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《聚醚技术工艺荟萃,聚醚硅氧烷、改性聚硅氧烷、氨基硅氧烷类技术工艺与配方全集》
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《聚醚技术工艺荟萃,聚醚硅氧烷、改性聚硅氧烷、氨基硅氧烷类技术工艺与配方全集》(图1)
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优秀研究生学位论文题录展示聚醚/紫外吸收基聚硅氧烷整理剂的合成及复配专 业: 有机化学关键词: 基聚硅氧烷 整理剂 紫外吸收剂 二苯甲酮衍生物 纳米TiO2分类号: TQ610.491形 态: 共 63 页 约 41,265 个字 约 1.974 M内容阅 读:
内容摘要本课题将研制的聚硅氧烷紫外吸收剂中效果较好的PE-PUVSi与纳米级紫外屏蔽剂进行复配,期望能产生协同效应,并降低成本。
利用自制的二苯甲酮衍生物与聚甲基氢硅氧烷的硅氢化加成反应,合成了一系列紫外吸收基聚硅氧烷。用红外光谱(IR)、紫外(UV)光谱、核磁共振氢谱(1H-NMR)、凝胶渗透色谱(GPC)等仪器对有关聚硅氧烷的结构、性能和应用进行了研究。用原子力扫描电镜AFM及SEM扫描电镜对有关硅膜的形态进行了观察。论文主要工作如下:
(1)在催化剂作用下,利用2,4-二羟基二苯甲酮与烯丙基缩水甘油醚的开环反应,合成了中间体4-(β-羟基-γ-烯丙氧)丙氧基-2-羟基二苯甲酮(MUV-O)。将含氢硅油(PHMS)与MUV-O、α-烯丙基聚氧乙烯醚(CG-5)进行硅氢化加成反应,继而合成了侧链同时携带有二苯甲酮衍生物侧基以及聚醚基的聚硅氧烷PE-PUVSi。用IR、1H-NMR、UV谱、GPC等仪器对PE-PUVSi的结构和性能进行了研究。结果表明,PE-PUVSi对波长为243.6nm、289.2nm、325.0nm的紫外光有强吸收作用。经其整理的织物柔软、紫外光透过率低。
(2)将合成的聚醚\二苯甲酮衍生物侧基聚硅氧烷PE-PUVSi与偶联剂改性后的纳米TiO2进行复配,获得了纳米复合聚硅氧烷整理剂TiO2\PE-PUVSi。利用IR、1H-NMR、UV谱、电脑测控柔软度测定仪等对其结构、性能和应用分别进行了研究。结果表明TiO2\PE-PUVSi对240~326nm区间的紫外光有强吸收作用,可见紫外吸收剂PE-PUVSi与紫外屏蔽剂TiO2之间产生了自协同效应。
(3)将4-(β-羟基-γ-烯丙氧)丙氧基-2-羟基二苯甲酮(MUV-O)与四甲基环四硅氧烷(D4H)及烯丙基缩水甘油醚(AGE)、烯丙基聚氧乙烯醚(CG-5)共同反应,合成了一种小分子水溶性、且可赋予织物良好抗紫外效果的环状低聚体聚硅氧烷整理剂(DMUV-O)。研究结果表明,DMUV-O对240~326nm的紫外光依然有强吸收作用。
(4)利用原子力扫描电镜(AFM)、扫描电镜(SEM)等仪器对负载在纤维和模拟纤维基质――单晶硅表面的PE-PUVSi和DMUV-O的膜形貌进行了观察。结果发现,侧基UV可使PE-PUVSi膜出现针状尖峰形貌,而侧基PE可在膜表面卷曲形成大的峰包。小分子水溶性紫外吸收剂聚硅氧烷DMUV-O在纤维和单晶硅基质表面同样也可成膜。在放大倍数为5000的宏观条件下,DMUV-O在纤维表面显示出一种相对较为平滑的硅膜。而在扫描范围为10μO、观察标尺为50nm微观条件下,DMUV-O则显示出一种弯曲的、类似河流状的不连续形貌..……
全文目录文摘英文文摘论文说明:符号说明1抗紫外后整理剂综述1.1紫外线的特性及其危害1.1.1紫外线的特性1.1.2紫外线的危害1.2织物用紫外线吸收剂的种类及其发展1.2.1水杨酸酯、二苯甲酮及其衍生物1.2.2苯并三唑及其衍生物1.2.3聚硅氧烷类紫外吸收剂1.3紫外屏蔽剂的特点及种类1.3.1纳米材料的定义、特性及其纳米效应1.4无机纳米粒子TiO2的抗紫外线机理1.5纳米TiO2的表面改性技术1.5.1纳米TiO2粒子的表面改性剂1.5.2纳米TiO2表面改性机理1.6课题的提出及创新之处2聚醚-紫外吸收基聚硅氧烷PE-PUVSi的合成、表征与应用2.1实验部分2.1.1原料与试剂2.1.2聚醚-紫外吸收基聚硅氧烷(PE-PUVSi)的合成2.1.3 PE-PUVSi的结构表征与物化性能测试2.1.4 PE-PUVSi的乳化及乳液稳定性测试2.1.5 PE-PUVSi整理的织物性能测试2.2结果与讨论2.2.1 PE-PUVSi的表征2.2.2 PE-PUVSi的应用性能与其分子结构的关系2.3小结3纳米TiO2的化学改性及其与PE-PUVSi的复配研究3.1实验部分3.1.1原料与试剂3.1.2 TiO2的改性及其与聚醚/紫外吸收基聚硅氧烷PE-PUVSi的纳米复配3.1.3纳米复合聚硅氧烷整理剂TiO2/PE-PUVSi的结构表征与物化性能测试3.1.4 TiO2/PE-PUVSi乳化及乳液性能测试3.1.5 TiO2/PE-PUVSi的应用性能研究3.2结果与讨论3.2.1 TiO2/PE-PUVSi的结构表征结果3.2.2制备TiO2/PE-PUVSi最佳反应条件的探索3.3TiO2/PE-PUVSi应用性能研究3.3.1 TiO2/PE-PUVSi所整理的棉织物的白度3.3.2 TiO2/PE-PUVSi所整理的棉织物的柔软性3.3.3 TiO2/PE-PUVSi所整理的棉织物的卫生透气性3.3.4 TiO2/PE-PUVSi所整理的棉织物的吸水性3.3.5 