【摘要】：現(xiàn)有間歇精餾的操作方式大多存在分離效率不高、分離時間較長、能耗較大、不能同時得到純度較高的輕組分和重組分產(chǎn)品等問題。本文依據(jù)常規(guī)間歇精餾的操作原理,通過儲罐設(shè)置和進料方法的改進,提出了一種全新的精餾操作策略——半連續(xù)恒全回流精餾操作法。該操作法在間歇精餾塔的基礎(chǔ)上設(shè)置了塔頂儲罐和塔底儲罐,整個精餾過程在恒全回流操作狀態(tài)下進行,通過對兩個儲罐內(nèi)液相的累積和倒罐完成采出和進料過程,可分別得到高濃度的輕組分產(chǎn)品和重組分產(chǎn)品,進行半連續(xù)操作。在半連續(xù)恒全回流精餾操作法的基礎(chǔ)上結(jié)合間歇精餾塔的液相串聯(lián)操作,論文又依次提出了半連續(xù)雙塔液相交換操作方式和半連續(xù)雙塔液相串聯(lián)操作方式。在分離過程中,雙塔各自進行恒全回流操作,互不干涉,僅僅通過各自儲罐內(nèi)的液相交換完成產(chǎn)品的采出和再進料,實現(xiàn)雙塔串聯(lián)操作。兩種雙塔操作方式有效減小了液相濃度差造成的塔內(nèi)擾動,最大程度的減少了返混現(xiàn)象對分離過程造成的不良影響。在等濃度進料條件下半連續(xù)雙塔液相交換操作的結(jié)果較好,而在低濃度和高濃度進料條件下,半連續(xù)雙塔液相串聯(lián)操作更具優(yōu)勢。隨著后續(xù)研究的深入,論文結(jié)合兩種雙塔操作方式,去繁留簡,提出了半連續(xù)多塔液相串聯(lián)操作方式。該操作方式包括開車、塔頂輕組分采出-交換-進料和塔底重組分采出-交換-進料三個階段。其中,開車階段主要用于建立各儲罐液相的濃度梯度,可采用塔頂-塔釜液相交換、串聯(lián)液相交換和梯度進料三種開車方法實現(xiàn)。論文通過不同進料濃度下的精餾實驗驗證了以上各操作方法的可行性。根據(jù)全回流操作的數(shù)學(xué)模型對其進料濃度、進料量、儲罐體積等各項操作參數(shù)分別進行了模擬實驗研究,比較實驗結(jié)果分析各操作方法的異同和優(yōu)缺點,優(yōu)化操作條件。實驗結(jié)果表明,本文提出的新型操作方式具有以下優(yōu)勢:分離效果好,操作時間短,能耗低;可同時獲得高純度的輕重組分產(chǎn)品;處理量大;產(chǎn)品回收率高;一塔多用,操作彈性大;受外界影響較小;可用于熱敏物料的分離任務(wù)。綜上所述,論文提出的新型操作方式可滿足各種分離任務(wù)的實際需求,為解決不同精餾問題提供了新的研究思路。
[Abstract]:Most of the existing operation methods of batch distillation have some problems such as low separation efficiency, long separation time, high energy consumption, and the high purity of light components and recombined fractions can not be obtained simultaneously. Based on the operation principle of conventional batch distillation and the improvement of tank setting and feed method, a new operation strategy of semi-continuous total reflux distillation is proposed in this paper. On the basis of batch distillation column, the tower top tank and bottom tank are set up. The whole distillation process is carried out under the condition of constant total reflux operation. The process of extraction and feeding is completed by the accumulation of liquid phase in the two tanks and the inversion of the tank. High concentration of light component product and recombination product can be obtained, and semi-continuous operation can be carried out. On the basis of semi-continuous constant total reflux distillation operation combined with liquid phase series operation of batch distillation column, the liquid phase exchange operation mode of semi-continuous two-column and the liquid-phase series operation mode of semi-continuous double-column were put forward in this paper. In the process of separation, the two towers are operated with constant total reflux and non-interference, only through the liquid phase exchange in their respective storage tanks to complete the extraction and refeed of the products, and realize the operation of the two towers in series. The two operation methods can effectively reduce the disturbance in the column caused by the liquid concentration difference and minimize the adverse effect of the backmixing phenomenon on the separation process. Under the condition of equal concentration of feed, the results of liquid exchange operation of semi-continuous double-tower are better, but the operation of semi-continuous double-tower liquid phase series is more advantageous under the condition of low concentration and high concentration of feed. With the development of further research, a semi-continuous multi-tower liquid-phase series operation is proposed in this paper. The operation includes three stages: starting up, extracting-exchanging-feeding of light components at the top of the tower and recombination of the bottom of the tower. The start-up stage is mainly used to establish the concentration gradient of the liquid phase of each tank, which can be realized by three starting methods: the liquid phase exchange between the tower and the tower, the series liquid phase exchange and the gradient feed. The feasibility of the above operation methods is verified by distillation experiments with different feed concentration in this paper. According to the mathematical model of total reflux operation, the operating parameters, such as feed concentration, feed volume and tank volume, were simulated and studied, respectively. The comparison of the experimental results was made to analyze the similarities and differences of each operation method and its advantages and disadvantages, and to optimize the operating conditions. The experimental results show that the new operation method proposed in this paper has the following advantages: good separation effect, short operating time, low energy consumption, high purity heavy and heavy component products can be obtained at the same time, large amount of treatment, high product recovery rate, one tower of multipurpose, The operation is flexible; less affected by the outside; can be used for the separation of heat sensitive materials. To sum up, the new operation mode proposed in this paper can meet the practical requirements of various separation tasks, and provide a new research idea for solving different distillation problems.
【學(xué)位授予單位】：天津大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2015
【分類號】：TQ028.31

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