核壳结构改性剂增韧聚甲基丙烯酸甲酯类树脂的研究
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摘要
聚甲基丙烯酸甲酯类树脂通常包括甲基丙烯酸甲酯均聚物与甲基丙烯酸甲酯及少量丙烯酸酯类单体的共聚物以及甲基丙烯酸甲酯与苯乙烯等单体的共聚物。该类材料是一种典型的刚性无定形聚合物,因其优异的耐紫外线性能与光学性能而广泛地应用于家用电器、电子产品、医疗与汽车等领域。但由于其宏观力学性能具有明显的脆性与缺口敏感性,因此对其增韧改性的研究一直备受关注,其中采用核壳结构改性剂的增韧方法是聚甲基丙烯酸甲酯类树脂增韧的最为重要的手段。与其它材料增韧相比,聚甲基丙烯酸甲酯类树脂的增韧更为复杂,增韧时不仅要求所采用改性剂能够有效地促进增韧产物断裂能的吸收以实现共混物的力学性能提高,而且还要求其折光指数与基体树脂相匹配以保持基体树脂的良好透光性能。虽然采用聚丙烯酸丁酯(PBA)为橡胶相的耐候级改性剂与聚丁二烯(PB)为橡胶相的非耐候级改性剂都能够增韧聚甲基丙烯酸甲酯类树脂,但由于PBA与PB的折光指数与基体树脂折光指数不匹配,会使增韧产物的透光性能显著下降,因此在改性剂橡胶相的乳液聚合过程中共聚定量的高折光指数的St以匹配改性剂与基体折光指数,才能获得较高透光性能的增韧产物。
本研究从结构与性能可控的改性剂合成出发,考察了改性剂结构、橡胶相交联程度、改性剂与基体树脂界面性能变化等因素对聚甲基丙烯酸甲酯类树脂的增韧的影响,主要研究内容与结论如下：
1、在丙烯酸酯类冲击改性剂(Acrylic impact modifiers, AIMs)的橡胶相P(BA-co-St)种子乳液聚合的反应恒速期内,考察了聚合反应速率与引发剂浓度之间关系,研究了在种子乳液聚合过程中橡胶相粒子粒径的变化规律。结果表明聚合反应速率与引发剂浓度关系为Rp∞I0.44,橡胶粒子粒径以逐步长大方式增长。合成出了BA-St共聚物为橡胶核,PMMA为外壳的两层结构AIM改性剂与PS或PMMA为内核,PBA或BA-St共聚物为橡胶层,PMMA为外壳的三层结构AIM改性剂。考察了AIM结构对PMMA树脂增韧的影响,结果表明采用两层结构AIM改性剂增韧PMMA时,其最大冲击强度、断裂能与最大应力强度因子(Kmax)所对应的最优AIM橡胶相粒子粒径为269nm,其裂纹增长能(Uprop)在AIM橡胶相粒子粒径为351nm时达到最大,增韧产物的可见光透过率随着橡胶相粒子粒径的增长逐步下降,雾度逐步上升。与两层结构AIM对PMMA的增韧相比较,三层结构AIM的增韧产物的Kmax明显高于两层结构AIM的增韧产物,表明了三层结构改性剂中橡胶相的形变形式更有利于阻止共混物断裂过程中裂纹的产生。通过两种三层结构AIM增韧PMMA的形变区透射电镜观察可见,改性剂中间橡胶层为BA-St共聚物时,橡胶粒子发生了明显的空洞化,而中间层橡胶为PBA时,断裂形变区中可发现银纹的产生,这表明三层结构改性剂的中间橡胶层的性质对增韧机理的影响显著。
2、研究了AIM的橡胶相交联程度对PMMA增韧的影响,结果发现随着橡胶相的交联程度上升,共混物冲击强度呈先上升后下降的趋势,当采用橡胶相交联程度适当的AIM时,共混物冲击强度、Kmax与Uprop达到最大值。共混物冲击断面的形态分析表明其断裂机理为橡胶粒子空洞化引起基体树脂的剪切屈服,适当交联程度的橡胶相在断裂时有利于形成较多的空洞并能够更有效地促进橡胶粒子周围基体树脂的局部剪切屈服。
3、为研究改性剂与基体树脂间界面粘结性能对增韧的影响,将带有羧酸基团的AIM、PMMA与本体法制备的甲基丙烯酸甲酯-甲基丙烯酸环氧丙酯-丙烯酸甲酯三元共聚物熔融共混制备出增韧产物,考察共混过程中共混物转矩值变化与所制得共混物的性能变化,结果显示随着AIM改性剂壳层中羧酸含量的提高,熔融共混过程中的最大转矩值与平衡转矩值逐步提高,共混物的冲击强度与Kmax逐步上升,但光学性能不受影响。这表明了共混过程中改性剂上的羧酸官能团已经与基体树脂中环氧官能团发生了反应,并且随着化学反应程度的上升,两相间的界面粘结性能提高。这不仅使共混物熔体粘度上升,转矩值提高,而且有利于共混物断裂形变过程中更多橡胶粒子发生了空洞化并促进基体树脂更大程度的剪切屈服。
4、采用乳液聚合方法合成了甲基丙烯酸甲酯-丁二烯-苯乙烯核壳结构接枝共聚物(MBS)作为聚甲基丙烯酸甲酯类树脂的非耐候级改性剂,研究了MBS中丁苯橡胶(SBR)粒子粒径随着乳液聚合中乳化剂用量变化的规律,考察了在SBR粒子上St与MMA的不同接枝方式制备的三种MBS与甲基丙烯酸甲酯-苯乙烯共聚物(MS)的界面粘结力变化对其增韧产物性能的影响。结果表明：SBR粒子粒径随乳液聚合中乳化剂用量上升而下降；三种MBS改性剂都能够在MS树脂中均匀分散,其中采用混合MMA与St的接枝方式制备的MBS壳层为St与MMA的无规共聚物,这种改性剂与MS熔融共混过程中平衡转矩值最高,共混物冲击强度最大,透光性能最好。而MMA与St按照不同先后顺序接枝在SBR上制备出的MBS,其壳层为接枝在SBR粒子上的MMA与St均聚物,这种改性剂对MS树脂的增韧效果较差,共混物透光性能较低。这表明了MBS与MS间良好的界面性能有助于共混物性能的提高。
本工作在保持聚甲基丙烯酸甲酯类树脂优异透光性能的前提下,成功地解决了其增韧问题,制备出透过率为88.6%,冲击强度较纯PMMA树脂提高了4倍的增韧产物,该材料的力学性能已超过HIPS等通用增韧树脂,能够满足实用要求。
Polymethyl methacrylate (PMMA) resins usually comprise the polymethyl methacrylate homopolymer and the compolymers containing predominantly methyl methacrylate but with small amounts of methyl or ethyl acrylate, acrylonitrile or styrene comonomers added for improved toughness. PMMA resins are rigid, amorphous polymers particularly noted for their exceptional clarity and UV resistance, and therefore wildly used for making household appliances, electronic products, medical devices and automobile, etc. Due to the poor toughness and notch sensitivity, the research on toughening receives much concern, in which adopting