长链烷基酯改性硅油的合成研究

以甲基含氢硅油和丙烯酸十二酯为原料,氯铂酸为催化剂,通过硅氢加成的方法直接合成了长链烷基酯改性硅油.考察了反应因素如催化剂用量、反应温度、反应时间和物料比等对反应的影响,确定了最佳反应条件.最后对合成产物进行了IR表征.     

聚醚改性氨基硅油的合成及应用

以α,ω-二羟基聚二甲基硅氧烷（W S-62M）、N-β-氨乙基-γ-氨丙基甲基二甲氧基硅烷（DL-602）、单端环氧聚醚（X-O9）为主要原料,合成了一系列聚醚改性氨基聚硅氧烷,探讨了最佳改性条件,并考察了DL-602用量、n（X-O9）∶n（DL-602）对聚醚改性氨基硅油乳液性能及其应用性能的影响.结果表明：以异丙醇作溶剂,偶联剂用量为10%,n（X-O9）∶n（DL-602）=3∶1,80℃下反应4h为最佳反应条件;所制聚醚改性氨基硅油乳液稳定性好,用该乳液整理的织物其白度和亲水性均较氨基硅油有提高,与氨基硅油的摩擦系数相差不大,耐洗.     

N-(甲基丙烯酰基)氨基苯乙酮的合成

与目前共混方法制备光存储材料不同,本实验采用共聚的方法制备光存储薄膜．主要介绍了其中间体N－（甲基丙烯酰基）氨基苯乙酮的合成,通过紫外、红外光谱及元素分析手段对其进行了表征．     

硅烷偶联剂改性水性丙烯酸酯乳液的制备及性能

以丙烯酸丁酯（BA）和甲基丙烯酸甲酯（MMA）、丙烯酸（AA）和γ-甲基丙烯酰氧基丙基三甲氧基硅烷（KH-570）为单体,过硫酸铵为引发剂,十二烷基苯磺酸钠（SDBS）和烷基酚聚氧乙烯醚（OP-10）为复合乳化剂,采用半连续乳液聚合法合成了复合胶黏剂乳液.采用红外光谱对聚合物结构进行了表征,热重分析研究了聚合物胶膜的热稳定性.接触角的测定表征了聚合物膜的表面性能.研究了反应温度,引发剂和乳化剂用量等因素的影响.结果表明,聚合反应速率随着反应温度的提高而加快.随着引发剂和乳化剂用量的增加,乳液的粒径减小,乳液更加稳定.硅改性后的聚合物具有较好的耐水性和热稳定性.     

长链烷基改性硅油的制备、表征与性能研究

采用无溶剂硅氢加成法,以１－辛烯、１－十二烯、１－十六烯、含氢硅油为原料,氯铂酸为催化剂,制备长链烷基改性硅油。产物的结构采用 ＦＴＩＲ 和 １Ｈ－ＮＭＲ 进行表征。通过正交试验和单因素实验,研究了反应温度、反应时间、催化剂用量、ｎ（Ｓｉ—Ｈ）∶ｎ（ＣＣ）对Ｓｉ—Ｈ 转化率的影响,确定 了产物的最佳合成工艺。研究了不同烷基摩尔质量比和烷基长度对产物的黏度指数、表面张力、润 滑性能、折光率的影响。结果表明：在优化工艺条件（ｎ（Ｓｉ—Ｈ）∶ｎ（ＣＣ）＝１∶１．２,反应时间６ｈ,反应温度１００℃,十二烯活化催化剂用量３ｍｇ／Ｌ）下,产物的ＳｉＨ 转化率高达９２．６％;随着烷 基摩尔质量比和烷基长度的增加,硅油的黏度指数逐渐下降至３５８,从而降低了硅油的黏温性能,但其表面张力变化不大。改性后的硅油的润滑性能和折光率得到了显著提升,其磨斑直径最小为 ０．３３ｍｍ,折光率最大值为１．４３９６。     

高效乳液型有机硅消泡剂的制备及性能研究

将质量比为100：8的甲基硅油和气相法二氧化硅于130～150℃处理3～5h,再和聚醚硅油、复合乳化剂（由Span80与Tween80组成）、羧甲基纤维素钠等复配,制得高效乳液型有机硅消泡剂．最佳制备条件是：甲基硅油的粘度为600-800mPa·s,用量为16％～17％（质量分数,下同）;气相法二氧化硅用量为1．3％;聚醚硅油（粘度800～1000mPa·s）用量为10％;复合乳化剂的亲水亲油平衡值（HLB值）为10,用量为6％;羧甲基纤维素钠用量为1％．实验结果表明：该消泡剂消泡效果好,其主要技术指标与国外同类型产品相当．消泡剂乳液的离心稳定性、耐热稳定性好,且在水中的分散性良好．     

