烟气脱硫石膏中杂质离子对其结构与性能的影响
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摘要
烟气脱硫石膏是火电厂采用湿法烟气脱硫技术的副产物。近年来，随着我国以湿法烟气脱硫为主流技术的大力实施推广，烟气脱硫石膏的排放量与日俱增。然由于烟气脱硫石膏中可溶性杂质对其性能的不利影响，烟气脱硫石膏在诸多建材领域的资源化利用受阻。鉴于此，本文首先就烟气脱硫石膏的物化特性及所含杂质的影响展开了研究。在此基础上，通过实验室模拟烟气脱硫过程制备了未掺杂及掺不同量杂质的合成石膏，研究了不同杂质对模拟合成石膏的结构、热脱水动力学及水化硬化性能等方面的影响，探讨了本文研究结果对烟气脱硫石膏实际应用的指导作用。
烟气脱硫石膏所含可溶性杂质主要包括钠离子、镁离子、氯离子等。其中，部分钠离子存在于烟气脱硫石膏的液相包含物中，部分钠离子和镁离子进入了烟气脱硫石膏晶体中；大部分氯离子存在于烟气脱硫石膏的液相包含物中。烟气脱硫石膏主要呈短柱状，存在表面光滑致密型和表面不平整型两种形貌。烟气脱硫石膏的两步脱水反应均遵循Avrami-Erofeev方程。较高含量的钠离子和氯离子共同作用缩短了烟气脱硫石膏水化放热的加速期，加快了半水石膏的溶解速率，导致其凝结时间大幅缩短，抗压强度降低。0.24%~0.67%含量的镁离子对烟气脱硫石膏的凝结时间无明显影响，1.1%含量的镁离子延长烟气脱硫石膏的凝结时间。
采用XRD和ESEM等测试手段研究了钠离子、镁离子和氯离子对模拟合成石膏结构及形貌的影响。结果表明，三种杂质基本未对模拟合成石膏的晶胞参数产生影响。未掺杂模拟合成石膏有两种不同的形貌特征：即表面光滑致密型和表面由许多不同长径比的小石膏微晶单元相互搭接构成型。钠离子、镁离子使模拟合成石膏形貌以表面光滑致密型为主；而氯离子使模拟合成石膏主要以表面突起小微晶组成型为主。与未掺杂模拟合成石膏相比，氯离子使这些小微晶单元由无序搭接变成有序排列。部分钠离子存在于模拟合成石膏的液相包含物中；部分钠离子和大量镁离子可能会通过偶极离子反应稳定存在于模拟合成石膏晶体内水分子的孔隙位置上；氯离子主要存在于液相包含物中。
通过热分析法研究了钠离子、镁离子和氯离子对模拟合成石膏热脱水动力学的影响。结果表明，三种杂质均使模拟合成石膏的第一第二脱水反应活化能降低。其中，氯离子的影响效果最为显著。活化能的降低宏观上表现为掺杂石膏脱水温度的下降。三种杂质离子降低模拟合成石膏活化能的原因：包含在液相包含物或石膏晶体水分子中的杂质将随温度的升高逐步脱离液相或水分子位置，进而吸附于石膏晶体表面上能量最高部位，这会增大石膏发生变形和扭曲的程度，增强石膏的结构活性，宏观上表现为活化能降低。
采用电导率仪、等温微量热仪及ESEM等测试手段研究了钠离子、镁离子和氯离子对模拟合成石膏水化硬化性能的影响。结果表明，随钠离子掺量的增大，模拟合成石膏的初终凝结时间逐渐缩短，抗压强度逐步降低。钠离子主要通过加速半水石膏的溶解过程促进水化。抗压强度降低的原因：钠离子使其水化产物形貌由未掺杂的交叉搭接度较高的针棒状，变为交叉搭接度较差的燕尾双生状和不规则片层状。0.5%掺量的镁离子对模拟合成石膏的初凝时间影响甚小，对缩短终凝时间的影响程度稍大；0.9%掺量的镁离子会延长其初终凝时间。镁离子对其抗压强度影响甚微。掺镁模拟合成石膏的水化产物仍以相互交叉搭接度较好的针棒状为主。掺有0.9%镁模拟合成石膏的水化产物表面存在诸多小点，考虑为镁离子在晶体表面的吸附，这些吸附的镁离子可能延缓了半水石膏的水化。0.5%掺量的氯离子通过促进半水石膏的溶解大幅缩短合成石膏的初终凝时间；降低合成石膏的抗压强度。与未掺杂模拟合成石膏相比，掺氯0.5%模拟合成石膏的水化产物主要以结晶接触点较少的短柱状和片层状为主。
Flue gas desulfurization (FGD) gypsum is a by-product, which is produced bywet gas desulphurization in coal-fired power stations. In recent years, with promotionand implement of wet gas desulphurization technology, large quantity of FGDgypsum has been produced. However, owing to impurities existed in FGD gypsum（such as, sodium, magnesium and chloride）, which can be detrimental to thegypsum products, the effective utilization of FGD gypsum hasn’t been carried out. Inview of these problems, the physicochemical characteristics and influence ofimpurities on properties of FGD gypsum were studied. Pure gypsum and gypsumcontaining different impurities were prepared by simulating FGD process atlaboratory. The effect of impurities on structure, thermal dehydration kinetics andhydration and hardening performance of synthetic gypsum were investigated. Theimpact of results on application of FGD gypsum was also briefly discussed
The soluble ions mainly monitored are sodium (Na+), magnesium (Mg2+) andchloride (Cl-) in FGD gypsum. Some sodium ions exist in the gypsum lattice and theother resides in fluid inclusions. Most magnesium ions may exist in the gypsum lattice.Most chloride ions reside in fluid inclusions. FGD gypsum exhibits smooth surfaceand coarse surface. The dehydration reaction of FGD gypsum occurs in two steps,which follow Avrami-Erofeev equation. Interaction of sodium and chloride isbelieved to promote the hemidyate to dihydrate, shorten the setting time and reducecompressive strength. Magnesium ion content from0.24wt%to0.67wt%has no effecton the setting time. In the presence of1.1wt%magnesium ions, the setting time ofgypsum plaster has been retarded.
