日用化学工业（中英文）

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铁离子对水解聚丙烯酰胺溶液流变性能影响研究
Research work with respect to effects of iron ion on rheological performance of hydrolytic polyacrylamide solution

陈斌,敖文君,陈士佳,朱洪庆,王成胜,吴彬彬,左清泉

2016 (11): 609-615. doi: 10.13218/j.cnki.csdc.2016.11.001

摘要 ( 302 )

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针对还原性物质使驱油水解聚丙烯酰胺(HPAM)体系黏度损失严重的问题,利用室内物理模拟方法,定量和定性地分析了Fe²⁺和Fe³⁺对HPAM溶液零剪切黏度、动态黏弹性以及瞬时拉伸流变性能的影响,分析了2种铁离子影响HPAM溶液黏度的机理。结果表明:Fe²⁺主要通过氧化还原反应以及水解的化学行为使HPAM分子链断裂,溶液黏度、流变性能大幅降低,同时,溶液中Fe²⁺的存在,不仅会使HPAM溶液弹性模量和损耗模量都急剧下降,也使HPAM溶液拉丝直径变小,拉伸断裂时间缩短,最终使HPAM分子与分子间的链缠结机会减小,缠结程度减弱,分子变得易于流动。Fe³⁺对HPAM溶液流变性能影响较小,其主要作用是使HPAM絮凝并沉淀。 Considering the problem that reducing substances cause serious viscosity loss of hydrolytic polyacrylamide (HPAM) solution used as oil displacement agent in crude oil field,the effects of Fe²⁺ and Fe³⁺ on the zero shear viscosity,dynamic viscoelasticity and rheological performance under instant extension were qualitatively and quantitatively analyzed with laboratory physical simulation method;then the mechanism for the effect of two kinds of iron ion on the viscosity of HPAM solution was examined.Results showed that the presence of Fe²⁺ in the solution mainly causes the break of the molecular chain of HPAM via redox reaction and chemical behavior of hydrolysis,which results in significant decline of viscosity and rheological performance of the HPAM solution.Meanwhile,the presence of Fe²⁺ in the HPAM solution not only causes the elastic modulus and loss modulus both fall sharply;but also reduces the filament diameter of HPAM solution and accelerates the break of the filament.Finally,degree of entanglement between polymer molecules reduces,and the molecules become easy to flow.Effect of Fe³⁺ on the rheological performance of HPAM solution is rather small,and its main functions are flocculation and precipitation of HPAM.

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氟表面活性剂和氟聚合物(Ⅺ) ——全氟碳流体
Fluorinated surfactants and fluoropolymers (Ⅺ) Perfluorocarbon fluids

窦增培,张甜甜,邢航,肖进新

2016 (11): 615-621. doi: 10.13218/j.cnki.csdc.2016.11.002

摘要 ( 343 )

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介绍了全氟碳流体的性能特点、发展历程、结构特点、制备方式和应用领域,分析了国内全氟碳流体市场现状,并对我国在该领域的发展前景进行了展望。 Performance,development course,structure features,preparation and applications of perfluorocarbon fluids were introduced.Current market situation of perfluorocarbon fluids was discussed.Outlook for development of perfluorocarbon fluids in China was prospected.

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12-3(OH)-12型表面活性剂ADAC的合成及性能研究
Synthesis and performance of 12-3(OH)-12 type surfactant ADAC

郭睿,李欢乐,刘爱玉,杨江月,程敏

2016 (11): 622-627. doi: 10.13218/j.cnki.csdc.2016.11.003

摘要 ( 240 )

