螺吡喃羥丙基纖維素的合成及其性能研究
發(fā)布時(shí)間：2018-08-27 13:02
【摘要】：自然界中產(chǎn)量最豐富的可再生資源天然高分子纖維素,取之不盡,用之不竭。由于其具有價(jià)格低廉、儲(chǔ)存穩(wěn)定、生物降解性及生物相容性好、無(wú)毒和無(wú)免疫原性等很多優(yōu)點(diǎn),纖維素這一綠色資源得到了人們的廣泛關(guān)注。本文將具有光響應(yīng)性的螺吡喃化合物通過(guò)酯化反應(yīng)接枝到羥丙基纖維素上,制備了螺吡喃功能化的羥丙基纖維素SP-HPC,并對(duì)接枝聚合物的結(jié)構(gòu)及性能進(jìn)行了表征和測(cè)試,主要研究?jī)?nèi)容如下：1.以四氫呋喃(THF)為溶劑,N,N'-二環(huán)己基碳二亞胺/4-二甲氨基吡啶DCC/DMAP)為催化體系,通過(guò)1’-(3-羧乙基)-3',3'-二甲基-6-硝基螺[吲哚啉-2,2[2H]吲哚啉苯并吡喃](SPCOOH)和羥丙基纖維素(HPC)的酯化反應(yīng)合成了螺吡喃功能化羥丙基纖維素SP-HPC�？疾炝瞬煌耐读媳葘�(duì)取代度的影響。采用1H-NMR、FT-IR、TGA等方法對(duì)聚合物進(jìn)行了表征；通過(guò)UV-Vis測(cè)試SP-HPC的四氫呋喃(THF)溶液的光致變色性能。結(jié)果表明,SP-HPC的THF溶液呈現(xiàn)可逆的快速光響應(yīng)性。交替的紫外光輻射和黑暗條件的存放,使得SP-HPC溶液呈現(xiàn)無(wú)色和紫色兩種狀態(tài)的可逆轉(zhuǎn)變。2.采用選擇性水溶劑透析方法制備了膠束溶液。通過(guò)動(dòng)態(tài)光散射、透射電鏡和掃描電鏡表征了自組裝所形成的膠束的尺寸和形態(tài)。結(jié)果表明,SP-HPC在水中組裝成了球形膠束,紫外光照射后,膠束內(nèi)部疏水閉環(huán)形式的SP能夠異構(gòu)化為開(kāi)環(huán)部花菁形式(MC),產(chǎn)生更緊密地堆疊作用,促使球形膠束收縮,粒徑分布變窄,顯示了光響應(yīng)性。隨著聚合物膠束水溶液濃度的增加和聚合物中螺吡喃取代度的增加,膠束的粒徑也相應(yīng)隨之增大。3.利用旋涂方法制備了SP-HPC固體膜。通過(guò)UV-Vis測(cè)試了SP-HPC固體膜的光致變色性能,采用接觸角測(cè)量?jī)x考察了聚合物固體膜表面潤(rùn)濕性的變化。結(jié)果表明,SP-HPC固體膜具有良好的光刺激響應(yīng)性,紫外光照射后再置于黑暗條件下,SP-HPC固體膜中開(kāi)環(huán)的MC轉(zhuǎn)變?yōu)镾P的光響應(yīng)性較慢,其表面接觸角隨著螺吡喃基團(tuán)開(kāi)環(huán)與閉環(huán)構(gòu)型的改變而發(fā)生改變；SP-HPC固體膜表面接觸角隨著聚合物取代度的增加而變小,紫外光照前后接觸角變化幅度隨螺吡喃取代度的增加而變小。
[Abstract]:Natural polymer cellulose, the most abundant renewable resource in nature, is inexhaustible. Because of its advantages of low cost, stable storage, good biodegradability and biocompatibility, nontoxic and non-immunogenicity, cellulose as a green resource has been paid more and more attention. In this paper, the spiropyran compounds with photoresponse were grafted onto hydroxypropyl cellulose by esterification reaction. The SP-HPC, functionalized hydroxypropyl cellulose was prepared, and the structure and properties of the grafted polymers were characterized and tested. The main research contents are as follows: 1. In this paper, tetrahydrofuran (THF) was used as the solvent for the catalytic system. The catalytic system consisted of N _ (N) N _ (-) -dicyclohexyl carbodiimide / 4-dimethylaminopyridine (DCC/DMAP). The functional hydroxyl propyl cellulose SP-HPC. was synthesized by the esterification of 1 (3-carboxyethyl) -3oxy 3- dimethyl-6-nitrospiroid [indoline -2azopyran] (SPCOOH) and hydroxypropyl cellulose (HPC) (HPC) by the esterification reaction of 1- (3-carboxyethyl) -3- (3-) -trimethylidene 3-nitropiro [indoline -2azopyran] (SPCOOH) and hydroxypropyl cellulose (HPC) The influence of different feed ratio on the degree of substitution was investigated. The polymer was characterized by 1H-NMR-FT-IRGA, and the photochromic property of SP-HPC tetrahydrofuran (THF) solution was tested by UV-Vis. The results show that the THF solution of SP-HPC exhibits a reversible fast photoresponse. The alternating ultraviolet radiation and the storage of dark conditions make the SP-HPC solution appear the reversible transition of colorless and purple state. 2. Micelle solution was prepared by selective water solvent dialysis. The size and morphology of the self-assembled micelles were characterized by dynamic light scattering, transmission electron microscopy and scanning electron microscopy. The results showed that SP-HPC was assembled into spherical micelles in water. After UV irradiation, SP in the hydrophobic closed loop form of the micelles could be isomerized into (MC), in the form of open ring cyanine, resulting in the contraction of the spherical micelles and the narrowing of the particle size distribution. The optical response is shown. With the increase of the concentration of polymer micelle aqueous solution and the degree of substitution of spiropyran in polymer, the particle size of micelle increases accordingly. SP-HPC solid film was prepared by spin coating method. The photochromic properties of SP-HPC solid films were measured by UV-Vis and the changes of surface wettability of polymer solid films were investigated by contact angle measuring instrument. The results showed that the SP-HPC solid film had a good photo-stimulative response, and the photoresponse of the open-loop MC in the SP-HPC solid film changed to that of SP slowly after UV irradiation. The surface contact angle of SP-HPC film decreases with the increase of the degree of substitution of the polymer, and the surface contact angle changes with the change of the open-loop and closed-loop configuration of the spiropyran group, and the surface contact angle of the SP-HPC solid film decreases with the increase of the degree of substitution of the polymer. The range of contact angle before and after UV irradiation decreases with the increase of the degree of substitution of spiropyran.
