碱法制浆过程中结垢离子的生成规律及数学模型的建立
摘要
蒸发器钙结垢是制浆造纸碱回收过程中普遍存在的严重问题,它制约着碱回收系统的正常运行。为此,研究者对控制和减少蒸发器钙结垢的产生进行了大量研究。然而,现有的相关研究主要集中在探讨如何除垢以及结垢的形成。关于在制浆过程中形成蒸发器钙结垢的草酸根、碳酸根和溶解钙产生规律的研究报道甚少。而对制浆过程中草酸根和碳酸根来源的研究更为鲜见。基于上述情况,本论文通过新建立的分析方法研究碱法制浆过程中草酸根、碳酸根和钙离子的生成规律及其来源,目的在于通过对制浆过程中碳酸根、草酸根和钙离子生成规律的研究有效地控制制浆废液中容易引起蒸发器钙结垢物质的产生。这对于深化蒸发器钙结垢问题的认识,控制和减少蒸发器的钙结垢程度,提高生产过程的能源利用效率,以及保证生产的正常运行,将具有重要的指导意义。
围绕上述研究目的,本论文采用典型的碱法制浆工艺条件,以南方松和相思木为原料,结合本论文建立的顶空气相色谱法测定制浆废液中草酸根的新方法,揭示了碱法制浆过程中草酸根的生成规律。结果表明,相思木中草酸根的含量高于南方松,约为南方松的6~7倍。在碱法制浆过程中草酸根的形成是随着蒸煮过程的进行而逐渐增加的。在碱法蒸煮的早期阶段草酸根随时间增加的生成速率较快。初始有效碱的浓度越高,蒸煮初期形成的草酸根的量越多。相思木与南方松在相同的条件下进行碱法蒸煮,相思木所产生的草酸根的量高于南方松。研究了主要工艺参数(如时间、H因子、用碱量和硫化度等)对碱法制浆过程中草酸根生成的影响。从而建立描述碱法制浆过程黑液中草酸根生成的动力学数学模型。将该数学模型应用于南方松和相思木碱法制浆过程,其预测值与实验测定值的线性相关系数R2分别为0.981和0.963,这表明其预测具有较高的准确性。同时,还揭示了碱法制浆过程中草酸根的来源,明确了碱法蒸煮过程中除了原料本身会释放溶出一部分草酸根外,木素和碳水化合物的降解也可以产生草酸根。
通过对碱法制浆过程中碳酸根的研究发现,在碱法制浆过程中碳酸根的形成随着蒸煮过程的进行而逐渐增加。相思木与南方松在相同的条件下进行碱法蒸煮,相思木所产生的碳酸根的量高于南方松。根据碳酸根的形成与H-因子和初始有效碱浓度的关系,建立了碱法蒸煮南方松和相思木过程中碳酸根产生的动力学数学模型。该模型的预测值与实验测得值之间有良好的线性关系,证明该数学模型的预测具有较高的准确性。进一步研究表明,在碱法蒸煮过程中木素和碳水化合物的降解都可以产生碳酸根。
通过对不同蒸煮过程中溶解钙的研究揭示了其生成规律,阐述了蒸煮时间、溶解木素、草酸根和碳酸根等对溶解钙离子生成的影响。结果发现:溶解钙离子随着蒸煮时间的增加而增加的,在碱法蒸煮的早期阶段溶解钙随时间增加的速率较快。硫酸盐法蒸煮黑液中溶解性钙离子的浓度大于烧碱法。黑液中溶解钙的含量是与溶出木素的含量成正比与碳酸根和草酸根的含量成反比关系。溶解木素与钙离子的络合稳定常数为102。当黑液中的碳酸根和草酸根总浓度大于0.3mol/L时,可有效地控制黑液中溶解钙的含量。
同时,揭示了氧脱木素过程中草酸根的生成规律,探讨了氧脱木素工艺条件对草酸根生成的影响。研究得出:在氧脱木素过程中草酸根的生成与时间呈线性关系,随着氧脱木素过程的进行草酸根的含量逐渐增加。氧脱木素的温度对草酸根形成有显著的影响,提高温度会增加氧脱木素过程中草酸根的形成。在其它条件相同的情况下,用碱量由2.5%增加至3.5%时,氧脱木素废液中草酸根的含量也有所增加。而氧压对草酸根的形成影响不大。研究了氧脱木素过程中草酸根的形成与溶解木素和卡伯值的关系。根据草酸根的形成与卡伯值的关系,建立氧脱木素过程中草酸根生成的动力学数学模型。该数学模型的预测具有较高的准确性,其预测值和测定值的线性相关系数R2为0.969,可以将其用于给定纸浆的氧脱木素废液中草酸根含量的预测。
此外,还揭示了热水和碱预抽提过程中草酸根和碳酸根的生成规律,探讨了热水和碱预抽提对蒸煮过程中草酸根和碳酸根的形成、黑液性质和纸浆性能的影响。得出:热水和碱预抽提可以减少南方松和相思木碱法制浆黑液中碳酸根和草酸根的含量。通过预抽提可以提高蒸煮过程中有效碱的作用效率,增加木素的溶出,减少制浆过程中甲醇的产生。
本研究不仅有助于改进制浆工艺,建立结合生物质精炼的制浆新模式和控制钙结垢物质的产生,还有利于深化对产生蒸发器钙结垢物质来源的认识,为控制蒸发器钙结垢、提高能源利用效率提供了新的途径。
Calcium scales of evaporator appear to be a serious problem in alkali recovery from black liquors, which restricts the normal operation of alkaline recovery system. Numbers of studies have been done on the control and reduction of calcium scales. However, most of them have focused on scale removal and reasons for scaling. There are few reports on the release or formation of oxalate, carbonate and dissolved calcium and even rarely known about the sources of oxalate and carbonate during the pulping processes. Therefore, the formation and sources of oxalate, carbonate and dissolved calcium were investigated in this work, in order to control these substances formation or release during the pulping processes. The result is significant to deepen the recognition of calcium scales of evaporator, control and reduce evaporator scaling, improve energy efficiency and ensure the normal operation of production.
