过氧化二异丙苯交联聚乙烯的制备及研究
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摘要
聚乙烯(PE)是五大通用塑料之一,具有优良的电绝缘性、耐低温性、易加工成型和足够的力学性能,以及优异的化学稳定性和介电性能,已被广泛应用于制作薄膜、泡沫制品、管材、电线电缆绝缘料等,其产量和用量居各合成树脂之首。但是PE的熔点低,易蠕变、耐热性较差等,大大限制了它的应用范围,因此对其进行改性一直是PE应用和理论研究的重要课题。对PE进行交联改性可以明显提高PE的拉伸强度、冲击强度、抗蠕变性及耐热性能等,而又几乎不损坏原有的其他性能。
本文选择过氧化二异丙苯(DCP)作为交联剂,在低于PE熔点的温度下,采取扩散的方法使DCP均匀扩散进入PE切片内部,并在160℃以上使PE发生交联反应,制备了交联PE。具体来说,主要开展了以下几个方面的工作:
1.采用搅拌共混法,在80℃下使DCP扩散进入PE切片内部。通过DSC测试,分析了扩散时间与DCP分解放热量之间的关系。采用菲克扩散模型描述了DCP在PE的扩散过程,揭示了DCP在PE中的扩散过程符合零级扩散方程。
2.通过DSC测试方法对DCP在PE切片内部的热分解过程进行研究,应用Arrhenius方程描述了DCP在PE切片内部的热分解反应动力学,确定了DCP在PE中的热分解按一级反应动力学进行,计算了反应动力学参数,频率因子lnA约为35～40,表观活化能E约为150～160 KJ/mol。根据等温条件下反应程度与时间的关系,得出可通过调节DCP组分含量及温度范围控制DCP交联PE反应的方法。
3.采用DSC测试方法对交联PE的非等温结晶行为和结晶动力学进行了研究。结果表明,交联PE的结晶温度明显降低,Avrami指数n介于3.2～4.2之间,说明纯PE和交联PE的结晶过程可能同时存在均相成核和异相成核,并且随着DCP含量的增加而增加,交联PE的结晶速率常数Z_c明显大于纯PE,与n呈相同变化趋势。
4.DCP交联反应在PE分子链之间形成了化学交联点,对PE及交联PE进行DMA测试的结果表明,DCP的交联作用使交联PE的储能模量有所提高,样品的α松弛峰移向低温,并且峰形变宽,说明PE晶相中的运动单元趋于多元化,晶体结构的规整性受到破坏。DSC测试表明,经DCP交联后的PE样品的熔点和熔融热呈有规律的降低,说明DCP的交联阻碍了PE大分子链有序堆切,使结晶程度降低。
Polyethylene(PE) is one of the five general plastics,which shows excellent electric insulation,low temperature tolerance,easy processing. PE has been the most widely used plastics in(?)hin film,foam,pipe material,insulated material and etc.However,PE has some disadvantages,i.e.,low melting point,poor creep behavior,which greatly limit its application.Recently,proper modifications of PE attract great attention in both application and theoretical studies.Crosslinkage of PE will improve its tensile strength,impact strength,anticreepy property,high temperature resistance and etc.with little effect on its original capabilities.Therefore,the study on the crosslink modification of PE has particular important significance.In this work,dicumyl peroxide(DCP) was chosen as a crosslinker and the diffusion of DCP into the PE chip at the temperature below the PE melting point has been studied.The crosslinking process of PE intiated by DCP was carried under the temperature above 160℃.Generally,the work of this thesis is summarized as follows:
1.Blending method was used to make DCP diffuse into PE chips.The same DCP/PE ratio samples with various diffusion times were prepared.The results of differential scanning calorimetry(DSC) characterization showed that the amount of DCP diffused into PE chips increased with the increase of time.The Fick model was adopted to theoretically describe the DCP diffusion process,showing that the diffusion process in this work is accord with zero-order diffusion equation.
2.The thermal decomposition process of DCP inside PE was studied by DSC.Arrhenius equation was used to depict the thermal decomposition kinetics and the results manifested that the decomposition accord with first-order reaction kinetics.Frequency factor(lnA) was about 35-40 and the apparent activation energy(E) was about 150-160 kJ/mol.According to the relationship between reaction degree and reaction time,a method to control the reaction process of DCP crosslink PE was also proposed.
3.DSC characterization was applied to study the non-isothermal crystallization kinetics and crystal behavior of DCP crosslinked PE. The results showed that crystallization rate of modified PE significantly decreased.Avrami index(n) is between 3.2 and 4.2, implying the coexistence of homogeneous nucleation and heterogeneous nucleation during the crystallization process in pure PE and crosslinked PE.The constant of crystallization rate(Z_c) is larger than that of pure PE and the same trend of n was also observed.
