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    2018年, 第48卷, 第11期 刊出日期:2018-11-22 上一期    下一期
    基础研究
    氟硅非离子表面活性剂的制备及性能
    Synthesis and properties of nonionic fluorosilicone surfactants
    叶志刚, 占昌朝, 曹小华, 胡庆华, 谭景林
    2018 (11):  605-610.  doi: 10.13218/j.cnki.csdc.2018.11.001
    摘要 ( 338 )   PDF(4703KB) ( 267 )  
    以含氢硅油(PMHS)、N-甲基-N-烯丙基-2-全氟-2-甲基-3-氧代己酰胺(NF2)和烯丙基聚醚(F6)为原料,在Karstedt催化剂作用下,通过硅氢加成反应制备了氟硅非离子表面活性剂PF2F6;采用FT-IR、1H NMR和19F NMR对产物结构进行了表征,并测定了产物的溶解度、浊点、表面张力和润湿性。结果表明,PF2F6在弱极性溶剂中具有良好的溶解度,在水中的溶解度随着F6物质的量的增大而增大;当n(Si-H)∶n(NF2)∶n(F6)=2∶0.7∶1.3时,临界胶束浓度(cmc)和平衡表面张力(γcmc)最小,其值分别为0.13 g/L和22.8 mN/m;随着反应体系中F6物质的量的增加,PF2F6的浊点增加,而在有机玻璃(PMMA)表面的接触角减小。 Hydrosilylation of poly(methylhydrosiloxane) (PMHS) with N-methyl-N-allyl-2- perfluoro-2-methyl-3-oxocaproamide (NF2) and allyl polyethylene glycol (F6) was conducted in the presence of the Karstedt catalyst in order to prepare a series of nonionic fluorosilicone surfactants (PF2F6).The structure of the products were characterized by FT-IR,1H NMR and19F NMR.The properties of the products including solubility,cloud point,surface tension and wettability were measured.The results show that the solubility of PF2F6 in polar solvents was excellent and the solubility in water increases with the increase of the content of F6.When the molar ratio of Si-H∶NF2∶F6 is 2∶0.7∶1.3,the critical micelle concentration (cmc) and the surface tension at cmc (γcmc) are minimum,which are 0.13 g/L and 22.8 mN/m,respectively.The cloud point of PF2F6 increases and the contact angle on PMMA surface decreases with the increase of the content of F6 in the reaction system.
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    科技讲座
    弱相互作用调控表面活性剂自组装(Ⅰ)——弱相互作用的分类
    Self-assembly of surfactants regulated by weak interaction (Ⅰ)The classification of weak interactions
    任姝静, 郑利强, 孙继超
    2018 (11):  611-616.  doi: 10.13218/j.cnki.csdc.2018.11.002
    摘要 ( 329 )   PDF(7084KB) ( 86 )  
    表面活性剂是依靠分子间的弱相互作用实现自组装的,包括疏水相互作用、氢键作用力、主客体相互作用、静电相互作用、π-π堆积相互作用、金属配位相互作用和电荷转移相互作用等。通过调节分子间的相互作用可以实现对两亲分子自组装的调控,本文介绍了弱相互作用对两亲分子自组装形成有序分子聚集体结构和功能的影响。 The self-assembly of surfactants relies on the weak interactions between molecules,including hydrophobic interaction,hydrogen bond interaction,host-guest interaction,electrostatic interaction,π-π stacking interaction,metal coordination interaction and charge transfer interaction.The self-assembly of amphiphilic molecules can be controlled by regulating the interaction between molecules.This paper introduces the influence of weak interactions on the structure and function of ordered molecular aggregates formed by self-assembly of amphiphilic molecules.
