聚二甲基硅烷的合成及光谱分析

以二甲基二氯硅烷（ （ＣＨ３）２ＳｉＣｌ２） 为原料, 通过Ｗüｒｔｚ 还原反应合成出聚二甲基硅烷。实验表明： 纯度高的原料使产物产率大幅提高, 用ＵＶ 和ＦＴ－ ＩＲ 对聚二甲基硅烷的结构进行表征。     

聚甲基氢硅烷及其共聚物的合成及发光性能的研究

以甲基二氯硅烷,二甲基二氯硅烷,二苯基二氯硅烷及甲基乙烯基二氯硅烷为原料,采用钠缩合法合成了聚甲基氢硅烷及聚甲基氢硅烷与聚二甲基硅烷,聚二苯基硅烷和聚甲基乙烯基硅烷的共聚物,并用IR,UV,1HNMR,GPC进行了表征。     

聚二甲基硅烷的合成及光谱分析

以二甲基二氯硅烷（ＣＨ３）２ＳｉＣｌ２）为原料,通过Ｗｕｅｒｔｚ还原反应合成出聚二甲基硅烷。实验表明：纯度高的原料使产物产率大幅提高,用ＵＶ和ＦＴ－ＩＲ对聚二甲基硅烷的结构进行表征。     

聚二甲基硅烷合成聚碳硅烷的研究

以聚二甲基硅烷为原料,采用正交设计的方法研究了常压高温裂解重排法中反应温度,裂解温度,保温时间对聚碳硅烷结构的影响,结果发现,该合成方法的最佳工艺条件为：反应温度470－475℃,裂解温度560℃,保温时间6h,3个因素对聚碳硅烷的显著性影响顺序为：反应温度＞保温时间＞裂解温度,从聚二甲基硅烷出发合成的先驱体聚碳硅烷的支化度较低,可纺性好。     

二苯基二乙氧基硅烷的合成研究

以乙醇、二苯基二氯硅烷为原料采用直接法合成二苯基二乙氧基硅烷。考察了反应时间、反应温度、原料配比、溶剂用量等因素对反应的影响。实验结果表明,最佳的反应条件为:n(乙醇)∶n(二苯基二氯硅烷)=2.6∶1,保温82℃反应5 h,甲苯用量50 g。在此条件下,产品收率达86.7%,产品纯度高达97.2%。采用红外光谱和核磁共振氢谱对其结构进行了确证。     

聚二苯基-二甲基硅氧烷的合成与应用研究进展

综述了聚二苯基-二甲基硅氧烷的合成与应用研究进展。     

二乙烯基苯/聚二甲基硅烷改良聚碳硅烷合成工艺的研究

在传统的合成体系中加入适量的二乙烯基苯,通过常压高温自由基聚合反应,获得了产率较高、可纺性优良的先驱体聚碳硅烷。采用正交实验设计研究了反应温度、升温速率、二乙烯基苯的质量分数、裂解温度和保温时间五个因素对聚碳硅烷产率的影响。方差分析表明,在反应温度为420℃、二乙烯基苯的质量分数为1·5%、升温速率为6℃/h、裂解温度为530℃、保温时间为5h条件下,可以得到粗产率为50%的黄色透明固态聚碳硅烷;各因素对聚碳硅烷产率影响的显著性依次为:升温速率>反应温度>二乙烯基苯的质量分数>保温时间>裂解温度。     

二苯基二氯硅烷的性质及合成方法概述

二苯基二氯硅烷（SiPh2Cl2）主要由氯苯和硅粉在催化剂的条件下反应或者由苯基氯化镁与四氯化硅反应生成,能与活泼金属（钠,锂,镁）发生反应,生成苯基环硅烷,除此之外,它还容易发生歧化,水解,醇解等反应.     

二甲基硅二醇的合成

本文报道了二甲基二氯硅烷直接水解制备二甲基硅二醇的过程，考察了二甲基二氯硅烷、水、乙醚在不同的投料比下产品二甲基硅二醇的收率。当水的加入量为理论需求量的１～１．０２５倍，乙醚的加入量为２．５～３Ｌ／ｍｏｌ（ＣＨ＿３）＿２ＳｉＣｌ＿２时，产品的收率在７０％以上。实验中选择了苯胺为氯化氢的吸收剂。所得产品为白色有光泽的鱼鳞片状物质，经熔点测定，Ｃ、Ｈ、Ｓｉ元素分析及电子轰击质谱测定，所得产品确系纯度较高的二甲基硅二醇。实验中考察了二甲基硅二醇产品的储存稳定性，室温下存放期不超过９０天，低温冷冻存放刚可超过一年。     

