超高分子量聚乙烯的流变行为及其在材料加工中的应用
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摘要
聚合物的流变性质决定了其加工性能,研究UHMWPE的流变行为,对制备性能优良的UHMWPE材料具有指导意义。本文系统的研究了UHMWPE的稀溶液、浓溶液及本体的在全浓度范围内的流变行为,得到UHMWPE长链分子缠结形态、粘度与剪切速率、温度、聚合物浓度等之间的关系,探讨适用于常规双螺杆挤出机的UHMWPE加工条件,并在此基础上制备了具有生物活性的UHMWPE/OCP(磷酸八钙)复合材料。同时本文提出利用亚稳性现象加工UHMWPE的新方法,并研究其加工工艺,实现在低温低压下加工制得高性能UHMWPE制品,为解决UHMWPE加工困难问题开辟了新的思路。
本文采用粘度法表征了UHMWPE液体石蜡稀溶液中临界缠结浓度与聚合度之间的关系,得到方程式。UHMWPE液体石蜡溶液凝胶中,UHMWPE分子链为单链多晶形态,随着溶液凝胶浓度的降低,凝胶中UHMWPE片晶晶粒更细小。UHMWPE液体石蜡凝胶凝胶点温度随着浓度的升高而升高,凝胶点温度Cc rNC cr? N1/2 =94Tg el与凝胶质量浓度C m之间的关系式为:Tg el = 0.32C m+ 110.4(0.8%≤≤8%) ;(10%≤≤40%);CmTg el = 31.9 Cm+ 115.1C mTg el = 24.5 Cm+ 113.2( Cm≥45%)。
UHMWPE液体石蜡凝胶是假塑性凝胶,在165℃时充分熔融,凝胶中UHMWPE分子链形成熔融充分的呈高斯分布的线团,具有较高的弹性模量和较低的损耗模量。温度在165℃时以上,剪切速率-粘度曲线在低剪切速率区域出现一个平台,然后随剪切速率的增加而下降,且温度高的凝胶的粘度平台区更宽。液体石蜡的溶胀作用可以有效地减小UHMWPE的粘度,不同浓度下的UHMWPE液体石蜡凝胶的粘度与剪切频率之间为幂律方程关系。凝胶粘度对温度及对浓度的敏感性均比其对剪切速率的敏感性更为显著。
UHMWPE本体的粘度-剪切速率关系符合幂律方程,可以用方程式η= kγα来描述。UHMWPE分子量在250万-600万之间时,分子量对UHMWPE的流变行为影响不大,但分子量高的UHMWPE比分子量低的UHMWPE的粘度随剪切频率的增加而下降的幅度要大,其流变行为对温度更为敏感。当温度升高至185℃时,UHMWPE分子链内部的结晶消失,相互贯穿的分子链到达网络缠结点密度的最高点,分子形态呈无规线团状。当温度升高到225℃以上时,分子链间缠绕与解缠绕达到动态平衡,粘度基本不再变化。粘均分子量为3.5×106g/mol的UHMWPE柱塞挤出过程中,在154℃-157℃的“温度窗口”中,出现亚稳性现象,表现为挤出压力出现突降并稳定下来,挤出棒材表面光滑,不出现熔体破裂现象。实现了低温低压下柱塞挤出成型加工UHMWPE,使得不需改进设备,采用传统的柱塞挤出机挤出成型UHMWPE成为现实,且显著降低了生产中所需能耗。
控制螺杆转速40N/min;温度165℃,可在常规双螺杆挤出机上实现50%的UHMWPE液体石蜡凝胶的顺利挤出。通过UHMWPE和OCP纤维在双螺杆挤出机上溶胀共混挤出制备的UHMWPE/OCP复合材料在OCP纤维质量分数为25%时具有较为优异的力学性能,该复合材料在仿生条件下可诱发表面类骨磷灰石层的生成。UHMWPE经丙烯酸改性后,表面含有大量活性基团,可用于原位化学合成UHMWPE/CaCO3复合材料。原位化学合成法制备的UHMWPE/CaCO3复合材料比纯UHMWPE以及机械共混法制备的复合材料具有更佳的拉伸强度和耐热变形温度。用该法制得的CaCO3含量为9.5%的UHMWPE/CaCO3复合材料的拉伸强度可达到43.8MPa,耐热变形温度可高达106℃。
Polymer processability depends on its rheological behavior. To improve the processability of ultrahigh molecular weight (UHMWPE), the rheological behaviors of UHMWPE, including dilute solution, concentrated solution, gel, and melt, were studied. The relationships of the entanglement state of UHMWPE long chains, viscosity, shear rate, temperature, polymer concentrations were obtained. The suitable processing parameters for ram extrusion of UHMWPE rod and twin screw extrusion of UHMWPE/octacalcium phosphate composite were explored using the theoretical results. A metastable phenomenon was observed during the ram extrusion of UHMWPE, and a low temperature and low pressure processing method was developed to solve the difficulties in processing UHMWPE. A bioactive UHMWPE/OCP composite was processed using twin screw extrusion of the UHMWPE gel. A heat resistant and high strength composite of UHMWPE and calcium carbonate was processed by in situ synthesis.