羧基／十二烷基改性聚硅氧烷的合成及在皮革防水中的应用

利用强碱性条件下六甲基二硅氧烷（MM）、八甲基环四硅氧烷（D4）、十二烷基甲基二甲氧基硅烷（HI）-109）及γ-氨丙基甲基二甲氧基硅烷（KH551）间的平衡化反应先制得一种侧链含有十二烷基／氨丙基的聚甲基硅氧烷（RASO）,然后RASO与马来酸酐反应制备了一种新型羧基／十二烷基改性聚硅氧烷（RCAS）,RCAS经乳化并用于山羊蓝湿革的防水处理．用红外光谱（IR）、核磁共振氢谱（^1HNMR）、透射电镜（TEM）、纳米粒度仪、ζ电位分析仪及静态接触角测量仪分别对产物结构、乳液粒子形态、粒径大小与分布、ζ电位及坯革粒面水静态接触角（WCA）进行表征．结果表明,合成产物具有预期结构．乳胶粒表面光滑,呈规则圆球状,平均粒径约为110Flm,粒径分布窄,乳液ζ电位为-24．09mV．蓝湿革经其质量1．92％的RCAS有效物处理后,粒面wCA可达126°,具有较好的疏水性．     

对二茂铁基苯甲酸的合成和表征

以对-氨基苯甲酸为原料与亚硝酸钠和盐酸在低温下反应,制备出对-氨基苯甲酸的重氮盐,再让其与二茂铁（摩尔比1：1）在低温和相转移催化剂的存在下反应,再由水蒸气蒸馏分离,合成出对-二茂铁基苯甲酸,通过多步实验确定出最佳合成条件,并用元素分析、红外光谱、质量对产物进行了表征。     

紫外光引发聚合P(AM-MAPTAC)及其响应面优化制备

以丙烯酰胺（AM）与甲基丙烯酰胺丙基三甲基氯化铵（MAPTAC）为共聚单体,通过紫外光引发聚合法制备阳离子聚丙烯酰胺絮凝剂P（AM-MAPTAC）。通过红外光谱（IR）与差热热重分析（TG/DSC）分别对P（AM-MAPTAC）进行结构表征与热稳定性分析,并采用响应曲面法得到优化制备条件：反应体系pH为4.75,引发剂v-044质量分数为0.07%,EDTA-2Na质量分数为0.20%,n（MATPAC）/n（AM）为0.33,光照时间为60 min。在优化条件下制备P（AM-MAPTAC）絮凝剂,特性粘度可达14.72 dL/g,通过污泥脱水实验可验证该特性粘度下的污泥脱水效果最好,滤饼含水率（FCMC）达70%,污泥比阻（SRF）达6.94×10¹²m/kg,上清液剩余浊度达9.70 NTU,污泥脱水效果优于市售常用絮凝剂。     

改性阴离子型水性聚氨酯的制备

采用聚碳酸亚丙酯二元醇、异佛尔酮二异氰酸酯（IPDI）、二羟甲基丙酸（DMPA）、自制氨基有机硅为主要原料制备了一种氨基有机硅改性的阴离子型水性聚氨酯织物整理剂.研究表明,合成最佳条件为预聚反应温度80℃,保温2h左右,扩链反应温度70℃,保温3h,氨基有机硅改性温度10℃,保温50min.自制的整理剂乳液粒径小、稳定性好,胶膜耐水性有明显提高,基本达到工业品要求,可以在工厂推广使用.     

低粘度氨基硅油的合成及微乳化

以八甲基环四硅氧烷(D4)、氨基硅烷偶联剂(YDH-602)及六甲基二硅氧烷(MM)为原料,以二甲基亚砜(DMSO)为促进剂,在KOH催化下,采用本体聚合法合成低粘度氨基硅油.通过IR和1HNMR对其进行结构表征;并选择壬基酚聚氧乙烯醚和脂肪醇聚氧乙烯醚作为复合乳化剂,将氨基硅油乳化成微乳液,研究复合乳化剂的配比和用量、助乳化剂的选择与用量、氨基硅油的含量对氨基硅油微乳化的影响,从而确定乳化的最佳工艺为:OP-4和AEO-9为复合乳化剂,mOP-4:mAEO-9=1∶1,其用量为氨基硅油质量的42%,乙二醇单丁醚为助乳化剂,其用量为氨基硅油质量的6%,形成氨基硅油质量分数为5%～15%、透明清晰且粒径小于50nm的氨基硅油微乳液.     

