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Effects of plant source selection and chemi-mechanical treatment on the fiber microstructures and mechanical behaviors of nanocellulose films 植物来源选择和化学机械处理对纳米纤维素薄膜的纤维微结构和机械性能的影响
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-09 DOI: 10.1007/s00226-024-01613-7
Yangyang Qian, Chunyu Wang, Yijun Liu, Bingfei Shi, Jianqiang Zhang, Yuan Wei, Gang Chen

Cellulose nanofibers (CNFs) were isolated and prepared from six different plant sources (Nordic pine, poplar, cotton, flax, bamboo, and pineapple leaf fibers) through a carboxymethylation-homogenization treatment. The surface morphologies, size distributions, and chemical structures of the CNFs and their microfibers were investigated in detail. Atomic force microscopy (AFM) analysis showed that all kinds of CNFs had uniform diameters of less than 10 nm. However, the length and aspect ratio of CNFs exhibited significant differences due to the differences of anatomical characteristics from pulp species. Among these six nanofibers, the pineapple leaf-based nanofibers had the highest length of ca. 2.21 μm and aspect ratio of ca. 1263. Meanwhile, the resulting pineapple leaf-based nanocellulose film possessed the strongest tensile strength (229.0 ± 9.8 MPa) and toughness (33.9 ± 2.9 MJ/m3). Interestingly, the aspect ratio of cotton nanofibers was only 556, lower than that of bamboo, Nordic pine, and flax nanofibers, but the tensile strength (210.6 ± 4.8 MPa) and toughness (22.4 ± 0.6 MJ/m3) of cotton-based nanocellulose film were second only to the pineapple leaf-based nanocellulose film. The critical reason is that the cotton-based nanocellulose exhibited the highest crystallinity index (76.6%), superior to the other source-based nanocellulose. These results suggested that the high aspect ratio or high crystallinity are responsible for the excellent mechanical strengths of the nanocellulose film. This work sheds light on the preparation and selection of highly spindly or crystalline nonwood nanofibrils, suggesting that the pineapple leaf or cotton nanofibers have great potential as strength additives for nanocomposites.

通过羧甲基化-均质化处理,从六种不同的植物(北欧松、杨树、棉花、亚麻、竹子和菠萝叶纤维)中分离制备了纤维素纳米纤维(CNFs)。详细研究了 CNFs 及其微纤维的表面形态、尺寸分布和化学结构。原子力显微镜(AFM)分析表明,各种 CNFs 的直径均小于 10 纳米。然而,由于不同纸浆品种的解剖特征不同,CNFs 的长度和长宽比表现出显著差异。在这六种纳米纤维中,菠萝叶基纳米纤维的长度最大,约为 2.21 μm,长宽比约为 1263。同时,菠萝叶基纳米纤维素薄膜具有最强的拉伸强度(229.0 ± 9.8 MPa)和韧性(33.9 ± 2.9 MJ/m3)。有趣的是,棉纳米纤维的长宽比仅为 556,低于竹纳米纤维、北欧松纳米纤维和亚麻纳米纤维,但棉基纳米纤维素薄膜的拉伸强度(210.6 ± 4.8 MPa)和韧性(22.4 ± 0.6 MJ/m3)仅次于菠萝叶基纳米纤维素薄膜。关键原因是棉基纳米纤维素的结晶度指数最高(76.6%),优于其他来源的纳米纤维素。这些结果表明,高纵横比或高结晶度是纳米纤维素薄膜具有优异机械强度的原因。这项研究揭示了如何制备和选择高刺或高结晶非木材纳米纤维,表明菠萝叶或棉纳米纤维作为纳米复合材料的强度添加剂具有巨大潜力。
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引用次数: 0
UV light-induced photodegradation of condensed tannins: obtaining bayberry tannins with different mean polymerization degrees 紫外线诱导缩合单宁的光降解:获得不同平均聚合度的杨梅单宁
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-07 DOI: 10.1007/s00226-024-01603-9
Ying Zhou, Yan Zhang, Yuting Zhang, Wenjing Hu, Shuguang Han