The relationship between the critical entanglement concentration (Ccr) of UHMWPE dilute solution in paraffin oil and the degree of polymerization (N) was obtained by measuring the viscosity, . UHMWPE gel in the paraffin oil exhibits a single chain with polycrystalline forms. The UHMWPE lamellar crystal size becomes smaller with the decrease of the gel concentration. The UHMWPE/paraffin oil gel point (TC cr? N1/2 =94gel) increases with the mass concentration of UHMWPE (Cm), Tg el = 0.32C m+ 110.4(0.8%≤≤8%), (10%≤≤40%), CmTg el = 31.9 Cm+ 115.1C mTg el = 24.5 Cm+ 113.2( Cm≥45%).
UHMWPE/paraffin oil gel is a pseudoplastic gel. When the gel melts sufficiently at 165℃, UHMWPE chains in the melt state exhibit as Gaussian distributed coils with higher storage modulus and lower loss modulus. At temperature above 165℃, a plateau appears in the low shear rate region of the viscosity curve, and the plateau decreases with the increase of shear rate. Higher temperature broadens the viscosity plateau. The swelling effects of paraffin oil can reduce the viscosity of UHMWPE, and the viscosity of gels with different UHMWPE concentration has a power law relation with the shear rate. The gel viscosity is more sensitive to temperature and UHMWPE concentration than to shear rate.
The viscosity (η) of UHMWPE melt has a power law relation with the shear rate (γ),η= kγα. In the molecular weight range of 2.5 million to 6.0 million (g/mol), molecular has little effect on the rheological behavior of UHMWPE, but the shear thinning behavior and the temperature sensitivity become more severe with the increase of molecular weight. When the temperature rises to 185℃, the intramolecular crystal structure disappears completely and the density of entanglement network is maximum, and the molecules exhibit a random coil conformation. When the temperature rises to 225℃, the entangling and disentangling of chains reach a dynamic equilibrium, so the viscosity keeps constant.
A metastable phenomenon was observed during the rheological behavior study of UHMWPE (viscosity average molecular weight 3.5 million g/mol) in a“temperature window”of 154-157℃using a capillary rheometer. The extrusion pressure decreased abruptly and then became stable, and the rods surface was smooth without melt fracture. A low temperature and low pressure extrusion method was developed to process UHMWPE using a traditional ram extruder, which can significantly decrease the energy consumption.
UHMWPE gel with a UHMWPE concentration of 50% in paraffin oil was successfully extruded using a twin-screw extruder at 165℃and screw speed of 40 N/min. When octacalcium phosphate (OCP) fiber weight 25%, the UHMWPE/OCP composite prepared by swell mix extrude through common twin-screw extruder have more excellent mechanical performance, and this composite can induce bone-like apatite layer generate at its surface. There will be many polar functional groups on the surface of UHMWPE powder after acrylic acid modification, which attracted Ca2+ and CO32- ions to grow nano-CaCO3 particles in-situ for prepare UHMWPE/CaCO3 composite by in-situ chemical synthesis. The as-prepared composite exhibited an improved tensile strength and heat distortion temperature compared to mechanical blended composite. When the load rate of CaCO3 is 9.5%, the tensile strength and heat distortion temperature of composite prepared by in-situ chemical synthesis are 43.8MPa and 106℃respectively.