For these reasons, under typical alkaline pulping conditions, southern pine and acacia were taken as raw materials to reveal the oxalate formation rule, in combination with the novel headspace gas chromatographic method for determination of oxalate in pulping effluents. The results showed that acacia was found to have more oxalate than southern pine, and the oxalate content in acacia wood is 6~7 times as that of southern pine. Also the oxalate content in black liquor was increased during alkaline pulping processes. The trend rapidly increased during the early stages of the cooking. It was found that a higher hydroxide concentration led to a higher oxalate content in the black liquor. The pulping of acacia resulted in more oxalate being formed than that of southern pine under the same pulping conditions. The effect of pulping time, H-Factor, alkaline charge and sulfidity on the oxalate formation was also studied. Then a kinetic model of oxalate formation was developed based on the experimental results. The good regression coefficients (R2 = 0.981 and 0.963 for southern pine and acacia respectively) indicate that the models are justifiable for the oxalate prediction, and applicable to kraft and soda pulping black liquors. These models are reasonable expressions for the concentration of oxalate formed during alkaline pulping. Meanwhile, the oxalate source was revealed during alkaline pulping processes. Oxalate is formed in the pulping process from two main sources, i.e., oxalate and oxalic acid are existed in native wood, formed from lignin and carbohydrate degradation in the cooking.
It was found that the carbonate content in black liquor was increased during alkaline pulping processes. At the same conditions, the pulping of acacia resulted in more carbonate being formed than that of southern pine. The relationships between the carbonate content and H-Factor, as well as the concentration of initial effective alkali were established. And then, a kinetic model of carbonate formation was developed based on the experimental results. The good regression coefficients indicate that the models are justifiable for the carbonate prediction, both for the kraft and soda pulping black liquors. Further investigation showed that carbonate was formed from lignin and carbonate degradation during pulping process
A detailed investigation on the effects of the major compositions of black liquor on the soluble calcium formation was conducted. The studies showed that the content of the soluble calcium in black liquor is mainly affected by the amount of the dissolved lignin and, carbonate and oxalate. The results clearly indicate that dissolved calcium content is negatively correlated with the content of dissolved lignin. The formation constant of the dissolved calcium-lignin complex in this equation is 102. More soluble calcium was found in the kraft pulping spent liquors. The amount of the soluble calcium in cooking liquor can be effectively suppressed when a total concentration of oxalate and carbonate reaches a level of 0.3mol/L in the kraft pulping process.