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以十二烷基二甲基叔胺(12DMA)为主原料,在酸性条件下,合成了一种羟丙基双子型阳离子季铵盐1,3-二(烷基二甲基氯化铵)异丙醇(ADAC)。利用亚甲基蓝逆向滴定法测得产物纯度为98.63%,熔点为70.7~71.2 ℃。用FT-IR和¹H NMR对产物进行了结构表征。以单因素试验为基础,采用响应面法优化的ADAC合成工艺条件为:反应温度91 ℃、反应时间11 h、溶剂为异丙醇、n(12DMA)∶n(盐酸)=2.03∶1、转速250 r/min。在此条件下,ADAC产率约为93.37%。15 ℃下对目标产物表面性能测定可知,cmc为4.5×10^-5 mol/L,γ_cmc为27.07 mN/m,有效性(π_cmc)为45.99 mN/m,效率(pc₂₀)为5.301。 A kind of hydroxyl propyl Gemini ammonium chloride cationic surfactant,1,3-bis(alkyldimethylammonium chloride) isopropanol (ADAC) was synthesized with dodecyl dimethyl amine (12DMA) as main starting material under acidic condition.The purity of ADAC in the product reaches 98.63%,which was determinated by methylene blue back titration method,and its melting point is 70.7~71.2 ℃.The chemical structure of the product was characterized by means of FT-IR and ¹H NMR.Based on single factor experiments,the optimum conditions were obtained using response surface methodology as:reaction temperature,91 ℃;reaction time,11 h;solvent,isopropanol;n(12DMA)∶n(hydrochloric acid)=2.03∶1;stirrer rotation speed,250 r/min.Under the aforesaid conditions,the reaction yield of ADAC achieves 93.37%.Surface performance of the target product at 15 ℃ was measured as:cmc,4.5×10^-5 mol/L;γ_cmc,27.07 mN/m;effectiveness (π_cmc),45.99 mN/m;efficiency (pc₂₀),5.301.

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一种耐电解质弱酸环境增稠剂的制备与性能
Synthesis and performance of a thickener with salt resistance in weak acid circumstance

周铮鸣,陈洪龄,汪昌国,李华山

2016 (11): 628-633. doi: 10.13218/j.cnki.csdc.2016.11.004

摘要 ( 301 )

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以甲基乙烯基醚/马来酸酐共聚物和脂肪醇聚氧乙烯醚为原料,采用溶剂接枝法合成了一种增稠剂。考察了反应温度、反应溶剂和催化剂种类对酯化反应的影响;采用红外光谱对产物进行了结构表征;考察了酯化率、中和度和中和介质对产物增稠性能的影响。结果表明,较佳的合成条件为:反应温度80~90 ℃,反应溶剂N,N-二甲基甲酰胺,催化剂对甲苯磺酸。在此条件下,将合成的增稠剂用三乙醇胺中和,配制成质量分数为0.5%的白浆,其黏度为14.8 Pa·s,对盐的黏度保留率为93.3%,PVI值为0.157,在弱酸性条件下增稠效果良好,耐盐性优于卡波增稠剂。 A thickener was prepared by solvent-grafting method with poly(methyl vinyl ether-alt-maleic anhydride) and ethoxylated fatty alcohol ether as starting materials.The influences on the esterification of reaction temperature,solvent and catalyst examined.The thickener product was characterized by infrared spectrum.The effects of esterification rate,neutralization degree and kinds of neutralization agent on the properties of the thickener product were also examined.The results showed that,the suitable conditions are as follows:reaction temperature,80-90 ℃;reaction solvent,N,N-dimethyl formamide (DMF);catalyst,p-toluene sulfonic acid.Under the aforesaid conditions,the triethanolamine was used as the suitable neutralization agent and formulated to a thickener product (white paste) with content of mass fraction 0.5%.The viscosity of the prepared white paste achieves 14.8 Pa·s,and its viscosity retention rate against salt achieves 93.3%.Its PVI value is 0.157.Under weak acid condition,it displays good thickening effect.The thickener product prepared is better than that of market thickener with respect to salt resistance.

