双极膜电渗析生产酒石酸的研究
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摘要
有机酸被广泛应用于食品、饮料、医药、化妆品、化学合成、生物化学领域，与人类生活具有广泛而密切的联系。生产有机酸主要有两种方法：化学合成和发酵法。无论是发酵法还是化学合成法，有机酸的分离、浓缩、提纯都是必要的步骤。传统提纯工艺包括沉淀、酸化、析出、结晶、离子交换等步骤，其过程中需要消耗大量的酸碱，并产生大量固体废弃物。传统有机酸的生产提纯方法这些缺点都不符合现代绿色化学节能减排的要求，迫切的需要替代工艺。为了实现节能减排和绿色化工的目标，我们需要一种更经济和环保的技术。
双极膜电渗析可以应用到这一领域，在通电条件下，双极膜解离水形成H~+和OH~-，同时在溶液中，有机酸盐解离为有机酸根离子和金属阳离子，H~+与有机酸根离子结合形成产品酸，OH~-同金属阳离子结合形成碱。因为离子交换膜具有较强的选择透过性，使用此方法生产有机酸具有较高纯度，后处理成本低的优点，同时生产的碱也可以应用于有机酸发酵过程，不产生任何废弃物，没有二次污染。
本论文以双极膜电渗析技术生产酒石酸作为切入点，探讨了该技术应用于有机酸生产中的如何节能等共性问题，研究内容和主要结论如下：
1.由于酒石酸氢钾的在水溶液中的低溶解度，实验的膜堆构型为BP—A—C构型。为了降低酸室中由于有机酸的低解离系数导致的高电阻，向酸室中添加了强酸型离子交换树脂。实验结果证明，添加离子交换树脂有效降低了相同电流密度下的操作电压，降低双极膜电渗析生产酒石酸的能量消耗。虽然添加离子交换树脂在一定程度上降低了酒石酸产量，但同能耗的降低幅度相比，仍然具有巨大的积极作用。
2.在同等条件下，将添加离子交换树脂的方法应用于传统电渗析。实验结果同双极膜电渗析大致类似。实验扩展了添加离子交换树脂的应用范围。
3.考虑到在大型电渗析器中添加离子交换树脂的复杂性，在中试规模的实验中采用了导离子隔板。导离子隔板由异相阳离子交换膜雕刻而成。实验结果证明导离子隔板有效降低了操作电压，降低了双极膜电渗析的能耗。实验还对国产双极膜和德国双极膜进行了对比实验，在酒石酸产量，电流效率等方面国产双极膜性能还有待提高。
4.对以上的4个实验进行了经济核算，按照实验规模进行了两两对比。(1)在小试规模下核算结果显示：无论是双极膜电渗析还是传统电渗析，酒石酸总生产成本和能耗成本随电流密度升高都呈上升趋势；添加树脂后酒石酸总生产成本和能耗成本均有显著降低；由于双极膜价格的昂贵，双极膜电渗析生产成本普遍高于普通电渗析生产成本。(2)中试规模下：随着操作电流升高，酒石酸总生产成本和能耗成本都降低；添加导离子隔板降低了酒石酸生产的能耗费用，由于添加导离子隔板后，酒石酸产量有一定程度降低，总生产成本的降低幅度小于能耗成本降低幅度，在部分操作电流下有小幅度升高；使用国产双极膜的成本低于德国双极膜。
5.实验简单考查了双极膜电渗析过程中的污染问题，基本重现了文献的污染现象。无机污染物污染阳离子交换膜，有机污染物污染阴离子交换膜。以腐殖酸为例，随着污染物浓度提高和电流强度提高，污染现象加重。
本文研究结果表明，添加离子交换树脂和导离子隔板，有效降低了双极膜电渗析生产酒石酸的能耗，毫无疑问这项技术也可以扩展到其他有机酸的生产过程中。
Organic acids have extensive and close contact with human life, which arewidely used in food, beverage, pharmaceutical, cosmetic, chemical synthesis andbiochemistry. There are two ways to produce organic acid, chemical synthesis andfermentation. No matter fermentation or chemical synthesis, organic acids separation,concentration, purification is needed in post-processing. Traditional purificationprocesses include sedimentation, acidification, precipitation, crystallization and ionexchange step. Precipitation acidification process consumes large amounts of acid andbase, which also produces large amounts of solid waste. Traditional organic acidproduction and purification of these shortcomings do not meet the requirements ofgreen chemistry and energy saving, there is an urgent need for alternative processes.In order to achieve the goal of energy saving and green chemicals, we need a moreeconomical and environment-friendly technology.
BPED (Bipolar membrane electrodialysis) can be applied to this area. If a directelectrical potential is established between bipolar membrane, water dissociationoccurs at the interphase of it, forming H~+and OH~-. Metal cations and anions of agiven organic salt combine with H~+and OH~-forming alkali and organic acidrespectively. Organic acid produced by this method has high purity, and the cost ofpost-processing is reduced. The alkali, which is by-product, can be applied to theorganic acid fermentation process, in this way it has no secondary pollution.
