合成改質含胺基奈米纖維素與二氧化矽混合膠體應用吸附CO2之評估研究

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段氏金娟(Doan Thi Kim Quyen) 查詢紙本館藏

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論文名稱

合成改質含胺基奈米纖維素與二氧化矽混合膠體應用吸附CO2之評估研究
(Facile synthesis of amine-modified cellulose nanocrystal/silica hybrid aerogel for CO2 adsorption)

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至系統瀏覽論文 (2028-7-15以後開放)

摘要(中)

本研究透過合成改質含胺基奈米纖維素與二氧化矽混合膠體，並進一步評估吸附CO2的可行性。該材料製備過程首先對棉布廢棄物(cotton cloth waste, CCW)進行鹼處理和脫色處理，再使用鹽酸進行酸水解處理後得到微晶纖維素(microcrystalline cellulose, MCC)，接下來使用硫酸水解和反應曲面法(response surface methodology, RSM)將微晶纖維素轉換為奈米纖維素(cellulose nanocrystal, CNC)。反應曲面法主要透過Box-Behnken design (BBD)設計三個獨立變數，分別為硫酸濃度(58¬64%)、水解溫度(50-70℃)和水解時間(40¬80分鐘)，然後使用溶膠凝膠法(sol-gel method)在常溫條件下進行乾燥，將奈米纖維素與二氧化矽合成為混合膠體(CNC/silica hybrid aerogel, CSA)，接著浸入聚乙烯亞胺(Polyethyleneimine, PEI)提高CO2吸附效果，最後探討溫度(30¬120℃)和PEI濃度等參數對CO2吸附的影響。
根據二次迴歸模型的判定係數顯示，對產物產率、結晶度指數(crystallinity index, CI)和平均粒徑的預測具有非常高的可靠性，顯示獨立變數和產物改變有顯著的相關性，而本研究發現當硫酸濃度為61.27 wt.%、水解溫度及水解時間分別在50℃及56分鐘時，具有提取CNC的最佳酸水解條件，此時CNC的產率、CI及平均粒徑分布則分別為44.57%、86.29%和160 nm，同時符合膠體製備的要求，具有成為CO2吸附劑的潛力。

在CO2吸附的試驗結果顯示，最佳的吸附劑 (CSA¬PE150) 在70℃和50 wt％的PEI濃度條件下具有最佳的CO2吸附能力，達到2.35 mmol g-1，透過多種吸附動力學模型解釋CSA-PEI50的吸附機制發現，Avrami動力學模型對CSA-PEI在不同溫度和PEI濃度下的CO2吸附行為最相符，反應階數介於0.352¬0.613之間，均方根誤差則可忽略不計。透過速率控制動力學(rate-limiting kinetic)分析結果顯示，膜擴散(film diffusion)和粒子間擴散阻力(intraparticle diffusion resistance)會影響吸附速率隨後控制吸附的過程，最後針對CNC進行十次的吸附¬脫附試驗中，發現CSA-PEI50具有非常高的穩定性，本研究證明CSA-PEI50具有成為捕捉燃燒後CO2吸附劑的潛力。

摘要(英)

The aim of the work is to synthesize and evaluate performance of amine-modified cellulose nanocrystal/ silica hybrid aerogel for CO2 adsorption. Firstly, cotton cloth waste (CCW) was subjected to alkali and decoloring treatments, and subsequent hydrochloric acid hydrolysis to obtain microcrystalline cellulose (MCC). The resulted MCC was furthered converted into cellulose nanocrystal (CNC) using sulfuric acid hydrolysis and response surface methodology (RSM). The RSM based on the Box-Behnken design (BBD) was designed with three independent variables: including sulfuric acid concentration (58-64 wt%), hydrolysis temperature (50-70 oC), and hydrolysis time (40-80 min). Then CNC/silica hybrid aerogel (CSA) was synthesized by hybridization of CNC and sodium silicate hybridization based on the one-step sol-gel method under atmospheric drying. Polyethyleneimine (PEI) was impregnated on CSA to improve CO2 adsorption performance. The parameters governing CO2 adsorption performance on CSA-PEI, such as temperatures (30-120 oC) and PEI concentrations (40-60 wt%), were investigated systematically.
According to the analyzed regression models, the predicted quadratic polynomial models for yield, crystallinity index (CI), and average particle size exhibited high reliability, corresponding to the close interaction between independent variables and responses. The study found the optimum acid hydrolysis conditions for CNC extraction were 61.27 wt%, 50 oC, and 56 min. At the optimal points, the results of experimental CNC yield, CI, and particle size distribution were 44.57%, 86.29%, and 160 nm respectively. The obtained CNC properties met the required specifications for aerogel preparation as an adsorbent for CO2 adsorption process.
For the CO2 adsorption performance, the optimum adsorbent (CSA-PEI50) exhibited an excellent CO2 adsorption capacity of 2.35 mmol g-1 at 70 oC and a PEI concentration of 50 wt%. The adsorption mechanism of CSA-PEI50 was elucidated by analyzing many adsorption kinetic models. The CO2 adsorption behaviors of CSA-PEI at various temperatures and PEI concentrations had the goodness of fit with the Avrami kinetic model, which can correspond to the multiple adsorption mechanism. The Avrami model also showed fractional reaction orders in a range of 0.352-0.613, and the root mean square error was negligible. Moreover, the rate-limiting kinetic analysis showed that film diffusion and intraparticle diffusion resistances controlled the CO2 adsorption process. The CSA-PEI50 also exhibited excellent stability after ten adsorption-desorption cycles. This work proved that CSA-PEI was a potential adsorbent in post-combustion CO2 capture.

