PVC的工程化技术研究
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摘要
本文在查阅、分析大量的有关通用塑料工程化技术、聚合物基纳米复合材料、PVC结晶、PVC共混改性、PVC与纳米CaCO_3复合改性等资料的基础上,提出了用结晶PVC微粉自增塑、自增韧增强PVC提高PVC的加工性能、力学性能和耐热性,并通过受限原位复合方法制备PVC/纳米CaCO_3复合材料来实现PVC的工程化。通过结晶改性、PA6共混复合及原位复合纳米CaCO_3填充等技术对PVC的工程化进行了研究,分析了共混工艺、结晶条件、原位复合等条件下改性PVC复合材料的结构、组成与性能的关系,获得了以下研究成果:
1.PA6与SMA在苯酚溶液中反应,可将SMA接枝到PA6分子链上。当反应物中SMA用量为60%,在100℃下反应时间8hr,接枝率最大为5.12%。PA6-g-SMA的熔点随其接枝率的升高而降低,当接枝率为5.12%时,熔点197.0℃。PA6-g-SMA能与PVC熔融共混,解决了PA6与PVC不能熔融加工的难题。
2.PA6-g-SMA对PVC有增韧增强作用。当PA6-SMA接枝率为5.12%,添加量为15%时,共混物的冲击强度为64.7kJ/m~2,为基体树脂的161.7%;拉伸强度为55MPa,为基体树脂的148.6%。PVC/PA6-g-SMA共混物中有共晶生成。说明PA6-g-SMA能作为PVC的异相成核剂诱使无规PVC分子链结晶。
3.以PA6-g-SMA作为PVC的异相成核剂,在适当的热处理条件下,可以诱导无规PVC结晶。当PA6-g-SMA用量为PVC原料的2%,在110℃下处理2小时,PVC结晶度最高达到了30.4%。
4.使用改进的重力加料式流化床对撞式气流粉碎机对结晶PVC进行粉碎,制备了结晶PVC微粉,且产率较大。结晶PVC微粉内的晶粒尺寸约78nm,熔点为128℃。其形成机理可以用晶区碰撞破碎机理和晶片剪切滑移机理来解释。
5.结晶PVC微粉对PVC具有较强的自增塑、自增韧增强作用,也具有提高PVC耐热性的作用。在PVC微粉添加量为10%时,结晶PVC微粉/PVC复合材料的玻璃化温度达到了90℃,冲击强度达到为70.3kJ/m~2;在结晶PVC微粉用量为5%时,拉伸强度达到57.3MPa。自增塑机理可用结晶PVC微粉晶粒解缠状态及速度梯度解释,其自增韧增强机理及提高耐热性机理可用PVC晶核异相作用解释。
Based on the reviews with plenty of references about the engineering technology of general plastics, nanoparticles/polymer composites, the crystallization behavior of poly(vinyl chloride)(PVC), modifying PVC by the way of blending with another polymer and mixing with nanometer CaCO_3 (nanoCaCO_3) , the new idea that engineering PVC materials may be prepared because of the effect of self-plasticization, self-toughening and self-reinforcement of nanocrystalline PVC on PVC is raised. Other new idea that high performance PVC/nanoCaCO_3 composites may be prepared through in-situ preparing nanoCaCO_3 is also raised. The three engineering technology of modifying by crystallization, blending with polyamide 6(PA6) grafted styrene-maleic anhydride (SMA) (PA6-g-SMA) and compositing with in situ prepared nanoCaCO_3 were studied respectively. The structure, morphology, composition and properties of modified PVC compounds and composites were investigated systematically. The main results obtained can be summarized in 15 parts as follow:(1) SMA can be grafted to molecular chain of PA6 by reaction between PA6 and SMA in phenol solution. The maximal grafting ratio of PA6-g-SMA can reach 5.12% when PA6 are reacted with 60% SMA for 8 hour at 100℃.The melting point of PA6-g-SMA decrease when it's grafting ratio increase. The melting point of PA6-g-SMA with 5.12% grafting ratio is 197℃. PA6-g-SMA can mix with PVC at 185℃ to prepare PVC/PA6-g-SMA compounds, it is said that, the problem of no way of PVC mixing with PA6 is solved.(2) PA6-g-SMA can toughen and reinforce PVC. The impact strength of PVC/PA6-g-SMA compound can reach 64.7kJ/m~2, which is 61.7% higher than that of pure PVC when the use level of PA6-g-SMA whose grafting ratio is 5.12% is 15%. The tensile strength of above mentioned materials can reach 55.0MPa, about 48.6% higher than that of pure PVC. Cocrystalline can found in PVC/PA6-g-SMA materials, it is suggested that PA6-g-SMA can used as nucleating agent of PVC and induce PVC crystallize.(3) After appropriate heat treated, unregulated PVC can crystallize when modified nylon uses as out-of-phase nucleating agent. The maximal crystallinity of PVC reaches 30.4% when raw PVC mixed with 2% modified nylon and heated for 2hr at 110℃.(4) Crystalline PVC can be crashed by improved flow clash crashing machine to prepare crystalline PVC micro powder effectively. The grain size of nanocrystalline in crystalline PVC micro powder is 80 nm. The melting point of nanocrystalline PVC is 128℃. The mechanism and