4.The results of dynamic mechanical analysis(DMA) measurement indicated that storage modulus of crosslinked FE was larger than that of pure PE.Theαrelaxation peak shifted towards lower temperature and the peak profile became wide,indicating that the addition of DCP lead to the multiple movement of PE chains and destruction of its crystal regularity.Furthermore,the decrease tendencies of the melting point and melting enthalpy of PE/DCP illustrated that the crosslink effect brought by DCP did hinder the arrangement of PE molecules into the crystal lattice,thus decreased the matrix crystallinity.
本文选择过氧化二异丙苯(DCP)作为交联剂,在低于PE熔点的温度下,采取扩散的方法使DCP均匀扩散进入PE切片内部,并在160℃以上使PE发生交联反应,制备了交联PE。具体来说,主要开展了以下几个方面的工作:
1.采用搅拌共混法,在80℃下使DCP扩散进入PE切片内部。通过DSC测试,分析了扩散时间与DCP分解放热量之间的关系。采用菲克扩散模型描述了DCP在PE的扩散过程,揭示了DCP在PE中的扩散过程符合零级扩散方程。
2.通过DSC测试方法对DCP在PE切片内部的热分解过程进行研究,应用Arrhenius方程描述了DCP在PE切片内部的热分解反应动力学,确定了DCP在PE中的热分解按一级反应动力学进行,计算了反应动力学参数,频率因子lnA约为35～40,表观活化能E约为150～160 KJ/mol。根据等温条件下反应程度与时间的关系,得出可通过调节DCP组分含量及温度范围控制DCP交联PE反应的方法。
3.采用DSC测试方法对交联PE的非等温结晶行为和结晶动力学进行了研究。结果表明,交联PE的结晶温度明显降低,Avrami指数n介于3.2～4.2之间,说明纯PE和交联PE的结晶过程可能同时存在均相成核和异相成核,并且随着DCP含量的增加而增加,交联PE的结晶速率常数Z_c明显大于纯PE,与n呈相同变化趋势。
4.DCP交联反应在PE分子链之间形成了化学交联点,对PE及交联PE进行DMA测试的结果表明,DCP的交联作用使交联PE的储能模量有所提高,样品的α松弛峰移向低温,并且峰形变宽,说明PE晶相中的运动单元趋于多元化,晶体结构的规整性受到破坏。DSC测试表明,经DCP交联后的PE样品的熔点和熔融热呈有规律的降低,说明DCP的交联阻碍了PE大分子链有序堆切,使结晶程度降低。
Polyethylene(PE) is one of the five general plastics,which shows excellent electric insulation,low temperature tolerance,easy processing. PE has been the most widely used plastics in(?)hin film,foam,pipe material,insulated material and etc.However,PE has some disadvantages,i.e.,low melting point,poor creep behavior,which greatly limit its application.Recently,proper modifications of PE attract great attention in both application and theoretical studies.Crosslinkage of PE will improve its tensile strength,impact strength,anticreepy property,high temperature resistance and etc.with little effect on its original capabilities.Therefore,the study on the crosslink modification of PE has particular important significance.In this work,dicumyl peroxide(DCP) was chosen as a crosslinker and the diffusion of DCP into the PE chip at the temperature below the PE melting point has been studied.The crosslinking process of PE intiated by DCP was carried under the temperature above 160℃.Generally,the work of this thesis is summarized as follows:
1.Blending method was used to make DCP diffuse into PE chips.The same DCP/PE ratio samples with various diffusion times were prepared.The results of differential scanning calorimetry(DSC) characterization showed that the amount of DCP diffused into PE chips increased with the increase of time.The Fick model was adopted to theoretically describe the DCP diffusion process,showing that the diffusion process in this work is accord with zero-order diffusion equation.
2.The thermal decomposition process of DCP inside PE was studied by DSC.Arrhenius equation was used to depict the thermal decomposition kinetics and the results manifested that the decomposition accord with first-order reaction kinetics.Frequency factor(lnA) was about 35-40 and the apparent activation energy(E) was about 150-160 kJ/mol.According to the relationship between reaction degree and reaction time,a method to control the reaction process of DCP crosslink PE was also proposed.
3.DSC characterization was applied to study the non-isothermal crystallization kinetics and crystal behavior of DCP crosslinked PE. The results showed that crystallization rate of modified PE significantly decreased.Avrami index(n) is between 3.2 and 4.2, implying the coexistence of homogeneous nucleation and heterogeneous nucleation during the crystallization process in pure PE and crosslinked PE.The constant of crystallization rate(Z_c) is larger than that of pure PE and the same trend of n was also observed.
4.The results of dynamic mechanical analysis(DMA) measurement indicated that storage modulus of crosslinked FE was larger than that of pure PE.Theαrelaxation peak shifted towards lower temperature and the peak profile became wide,indicating that the addition of DCP lead to the multiple movement of PE chains and destruction of its crystal regularity.Furthermore,the decrease tendencies of the melting point and melting enthalpy of PE/DCP illustrated that the crosslink effect brought by DCP did hinder the arrangement of PE molecules into the crystal lattice,thus decreased the matrix crystallinity.
引文
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