Condensed tannins (CTs) characterized by a low degree of polymerization (DP) are recognized to have substantial value for applications across diverse industrial sectors, including food production, pharmaceuticals, and wood adhesive manufacturing. To acquire CTs with a low DP, the depolymerization of bayberry tannins (BTs) through a novel approach utilizing UV light-driven photocatalytic degradation, facilitated by the ultrasonic dispersion of TiO2 nanoparticles was investigated. Under the optimal degradation conditions (a tannin concentration of 6%, a TiO2 nanoparticles loading amount of 0.20%, and a degradation time of 4 h), the study delineated a discernible linear relationship correlating both the degradation time with the formaldehyde reactivity of the photocatalytic degradation products, and the formaldehyde reactivity with the mean degree of polymerization (mDP) of these photocatalytic degradation products. With the establishment of these correlative relationships, it is feasible to systematically control the degradation process of BTs. The photocatalytic degradation process adhered to the following mechanism: The degradation process of BTs is initiated by the cleavage of the C4-C8 bond which, at the incipient stage of degradation, results in the elimination of one gallocatechin gallate unit and one gallocatechin unit, or alternatively, the removal of a gallocatechin dimer. During the advanced stages of degradation, the opening of the C ring gives rise to different derivatives. Upon establishing optimal degradation parameters, it was observed that the primary constituents of the photocatalytic degradation products were dimers. The utilization of photocatalytic degradation exhibited an ability to break down condensed tannins in a manner that is both controllable and in an environmentally friendly way.

以低聚合度(DP)为特征的缩合单宁(CTs)被认为在食品生产、制药和木材粘合剂制造等多个工业领域具有重要的应用价值。为了获得低聚合度的月桂单宁,研究人员采用了一种新方法,即利用紫外线驱动光催化降解,并在 TiO2 纳米粒子超声波分散的促进下,对月桂单宁(BTs)进行解聚。在最佳降解条件下(单宁酸浓度为 6%,TiO2 纳米粒子的负载量为 0.20%,降解时间为 4 小时),研究发现降解时间与光催化降解产物的甲醛反应性以及甲醛反应性与这些光催化降解产物的平均聚合度(mDP)之间存在明显的线性关系。建立了这些相关关系,就可以系统地控制 BTs 的降解过程。光催化降解过程遵循以下机理:BTs 的降解过程由 C4-C8 键的裂解开始,在降解的初级阶段,一个没食子儿茶素没食子酸酯单元和一个没食子儿茶素单元被清除,或者一个没食子儿茶素二聚体被清除。在降解的高级阶段,C 环的打开会产生不同的衍生物。在确定最佳降解参数后,发现光催化降解产物的主要成分是二聚体。利用光催化降解技术能够以可控和环保的方式分解缩合单宁酸。
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引用次数: 0
Tangential veneer fabrication of Fenton-like catalyst for the removal of organic dye from wastewater 用于去除废水中有机染料的类芬顿催化剂切向单板制备技术
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-07 DOI: 10.1007/s00226-024-01608-4
Jiani Zhou, Gonggang Liu, Xuebing Yi, Yuanyuan Liao, Chongqing Wang, Shanshan Chang, Jinbo Hu

The exploitation of low-cost, non-fossil membrane materials with flourishing pore structure is essential to complete an organic dye wastewater treatment in Fenton-like catalytic technology. The accessible and scalable veneer functionalized Fenton-like catalysis has been manufactured to decolorize the effluents by a hydrogen peroxide-Mn-based oxides system. The nanocatalyst of Mn-based oxides has been loaded on the veneer surface by the hydrothermal in-situ growth, which could accomplish the coupling of Fenton-like catalyst and membrane technology. Fir and poplar veneers with unique three-dimensional porous structure have been investigated in detail to manifest the respective performance of decolorization during the dye wastewater treatment. This work not only has invented a promising membrane material coupling with Fenton-like catalysis to dispose dye wastewater, but also provides a reference in high-performance membrane design of biomimetic membrane.

