【摘要】：搭建了超臨界流體萃噴裝置(Supercritical Fluid Extraction and Expansion, SFEE),該裝置耦合聯(lián)用了超臨界流體萃取技術(shù)(Supercritical Fluid Extraction, SFE)和超臨界流體快速膨脹技術(shù)(Rapid Expansion of Supercritical Solution, RESS)兩個(gè)成熟工藝,將二者功能組合在一起實(shí)現(xiàn)一機(jī)多樣是本課題的目的之一。本文利用SFEE裝置制備硬脂酸和烷基烯酮二聚物(Alkyl Ketene Dimer,AKD)產(chǎn)品。通過實(shí)驗(yàn)和相關(guān)數(shù)據(jù)分析,改進(jìn)裝置不足之處,硬件控制方面優(yōu)化了裝置噴嘴；軟件控制方面引進(jìn)蒙特卡羅方法(Monte Carlo Method, MCM)評(píng)估產(chǎn)品不確定度,并用MATLAB編程實(shí)現(xiàn)該方法的計(jì)算,最后將程序整合到SFEE裝置的自動(dòng)控制系統(tǒng)；優(yōu)化了SFEE裝置。制備硬脂酸產(chǎn)品中,預(yù)膨脹壓力從15MPa升至35MPa時(shí)：預(yù)膨脹溫度60℃,顆粒粒徑從1.4μm降至0.98gm；預(yù)膨脹溫度75℃,顆粒粒徑從1.71μm降至1.16gm；在75℃時(shí),所制備硬脂酸產(chǎn)品尖端出現(xiàn)彎曲,說明SFEE可以解決熱敏性物質(zhì)的制備問題。實(shí)驗(yàn)范圍內(nèi)制備硬脂酸產(chǎn)品的最優(yōu)條件為35MPa,60℃,高壓低溫有利于獲得粒徑更小的硬脂酸產(chǎn)品。制備AKD產(chǎn)品中,預(yù)膨脹壓力從15MPa升至30MPa時(shí)：預(yù)膨脹溫度40℃,顆粒粒徑從2.28μm降至1.50μm；預(yù)膨脹溫度60℃,顆粒粒徑從2.2gm降至1.19gm；經(jīng)過SFEE處理的紙張表面達(dá)到了超疏水性能；實(shí)驗(yàn)范圍內(nèi)制備AKD產(chǎn)品的最優(yōu)工藝條件為30MPa,60℃,說明高壓高溫有利于獲得粒徑更小的AKD產(chǎn)品。利用FLUENT軟件模擬分析,對(duì)SFEE裝置噴嘴做進(jìn)一步改進(jìn),優(yōu)化噴嘴的結(jié)構(gòu)參數(shù)和工藝參數(shù),得到所設(shè)計(jì)噴嘴的最優(yōu)條件組合為噴嘴入射角α=125。,動(dòng)環(huán)圓錐孔角β=80°,預(yù)膨脹壓力P=17MPa,預(yù)膨脹溫度T=373K,環(huán)隙寬度e=0.3mm。MCM不確定度評(píng)估以概率產(chǎn)生輸入量的樣本Xi,通過概率模型f傳播,估計(jì)輸出量Y的分布,通過輸出量的離散分布G獲得其估計(jì)值y,標(biāo)準(zhǔn)不確定度材(y),100p%包含區(qū)間的左端點(diǎn)ylow,和右端點(diǎn)yhigh。將上述原理用MATLAB編程實(shí)現(xiàn)計(jì)算,最后將程序整合到SFEE自動(dòng)控制系統(tǒng),完成實(shí)驗(yàn)后的數(shù)據(jù)自動(dòng)分析處理程序。
[Abstract]:A supercritical fluid extraction and spray device (Supercritical Fluid Extraction and Expansion, SFEE),) is built. The device is coupled with two mature processes: supercritical fluid extraction (Supercritical Fluid Extraction, SFE) and supercritical fluid rapid expansion (Rapid Expansion of Supercritical Solution, RESS). It is one of the purposes of this subject to combine the two functions together to realize the diversity of one machine. In this paper, stearic acid and alkyl ketene dimer (Alkyl Ketene Dimer,AKD were prepared by SFEE device. Through the experiment and the related data analysis, the deficiency of the device is improved, the device nozzle is optimized in the aspect of hardware control, the Monte Carlo method (Monte Carlo Method, MCM) is introduced in the software control to evaluate the uncertainty of the product, and the calculation of the method is realized by MATLAB programming. Finally, the program is integrated into the automatic control system of SFEE device, and the SFEE device is optimized. In the preparation of stearic acid products, the pre-expansion pressure increases from 15MPa to 35MPa: the pre-expansion temperature is 60 鈩，

本文編號(hào)：2277473