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    开发与应用
    三元复合体系渗流特征及其动态损失规律研究
    Research on the seepage characteristics and dynamic damage rules of thealkali/surfactant/polymer flooding system (ASP)
    赵习森, 杨红, 于峰, 汪杰, 王宏, 金志
    2018 (11):  617-621.  doi: 10.13218/j.cnki.csdc.2018.11.003
    摘要 ( 238 )   PDF(5044KB) ( 247 )  
    针对以单一岩心尺度作为实验介质研究复合体系渗流特征及各组分损失规律不能完全真实地模拟其在实际油藏中的渗流特性的问题和评价各组分的损失规律仅以静态损失量作为评价指标存在局限性的问题,在优化各组分检测方法的基础上,开展了多个岩心尺度的三元复合体系渗流实验,研究了复合体系各组分的渗流特征及其动态损失规律。实验结果表明:随着岩心尺度的增大,碱和聚合物浓度曲线均呈逐渐滞后的趋势,且二者受吸附、滞留作用的损失率逐渐增大,而表面活性剂则变化不明显;各组分渗流前缘上游区域同一位置处各组分相对浓度大小顺序依次为:碱>表面活性剂>聚合物;同一岩心尺度下,复合体系注入不同阶段,吸附、滞留作用和多孔介质的剪切作用对聚合物黏度损失的贡献有所不同。 To solve the problems that (1) the ASP seepage characteristics in real petroleum reservoir can’t be properly simulated when using single core only;and (2) the loss can’t be evaluated accurately by the evaluation with just static loss,in this work,a seepage experiment for the ASP system was carried out to study its seepage characteristics and loss rules with different core scales on the basis of measuring method optimization.The experimental results show that,with the increase of core scale,the alkali and polymer curves are gradually pushed to the right and their loss ratios influenced by adsorption and retention are gradually increased.In contrast,the increase of core scale nearly has no influence on surfactant.The sequence of the relative concentration at the same position of the upstream region of seepage front is:alkali>surfactant>polymer.In addition,the contribution of adsorption,retention and shear on polymer viscosity loss are different with different stages of injection.
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    烷基木糖苷物化性能研究
    Study of physical and chemical properties of alkyl polyxylosidase
    白亮, 杨秀全, 吴志宇
    2018 (11):  622-626.  doi: 10.13218/j.cnki.csdc.2018.11.004
    摘要 ( 279 )   PDF(3589KB) ( 265 )  
    分别对不同长度碳链和平均聚合度(DP)的烷基木糖苷(AX)进行性能评价,结果表明,AX可将水的表面张力降低到26 mN/m以下,随碳链长度增加,AX临界胶束浓度(cmc)减小,饱和吸附量(Гmax)降低,且Гmax高于相同碳链的烷基葡糖苷(APG),AX的发泡力、泡沫稳定性、抗硬水能力及润湿性能均优于相同碳链的APG。随DP的增大,AX平衡表面张力(γcmc)及cmc均增大,Гmax呈降低趋势,DP对发泡力的影响有限,DP的降低使得AX的抗硬水能力、润湿力和乳化能力有所提高。 The properties of alkyl polyxylosidase (AX) with different carbon chain length and average polymerization degree (DP) were evaluated.The results show that AX can reduce the surface tension of water to below 26 mN/m.The critical micelle concentration (cmc) and surface excess concentration (Гmax) of AX are decreased with the increasing length of carbon chain,and the Гmax is higher than that of alkyl polyglycoside (APG) with the same carbon chain.The foaming ability,foam stability,hard water resistance and wetting power of AX are all superior to that of APG with the same carbon chain.With the increase of DP of AX,the cmc and the surface tension at cmc (γcmc) are both increased,and the Гmax is decreased.The DP of AX has no significant effect on the foaming ability.However,the hard water resistance,wetting power and emulsifying ability of AX are enhanced with the decrease of DP.