TiO2/PE-PUVSi所整理的棉织物的抗紫外性能3.4小结4环状聚醚/二苯甲酮衍生物侧基硅氧烷低聚体(DMUV-O)的合成、表征与应用4.1实验部分4.1.1原料及试剂4.1.2 DMUV-O的合成4.1.3 DMUV-O结构表征与物理性能4.1.4 DMUV-O的溶解4.1.5 DMUV-O的应用性能测试4.2结果与讨论4.2.1 DMUV-O的表征4.2.2 DMUV-O的应用性能研究4.3小结5紫外吸收基聚硅氧烷PE-PUVSi、DMUV-O的成膜性及膜形貌5.1实验部分5.1.1原材料与试剂5.1.2纤维基质表面PE-PUVSi、DMUV-O成膜性的SEM观察5.1.3单晶硅表面PE-PUVSi、DMUV-O微观膜形貌的AFM观察5.1.4 PE-PUVSi、DMUV-O膜表面的亲、疏水性能5.2结果与讨论5.2.1 PE-PUVSi的成膜形态、精细结构及其影响因素5.2.2 DMUV-O的成膜形态及其精细结构5.3小结6结论参考文献
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> TQ610.491 > 工业技术 > 化学工业 > 染料及中间体工业 > 一般性问题
& 2012 book.作者:&作者本人请参看导师姓名:&学位授予单位:&授予学位:博士学位年度:2007专业:&关键词:&&&&摘要:(摘要内容经过系统自动伪原创处理以避免复制,下载原文正常,内容请直接查看目录。)最近几年来,硅橡胶资料凭仗其优良的机能特色在口腔医学范畴运用日渐普遍,个中加成型硅橡胶更成为口腔印模资料中的研讨热门。该资料基本聚合物为乙烯基聚硅氧烷(Vinyl Polysiloxane;VPS),故简称VPS资料,其交联剂为含氢硅油,催化剂为铂盐或氯铂酸。资料混杂后,乙烯基聚硅氧烷的乙烯基与被催化剂活化的含氢硅油的硅氢键之间产生加成反响,反响快而完整,不伴任何副产品生成,是以,VPS资料固化时光较短,且固化后具有极佳的尺寸准确性和尺寸稳固性。同时,交联生成的网状高份子聚合物主链为高能硅氧键,性质稳固,且网格构造可以在受力时产生滑动、取向,故资料具有较好的机械机能。然则,无机硅工业中应用的VPS资料某些机能与口腔印模资料的请求相去甚远,不克不及直策应用。是以须要经由过程配方设计,取得合适临床运用的VPS口腔印模资料。最近几年来对其配方的研发和对其机能的改进在欧美蓬勃国度从未停滞,而我国国际却鲜见报导。本研讨即旨在研发机能优秀的中等稠度VPS口腔印模资料;并在资料中参加聚醚改性的无机硅化合物,使其具有必定的亲水性;另外,测验考试经由过程添加抗菌成份,使其具有必定的本身消毒功效,从而防止或下降化学浸泡消毒对其机能的不良影响。本研讨分为三部门。第一部门是VPS口腔印模资料的制备,即配方设计进程。起首参考VPS工业模具硅橡胶配方,肯定基本配方,由此动身,以拉伸强度、断裂延伸率、硬度和粘度为不雅察目标,慢慢肯定各重要成份的品种和用量,包含乙烯基聚硅氧烷封端乙烯基的含量、交联剂含氢硅油的用量,补强填料白碳黑的用量和乙烯基MQ硅树脂的用量。经由过程该部门试验研讨,明白了各重要成份与资料特定机能间的函变关系,终究肯定了资料的机能配方,制备了双组分的VPS口腔印模资料,暂定名为HC印模资料。本文第二部门较为具体地研讨了HC印模资料的操作机能、复模精度、机械机能和外面润湿性,并选择了3种国外同类产物作为对比研讨。成果显示:HC资料的折衷时光为21。0±1。6s;任务时光为100。0±4。2s;固化时光为308。2+6。2s;可以或许完全再现20μm线宽;取模24h后线性尺寸变更分离为0。17±0。06%;HC资料与3型及4型牙科天然石配伍性优越;弹性答复率99。1±0。4%;压应变2。9±0。2%;拉伸强度3。1±0。1MPa;扯破强度5。0±0。7/m;Shore一A硬度为56。8+0。7;进步接触角为90。2±1。3°。与国外同类产物比拟,除润湿性不及AFFINIS 75 MonoBody以外,其他机能均到达或跨越对比资料程度。本文第三部门向HC资料中添加分歧品种的无机抗菌剂,制备了三种抗菌VPS印模资料,个中添加Conval Pag40无机载银抗菌剂的Ag一HC资料具有较好的抗菌机能,且其稠度、精度、拉伸强度和硬度与HC资料无明显差异。经由过程本研讨,取得了VPS口腔印模资料的机能配方;对资料样品的机能测试成果显示,HC资料具有较好的操作机能、复模精度、机械机能和外面润湿性。向HC资料中添加恰当的无机抗菌剂可以在纰谬资料机能发生明显影响的条件下使资料取得抗菌功效,从而战胜了浸泡消毒进程对印模的不良影响。Abstract:In recent years, the silicone rubber material with its excellent performance characteristics in the field of oral medicine use is increasingly common, medium addition silicone rubber has become more popular dental impression materials research. The basic data of polymer vinyl polysiloxane (vinyl P the VPS), therefore, hereinafter referred to as VPS data, which is cross-linked silicone oil containing hydrogen, catalyst platinum