微化蒙脱土悬浮液的制备及其处理材性能和表征
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摘要
蒙脱土是粘土的一种,是一类层状硅酸盐类化合物,在我国资源丰富,价格低廉,广泛应用于高分子材料的改性中。为了改善木材的物理、力学等性能,本研究制备了微化蒙脱土悬浮液并对木材进行改性。研究采用一步法以及两步法制备工艺,利用蒙脱土的阳离子可交换性、添加化学分散剂和物理分散方式提高有机蒙脱土颗粒在水相中的分散稳定性,制备稳定的微化蒙脱土悬浮液,通过满细胞法真空-加压浸注杉木试材,制备微化蒙脱土悬浮液改性处理材(以下简称改性处理材),并采用X-射线衍射分析(XRD)、傅里叶红外光谱分析(FTIR)、扫描电镜-能谱分析(SEM-EDXA)、差热-热重分析(DTA-TG)、Zeta电位仪以及激光粒度仪进行表征及分析,得到如下主要结论：
(1)采用二甲基双癸基氯化铵(DDAC)对蒙脱土进行有机改性可以明显提高层间距以及表面疏水性,降低吸水膨胀性。其中影响蒙脱土改性效果的各因素的影响因子的顺序为：改性剂的加入量>改性体系的pH值>蒙脱土的分散浓度>改性时间>陈化时间>改性温度。制备有机蒙脱土的优化工艺为：DDAC过量150%,原土分散浓度为5%,体系pH值为10,改性时间为2h,陈化24h,改性温度为50℃。在该工艺下制备的有机蒙脱土的层间距达到27.34 A,部分片层甚至完全剥离,疏水性得到明显改善。
(2)采用聚乙烯醇(PVA)或聚乙二醇(PEG)作为分散剂均能有效提高有机蒙脱土在水相中的分散稳定性,其效果与分散剂浓度等因素相关。研究结果表明,制备微化蒙脱土悬浮液分散剂的优化参数为：(1)当高分子分散剂浓度>1%时,选择PVA高分子分散剂,DDAC浓度为1.4%,高分子分散剂浓度为2%或者1%,pH值为8-10；OMMT分散浓度为5%。(2)当高分子分散剂浓度<1%时,选择PEG高分子分散剂,DDAC浓度为<0.7%,高分子分散剂浓度为0.5%或者0.25%,pH值为8-10,OMMT分散浓度为2%。分散方式对微化蒙脱土悬浮液制备的影响顺序：球磨分散>机械搅拌分散>超声波分散。
(3)使用PVA复配分散剂,分别采用一步法以及两步法制备稳定的PVA微化蒙脱土悬浮液,通过满细胞法真空-加压浸注处理木材,制备PVA微化蒙脱土悬浮液改性处理材(PVDMW)。结果表明,两步法制备的改性处理材中蒙脱土主要以大颗粒的形式填充在木材管胞腔等大细胞腔中,而未进入木材细胞壁中与其主要成分发生作用,因此改性处理材的性能提高较小。而一步法制备改性处理材中一小部分剥离的蒙脱土小片层进入了木材细胞壁的非结晶区,并与木材的主要成分发生一定的化学反应,使木材细胞壁中含有部分的Si元素,改性处理材的结晶度提高,对应的改性处理材的热稳定性、抗水流失性、尺寸稳定性、表面硬度、抗压强度等都有一定程度的提高,改性处理材的性能在一定程度上得到改善。然而由于PVA过长的分子长链降低了球磨效果,剥离的蒙脱土小片层含量较低,因此改性处理材各项性能虽然各有提高,但效果却并不显著。
(4)使用PEG复配分散剂,分别采用一步法以及两步法制备稳定的PEG微化蒙脱土悬浮液,通过满细胞法浸注真空-加压浸注处理木材,制备PEG微化蒙脱土悬浮液改性处理材(PEDMW),其中添加PEG1000的一步法制备改性处理材中,蒙脱土主要以小颗粒状以及纳米片状的形式分布在木材细胞腔以及进入木材细胞壁中,使木材细胞壁中Si元素的含量显著提高,其中OMMT通过PEG的络合作用进一步与木材纤维素及半纤维中的醇羟基发生络合反应,生成新的络合物,还可以与木素中的羰基发生作用。而随着蒙脱土纳米片层进入木材细胞壁的非结晶区使改性处理材的结晶度显著提高,蒙脱土纳米效应的发挥使相应的一步法改性处理材在抗水流失性、尺寸稳定性、表面硬度以及抗压强度等方面都得到显著的提高。而两步法制备改性处理材中由于蒙脱土片层的粒度没有降低,蒙脱土主要以大颗粒的形式吸附在木材的大孔隙中,没有进入木材的细胞壁,导致两步法制备改性处理材在性能提高方面低于一步法制备改性处理材。而当添加PEG8000时,PEG8000降低木材的渗透性,阻止了蒙脱土等有效成分进入木材细胞腔中,改性处理材的各项性能的提高也明显低于PEG1000作为分散剂的一步法制备改性处理材。
Montmorillonite (MMT) is a crystalline aluminosilicate with a platete morphology. Because of its rich resources and low price, it has been widely used to prepare montmorillonte/polymer nanocomposite to improve the properties of polymer. In order to improve the properties of wood, micronized montmorillonite suspension as a wood modifier was prepared in this study by using the exchangeable cations in MMT, proper dispersion method and compound dispersants in both one-step and two-step methods. It was then used to treat wood through a full-cell process and the X-ray diffractometer (XRD), fourier transform infraredspectroscopy (FTIR), scanning electron microscope with energy dispersive X-ray analysis (SEM-EDXA), differential thermal analysis-thermogravimetric analysis (DTA-TG), Zeta potential analyzer and laser particle instrument were used to analysis and character, and the following results are obtained:
(1) The interlayer distance and surface hydrophobicity of organic montmorillonite modified with DDAC was obviously improved. The order of main factors which influence the modification effect of MMT is:addition amount of modification agent> pH value of system>MMT diffraction concentration>reaction time> aging time>reaction temperature. The optimized process is as follows: modification agent:DDAC; addition amount of DDAC:150%; pH value:10; reaction time:2h; aging time:24h; reaction temperature:50℃. By using this modification process, the interlayer distance of organic montmorillonite (OMMT) was enlarged to a maximum of 27.34 (?) with some layers exfoliated totally. Besides, the surface hydrophobicity of OMMT is obviously improved.
(2) The stability of OMMT suspension in aqueous solution was greatly improved by using polyvinyl alcohol (PVA) or polyethylene glycol (PEG) dispersants. The optimized parameters vary with the polymer concentrations. (1) at polymer concentrations higher than 1%, PVA is preferred and the parameters are as follows:DDAC concentration:1.4%; PVA concentration:1% or 2%; pH value: 8-10; OMMT concentration:5%. (2) at polymer concentrations lower than 1%, PEG is preferred and the parameters are as follows:DDAC concentration:<0.7%; PEG concentration:0.25% or 0.5%; pH value:8-10; OMMT concentration:2%. The dispersion method in a order of best to worst is:ball milling>mechanical stirring>ultrasonic dispersion.
(3) Samples treated with micronized montmorillonte suspension using PVA as dispersant (PVDMW) were characterized and the properties were tested. PVDMW-2 treated with suspension prepared by two step method showed a great amount of large OMMT clusters blocking in wood cell lumen or covering on the surface of wood cell wall without penetrating into the wood cell wall. As a result, the properties of treated wood are not improved significantly. However, PVDMW-1 treated with suspension prepared by the one-step method showed some exfoliated OMMT layers entering into the amorphous region of wood cell wall, which increased the crystallinity of wood and consequently improved the wood properties to some extent including the thermal property, leaching resistance, dimensional stability, surface hardness and compression strength.
(4) Samples treated with micronized organic montmorillonite suspension using PEG1000 or PEG8000 as dispersants (PEDMW) were characterized and the properties were tested. In PEDMW-1 samples treated with suspension prepared by one-step method, the small particles or exfoliated layers of OMMT filled the cell lumen or wood cell wall, which was demonstrated in the detected increasing content of Si element in the wood cell wall. OMMT layers formed complex bonds with alcoholic hydroxyl groups in wood cellulouse and hemicelluloses as well as the carboxyl group in lignin through PEG. As a result, the wood crtstallinity was greated increased and the properties including the thermal property, leaching resistance, dimensional stability, surface hardness and compression streangth of PEDMW-1 were improved significantly. The performance of PEDMW-2 treated with suspension prepared by two-step method is similar to that of PVDMW-2. In PEDMW-8 samples treated with suspension dispersed by PEG8000 in one-step method, the OMMT nano-layers could not get into wood cell wall due to the long chains of PEG8000, which also led to relatively low properties of PEDMW-8.