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    功能化离子液体[C3SO3Hnhm]HSO4催化合成苯并氧杂蒽
    Synthesis of benzoxanthene catalyzed by functionalized ionic liquids [C3SO3Hnhm]HSO4
    汤小芳, 刘显明, 周思言, 李双
    2018 (11):  627-631.  doi: 10.13218/j.cnki.csdc.2018.11.005
    摘要 ( 230 )   PDF(4123KB) ( 242 )  
    无溶剂下以功能化酸性离子液体4-(3-磺丙基)吗啡啉硫酸氢盐([C3SO3Hnhm]HSO4)为催化剂,催化β-萘酚和芳香醛合成苯并氧杂蒽。通过单因素试验和正交试验优化反应条件,并考察了该离子液体的重复使用性能。结果表明,当苯甲醛用量为0.005 mol,β-萘酚与苯甲醛摩尔比为2∶1,催化剂用量为苯甲醛的6%,100 ℃下反应10 min后苯并氧杂蒽的产率达到91%以上。[C3SO3Hnhm]HSO4催化剂重复使用5次,其催化活性下降不明显,为苯并氧杂蒽类化合物的绿色合成提供了一种新方法。 A solvent-free synthesis of benzoxanthene was operated,in which functionalized acidic ionic liquids,4-(3-propanesulfonic acid) morphinehydrogen sulfate [C3SO3Hnhm]HSO4 were used as catalysts,andβ-naphthol and aromatic aldehyde were used as raw materials.The reaction conditions were optimized by the single factor experiment and orthogonal experiment,and the reusability of the ionic liquid catalyst was also studied.The results show that when the dosage of benzaldehyde is 0.005 mol,the molar ratio ofβ-naphthol to benzaldehyde is 2∶1,and the catalyst is in an amount corresponding to 6% of benzaldehyde,the yield can reach more than 91% after reaction for 10 min at 100 ℃.The catalytic activity of [C3SO3Hnhm]HSO4 was not significantly reduced for being reused 5 times.This work has provided a new method for green synthesis of benzoxanthene compounds.
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    聚醋酸乙烯酯及其铕配合物的合成和性能研究
    Synthesis and properties of polyvinyl acetate and its europium complexes
    李善吉, 谢鹏波, 袁宁宁, 欧阳英
    2018 (11):  632-636.  doi: 10.13218/j.cnki.csdc.2018.11.006
    摘要 ( 312 )   PDF(4487KB) ( 256 )  
    以过氧化苯甲酰(BPO)为引发剂,甲醇为溶剂合成了聚醋酸乙烯酯(PVAc),研究了引发剂和甲醇用量、反应时间对转化率和固含量的影响,并对聚合物进行了粘接性能测试;同时以PVAc为高分子配体,合成了PVAc-铕(PVAc-Eu)配合物,并通过红外光谱对配体和配合物的结构进行了表征,测定了配合物的发光和热性能。结果表明,醋酸乙烯酯聚合的较佳条件是:甲醇体积为单体体积的11.9%,引发剂用量为0.19 g(单体质量的0.5%),反应时间为3 h;用508 nm作激发波长,配合物荧光光谱在612 nm处出现铕的特征吸收峰;热重(TG)测试显示,PVAc和PVAc-铕起始热分解温度分别是300和86 ℃。 Polyvinyl acetate (PVAc) was synthesized with benzoyl peroxide (BPO) as initiator and methanol as solvent.The effects of the amounts of initiator and methanol and the reaction time on conversion and solid content were studied.The adhesive performance of polymers was also measured.In addition,the europium complex of PVAc (PVAc-Eu) was synthesized using PVAc as polymer ligand,and the structures of ligand and complex were characterized by IR spectroscopy.The luminescent and thermal properties of complex were also studied.The results show that,the optimized conditions for polymerization are as follows:methanol is in an amount corresponding to 11.9% of the volume of monomer,the dosage of initiator is 0.19 g,0.5% of mass initiator ratio to monomer and the reaction time is 3 hours,Using 508 nm as excitation wavelength,the fluorescence spectrum of the complex has a characteristic absorption peak of europium at 612 nm.Thermogravimetric (TG) experiments show that the initial thermal decomposition temperature of PVAc and PVAc-Eu are 300 ℃ and 86 ℃,respectively.
