纳米碱式氯化镁（BMC）晶须的合成、改性以其在塑料中的应用
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摘要
碱式氯化镁(BMC)的化学组成为Mgx(OH)y Clz·mH2O(2x-y-z=0,0≤m≤6),晶体的形貌为针状或纤维状,具有高耐火性,低热传导性、高耐磨性以及优异的机械性能等优点,可用作塑料、橡胶和树脂的填充剂和阻燃剂以及热稳定剂。随着材料科学的突飞猛进,人们对塑料的要求越来越高,然而现阶段塑料填充剂存在着热稳定性能差、力学性能降低以及成本高等缺点,寻找一种高效低成本的热稳定剂和填充剂的愿望越来越迫切。BMC作为填充剂能够有效地提高塑料的力学性能,改善塑料的热稳定性,且成本低,然而,BMC存在着与塑料的相容性较差,且晶须结构不稳定等缺点,亟须改善。
为了深入研究BMC的制备原理,降低制备成本,并改进BMC晶须在塑料中的分散性,从而达到控制制备、降低成本以及纤维增强增韧的作用,本文首先在两种不同的体系(CaO-MgCl2-H2O体系以及以白云岩为原料的CaO/MgO-MgCl2-H2O)中通过水热反应可控合成了BMC晶须,并研究了BMC的结构、形貌、性质等随反应物浓度、摩尔比、水热条件的变化。随后,我们针对BMC晶须的特性,将其经过硅烷偶联剂γ-MPS表面处理后,进行表面接枝改性,最后将表面接枝改性后的g-BMC分别与PVC混合制备了g-BMC/PVC、和ABS、PP熔融共混制备了ABS/PP合金材料,并研究了乙醇／水介质体系、反应时间对晶须形态和悬浮接枝聚合反应的影响以及对PVC热稳定性的影响和ABS/PP合金材料的力学性能和熔融指数等影响。
合成实验结果表明：在CaO-MgCl2-H2O体系以及CaO/MgO-MgCl2-H2O体系中,当氯化镁浓度大于3 mol/L能得到一维BMC,且BMC的长径比随氯化镁浓度和CaO、(CaO+MgO)与MgCl2的摩尔比R的增大而减小。在CaO-MgCl2-H2O体系,R小于0.5时,制备具有高长径比的BMC的最佳条件为[MgCl2]=4 mol/L,R=0.05。水热条件不仅影响着BMC的长径比及有序度,还决定了BMC的合成相：较低温度(≤150℃)下合成的产物为相3或相5,而高温下的产物为相9。以白云岩煅粉为原料的CaO/MgO-MgCl2-H2O体系,R介于0.025-0.075之间可得到一维BMC,直径为50-120 nm。
表面接枝改性实验中,以乙醇/水为反应介质,K2S2O8(KPS)为引发剂的反应条件能够在满足保持BMC晶须形貌的前提下获得较好的MMA接枝效果。最佳反应条件为乙醇/水介质配比为8:2、反应温度82℃、反应时间6 h。此时,BMC晶须形貌很好的被保存下来(经FT-IR、SEM、XRD表征),并且接枝效果较好(接枝效率达到56.1%)。
将表面接枝改性后的BMC晶须材料与PVC熔融共混,能够有效地改善PVC的热稳定性和提高PVC的初始降解温度。随着g-BMC添加量的增加,PVC的白度有所降低。当g-BMC的添加量为2.5%时,PVC的变色时间和刚果红变色时间分别为140 min和204 min。
将表面接枝改性后的BMC晶须材料包覆一层TPE橡胶制成BMC母料添加入ABS中,分别考察BMC母料含量以及BMC母料中BMC含量对BMC填充ABS材料性能的影响。研究结果表明：ABS/BMC复合材料的拉伸强度随着BMC含量的增加而增加,当BMC母料含量为15%,BMC母料中BMC含量为55%左右时有较佳的冲击性能。然后,固定BMC母料与ABS比例不变,将BMC母料、ABS、PP、PP-g-MAH熔融共混获得ABS/PP合金材料,实验分别研究了PP含量、BMC含量对ABS/PP合金材料的影响。研究结果表明：当PP含量为9-10%时BMC填充ABS/PP合金材料有最好的拉伸强度和冲击强度；BMC填料含量对BMC填充ABS/PP合金材料的拉伸强度影响不大,但随其用量增加冲击强度有明显的提高；BMC填充ABS/PP合金材料的熔体流动性能在PP含量10%左右时达到最大,但随BMC含量增加而下降。
本论文不仅提供了一种可控制备BMC的新途径和表面改性的新方法,更拓宽了白云岩的应用领域,拓展了碳酸盐矿物如石灰石等的潜在用途,对完整保存晶须形态的改性方法具有借鉴意义,对BMC的应用研究具有补充发展的作用。
The chemical composition of basic magnesium chloride(BMC) whisker is Mgx(OH)y Clz·mH2O(2x-y-z=0,0≤m≤6), and its morphology is needle or fiber. Due to the characteristics of high fire behavior, low thermal conductivity, excellent wear-resisting and mechanical properties, BMC is widely use in areas of plastics, rubbers and resins as filling agents and heat stabilizer. With the development of material science, more and more researches were studied to settle the problem between increasing requirements of people and short points of meterials. However, BMC can inhance plastics'thermal stability and mechanical properties unless its compatibility and whisker structure well preserved.
