO2/N2开关微乳液及其油污洗涤和分离性能 CO2/N2-switchable microemulsion as well as its oil dirt washing and separation performance 黄曼,李灿琪,刘雪锋 2016 (6):  328-333.  doi: 10.13218/j.cnki.csdc.2016.06.006 摘要 ( 217 )   PDF(3486KB) ( 324 )   采用等摩尔的十二烷基苯磺酸钠与N-十二烷基-N,N-二甲基叔胺为主乳化剂,正丁醇为助乳化剂,正庚烷为油相,制得O/W型微乳液。在CO2/N2交替作用下,可实现微乳液-相分离-微乳液的可逆转换;原始微乳液与复原微乳液半径分别为(10.89±0.21)和(11.50±0.47) nm。该微乳液对多孔固体和织物表面烃类矿物油的洗油率分别为99.13%±0.32%和98.30%±0.28%,对油砂表面原油的洗油率为54.52%±0.25%。活性物质量分数相等时,微乳稀释液对织物表面油性记号笔渍的去污力是市售洗衣粉的1.90倍;而微乳原液的去污力是市售洗衣粉的2.02倍。洗后含油废液通入CO2可迅速实现油水分层,分离油相后的残余水相经阴、阳离子交换树脂和活性炭常规处理,COD和TOC分别为40.62和17.51 mg/L,符合GB 18918-2002中一级水排放标准(COD≤100 mg/L,TOC≤20 mg/L)。 To obtain an O/W microemulsion,blend of sodium dodecyl benzene sulfonate and N,N-dimethyl-N-dodecyl tert-amine with equimolar ratio was used as main emulsifier,butanol as co-emulsifier and n-heptane as oil phase.The reversible conversion of microemulsion-phase separated liquid-microemulsion can be realized by alternate action of CO2 and N2.The radii of the original and recovered microemulsion are (10.89±0.21) and (11.50±0.47) nm respectively.The oil removal rate for mineral oil on porous solid,textiles and industrial crude oil sand are 99.13%±0.32%,98.30%±0.28% and 54.52%±0.25% respectively.On an equal mass fraction basis,the removal rate of soil made by mark pen of the diluted microemulsion to that of laundry powder from market achieves 1.90 while that of the microemulsion without dilution achieves 2.02.The phase separation of oil containing waste liquid could be quickly and completely realized by bubbling of CO2.After separating the oil phase,the water phase left was treated with anion and cation exchange resins and activated carbon.The values of chemical oxygen demand (COD) and total organic carbon (TOC) of the waste water drop to 40.62 and 17.51 mg/L respectively,which are in conformity with the first class standard of discharged water (COD≤100 mg/L,TOC≤20 mg/L) according to GB 18918-2002. 参考文献 | 相关文章 | 计量指标

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十二烷基硫酸钠对角质细胞基因表达的影响及作用通路研究 Study with respect to effect of sodium dodecyl sulfate on gene expression of keratinocytes and its signaling pathway 赵丹,苏宁,张佳婵,李萌,霍彤,王昌涛 2016 (6):  334-338.  doi: 10.13218/j.cnki.csdc.2016.06.007     摘要 ( 169 )   PDF(1370KB) ( 261 )   利用人全基因表达谱芯片对十二烷基硫酸钠(SDS)刺激后的角质细胞总RNA进行检测,研究SDS刺激对角质细胞基因表达的影响及作用通路,并对可能引发的疾病进行预测。SDS刺激引起角质细胞中605个基因表达显著上调,368个基因显著下调。主要通过TNF信号通路进行信号传导,经分析筛选出10个关键差异表达基因,包括IL-6,TNF,CCL5,CCL20,CXCL8,CXCL3,CSF2,CSF1,TNFAIP3和NLRC4,以上基因表达异常会促进炎症的发展并激活免疫系统。SDS刺激可能引发特应性皮炎并对过敏与自身免疫疾病有促进作用。 Detection of total RNA of keratinocytes after irritation of sodium dodecyl sulfate (SDS) was conducted utilizing human mRNA micro array to study the effect of SDS on gene expression of keratinocytes and its signaling pathway,as well as to predict the possibility of inducing disease by the SDS.Results showed that expression of 605 genes are significantly up regulated and 368 genes are significantly down regulated after exposing to SDS.The signals are transformed mainly by TNF signaling pathway.Ten critical genes (IL-6,TNF,CCL5,CCL20,CXCL8,CXCL3,CSF2,CSF1,TNFAIP3 and NLRC4) are screened by the pathways.Abnormal expression of these genes will affect the development of inflammation and activation of immunity.Possibly,irritation of SDS may cause atopic dermatitis as well as promotion of allergies and autoimmune disease. 参考文献 | 相关文章 | 计量指标