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    枸杞多糖面膜的制备与性能评价
    Preparation and performance evaluation of Lycium barbarum polysaccharide mask
    刘艺, 郭俞辰, 蔡林军, 龙晓燕
    2018 (11):  637-642.  doi: 10.13218/j.cnki.csdc.2018.11.007
    摘要 ( 369 )   PDF(4938KB) ( 290 )  
    以魔芋精粉和枸杞为原料,制备了一种新型的凝胶面膜,并对其工艺和性能进行了考察。结果表明魔芋枸杞凝胶面膜的较优配方为:魔芋精粉3%,甘油6%,枸杞多糖0.2%,山梨醇2%,在室温条件下形成凝胶。枸杞多糖对羟基自由基的抑制率为51.9%;对DPPH自由基的抑制率为87.7%;对酪氨酸酶的抑制率为51.1%。25 ℃时所制备的面膜在25 min内的保湿率为81.6%;当面膜质量浓度为0.5 g/mL时,对羟基自由基的抑制率为37.4%;当面膜质量浓度为0.25 g/mL时,对DPPH自由基的抑制率为61.7%。 A new type of gel mask was prepared from konjac flour and Chinese wolfberry,and its process and properties were investigated.The results show that the superior formula of konjac wolfberry gel mask is:3% of konjac flour,6% of glycerin,0.2% ofLycium barbarum polysaccharide and 2% of sorbitol,forming a gel at room temperature.The inhibition rate ofLycium barbarum polysaccharide on hydroxyl radical,DPPH free radical and tyrosinase is 51.9%,87.7% and 51.1%,respectively.For gel mask,the moisture retention rate reaches 81.6% within 25 min at 25 ℃;when the mask mass concentration is 0.5 g/mL,the inhibition rate on hydroxyl radicals is 37.4%;when the mask mass concentration is 0.25 g/mL,the inhibition rate on DPPH free radicals is 61.7%.
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    光甘草定对小鼠银屑病模型治疗作用的初步研究
    Preliminary study on the therapeutic effect of glabridin on mouse psoriasis model
    洪婷, 刘晓英, 车飙, 唐健, 刘光荣, 杜志云
    2018 (11):  643-646.  doi: 10.13218/j.cnki.csdc.2018.11.008
    摘要 ( 299 )   PDF(3154KB) ( 248 )  
    为探索光甘草定(PT)在治疗银屑病方面的作用,通过建立咪喹莫特乳剂(IMQ)诱导的小鼠银屑病耳廓肿胀模型和背部皮肤破损模型,再根据PT在人体皮肤用药标准设置不同含量进行给药。结果表明,在PT含量分别为30和15 g/kg时对小鼠耳廓红肿程度具有明显抑制效果,抑制率高达68.37%和56.98%。同时,对小鼠背部皮肤红肿、鳞屑、浸润增厚程度进行银屑病面积和严重程度指数(Psoriasis area severity index,PAIS)评分,绘制趋势线以观察各组小鼠皮损的变化情况,发现PT含量为30 g/kg时对小鼠皮损具有明显的抑制效果。 To explore the role of glabridin in the treatment of psoriasis,the model of auricle swelling and back skin damage induced by imiquimod emulsion (IMQ) in mouse were established,and then different doses of PT were given according to the standard of human skin administration.Results show that the PT contents of 30 and 15 g/kg have significant inhibitory effects on the degree of auricle swelling in mouse,and the inhibitory rate is 68.37% and 56.98% respectively.In the meantime,the psoriasis area severity index (PAIS) was scored on the back skin erythema,scale and thickness of the mouse.The trend line was drawn to observe the changes of skin lesions in each group.At 30 g/kg,PT has significant inhibitory effect on skin lesions of mouse.
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    专论与综述
    乙二醇基Gemini表面活性剂的合成研究进展
    Research progress in synthesis of glycol-based Gemini surfactants
    葛秀娟, 高文超, 黄双平, 李兴, 魏文珑, 常宏宏
    2018 (11):  647-655.  doi: 10.13218/j.cnki.csdc.2018.11.009
    摘要 ( 275 )   PDF(7055KB) ( 58 )  
    综述了以乙二醇为原料制备阳离子、阴离子、非离子和两性离子Gemini表面活性剂的合成方法,并对合成路线进行了总结和分析,对产物的性能及其应用进行了阐述。以乙二醇为主要原料合成的Gemini表面活性剂具有更高的表面活性、较低的临界胶束浓度、良好的润湿性和抗菌性,应用范围较广。 The synthesis of cationic,anionic,nonionic and zwitterionic Gemini surfactants using ethylene glycol as raw materials has been reviewed.The synthetic routes have been summarized and analyzed,and the properties and applications of the products have been described.The Gemini surfactants with ethylene glycol as raw material have higher surface activity,lower critical micelle concentration,and good wetting and antibacterial properties,which have a wider application range.