core-shell modifiers toughening PMMA resins is one of the most important method. The strategy of PMMA resins toughened by core-shell modifiers show more complexity than other amorphous polymer, which demands modifiers not only promote more fracture energy absorption in the process of toughened blends fracture, which highen the mechanical properties, but refractive index of modifiers match with PMMA resins to maintain better optical property of matrix resins. Both weatherable modifiers with polybutyl acrylate (PBA) rubber phase and non-weatherable modifier with polybutadiene (PB) rubber phase can toughen PMMA resins effectively, but transmittance of blends decreases markly for mismatch of refractive index of PBA and PB with PMMA resins. So combined St with PBA or PB to match refractive index of modifiers with matrix resins can prepare toughening blends with high light transmittance.
In this paper, preformed modifiers with controllable structure and proterties were synthesized. The influence of modifiers structure, cross-linking density of rubber phase, and the variance of interface property between modifiers and matrix on PMMA resins toughening were investigated. The main research works and conclusions are as follows:
1. The relationship between reaction rate and initior concentration was investigated in the process of constant rate period of P(BA-co-St) emulsion polymerization, and the results showed that the relationship of reaction rate and initior concentration was Rp∞I0.44. The diameter of P(BA-co-St) rubber particles increased according to grow-out manner. Two layers acrylic impact modifiers (AIM), which was composed of BA-St copolymer rubber core and PMMA outer shell, and three layer modifiers with PS or PMMA inner core, BA or BA-St copolymer interface layer and PMMA external shell were synthsized by emulsion polymerization. The influence of AIM structure on PMMA toughess was investigated, and results showed that the optimum diameter of rubber particle of two layers AIMs was269nm, which led to maxium impact strength, fracture energy and stress intensity factor (Kmax) of AIM/PMMA blends, and crack propagating energy (Uprop) reached maxium when rubber particle diameter of AIM was351nm. The transmittance of blends decreased with the increament of rubber particles diameter, whereas the haze increased. The blends with three layers AIM had higher Kmax than those blends with two layers AIM, which indicated that the deformation of rubber phase of three layers AIM was benificial to hinder the generation of crack in the process of blends fracture. Morphology analysis of deformation zone of three layers AIM toughening PMMA blends showed that the AIM with BA-St copolymer as interface rubber layer generated evident cavitation, and the AIM with PBA as interface rubber layer arised matrix crazing, which can be attributing to the influence of rubber phase property on toughening mechanism.