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超声波辐射相转移催化合成十二烷基缩水甘油醚
Synthesis of dodecyl glycidyl ether under ultrasonic irradiation by phase transfer catalysis

杜彬,罗志臣,丁乙,王晨

2016 (11): 634-637. doi: 10.13218/j.cnki.csdc.2016.11.005

摘要 ( 269 )

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超声波辐射下三乙基苄基氯化铵相转移催化由十二醇与环氧氯丙烷合成十二烷基缩水甘油醚,产品用FT-IR进行结构表征。考察了催化剂的种类、反应物的摩尔比及其与催化剂和NaOH的摩尔比、超声波辐射功率和辐射时间等因素对产品收率的影响。结果表明,超声波辐射下,三乙基苄基氯化铵具有良好的催化活性,较佳反应条件为:十二醇0.15 mol,n(十二醇)∶n(环氧氯丙烷)∶n(三乙基苄基氯化铵)∶n(NaOH)=1∶1.15∶0.05∶1.05,甲苯15 mL,超声波辐射功率100 W下辐射45 min,此时产品的收率达到93%以上。 Dodecyl glycidyl ether was synthesized by the reaction of epichlorohydrin and lauryl alcohol under ultrasonic irradiation with benzyltriethylammonium chloride as the phase transfer catalyst.Chemical structure of the product was characterized by FT-IR spectrum.The effects of kinds of catalyst,molar ratio of reactants,dosage of NaOH and the catalyst,ultrasonic irradiation power and time on the yield of dodecyl glycidyl ether were investigated.Results showed that benzyltriethylammonium chloride displays high catalytic activity on the reaction under ultrasonic irradiation.The optimal reaction conditions were as follows:n(lauryl alcohol)∶n(epichlorohydrin)∶n(benzyltriethylammonium chloride)∶n(NaOH)=1∶1.15∶0.05∶1.05 (based on 0.15 mol lauryl alcohol and 15 mL toluene);power of ultrasonic irradiation 100 W;time for ultrasonic irradiation 45 min.Yield of the product reaches higher than 93%.

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汉麻粉的防晒性能研究
Study on sun-screening performance of hemp powder

甘亮,张晨,杨雪芳,牛玉莲,张志伟

2016 (11): 638-647. doi: 10.13218/j.cnki.csdc.2016.11.006

摘要 ( 315 )

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分别采用球磨、酸和碱对汉麻粉进行处理。通过红外光谱、扫描电镜、紫外可见分光光度计和SPF测试仪对汉麻粉的结构、表观形态及其防晒性能进行表征。实验结果表明:在全波段范围内,单一依赖汉麻粉质量分数的增加,对提高样品紫外吸收性能是非常有限的;球磨破碎法处理时间对吸光度影响不大;对比不同种类酸处理以及未做任何处理的结果,醋酸对吸光度的提高最大;对比不同种类碱处理以及未做任何处理的结果,三乙醇胺对吸光度的提高最大,并且其对吸光度的提高大于醋酸;经酸、碱处理后,汉麻粉红外吸收峰的强度有所下降,汉麻粉本身的不规则片状结构并未发生改变;对比不同处理方法的汉麻粉的SPF值,碱处理的SPF值最高。 Hemp powder was treated by separate technological operations,such as ball mill grinding,acid treatment and alkali treatment.Then the structure,apparent morphology and sun-screening performance of the treated samples were characterized by infrared spectroscopy,scanning electron microscope,UV-vis spectrophotometer and sun protection factor (SPF) measurement.Experimental results showed that,the upgrading effect for UV absorbance within whole wavelength range by simple increase of hemp powder mass fraction is very limited.Effect of increase of treating time of ball mill grinding for improving light absorbance is not obvious.Comparing the samples that treated by separate kinds of acid and the sample without any treatment,results showed that the sample treated by acetic acid displays the highest light absorbance.Comparing the samples that treated by separate kinds of alkali and the sample without any treatment,results showed that the sample treated by triethanolamine displays the highest light absorbance,even higher than that treated by acetic acid.After the treatment of acid or alkali,the peak intensity of infrared absorption of the hemp powder decreases,but its irregular chip structure remains unchanged.Comparing the SPF of samples that treated by separate methods,results showed that the sample treated by alkali displays the highest SPF value.