Effect of impurities (sodium, magnesium and chloride) on the structure andmorphology of synthetic gypsum was studied by XRD and SEM. The results showthat impurities have no effect on the lattice parameter of synthetic gypsum. Puresynthetic gypsum exhibits two different morphological features: compact, smoothsurface and coarse surface made of small gypsum crystal units. Synthetic Gypsumcontaining sodium and magnesium ions exhibits smooth and compact surface.Synthetic gypsum containing chloride shows coarse surface, and chloride ions couldmodified small gypsum crystal units from disordered to certain arrangement. Chlorideexists mainly in the fluid inclusions. Some sodium ions exist in the fluid inclusions. Some sodium and most magnesium ions may reside in interstitial positions amongstructural water molecules by dipole-ion interaction with water.
Effect of impurities (sodium, magnesium and chloride) on thermal dehydrationkinetics of synthetic gypsum was studied by TG-DSC. The results show that theactivation energy of gypsum containing impurities is lower than that of pure gypsum.The activation energy of gypsum containing chloride ions is lower than that of sodiumand magnesium ions. Lower activation energy is responsible for lower dehydrationtemperature. It can be noted that with dehydration temperature increasing, impuritiesexisted in fluid inclusions or interstitial positions among structural water are released,and these impurities are adsorbed at crystal surface of the highest energy. It leads tothe deformation and distortion of gypsum lattice. Consequently synthetic gypsumcontaining impurities exhibits lower activation energy.
Effect of impurities (sodium, magnesium and chloride) on the hydration andhardening performance of synthetic gypsum was studied by conductivity, ICC andSEM. The results show that with an increase of sodium ions concentration, the settingtime is retarded and the compressive strength is reduced, but there is a suddendecrease in sodium ions up to0.5wt%. It is believed that sodium ions acceleratehydration by increasing rate of hemihydrate dissolution. In the presence of sodiumions, gypsum plaster which normally crystallizes into long interlocking needle shapedcrystals has been modified to lath and twin shaped crystals of variable sizes. Thesetwin and lamellar-like crystals are related to poor interlocking structure. Magnesiumions up to0.5wt%have no effect on the initial setting time, and reduce the finalsetting time. In the presence of0.9wt%magnesium ions, the setting time of gypsumplaster has been retarded.There is many pots at the surfaces of gypsum. It is inferedthat magnesium ions are adsorbed at the crystal surfaces of growing gypsum, whichresults in retardation of hemihydrate hydration. In the presence of magnesium ions,the hyration products exhibit interlocking structures. In the presence of0.5wt%chloride, the setting time is retarded, and the compressive strength is reducedconsiderably. The formation of poor lath and tabular shaped crystals are responsiblefor fall in strength.