本文采用粘度法表征了UHMWPE液体石蜡稀溶液中临界缠结浓度与聚合度之间的关系,得到方程式。UHMWPE液体石蜡溶液凝胶中,UHMWPE分子链为单链多晶形态,随着溶液凝胶浓度的降低,凝胶中UHMWPE片晶晶粒更细小。UHMWPE液体石蜡凝胶凝胶点温度随着浓度的升高而升高,凝胶点温度Cc rNC cr? N1/2 =94Tg el与凝胶质量浓度C m之间的关系式为:Tg el = 0.32C m+ 110.4(0.8%≤≤8%) ;(10%≤≤40%);CmTg el = 31.9 Cm+ 115.1C mTg el = 24.5 Cm+ 113.2( Cm≥45%)。
UHMWPE液体石蜡凝胶是假塑性凝胶,在165℃时充分熔融,凝胶中UHMWPE分子链形成熔融充分的呈高斯分布的线团,具有较高的弹性模量和较低的损耗模量。温度在165℃时以上,剪切速率-粘度曲线在低剪切速率区域出现一个平台,然后随剪切速率的增加而下降,且温度高的凝胶的粘度平台区更宽。液体石蜡的溶胀作用可以有效地减小UHMWPE的粘度,不同浓度下的UHMWPE液体石蜡凝胶的粘度与剪切频率之间为幂律方程关系。凝胶粘度对温度及对浓度的敏感性均比其对剪切速率的敏感性更为显著。
UHMWPE本体的粘度-剪切速率关系符合幂律方程,可以用方程式η= kγα来描述。UHMWPE分子量在250万-600万之间时,分子量对UHMWPE的流变行为影响不大,但分子量高的UHMWPE比分子量低的UHMWPE的粘度随剪切频率的增加而下降的幅度要大,其流变行为对温度更为敏感。当温度升高至185℃时,UHMWPE分子链内部的结晶消失,相互贯穿的分子链到达网络缠结点密度的最高点,分子形态呈无规线团状。当温度升高到225℃以上时,分子链间缠绕与解缠绕达到动态平衡,粘度基本不再变化。粘均分子量为3.5×106g/mol的UHMWPE柱塞挤出过程中,在154℃-157℃的“温度窗口”中,出现亚稳性现象,表现为挤出压力出现突降并稳定下来,挤出棒材表面光滑,不出现熔体破裂现象。实现了低温低压下柱塞挤出成型加工UHMWPE,使得不需改进设备,采用传统的柱塞挤出机挤出成型UHMWPE成为现实,且显著降低了生产中所需能耗。
控制螺杆转速40N/min;温度165℃,可在常规双螺杆挤出机上实现50%的UHMWPE液体石蜡凝胶的顺利挤出。通过UHMWPE和OCP纤维在双螺杆挤出机上溶胀共混挤出制备的UHMWPE/OCP复合材料在OCP纤维质量分数为25%时具有较为优异的力学性能,该复合材料在仿生条件下可诱发表面类骨磷灰石层的生成。UHMWPE经丙烯酸改性后,表面含有大量活性基团,可用于原位化学合成UHMWPE/CaCO3复合材料。原位化学合成法制备的UHMWPE/CaCO3复合材料比纯UHMWPE以及机械共混法制备的复合材料具有更佳的拉伸强度和耐热变形温度。用该法制得的CaCO3含量为9.5%的UHMWPE/CaCO3复合材料的拉伸强度可达到43.8MPa,耐热变形温度可高达106℃。
Polymer processability depends on its rheological behavior. To improve the processability of ultrahigh molecular weight (UHMWPE), the rheological behaviors of UHMWPE, including dilute solution, concentrated solution, gel, and melt, were studied. The relationships of the entanglement state of UHMWPE long chains, viscosity, shear rate, temperature, polymer concentrations were obtained. The suitable processing parameters for ram extrusion of UHMWPE rod and twin screw extrusion of UHMWPE/octacalcium phosphate composite were explored using the theoretical results. A metastable phenomenon was observed during the ram extrusion of UHMWPE, and a low temperature and low pressure processing method was developed to solve the difficulties in processing UHMWPE. A bioactive UHMWPE/OCP composite was processed using twin screw extrusion of the UHMWPE gel. A heat resistant and high strength composite of UHMWPE and calcium carbonate was processed by in situ synthesis.