要利用 Fenton 类催化技术完成有机染料废水处理,就必须利用具有良好孔隙结构的低成本非化石膜材料。利用过氧化氢-锰基氧化物系统,制造出了易于获得且可扩展的单板功能化 Fenton-like 催化技术,用于对废水进行脱色处理。锰基氧化物的纳米催化剂通过水热原位生长被负载在单板表面,从而实现了芬顿类催化剂与膜技术的耦合。研究人员对具有独特三维多孔结构的杉木和杨木单板进行了详细研究,以显示它们在染料废水处理过程中各自的脱色性能。这项工作不仅为处理染料废水发明了一种前景广阔的与 Fenton-like 催化技术相结合的膜材料,而且为高性能仿生物膜的设计提供了参考。
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引用次数: 0
Tuning the antioxidant and antibacterial properties of lignin by physicochemical modification during sequential acid precipitation from Kraft black liquor 在从牛皮纸黑液中进行连续酸沉淀的过程中,通过物理化学改性调整木质素的抗氧化和抗菌特性
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-07 DOI: 10.1007/s00226-024-01612-8
María E. Eugenio, Luisa García-Fuentevilla, Raquel Martín-Sampedro, José I. Santos, Bernd Wicklein, David ibarra

Turning lignin from black liquor waste into value-added bioactive agents is one of the possible routes for improving the sustainability and profitability of lignocellulosic industry. However, due to chemical and structural variability of lignin, it is necessary to isolate specific lignin fractions from black liquor with the purpose to achieve samples with unique chemical and structural characteristics and therefore, specific biological activities. In this study, poplar lignin fractions isolated from Kraft black liquor by sequential acid precipitation at pH´s 7.5, 5 and 2.5 (denoted as P-7.5, P-5 and P-2.5) were characterized according to their physicochemical, antioxidant and antibacterial properties. In general, lignin fractions displayed a wide elimination of lateral chains (aryl-β ether and C–C) and, therefore a high phenolic content and low molecular weight, as the pH sequential precipitation was decreased from 7.5 to 2.5. Moreover, thermal analysis revealed that the P-7.5 lignin fraction showed higher thermal stability than P-2.5 and P-5. In terms of antioxidant activity, the P-7.5 lignin fraction, with a higher S/G ratio and a less oxidized structure compared to P-5 and P-2.5, exhibited higher antioxidant activity. In addition, lower antibacterial effect was observed for all lignin fractions against Escherichia coli compared to that obtained against Staphylococcus aureus. Among them, the P-2.5 and P-5 fractions, with higher phenolic content and lower molecular weight values than P-7.5, showed a greater antibacterial effect against S. aureus.

将黑液废料中的木质素转化为高附加值的生物活性剂,是提高木质纤维素工业可持续性和盈利能力的可行途径之一。然而,由于木质素在化学和结构上的可变性,有必要从黑液中分离出特定的木质素馏分,以获得具有独特化学和结构特征的样品,从而获得特定的生物活性。在本研究中,通过在 pH 值为 7.5、5 和 2.5 的条件下进行连续酸沉淀,从牛皮纸黑液中分离出了杨木素馏分(分别称为 P-7.5、P-5 和 P-2.5),并根据其物理化学、抗氧化和抗菌特性对其进行了表征。一般来说,当 pH 值从 7.5 降到 2.5 时,木质素馏分的横向链(芳基-β 醚和 C-C)被广泛消除,因此酚含量高、分子量低。此外,热分析表明,P-7.5 木质素馏分的热稳定性高于 P-2.5 和 P-5。在抗氧化活性方面,与 P-5 和 P-2.5 相比,P-7.5 木质素馏分的 S/G 比率更高,氧化结构更少,因此具有更高的抗氧化活性。此外,所有木质素馏分对大肠杆菌的抗菌效果均低于对金黄色葡萄球菌的抗菌效果。其中,P-2.5 和 P-5 与 P-7.5 相比,酚含量更高,分子量值更低,对金黄色葡萄球菌的抗菌效果更好。
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引用次数: 0
A novel cross-flow Ag/wood composite filter for high-concentration organic dye wastewater treatment 用于高浓度有机染料废水处理的新型横流 Ag/wood 复合过滤器
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-06 DOI: 10.1007/s00226-024-01605-7
Gensheng Wu, Tong Su, Pingan Li, Yunfeng Gu, Weiyu Chen, Bo Yu