Tartaric acid production by bipolar membrane is a starting point of this research.We focus on the energy-saving and other common problems of electrodialysis in thispaper, and the main conclusions are as follows:
1. Due to low solubility of potassium hydrogen tartrate in aqueous solution, theconfiguration of experimental membrane stack is BP-A-C. In order to reduce the highresistance of the acid compartment which is caused by the low resolution of tartaricacid, strong acid ion exchange resin is added to the acid compartment.Experimental results show that adding ion exchange membrane reduces the operating voltage andthe energy consumption under the same current density. In some extend, adding ionexchange resin reduce the tartaric acid production. But comparing with the decreaseof energy consumption this method still has a tremendous positive performance.
2. Under the same conditions, we add the ion exchange resins to ED(electrodislysis). The results are similar to the bipolar membrane electrodialysis. Theexperiment extends the application range of adding ion exchange resin.
3. Considering the complexity of adding tiny resin to large-scale electrodialyzer,conductive spacer carved from cation exchange membrane is used in the pilot scaleexperiment. Experimental results show that the conductive spacer effectively reducesthe operating voltage, reducing energy consumption. Comparative experiment iscarried out between the Germany bipolar membrane and domestic bipolar membrane.The results show the tartaric acid yield and current efficiency of domestic bipolarmembrane should be improved in future.
4. The process cost of four experiments is estimated according to theexperimental results, and there is a pair-wise comparison in accordance with theexperimental scale.(1) In small scale the accounting result of process cost show that：no matter BPED or ED, the total production cost increase with the current density;adding resin can reduce the total production cost and energy consumption costsignificantly; the total production cost of BPED is higher than ED,which is caused bythe expensive price of bipolar membrane.(2) In pilot scale, the tatal production costand energy consumption cost decrease with the current rising. The use of conductivespacer reduces the cost of energy consumption, and the decreased range of totalproduction cost is smaller than the decreased range of energy consumption cost,because of the reduce of tartaric acid production after adding the conductivespacer.The cost using domestic bipolar membrane is less than that of Germany bipolarmembrane.
5. We also investigate the problem of pollution in the bipolar membraneelectrodialysis process; the results basically reproduce the phenomenon of pollution inthe literature. Cation exchange membrane is mainly affected by inorganic pollutants, and anion exchange membrane is mainly affected by organic pollutants. For example,the phenomenon of pollution increases with the holmic acid concentration and currentintensity.
The results of this study show that add of ion exchange resin and conductivespacer effectively reduces the energy consumption of tartaric acid production byBPED. There is no doubt that this technology can also be extended to the productionprocess of other organic acids.
双极膜电渗析可以应用到这一领域，在通电条件下，双极膜解离水形成H~+和OH~-，同时在溶液中，有机酸盐解离为有机酸根离子和金属阳离子，H~+与有机酸根离子结合形成产品酸，OH~-同金属阳离子结合形成碱。因为离子交换膜具有较强的选择透过性，使用此方法生产有机酸具有较高纯度，后处理成本低的优点，同时生产的碱也可以应用于有机酸发酵过程，不产生任何废弃物，没有二次污染。
本论文以双极膜电渗析技术生产酒石酸作为切入点，探讨了该技术应用于有机酸生产中的如何节能等共性问题，研究内容和主要结论如下：
1.由于酒石酸氢钾的在水溶液中的低溶解度，实验的膜堆构型为BP—A—C构型。为了降低酸室中由于有机酸的低解离系数导致的高电阻，向酸室中添加了强酸型离子交换树脂。实验结果证明，添加离子交换树脂有效降低了相同电流密度下的操作电压，降低双极膜电渗析生产酒石酸的能量消耗。虽然添加离子交换树脂在一定程度上降低了酒石酸产量，但同能耗的降低幅度相比，仍然具有巨大的积极作用。
2.在同等条件下，将添加离子交换树脂的方法应用于传统电渗析。实验结果同双极膜电渗析大致类似。实验扩展了添加离子交换树脂的应用范围。
3.考虑到在大型电渗析器中添加离子交换树脂的复杂性，在中试规模的实验中采用了导离子隔板。导离子隔板由异相阳离子交换膜雕刻而成。实验结果证明导离子隔板有效降低了操作电压，降低了双极膜电渗析的能耗。实验还对国产双极膜和德国双极膜进行了对比实验，在酒石酸产量，电流效率等方面国产双极膜性能还有待提高。
4.对以上的4个实验进行了经济核算，按照实验规模进行了两两对比。(1)在小试规模下核算结果显示：无论是双极膜电渗析还是传统电渗析，酒石酸总生产成本和能耗成本随电流密度升高都呈上升趋势；添加树脂后酒石酸总生产成本和能耗成本均有显著降低；由于双极膜价格的昂贵，双极膜电渗析生产成本普遍高于普通电渗析生产成本。(2)中试规模下：随着操作电流升高，酒石酸总生产成本和能耗成本都降低；添加导离子隔板降低了酒石酸生产的能耗费用，由于添加导离子隔板后，酒石酸产量有一定程度降低，总生产成本的降低幅度小于能耗成本降低幅度，在部分操作电流下有小幅度升高；使用国产双极膜的成本低于德国双极膜。
5.实验简单考查了双极膜电渗析过程中的污染问题，基本重现了文献的污染现象。无机污染物污染阳离子交换膜，有机污染物污染阴离子交换膜。以腐殖酸为例，随着污染物浓度提高和电流强度提高，污染现象加重。
本文研究结果表明，添加离子交换树脂和导离子隔板，有效降低了双极膜电渗析生产酒石酸的能耗，毫无疑问这项技术也可以扩展到其他有机酸的生产过程中。
