本文關(guān)鍵詞： 光致變色 螺吡喃 聚甲氧基含氫硅氧烷 色變探針 靈敏　出處：《東華大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：螺吡喃作為一種光致變色材料,可以響應(yīng)外界的各種刺激如光、溫度、pH、應(yīng)力等,因此在光信息存儲(chǔ)與生物領(lǐng)域具有重大的研究意義。本文在實(shí)驗(yàn)室研究的基礎(chǔ)上將一種光致變色性能良好的螺吡喃單元與聚甲基含氫硅氧烷進(jìn)行反應(yīng),得到了一種新型的光致變色聚合物,并對(duì)其性質(zhì)做了深入的研究,研究內(nèi)容分為兩部分:第一部分是合成兩種帶有雙鍵的螺吡喃類光致變色材料,然后將這兩種螺吡喃分子在六水氯鉑酸的異丙醇溶液的催化下分別與聚甲基含氫硅氧烷進(jìn)行硅氫化反應(yīng)。以1-烯丙基-2,3,3-三甲基吲哚啉為原料分別與5-硝基水楊醛、5-氯水楊醛合成了兩種螺吡喃化合物: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]。兩種螺吡喃分子的產(chǎn)率分別為49%與57%。通過硅氫加成反應(yīng)將螺吡喃分子連接到聚甲基硅氧烷鏈上,得到兩種新型光致變色材料(SP1-Si,SP2-Si)。通過紅外光譜對(duì)兩種新型光致變色材料進(jìn)行表征,發(fā)現(xiàn)兩者聚合物在2100cm-1并沒有屬于Si?H的特征吸收峰,并且在1100cm-1附近有屬于Si?O?Si的特征吸收峰,初步表明了螺吡喃分子已經(jīng)與聚甲基含氫硅氧烷發(fā)生了硅氫加成反應(yīng);再利用凝膠滲透色譜(GPC)對(duì)兩種光致變色材料做了分子量的測定。SP1-Si;Mw:21660,Mn:19410,PDI:1.116;SP2-Si;Mw:59094,Mn:41482,PDI:1.425。本實(shí)驗(yàn)主要采用了IR,GPC作為分析手段對(duì)合成的兩種新型光致變色材料進(jìn)行了結(jié)構(gòu)的表征。第二部分主要對(duì)這兩種新型光致變色材料進(jìn)行性能對(duì)比研究。首先對(duì)SP1-Si、SP2-Si兩種聚合物進(jìn)行了熱穩(wěn)定性的測試,實(shí)驗(yàn)測得聚合物SP1-Si從190.3oC到309.1oC質(zhì)量只損失了22.1%;而聚合物SP2-Si從245.3℃到552.4℃質(zhì)量只損失78.72%,因此聚合物具有較好的耐熱穩(wěn)定性。接下來我們對(duì)在兩種聚合物進(jìn)行了光譜性質(zhì)測試,發(fā)現(xiàn)SP1-Si在黑暗與紫外條件下為深黃色溶液,而在可見光下為淺黃色;而SP2-Si在黑暗條件下為深黃色,而在紫外與可見光條件下為淺黃色,呈現(xiàn)逆光致變色現(xiàn)象。并且發(fā)現(xiàn)聚合物SP1-Si、SP2-Si可以對(duì)p H、Ag~+與Fe~(3+)響應(yīng)。聚合物SP1-Si在酸性條件下為淺黃色,隨著pH的不斷增大,溶液顏色變深,最后變?yōu)樯铧S色;而聚合物SP2-Si在酸性條件下為黃色,隨著pH的增大,溶液逐漸變?yōu)闇\黃色。兩者聚合物在添加Ag~+后會(huì)變?yōu)槌赛S色,并且隨著絡(luò)合時(shí)間的增大顏色逐漸加深,具有良好的抗干擾性,得到最低檢測限分別1.06×10-5 M、1.45×10-6 M為:,對(duì)于添加Fe~(3+)后會(huì)迅速變?yōu)辄S色,得到Fe~(3+)的最低檢測限分別為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，

本文編號(hào)：1500998