The rule of oxalate formation was revealed during oxygen delignification. The effects of process conditions of oxygen delignification on oxalate formation were also explored. Results showed that oxalate content in the effluent oxygen delignification increased with increasing time and the relationship between them was linear. The effect of temperature on oxalate formation was significance during oxygen delignification process. The oxalate content in the effluent of oxygen delignification increased with the temperature during oxygen delignification process. At the same conditions, the oxalate content increased when the alkali charge increased from 2.5% to 3.5%. Oxygen pressure had a little effect on oxalate formation. The relationship between the oxalate formation and dissolved lignin and Kappa number was investigated during oxygen delignification process. According to the relationship, a kinetic model of oxalate formation was developed based on the experimental results. There is a good agreement between the calculated and measured data, indicating that this model is reasonable expression for the concentration of oxalate during oxygen delignification. The regression coefficient between the predicted and the measured was 0.969. The empirical models can predict the oxalate content in the effluent of oxygen delignification.
Furthermore, oxalate and carbonate formation rules were also revealed during hot-water and alkaline pre-extraction processes. The effects of hot-water and alkaline pre-extraction on the formation of oxalate and carbonate, characteristics of black liquor and pulp properties were analyzed. The investigation showed that the contents of oxalate and carbonate in black liquor of southern pine and acacia after hot-water and alkaline pre-extract were lower than those of corresponding control alkaline pulping. Hot-water and alkaline pre-extraction can improve action efficiency of effective alkali, increase the lignin solubility and reduce the methanol formation.
This study will promote a new pulping approach of combining pulping with bio-refinery, control the formation of calcium scales and deepen the understanding of the evaporator scaling source, and provide a novel way to control evaporator scaling and increase energy efficiency.
围绕上述研究目的,本论文采用典型的碱法制浆工艺条件,以南方松和相思木为原料,结合本论文建立的顶空气相色谱法测定制浆废液中草酸根的新方法,揭示了碱法制浆过程中草酸根的生成规律。结果表明,相思木中草酸根的含量高于南方松,约为南方松的6~7倍。在碱法制浆过程中草酸根的形成是随着蒸煮过程的进行而逐渐增加的。在碱法蒸煮的早期阶段草酸根随时间增加的生成速率较快。初始有效碱的浓度越高,蒸煮初期形成的草酸根的量越多。相思木与南方松在相同的条件下进行碱法蒸煮,相思木所产生的草酸根的量高于南方松。研究了主要工艺参数(如时间、H因子、用碱量和硫化度等)对碱法制浆过程中草酸根生成的影响。从而建立描述碱法制浆过程黑液中草酸根生成的动力学数学模型。将该数学模型应用于南方松和相思木碱法制浆过程,其预测值与实验测定值的线性相关系数R2分别为0.981和0.963,这表明其预测具有较高的准确性。同时,还揭示了碱法制浆过程中草酸根的来源,明确了碱法蒸煮过程中除了原料本身会释放溶出一部分草酸根外,木素和碳水化合物的降解也可以产生草酸根。
通过对碱法制浆过程中碳酸根的研究发现,在碱法制浆过程中碳酸根的形成随着蒸煮过程的进行而逐渐增加。相思木与南方松在相同的条件下进行碱法蒸煮,相思木所产生的碳酸根的量高于南方松。根据碳酸根的形成与H-因子和初始有效碱浓度的关系,建立了碱法蒸煮南方松和相思木过程中碳酸根产生的动力学数学模型。该模型的预测值与实验测得值之间有良好的线性关系,证明该数学模型的预测具有较高的准确性。进一步研究表明,在碱法蒸煮过程中木素和碳水化合物的降解都可以产生碳酸根。
通过对不同蒸煮过程中溶解钙的研究揭示了其生成规律,阐述了蒸煮时间、溶解木素、草酸根和碳酸根等对溶解钙离子生成的影响。结果发现:溶解钙离子随着蒸煮时间的增加而增加的,在碱法蒸煮的早期阶段溶解钙随时间增加的速率较快。硫酸盐法蒸煮黑液中溶解性钙离子的浓度大于烧碱法。黑液中溶解钙的含量是与溶出木素的含量成正比与碳酸根和草酸根的含量成反比关系。溶解木素与钙离子的络合稳定常数为102。当黑液中的碳酸根和草酸根总浓度大于0.3mol/L时,可有效地控制黑液中溶解钙的含量。