(1)采用二甲基双癸基氯化铵(DDAC)对蒙脱土进行有机改性可以明显提高层间距以及表面疏水性,降低吸水膨胀性。其中影响蒙脱土改性效果的各因素的影响因子的顺序为：改性剂的加入量>改性体系的pH值>蒙脱土的分散浓度>改性时间>陈化时间>改性温度。制备有机蒙脱土的优化工艺为：DDAC过量150%,原土分散浓度为5%,体系pH值为10,改性时间为2h,陈化24h,改性温度为50℃。在该工艺下制备的有机蒙脱土的层间距达到27.34 A,部分片层甚至完全剥离,疏水性得到明显改善。
(2)采用聚乙烯醇(PVA)或聚乙二醇(PEG)作为分散剂均能有效提高有机蒙脱土在水相中的分散稳定性,其效果与分散剂浓度等因素相关。研究结果表明,制备微化蒙脱土悬浮液分散剂的优化参数为：(1)当高分子分散剂浓度>1%时,选择PVA高分子分散剂,DDAC浓度为1.4%,高分子分散剂浓度为2%或者1%,pH值为8-10；OMMT分散浓度为5%。(2)当高分子分散剂浓度<1%时,选择PEG高分子分散剂,DDAC浓度为<0.7%,高分子分散剂浓度为0.5%或者0.25%,pH值为8-10,OMMT分散浓度为2%。分散方式对微化蒙脱土悬浮液制备的影响顺序：球磨分散>机械搅拌分散>超声波分散。
(3)使用PVA复配分散剂,分别采用一步法以及两步法制备稳定的PVA微化蒙脱土悬浮液,通过满细胞法真空-加压浸注处理木材,制备PVA微化蒙脱土悬浮液改性处理材(PVDMW)。结果表明,两步法制备的改性处理材中蒙脱土主要以大颗粒的形式填充在木材管胞腔等大细胞腔中,而未进入木材细胞壁中与其主要成分发生作用,因此改性处理材的性能提高较小。而一步法制备改性处理材中一小部分剥离的蒙脱土小片层进入了木材细胞壁的非结晶区,并与木材的主要成分发生一定的化学反应,使木材细胞壁中含有部分的Si元素,改性处理材的结晶度提高,对应的改性处理材的热稳定性、抗水流失性、尺寸稳定性、表面硬度、抗压强度等都有一定程度的提高,改性处理材的性能在一定程度上得到改善。然而由于PVA过长的分子长链降低了球磨效果,剥离的蒙脱土小片层含量较低,因此改性处理材各项性能虽然各有提高,但效果却并不显著。
(4)使用PEG复配分散剂,分别采用一步法以及两步法制备稳定的PEG微化蒙脱土悬浮液,通过满细胞法浸注真空-加压浸注处理木材,制备PEG微化蒙脱土悬浮液改性处理材(PEDMW),其中添加PEG1000的一步法制备改性处理材中,蒙脱土主要以小颗粒状以及纳米片状的形式分布在木材细胞腔以及进入木材细胞壁中,使木材细胞壁中Si元素的含量显著提高,其中OMMT通过PEG的络合作用进一步与木材纤维素及半纤维中的醇羟基发生络合反应,生成新的络合物,还可以与木素中的羰基发生作用。而随着蒙脱土纳米片层进入木材细胞壁的非结晶区使改性处理材的结晶度显著提高,蒙脱土纳米效应的发挥使相应的一步法改性处理材在抗水流失性、尺寸稳定性、表面硬度以及抗压强度等方面都得到显著的提高。而两步法制备改性处理材中由于蒙脱土片层的粒度没有降低,蒙脱土主要以大颗粒的形式吸附在木材的大孔隙中,没有进入木材的细胞壁,导致两步法制备改性处理材在性能提高方面低于一步法制备改性处理材。而当添加PEG8000时,PEG8000降低木材的渗透性,阻止了蒙脱土等有效成分进入木材细胞腔中,改性处理材的各项性能的提高也明显低于PEG1000作为分散剂的一步法制备改性处理材。
Montmorillonite (MMT) is a crystalline aluminosilicate with a platete morphology. Because of its rich resources and low price, it has been widely used to prepare montmorillonte/polymer nanocomposite to improve the properties of polymer. In order to improve the properties of wood, micronized montmorillonite suspension as a wood modifier was prepared in this study by using the exchangeable cations in MMT, proper dispersion method and compound dispersants in both one-step and two-step methods. It was then used to treat wood through a full-cell process and the X-ray diffractometer (XRD), fourier transform infraredspectroscopy (FTIR), scanning electron microscope with energy dispersive X-ray analysis (SEM-EDXA), differential thermal analysis-thermogravimetric analysis (DTA-TG), Zeta potential analyzer and laser particle instrument were used to analysis and character, and the following results are obtained:
(1) The interlayer distance and surface hydrophobicity of organic montmorillonite modified with DDAC was obviously improved. The order of main factors which influence the modification effect of MMT is:addition amount of modification agent> pH value of system>MMT diffraction concentration>reaction time> aging time>reaction temperature. The optimized process is as follows: modification agent:DDAC; addition amount of DDAC:150%; pH value:10; reaction time:2h; aging time:24h; reaction temperature:50℃. By using this modification process, the interlayer distance of organic montmorillonite (OMMT) was enlarged to a maximum of 27.34 (?) with some layers exfoliated totally. Besides, the surface hydrophobicity of OMMT is obviously improved.