Synthesis and properties of perfluorinated alkyl silicone oil modified epoxy resin

Perfluorinated alkyl silicone oil （PFASO） was successfully synthesized from N-ethyl-N- hydroxylethyl perfluorinated octane sulfonamide, succinie anhydride and amino silicone oil by esterification and amide reaction at moderate temperature in the presence of different catalysts. The chemical structure of the synthesized samples was characterized by Fourier transform infrared spectroscopy （FT-IR）, the relative molecular mass（MM） and molecular mass distribution（MMD） of PFASO were tested by gel filtration chromatography（GFC）. A commercial epoxy resin （DGEBA） was modified with PFASO, with the content of PFASO 1-5 phr. Thermo-gravimetric analysis （TGA）, impact tests, scanning electron microscope （SEM） and water contact angle test were applied to provide accurate results on the thermal stability, toughness and hydrophobicity of PFASO/epoxy complex. The experimental results reveal that epoxy resins can be successfully modified by adding a small amount of as-synthesized modifiers via simple direct mixing, and verify that the as-synthesized modifier can improve the toughness and hydrophobicity of epoxy resin without sacrificing its thermal properties.     

乳化硅油制备的研究

采用转相乳化法，以较低黏度的二甲基硅油进行为原料，Span—60和Tween—60为乳化剂，成功制得了硅油乳液，质量配比为硅油10％，Span—60和Tween—60各占2.5％，增稠剂C占2％，离心及冻融实验证明乳液具有良好的稳定性，有一定应用价值。     

Special epoxy silicone adhesive for inertial confinement fusion experiment

The effects of toughener and coupling agent on special epoxy silicone adhesive were discussed by researching the surface morphology characters, thermal properties and shear strength of the adhesive. The results indicate that silicone coupling agent （KH-550） can improve the shear strength of the epoxy silicone adhesive effectively. The mass fraction of the toughener in the epoxy silicone adhesive plays an important role in its properties. When the mass fraction of the toughener is less than 14%, the shear strength of the adhesive is low. When the mass fraction of the toughener is over 33%, thermal properties and shear strength of the adhesive decrease with the increasing of the toughener. The mass fraction of toughener of 25% results in good integral properties of the epoxy silicone adhesive. The morphologic analysis indicates that the micro-phase separation exists in the epoxy molecular chain and the silicone molecular chain of the epoxy silicone adhesive.     

稠油化学组成对其粘度影响的灰熵分析

从稠油高粘度形成机制出发,采用灰色关联熵分析方法,以MATLAB为平台从计算化学角度探讨了稠油粘度特性与其组成、结构和性质之间的内在联系,考察了稠油化学组成和化学结构诸因素参与稠油高粘度形成过程的性质。由于对灰色关联分析法进行改进,不仅将稠油粘度与稠油组成关联起来,而且定量说明相关化学组成对稠油粘度的影响。结果表明,沥青质是影响稠油粘度的最主要因素,胶质和芳香烃起着稳定沥青质,防止其聚集分相的作用;而沥青质分子之间、沥青质与胶质分子之间的缔合与其分子中的杂原子、过渡金属、芳香结构和烷基侧链有着密切关系;沥青质分子中的极性部位(电负性部位)和配位基部位是引发沥青质分子聚沉的关键因素。有效降低沥青质分子内及分子之间的极性相互作用和配位作用,对稠油开采、集输及后加工处理将起到推动作用。     

Properties of functionalized graphene/room temperature vulcanized silicone rubber composites prepared by an In-situ reduction method