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复凝聚法制备β-大马酮微胶囊的工艺研究
Study on the technology for preparation of β-damascone microcapsules with complex coacervation method

肖维毅,沈妍,尧珍玉,刘哲,黄海群

2016 (11): 643-653. doi: 10.13218/j.cnki.csdc.2016.11.007

摘要 ( 287 )

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以β-大马酮为囊芯材料,明胶和羧甲基纤维素钠(CMC)为壁材,通过复凝聚法制备了β-大马酮微胶囊。以单因素试验为基础,通过正交试验优化了β-大马酮微胶囊制备的工艺条件。确定较佳工艺条件为:m(明胶)∶m(CMC)=9∶1,m(芯材)∶m(壁材)＝1∶1,乳化速度8 500 r/min,固化剂用量0.25%,溶液pH=4.5～4.6,反应温度40 ℃。在此条件下,微胶囊的包埋率达到了97.83%±2.16%,其粒径约为30 μm,形貌圆整规则。 β-Damascone microcapsules were prepared by complex coacervation method with β-damascone as core material and gelatin and sodium carboxymethyl cellulose (CMC) as coating materials.Based on the results from single factor experiment,the orthogonal design was used to optimize the preparation conditions of β-damascone microcapsules.The better process conditions were determined as:gelatin and CMC mass ratio,9∶1;core and coating mass ratio,1∶1;rotation speed of the emulsification,8 500 r/min;dosage of the curing agent,0.25%;pH value,4.5-4.6;operation temperature,40 ℃.Under the aforesaid conditions,the microcapsule embedding rate achieves 97.83%±2.16%;the particle size is about 30 μm,with morphology of the microcapsules round and regular.

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微乳液的理论及应用研究进展
Progress in research work field with respect to theory and application of microemulsion

毛雪彬,杜志平,台秀梅,刘晓英

2016 (11): 648-653. doi: 10.13218/j.cnki.csdc.2016.11.008

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综述了微乳液与普通乳状液的相似与不同之处,并对微乳液的形成机理和体系结构、性质的一些研究方法和手段作了介绍;探讨了微乳液在不同领域中的应用,并对其应用前景进行了展望。 Similarities and differences between microemulsion and ordinary emulsion were summarized.Mechanism for formation of microemulsion as well as the research methods for structure and properties of microemulsions were introduced.The applications of microemulsion in different areas were summarized,and its application foreground was prospected.

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表面活性剂在不同固体表面的润湿性能研究进展
Progress in research work field with respect to wetting performance of surfactants on separate solid surfaces

韩兵,崔勇,魏文珑,常宏宏

2016 (11): 654-660. doi: 10.13218/j.cnki.csdc.2016.11.009

摘要 ( 314 )

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综述了表面活性剂在不同极性固体表面的润湿性能研究进展,主要总结了表面活性剂在石英和玻璃等极性表面、聚甲基丙烯酸甲酯(PMMA)等中等极性表面、聚四氟乙烯(PTFE)等非极性表面的润湿作用规律及影响因素。结合作者的研究工作,特别阐述了系列表面活性剂在煤沥青表面的润湿规律。对表面活性剂在固体表面的应用趋势进行了展望。 Progress in research work field with respect to wetting performance of surfactants on solid surface of separate polarity was described,focusing on rules of wetting action and effecting factors for polar materials such as quartz and glass,middle polar material such as polymethylmethacrylate (PMMA) as well as non-polar material such as polytetrafluoroethylene (PTFE).In combination with the author's research work,the wetting mechanism for series of surfactants on surface of coal pitch was emphatically discussed.Finally,the application trend of surfactants for wetting of solid surface was prospected.