decisive factor of forming nanocrystalline PVC can be simulated by the crashing broken principle schematic plan of crystalline region model and shearing slip principle schematic plan of crystal plate model.(5) Nanocrystalline PVC has obvious effect of self-plasticization, self-toughen and self-reinforcement on PVC. Nanocrystalline PVC can also improve the heat-resisting property of PVC. The impact strength of PVC/nanocrystalline PVC materials can reach 70.3kJ/m2, at the same time;the glass transition temperate of the composite can reach 90 °C when 10% nanocrystalline PVC are dispersed to PVC matrix. The tensile strength of PVC/nanocrystalline PVC composite can reach 57.3MPa when 5% nanocrystalline PVC are dispersed to PVC matrix. The mechanism and decisive factor of self-plasticization can be simulated by being relieving from wrapping model and inducing molecular to relief from wrapping through generating velocity gradient model. The mechanism and decisive factor of self-toughen but self-reinforcement also improving the heat-resisting property of PVC can be simulated by out-of-phase nucleating of crystal nucleus model.(6) Microporous PVC with pore size of 0.2-2micron can be obtained by foaming of suspension PVC powders using the solution of 2, 2'-azo-bis-iso-butyronitrile in butanone when heated in 112°C oil bath for 8min. The pore of microporous PVC can be used as reactors to in-situ restricted prepare nanoCaCO3(7) It is found that macromolecular surface-activator and chelating agent of citric acid play a key role in the formation of CaCO3 nanoparticles through affecting the yield and particle size of in-situ prepared nanoCaCO3 The maximal yield can reach 10% when 18% Ca(OH)2, 0.18% macromolecular surface-activator and 0.5% citric acid are used and CO2 aerates for 15min at the velocity of 0.25L/min.(8) It is found that in-situ nanoCaCC>3 has obvious effect of toughen and reinforcement on PVC and can also increase the glass transition temperate of PVC. The impact strength of PVC/in-situ nanoCaC03 composites can reach 90.6kJ/m2, which is 93% higher than that of pure PVC when 5% in-situ nanoCaCO3 are dispersed to PVC matrix. The tensile strength of above mentioned PVC/in-situ nanoCaC03 composites can reach 70.2 MPa, which is 63% higher than that of pure PVC. The glass transition temperate of above mentioned PVC/in-situ nanoCaCO3 composites can reach 89.4°C.(9) It is found that in-situ nanoCaCO3 and nanocrystalline PVC have obvious synergistic effect of toughen and reinforcement on PVC and can also increase the glass transition temperate
of PVC. The impact strength of nanocrystalline PVC/PVC/in-situ nanoCaC03 composites can reach 96.5kJ/m2, which is 105% higher than that of pure PVC when 10% nanocrystalline PVC and 5% in-situ nanoCaCO3 are dispersed to PVC matrix. The tensile strength of above mentioned nanocrystalline PVC/PVC/in-situ nanoCaC03 composites can reach 95.0 MPa, which is 121% higher than that of pure PVC. The glass transition temperature of above mentioned nanocrystalline PVC/PVC/in-situ nanoCaC03 composites can reach 105.68 °C(10) PVC plastics can be used as sectional material and tubular product when PVC is modified by both nanocrystalline PVC and in-situ nanoCaCO3 The maximal impact strength of PVC sectional material can reach 85kJ/m2;its maximal tensile strength can reach 78MPa when 10% nanocrystalline PVC and 5% in-situ nanoCaC03 are dispersed to PVC matrix. The maximal impact strength of tubular product material can reach 83kJ/m2;its maximal tensile strength can reach 75MPa when 10% nanocrystalline PVC and 5% in-situ nanoCaCO3 are dispersed to PVC matrix. The vicat softening point of sectional material and tubular product can reach 110 °C.