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利用3D皮肤模型研究不同分子量透明质酸的抗刺激作用 Study of anti-irritation effect of hyaluronic acid using 3D skin model 喻欢,陈彧,程树军,秦瑶 2016 (6):  339-343.  doi: 10.13218/j.cnki.csdc.2016.06.008 摘要 ( 263 )   PDF(3346KB) ( 326 )   将十二烷基硫酸钠(SDS)和不同分子量的透明质酸(HA)共同作用于人永生化表皮细胞(HaCaT)和3D皮肤模型,作用24 h后通过MTT比色法检测细胞活性,利用ELISA方法检测培养液中人白细胞介素(IL-1α)的水平,并进行组织学观察细胞形态。研究在不同实验模型中,不同分子量HA影响SDS对细胞的损伤和释放IL-1α的差异。结果表明,3D皮肤模型可用于HA的体外抗皮肤刺激作用的研究,实验结果更接近人体实际使用情况以及能提供更多的机制信息。 Sodium dodecyl sulfate (SDS) mixed with hyaluronic acid (HA) of separate molecular weight were applied on HaCaT cells and 3D skin model separately.After action of 24 h,the cell viability was detected by MTT assay and the level of IL-1α by ELISA method.The difference of exogenous effect of HA to reduce irritation induced by SDS on cell viability and IL-1α releasing between the two in vitro test models was studied.In conclusion,3D skin model can be used to test the anti-irritation effect of HA in vitro.Meanwhile,the exposure and testing results of 3D skin model are more close to human situation and can provide further mechanism information as comparing with the monolayer cell. 参考文献 | 相关文章 | 计量指标

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H4GeW12O40/Cu3(BTC)2催化Biginelli反应合成3,4-二氢嘧啶-2(1H)-酮衍生物 Synthesis of 3,4-dihydropyrimidine-2(1H)-one derivatives via Biginelli reaction with H4GeW12O40/Cu3(BTC)2 as catalyst 龚文朋,马海芹,周州,杨水金 2016 (6):  344-348.  doi: 10.13218/j.cnki.csdc.2016.06.009 摘要 ( 194 )   PDF(1890KB) ( 502 )   采用浸渍法以金属有机骨架Cu3(BTC)2负载锗钨酸(H4GeW12O40)制备H4GeW12O40/Cu3(BTC)2催化剂,并用该催化剂催化芳醛、尿素和乙酰乙酸乙酯通过“一锅法”Biginelli缩合反应,以无水乙醇为溶剂,合成6种3,4-二氢嘧啶-2(1H)-酮衍生物;通过熔点的测定,IR,1H NMR和MS等对产物3,4-二氢嘧啶-2(1H)-酮衍生物进行表征。结果表明:在芳醛用量为0.04 mol,n(芳醛)∶n(乙酰乙酸乙酯)∶n(尿素)=1∶1.5∶1.5,催化剂的用量占反应物料总质量的4.0%,反应温度为90 ℃,反应时间为90 min的条件下,目标产物收率可达63.0%~76.3%。 Six kinds of 3,4-dihydropyrimidine-2(1H)-one derivative were prepared via Biginelli-type condensation by one-pot method with ethyl acetoacetate,aromatic aldehyde and urea as starting materials,anhydrous ethanol as solvent and H4GeW12O40/Cu3(BTC)2 as catalyst.The catalyst was prepared by loading of germanic-tungstic acid on metal organic skeleton by impregnation method.Structures of the target compounds were characterized by melting point determination,1H NMR,IR,and MS.The experimental results showed that,under the conditions of fixed aromatic aldehyde feed of 0.04 mol;n(aromatic aldehyde)∶n(ethyl acetoacetate)∶n(urea)=1∶1.5∶1.5;the dosage of catalyst at 4.0% of total mass of the starting materials;reaction temperature at 90 ℃;and reaction time of 90 min;the yield of the target products achieves 63.0%-76.3%. 参考文献 | 相关文章 | 计量指标

