静电纺聚酰亚胺纤维的制备及结构性能研究
摘要
静电纺丝是制备聚合物纳米连续纤维的最有效的方法,近年来已经通过静电纺丝制备了不同聚合物纳米纤维。静电纺丝的研究主要集中在聚合物的溶液方面,对于熔体研究的很少,而静电纺丝要求聚合物能溶于易挥发的溶剂,这对静电纺丝的发展有一定的影响。目前静电纺丝纤维的应用已经在研发中,主要用来增强纳米复合材料,尽管关于静电纺丝理论的研究已经很深入,但是对于其工业化的研究还有待进一步的发展。
静电纺丝技术是基于高压电场下导电流体产生高速喷射的原理发展起来的,基本过程是:聚合物溶液或者熔体在几万伏的高压电下表面分布了电荷,克服表面张力后产生射流,射流在运动的过程中伴随着溶剂的挥发,发生固化,最终落到接收板上形成纳米纤维毡,电纺丝制得的纤维直径一般在数十纳米到几微米之间。
本文研究了聚酰亚胺的静电纺丝纤维,由于聚酰亚胺具有很大的刚性,因此我们使用聚酰亚胺的前驱体聚酰胺酸溶液进行纺丝,转化为聚酰亚胺。首先用PDA和ODPA在DMAc中合成聚酰胺酸溶液,研究了反应物浓度、反应时间等对聚酰胺酸溶液特性粘度的影响,从而找出了反应时间快、溶液特性粘度又比较高的条件,之后对溶液的动态流变性能进行了研究。
合成的聚酰胺酸溶液,稀释制成了不同质量分数的聚酰胺酸溶液,静电纺丝制备聚酰胺酸纤维,静电纺丝中纤维受到电压、距离、溶液性质等方面的影响,因而我们研究了不同的质量分数溶液、电压和纺丝距离对聚酰胺酸纤维直径的影响,同时比较了加盐前后纤维的直径和形貌的变化,发现电压和接收距离对纤维的直径影响不是很大,加入盐后纤维的直径有大幅度的减小,纤维直径在几十到几百纳米之间。
静电纺丝得到的聚酰胺酸纤维通过热处理和化学处理成功转化成了聚酰亚胺纳米纤维,转化后聚酰亚胺纤维的直径变小,纤维在转化过程中脱水酰亚胺化。对纤维进行了TGA、DSC热分析,发现酰亚胺化前后纤维的热性能有很大的变化。聚酰亚胺纤维有很高的耐热性。
聚酰胺酸纤维热转化为聚酰亚胺纤维的过程比较复杂,不同的温度酰亚胺化的程度不同,实验分析了不同酰亚胺化温度下聚酰亚胺的反应动力学和热分解动力学特征,对其分别用Kissinger和Ozawa计算了不同升温速率下的活化能,用两种方法得到的活化能相差不大,同时发现得到的聚酰亚胺纤维的活化能较大,再次证明聚酰亚胺的耐热性能较好。
Electrospinning has been recognized as an efficient technique for the fabrication of polymer nanofibers. Various polymers have been successfully electrospinning into ultrafine fibers in recent years mostly in solvent solution and some in melt form. The solution must be volatile, which has a great effect on the development of electrospinning. Potential applications based on such fibers specifically their use as reinforcement in nanocomposite development have been realized. The theory of electrospinning has already been matured while the applications have been underway.
Electropinning origins from that electrically charged fluid is forced jets in the high voltage electrostatic field. Electrospinning occurs when the electrical forces at the surface of a polymer solution or melt overcomes the surface tension and causes an electrically charged jet to be ejected. When the jet dries or solidifies, an electrically charged fiber remains. This charged fiber can be directed or accelerated by electrical forces and then collected in mats or other useful geometrical forms. The diameters of electrospun fibers are in the range of tens of nanometers to several micrometers.
In this paper PDA and ODPA were dissolved in dimethylacetamide(DMAc), which reacted with each other in order to produce the PAA solution. Then the PAA solution was electrospun into nanofibers which was then imidized into PI nanofibers.
Research about the effects of reaction time, reaction concentrations et al on the intrinsic viscosit of the PAA solution were done. And the best conditions to synthesize the solution with a higher intrinsic viscosit were found. Then the dynamic rheology of the solution was studied.
There are several effects on the electrospinning of solutions, such as voltage, distance, and solution property. In this paper the solution was diluted into different concentrations in order to study these effects. As a result the voltage and distance had a slight influence on the diameters of the nanofibers. The solutions that added with salt and without salt were electrospun into nanofibers too, the result showed that the diameter of the solution with salt was much smaller than the solution without salt, so the adding of the salt can reforce the electricity of the solution which would get thinner nanofibers.
The PAA nanofibers were imidized into PI nanofibers by thermal and chemical methods. The diameter of PI nanofibers was much smaller than the PAA nanofibers. The PI nanofibers were characterized by TGA and DSC, which concluded that the PI nanofibers had a high heat resistant.