同时,揭示了氧脱木素过程中草酸根的生成规律,探讨了氧脱木素工艺条件对草酸根生成的影响。研究得出:在氧脱木素过程中草酸根的生成与时间呈线性关系,随着氧脱木素过程的进行草酸根的含量逐渐增加。氧脱木素的温度对草酸根形成有显著的影响,提高温度会增加氧脱木素过程中草酸根的形成。在其它条件相同的情况下,用碱量由2.5%增加至3.5%时,氧脱木素废液中草酸根的含量也有所增加。而氧压对草酸根的形成影响不大。研究了氧脱木素过程中草酸根的形成与溶解木素和卡伯值的关系。根据草酸根的形成与卡伯值的关系,建立氧脱木素过程中草酸根生成的动力学数学模型。该数学模型的预测具有较高的准确性,其预测值和测定值的线性相关系数R2为0.969,可以将其用于给定纸浆的氧脱木素废液中草酸根含量的预测。
此外,还揭示了热水和碱预抽提过程中草酸根和碳酸根的生成规律,探讨了热水和碱预抽提对蒸煮过程中草酸根和碳酸根的形成、黑液性质和纸浆性能的影响。得出:热水和碱预抽提可以减少南方松和相思木碱法制浆黑液中碳酸根和草酸根的含量。通过预抽提可以提高蒸煮过程中有效碱的作用效率,增加木素的溶出,减少制浆过程中甲醇的产生。
本研究不仅有助于改进制浆工艺,建立结合生物质精炼的制浆新模式和控制钙结垢物质的产生,还有利于深化对产生蒸发器钙结垢物质来源的认识,为控制蒸发器钙结垢、提高能源利用效率提供了新的途径。
Calcium scales of evaporator appear to be a serious problem in alkali recovery from black liquors, which restricts the normal operation of alkaline recovery system. Numbers of studies have been done on the control and reduction of calcium scales. However, most of them have focused on scale removal and reasons for scaling. There are few reports on the release or formation of oxalate, carbonate and dissolved calcium and even rarely known about the sources of oxalate and carbonate during the pulping processes. Therefore, the formation and sources of oxalate, carbonate and dissolved calcium were investigated in this work, in order to control these substances formation or release during the pulping processes. The result is significant to deepen the recognition of calcium scales of evaporator, control and reduce evaporator scaling, improve energy efficiency and ensure the normal operation of production.
For these reasons, under typical alkaline pulping conditions, southern pine and acacia were taken as raw materials to reveal the oxalate formation rule, in combination with the novel headspace gas chromatographic method for determination of oxalate in pulping effluents. The results showed that acacia was found to have more oxalate than southern pine, and the oxalate content in acacia wood is 6~7 times as that of southern pine. Also the oxalate content in black liquor was increased during alkaline pulping processes. The trend rapidly increased during the early stages of the cooking. It was found that a higher hydroxide concentration led to a higher oxalate content in the black liquor. The pulping of acacia resulted in more oxalate being formed than that of southern pine under the same pulping conditions. The effect of pulping time, H-Factor, alkaline charge and sulfidity on the oxalate formation was also studied. Then a kinetic model of oxalate formation was developed based on the experimental results. The good regression coefficients (R2 = 0.981 and 0.963 for southern pine and acacia respectively) indicate that the models are justifiable for the oxalate prediction, and applicable to kraft and soda pulping black liquors. These models are reasonable expressions for the concentration of oxalate formed during alkaline pulping. Meanwhile, the oxalate source was revealed during alkaline pulping processes. Oxalate is formed in the pulping process from two main sources, i.e., oxalate and oxalic acid are existed in native wood, formed from lignin and carbohydrate degradation in the cooking.
