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二甲基二(甲氨基)硅烷的合成工艺改进 被引量:1
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作者 滕雅娣 牛永伟 舒燕 《沈阳化工大学学报》 CAS 2011年第1期15-17,29,共4页
以乙醚为溶剂,二甲基二氯硅烷和甲胺反应得到二甲基二(甲氨基)硅烷.通过正交实验考察二甲基二氯硅烷浓度、反应温度和反应时间对二甲基二(甲氨基)硅烷产率的影响,用IR和1 HNMR对二甲基二(甲氨基)硅烷结构进行表征,发现二甲基二氯硅烷浓... 以乙醚为溶剂,二甲基二氯硅烷和甲胺反应得到二甲基二(甲氨基)硅烷.通过正交实验考察二甲基二氯硅烷浓度、反应温度和反应时间对二甲基二(甲氨基)硅烷产率的影响,用IR和1 HNMR对二甲基二(甲氨基)硅烷结构进行表征,发现二甲基二氯硅烷浓度为1.08 mol.L-1,反应温度为-12~-10℃,反应时间为4 h,产率可提高到80.6%. 展开更多
关键词 甲基二(氨基) 甲基二氯 合成 表征
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γ-氯丙基甲基二甲氧基硅烷合成工艺的研究 被引量:5
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作者 任海云 兰支利 尹笃林 《工业催化》 CAS 2005年第6期37-41,共5页
γ氯丙基甲基二甲氧基硅烷通常先由甲基二氯硅烷与氯丙烯通过硅氢加成生成γ氯丙基甲基二氯硅烷,再经醇解得到。在合成γ氯丙基甲基二氯硅烷的硅氢加成反应中,选用三乙胺作助催化剂与氯铂酸复合形成催化剂体系,并通过正交实验法优选出... γ氯丙基甲基二甲氧基硅烷通常先由甲基二氯硅烷与氯丙烯通过硅氢加成生成γ氯丙基甲基二氯硅烷,再经醇解得到。在合成γ氯丙基甲基二氯硅烷的硅氢加成反应中,选用三乙胺作助催化剂与氯铂酸复合形成催化剂体系,并通过正交实验法优选出该反应的最佳工艺条件,其产率达到85%,而且反应时间大大缩短。使用正交实验法对合成最终目标产物的醇解反应进行改进以选出最佳工艺条件,并且在反应过程中通过不断通入氮气来排尽HCl气体。反应过程中无需另外加入溶剂,使分离与提纯大大简化,从而达到节约成本、降低能耗的目的,是工业上切实可行的优选合成工艺。 展开更多
关键词 氢加成 r-氯丙基甲基二氯 r-氯丙基甲基
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甲基环己基二甲氧基硅烷的合成 被引量:2
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作者 杨春莉 周春艳 +1 位作者 李丽 金东升 《化学工程师》 CAS 2004年第4期12-13,共2页
本文以甲基三甲氧硅烷 ,氯代环己烷和镁为原料 ,通过格氏法合成甲基环己基二甲氧基硅烷。确定了合成工艺 ,同时分析了影响合成反应的主要因素。结果表明 ,在适宜的反应条件下 ,甲基环己基二甲氧基硅烷的产率可达 80 .2 %。
关键词 甲基环己基二氧基 甲基 氯代环己 格氏反应 助催化剂
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氨烃基与长链烷基共改性硅油的制备及应用性能 被引量:8
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作者 黄良仙 安秋凤 +3 位作者 李明涛 杨刚 王前进 付永山 《有机硅材料》 CAS 2007年第1期36-40,共5页
以八甲基环四硅氧烷、十二烷基甲基二甲氧基硅烷、N-β-氨乙基-γ-氨丙基甲基二甲基硅烷和六甲基二硅氧烷为原料,在四甲基氢氧化铵催化下,通过本体聚合反应合成了氨烃基与十二烷基共改性硅油(ADMPS);用红外光谱、核磁共振氢谱对其结构... 以八甲基环四硅氧烷、十二烷基甲基二甲氧基硅烷、N-β-氨乙基-γ-氨丙基甲基二甲基硅烷和六甲基二硅氧烷为原料,在四甲基氢氧化铵催化下,通过本体聚合反应合成了氨烃基与十二烷基共改性硅油(ADMPS);用红外光谱、核磁共振氢谱对其结构进行了表征,并用于白棉布的整理。结果表明,随着ADMPS的氨值的增加,经其整理的棉布的弯曲刚度减小、柔软性增强,折皱回复角增大、弹性提高、抗皱性能增强,吸湿性显著提高,而白度略下降;随着ADMPS的烷值的增加,经其整理的棉布的柔软性、抗皱性及弹性略有下降,而白度和吸湿性变化不大。在氨值相近的情况下,经通用型柔软剂N-β-氨乙基-β-氨丙基改性硅油整理的棉布的柔软性、弹性较好;而经ADMPS(烷值0.3mmol/g)整理的棉布的柔软性、弹性稍差一些,但平滑性和静态吸湿性更好;经二者整理的棉布的白度相当。 展开更多
关键词 N-β-氨乙基-γ-氨丙基甲基甲基 氨基 十二甲基氨基 织物 柔软剂
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含硅芳香二酐的合成及其聚酰亚胺 被引量:4
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作者 潘英 林保平 +3 位作者 钱鹰 浅井清次 井上真一 冈本弘 《功能高分子学报》 CAS CSCD 2003年第2期225-228,共4页
从4-溴-1,2-二甲苯出发,经过三步反应合成了双-(3,4-苯二甲酸酐)二甲基硅烷单体,总产率为24.7%;由该单体与4,4’-二氨基二苯醚共聚合,经环化脱水反应得含硅聚酰亚胺,并对该共聚物进行了初步表征。
关键词 4-溴-l 2-二 双-(3 4-苯二酸酐)二甲基 4 4′-二氨基二苯醚 共聚 环化脱水 合成 聚酰亚胺 芳香二酐
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氯化锌催化合成含硅芳炔树脂 被引量:4
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作者 姜欢 邓诗峰 阮湘政 《高分子材料科学与工程》 EI CAS CSCD 北大核心 2017年第11期18-21,28,共5页
以二乙炔基苯、双(二甲氨基)二甲基硅烷为原料,乙腈为溶剂,通过氯化锌催化实现单步硅烷化合成含硅芳炔树脂。研究结果表明,乙腈做溶剂,二乙炔基苯与双(二甲氨基)二甲基硅烷投料比为9∶8(摩尔比),ZnCl_2相对于炔过量0.65倍,回流反应11h... 以二乙炔基苯、双(二甲氨基)二甲基硅烷为原料,乙腈为溶剂,通过氯化锌催化实现单步硅烷化合成含硅芳炔树脂。研究结果表明,乙腈做溶剂,二乙炔基苯与双(二甲氨基)二甲基硅烷投料比为9∶8(摩尔比),ZnCl_2相对于炔过量0.65倍,回流反应11h效果最佳,收率高达90%以上;制备的含硅芳炔树脂在室温下呈流动状态,加工性能良好,加工温度为40~180℃,加工窗口为140℃;固化后的含硅芳炔树脂,在N_2气氛下热分解5%时的温度(T_(d5))为587℃。 展开更多
关键词 芳炔树脂 单步 氯化锌 双(二氨基)二甲基
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Synthesis and characterization of copolyimides from bis(3,4-dicarboxyphenyl)dimethylsilane dianhydride 被引量:2
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作者 林保平 钱鹰 +1 位作者 潘英 袁春伟 《Journal of Southeast University(English Edition)》 EI CAS 2004年第2期216-220,共5页