Dye wastewater produced from industry production is difficult to degrade naturally. Natural wood possesses a hierarchical and three-dimensional (3D) interconnected microstructure, making it a desirable material for water treatment. However, limited water transport pathways can reduce the efficiency of removing high-concentration organic dyes. To address this, we present a low-cost, scalable, and efficient cross-flow Ag/wood composite filter by combing the structural design and hydrothermal treatment using a silver-ammonia solution. Silver ions (Ag+) are effectively reduced to silver nanoparticles (Ag NPs) by wood lignin and then anchored by hydroxyl groups in the cellulose and hemicellulose of the wood. Importantly, the incorporation of Ag NPs does not compromise the 3D porous structure of the wood. Diagonal grooves and exposed channels on both sides of the filter guide pollutants, ensuring extensive interaction with Ag NPs along elongated reaction pathways and through microstructural vessel disturbances. An 8 mm-thick cross-flow Ag/wood composite filter, featuring grooves with a diameter of 15 mm and a depth of 4 mm, achieves a remarkable 99% degradation efficiency of methylene blue (MB) at a water flux of up to 1775 L/(m2∙h). The performance in water flux and decolorization efficiency hinges significantly on groove diameter, groove depth, and filter thickness. This cross-flow Ag/wood composite filter represents a promising advancement for rapid and effective removal of various organic pollutants in a single-step process, showcasing extensive potential for applications in water treatment. This work aims to enhance clarity and readability while maintaining the technical details and impact of the research.

工业生产中产生的染料废水很难自然降解。天然木材具有分层和三维(3D)互连的微观结构,是一种理想的水处理材料。然而,有限的水传输途径会降低去除高浓度有机染料的效率。为了解决这个问题,我们结合结构设计和银氨溶液的水热处理,提出了一种低成本、可扩展的高效横流 Ag/wood 复合过滤器。银离子(Ag+)被木材木质素有效还原成银纳米粒子(Ag NPs),然后被木材纤维素和半纤维素中的羟基锚定。重要的是,银纳米粒子的加入不会破坏木材的三维多孔结构。过滤器两侧的对角线凹槽和外露通道可以引导污染物,确保污染物沿着细长的反应路径并通过微结构容器的扰动与银氧化物发生广泛的相互作用。8 毫米厚的横流式银/木复合过滤器具有直径 15 毫米、深度 4 毫米的凹槽,在水流量高达 1775 升/(m2∙h)的条件下,亚甲基蓝(MB)的降解效率达到了 99%。水通量和脱色效率的性能很大程度上取决于沟槽直径、沟槽深度和过滤器厚度。这种横流 Ag/wood 复合过滤器在一步法快速、有效去除各种有机污染物方面取得了重大进展,在水处理领域具有广泛的应用潜力。这项工作旨在提高清晰度和可读性,同时保留研究的技术细节和影响。
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引用次数: 0
Impregnation of wood with water using ultrasonic irradiation and water containing bulk nanobubbles 利用超声波辐照和含有大量纳米气泡的水对木材进行水浸渍
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-02 DOI: 10.1007/s00226-024-01611-9
Toru Tuziuti, Kyuichi Yasui, Wataru Kanematsu

This paper investigates the impregnation of Japanese cedar (Cryptomeria japonica D. Don) with water using ultrasound irradiation, followed by immersion in water containing bulk nanobubbles (NBs). Cavitation bubbles generated during ultrasound irradiation mechanically remove extractives from the wood surface, enhancing the mass transfer of water into the wood. Water containing bulk NBs has a lower surface tension compared to pure water, enabling superior permeability into narrow spaces. However, the application of water containing NBs for wood impregnation post-sonication remains underexplored. In this study, wood was subjected to ultrasound irradiation at 38 kHz, followed by immersion in water containing bulk NBs, to determine the optimal sonication time and NB concentration for efficient impregnation. The results indicate that water uptake by the wood initially increases and then decreases with increasing NB concentration and sonication time. Optimal sonication time and NB concentration resulted in highly efficient impregnation.