Functionalized graphene oxide (FGO) was prepared by treating graphene oxide with γ-aminopropyl triethoxysilane (KH-550) before the mixture was dispersed into α, ω-dihydroxy polydimethylsiloxane to get room temperature vulcanized (RTV) silicone rubber composites by solution casting. The cured composites were then reduced with hydrazine hydrate to obtain functionalized graphene (FG)/RTV silicone rubber composites. The structures of FGO and the resultant composites were characterized by atomic force microscopy, FT-IR spectra and X-ray diffraction. KH-550 was found to be grafted onto graphene sheets, leading to an increased interlayer spacing. Significant improvements in thermal and mechanical properties were obtained. Both the FGO/RTV silicone rubber composite contain 1.0 wt% of FGO, and its reduced product showed an increase of one-step weight loss temperature with 61 ℃ and 133 ℃ higher than that of pure silicone rubber. Tensile strength and elongation at break of FG/RTV silicone rubber composite (with 0.5 wt% FGO content) increased by 175% and 67%, respectively, compared with those of pure silicone rubber.     

Effect of carrier liquid on electrorheological performance and stability of oxalate group-modified TiO<Subscript>2</Subscript> suspensions

By using oxalate group-modified TiO₂ nanoparticles as the dispersing phase, different kinds of silicone oil with various viscosities and terminal groups (hydroxyl, hydrogen, and methyl) were used as the dispersing media to prepare different electrorheological (ER) fluids. Their zero-field viscosity, yield stress under direct current electric fields, ER efficiency, shear stability, leakage current density, and sedimentation stability were tested to study the effect of carrier liquid on the properties of ER fluids. The results indicate that the zero-field viscosity, the yield stress, and the leakage current density increase with increasing viscosity of the silicone oils. The effects of the viscosity on the ER efficiency, the shear stability, and the sedimentation ratio depend on the competition between the viscous resistance and the aggregation of the particles. Among the three ER fluids prepared with silicone oil with different terminal groups, hydroxyl-terminated oil based sample has the highest zero-field viscosity, the highest field-induced yield stress and ER efficiency, the largest current density, and the best sedimentation stability.     

空间用氯苯基硅油的弹流牵曳特性

基于Carreau剪切稀化非牛顿流变模型,针对一种空间用国产氯苯基硅油(CSO)弹流牵曳特性进行了完全数值解,CSO相关流变参数值为拟合实验数据所得.采用球-盘式弹流牵曳试验装置,测定了CSO在不同工况下弹流牵曳系数.将理论与实验结果进行比较表明,随着滑滚比的增大,CSO弹流牵曳系数经历了由急剧增加到缓慢增加,直至逐渐减小的过程.与其他2种润滑油相比,CSO弹流牵曳系数对载荷敏感度低,且在大滑滚比工况下弹流牵曳系数随滚动速度增大而减小.因此,在高速重载工况下,用CSO润滑的空间摩擦学部件寿命更长,动力消耗更低.但是,CSO在宽温度范围内,粘度变化幅度为5个数量级,因此,不适合在低温工况环境下使用.     

Effect of Carrier Liquid on Electrorheological Performance and Stability of Oxalate Group-modified TiO_2 Suspensions

By using oxalate group-modified TiO_2 nanoparticles as the dispersing phase, different kinds of silicone oil with various viscosities and terminal groups(hydroxyl, hydrogen, and methyl) were used as the dispersing media to prepare different electrorheological(ER) fluids. Their zero-field viscosity, yield stress under direct current electric fields, ER efficiency, shear stability, leakage current density, and sedimentation stability were tested to study the effect of carrier liquid on the properties of ER fluids. The results indicate that the zerofield viscosity, the yield stress, and the leakage current density increase with increasing viscosity of the silicone oils. The effects of the viscosity on the ER efficiency, the shear stability, and the sedimentation ratio depend on the competition between the viscous resistance and the aggregation of the particles. Among the three ER fluids prepared with silicone oil with different terminal groups, hydroxyl-terminated oil based sample has the highest zero-field viscosity, the highest field-induced yield stress and ER efficiency, the largest current density, and the best sedimentation stability.     

改善有机硅改性丙烯酸酯聚氨酯相容性的研究

采用丙烯酸酯单体与端羟基硅油、聚氧乙烯基醚进行自由基聚合反应和羟基缩合反应,制得了含有羟基的有机硅改性丙烯酸酯树脂,并以多异氰酸酯预聚体为交联剂配制成常温自干涂料,较好地改善了有机硅丙烯酸酯聚氨酯之间的相容性.借助红外光谱测试、差示扫描量热分析法、溶解度参数值分析等方法对产物的相容性进行了研究.实验表明,含有聚醚链段的有机硅改性丙烯酸酯聚氨酯涂料具有优异的综合性能.