The silicon-containing poly (amic acid)s were synthesized from bis (3, 4-dicarboxyphenyl) dimethylsilane dianhydride (SIDA), pyromellitic dianhydride (PMDA) and 4,4′-oxydianiline (4,4'-ODA) in N, N-dimethylacetam... The silicon-containing poly (amic acid)s were synthesized from bis (3, 4-dicarboxyphenyl) dimethylsilane dianhydride (SIDA), pyromellitic dianhydride (PMDA) and 4,4′-oxydianiline (4,4'-ODA) in N, N-dimethylacetamide (DMAc). The poly (amic acid) films were obtained by solution-cast method from DMAc solutions and thermally converted into transparent, flexible and tough polyimide films. The wide-angle X-ray diffraction diagrams revealed that all the polyimides possessed amorphous character, and the regulation of those polyimides were decreased with the increase of the molar ratio of SIDA to PMDA. Differential scanning calorimeter measurements showed that the introduction of SIDA to polyimide backbone would make glass transition temperature shift to lower temperature. Thermogravimetric analyses indicated that the silicon-containing polyimides lowered decomposition temperature as compared with PMDA/4, 4′-ODA polyimides. However, UV-visible transmission and reflection spectra showed that the optical transparency of silicon-containing polyimide thin films was superior to that of PMDA/4, 4'-ODA polyimide thin films. 展开更多
关键词 CALORIMETERS Glass transition Thin films TRANSPARENCY X ray diffraction
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憎水涂料
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《涂料技术与文摘》 2002年第6期67-67,共1页
形成疏水、疏油和热反射涂膜的题述组合物含可水解的烃基硅烷或它们的水解缩合物、粒径为1~50μm的红外反射颜料,溶剂和/或分散介质,也可以存在一定量的使涂膜不透明的颜料,或使用提供不透明性的材料。将3-((?)乙氧基甲基甲硅烷基... 形成疏水、疏油和热反射涂膜的题述组合物含可水解的烃基硅烷或它们的水解缩合物、粒径为1~50μm的红外反射颜料,溶剂和/或分散介质,也可以存在一定量的使涂膜不透明的颜料,或使用提供不透明性的材料。将3-((?)乙氧基甲基甲硅烷基)丙胺1.91 g、(EtO)<sub>4</sub>Si0.208 g和水10 g的混合物预水解20 min, 展开更多
关键词 甲基甲硅烷 涂料 反射涂膜 憎水 红外反射 分散介质 水解缩合 不透明性 预水解 聚丙烯酸
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Isobaric Vapor-Liquid Equilibrium for Methyldichlorosi-lane+Methylvinyldichlorosilane+Toluene and Constituent Binary Systems 被引量:8
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作者 余淑娴 余祖兵 +1 位作者 邱祖民 孙韡 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2003年第2期213-216,共4页
Vapor-liquid equilibrium (VLE) for a ternary system of methyldichlorosilane + methylvinyldichlorosi-lane + toluene and constituent binary systems were measured at 101.3kPa using a new type of magnetical pump-ebulliome... Vapor-liquid equilibrium (VLE) for a ternary system of methyldichlorosilane + methylvinyldichlorosi-lane + toluene and constituent binary systems were measured at 101.3kPa using a new type of magnetical pump-ebulliometer. The equilibrium compositions of the vapor phase of binary systems were calculated indirectly from the total pressure-temperature-liquid composition (pTx). The experimental data were correlated with the Wilson and NRTL(non-random two liquid) equations. The parameters of the Wilson model were employed to predict the ternary VLE data. The calculated boiling points were in good agreement with the experimental ones. 展开更多
关键词 METHYLDICHLOROSILANE methylvinyldichlorosilane TOLUENE vapor-liquid equilibrium
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A Bi-component Cu Catalyst for the Direct Synthesis of Methylchlorosilane from Silicon and Methyl Chloride 被引量:2
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作者 汪超 王光润 王金福 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2014年第3期299-304,共6页