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液相色谱-串联质谱法测定祛痘化妆品中5种硝基咪唑类化合物
Determination of five kinds of nitroimidazole compound in whelk dispelling cosmetics by liquid chromatography- tandem mass spectrometry

张鑫鑫,高媛惠,花锦,杨燕强,申迎华

2016 (11): 661-664. doi: 10.13218/j.cnki.csdc.2016.11.010

摘要 ( 228 )

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采用液相色谱-串联质谱(LC-MS/MS)法建立了测定祛痘化妆品中5种硝基咪唑类化合物(甲硝唑(MNZ)、洛硝哒唑(RNZ)、二甲硝咪唑(DMZ)、羟基甲硝唑(MNZOH)和1-甲基-5-硝基-2-羟甲基咪唑(HMMNI))的方法。样品经乙酸乙酯提取,采用Hypersil GOLD C₁₈色谱柱(2.1 mm×100 mm,3 μm)分离,依次用丙酮、甲醇和V(氨水)∶V(乙腈)=5∶95的混合溶液淋洗,采用LC-MS/MS在多反应监测(MRM)正离子模式下检测,基质外标法定量。结果表明:MNZ,RNZ和DMZ在0~50 μg/L内呈良好线性关系,MNZOH和HMMNI在0~100 μg/L内呈良好线性关系;5种硝基咪唑药物线性相关系数R²>0.99;在试样中进行3个水平的加标回收实验,平均回收率为84.3%～115.0%,相对标准偏差(RSD)为1.66%～10.30% (n=6),适用于祛痘化妆品中硝基咪唑类化合物的检测和确证需要。 A method for determination of five kinds of nitroimidazole compound (metronidazole (MNZ),ronidazole (RNZ),dimetridazole (DMZ),hydroxyl metronidazole (MNZOH) and 2-hydroxymethyl-1-methyl-5-nitroimidazole (HMMNI)) in whelk dispelling cosmetics by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established.The target analyte was extracted from the product sample with ethyl acetate as solvent,and the extract was separated on a Hypersil GOLD C₁₈ column (2.1 mm×100 mm,3 μm),sequentially eluted with acetone,methanol and blend solution with V(ammonia water)∶V(acetonitrile)=5∶95,detected using LC-MS/MS in the multiple reaction monitoring (MRM) positive ion mode,and quantified by external standard matrix method.The results indicated that good linearity displays when mass concentration of MNZ,RNZ and DMZ is within 0~50 μg/L,and when mass concentration of MNZOH and HMMNI is within 0~100 μg/L.Linear correlation coefficient (R²) is higher than 0.99.In the spiked test of three levels,the average recovery rate is in the range of 84.3%-115.0%,and relative standard deviation (RSD) is in the range of 1.66%-10.30% (n=6).This analysis method meets the testing requirements for detection and confirmation.

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日化行业挥发性有机物排放特征调查研究——以广州市某典型日化企业为例
Investigation for emission features of volatile organic compounds from daily chemical industry:taking a typical daily chemical enterprise in Guangzhou city as an example

陈小燕,戴殷

2016 (11): 665-670. doi: 10.13218/j.cnki.csdc.2016.11.011

摘要 ( 225 )

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利用物料衡算法,结合生产工艺调查、现场采样及实验分析,研究了广州市某典型日化企业生产过程中挥发性有机物(VOCs)从原料输入到产品输出各环节的排放特征。结果表明,有组织排放检测口的总VOCs质量浓度接近,其中柠檬烯成分质量浓度均为最高,而无组织采样点中原料混合区的VOCs质量浓度最高,其中柠檬烯成分质量浓度也是最高。有、无组织排放环节分别检测出11和16种主要的VOCs物种,经分析可知该企业的特征污染物为柠檬烯,且通过物料衡算得出该企业的VOCs综合排放因子为0.199 kg/t。 In combination with the production process investigations,field sampling and experimental analysis,the emission features of volatile organic compounds (VOCs) from raw material input to product output in the manufacturing process of a typical daily chemical enterprises in Guangzhou city were examined via material balance method.Results indicated that the mass concentration of VOCs of organized discharge detection port is basically identical.The mass concentration of VOCs of unorganized sampling at raw material mixing area is the highest.The mass concentration of limonene component is the largest both in organized discharge port and unorganized sampling.11 and 16 kinds of main VOCs were detected in the organized discharge and unorganized emission respectively.The main pollutant of this enterprise is limonene.The comprehensive emission factor of this enterprise was 0.199 kg/t based on the material balance method.

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