烟气脱硫石膏所含可溶性杂质主要包括钠离子、镁离子、氯离子等。其中，部分钠离子存在于烟气脱硫石膏的液相包含物中，部分钠离子和镁离子进入了烟气脱硫石膏晶体中；大部分氯离子存在于烟气脱硫石膏的液相包含物中。烟气脱硫石膏主要呈短柱状，存在表面光滑致密型和表面不平整型两种形貌。烟气脱硫石膏的两步脱水反应均遵循Avrami-Erofeev方程。较高含量的钠离子和氯离子共同作用缩短了烟气脱硫石膏水化放热的加速期，加快了半水石膏的溶解速率，导致其凝结时间大幅缩短，抗压强度降低。0.24%~0.67%含量的镁离子对烟气脱硫石膏的凝结时间无明显影响，1.1%含量的镁离子延长烟气脱硫石膏的凝结时间。
采用XRD和ESEM等测试手段研究了钠离子、镁离子和氯离子对模拟合成石膏结构及形貌的影响。结果表明，三种杂质基本未对模拟合成石膏的晶胞参数产生影响。未掺杂模拟合成石膏有两种不同的形貌特征：即表面光滑致密型和表面由许多不同长径比的小石膏微晶单元相互搭接构成型。钠离子、镁离子使模拟合成石膏形貌以表面光滑致密型为主；而氯离子使模拟合成石膏主要以表面突起小微晶组成型为主。与未掺杂模拟合成石膏相比，氯离子使这些小微晶单元由无序搭接变成有序排列。部分钠离子存在于模拟合成石膏的液相包含物中；部分钠离子和大量镁离子可能会通过偶极离子反应稳定存在于模拟合成石膏晶体内水分子的孔隙位置上；氯离子主要存在于液相包含物中。
通过热分析法研究了钠离子、镁离子和氯离子对模拟合成石膏热脱水动力学的影响。结果表明，三种杂质均使模拟合成石膏的第一第二脱水反应活化能降低。其中，氯离子的影响效果最为显著。活化能的降低宏观上表现为掺杂石膏脱水温度的下降。三种杂质离子降低模拟合成石膏活化能的原因：包含在液相包含物或石膏晶体水分子中的杂质将随温度的升高逐步脱离液相或水分子位置，进而吸附于石膏晶体表面上能量最高部位，这会增大石膏发生变形和扭曲的程度，增强石膏的结构活性，宏观上表现为活化能降低。
采用电导率仪、等温微量热仪及ESEM等测试手段研究了钠离子、镁离子和氯离子对模拟合成石膏水化硬化性能的影响。结果表明，随钠离子掺量的增大，模拟合成石膏的初终凝结时间逐渐缩短，抗压强度逐步降低。钠离子主要通过加速半水石膏的溶解过程促进水化。抗压强度降低的原因：钠离子使其水化产物形貌由未掺杂的交叉搭接度较高的针棒状，变为交叉搭接度较差的燕尾双生状和不规则片层状。0.5%掺量的镁离子对模拟合成石膏的初凝时间影响甚小，对缩短终凝时间的影响程度稍大；0.9%掺量的镁离子会延长其初终凝时间。镁离子对其抗压强度影响甚微。掺镁模拟合成石膏的水化产物仍以相互交叉搭接度较好的针棒状为主。掺有0.9%镁模拟合成石膏的水化产物表面存在诸多小点，考虑为镁离子在晶体表面的吸附，这些吸附的镁离子可能延缓了半水石膏的水化。0.5%掺量的氯离子通过促进半水石膏的溶解大幅缩短合成石膏的初终凝时间；降低合成石膏的抗压强度。与未掺杂模拟合成石膏相比，掺氯0.5%模拟合成石膏的水化产物主要以结晶接触点较少的短柱状和片层状为主。
Flue gas desulfurization (FGD) gypsum is a by-product, which is produced bywet gas desulphurization in coal-fired power stations. In recent years, with promotionand implement of wet gas desulphurization technology, large quantity of FGDgypsum has been produced. However, owing to impurities existed in FGD gypsum（such as, sodium, magnesium and chloride）, which can be detrimental to thegypsum products, the effective utilization of FGD gypsum hasn’t been carried out. Inview of these problems, the physicochemical characteristics and influence ofimpurities on properties of FGD gypsum were studied. Pure gypsum and gypsumcontaining different impurities were prepared by simulating FGD process atlaboratory. The effect of impurities on structure, thermal dehydration kinetics andhydration and hardening performance of synthetic gypsum were investigated. Theimpact of results on application of FGD gypsum was also briefly discussed
The soluble ions mainly monitored are sodium (Na+), magnesium (Mg2+) andchloride (Cl-) in FGD gypsum. Some sodium ions exist in the gypsum lattice and theother resides in fluid inclusions. Most magnesium ions may exist in the gypsum lattice.Most chloride ions reside in fluid inclusions. FGD gypsum exhibits smooth surfaceand coarse surface. The dehydration reaction of FGD gypsum occurs in two steps,which follow Avrami-Erofeev equation. Interaction of sodium and chloride isbelieved to promote the hemidyate to dihydrate, shorten the setting time and reducecompressive strength. Magnesium ion content from0.24wt%to0.67wt%has no effecton the setting time. In the presence of1.1wt%magnesium ions, the setting time ofgypsum plaster has been retarded.