1.PA6与SMA在苯酚溶液中反应,可将SMA接枝到PA6分子链上。当反应物中SMA用量为60%,在100℃下反应时间8hr,接枝率最大为5.12%。PA6-g-SMA的熔点随其接枝率的升高而降低,当接枝率为5.12%时,熔点197.0℃。PA6-g-SMA能与PVC熔融共混,解决了PA6与PVC不能熔融加工的难题。
2.PA6-g-SMA对PVC有增韧增强作用。当PA6-SMA接枝率为5.12%,添加量为15%时,共混物的冲击强度为64.7kJ/m~2,为基体树脂的161.7%;拉伸强度为55MPa,为基体树脂的148.6%。PVC/PA6-g-SMA共混物中有共晶生成。说明PA6-g-SMA能作为PVC的异相成核剂诱使无规PVC分子链结晶。
3.以PA6-g-SMA作为PVC的异相成核剂,在适当的热处理条件下,可以诱导无规PVC结晶。当PA6-g-SMA用量为PVC原料的2%,在110℃下处理2小时,PVC结晶度最高达到了30.4%。
4.使用改进的重力加料式流化床对撞式气流粉碎机对结晶PVC进行粉碎,制备了结晶PVC微粉,且产率较大。结晶PVC微粉内的晶粒尺寸约78nm,熔点为128℃。其形成机理可以用晶区碰撞破碎机理和晶片剪切滑移机理来解释。
5.结晶PVC微粉对PVC具有较强的自增塑、自增韧增强作用,也具有提高PVC耐热性的作用。在PVC微粉添加量为10%时,结晶PVC微粉/PVC复合材料的玻璃化温度达到了90℃,冲击强度达到为70.3kJ/m~2;在结晶PVC微粉用量为5%时,拉伸强度达到57.3MPa。自增塑机理可用结晶PVC微粉晶粒解缠状态及速度梯度解释,其自增韧增强机理及提高耐热性机理可用PVC晶核异相作用解释。
Based on the reviews with plenty of references about the engineering technology of general plastics, nanoparticles/polymer composites, the crystallization behavior of poly(vinyl chloride)(PVC), modifying PVC by the way of blending with another polymer and mixing with nanometer CaCO_3 (nanoCaCO_3) , the new idea that engineering PVC materials may be prepared because of the effect of self-plasticization, self-toughening and self-reinforcement of nanocrystalline PVC on PVC is raised. Other new idea that high performance PVC/nanoCaCO_3 composites may be prepared through in-situ preparing nanoCaCO_3 is also raised. The three engineering technology of modifying by crystallization, blending with polyamide 6(PA6) grafted styrene-maleic anhydride (SMA) (PA6-g-SMA) and compositing with in situ prepared nanoCaCO_3 were studied respectively. The structure, morphology, composition and properties of modified PVC compounds and composites were investigated systematically. The main results obtained can be summarized in 15 parts as follow:(1) SMA can be grafted to molecular chain of PA6 by reaction between PA6 and SMA in phenol solution. The maximal grafting ratio of PA6-g-SMA can reach 5.12% when PA6 are reacted with 60% SMA for 8 hour at 100℃.The melting point of PA6-g-SMA decrease when it's grafting ratio increase. The melting point of PA6-g-SMA with 5.12% grafting ratio is 197℃. PA6-g-SMA can mix with PVC at 185℃ to prepare PVC/PA6-g-SMA compounds, it is said that, the problem of no way of PVC mixing with PA6 is solved.(2) PA6-g-SMA can toughen and reinforce PVC. The impact strength of PVC/PA6-g-SMA compound can reach 64.7kJ/m~2, which is 61.7% higher than that of pure PVC when the use level of PA6-g-SMA whose grafting ratio is 5.12% is 15%. The tensile strength of above mentioned materials can reach 55.0MPa, about 48.6% higher than that of pure PVC. Cocrystalline can found in PVC/PA6-g-SMA materials, it is suggested that PA6-g-SMA can used as nucleating agent of PVC and induce PVC crystallize.(3) After appropriate heat treated, unregulated PVC can crystallize when modified nylon uses as out-of-phase nucleating agent. The maximal crystallinity of PVC reaches 30.4% when raw PVC mixed with 2% modified nylon and heated for 2hr at 110℃.(4) Crystalline PVC can be crashed by improved flow clash crashing machine to prepare crystalline PVC micro powder effectively. The grain size of nanocrystalline in crystalline PVC micro powder is 80 nm. The melting point of nanocrystalline PVC is 128℃. The mechanism and
