玻璃配合料窑外预分解与熔化澄清机理的研究
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摘要
近年来为了解决能源日趋紧张以及大气污染加剧的问题,平板玻璃熔窑的单线产量越来越大,目前最高已达1200t/d。但是与此同时,熔窑自身重量、跨度也都随之增大,这对耐火材料、钢结构的性能提出了更高的要求。因此,单纯从扩大单线规模来扩大生产规模,降低能源消耗及减少废气排放已经越来越困难。所以开发出一种新型的、先进的玻璃熔制技术工艺,对我国玻璃产业的进步与发展具有极大的现实意义和价值。本课题提出的玻璃配合料窑外预分解技术是将玻璃配合料中的硅酸盐形成过程从传统的浮法玻璃熔制工艺中全部或部分地“分割”出来,使得配合料在窑外完成碳酸盐的分解,再直接在高温状态下以硅酸盐的形式进入熔窑,并使其在一进入熔窑后,就得到强制熔化。
本文以普通Na2O-CaO-SiO2系平板玻璃为研究对象,利用万能试验机、X射线荧光光谱仪、导热系数仪和差式扫描量热仪等测试手段研究了玻璃配合料由粉状压制成粒状后的性能变化；利用失重分析仪、X射线衍射分析仪、超高温接触角测量仪、偏光显微镜、体视显微镜等测试手段研究了粒状玻璃配合料在775-850℃预分解的变化规律,并通过实验测得反应程度、反应速率常数及反应活化能；用熔化时间、澄清时间、熔化效率及熔化面积等参数对比了粉状、粒状及高温预处理的粒状配合料的熔制性能；理论计算了玻璃配合料的玻璃形成过程热量消耗及熔窑热效率。得到了以下结论：
粉状配合料在775-850℃失重量最大,硅酸盐形成反应最剧烈,1050℃时观察不到晶体二氧化硅的特征衍射峰。当配合料由粉状压制成粒状时,体积密度和导热系数增大,体积气孔率下降,硅酸盐形成反应速率加快,高温熔制的玻璃中未熔固体颗粒及气泡减少。
粒化配合料在从室温升至775-850℃的过程中,随着羧甲基纤维素钠溶液和水玻璃溶液浓度的增大,硅酸盐形成反应速率,抗压碎力、反应程度增大,在850℃保温1h时生成的液相大到足以使生料球之间相互粘连。粒状配合料在775-850℃恒温处理时,随保温时间和粘结剂浓度的增大,抗压碎力、反应程度增大,拟合得到的反应活化能逐渐减小。粒化配合料的熔化时间和澄清时间均低于粉状配合料,随着预处理温度的升高,粒状配合料熔化所需的时间是先增加后降低的,而澄清时间逐渐延长。
随着粒状配合料中二氧化硅粒度减小,在775-850℃预处理后的样品的抗压碎力增大,残留的晶体二氧化硅含量减少,硅酸盐反应活性增大,反应所需要克服的能量势垒降低。未处理的粒状配合料的熔化时间要短于粉状配合料,但长于经高温预分解的粒状配合料。另外,随着二氧化硅粒度的增大,粉状样和生料球在1350-1450℃的熔化时间均延长。
理论计算了粉状玻璃配合料的玻璃形成过程中生成硅酸盐耗热、玻璃形成耗热、玻璃加热到熔化温度耗热、逸出气体加热到熔化温度耗热、水分蒸发耗热及配合料带入的热量。粉状配合料、生料球及熟料球的玻璃形成所需热量差距不大。只用从蓄热室出来的废气预热生料球,还不足以使生料球部分或完全完成硅酸盐形成过程,还需要额外的加入热量。采用配合料窑外预分解技术,产量可从1200.00t/d提高至2159.89t/d,热效率可从40.00%提高至64.70%。
Recently, in order to solve the problem of increasingly nervous energy and atmospheric pollution, the single-line production of glass melting furnace has become larger and larger and the largest has reached1200t/d. However, at the same time, it has found few problems, such as the enlarged furnace weight and span put forward higher requirement of refractory and steel performance. Therefore, it has become more and more difficult to reduce energy consumption and emissions simply by expanding single-line to expand production scale. So developing a novel and advanced glass melting technology has maximal practical significance and value on progress and development of glass industry. The glass batch silicate kiln decomposition technology mentioned in this topic is whole or partly "split" the process of silicate formation from the conventional melting process of float glass. Glass batch would complete the carbonate decomposition process outside the furnace, and then enter the kiln in form of silicate under high temperature, so it would mandatory be melted.