2. The influence of rubber phase cross-linking density of AIM on PMMA toughening was studied. It was shown that Kmax, Uprop and Izod impact strength of AIM/PMMA blends reached maximum when appropriate rubber cross-linking density was adopted. Morphology analysis of impact fracture surface showed that deformation mechanism of AIM/PMMA blends was local matrix shear yielding initiated by rubber particles cavitation. The rubber of AIM with appropriate cross-linking density was beneficial to form intensive voids and initiated local shear yielding of PMMA matrix nearby modifiers effectively in impact test.
3. Blends of PMMA, AIM with carboxylic acid group and methyl methacrylate-glycidyl methacrylate-methacrylate copolymer were prepared by melt blending. Maxium torque and equilibrium torque of blends in the process of melt blending increased with the increase of carboxylic acid group content in the shell of AIM increament, and impact strength and Kmax of blends enhanced accordingly, but the optical propertie of blends was not affected. It indicated that the reaction of carboxylic acid group of modifiers and epoxy group of matrix resin increased interfacial cohesion of two phases, which led to not only the cohension increament of mixture melt but also more rubber particles cavitation and promoted massive yielding of maxtrix resins in the process of fracture deformation.
4. Methyl methacrylate-butadiene-styrene copolymers (MBS), which were used as no-whetherable modifiers in PMMA toughening, were synthsized by emulsion polymerization. The variance of diameter of SBR, which was rubber phase of MBS modifiers, with emulsifier content was studied, and result showed that the diameter of SBR particles decreased with the increase of emulsifier content in emulsion polymerization. Three kinds of MBS core-shell modifier, synthesized by seeded-emulsion polymerization by changing St and MMA addition sequence, can disperse uniformly in MS resins. MBS prepared by grafting St and MMA mixture on SBR can strengthen interfacial adhesion between modifiers and matrix, and the blend showed higher notched-Izod impact strength and transmittance. It indicated that better interfacial property highen the mechanical and optical properties.
In this work, on the premise of maintaining PMMA resins outstanding optical properties, the toughening of PMMA was solved successfully. High preformance blends, which transmittance was88.6%and impact strength increased four times than pure PMMA resins, were prepared. The mechanical properties of blends had exceeded general-purpose toughening resins, such as HIPS, and can fulfilled practice demand.
本研究从结构与性能可控的改性剂合成出发,考察了改性剂结构、橡胶相交联程度、改性剂与基体树脂界面性能变化等因素对聚甲基丙烯酸甲酯类树脂的增韧的影响,主要研究内容与结论如下：
