新型光致变色材料的研究

发布时间：2018-02-10 16:58

  本文关键词： 光致变色 螺吡喃 聚甲氧基含氢硅氧烷 色变探针 灵敏　出处：《东华大学》2017年硕士论文　论文类型：学位论文

【摘要】：螺吡喃作为一种光致变色材料,可以响应外界的各种刺激如光、温度、pH、应力等,因此在光信息存储与生物领域具有重大的研究意义。本文在实验室研究的基础上将一种光致变色性能良好的螺吡喃单元与聚甲基含氢硅氧烷进行反应,得到了一种新型的光致变色聚合物,并对其性质做了深入的研究,研究内容分为两部分:第一部分是合成两种带有双键的螺吡喃类光致变色材料,然后将这两种螺吡喃分子在六水氯铂酸的异丙醇溶液的催化下分别与聚甲基含氢硅氧烷进行硅氢化反应。以1-烯丙基-2,3,3-三甲基吲哚啉为原料分别与5-硝基水杨醛、5-氯水杨醛合成了两种螺吡喃化合物:1-烯丙基-6-硝基螺[2H-1-苯并吡喃-2,2’-吲哚啉]、1-烯丙基-6-氯螺[2H-1-苯并吡喃-2,2’-吲哚啉]。两种螺吡喃分子的产率分别为49%与57%。通过硅氢加成反应将螺吡喃分子连接到聚甲基硅氧烷链上,得到两种新型光致变色材料(SP1-Si,SP2-Si)。通过红外光谱对两种新型光致变色材料进行表征,发现两者聚合物在2100cm-1并没有属于Si?H的特征吸收峰,并且在1100cm-1附近有属于Si?O?Si的特征吸收峰,初步表明了螺吡喃分子已经与聚甲基含氢硅氧烷发生了硅氢加成反应;再利用凝胶渗透色谱(GPC)对两种光致变色材料做了分子量的测定。SP1-Si;Mw:21660,Mn:19410,PDI:1.116;SP2-Si;Mw:59094,Mn:41482,PDI:1.425。本实验主要采用了IR,GPC作为分析手段对合成的两种新型光致变色材料进行了结构的表征。第二部分主要对这两种新型光致变色材料进行性能对比研究。首先对SP1-Si、SP2-Si两种聚合物进行了热稳定性的测试,实验测得聚合物SP1-Si从190.3oC到309.1oC质量只损失了22.1%;而聚合物SP2-Si从245.3℃到552.4℃质量只损失78.72%,因此聚合物具有较好的耐热稳定性。接下来我们对在两种聚合物进行了光谱性质测试,发现SP1-Si在黑暗与紫外条件下为深黄色溶液,而在可见光下为浅黄色;而SP2-Si在黑暗条件下为深黄色,而在紫外与可见光条件下为浅黄色,呈现逆光致变色现象。并且发现聚合物SP1-Si、SP2-Si可以对p H、Ag~+与Fe~(3+)响应。聚合物SP1-Si在酸性条件下为浅黄色,随着pH的不断增大,溶液颜色变深,最后变为深黄色;而聚合物SP2-Si在酸性条件下为黄色,随着pH的增大,溶液逐渐变为浅黄色。两者聚合物在添加Ag~+后会变为橙黄色,并且随着络合时间的增大颜色逐渐加深,具有良好的抗干扰性,得到最低检测限分别1.06×10-5 M、1.45×10-6 M为:,对于添加Fe~(3+)后会迅速变为黄色,得到Fe~(3+)的最低检测限分别为1.25×10-5 M、3.52×10-6 M。
[Abstract]:As a photochromic material, spiropyran can respond to various external stimuli such as light, temperature, pH, stress, etc. Therefore, it is of great significance in the field of optical information storage and biology. On the basis of laboratory research, a spiropyran unit with good photochromic properties is reacted with poly (methyl hydrosiloxane). A new type of photochromic polymer was obtained, and its properties were studied in depth. The research content is divided into two parts: the first part is the synthesis of two kinds of spiropyran photochromic materials with double bonds. Then, the two spiropyran molecules were hydrogenated with polymethyl hydrosiloxane under the catalysis of isopropanol solution of chloroplatinic acid hexahydrate. Two kinds of spiropyrans: 1-allyl-6-nitrospiroid [2H-1-benzopyran-2azopyrane-2-indoline] 1-allyl -6-chloropyrano [2H-1-benzopyran-2azopyran-2-indoline] were synthesized. The yields of the two kinds of spiropyrans were 49% and 57.The yields of the two spiropyrans were 49% and 57.The yields of the two kinds of spiropyrans were 49% and 57.The yields of the two kinds of spiropyrans were 49% and 57.The yields of the two kinds of spiropyrans were 49% and 57, respectively. The addition reaction connects the spiropyran molecule to the polymethylsiloxane chain. Two kinds of new photochromic materials were obtained. The two new photochromic materials were characterized by infrared spectroscopy. It was found that the two polymers did not belong to Si at 2100cm ~ (-1). The characteristic absorption peak of H is found near 1100cm ~ (-1). O? The characteristic absorption peak of Si indicates that the spiropyran molecule has already reacted with polymethyl-hydrosiloxane. The molecular weight of two photochromic materials was determined by gel permeation chromatography (GPC). SP1-SiMw: 21660: Mn19410 / PDI: 1.116: SP2-SiMw: 59094 / Mw: 41482 / PDI / 1.425.The structure of the two new photochromic materials was characterized by IRGPC. The second part is the structure of the two new photochromic materials. The second part is the characterization of the structure of the two new photochromic materials. The second part is the characterization of the structure of the two new photochromic materials. The second part is the structure of the two new photochromic materials. The second part is the characterization of the structure of the two new photochromic materials. The properties of the two new photochromic materials were compared and studied. Firstly, the thermal stability of SP1-Si-Si SP2-Si polymers was tested. The experimental results show that the mass loss of polymer SP1-Si from 190.3 OC to 309.1 OC is only 22.1%, while the mass loss of polymer SP2-Si from 245.3 鈩，

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