This study was aimed to settle the utilization problem of BMC's applications and cost in Plastic. Firstly, one-dimensional BMC was controlled prepared in two different system. Then, BMC was pretreated by silane coupling agent 3-(trimethoxysilyl) propyl methacrylate (y-MPS) and then conducted to surface radical grafting polymerization, the grafted BMC was applied to poly(vinyl chloride)(PVC) and ABS/PP composites respectively at last. The effects of MgCl2 concentration, molar ratio (R), and hydrothermal conditions on the structure and morphology of BMC were investigated, Besides, the influence of reaction conditions on both conservation of whisker topography and the effect of grafting polymerization is discussed, both thermal stability of PVC and mechanical properties of ABS/PP composites were studied in this paper. The main contents and results were as follows:
It is found that, both in two systems of CaO-MgCl2-H2O and CaO/MgO-MgCl2-H2O, BMC can only be synthesized when the MgCl2 concentration was greater than 3 mol/L The molar ratio R plays a key role to the structure and morphology of BMC. The diameter and radius-length ratio of BMC increase with the MgCl2 concentration and R. In the system of CaO-MgCl2-H2O, the optimum conditions to prepare BMC are [MgCl2]=4 mol/L and R=0.05. The reaction temperature determines the phases of BMC, where phase 3 (Mg2(OH)3Cl·4H2O) is stable at below 150℃and phase 9 (Mg10(OH)18Cl2·5H2O) is obtained at above 150℃. The optimum R to prepare BMC is between 0.025 and 0.075 in the system of CaO/MgO-MgCl2-H2O, using calcined dolomite.
The result of grafting study shows that the reaction condition has a strong impact on the topography of nano-composite material. The grafting efficiency is maximum (up to 56.1%) and the appearance of BMC whisker is well conserved when ethanol:water=8:2,the reaction temperature is 82℃,and the reaction time is 6 hours.
When applied to PVC composites, g-BMC can enhance the thermal stability and increase the decomposition temperature of PVC. When 2.5 wt% g-BMCwas added, the color change time and Congo red time of PVC composites are 140 min and 204 min.
The test results of composites'mechanical property and melt performance indicated that as the g-BMC packing content increased when in experimental range, the composites tensile strength improved as well; When the content of master batch was 15% and the g-BMC packing content was about 55%, the composites had better impact property; when the content of PP is 9% to 10%, the composites has the best tensile strength and impact property; while the g-BMC packing content has little effect on the tensile strength, it has improved impact property greatly with its increased use; with respect to melt performance, it reached the maximum when the content of PP is about 10%, while it decreased with the increase of g-BMC packing content.
为了深入研究BMC的制备原理,降低制备成本,并改进BMC晶须在塑料中的分散性,从而达到控制制备、降低成本以及纤维增强增韧的作用,本文首先在两种不同的体系(CaO-MgCl2-H2O体系以及以白云岩为原料的CaO/MgO-MgCl2-H2O)中通过水热反应可控合成了BMC晶须,并研究了BMC的结构、形貌、性质等随反应物浓度、摩尔比、水热条件的变化。随后,我们针对BMC晶须的特性,将其经过硅烷偶联剂γ-MPS表面处理后,进行表面接枝改性,最后将表面接枝改性后的g-BMC分别与PVC混合制备了g-BMC/PVC、和ABS、PP熔融共混制备了ABS/PP合金材料,并研究了乙醇／水介质体系、反应时间对晶须形态和悬浮接枝聚合反应的影响以及对PVC热稳定性的影响和ABS/PP合金材料的力学性能和熔融指数等影响。
合成实验结果表明：在CaO-MgCl2-H2O体系以及CaO/MgO-MgCl2-H2O体系中,当氯化镁浓度大于3 mol/L能得到一维BMC,且BMC的长径比随氯化镁浓度和CaO、(CaO+MgO)与MgCl2的摩尔比R的增大而减小。在CaO-MgCl2-H2O体系,R小于0.5时,制备具有高长径比的BMC的最佳条件为[MgCl2]=4 mol/L,R=0.05。水热条件不仅影响着BMC的长径比及有序度,还决定了BMC的合成相：较低温度(≤150℃)下合成的产物为相3或相5,而高温下的产物为相9。以白云岩煅粉为原料的CaO/MgO-MgCl2-H2O体系,R介于0.025-0.075之间可得到一维BMC,直径为50-120 nm。
表面接枝改性实验中,以乙醇/水为反应介质,K2S2O8(KPS)为引发剂的反应条件能够在满足保持BMC晶须形貌的前提下获得较好的MMA接枝效果。最佳反应条件为乙醇/水介质配比为8:2、反应温度82℃、反应时间6 h。此时,BMC晶须形貌很好的被保存下来(经FT-IR、SEM、XRD表征),并且接枝效果较好(接枝效率达到56.1%)。
将表面接枝改性后的BMC晶须材料与PVC熔融共混,能够有效地改善PVC的热稳定性和提高PVC的初始降解温度。随着g-BMC添加量的增加,PVC的白度有所降低。当g-BMC的添加量为2.5%时,PVC的变色时间和刚果红变色时间分别为140 min和204 min。