Organic acids have extensive and close contact with human life, which arewidely used in food, beverage, pharmaceutical, cosmetic, chemical synthesis andbiochemistry. There are two ways to produce organic acid, chemical synthesis andfermentation. No matter fermentation or chemical synthesis, organic acids separation,concentration, purification is needed in post-processing. Traditional purificationprocesses include sedimentation, acidification, precipitation, crystallization and ionexchange step. Precipitation acidification process consumes large amounts of acid andbase, which also produces large amounts of solid waste. Traditional organic acidproduction and purification of these shortcomings do not meet the requirements ofgreen chemistry and energy saving, there is an urgent need for alternative processes.In order to achieve the goal of energy saving and green chemicals, we need a moreeconomical and environment-friendly technology.
BPED (Bipolar membrane electrodialysis) can be applied to this area. If a directelectrical potential is established between bipolar membrane, water dissociationoccurs at the interphase of it, forming H~+and OH~-. Metal cations and anions of agiven organic salt combine with H~+and OH~-forming alkali and organic acidrespectively. Organic acid produced by this method has high purity, and the cost ofpost-processing is reduced. The alkali, which is by-product, can be applied to theorganic acid fermentation process, in this way it has no secondary pollution.
Tartaric acid production by bipolar membrane is a starting point of this research.We focus on the energy-saving and other common problems of electrodialysis in thispaper, and the main conclusions are as follows:
1. Due to low solubility of potassium hydrogen tartrate in aqueous solution, theconfiguration of experimental membrane stack is BP-A-C. In order to reduce the highresistance of the acid compartment which is caused by the low resolution of tartaricacid, strong acid ion exchange resin is added to the acid compartment.Experimental results show that adding ion exchange membrane reduces the operating voltage andthe energy consumption under the same current density. In some extend, adding ionexchange resin reduce the tartaric acid production. But comparing with the decreaseof energy consumption this method still has a tremendous positive performance.
2. Under the same conditions, we add the ion exchange resins to ED(electrodislysis). The results are similar to the bipolar membrane electrodialysis. Theexperiment extends the application range of adding ion exchange resin.
3. Considering the complexity of adding tiny resin to large-scale electrodialyzer,conductive spacer carved from cation exchange membrane is used in the pilot scaleexperiment. Experimental results show that the conductive spacer effectively reducesthe operating voltage, reducing energy consumption. Comparative experiment iscarried out between the Germany bipolar membrane and domestic bipolar membrane.The results show the tartaric acid yield and current efficiency of domestic bipolarmembrane should be improved in future.
4. The process cost of four experiments is estimated according to theexperimental results, and there is a pair-wise comparison in accordance with theexperimental scale.(1) In small scale the accounting result of process cost show that：no matter BPED or ED, the total production cost increase with the current density;adding resin can reduce the total production cost and energy consumption costsignificantly; the total production cost of BPED is higher than ED,which is caused bythe expensive price of bipolar membrane.(2) In pilot scale, the tatal production costand energy consumption cost decrease with the current rising. The use of conductivespacer reduces the cost of energy consumption, and the decreased range of totalproduction cost is smaller than the decreased range of energy consumption cost,because of the reduce of tartaric acid production after adding the conductivespacer.The cost using domestic bipolar membrane is less than that of Germany bipolarmembrane.
5. We also investigate the problem of pollution in the bipolar membraneelectrodialysis process; the results basically reproduce the phenomenon of pollution inthe literature. Cation exchange membrane is mainly affected by inorganic pollutants, and anion exchange membrane is mainly affected by organic pollutants. For example,the phenomenon of pollution increases with the holmic acid concentration and currentintensity.
The results of this study show that add of ion exchange resin and conductivespacer effectively reduces the energy consumption of tartaric acid production byBPED. There is no doubt that this technology can also be extended to the productionprocess of other organic acids.
引文
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