硅烷芳炔-硅氧烷芳炔嵌段共聚物的合成与表征

合成了不同链段长度的卤代硅氧烷,并用其与间二乙炔基苯格氏试剂反应,合成了两种硅烷芳炔-硅氧烷芳炔嵌段共聚物（SiO-b-PSA）,并制成碳纤维增强树脂复合材料。利用红外光谱（FT-IR）、核磁共振氢谱（¹H NMR）、凝胶渗透色谱（GPC）、旋转流变、差示扫描量热分析（DSC）、热失重分析（TGA）和悬梁臂冲击实验对共聚物及其复合材料的结构和性能进行表征。研究结果表明所合成的共聚物具有优良的耐热性和韧性,硅烷芳炔-硅氧烷芳炔嵌段共聚物在氮气气氛下的T_d5高于513℃,1000℃残留率高于78.9%,硅烷芳炔-硅氧烷芳炔嵌段共聚物/碳纤维复合材料的冲击强度高达（30.92±0.44） kJ·m^-2。     

Synthesis and characterization of hyperbranched poly(silyl ester)s

Hyperbranched poly(silyl ester)s were synthesized via the A₂ + B₄ route by the polycondensation reaction. The solid poly(silyl ester) was obtained by the reaction of di‐tert‐butyl adipate and 1,3‐tetramethyl‐1,3‐bis‐β(methyl‐dicholorosilyl)ethyl disiloxane. The oligomers with tert‐butyl terminal groups were obtained via the A₂ + B₂ route by the reaction of 1,5‐dichloro‐1,1,5,5‐tetramethyl‐3,3‐diphenyl‐trisi1oxane with excess amount of di‐tert‐butyl adipate. The viscous fluid and soft solid poly(silyl ester)s were obtained by the reaction of the oligomers as big monomers with 1,3‐tetramethyl‐1,3‐bis‐β(methyl‐dicholorosilyl)ethyl disiloxane. The polymers were characterized by ¹H NMR, IR, and UV spectroscopies, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). The ¹H NMR and IR analysis proved the existence of the branched structures in the polymers. The glass transition temperatures (T_g's) of the viscous fluid and soft solid polymers were below room temperature. The T_g of the solid poly(silyl ester) was not found below room temperature but a temperature for the transition in the liquid crystalline phase was found at 42°C. Thermal decomposition of the soft solid and solid poly(silyl ester)s started at about 130°C and for the others it started at about 200°C. The obtained hyperbranched polymers did not decompose completely at 700°C. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 3430–3436, 2006     

Synthesis and characterization of linear asymmetrical poly(propylene oxide) diol

Linear asymmetrical poly(propylene oxide) was synthesized through four‐step reactions: selective benzylation, alcohol exchange reaction, propylene oxide anionic polymerization, debenzylation. One terminal of the asymmetrical polymer chains is alcohol hydroxyl and the other is phenol hydroxyl. It was characterized with infrared (IR) and ¹H Nuclear Magnetic Resonance (¹H‐NMR). Peaks at 1.11, 3.38, and 3.53 ppm were attributed to side groups (? OCH₂CH(CH₃)? ), backbone units (? OCH₂CH(CH₃)? ) and (? OCH₂CH(CH₃)? ) of poly(propylene oxide), respectively. Molecular weight and molecular weight distribution were measured with ¹H‐NMR and laser light scattering (LLS), which showed that the linear asymmetrical poly(propylene oxide) was mono‐disperse (PDI = 1.02–1.07). Then, its carbamate reaction with phenyl isocyanate was studied; the reaction rate constants for phenol hydroxyl and alcohol hydroxyl of poly(propylene oxide) were k₁ = 0.209 mol L^?1 min^?1 and k₂ = 0.051 mol L^?1 min^?1. There was a great reactivity difference for two types of hydroxyls in asymmetrical poly(propylene oxide), contrasting to the single carbamate reaction rate constant of symmetrical poly(propylene oxide) (k₃ = 0.049 mol L^?1 min^?1). © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Synthesis, characterization and catalytic properties of palladium-containing poly(allylbenzene p-sulphonic acid) films

This work reports results achieved when a specially designed monomer, the allyl ether of p-benzenesulphonic acid, with a pendent anionic group, was used to prepare a polymeric matrix. Ion exchange with cupric ions followed by electrochemical reduction provided polymer films with highly dispersed Cu⁰ particles. Immersion of the copper bearing modified electrode in a PdCl₄ ²⁻ containing solution produced a displacement reaction causing the deposition of 50–200 nm sized Pd particles. The presence of Pd particles in the so-prepared films was confirmed by voltammetry, SEM/EDS and XRD. The behaviour of the submicron Pd particle/poly(allylbenzene p-sulphonic acid) modified electrode towards the HER was evaluated by recording polarization curves. The electrocatalytic activity reveals that the methodology is a promising approach for the preparation of cathodes for the electrohydrogenation of organic molecules.     