The relationship between the critical entanglement concentration (Ccr) of UHMWPE dilute solution in paraffin oil and the degree of polymerization (N) was obtained by measuring the viscosity, . UHMWPE gel in the paraffin oil exhibits a single chain with polycrystalline forms. The UHMWPE lamellar crystal size becomes smaller with the decrease of the gel concentration. The UHMWPE/paraffin oil gel point (TC cr? N1/2 =94gel) increases with the mass concentration of UHMWPE (Cm), Tg el = 0.32C m+ 110.4(0.8%≤≤8%), (10%≤≤40%), CmTg el = 31.9 Cm+ 115.1C mTg el = 24.5 Cm+ 113.2( Cm≥45%).
UHMWPE/paraffin oil gel is a pseudoplastic gel. When the gel melts sufficiently at 165℃, UHMWPE chains in the melt state exhibit as Gaussian distributed coils with higher storage modulus and lower loss modulus. At temperature above 165℃, a plateau appears in the low shear rate region of the viscosity curve, and the plateau decreases with the increase of shear rate. Higher temperature broadens the viscosity plateau. The swelling effects of paraffin oil can reduce the viscosity of UHMWPE, and the viscosity of gels with different UHMWPE concentration has a power law relation with the shear rate. The gel viscosity is more sensitive to temperature and UHMWPE concentration than to shear rate.
The viscosity (η) of UHMWPE melt has a power law relation with the shear rate (γ),η= kγα. In the molecular weight range of 2.5 million to 6.0 million (g/mol), molecular has little effect on the rheological behavior of UHMWPE, but the shear thinning behavior and the temperature sensitivity become more severe with the increase of molecular weight. When the temperature rises to 185℃, the intramolecular crystal structure disappears completely and the density of entanglement network is maximum, and the molecules exhibit a random coil conformation. When the temperature rises to 225℃, the entangling and disentangling of chains reach a dynamic equilibrium, so the viscosity keeps constant.
A metastable phenomenon was observed during the rheological behavior study of UHMWPE (viscosity average molecular weight 3.5 million g/mol) in a“temperature window”of 154-157℃using a capillary rheometer. The extrusion pressure decreased abruptly and then became stable, and the rods surface was smooth without melt fracture. A low temperature and low pressure extrusion method was developed to process UHMWPE using a traditional ram extruder, which can significantly decrease the energy consumption.
UHMWPE gel with a UHMWPE concentration of 50% in paraffin oil was successfully extruded using a twin-screw extruder at 165℃and screw speed of 40 N/min. When octacalcium phosphate (OCP) fiber weight 25%, the UHMWPE/OCP composite prepared by swell mix extrude through common twin-screw extruder have more excellent mechanical performance, and this composite can induce bone-like apatite layer generate at its surface. There will be many polar functional groups on the surface of UHMWPE powder after acrylic acid modification, which attracted Ca2+ and CO32- ions to grow nano-CaCO3 particles in-situ for prepare UHMWPE/CaCO3 composite by in-situ chemical synthesis. The as-prepared composite exhibited an improved tensile strength and heat distortion temperature compared to mechanical blended composite. When the load rate of CaCO3 is 9.5%, the tensile strength and heat distortion temperature of composite prepared by in-situ chemical synthesis are 43.8MPa and 106℃respectively.
引文
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