本文研究了利用超声波辐照对日本杉木(Cryptomeria japonica D. Don)进行水浸渍,然后将其浸入含有大量纳米气泡(NBs)的水中。超声波辐照时产生的空化气泡可以机械地去除木材表面的萃取物,促进水向木材的传质。与纯水相比,含有大量 NBs 的水表面张力较低,因此在狭窄空间中具有极佳的渗透性。然而,含 NBs 的水在木材浸渍后超声波处理中的应用仍未得到充分探索。在这项研究中,对木材进行了 38 千赫的超声波辐照,然后将其浸入含有大量 NBs 的水中,以确定有效浸渍的最佳超声时间和 NB 浓度。结果表明,木材的吸水率最初会随着 NB 浓度和超声时间的增加而增加,然后减少。最佳超声时间和 NB 浓度可实现高效浸渍。
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引用次数: 0
Acetylation of reed (Arundo donax) to prevent the contact dermatitis of woodwind musicians 对芦苇(Arundo donax)进行乙酰化处理,防止木管乐器演奏家患上接触性皮炎
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-01 DOI: 10.1007/s00226-024-01604-8
Yoshikazu Arai, Eiichi Obataya, Akiko Nakagawa-Izumi, Naoko Okiyama

A reed (Arundo donax) was acetylated to prevent serious cheilitis (reed allergy) in woodwind musicians in contact with the vibrating plate made of the reed. The reed was acetylated almost completely at 120 °C for 8 to 24 h. The maximum weight% gain (WPG) of the reed was lower than that of wood, reflecting a lower number of active reaction sites. The WPG of the inner part of the reed was slightly higher than that of the outer part, probably because the reactivity of the parenchyma cells is higher than that of the bundle sheaths. The acetylated reeds were tested by eleven skilled musicians suffering from the reed allergy. Eight musicians reported no allergic reactions. Three musicians reacted with the acetylated reed, but the reactions were much weaker than those induced by the unmodified reed. Thus, acetylation has been proven effective in preventing reed allergy. The patch test was not sufficient to detect allergies because although some musicians tested negative in the patch test, their mouths reacted seriously.

对芦苇(Arundo donax)进行乙酰化处理,以防止木管乐器演奏者在接触芦苇制成的振动板时发生严重的腮腺炎(芦苇过敏症)。在 120 °C、8 至 24 小时的条件下,芦苇几乎完全被乙酰化。芦苇的最大增重率(WPG)低于木材,这反映了活性反应位点的数量较少。芦苇内部的 WPG 略高于外部,这可能是因为实质细胞的反应活性高于束鞘。11 名患有哨片过敏症的熟练音乐家对乙酰化哨片进行了测试。八位音乐家表示没有过敏反应。三位音乐家对乙酰化哨片产生了反应,但反应程度远低于未改良哨片。因此,乙酰化被证明可以有效预防哨片过敏。贴片测试并不足以检测出过敏现象,因为尽管有些乐手的贴片测试结果为阴 性,但他们的口腔却出现了严重的反应。
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引用次数: 0
Multifunctional MnO2 nanorods-modified wood sponge for water remediation: applications for heavy metal sorption and oil/water separation 用于水修复的多功能 MnO2 纳米棒改性木质海绵:在重金属吸附和油/水分离方面的应用
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-10-03 DOI: 10.1007/s00226-024-01602-w
Siavosh Vojdani Saghir, Elaheh K. Goharshadi