A bi-component catalyst comprising CuC1 and metallic copper was used in the direct synthesis of me- thylchlorosilane to study the catalytic synergy between the different copper sources. The catalyst exhibited high ac-... A bi-component catalyst comprising CuC1 and metallic copper was used in the direct synthesis of me- thylchlorosilane to study the catalytic synergy between the different copper sources. The catalyst exhibited high ac- tivity and high selectivity of dimethyldichlorosilane (M2) in the stirred bed reactor. The effect of the proportion of CuC1 used was studied and 10%-30% CuC1 gave the best yield of M2. The use of CuC1 decreased the induction pe- riod of reaction, improved the selectivity in the induction stage, and gave a longer stable stage. These results sug- gest that bi-comoonent catalyst has advantazes in the direct synthesis reaction. 展开更多
关键词 methylchlorosiiane direct synthesis bi-component catalyst SYNERGY
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Modification of methyl oleate for silicon-based biological lubricating base oil 被引量:1
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作者 Shixing Cui Zhi Yun Xia Gui 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2017年第1期130-136,共7页
A new kind of silicon-based biological lubricating base oil with good viscosity-temperature behavior,viscosity index,thermostability,oxidation stability and wear resistance performance was synthesized as a derivative ... A new kind of silicon-based biological lubricating base oil with good viscosity-temperature behavior,viscosity index,thermostability,oxidation stability and wear resistance performance was synthesized as a derivative of methyl oleate.Trimethylsilylation reaction was introduced to further improve methyl oleate oxidation stability and lubricity after epoxidation and open-ring reactions.The order of effectiveness of acid binding agent was N,N-diisopropylethylamine(DIEA) > pyridine > diethylamine > triethylamine,and the effects of various parameters on the trimethylsilylation reaction as well as on the silicon-oxygen bond stability and reaction yield were studied.A maximum yield of 34.54%was achieved at hydroxyl/trimethyl chlorosilane/DIEA molar ratio of1:1.25:1,reaction temperature 40℃,reaction time 1.5 h. 展开更多
关键词 Methyl oleate Trimethyl chlorosilane Acid binding agent N N-diisopropylethylamine Lubricity Silicon-based biological lubricating base oil
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Isobaric vapor-liquid equilibrium for methyldichlorosilane-methyltrichlorosilane-dimethyldichlorosilane system
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作者 邱祖民 谢心亮 +1 位作者 罗美 谢凤霞 《Journal of Zhejiang University-Science B(Biomedicine & Biotechnology)》 SCIE CAS CSCD 2005年第6期559-562,共4页
The elucidation of vapor-liquid equilibrium (VLE) of the halogenated silane was necessary for the production of silicon derivatives, especially for methylvinyldichlorosilane, due to the lack of the relevant reports. I... The elucidation of vapor-liquid equilibrium (VLE) of the halogenated silane was necessary for the production of silicon derivatives, especially for methylvinyldichlorosilane, due to the lack of the relevant reports. Isobaric VLE for the system methyldichlorosilane-dimethyldichlorosilane-benzene and isobaric VLE of the three binary systems were measured with a new pump-ebulliometer at the pressure of 101.325 kPa. These binary compositions of the equilibrium vapor were calculated according to the Q function of molar excess Gibbs energy by the indirect method and the resulted VLE data agreed well with the thermo-dynamic consistency. Moreover, the experimental data were correlated with the Wilson, NRTL, Margules and van Laar equations by means of the least-squares fit, the acquired optimal interaction parameters were fitted to experimental vapor-liquid equilibrium data for binary systems. The binary parameters of Wilson equation were also used to calculate the bubble point temperature and the vapor phase composition for the ternary mixtures without any additional adjustment. The predicted vapor-liquid equilibrium for the ternary system was in a good agreement with the experimental results. The VLE of binary and multilateral systems provided essential theory for the production of the halogenated silane. 展开更多