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    海军用多效防护剂的研究进展
    Research progress of multi-effect protective agents for navy personnel
    韩凌, 鲁莹, 李嘉鑫, 孙治国, 刘俊杰
    2018 (11):  656-660.  doi: 10.13218/j.cnki.csdc.2018.11.010
    摘要 ( 273 )   PDF(5799KB) ( 254 )  
    基于海军官兵训练伤中日晒伤和水母蜇伤发生率较高。从紫外线对人体的影响,无机、有机和天然3类防晒剂防晒方向进行了介绍,并对水母刺胞的结构、蜇伤发生的机制以及防护制剂等水母蜇伤防护方向进行了综述,结合国外现有产品,提出将防晒和水母蜇伤防护相结合制作多效防护霜的可行性。 Among the military training injuries of navy personnel,sunburn and jellyfish stings are shown to have high incidence.Therefore,in terms of sunburn protection,the effects of ultraviolet radiation on human body and three kinds of sunscreens (inorganic,organic and natural sunscreens) were introduced.In the protection of jellyfish stings,the structure of jellyfish’s nematocysts,mechanism of stings and protective agents of jellyfish stings were reviewed.Considering that similar products are already available abroad,it is feasible to create a multi-effect protective agent combining sunburn protection and jellyfish sting protection.
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    分析与检测
    高效液相色谱法测定牙膏中叶绿素铜钠盐的含量
    Determination of sodium copper chlorophyllin in toothpaste by high performance liquidchromatography
    李玉静, 王雪平
    2018 (11):  661-664.  doi: 10.13218/j.cnki.csdc.2018.11.011
    摘要 ( 392 )   PDF(3442KB) ( 256 )  
    在酸性条件下,以聚酰胺粉吸附牙膏中叶绿素铜钠盐,解吸附洗脱,经YMC Carotenoid C30 (4.6 mm×250 mm,3 μm)色谱柱分离,光二极管阵列检测器(PDA)检测,建立了高效液相色谱法测定牙膏中叶绿素铜钠盐含量的方法。样品经甲醇-叔丁基甲醚-0.5%醋酸混合溶液为流动相进行梯度洗脱,流速1.0 mL/min,柱温30 ℃,检测波长405 nm。结果表明,叶绿素a铜钠盐和叶绿素b铜钠盐在5.0~100.0 mg/L质量浓度范围内,具有较好的线性关系,相关系数分别为0.999 8和0.999 7;检出限均为1.5 μg/kg,定量限均为5.0 μg/kg;加标回收率为87.2%~97.8%,RSD为1.7%~2.9%。 The sodium copper chlorophyllin in toothpaste was adsorbed by polyamide under acidic conditions,eluted by desorption,separated by YMC Carotenoid C30 chromatographic column (4.6 mm×250 mm,3 μm),and detected by photodiode array detector (PDA).A method for the determination of sodium copper chlorophyllin in toothpaste by high performance liquid chromatography (HPLC) was established.The sample was subjected to gradient elution with methanol-tert-butyl methyl ether-0.5% acetic acid mixed solution as a mobile phase at a flow rate of 1.0 mL/min,a column temperature of 30 °C,and a detection wavelength of 405 nm.The results show that sodium copper chlorophyllin a and sodium copper chlorophyllin b have a good linear relationship in the range of 5.0-100.0 mg/L,and the correlation coefficients are 0.999 8 and 0.999 7 respectively.The detection limits are 1.5 μg/kg;the limits of quantitation are 5.0 μg/kg;the recovery rate is 87.2%-97.8% and the relative standard deviation is 1.7%-2.9%.
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