【摘要】：荷電膜技術作為一種新型的分離技術,由于其獨特的荷電特性,可以進行離子物系的分離分級,在綠色化學和清潔化工方面具有十分廣泛的應用前景。本論文圍繞荷電膜分離過程設備開發(fā)和應用方面進行了相關的研究與討論。第一部分,針對現(xiàn)有板式擴散滲析器裝填密度小、傳質效率低的缺點,設計了一種全新的擴散滲析組器——螺旋卷式擴散滲析膜組件,并對其進行結構優(yōu)化和工業(yè)化應用研究,實現(xiàn)了該膜組件的批量制備。第二部分,研制了一種實驗用集成式雙極膜電滲析器,并應用于煙酸的清潔化生產(chǎn)實驗研究。主要結果如下:1)發(fā)明了一種螺旋卷式擴散滲析膜組件,將膜組件用于H2SO4/FeSO4料液和HCl/FeCl2料液的酸回收過程,結果顯示,兩種體系的回收率都可達85%以上,同時Fe2+的泄漏率都小于20%,采用螺旋卷式擴散滲析膜組件的單位膜面積廢酸處理量大于小型實驗用板框式擴散滲析器的單位膜面積廢酸處理量,說明本螺旋卷式擴散滲析膜組件的傳質效率優(yōu)于現(xiàn)有技術的板框式擴散滲析器,而對于HCl/FeCl2體系,這種優(yōu)勢更加明顯。2)基于阿基米德螺線,建立了螺旋卷式擴散滲析膜組件的幾何模型,并對其進行了模型驗證,誤差小于1%;對螺旋卷式擴散滲析膜組件的傳質模型進行了討論分析,提出總傳質系數(shù)的表達式。3)作為螺旋卷式擴散滲析膜組件的結構優(yōu)化,研制了一種雙程螺旋卷式擴散滲析膜組件,該新型膜組件省略了側流管,有比單程式膜組件更大的裝填密度,單位膜面積料液處理量更大。4)設計加工了SWDD-01型預緊式卷膜機,可實現(xiàn)11 m2、5 m2、10 m2三個規(guī)格的膜組件的同線生產(chǎn);提出了螺旋卷式擴散滲析膜組件產(chǎn)品的質量控制指標和控制方法;長期穩(wěn)定性試驗顯示膜組件在30%硫酸介質連續(xù)運行6個月,膜組件不串漏;第三方性能測試結果顯示:對于HCl/AlCl3料液樣品(含Al3+ 0.995 mol/L,H+ 2.96 mol/L),10平方米組件在回收酸流量達7.4 mL/m2.min時H+回收率達96.9%,而Al3+截留率達99.5%;提出了螺旋卷式擴散滲析膜組件作為廢酸回收工程應用的工藝流程和實現(xiàn)方法。5)設計加工了一種集成式雙極膜電滲析器,可以滿足各種膜堆構型的雙極膜電滲析實驗的需要;進行了雙極膜電滲析法由煙酸鈉清潔生產(chǎn)煙酸的實驗,使用BP-C-BP膜堆構型,考察了料液濃度、電流效率等操作參數(shù)對雙極膜電滲析效果(諸如能量消耗、電流效率、膜堆電壓和轉化率等)的影響,在經(jīng)濟可行的條件下煙酸鈉轉化效率可達73%,電流效率最高可達95%,產(chǎn)生每千克煙酸(0.1 mol/L)的能耗最低可達4.1 kWh。所得煙酸可通過冷卻結晶法簡易地從溶液中析出,所得煙酸純度達99%,實現(xiàn)了煙酸的清潔化生產(chǎn)。
[Abstract]:As a new separation technology, charged membrane technology can be used in separation and classification of ion system because of its unique charged characteristics. It has a wide application prospect in green chemistry and clean chemical industry. In this paper, the development and application of charged membrane separation equipment are studied and discussed. In the first part, aiming at the shortcomings of low loading density and low mass transfer efficiency of the existing plate diffusivity dialyzers, a new diffusing dialyzer, spiral coil diffused dialysate membrane assembly, is designed, and its structure optimization and industrial application are studied. The batch preparation of the membrane module was realized. In the second part, an integrated bipolar membrane electrodialysis device is developed and applied to the clean production of nicotinic acid. The main results are as follows: 1) A spiral coil diffusion dialysis membrane module was invented, which was used in the acid recovery process of H2SO4/FeSO4 and HCl/FeCl2 feed solution. The results show that the recovery rate of both systems can reach more than 85%. At the same time, the leakage rate of Fe2 is less than 20%, and the waste acid treatment capacity per unit membrane area using spiral coil diffusion dialyzer module is larger than that of small-scale plate-frame diffusing dialyzer. It is shown that the mass transfer efficiency of the spiral coil diffusion dialyzer module is better than that of the frame diffusion dialyzer with the prior art, and this advantage is more obvious for the HCl/FeCl2 system. 2) based on Archimedes solenoid, The geometric model of the diffuser-dialyzed membrane module with spiral coil is established and verified. The error is less than 1%. The mass transfer model of the diffusion dialysis membrane module with spiral coil is discussed and analyzed, and the expression of the total mass transfer coefficient is put forward. 3) as the structural optimization of the diffusion dialysis membrane module with spiral coil, a kind of two-way spiral coil diffusion dialysis membrane module is developed. The new membrane assembly omits the sideflow tube, has a higher loading density than the single-pass membrane module, and a larger liquid handling capacity per unit membrane area. 4) the SWDD- 01 pre-tight film coiling machine is designed and processed. Can achieve 11 m ~ 2, 5 m ~ 2, 10 m ~ 2 three specifications of membrane assembly of the same line production; The quality control index and control method of the product of spiral coil diffusion dialysis membrane module were put forward, the long-term stability test showed that the membrane module operated continuously in 30% sulfuric acid medium for 6 months, and the membrane module did not leak in series. The results of the third-party performance test showed that for the HCl/AlCl3 sample (including Al3 0.995 mol/L,H 2.96 mol/L), the H recovery rate of 10 square meter components reached 96.9% when the recovery rate of acid reached 7.4 mL/m2.min. The rejection rate of Al3 was 99.5%. The technological process and realization method for the application of spiral coil diffusion dialysate module as waste acid recovery engineering are put forward. 5) an integrated bipolar membrane electrodialysis device is designed and manufactured. It can meet the needs of bipolar membrane electrodialysis experiments of various membrane stack configurations. The experiment of clean production of nicotinic acid from sodium nicotinate by bipolar membrane electrodialysis was carried out. The BP-C-BP membrane stack configuration was used to investigate the effects of operating parameters such as liquid concentration and current efficiency on electrodialysis of bipolar membrane, such as energy consumption, current efficiency, and so on. Under the economical and feasible conditions, the conversion efficiency of sodium nicotinate can reach 73%, the current efficiency can be up to 95%, and the energy consumption per kilogram of nicotinic acid (0.1 mol/L) can be as low as 4.1 kWh.. The obtained nicotinic acid can be easily precipitated from the solution by cooling crystallization. The purity of niacin can reach 99% and the clean production of nicotinic acid can be realized.
【學位授予單位】：中國科學技術大學
【學位級別】：博士
【學位授予年份】：2016
【分類號】：TQ051.893

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