关键词 EBULLIOMETER Vapor-liquid equilibrium METHYLDICHLOROSILANE DIMETHYLDICHLOROSILANE BENZENE
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Toluene degradation by a water/silicone oil mixture for the design of two phase partitioning bioreactors 被引量:3
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作者 Maxime Guillerm Annabelle Couvert +3 位作者 Abdeltif Amrane Edith Norrant Audrey Breton éric Dumont 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2017年第10期1512-1518,共7页
Toluene degradation performances were studied in a 10 L Two-Phase Partitioning Bioreactor(TPPB).The liquid phase consisted of a mixture of water and PDMS 50(Poly Di Methyl Siloxane,i.e.silicone oil,viscosity of 46 m P... Toluene degradation performances were studied in a 10 L Two-Phase Partitioning Bioreactor(TPPB).The liquid phase consisted of a mixture of water and PDMS 50(Poly Di Methyl Siloxane,i.e.silicone oil,viscosity of 46 m Pa·s) in the volume ratio of 75%/25%.Two series of experiments were carried out:in the first,the reactor was sequentially supplied with toluene whereas in the second,toluene was continuously supplied.Activated sludge from the wastewater treatment plant of Beaurade(Rennes,France) was used at an initial concentration of 0.5 dry mass g·(mixture L)^(-1).The elimination capacity(EC) was investigated as well as the change in biomass concentration over time.Toluene biodegradation was very ef ficient(removal ef ficiency,RE=100%) for toluene flows ranging from 0.2 to 1.2 ml·h^(-1),corresponding to elimination capacities of up to 104 g·m^(-3)·h^(-1).For a toluene flow of 1.2 ml·h^(-1),the biomass concentration measured at the end of the experiment was 4.7 dry mass g·(mixture L)^(-1).The oxygen concentration in the liquid phase was clearly not a limiting factor in these operating conditions.Based on these results,an extrapolation leading to the design of a large-scale pilot TPPB can now be considered to study toluene degradation performances in industrial conditions. 展开更多
关键词 Degradation Toluene Silicone oil Multiphase reactor Biomass
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A novel method for fabricating polydimethylsiloxane microfluidic chip master molds
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作者 甘婷婷 夏之宁 《Journal of Chongqing University》 CAS 2009年第2期139-144,共6页
We proposed a novel method of fabricating polydimethylsiloxane (PDMS) microfluidic chip polymer master molds in this paper. The method mainly includes two steps. First, a stainless steel slice was laser etched to form... We proposed a novel method of fabricating polydimethylsiloxane (PDMS) microfluidic chip polymer master molds in this paper. The method mainly includes two steps. First, a stainless steel slice was laser etched to form a metal model. Then, the organic solution of poly(methyl methacrylate) (PMMA) was casted onto the metal model to fabricate the PMMA master which subsequently would be used to fabricate PDMS chips. We systematically researched different laser parameters influencing the surface status of microchannels and obtained optimized etching parameters. We investigated and optimized the organic