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超音速氣流法低溫固相合成有機骨架類聚合物及機理研究

發(fā)布時間:2018-03-31 10:56

  本文選題:超音速氣流法 切入點:數學模型 出處:《西南科技大學》2017年碩士論文


【摘要】:固相反應作為綠色化學中重要組成部分,受到廣泛關注。機械化學合成法作為固相化學合成的分支,受到越來越多的重視。傳統(tǒng)的機械化學合成方法主要包括球磨法、研磨法、雙螺旋擠壓法、高壓法以及微波輔助法,這些方法存在提供反應能量低、經濟成本高、反應時間長、不能連續(xù)循環(huán)及難以實現工業(yè)化生產等缺陷。為此,本課題組提出超音速氣流低溫固相合成,充分利用流體力學和動力學反應原理,通過超音速氣流加速和碰撞技術實現低溫固相反應合成中的能量傳遞,為固相反應合成開辟了新的技術途徑,該方法具有連續(xù)循環(huán)、高效快速、操作簡單、環(huán)境友好、適合大規(guī)模合成等優(yōu)點。本文主要研究內容包括超音速氣流低溫固相反應裝置的改進,利用超音速氣流法低溫固相合成不同的骨架類聚合物,探究超音速氣流低溫固相合成能夠適應的反應體系,同時探究不同實驗條件對實驗的影響,探究機理及建立動力學數學模型。(1)在實驗的過程中,不斷發(fā)現超音速氣流低溫固相反應裝置的不足,提出改進方案,不斷改進裝置,提高能量利用率和反應速率,滿足更多固相反應合成在超音速氣流低溫固相裝置上實現;(2)用超音速氣流法低溫固相合成兩種金屬有機框架、聚酰亞胺以及聚2,5-二甲氧基苯胺聚合物,并采用傅里葉紅外光譜(FT-IR),粉末X射線衍射(XRD),差熱分析(DTA),場發(fā)射掃描電鏡(SEM),紫外吸收光譜(UV-vis),熱分析(TG-DSC)以及循環(huán)伏安對合成目標化合物的結構和性能進行表征,證明目標產物的成功合成及合理應用;(3)為探究該裝置的反應機理,研究不同壓力、反應時間、顆粒度大小對合成反應的影響,采用非原位粉末X射線衍射跟蹤監(jiān)測反應過程,將檢測結果轉化成轉化率(α),建立動力學數學模型,篩選出最佳動力學模型,探究反應的機理。
[Abstract]:As an important part of green chemistry, solid-state reaction has attracted wide attention. As a branch of solid-state chemical synthesis, mechanochemical synthesis has attracted more and more attention. Traditional mechanochemical synthesis methods mainly include ball milling and grinding. Double helix extrusion method, high pressure method and microwave assistant method have some disadvantages, such as low reaction energy, high economic cost, long reaction time, no continuous cycle and difficulty in industrial production. In this paper, the supersonic airflow low temperature solid phase synthesis is proposed. The energy transfer in the low temperature solid state reaction synthesis is realized by the hypersonic airflow acceleration and collision technology, which makes full use of the principles of hydrodynamics and kinetic reaction. This method has the advantages of continuous cycle, high efficiency, high speed, simple operation and friendly environment. The main contents of this paper include the improvement of the low temperature solid state reaction device of supersonic airflow and the synthesis of different skeleton polymers by using the low temperature solid phase method of supersonic airflow. To explore the reaction system of supersonic airflow low temperature solid-state synthesis, and to explore the influence of different experimental conditions on the experiment, to explore the mechanism and to establish a kinetic mathematical model. The deficiency of supersonic airflow low-temperature solid-state reaction device is found continuously. The improvement scheme is put forward, and the equipment is continuously improved to increase the energy utilization rate and reaction rate. Two kinds of metal-organic frames, polyimide and poly2-dimethoxyaniline were synthesized by supersonic flow method at low temperature. The structure and properties of the synthesized target compounds were characterized by Fourier transform infrared spectroscopy (FTIR), powder X-ray diffraction (XRD), differential thermal analysis (DTAA), field emission scanning electron microscopy (SEM), ultraviolet absorption spectroscopy (UV), TG-DSCC and cyclic voltammetry. It is proved that the successful synthesis of the target product and its rational application are used to investigate the reaction mechanism of the device, and to study the effects of different pressure, reaction time and particle size on the synthetic reaction. Non-in-situ powder X-ray diffraction is used to monitor the reaction process. The test results were transformed into conversion rate (偽), the kinetic mathematical model was established, the best kinetic model was screened out, and the mechanism of the reaction was explored.
【學位授予單位】:西南科技大學
【學位級別】:碩士
【學位授予年份】:2017
【分類號】:O631

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