This study presents the development of a wood sponge (WS) modified with MnO2 nanorods (MnO2/WS) derived from balsa natural wood, an abundant and environmentally friendly raw material, for the adsorption of organic solvents, oils, and heavy metal ions from water. The MnO2/WS composite exhibits an exceptionally low density of 0.014 g cm− 3 and a high porosity of approximately 97%. It demonstrates consistent sorption-desorption performance over 20 cycles. Zeta potential analysis reveals that MnO2 nanorods carry a negative charge (-22.31 mV) at pH 4.68, indicating their affinity for adsorbing positively charged heavy metal ions, which are commonly found in industrial effluents. Moreover, WS shows remarkable mechanical robustness, enduring 1000 stress-strain cycles with high shape recovery, ensuring its durability under operational conditions. The data highlight several strengths of MnO2/WS, including cost-effective production process, high reusability, remarkable sorption capacities for carbon tetrachloride and soybean oil (29.56 and 17.65 times its mass, respectively), and efficient performance. Its capability to produce potable water from real industrial effluents positions MnO2/WS as an ideal solution for addressing water crises.

本研究介绍了一种用二氧化锰纳米棒(MnO2/WS)改性的木质海绵(WS)的开发情况,这种木质海绵取自巴尔萨天然木材(一种丰富的环保型原材料),用于吸附水中的有机溶剂、油类和重金属离子。MnO2/WS 复合材料的密度极低,仅为 0.014 g cm-3,孔隙率高达约 97%。在 20 个循环中,它的吸附-解吸性能始终如一。Zeta 电位分析表明,MnO2 纳米棒在 pH 值为 4.68 时带负电荷(-22.31 mV),这表明它们对吸附工业废水中常见的带正电荷的重金属离子具有亲和力。此外,WS 还表现出卓越的机械坚固性,可承受 1000 次应力应变循环,形状恢复能力强,确保了其在操作条件下的耐用性。数据凸显了二氧化锰/WS 的几大优势,包括生产工艺成本低、可重复使用性高、对四氯化碳和豆油的吸附能力强(分别为其质量的 29.56 倍和 17.65 倍)以及性能高效。二氧化锰/WS 能够利用真正的工业废水生产饮用水,是解决水危机的理想解决方案。
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引用次数: 0
Effects of high-intensity microwave (HIMW) treatment on mechanical properties and bending failure mechanisms of radiata pine (Pinus radiata D. Don) 高强度微波(HIMW)处理对辐射松(Pinus radiata D. Don)机械性能和弯曲破坏机理的影响
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-09-27 DOI: 10.1007/s00226-024-01601-x
Xuefeng Xing, Shanming Li, Juwan Jin, Zhenyu Wang, Feng Fu

This study investigated the effects of high-intensity microwave (HIMW) treatment on the mechanical properties of radiata pine wood. The treatment, conducted on sapwood and heartwood with 60% initial moisture content, involved varied microwave energy densities: 60, 80, and 100 kWh/m3. Tests evaluated tensile and compressive properties in three directions, alongside shear strength and bending properties. Acoustic emission (AE) and digital image correlation (DIC) techniques probed damage evolution under bending loads before and after HIMW treatment. As microwave energy density increased, compressive, tensile, and shear strength decreased, with heartwood being the most susceptible. Substantial reductions occurred in longitudinal compressive properties and tensile properties perpendicular to the grain. After HIMW treatment (80 kWh/m3 and 100 kWh/m3 for sapwood and heartwood, respectively), although there was a slight decrease in the modulus of elasticity and bending strength, there was a significant increase in bending plasticity. HIMW-treated specimens exhibited more high-frequency AE signals during elastic–plastic deformation, indicating more frequent fractures in the treated wood during three-point bending. Changes in the microscopic structure of the wood specimens caused by HIMW treatment increased the damage growth rate and stress redistribution efficiency during loading, augmenting the bending plasticity of wood.