salt acid. Data is mixed, vinyl polysiloxane vinyl and actived by catalyst containing hydrogen silicone silicon hydrogen bonds between the addition reaction, quick response and complete, without any by-products is the VPS curable materials in a relatively short time, and after curing with excellent size accuracy and dimensional stability. At the same time, the network formed by the cross-linking of high molecular polymer backbone of the high energy silicon oxygen bond, the properties are stable, and the grid structure can generate sliding, orientation, so the information has better mechanical properties. However, a far cry from the VPS data used in the inorganic silicon industry, some functions and oral impression material request, cannot be directly applied. Is to be through the process of formulation design, to obtain the appropriate clinical use of VPS dental impression materials. In recent years, the research and development of its formula and the improvement of its function in Europe and America have never stopped, while China's international is rarely reported. This study aims to R & D function good secondary thickening of VPS dental
and in the data in polyether modification of inorganic silicon compound, which has in addition, test through add anti-bacterial ingredients, which has certain itself disinfection efficacy, so as to prevent or decrease adverse effects of chemical immersion disinfection on its performance. This study is divided into three sectors. The first part is the preparation of VPS dental impression materials, namely the formula design process. Chapeau reference VPS industrial mold silicone rubber formulation, and certainly the basic formula, started from here, to tensile strength, breaking elongation, hardness and viscosity for indecent observes the target, slowly certainly the variety and dosage of the important ingredients, containing vinyl polysiloxane terminated vinyl content, crosslinking agent containing hydrogen silicone dosage, the amount of filler for white carbon black dosage and ethylene MQ silicone resin. Through the experimental research in the Department of, understand the the important component and data specific function between function relation, eventually affirmed the function formula of data, two groups of VPS dental impression materials were prepared, tentative name for HC impression materials. The second part of this article more detailed discussion of the HC impression materials operating performance of composite precision mold, mechanical function and outside wettability, three foreign congener product is selected as a comparative study. The results show that: the HC data of the compromise time is 21. 