(2) The stability of OMMT suspension in aqueous solution was greatly improved by using polyvinyl alcohol (PVA) or polyethylene glycol (PEG) dispersants. The optimized parameters vary with the polymer concentrations. (1) at polymer concentrations higher than 1%, PVA is preferred and the parameters are as follows:DDAC concentration:1.4%; PVA concentration:1% or 2%; pH value: 8-10; OMMT concentration:5%. (2) at polymer concentrations lower than 1%, PEG is preferred and the parameters are as follows:DDAC concentration:<0.7%; PEG concentration:0.25% or 0.5%; pH value:8-10; OMMT concentration:2%. The dispersion method in a order of best to worst is:ball milling>mechanical stirring>ultrasonic dispersion.
(3) Samples treated with micronized montmorillonte suspension using PVA as dispersant (PVDMW) were characterized and the properties were tested. PVDMW-2 treated with suspension prepared by two step method showed a great amount of large OMMT clusters blocking in wood cell lumen or covering on the surface of wood cell wall without penetrating into the wood cell wall. As a result, the properties of treated wood are not improved significantly. However, PVDMW-1 treated with suspension prepared by the one-step method showed some exfoliated OMMT layers entering into the amorphous region of wood cell wall, which increased the crystallinity of wood and consequently improved the wood properties to some extent including the thermal property, leaching resistance, dimensional stability, surface hardness and compression strength.
(4) Samples treated with micronized organic montmorillonite suspension using PEG1000 or PEG8000 as dispersants (PEDMW) were characterized and the properties were tested. In PEDMW-1 samples treated with suspension prepared by one-step method, the small particles or exfoliated layers of OMMT filled the cell lumen or wood cell wall, which was demonstrated in the detected increasing content of Si element in the wood cell wall. OMMT layers formed complex bonds with alcoholic hydroxyl groups in wood cellulouse and hemicelluloses as well as the carboxyl group in lignin through PEG. As a result, the wood crtstallinity was greated increased and the properties including the thermal property, leaching resistance, dimensional stability, surface hardness and compression streangth of PEDMW-1 were improved significantly. The performance of PEDMW-2 treated with suspension prepared by two-step method is similar to that of PVDMW-2. In PEDMW-8 samples treated with suspension dispersed by PEG8000 in one-step method, the OMMT nano-layers could not get into wood cell wall due to the long chains of PEG8000, which also led to relatively low properties of PEDMW-8.
引文
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