明膠與羧甲基纖維素鈉的復合凝聚作用及其微膠囊制備
本文選題:復合凝聚 + 羧甲基纖維素鈉; 參考:《江南大學》2017年碩士論文
【摘要】:復合凝聚微膠囊具有載量高、可控制釋放等優(yōu)點。目前復合凝聚微膠囊多以明膠和阿拉伯膠為壁材,其中阿拉伯膠價格昂貴且性質不穩(wěn)定,羧甲基纖維素鈉(CMC)來源廣且價格低廉,有望替代阿拉伯膠從而降低復合凝聚微膠囊的成本。然而,由于CMC、明膠的類型及性質參數(shù)眾多,明確適合于復合凝聚微膠囊包埋的CMC與明膠的關鍵屬性,對于拓展復合凝聚微膠囊壁材的選擇范圍具有重要意義。本論文研究了CMC粘度及明膠凝凍強度對復合凝聚物形成與性質的影響,探討了優(yōu)選所得的明膠/CMC復合凝聚行為,在此基礎上,優(yōu)化并確定了復合凝聚法制備肉桂醛微膠囊的工藝參數(shù)。以體系濁度、復聚物產率、顯微形態(tài)及粒徑分布差異為指標,研究CMC粘度及明膠凝凍強度對復聚物形成與界面性質的影響。結果表明,不同粘度CMC及不同凝凍強度明膠的復合凝聚體系,均在明膠/CMC之比為9:1(w/w)、復凝聚pH為4.50時具有較高的復聚物產率;诿髂z(200,Bloom g)/CMC(FL9)的復合凝聚體系具有較高的乳化活性和較低的界面張力,可形成大小均一的球形多核微膠囊,產率及效率可達87.56%、91.03%。通過改變總濃度、明膠/CMC混合之比和混合順序確立了明膠/CMC/水/三元體系的相邊界,繪制明膠/CMC復合凝聚體系的相圖,研究了明膠與CMC之間的復合凝聚行為。結果發(fā)現(xiàn),pH對明膠/CMC體系的相分離行為有重要影響,相比于pH 4.50時的三相圖,pH 3.50時的相分離區(qū)域要更大,表明相分離需要在更高的電荷濃度下才能發(fā)生。借助濁度滴定曲線,確定了明膠/CMC混合質量比為1:5,1:3,1:1,3:1,5:1,9:1的體系開始形成不可溶性復聚物所對應的臨界pH值(pHφ1)分別為2.97,3.10,3.76,4.23,4.71,4.80。通過軟粒子理論、傅里葉紅外光譜、圓二色譜技術對明膠/CMC復聚物的形成過程進行分析。結果表明,在不同明膠/CMC之比對應的pHφ1值下,不可溶性復聚物形成過程中明膠與CMC所帶電荷的絕對值相等;明膠與CMC之間無化學鍵生成;明膠、CMC復凝聚過程中明膠分子由無規(guī)卷曲狀態(tài)轉變?yōu)橛行虻腜PII螺旋。采用明膠/CMC復凝聚體系對肉桂醛進行微膠囊化。通過比較不同pH、壁材濃度、乳化條件、攪拌速率下肉桂醛微膠囊的顯微形態(tài)、粒徑分布、包埋效果,確定了最佳制備條件:pH 4.50,壁材質量濃度為1.0%,明膠/CMC質量之比為9:1,乳化條件(10000r/min、2 min),攪拌速率400 r/min,微膠囊產率及效率可達88.92%、92.13%。對芯材濃度分別為1.0%、2.0%肉桂醛微膠囊的熱穩(wěn)定性、高鹽離子穩(wěn)定性進行研究,發(fā)現(xiàn)芯材濃度1.0%時制備的微膠囊的熱穩(wěn)定性及高鹽離子穩(wěn)定性更佳。將芯材濃度1.0%肉桂醛微膠囊應用于卷煙中,結果表明肉桂醛微膠囊化后進入主流煙氣的轉移率有所提高,并且在烘絲過程中的損失率降低。
[Abstract]:Composite condensed microcapsules have the advantages of high loading and controllable release. At present, gelatin and Arabic gum are used as wall materials in compound condensed microcapsules, among which Arabic gum is expensive and unstable, and sodium carboxymethyl cellulose (CMC) comes from a wide range of sources and the price is low. It is expected to replace Arabic gum so as to reduce the cost of composite condensed microcapsules. However, due to the large number of types and properties of CMC gelatin, it is of great significance to define the key properties of CMC and gelatin which are suitable for the encapsulation of composite condensed microcapsules, which is of great significance to expand the selection range of wall materials for composite condensed microcapsules. In this paper, the effects of CMC viscosity and gelatin freezing strength on the formation and properties of composite condensate were studied. The process parameters for the preparation of cinnamaldehyde microcapsules by complex coagulation method were optimized and determined. The effects of CMC viscosity and gelatin freezing strength on the formation and interfacial properties of the polymer were studied based on the differences of turbidity, yield, morphology and particle size distribution of the system. The results show that when the ratio of gelatin / CMC is 9:1 (w / w) and the pH of complex coagulation is 4.50, the composite condensing system with different