将表面接枝改性后的BMC晶须材料包覆一层TPE橡胶制成BMC母料添加入ABS中,分别考察BMC母料含量以及BMC母料中BMC含量对BMC填充ABS材料性能的影响。研究结果表明：ABS/BMC复合材料的拉伸强度随着BMC含量的增加而增加,当BMC母料含量为15%,BMC母料中BMC含量为55%左右时有较佳的冲击性能。然后,固定BMC母料与ABS比例不变,将BMC母料、ABS、PP、PP-g-MAH熔融共混获得ABS/PP合金材料,实验分别研究了PP含量、BMC含量对ABS/PP合金材料的影响。研究结果表明：当PP含量为9-10%时BMC填充ABS/PP合金材料有最好的拉伸强度和冲击强度；BMC填料含量对BMC填充ABS/PP合金材料的拉伸强度影响不大,但随其用量增加冲击强度有明显的提高；BMC填充ABS/PP合金材料的熔体流动性能在PP含量10%左右时达到最大,但随BMC含量增加而下降。
本论文不仅提供了一种可控制备BMC的新途径和表面改性的新方法,更拓宽了白云岩的应用领域,拓展了碳酸盐矿物如石灰石等的潜在用途,对完整保存晶须形态的改性方法具有借鉴意义,对BMC的应用研究具有补充发展的作用。
The chemical composition of basic magnesium chloride(BMC) whisker is Mgx(OH)y Clz·mH2O(2x-y-z=0,0≤m≤6), and its morphology is needle or fiber. Due to the characteristics of high fire behavior, low thermal conductivity, excellent wear-resisting and mechanical properties, BMC is widely use in areas of plastics, rubbers and resins as filling agents and heat stabilizer. With the development of material science, more and more researches were studied to settle the problem between increasing requirements of people and short points of meterials. However, BMC can inhance plastics'thermal stability and mechanical properties unless its compatibility and whisker structure well preserved.
This study was aimed to settle the utilization problem of BMC's applications and cost in Plastic. Firstly, one-dimensional BMC was controlled prepared in two different system. Then, BMC was pretreated by silane coupling agent 3-(trimethoxysilyl) propyl methacrylate (y-MPS) and then conducted to surface radical grafting polymerization, the grafted BMC was applied to poly(vinyl chloride)(PVC) and ABS/PP composites respectively at last. The effects of MgCl2 concentration, molar ratio (R), and hydrothermal conditions on the structure and morphology of BMC were investigated, Besides, the influence of reaction conditions on both conservation of whisker topography and the effect of grafting polymerization is discussed, both thermal stability of PVC and mechanical properties of ABS/PP composites were studied in this paper. The main contents and results were as follows:
It is found that, both in two systems of CaO-MgCl2-H2O and CaO/MgO-MgCl2-H2O, BMC can only be synthesized when the MgCl2 concentration was greater than 3 mol/L The molar ratio R plays a key role to the structure and morphology of BMC. The diameter and radius-length ratio of BMC increase with the MgCl2 concentration and R. In the system of CaO-MgCl2-H2O, the optimum conditions to prepare BMC are [MgCl2]=4 mol/L and R=0.05. The reaction temperature determines the phases of BMC, where phase 3 (Mg2(OH)3Cl·4H2O) is stable at below 150℃and phase 9 (Mg10(OH)18Cl2·5H2O) is obtained at above 150℃. The optimum R to prepare BMC is between 0.025 and 0.075 in the system of CaO/MgO-MgCl2-H2O, using calcined dolomite.
The result of grafting study shows that the reaction condition has a strong impact on the topography of nano-composite material. The grafting efficiency is maximum (up to 56.1%) and the appearance of BMC whisker is well conserved when ethanol:water=8:2,the reaction temperature is 82℃,and the reaction time is 6 hours.
When applied to PVC composites, g-BMC can enhance the thermal stability and increase the decomposition temperature of PVC. When 2.5 wt% g-BMCwas added, the color change time and Congo red time of PVC composites are 140 min and 204 min.
The test results of composites'mechanical property and melt performance indicated that as the g-BMC packing content increased when in experimental range, the composites tensile strength improved as well; When the content of master batch was 15% and the g-BMC packing content was about 55%, the composites had better impact property; when the content of PP is 9% to 10%, the composites has the best tensile strength and impact property; while the g-BMC packing content has little effect on the tensile strength, it has improved impact property greatly with its increased use; with respect to melt performance, it reached the maximum when the content of PP is about 10%, while it decreased with the increase of g-BMC packing content.
引文
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