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4种中草药乙醇提取物体外抗氧化及美白活性研究 Test for antioxidation and whitening activity of ethanol extract from four kinds of Chinese herbal medicine in vitro 黄立森,庞海月,吴黉坦,叶子坚,王鹏,王贵弘 2016 (6):  349-352.  doi: 10.13218/j.cnki.csdc.2016.06.010 摘要 ( 282 )   PDF(687KB) ( 396 )   采用乙醇浸提法从干燥的芦荟叶、白芷、怀山药和黄芩4种中草药中提取分离得到其乙醇提取物。应用自由基清除活性和总抗氧化活性检测方法评估这4种中草药乙醇提取物的抗氧化活性,应用酪氨酸酶活性抑制实验、黑色素B16细胞增殖抑制和黑色素生成抑制实验对其进行美白活性评估。结果表明:4种中草药的乙醇提取物虽然具有一定的抗氧化活性、清除自由基能力、抑制酪氨酸酶活性、抑制黑色素B16细胞增殖和黑色素形成作用,但与市售护肤品常用的抗氧化美白功效成分BHT(2,6-二叔丁基-4-甲基苯酚)相比,其活性水平偏低,需要进一步分离纯化,富集活性成分,提高抗氧化美白活性。 Extracts,with ethanol as solvent,from 4 kinds of Chinese herbal medicine (dried aloe leaves,Angelica dahurica,Huaiqing yam and Radix scutellariae) were assessed for their antioxidation activity by free radical scavenging activity detection method and total antioxidation activity detection method.Meanwhile,their human skin whitening activity was assessed by tyrosinase inhibition test,B16 melanoma cells proliferation inhibition test and melanin formation inhibition test.The results showed that although the aforesaid four kinds of Chinese herbal medicine extract display certain antioxidation and free radical scavenging activity as well as tyrosinase inhibition activity,B16 melanoma cells proliferation inhibition and melanin formation inhibition capacity;however,as comparing with BHT (2,6-di-tert-butyl-4-methylphenol) that containing in conventional skin care cosmetic products from the market,their antioxidation and whitening effect are lower.So it is necessary to separate and purify the ethanol extracts for enriching the active ingredients,as well as to improve their antioxidation and whitening activity. 参考文献 | 相关文章 | 计量指标

专论与综述

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α-蒎烯催化环氧化研究进展 Progress of catalytic α-pinene epoxidation 王中天,于凤丽,袁冰,解从霞,于世涛 2016 (6):  353-358.  doi: 10.13218/j.cnki.csdc.2016.06.011 摘要 ( 334 )   PDF(771KB) ( 426 )   从使用不同氧化剂的角度,综述了近年来国内外α-蒎烯环氧化反应的研究进展,列举了α-蒎烯环氧化中分别以过氧乙酸、烃基过氧化氢、非金属氧酸盐、H2O2和O2作为氧化剂时的优缺点,重点介绍了以环境友好的H2O2和O2为氧化剂的α-蒎烯环氧化反应。 In view of different oxidants,the advances of the catalytic epoxidation of α-pinene in recent years were summarized.The advantages and disadvantages of various oxidants such as acetic acid peroxide,hydrocarbonyl hydrogen peroxide,nonmetallic oxygen acid salt,H2O2 and O2 respectively as an oxidizing agent in the α-pinene epoxidation were listed.The epoxidation of α-pinene conducted by environmentally friendly oxidant H2O2 and O2 was emphatically introduced. 参考文献 | 相关文章 | 计量指标

分析与检测

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高效液相色谱-质谱法同时测定染发剂中33种禁限用染料 Simultaneous determination of 33 kinds of banned and/or restricted component in hair dyes by high performance liquid chromatography-mass spectrometry 陈梦,胡磊,许立,周明昊 2016 (6):  359-364.  doi: 10.13218/j.cnki.csdc.2016.06.012 摘要 ( 223 )   PDF(748KB) ( 344 )   建立了高效液相色谱-质谱(HPLC-MS/MS)同时测定染发剂中33种禁限用染料的方法。样品用甲醇和2 g/L抗坏血酸水溶液的混合溶液溶解,正己烷净化,以5 mmol/L的乙酸铵水溶液和乙腈为流动相进行梯度洗脱,经Agilent ZORBAX Extend C18柱(2.1 mm×100 mm,1.8 μm)分离。在电喷雾离子模式下,采用多重反应监测模式(MRM)进行定性和定量分析。33种染料在相应的质量浓度范围内线性关系良好,线性相关系数均大于0.99,检出限为0.01~29.5 mg/kg,回收率为71%~115%。 A high performance liquid chromatography-mass spectrometry (HPLC-MS/MS) method was established for simultaneous determination of 33 kinds of banned and/or restricted component in hair dyes.After extracted by mixed solution with methanol and 2 g/L ascorbic acid aqueous solution,purified by n-hexane,the samples were analyzed by HPLC-MS/MS.The separation was performed on an Agilent ZORBAX Extend C18 column (2.1 mm×100 mm,1.8 μm) and gradient eluted with aqueous solution of 5 mmol/L ammonium acetate and acetonitrile.The electro spray ionization source in positive and negative ion mode was used for qualitative and quantitative analysis of the 33 components under the multiple reaction monitoring mode (MRM).The results show good linear relationships with all correlation coefficients higher than 0.99.The limits of detection for the 33 components are in the range of0.01-29.5 mg/kg.The average spiked recoveries of the 33 components are in the range of 71%-115%. 参考文献 | 相关文章 | 计量指标