It was found that the carbonate content in black liquor was increased during alkaline pulping processes. At the same conditions, the pulping of acacia resulted in more carbonate being formed than that of southern pine. The relationships between the carbonate content and H-Factor, as well as the concentration of initial effective alkali were established. And then, a kinetic model of carbonate formation was developed based on the experimental results. The good regression coefficients indicate that the models are justifiable for the carbonate prediction, both for the kraft and soda pulping black liquors. Further investigation showed that carbonate was formed from lignin and carbonate degradation during pulping process
A detailed investigation on the effects of the major compositions of black liquor on the soluble calcium formation was conducted. The studies showed that the content of the soluble calcium in black liquor is mainly affected by the amount of the dissolved lignin and, carbonate and oxalate. The results clearly indicate that dissolved calcium content is negatively correlated with the content of dissolved lignin. The formation constant of the dissolved calcium-lignin complex in this equation is 102. More soluble calcium was found in the kraft pulping spent liquors. The amount of the soluble calcium in cooking liquor can be effectively suppressed when a total concentration of oxalate and carbonate reaches a level of 0.3mol/L in the kraft pulping process.
The rule of oxalate formation was revealed during oxygen delignification. The effects of process conditions of oxygen delignification on oxalate formation were also explored. Results showed that oxalate content in the effluent oxygen delignification increased with increasing time and the relationship between them was linear. The effect of temperature on oxalate formation was significance during oxygen delignification process. The oxalate content in the effluent of oxygen delignification increased with the temperature during oxygen delignification process. At the same conditions, the oxalate content increased when the alkali charge increased from 2.5% to 3.5%. Oxygen pressure had a little effect on oxalate formation. The relationship between the oxalate formation and dissolved lignin and Kappa number was investigated during oxygen delignification process. According to the relationship, a kinetic model of oxalate formation was developed based on the experimental results. There is a good agreement between the calculated and measured data, indicating that this model is reasonable expression for the concentration of oxalate during oxygen delignification. The regression coefficient between the predicted and the measured was 0.969. The empirical models can predict the oxalate content in the effluent of oxygen delignification.
Furthermore, oxalate and carbonate formation rules were also revealed during hot-water and alkaline pre-extraction processes. The effects of hot-water and alkaline pre-extraction on the formation of oxalate and carbonate, characteristics of black liquor and pulp properties were analyzed. The investigation showed that the contents of oxalate and carbonate in black liquor of southern pine and acacia after hot-water and alkaline pre-extract were lower than those of corresponding control alkaline pulping. Hot-water and alkaline pre-extraction can improve action efficiency of effective alkali, increase the lignin solubility and reduce the methanol formation.
This study will promote a new pulping approach of combining pulping with bio-refinery, control the formation of calcium scales and deepen the understanding of the evaporator scaling source, and provide a novel way to control evaporator scaling and increase energy efficiency.
引文
[1] Herbert Sixta. Hand Book of Pulp [M]. Weinheim, Germany: Wiley-VCH Verlag GmbH& Co. KGaA, 2006: 973-974
[2]刘秉钺.制浆黑液的碱回收[M].北京:化学工业出版社, 2006:前言
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[10] Gullichsen J., Paulapuro H.. Papermaking Science and Technology, Book 6B: Chemical Pulping [M]. Helsinki: Fapet Oy, 2000: B8-B11
[11] Grace T. M.. Chemical Recovery in the Alkaline Pulping Processes [M]. 3ed Edition. Atlanta: TAPPI press, 1992: 2-3
[12] Gullichsen J., Paulapuro H.. Papermaking Science and Technology, Book 6B: Chemical Pulping [M]. Helsinki: Fapet Oy, 2000: B12-B13
[13] Grace T. M.. Chemical Recovery in the Alkaline Pulping Processes [M]. 3ed Edition. Atlanta: TAPPI press, 1992: 10-11
[14]刘秉钺.制浆黑液的碱回收[M].北京:化学工业出版社, 2006: 10-11
[15] Sixta H.. Hand Book of Pulp [M]. Weinheim, Germany: Wiley-VCH Verlag GmbH& Co. KGaA, 2006: 967-968
[16] Grace T. M.. A Study of Evaporator Scaling in the Alkaline Pulp Industry, Project 3234, Progress Report 1 [R]. Atlanta, GA: The Institute of Paper Chemistry, 1975
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