Research progress of hydrophobically modified Halloysite nanotube-based composite materials
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摘要: 埃洛石是一種卷曲的層狀硅鋁酸鹽黏土，其儲量豐富、價格低廉。埃洛石的內外表面分別由Al?OH八面體和Si?O四面體組成，它們在水中以相反的方式電離，導致埃洛石管腔內帶正電荷，外表面帶負電荷，因此可分別利用內外表面成分與電荷性質的不同對其進行疏水改性，用于藥物的裝載和緩釋。同時，埃洛石具有納米管狀結構，可用來構造微?納米分級結構，協同低表面能物質的修飾，增強界面疏水性能，用于高效自清潔和油水分離。本文在介紹埃洛石的疏水結構設計理論的基礎上，綜述了埃洛石納米管（HNTs）的表面進行疏水改性所得到的復合材料在油水分離、疏水自清潔涂料以及藥物的裝載和釋放方面的應用。Abstract: With the development of material design theories and synthesis technologies, clay-based composite materials have been controllably prepared and successfully applied in many fields, such as biomedicine, the automotive industry, petrochemical engineering, and wastewater treatment. To date, for the preparation of clay-based composite materials, the physical and chemical properties of clay must be fully considered, including the chemical composition, crystal structure, particle size, morphology, and surface charge. Halloysite, which has a tubular crystal structure, is a curly layered aluminosilicate clay with abundant reserves and a low price for constructing composite materials. The inner and outer surfaces of halloysite nanotubes are composed of Al?OH octahedrons and Si?O tetrahedrons, respectively, which ionize in opposite ways in water, resulting in opposite charges on the inner and outer surfaces. Therefore, the selective modification of halloysite can be achieved by chemical or electrostatic adsorption of the required chemical reagent. Additionally, the modified halloysite nanotubes can be used in catalysis and the loading and release of drug molecules. Moreover, because of its nanotube structure, the halloysite can be used to construct rough structures in micro- or nano-scale. By incorporation with low-surface-energy materials, the hydrophobic halloysite-based composite materials can be prepared for self-cleaning and oil-water separation. In this review, we introduced the rational design and preparation strategies of the hydrophobic halloysite-based composite materials. Then, we summarized the applications of these prepared composite materials in oil-water separation, hydrophobic self-cleaning coating, and the loading and sustained release of drug molecules. In addition, the related mechanisms and strategies for performance improvement were systematically discussed. Finally, the existing challenges and promising future directions in this research field were proposed. The halloysite-based composite materials have enhanced properties that are highly required, including enhanced mechanical and adhesive strength, excellent scratch and wear resistance, self-healing, and higher compatibility with living organisms. We believe fruitful promising results can be achieved in this field with more effort.
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Key words:
- halloysite /
- hydrophobic /
- coating /
- oil-water separation /
- nanometer carrier
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圖 1 HNTs形態圖（a）（內表面為Al?OH層（綠色），外表面為Si?O層（紅色））；HNTs的晶體結構示意圖（b）；HNTs內表面的選擇性修飾（c）；HNTs（紫色）、二氧化硅（藍色）和氧化鋁（紅色）納米顆粒的ζ電位比較（d）；陰離子和陽離子選擇性吸附在HNTs的內/外表面（e）；硅氧烷包覆黏土材料的透射電鏡圖（f）[23, 25, 31-32]
Figure 1. Morphology (a) of halloysite nanotubes: alumina forms on the inside surface (green) and silica on the outside surface (red); schematic illustration (b) of the crystalline structure of halloysite; selective modification of HNTs (c); comparison of ζ-potential curves for halloysite nanotubes (violet), silica (blue), and alumina (red) nanoparticles (d); scheme of selective anionic and cationic amphiphile molecules adsorbed inside and outside of the halloysite nanotubes, respectively (e); TEM image (f) of PAL@fluoroPOS composites[23, 25, 31-32]