solution composition of PMMA while casting chip masters, and developed a method to form fine polymer masters using two different viscosity solutions to cast the model in turn, and studied the repeatable replication. Then, we investigated physical performance of this chip and evaluated the practicability by analyzing Rhodamine B. Compared with present methods, the proposed method does not need photolithography on photoresistant and chemical etching. The entire fabricating progress is simple, fast, low-cost and can be controlled easily. Only several minutes are required to make a metal model, 3 hours for a PMMA master, and one day for PDMS chips. 展开更多
关键词 microfluidic chip laser etching stainless steel model POLYDIMETHYLSILOXANE poly(methyl methacrylate)
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Nano-indentation profiles of intrinsic hardness and modulus of films based on silsesquioxane modified with titanium tetrabutoxide
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作者 陈平 孙科军 +2 位作者 刘今成 崔津津 胡立江 《Journal of Harbin Institute of Technology(New Series)》 EI CAS 2004年第6期644-648,共5页
This study is to analyze the influence of the modifier, 5~25 wt % titanium tetrabutoxide (TBO), on the hardness and elastic modulus of the films based on SSO deriving from hydrolytic condensation of (3-glycidoxypropy... This study is to analyze the influence of the modifier, 5~25 wt % titanium tetrabutoxide (TBO), on the hardness and elastic modulus of the films based on SSO deriving from hydrolytic condensation of (3-glycidoxypropyl)trimethoxysilane (GPMS) and vinyltrimethoxysilane (VMS), by the continuous stiffness measurement (CSM) technique of an instrumented-indentation testing (IIT) device. Films were synthesized by adding the stoichiometric amount of ethylenediamine (EDA) and benzoyl proxide (BPO) to SSO solutions in ethanol, dip-coating over glass substrates, and curing using an appropriate thermal cycle. Intrinsic values of hardness and elastic modulus were determined with the average values in “plateau region” from “four-layer” explanation. And the brittle index of the modified coating systems was analyzed. 展开更多
关键词 silesesquioxanes (3-glycidoxypropyl)trimethoxysilane VINYLTRIMETHOXYSILANE titanium tetrabutoxide HARDNESS elastic modulus brittle index
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Disiloxane-Bridged Cyclopolymer as Polymer Dielectrics
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作者 邓昶 刘和文 《Chinese Journal of Chemical Physics》 SCIE CAS CSCD 2017年第5期571-575,I0002,共6页
We studied the dielectric properties of organosilicon-containing helical cyclopolymer PbMA which consists of PMMA main chains and tetramethyldisiloxane side rings. PbMA formed films with excellent uniformity through s... We studied the dielectric properties of organosilicon-containing helical cyclopolymer PbMA which consists of PMMA main chains and tetramethyldisiloxane side rings. PbMA formed films with excellent uniformity through spin-coating onto highly n-doped silicon (n-Si) wafers for constructing devices of dielectric measurements, on which the dielectric properties and I-V characteristics of PbMA were studied. PbMA has a much lower dielectric constant (lower than 2.6) in the frequency range of 10-105 Hz, and better thermal stability than PMMA does. I-V data showed that the metal/PbMA/n-Si devices have different conducting directions, depending on whether Au or Al deposited over PbMA layers. 展开更多
关键词 Polymer dielectrics Spin-coating film Disiloxane-bridged cyclopolymer
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