1、在丙烯酸酯类冲击改性剂(Acrylic impact modifiers, AIMs)的橡胶相P(BA-co-St)种子乳液聚合的反应恒速期内,考察了聚合反应速率与引发剂浓度之间关系,研究了在种子乳液聚合过程中橡胶相粒子粒径的变化规律。结果表明聚合反应速率与引发剂浓度关系为Rp∞I0.44,橡胶粒子粒径以逐步长大方式增长。合成出了BA-St共聚物为橡胶核,PMMA为外壳的两层结构AIM改性剂与PS或PMMA为内核,PBA或BA-St共聚物为橡胶层,PMMA为外壳的三层结构AIM改性剂。考察了AIM结构对PMMA树脂增韧的影响,结果表明采用两层结构AIM改性剂增韧PMMA时,其最大冲击强度、断裂能与最大应力强度因子(Kmax)所对应的最优AIM橡胶相粒子粒径为269nm,其裂纹增长能(Uprop)在AIM橡胶相粒子粒径为351nm时达到最大,增韧产物的可见光透过率随着橡胶相粒子粒径的增长逐步下降,雾度逐步上升。与两层结构AIM对PMMA的增韧相比较,三层结构AIM的增韧产物的Kmax明显高于两层结构AIM的增韧产物,表明了三层结构改性剂中橡胶相的形变形式更有利于阻止共混物断裂过程中裂纹的产生。通过两种三层结构AIM增韧PMMA的形变区透射电镜观察可见,改性剂中间橡胶层为BA-St共聚物时,橡胶粒子发生了明显的空洞化,而中间层橡胶为PBA时,断裂形变区中可发现银纹的产生,这表明三层结构改性剂的中间橡胶层的性质对增韧机理的影响显著。
2、研究了AIM的橡胶相交联程度对PMMA增韧的影响,结果发现随着橡胶相的交联程度上升,共混物冲击强度呈先上升后下降的趋势,当采用橡胶相交联程度适当的AIM时,共混物冲击强度、Kmax与Uprop达到最大值。共混物冲击断面的形态分析表明其断裂机理为橡胶粒子空洞化引起基体树脂的剪切屈服,适当交联程度的橡胶相在断裂时有利于形成较多的空洞并能够更有效地促进橡胶粒子周围基体树脂的局部剪切屈服。
3、为研究改性剂与基体树脂间界面粘结性能对增韧的影响,将带有羧酸基团的AIM、PMMA与本体法制备的甲基丙烯酸甲酯-甲基丙烯酸环氧丙酯-丙烯酸甲酯三元共聚物熔融共混制备出增韧产物,考察共混过程中共混物转矩值变化与所制得共混物的性能变化,结果显示随着AIM改性剂壳层中羧酸含量的提高,熔融共混过程中的最大转矩值与平衡转矩值逐步提高,共混物的冲击强度与Kmax逐步上升,但光学性能不受影响。这表明了共混过程中改性剂上的羧酸官能团已经与基体树脂中环氧官能团发生了反应,并且随着化学反应程度的上升,两相间的界面粘结性能提高。这不仅使共混物熔体粘度上升,转矩值提高,而且有利于共混物断裂形变过程中更多橡胶粒子发生了空洞化并促进基体树脂更大程度的剪切屈服。
4、采用乳液聚合方法合成了甲基丙烯酸甲酯-丁二烯-苯乙烯核壳结构接枝共聚物(MBS)作为聚甲基丙烯酸甲酯类树脂的非耐候级改性剂,研究了MBS中丁苯橡胶(SBR)粒子粒径随着乳液聚合中乳化剂用量变化的规律,考察了在SBR粒子上St与MMA的不同接枝方式制备的三种MBS与甲基丙烯酸甲酯-苯乙烯共聚物(MS)的界面粘结力变化对其增韧产物性能的影响。结果表明：SBR粒子粒径随乳液聚合中乳化剂用量上升而下降；三种MBS改性剂都能够在MS树脂中均匀分散,其中采用混合MMA与St的接枝方式制备的MBS壳层为St与MMA的无规共聚物,这种改性剂与MS熔融共混过程中平衡转矩值最高,共混物冲击强度最大,透光性能最好。而MMA与St按照不同先后顺序接枝在SBR上制备出的MBS,其壳层为接枝在SBR粒子上的MMA与St均聚物,这种改性剂对MS树脂的增韧效果较差,共混物透光性能较低。这表明了MBS与MS间良好的界面性能有助于共混物性能的提高。
本工作在保持聚甲基丙烯酸甲酯类树脂优异透光性能的前提下,成功地解决了其增韧问题,制备出透过率为88.6%,冲击强度较纯PMMA树脂提高了4倍的增韧产物,该材料的力学性能已超过HIPS等通用增韧树脂,能够满足实用要求。
Polymethyl methacrylate (PMMA) resins usually comprise the polymethyl methacrylate homopolymer and the compolymers containing predominantly methyl methacrylate but with small amounts of methyl or ethyl acrylate, acrylonitrile or styrene comonomers added for improved toughness. PMMA resins are rigid, amorphous polymers particularly noted for their exceptional clarity and UV resistance, and therefore wildly used for making household appliances, electronic products, medical devices and automobile, etc. Due to the poor toughness and notch sensitivity, the research on toughening receives much concern, in which adopting core-shell modifiers toughening PMMA resins is one of the most important method. The strategy of PMMA resins toughened by core-shell modifiers show more complexity than other amorphous polymer, which demands modifiers not only promote more fracture energy absorption in the process of toughened blends fracture, which highen the mechanical properties, but refractive index of modifiers match with PMMA resins to maintain better optical property of matrix resins. Both weatherable modifiers with polybutyl acrylate (PBA) rubber phase and non-weatherable modifier with polybutadiene (PB) rubber phase can toughen PMMA resins effectively, but transmittance of blends decreases markly for mismatch of refractive index of PBA and PB with PMMA resins. So combined St with PBA or PB to match refractive index of modifiers with matrix resins can prepare toughening blends with high light transmittance.