利用Heck反应制备立构规整聚(3-己基噻吩)

采用Heck反应法合成了具有较高分子量和立构规整度的聚(3-己基噻吩)。研究了溶剂的种类及配比、相转移催化剂及催化剂的种类以及反应温度、反应时间对所得聚(3-己基噻吩)的分子量和规整度的影响。用凝胶色谱(GPC)和核磁共振谱(1HNMR)对聚(3-己基噻吩)的分子量及立构规整度进行了表征。用紫外-可见分光光度计和荧光分光光度计研究了聚(3-己基噻吩)的吸收光谱和发射光谱。结果表明,当溶剂为二甲基甲酰胺与四氢呋喃(DMF:THF=1:1)的混合溶剂,采用醋酸钯[用量为单体量的5%(摩尔分数)]为催化剂,四丁基溴化铵[用量为单体量的100%(摩尔分数)]为相转移催化剂时,在80℃下反应12h所得聚(3-己基噻吩)的分子量可达6700,立构规整度超过96%。     

2-[4-(9H-9-咔唑)-苯基]蒽醌的合成与表征

以苯酐和咔唑为原料,通过Friedel-Crafts酰基化、浓硫酸催化、Ullman、Suzuki偶联等反应,合成了标题化合物,并对该化合物进行紫外可见吸收和荧光分析。     

Synthesis and characterization of new poly(siloxysilanes)

The efficient synthesis of two new monomers, vinyltris(dimethylsiloxy)silane (2) and tris(dimethylvinylsiloxy)silane (3), was developed. Hydrosilation of these new A–B₃ monomers affords highly branched starburst poly(siloxysilane) polymers. Polymerization of2 yields a polymer structure that has siliconhydride functional groups on the outer sphere. Polymerization of3 yields a polymer that has the same hyperbranched poly(siloxysilane) core as the polymer produced from2, but the outer sphere contains vinyl moieties. The presence of silicon-hydride or vinyl groups on the surface of both polymers allows functionalization of these materials with a wide variety of reagents.Presented at the XXVIth Silicon Symposium, Indiana University—Purdue University at Indianapolis, March 26–27, 1993.     

聚4-乙烯基吡啶的合成与表征

以过氧化二苯甲酰(BPO)为引发剂,用悬浮聚合的方法制备了较高相对分子质量的聚4 乙烯基吡啶(P4VP)。通过对聚合产物相对分子质量测试结果的分析,研究了单体与水的体积比、引发剂用量、分散剂用量、反应时间、反应温度、搅拌速度等因素对4 VP聚合反应的影响。结果表明,聚合时间为1h、聚合温度为60℃、引发剂的质量分数(占单体量)为0.8%左右、分散剂的质量分数(占单体量)为0.6%、搅拌速度为300r/min时,P4VP的重均分子量就能达到6×105～9×105。另外,采用紫外吸收光谱(UV)、红外吸收光谱(IR)、核磁共振氢谱(1H NMR)、核磁共振碳谱(13C NMR)、热重 差热分析(TG DTA)等测试手段研究了P4VP的结构和性能。     

Grafting of oligopeptide on poly(aminostyrene)s and characterization of the polymers

Graft copolymers that have oligopeptides (OP) as graft molecules were prepared through the coupling reaction of the carboxylic acids of OP with the amino groups of poly(aminostyrene)s (PAS). The three OPs are Boc‐Gly, Z‐Gly‐Pro, and Z‐Gly‐Pro‐Leu‐Gly‐Pro, where Boc and Z are, respectively, the t‐butyloxycarbonyl group and benzyloxycarbonyl group as protective groups on nitrogen. The two PASs are poly(4‐vinylphenylamine) and poly(N‐isopropyl‐4‐vinylbenzylamine). These polymers that have narrow molecular weight distributions were prepared via anionic living polymerization. The coupling reaction to form the peptide bonds was mediated by dicyclohexylcarbodiimide in a mixed solvent of N,N′‐dimethylformamide and methyl chloride. The degree of grafting (DOG) on PAS was determined from the ¹H‐NMR spectrum. The dependence of the reaction time (0–8 h) on the DOG, the dependence of the reaction temperature (0–45°C) on the DOG, and the dependence of the molar ratio of OP to the amino group of PAS (1–4 times) on the DOG were studied. By alternating the reaction time and the molar ratio, the DOG values of PAS could be controlled in the range from 0 to 100%. DOG seems to be independent of the molecular weight of OP and the degree of basicity of PAS. The contact angle of the resultant graft copolymers was measured and the preliminary nonthrombogenic test was also performed. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 1558–1567, 2000     

羟基聚甲基苯基硅氧烷的合成与表征

以甲基苯基二乙氧基硅烷(MPS)和八甲基环四硅氧烷(D4)为原料,在酸性条件下水解MPS,水解产物在碱催化下与D4开环共聚合制备了高苯基含量羟基封端的聚甲基苯基硅氧烷齐聚物(PMPS)。用GPC测试了相对分子质量及其分布;用FTIR,^1H—NMR对其结构进行了表征。结果发现,在试样PMPS—6中,苯基结构单元与非苯基结构单元组成比为0．65,硅羟基质量分数为0．5％。