0 + 1. 6S; mission time is 100. 0 + 4. 2S; curing time is 308. 2+6. 2S; can completely reproduce the 20 after the model 24h, the linear dimension change is separated into 0. 17 + 0. 06%; HC data and the 3 type and 4 type of dental natural stone su elastic response rate of 99. 1 + 0. 4%; compressive strain 2. 9 + 0. 2%; tensile strength 3. 1 + 0. 1MPa; tear strength 5. 0 + 0. 7 / M; Shore a A hardness of 56. 8+0. 7; the contact angle is 90. 2 + 1. 3 degrees. Compared with foreign similar products, in addition to the wettability of less than MonoBody 75 AFFINIS, the other functions are to reach or cross the level of contrast. The third part to the HC data add different kinds of inorganic antibacterial agent prepared three antibacterial VPS data and medium added Conval inorganic Pag40 silver antibacterial agent Ag a HC data has good antibacterial function and its consistency, precision, tensile strength and hardness and HC data no significant difference. Through this research, has obtained the functional formula of VPS dental
the data sample performance test results show that HC has better operating performance, complex precision mold, mechanical function and outside wettability. HC data to add appropriate inorganic antibacterial agent can be when PI perverted material performance are significantly affected the information to get the antibacterial efficacy, so as to overcome the adverse effects of immersion disinfection process of impression.目录:缩略词表5-6中文摘要6-8英文摘要8-10前言11-14第一部分 自制VPS口腔印模材料配方设计14-31第二部分 自制VPS口腔印模材料性能测试31-71&&&&实验一 调和时间测试32-34&&&&实验二 稠度测试34-37&&&&实验三 工作时间和固化时间测试37-42&&&&实验四 细节再现测试42-45&&&&实验五 线性尺寸变化测试45-48&&&&实验六 与石膏配伍性测试48-52&&&&实验七 弹性回复测试52-55&&&&实验八 压应变测试55-57&&&&实验九 拉伸强度、撕裂强度及硬度测试57-61&&&&实验十 润湿性测试61-71第三部分 抗菌VPS口腔印模材料初探71-88&&&&实验一 抗菌VPS口腔印模材料的制备和表面形貌观察72-76&&&&实验二 添加抗菌成分对VPS口腔印模材料性能的影响76-82&&&&实验三 抗菌性能测试82-88全文总结88-89参考文献89-98综述98-113个人简历113-114致谢114原价:¥20.00元折价:¥5.00元分享到:相关文献| 上传我的文档
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聚醚型聚硅氧烷的研究进展及应用
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