In this paper, preformed modifiers with controllable structure and proterties were synthesized. The influence of modifiers structure, cross-linking density of rubber phase, and the variance of interface property between modifiers and matrix on PMMA resins toughening were investigated. The main research works and conclusions are as follows:
1. The relationship between reaction rate and initior concentration was investigated in the process of constant rate period of P(BA-co-St) emulsion polymerization, and the results showed that the relationship of reaction rate and initior concentration was Rp∞I0.44. The diameter of P(BA-co-St) rubber particles increased according to grow-out manner. Two layers acrylic impact modifiers (AIM), which was composed of BA-St copolymer rubber core and PMMA outer shell, and three layer modifiers with PS or PMMA inner core, BA or BA-St copolymer interface layer and PMMA external shell were synthsized by emulsion polymerization. The influence of AIM structure on PMMA toughess was investigated, and results showed that the optimum diameter of rubber particle of two layers AIMs was269nm, which led to maxium impact strength, fracture energy and stress intensity factor (Kmax) of AIM/PMMA blends, and crack propagating energy (Uprop) reached maxium when rubber particle diameter of AIM was351nm. The transmittance of blends decreased with the increament of rubber particles diameter, whereas the haze increased. The blends with three layers AIM had higher Kmax than those blends with two layers AIM, which indicated that the deformation of rubber phase of three layers AIM was benificial to hinder the generation of crack in the process of blends fracture. Morphology analysis of deformation zone of three layers AIM toughening PMMA blends showed that the AIM with BA-St copolymer as interface rubber layer generated evident cavitation, and the AIM with PBA as interface rubber layer arised matrix crazing, which can be attributing to the influence of rubber phase property on toughening mechanism.
2. The influence of rubber phase cross-linking density of AIM on PMMA toughening was studied. It was shown that Kmax, Uprop and Izod impact strength of AIM/PMMA blends reached maximum when appropriate rubber cross-linking density was adopted. Morphology analysis of impact fracture surface showed that deformation mechanism of AIM/PMMA blends was local matrix shear yielding initiated by rubber particles cavitation. The rubber of AIM with appropriate cross-linking density was beneficial to form intensive voids and initiated local shear yielding of PMMA matrix nearby modifiers effectively in impact test.
3. Blends of PMMA, AIM with carboxylic acid group and methyl methacrylate-glycidyl methacrylate-methacrylate copolymer were prepared by melt blending. Maxium torque and equilibrium torque of blends in the process of melt blending increased with the increase of carboxylic acid group content in the shell of AIM increament, and impact strength and Kmax of blends enhanced accordingly, but the optical propertie of blends was not affected. It indicated that the reaction of carboxylic acid group of modifiers and epoxy group of matrix resin increased interfacial cohesion of two phases, which led to not only the cohension increament of mixture melt but also more rubber particles cavitation and promoted massive yielding of maxtrix resins in the process of fracture deformation.
4. Methyl methacrylate-butadiene-styrene copolymers (MBS), which were used as no-whetherable modifiers in PMMA toughening, were synthsized by emulsion polymerization. The variance of diameter of SBR, which was rubber phase of MBS modifiers, with emulsifier content was studied, and result showed that the diameter of SBR particles decreased with the increase of emulsifier content in emulsion polymerization. Three kinds of MBS core-shell modifier, synthesized by seeded-emulsion polymerization by changing St and MMA addition sequence, can disperse uniformly in MS resins. MBS prepared by grafting St and MMA mixture on SBR can strengthen interfacial adhesion between modifiers and matrix, and the blend showed higher notched-Izod impact strength and transmittance. It indicated that better interfacial property highen the mechanical and optical properties.
In this work, on the premise of maintaining PMMA resins outstanding optical properties, the toughening of PMMA was solved successfully. High preformance blends, which transmittance was88.6%and impact strength increased four times than pure PMMA resins, were prepared. The mechanical properties of blends had exceeded general-purpose toughening resins, such as HIPS, and can fulfilled practice demand.
引文
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