viscosity CMC and different freezing strength has a higher yield. The composite condensate system based on Gelatin (200m Bloom g) / CMC (FL9) has higher emulsifying activity and lower interfacial tension, and can form uniform spherical polynuclear microcapsules. The yield and efficiency can reach 87.56% and 91.03%. The phase boundary of gelatin / CMC / water / ternary system was established by changing the total concentration, the mixing ratio and the mixing sequence of gelatin / CMC. The phase diagram of gelatin / CMC composite condensate system was drawn, and the composite condensation behavior between gelatin and CMC was studied. The results show that pH has an important effect on the phase separation behavior of gelatin / CMC system, and the phase separation region is larger than that at pH 4.50, which indicates that the phase separation takes place at a higher charge concentration. With the help of turbidimetric titration curve, the critical pH value (pH 蠁 1) corresponding to the formation of insoluble polymer was determined to be 2.97% 3.103.103.64.234.71.80 for the gelatin / CMC mixed mass ratio of 1: 5: 1, 1: 1, 1: 1, 1: 1. The formation process of gelatin / CMC complex was analyzed by soft particle theory, Fourier transform infrared spectroscopy and circular dichroism. The results show that the absolute value of the charge between gelatin and CMC is equal during the formation of insoluble polymer under the condition of pH 蠁 1 corresponding to the ratio of gelatin / CMC, and there is no chemical bond formation between gelatin and CMC. The gelatin molecules changed from random coiling state to an ordered PPII helix during the complex condensation of gelatin and CMC. The gelatin / CMC complex condensation system was used to microencapsulate cinnamaldehyde. The micromorphology, particle size distribution and embedding effect of cinnamaldehyde microcapsules under different pH, wall material concentration, emulsification conditions and stirring rate were compared. The optimum preparation conditions were determined as follows: ph = 4.50, mass concentration of wall material 1.0, mass ratio of gelatin / CMC 9: 1, emulsification condition (10000r / min ~ 2 min), stirring rate 400rmin), yield and efficiency of microcapsule up to 88.92% ~ 92.13%. The thermal stability and high salt ion stability of cinnamaldehyde microcapsules with 1.0% core concentration were studied. It was found that the thermal stability and high salt ion stability of the microcapsules were better when the core material concentration was 1.0%. The application of 1.0% cinnamaldehyde microcapsule in cigarette showed that the transfer rate of cinnamaldehyde into mainstream smoke increased and the loss rate decreased during the drying process.
【學位授予單位】:江南大學
【學位級別】:碩士
【學位授予年份】:2017
【分類號】:TS426;TB332
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