圖 2 HNTs@POS涂層的合成示意圖（a）；涂層的水接觸角（b）和滾動角（c）；亞甲基藍染色的水在不同基體涂層上以及不同液體在涂層上的實物圖（d）[10]
Figure 2. Schematic illustration (a) of the synthesis of the HNTs@POS; water contact angle (b) and slide angle (c) images of the hydrophobic HNTs@POS coatings; photographs (d) of water (dyed with methylene blue) on the hydrophobic HNTs coating sprayed on different substrates and photographs of 1 mol·L?1 HCl, 1 mol·L?1 NaOH, tea, water, and milk droplets on the hydrophobic HNTs coating[10]
圖 3 PP/HNTs球晶結構形成的假想機理示意圖（a）；PP與PP/HNTs復合材料表面的水接觸角和滾動角（b）；PP及其復合材料在空氣中的熱重曲線（c）；PP和PP/HNTs復合材料的掃描電鏡照片：（d, e）純PP；（f, g）85% PP，15% HNTs；（h,i）60%PP，40% HNTs[77]
Figure 3. Schematic (a) of the hypothetical formation mechanism of PP/HNTs hybrid spherulite superstructure; water contact angles and sliding angles (b) of the PP and PP/HNTs composite surfaces; TGA curves (c) of PP and PP/HNTs composites in air; SEM images of PP and PP/HNTs composites: (d, e) pure PP; (f, g) 85% PP, 15% HNTs; (h, i) 60%PP, 40% HNTs[77]
圖 5 制備和改性海綿的工藝示意圖（a）；海綿形貌的掃描電鏡圖像（b）；油水分離實驗裝置（c）；海綿的孔隙度和密度（d）；復合海綿改性前后的水接觸角（e）；改性的復合海綿對有機試劑的最大吸油能力（每克改性復合海綿吸收有機試劑質量）（f）；改性的復合海綿對葵花籽油的循環吸收能力（g）[86]
Figure 5. Schematic illustration (a) of the preparation process of modified sponges; SEM images (b) of the morphologies of sponges; oil-water separation experiment (c); the porosity and density of sponges (d); water contact angles (e) of composite sponges before and after modification; the maximum oil absorption ratios of organic solvent (f); cycle absorption capacity of sunflower seed oil (g)[86]
圖 6 二氯甲烷（油紅染色）/水（亞甲基藍染色）混合物（a）；油水混合物的分離過程（b～c）[10]；合成超疏水高聚物基狀結構的示意圖（d）；水接觸角和滾動角圖像（e）；涂層網格對不同油水混合物分離效率（f）[87]
Figure 6. Dichloromethane (dyed with oil red)/water (dyed with methylene blue) mixture (a); the separation processes (b?c) of the oil/water mixture using the coated mesh[10]; schematic illustration (d) of the fabrication of the superhydrophobic halloysite-based mesh; the water contact angle and slide angle on the mesh (e); efficiency of different oil-water mixture separations with the coated mesh (f)[87]
圖 7 超濾膜的制備工藝（a）；膜的橫截面掃描電鏡圖像（b）；不同膜的孔隙率和平均孔隙半徑（c）；超濾膜的分離效率：（d）柴油/水；（e）石油醚/水；（f）正十六烷/水；（g）植物油/水[21]
Figure 7. Preparation process (a) of APTES-HNT/PVDF; cross-sectional SEM images (b) of membranes; porosities and mean pore radii of various membranes (c); oil rejections of membranes M0 and M2-3: (d) diesel oil/water (D/W); (e) petroleum ether/water (P/W); (f) n-hexadecane/water (H/W); (g) vegetable oil/water (V/W)[21]
圖 9 HNTs的選擇性修飾和雙功能化示意圖（a）；二茂鐵從HNTs和ODP修飾的HNTs中的釋放曲線（b）和Higuchi時間平方根曲線（c）；烷基三甲基溴化銨/ HNTs雜化材料的水接觸角（d）；烷基三甲基溴化銨/HNTs雜化材料（e）；硫酸銅和氯仿雙相體系攪拌10 h后照片（f）[95]
Figure 9. Schematic illustration (a) of selective modification and bifunctionalization of halloysite nanotubes; release profile (b) and Higuchi square root of time plots for release (c) of ferrocene from halloysite and halloysite-ODP; water contact angle on alkyl trimethylammonium bromide/ HNTs hybrid materials (d); illustration of the alkyl trimethylammonium bromide/HNTs hybrid materials (e); photo (f) of the biphasic system composed of a saturated aqueous phase (top) of copper sulfate and chloroform C16Br/HNTs dispersion (bottom) after 10 h of stirring[95]
圖 10 布洛芬裝載、修改和藥物釋放過程示意圖（a）；HNTs（b）、EHNTs@OS-4（c）和EHNTs@OS-1（d）的接觸角；不同組成的EHNTs@OS中布洛芬的釋放情況（e）[96]
Figure 10. Schematic representation (a) of IBU loading, modification, and drug-release process; wettability of the nanotubes (b), EHNTs@OS-4 (c), and EHNTs@OS-1 (d); release profiles (e) of IBU from the EHNTs@OS with different compositions[96]
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