这项研究调查了高强度微波(HIMW)处理对辐射松木材机械性能的影响。处理对象是边材和心材,初始含水率为 60%,微波能量密度各不相同:60、80 和 100 kWh/m3:60、80 和 100 kWh/m3。测试评估了三个方向的拉伸和压缩特性,以及剪切强度和弯曲特性。声发射(AE)和数字图像相关(DIC)技术探测了 HIMW 处理前后弯曲负载下的损伤演变。随着微波能量密度的增加,压缩强度、拉伸强度和剪切强度都有所下降,心材最容易受到影响。垂直于纹理的纵向抗压性能和抗拉性能也大幅降低。经过 HIMW 处理(边材和心材分别为 80 kWh/m3 和 100 kWh/m3)后,虽然弹性模量和弯曲强度略有下降,但弯曲塑性却显著增加。经过 HIMW 处理的试样在弹塑性变形过程中表现出更多的高频 AE 信号,表明经过处理的木材在三点弯曲过程中更频繁地发生断裂。HIMW 处理导致木材试样的微观结构发生变化,从而提高了加载过程中的损伤增长速度和应力再分布效率,增强了木材的弯曲塑性。
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引用次数: 0
Mechanistic insight into hydroxy-methylation of hardwood Kraft lignin 硬木牛皮纸木质素羟基甲基化的机理研究
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-09-24 DOI: 10.1007/s00226-024-01596-5
Micaela B. Peralta, Nicolò Pajer, Claudia Crestini, Verónica V. Nicolau

In view of developing upcycling strategies for hardwood Kraft lignin, hydroxy-methylation of Eucalyptus Kraft lignin under alkaline conditions (pH 9 and 11) at different temperatures (50 °C and 70 °C) was studied in the present effort with the double objective of optimizing the reaction conditions and understanding the functionalization mechanism of C5 in either terminal or internal guaiacyl units during hydroxy-methylation. Formaldehyde consumption was estimated via titration of the oximated free formaldehyde; the hydroxy-methylation degree under the reaction was estimated by calculating the ratio in Condensed hydroxyl/Guaiacyl (Condensed OH/G-OH) via a new difference UV-spectroscopy. The reliability of the difference UV-method results for the analyses of the hydroxy-methylated lignins was statistically analysed and compared with that of vacuum-dried and sonicated samples. Hydroxy-methylated samples were then fully characterised by NMR (31P and HSQC) and GPC. The reaction temperature of 50 °C, pH 11, and period time of one hour resulted as the optimal conditions for the hydroxy-methylation, preventing the side-reactions leading to the formation of dimethylene-glycol addition products. The 31P and 1H–13C HSQC NMR revealed the absence of undesirable formaldehyde Cannizzaro by-products and the lack of hydroxymethyl groups in the aliphatic side chain under the studied conditions. GPC analyses, comparing two methodologies, revealed increases in molar mass of the hydroxy-methylated samples upon the formaldehyde addition. The selective hydroxy-methylation at the C5 guaiacyl site demonstrates that Eucalyptus Kraft lignin is as a promising candidate for resol production.

为了开发硬木牛皮纸木质素的升级再循环策略,本研究在不同温度(50 °C和70 °C)、碱性条件(pH值为9和11)下对桉树牛皮纸木质素进行了羟基甲基化,其双重目的是优化反应条件,并了解羟基甲基化过程中端部或内部愈创木酰基单元中C5的官能化机制。甲醛消耗量是通过滴定氧化游离甲醛来估算的;反应中的羟甲基化程度是通过新的紫外光谱差异法计算缩合羟基/愈创木酰基(缩合 OH/G-OH)的比率来估算的。经统计分析,差分紫外法分析羟甲基化木质素结果的可靠性与真空干燥和超声处理样品的可靠性进行了比较。然后通过核磁共振(31P 和 HSQC)和气相色谱对羟甲基化样品进行了全面表征。反应温度为 50 °C、pH 值为 11、反应时间为一小时是羟基甲基化的最佳条件,可防止副反应导致二亚甲基乙二醇加成产物的形成。31P 和 1H-13C HSQC NMR 显示,在所研究的条件下,不存在不良的甲醛 Cannizzaro 副产物,脂肪族侧链中也没有羟甲基。通过比较两种方法进行的 GPC 分析表明,添加甲醛后,羟甲基化样品的摩尔质量增加。C5 愈创木酰基位点的选择性羟甲基化表明,桉树牛皮纸木质素是一种很有希望用于生产 resol 的候选物质。
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Wood Science and Technology
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