This work set Na2O-CaO-SiO2system flat glass as research object. The performance change of loose glass batch and compacted glass batch was investigated by universal testing machine, X-ray fluorescence spectrometer, thermal conductivity analyzer and Pressure Differential Scanning Calorimetry. The laws in silicate formation of granular glass batch in775-850℃was investigated by gravimetric analyzer tester, X-ray diffraction analyzer, ultra-high temperature contact angle measuring instrument, polarizing microscope and stereo microscope. The degree of reaction, the reaction rate constant and the activation energy were measured. The melting properties of loose glass batch, granulated glass-forming batch and sintered compacted glass batch were contrasted by measuring melting time, fining time, melting efficiency and melting area. Finally, the heat consumption and the thermal efficiency of the furnace during the glass forming process were calculated theoretically. The results were shown as follows:
The weight loss of loose glass batch reached the largest at775-850℃, at this time, silicate formation reaction became dramatic. There were no characteristic diffraction peaks of crystalline silica be observed at1050℃. When glass batch was compressed from loose to a granular, the bulk density and thermal conductivity of batch were increased, and the volume porosity was decreased, meanwhile, the temperature of silicates forming followed towards lower temperatures. The unmelted solid particles and bubbles in high-temperature melting glass were reduced.
In the procedure of granulated glass batch treated from room temperature to775-850℉, as the increasing of sodium carboxymethyl cellulose solution and sodium silicate solution concentration, the temperature of silicate reaction was reduced, the anti-crushing ability and the degree of reaction were increased. The cohesive force between samples was strong enough to bond together when a large amount of liquid phases was produced at850℃for lh. When glass batch was treated in a constant temperature of775-850℃, as the increasing of holding time and concentration of binder, the anti-crushing ability and the degree of reaction were increased, and the calculated activation energy was decreased. The melting time and fining time of granulated glass batch were less than that of loose glass batch. As the increasing of pretreatment temperature, the time for melting granulated glass batch was increased first and then decreased, however, the fining was gradually extended,
As the smaller of silica particle size, the anti-crushing ability of sample treated at775-850℃was increased, the content of residual silica crystal was reduced, the silicate reaction activation was increased, the energy barrier which was needed to overcome was decreased. The melting time of the untreated granulated glass batch was shorter than that of loose glass batch, but longer than that of the treated compacted glass batch. In addition, with the increasing of silica, the melting time of loose glass batch and pellets at1350-1450℃were both extended.
The heat consumption of loose glass batch in the process of glass formation, including the silicate forming heating, the glass forming heating, the heating when glass was heated to melting temperature, the heating when escaping gas was heated to melting temperature, moisture evaporation heating and the heating brought by glass batch, were calculated theoretically. The heat consumption of loose glass batch, the untreated granulated glass batch and sintered granulated glass batch had little difference. Only using the exhaust gas which came from regenerator to preheat granulated glass batch was not enough, because the energy was barely provided to partially or fully completed the process of silicate forming, so it needed extra added heating energy. The output of furnace was increased from1200.00t/d to2159.89t/d and the thermal efficiency of furnace was increased from40.00%to65.70%when using the glass batch silicate kiln decomposition technology.
本文以普通Na2O-CaO-SiO2系平板玻璃为研究对象,利用万能试验机、X射线荧光光谱仪、导热系数仪和差式扫描量热仪等测试手段研究了玻璃配合料由粉状压制成粒状后的性能变化；利用失重分析仪、X射线衍射分析仪、超高温接触角测量仪、偏光显微镜、体视显微镜等测试手段研究了粒状玻璃配合料在775-850℃预分解的变化规律,并通过实验测得反应程度、反应速率常数及反应活化能；用熔化时间、澄清时间、熔化效率及熔化面积等参数对比了粉状、粒状及高温预处理的粒状配合料的熔制性能；理论计算了玻璃配合料的玻璃形成过程热量消耗及熔窑热效率。得到了以下结论：
粉状配合料在775-850℃失重量最大,硅酸盐形成反应最剧烈,1050℃时观察不到晶体二氧化硅的特征衍射峰。当配合料由粉状压制成粒状时,体积密度和导热系数增大,体积气孔率下降,硅酸盐形成反应速率加快,高温熔制的玻璃中未熔固体颗粒及气泡减少。
粒化配合料在从室温升至775-850℃的过程中,随着羧甲基纤维素钠溶液和水玻璃溶液浓度的增大,硅酸盐形成反应速率,抗压碎力、反应程度增大,在850℃保温1h时生成的液相大到足以使生料球之间相互粘连。粒状配合料在775-850℃恒温处理时,随保温时间和粘结剂浓度的增大,抗压碎力、反应程度增大,拟合得到的反应活化能逐渐减小。粒化配合料的熔化时间和澄清时间均低于粉状配合料,随着预处理温度的升高,粒状配合料熔化所需的时间是先增加后降低的,而澄清时间逐渐延长。
随着粒状配合料中二氧化硅粒度减小,在775-850℃预处理后的样品的抗压碎力增大,残留的晶体二氧化硅含量减少,硅酸盐反应活性增大,反应所需要克服的能量势垒降低。未处理的粒状配合料的熔化时间要短于粉状配合料,但长于经高温预分解的粒状配合料。另外,随着二氧化硅粒度的增大,粉状样和生料球在1350-1450℃的熔化时间均延长。
理论计算了粉状玻璃配合料的玻璃形成过程中生成硅酸盐耗热、玻璃形成耗热、玻璃加热到熔化温度耗热、逸出气体加热到熔化温度耗热、水分蒸发耗热及配合料带入的热量。粉状配合料、生料球及熟料球的玻璃形成所需热量差距不大。只用从蓄热室出来的废气预热生料球,还不足以使生料球部分或完全完成硅酸盐形成过程,还需要额外的加入热量。采用配合料窑外预分解技术,产量可从1200.00t/d提高至2159.89t/d,热效率可从40.00%提高至64.70%。