【學(xué)位授予單位】：廣西大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類(lèi)號(hào)】：O636.1
本文編號(hào)：2207374
[Abstract]:Natural polymer cellulose, the most abundant renewable resource in nature, is inexhaustible. Because of its advantages of low cost, stable storage, good biodegradability and biocompatibility, nontoxic and non-immunogenicity, cellulose as a green resource has been paid more and more attention. In this paper, the spiropyran compounds with photoresponse were grafted onto hydroxypropyl cellulose by esterification reaction. The SP-HPC, functionalized hydroxypropyl cellulose was prepared, and the structure and properties of the grafted polymers were characterized and tested. The main research contents are as follows: 1. In this paper, tetrahydrofuran (THF) was used as the solvent for the catalytic system. The catalytic system consisted of N _ (N) N _ (-) -dicyclohexyl carbodiimide / 4-dimethylaminopyridine (DCC/DMAP). The functional hydroxyl propyl cellulose SP-HPC. was synthesized by the esterification of 1 (3-carboxyethyl) -3oxy 3- dimethyl-6-nitrospiroid [indoline -2azopyran] (SPCOOH) and hydroxypropyl cellulose (HPC) (HPC) by the esterification reaction of 1- (3-carboxyethyl) -3- (3-) -trimethylidene 3-nitropiro [indoline -2azopyran] (SPCOOH) and hydroxypropyl cellulose (HPC) The influence of different feed ratio on the degree of substitution was investigated. The polymer was characterized by 1H-NMR-FT-IRGA, and the photochromic property of SP-HPC tetrahydrofuran (THF) solution was tested by UV-Vis. The results show that the THF solution of SP-HPC exhibits a reversible fast photoresponse. The alternating ultraviolet radiation and the storage of dark conditions make the SP-HPC solution appear the reversible transition of colorless and purple state. 2. Micelle solution was prepared by selective water solvent dialysis. The size and morphology of the self-assembled micelles were characterized by dynamic light scattering, transmission electron microscopy and scanning electron microscopy. The results showed that SP-HPC was assembled into spherical micelles in water. After UV irradiation, SP in the hydrophobic closed loop form of the micelles could be isomerized into (MC), in the form of open ring cyanine, resulting in the contraction of the spherical micelles and the narrowing of the particle size distribution. The optical response is shown. With the increase of the concentration of polymer micelle aqueous solution and the degree of substitution of spiropyran in polymer, the particle size of micelle increases accordingly. SP-HPC solid film was prepared by spin coating method. The photochromic properties of SP-HPC solid films were measured by UV-Vis and the changes of surface wettability of polymer solid films were investigated by contact angle measuring instrument. The results showed that the SP-HPC solid film had a good photo-stimulative response, and the photoresponse of the open-loop MC in the SP-HPC solid film changed to that of SP slowly after UV irradiation. The surface contact angle of SP-HPC film decreases with the increase of the degree of substitution of the polymer, and the surface contact angle changes with the change of the open-loop and closed-loop configuration of the spiropyran group, and the surface contact angle of the SP-HPC solid film decreases with the increase of the degree of substitution of the polymer. The range of contact angle before and after UV irradiation decreases with the increase of the degree of substitution of spiropyran.
【學(xué)位授予單位】：廣西大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類(lèi)號(hào)】：O636.1
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