The process of the imidization was very complicated, and different tempetature reflected different degree imidization, the thermal dynamics of the PI nanofibers with different degree imidization were analysised. We calculated the reaction activation energy and decompositon activation energy of the PI nanofibers using Kissinger and Ozawa at different calefactive rates by the DSC and TGA. The activation energy was almost equal by this two methods. This also gave the evidence that the PI nanofibers have a high heat resistant property.
静电纺丝技术是基于高压电场下导电流体产生高速喷射的原理发展起来的,基本过程是:聚合物溶液或者熔体在几万伏的高压电下表面分布了电荷,克服表面张力后产生射流,射流在运动的过程中伴随着溶剂的挥发,发生固化,最终落到接收板上形成纳米纤维毡,电纺丝制得的纤维直径一般在数十纳米到几微米之间。
本文研究了聚酰亚胺的静电纺丝纤维,由于聚酰亚胺具有很大的刚性,因此我们使用聚酰亚胺的前驱体聚酰胺酸溶液进行纺丝,转化为聚酰亚胺。首先用PDA和ODPA在DMAc中合成聚酰胺酸溶液,研究了反应物浓度、反应时间等对聚酰胺酸溶液特性粘度的影响,从而找出了反应时间快、溶液特性粘度又比较高的条件,之后对溶液的动态流变性能进行了研究。
合成的聚酰胺酸溶液,稀释制成了不同质量分数的聚酰胺酸溶液,静电纺丝制备聚酰胺酸纤维,静电纺丝中纤维受到电压、距离、溶液性质等方面的影响,因而我们研究了不同的质量分数溶液、电压和纺丝距离对聚酰胺酸纤维直径的影响,同时比较了加盐前后纤维的直径和形貌的变化,发现电压和接收距离对纤维的直径影响不是很大,加入盐后纤维的直径有大幅度的减小,纤维直径在几十到几百纳米之间。
静电纺丝得到的聚酰胺酸纤维通过热处理和化学处理成功转化成了聚酰亚胺纳米纤维,转化后聚酰亚胺纤维的直径变小,纤维在转化过程中脱水酰亚胺化。对纤维进行了TGA、DSC热分析,发现酰亚胺化前后纤维的热性能有很大的变化。聚酰亚胺纤维有很高的耐热性。
聚酰胺酸纤维热转化为聚酰亚胺纤维的过程比较复杂,不同的温度酰亚胺化的程度不同,实验分析了不同酰亚胺化温度下聚酰亚胺的反应动力学和热分解动力学特征,对其分别用Kissinger和Ozawa计算了不同升温速率下的活化能,用两种方法得到的活化能相差不大,同时发现得到的聚酰亚胺纤维的活化能较大,再次证明聚酰亚胺的耐热性能较好。
Electrospinning has been recognized as an efficient technique for the fabrication of polymer nanofibers. Various polymers have been successfully electrospinning into ultrafine fibers in recent years mostly in solvent solution and some in melt form. The solution must be volatile, which has a great effect on the development of electrospinning. Potential applications based on such fibers specifically their use as reinforcement in nanocomposite development have been realized. The theory of electrospinning has already been matured while the applications have been underway.
Electropinning origins from that electrically charged fluid is forced jets in the high voltage electrostatic field. Electrospinning occurs when the electrical forces at the surface of a polymer solution or melt overcomes the surface tension and causes an electrically charged jet to be ejected. When the jet dries or solidifies, an electrically charged fiber remains. This charged fiber can be directed or accelerated by electrical forces and then collected in mats or other useful geometrical forms. The diameters of electrospun fibers are in the range of tens of nanometers to several micrometers.
In this paper PDA and ODPA were dissolved in dimethylacetamide(DMAc), which reacted with each other in order to produce the PAA solution. Then the PAA solution was electrospun into nanofibers which was then imidized into PI nanofibers.
Research about the effects of reaction time, reaction concentrations et al on the intrinsic viscosit of the PAA solution were done. And the best conditions to synthesize the solution with a higher intrinsic viscosit were found. Then the dynamic rheology of the solution was studied.
There are several effects on the electrospinning of solutions, such as voltage, distance, and solution property. In this paper the solution was diluted into different concentrations in order to study these effects. As a result the voltage and distance had a slight influence on the diameters of the nanofibers. The solutions that added with salt and without salt were electrospun into nanofibers too, the result showed that the diameter of the solution with salt was much smaller than the solution without salt, so the adding of the salt can reforce the electricity of the solution which would get thinner nanofibers.
The PAA nanofibers were imidized into PI nanofibers by thermal and chemical methods. The diameter of PI nanofibers was much smaller than the PAA nanofibers. The PI nanofibers were characterized by TGA and DSC, which concluded that the PI nanofibers had a high heat resistant.
The process of the imidization was very complicated, and different tempetature reflected different degree imidization, the thermal dynamics of the PI nanofibers with different degree imidization were analysised. We calculated the reaction activation energy and decompositon activation energy of the PI nanofibers using Kissinger and Ozawa at different calefactive rates by the DSC and TGA. The activation energy was almost equal by this two methods. This also gave the evidence that the PI nanofibers have a high heat resistant property.
引文
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