關鍵字(中)

★ 奈米纖維素
★ 二氧化矽
★ 混合膠體
★ CO2吸附
★ 胺改質
★ 吸附動力學

關鍵字(英)

★ Cellulose nanocrystal
★ silica
★ hybrid aerogel
★ CO2 adsorption
★ amine modification
★ adsorption kinetic

論文目次

Table of Contents

摘要 i
Abstract iii
Acknowledgements v
List of Tables x
List of Figures xii
Explanation of acronyms xvii
Chapter 1 Introduction 1
Chapter 2 Literature Review 7
2-1 Cellulose nanocrystal (CNC) 7
2-1-1 Cellulose structure and CNC 7
2-1-2 Properties of CNC 10
2-2 Preparation of CNC 13
2-2-1 Feedstocks for CNC preparation 13
2-2-2 Extraction of cellulose from lignocellulosic sources 17
2-2-3 CNC preparation using sulfuric acid hydrolysis 20
2-2-4 Response surface methodology in optimization of CNC extraction 39
2-3 Application of CNC 46
2-4 Synthesis of CNC-Silica (CNC-Si) hybrid aerogel 47
2-4-1 Cellulose-based hybrid aerogel 47
2-4-2 Fabrication approach of CNC-Si hybrid aerogel 50
2-4-2-1 Gelation process 51
2-4-2-2 Drying method 52
2-4-2-3 Amino group-surface functionalization 55
2-5 Properties of amino-functionalized CNC-Si hybrid aerogel 59
2-5-1 Density and porosity 59
2-5-2 Morphological structure 61
2-5-3 Textural structure 62
2-5-4 Other properties 63
2-6 Important parameters controlling CO2 adsorption capacity of amino-functionalized CNC-Si hybrid aerogel 64
2-6-1 Effect of textural properties 64
2-6-2 Effect of temperature 65
2-6-3 Effect of humidity 67
2-6-4 Effect of amine contents and amine types 68
2-6-5 Other adsorption conditions 70
2-7 Theoretical study of CO2 adsorption kinetic 70
Chapter 3 Materials and Methods 76
3-1 Materials 76
3-2 Cellulose nanocrystal (CNC) preparation process 76
3-2-1 Extraction process of microcrystalline cellulose (MCC) 76
3-2-2 Preparation process of CNC 77
3-3 Optimization process of CNC extraction 78
3-4 Preparation of PEI-modified CNC/ silica aerogel (CSA) material 81
3-4-1 CSA preparation procedure 81
3-4-2 PEI-modified CSA preparation 82
3-5 Characterization methods 82
3-5-1 Proximate and ultimate analysis of CCW 82
3-5-2 Chlorine content 84
3-5-3 Functional group analysis 84
3-5-5 Zeta potential 85
3-5-6 Morphological examination 85
3-5-7 Elemental composition 85
3-5-8 Dynamic rheological properties 85
3-5-9 Pore structure analysis 86
3-5-10 Crystalline structure analysis 86
3-6 Yield and sulfate group density calculation 87
3-7 CO2 adsorption process 87
3-7-1 CO2 adsorption measurement 87
3-7-2 CO2 adsorption kinetic 88
Chapter 4 Results and Discussion 91
4-1 Characterization of MCC extracted from CCW 91
4-1-1 Proximate and ultimate analysis of CCW 91
4-1-2 MCC yield and elemental compositions 92
4-1-3 Morphological structure 93
4-1-4 Functional group analysis 94
4-1-5 Crystalline structure 95
4-2 CNC characterization from the Box-Behnken design 96
4-2-1 CNC yield 96
4-2-4 Chemical structures 99
4-2-5 Crystallinity analysis 100
4-2-6 Thermostability properties 103
4-3 Regression model analysis of CNC extraction process 105
4-3-1 Yield model development 105
4-3-2 CI model development 109
4-3-3 Average particle size model development 111
4-4 Analysis of interaction effects 114
4-4-1 Interaction effects on CNC yield 114
4-4-3 Interaction effects on average particle size 117
4-5 Optimization analysis 118
4-6 Characteristics of CNC/si gel, CSA-x and CSA-PEI-y samples 121
4-6-1 Rheological property of CNC/Si gel 121
4-6-2 Morphological structure of CSA and CSA-PEI50 samples 122
4-6-3 Thermostability analysis 125
4-6-4 Pore structure analysis 126
4-7 CO2 adsorption performance 129
4-7-1 Effect of CNC to silica ratio 129
4-7-2 Effect of adsorption temperatures and PEI contents 130
4-8 CO2 adsorption kinetic 133
4-8-1 Apparent kinetic analysis 133
4-8-2 Diffusional mass transfer analysis 137
4-9 CO2 adsorption-desorption cycles 141
Chapter 5 Conclusions and Recommendations 144
5-1 Conclusions 144
5-2 Recommendations 146
References 147
Appendix xiii
Publication list xxxv

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指導教授

江康鈺(Chiang Kung Yuh)

審核日期

2023-7-18

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