Recently, in order to solve the problem of increasingly nervous energy and atmospheric pollution, the single-line production of glass melting furnace has become larger and larger and the largest has reached1200t/d. However, at the same time, it has found few problems, such as the enlarged furnace weight and span put forward higher requirement of refractory and steel performance. Therefore, it has become more and more difficult to reduce energy consumption and emissions simply by expanding single-line to expand production scale. So developing a novel and advanced glass melting technology has maximal practical significance and value on progress and development of glass industry. The glass batch silicate kiln decomposition technology mentioned in this topic is whole or partly "split" the process of silicate formation from the conventional melting process of float glass. Glass batch would complete the carbonate decomposition process outside the furnace, and then enter the kiln in form of silicate under high temperature, so it would mandatory be melted.
This work set Na2O-CaO-SiO2system flat glass as research object. The performance change of loose glass batch and compacted glass batch was investigated by universal testing machine, X-ray fluorescence spectrometer, thermal conductivity analyzer and Pressure Differential Scanning Calorimetry. The laws in silicate formation of granular glass batch in775-850℃was investigated by gravimetric analyzer tester, X-ray diffraction analyzer, ultra-high temperature contact angle measuring instrument, polarizing microscope and stereo microscope. The degree of reaction, the reaction rate constant and the activation energy were measured. The melting properties of loose glass batch, granulated glass-forming batch and sintered compacted glass batch were contrasted by measuring melting time, fining time, melting efficiency and melting area. Finally, the heat consumption and the thermal efficiency of the furnace during the glass forming process were calculated theoretically. The results were shown as follows:
The weight loss of loose glass batch reached the largest at775-850℃, at this time, silicate formation reaction became dramatic. There were no characteristic diffraction peaks of crystalline silica be observed at1050℃. When glass batch was compressed from loose to a granular, the bulk density and thermal conductivity of batch were increased, and the volume porosity was decreased, meanwhile, the temperature of silicates forming followed towards lower temperatures. The unmelted solid particles and bubbles in high-temperature melting glass were reduced.
In the procedure of granulated glass batch treated from room temperature to775-850℉, as the increasing of sodium carboxymethyl cellulose solution and sodium silicate solution concentration, the temperature of silicate reaction was reduced, the anti-crushing ability and the degree of reaction were increased. The cohesive force between samples was strong enough to bond together when a large amount of liquid phases was produced at850℃for lh. When glass batch was treated in a constant temperature of775-850℃, as the increasing of holding time and concentration of binder, the anti-crushing ability and the degree of reaction were increased, and the calculated activation energy was decreased. The melting time and fining time of granulated glass batch were less than that of loose glass batch. As the increasing of pretreatment temperature, the time for melting granulated glass batch was increased first and then decreased, however, the fining was gradually extended,
As the smaller of silica particle size, the anti-crushing ability of sample treated at775-850℃was increased, the content of residual silica crystal was reduced, the silicate reaction activation was increased, the energy barrier which was needed to overcome was decreased. The melting time of the untreated granulated glass batch was shorter than that of loose glass batch, but longer than that of the treated compacted glass batch. In addition, with the increasing of silica, the melting time of loose glass batch and pellets at1350-1450℃were both extended.
The heat consumption of loose glass batch in the process of glass formation, including the silicate forming heating, the glass forming heating, the heating when glass was heated to melting temperature, the heating when escaping gas was heated to melting temperature, moisture evaporation heating and the heating brought by glass batch, were calculated theoretically. The heat consumption of loose glass batch, the untreated granulated glass batch and sintered granulated glass batch had little difference. Only using the exhaust gas which came from regenerator to preheat granulated glass batch was not enough, because the energy was barely provided to partially or fully completed the process of silicate forming, so it needed extra added heating energy. The output of furnace was increased from1200.00t/d to2159.89t/d and the thermal efficiency of furnace was increased from40.00%to65.70%when using the glass batch silicate kiln decomposition technology.
引文
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