decisive factor of forming nanocrystalline PVC can be simulated by the crashing broken principle schematic plan of crystalline region model and shearing slip principle schematic plan of crystal plate model.(5) Nanocrystalline PVC has obvious effect of self-plasticization, self-toughen and self-reinforcement on PVC. Nanocrystalline PVC can also improve the heat-resisting property of PVC. The impact strength of PVC/nanocrystalline PVC materials can reach 70.3kJ/m2, at the same time;the glass transition temperate of the composite can reach 90 °C when 10% nanocrystalline PVC are dispersed to PVC matrix. The tensile strength of PVC/nanocrystalline PVC composite can reach 57.3MPa when 5% nanocrystalline PVC are dispersed to PVC matrix. The mechanism and decisive factor of self-plasticization can be simulated by being relieving from wrapping model and inducing molecular to relief from wrapping through generating velocity gradient model. The mechanism and decisive factor of self-toughen but self-reinforcement also improving the heat-resisting property of PVC can be simulated by out-of-phase nucleating of crystal nucleus model.(6) Microporous PVC with pore size of 0.2-2micron can be obtained by foaming of suspension PVC powders using the solution of 2, 2'-azo-bis-iso-butyronitrile in butanone when heated in 112°C oil bath for 8min. The pore of microporous PVC can be used as reactors to in-situ restricted prepare nanoCaCO3(7) It is found that macromolecular surface-activator and chelating agent of citric acid play a key role in the formation of CaCO3 nanoparticles through affecting the yield and particle size of in-situ prepared nanoCaCO3 The maximal yield can reach 10% when 18% Ca(OH)2, 0.18% macromolecular surface-activator and 0.5% citric acid are used and CO2 aerates for 15min at the velocity of 0.25L/min.(8) It is found that in-situ nanoCaCC>3 has obvious effect of toughen and reinforcement on PVC and can also increase the glass transition temperate of PVC. The impact strength of PVC/in-situ nanoCaC03 composites can reach 90.6kJ/m2, which is 93% higher than that of pure PVC when 5% in-situ nanoCaCO3 are dispersed to PVC matrix. The tensile strength of above mentioned PVC/in-situ nanoCaC03 composites can reach 70.2 MPa, which is 63% higher than that of pure PVC. The glass transition temperate of above mentioned PVC/in-situ nanoCaCO3 composites can reach 89.4°C.(9) It is found that in-situ nanoCaCO3 and nanocrystalline PVC have obvious synergistic effect of toughen and reinforcement on PVC and can also increase the glass transition temperate
of PVC. The impact strength of nanocrystalline PVC/PVC/in-situ nanoCaC03 composites can reach 96.5kJ/m2, which is 105% higher than that of pure PVC when 10% nanocrystalline PVC and 5% in-situ nanoCaCO3 are dispersed to PVC matrix. The tensile strength of above mentioned nanocrystalline PVC/PVC/in-situ nanoCaC03 composites can reach 95.0 MPa, which is 121% higher than that of pure PVC. The glass transition temperature of above mentioned nanocrystalline PVC/PVC/in-situ nanoCaC03 composites can reach 105.68 °C(10) PVC plastics can be used as sectional material and tubular product when PVC is modified by both nanocrystalline PVC and in-situ nanoCaCO3 The maximal impact strength of PVC sectional material can reach 85kJ/m2;its maximal tensile strength can reach 78MPa when 10% nanocrystalline PVC and 5% in-situ nanoCaC03 are dispersed to PVC matrix. The maximal impact strength of tubular product material can reach 83kJ/m2;its maximal tensile strength can reach 75MPa when 10% nanocrystalline PVC and 5% in-situ nanoCaCO3 are dispersed to PVC matrix. The vicat softening point of sectional material and tubular product can reach 110 °C.
引文
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