本文選題：超細(xì)顆粒 + 超臨界CO_2輔助霧化法��； 參考：《華東理工大學(xué)》2011年碩士論文

【摘要】：近年來,采用超臨界流體技術(shù)制備功能性超細(xì)顆粒一直是研究的熱點,該類技術(shù)擁有操作條件溫和、操作條件可控與顆粒制備的形貌和大小可控的優(yōu)點。其中一種較為先進(jìn)的方法-超臨界輔助霧化法(全稱Supercritical assisted atomization,簡稱SAA)是此類方法中的最有潛力的。它是主要從超臨界抗溶劑法中衍生出來的一種新工藝方法。一方面,它克服了傳統(tǒng)顆粒制備工藝中制備得到的顆粒粒徑大,并且粒徑分布不集中的缺點；另一方面,它彌補(bǔ)了超臨界流體快速膨脹法和超臨界抗溶劑法在材料選擇中的不足,既可以用于脂溶性產(chǎn)品顆粒的制備,也可以用于水溶性產(chǎn)品顆粒的制備。 本論文討論了SAA方法的工藝基礎(chǔ)和工藝發(fā)展過程,并主要對SAA法制備功能性材料殼聚糖-香精超細(xì)顆粒的過程進(jìn)行了研究。本論文從兩種體系(分別為固液互相包埋和固固互相包埋的體系)出發(fā),以殼聚糖為載體,采取互相包埋的形式制備以香蘭素固體、薰衣草液體香精為香精主料的超細(xì)顆粒。討論了引起顆粒粒徑改變、粒徑分布變化以及顆粒粘連程度的各種操作因素,包括沉降室溫度,物料配比,預(yù)膨脹溫度,預(yù)膨脹壓力和溶液流量等。采用掃描電鏡對制備得到的顆粒進(jìn)行形貌觀察,同時以掃描電鏡照片為基礎(chǔ)進(jìn)行粒徑大小和分布統(tǒng)計,采用氣相色譜考察其緩釋效果。 本論文最后結(jié)果表明：保持一定范圍內(nèi)的沉降室溫度,升高預(yù)膨脹壓力和溶液流量,降低殼聚糖/香精的物料配比和預(yù)膨脹溫度都有利于制備顆粒粒徑較小的顆粒。操作條件對兩種體系的顆粒粒徑分布和顆粒間粘連程度的影響則不同：對殼聚糖/薰衣草顆粒來說,降低殼聚糖/薰衣草的物料配比和預(yù)膨脹溫度有利于得到粒徑分布集中,粘連程度小的顆粒；但升高預(yù)膨脹壓力和溶液流量,顆粒粒徑的分布則會先變集中變分散,粒徑分布相對集中的顆粒同時顆粒粘連程度也低。對殼聚糖/香蘭素顆粒來說,降低殼聚糖/香精的物料配比和預(yù)膨脹溫度,升高預(yù)膨脹壓力和溶液流量有利于制備得到顆粒粒徑分布窄的顆粒。但過低的物料配比和過高的溶液流量溶液得到相互粘連的顆粒。 最終得到的產(chǎn)物顆粒基本為球形,對殼聚糖/薰衣草顆粒來說,在物料配比0.8/1、預(yù)膨脹溫度50℃,預(yù)膨脹壓力10.5Mpa,溶液流量1.5mL/min條件下,顆粒的平均粒徑在2.2μm左右。對殼聚糖/香蘭素顆粒來說,物料配比0.8/0.8,預(yù)膨脹溫度50℃,預(yù)膨脹壓力10.5Mpa,溶液流量1.5mL/min條件下,殼聚糖/香蘭素顆粒的平均粒徑在2.0μm左右。顆粒存在一定的內(nèi)部結(jié)構(gòu),為香精緩釋提供了結(jié)構(gòu)基礎(chǔ)。通過氣相色譜考察得知：殼聚糖/薰衣草香精顆粒的香氣保持時間較長,能在5個月以上；而殼聚糖/香蘭素顆粒的香氣保持時間則只在4個月內(nèi)。
[Abstract]:In recent years, the preparation of functional ultrafine particles by supercritical fluid technology has been a hot topic. This kind of technology has the advantages of mild operating conditions, controllable operating conditions and controllable morphology and size of particles. One of the more advanced methods, Supercritical assisted atomization (SAA), is the most promising one. It is a new process derived mainly from supercritical anti-solvent method. On the one hand, it overcomes the shortcoming that the particle size is large and the particle size distribution is not concentrated in the traditional particle preparation process; on the other hand, It can be used in the preparation of liposoluble product particles as well as in the preparation of water-soluble product particles because of the deficiency of supercritical fluid rapid expansion method and supercritical anti-solvent method in material selection. In this paper, the technological basis and development process of SAA method are discussed, and the process of preparing functional material chitosan-essence ultrafine particles by SAA method is mainly studied. In this paper, starting from two systems (solid liquid and solid mutually entrapped), superfine particles with vanillin solid and lavender liquid flavor as main ingredient were prepared by using chitosan as carrier. Various operating factors, such as settling chamber temperature, material ratio, preexpansion temperature, preexpansion pressure and solution flow rate, are discussed which cause particle size change, particle size distribution change and particle adhesion degree. The morphology of the prepared particles was observed by scanning electron microscope (SEM), and the particle size and distribution were analyzed based on SEM photos. The sustained release effect was investigated by gas chromatography. The results show that maintaining the temperature of the settling chamber, increasing the pre-expansion pressure and the flow rate of solution, reducing the ratio of chitosan to flavor and the pre-expansion temperature are all beneficial to the preparation of the smaller particle size. The effect of operation conditions on particle size distribution and particle adhesion was different. For chitosan / lavender particles, reducing the ratio of chitosan / lavender and pre-expansion temperature was beneficial to the concentration of particle size distribution. The particles with small adhesion degree, but with the increase of preexpansion pressure and solution flow rate, the particle size distribution will first change into concentration and dispersion, and the particle size distribution with relatively concentrated particle size distribution at the same time the degree of particle adhesion is also low. For chitosan / vanillin granules, reducing the ratio of chitosan to essence and preexpansion temperature, increasing preexpansion pressure and solution flow rate are beneficial to the preparation of narrow particle size distribution. However, too low material ratio and too high solution flow rate to obtain mutually adhesive particles. For chitosan / lavender particles, the average particle size was about 2.2 渭 m under the conditions of 0.8 / 1 material ratio, 50 鈩，

本文編號：1833381