Effect of impurities (sodium, magnesium and chloride) on the structure andmorphology of synthetic gypsum was studied by XRD and SEM. The results showthat impurities have no effect on the lattice parameter of synthetic gypsum. Puresynthetic gypsum exhibits two different morphological features: compact, smoothsurface and coarse surface made of small gypsum crystal units. Synthetic Gypsumcontaining sodium and magnesium ions exhibits smooth and compact surface.Synthetic gypsum containing chloride shows coarse surface, and chloride ions couldmodified small gypsum crystal units from disordered to certain arrangement. Chlorideexists mainly in the fluid inclusions. Some sodium ions exist in the fluid inclusions. Some sodium and most magnesium ions may reside in interstitial positions amongstructural water molecules by dipole-ion interaction with water.
Effect of impurities (sodium, magnesium and chloride) on thermal dehydrationkinetics of synthetic gypsum was studied by TG-DSC. The results show that theactivation energy of gypsum containing impurities is lower than that of pure gypsum.The activation energy of gypsum containing chloride ions is lower than that of sodiumand magnesium ions. Lower activation energy is responsible for lower dehydrationtemperature. It can be noted that with dehydration temperature increasing, impuritiesexisted in fluid inclusions or interstitial positions among structural water are released,and these impurities are adsorbed at crystal surface of the highest energy. It leads tothe deformation and distortion of gypsum lattice. Consequently synthetic gypsumcontaining impurities exhibits lower activation energy.
Effect of impurities (sodium, magnesium and chloride) on the hydration andhardening performance of synthetic gypsum was studied by conductivity, ICC andSEM. The results show that with an increase of sodium ions concentration, the settingtime is retarded and the compressive strength is reduced, but there is a suddendecrease in sodium ions up to0.5wt%. It is believed that sodium ions acceleratehydration by increasing rate of hemihydrate dissolution. In the presence of sodiumions, gypsum plaster which normally crystallizes into long interlocking needle shapedcrystals has been modified to lath and twin shaped crystals of variable sizes. Thesetwin and lamellar-like crystals are related to poor interlocking structure. Magnesiumions up to0.5wt%have no effect on the initial setting time, and reduce the finalsetting time. In the presence of0.9wt%magnesium ions, the setting time of gypsumplaster has been retarded.There is many pots at the surfaces of gypsum. It is inferedthat magnesium ions are adsorbed at the crystal surfaces of growing gypsum, whichresults in retardation of hemihydrate hydration. In the presence of magnesium ions,the hyration products exhibit interlocking structures. In the presence of0.5wt%chloride, the setting time is retarded, and the compressive strength is reducedconsiderably. The formation of poor lath and tabular shaped crystals are responsiblefor fall in strength.
引文
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