预处理稻壳流化床燃烧制备纳米SiO_2的小试实验
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摘要
为研究预处理稻壳在流化床中燃烧制备纳米SiO_2工艺可行性,在小型流化床试验台上进行预处理稻壳的燃烧试验,并得到活性稻壳灰样品.采用扫描电镜仪(SEM)、能谱仪(EDS)、透射电镜(TEM)、X射线荧光光谱仪和比表面积及孔径分析仪等设备表征床料和稻壳灰的微观结构和理化特性,深入研究酸预处理对稻壳流化床燃烧状态和稻壳灰性能的改善.结果表明:预处理稻壳在流化床内燃烧状况良好,床料无粘结现象,避免了高温下流化床的团聚问题;所得稻壳灰理化特性大幅提高,稻壳灰由15～50 nm的纳米颗粒聚集而成,并具有丰富的约4 nm的介孔孔隙、≥98%的SiO_2纯度以及≤0.08%的超低残炭质量分数;低温条件下酸预处理可以大幅度消除燃烧温度对稻壳灰性能的制约,但高于800℃时温度制约逐渐显现.酸预处理稻壳流化床燃烧可实现制备高纯高活性稻壳灰的目的,且硫酸预处理效果优于柠檬酸.
To investigate the feasibility of industrial preparation of nano-silica process by pretreated rice husk combustion in fluidized bed, the combustion test of pretreated rice husk was carried out in a bench-scale fluidized bed and active rice husk ash(RHA) samples were obtained. Scanning electron microscopy, energy dispersive spectroscopy, transmission electron microscopy, X-ray fluorescence spectrometer and specific surface area and pore size analyzer were used to characterize the microstructure and physicochemical properties of bed material and RHA, and then the effects of acid pretreatment on the combustion state of rice husk in fluidized bed and the performance of RHA were deeply studied. The results showed that the pretreated rice husk burned well in the bench-scale fluidized bed and the bed material′s agglomeration was not happened. The obtained RHA consisted of 15-50 nm nanoparticles and had abundant mesoporous pores of about 4 nm, SiO_2 purity of higher than 98 wt.% and ultra-low residual carbon content of less than 0.08 wt.%. Acid pretreatment greatly eliminated the limitation of combustion temperature on RHA properties under low temperature condition, however, the temperature constraints gradually appeared when temperature above 800 ℃. In brief, the fluidized bed combustion of acid-pretreated rice husk could achieve the purpose of preparing high purity and high active RHA, and the pretreatment effect of sulfuric acid was better than citric acid.
To investigate the feasibility of industrial preparation of nano-silica process by pretreated rice husk combustion in fluidized bed, the combustion test of pretreated rice husk was carried out in a bench-scale fluidized bed and active rice husk ash(RHA) samples were obtained. Scanning electron microscopy, energy dispersive spectroscopy, transmission electron microscopy, X-ray fluorescence spectrometer and specific surface area and pore size analyzer were used to characterize the microstructure and physicochemical properties of bed material and RHA, and then the effects of acid pretreatment on the combustion state of rice husk in fluidized bed and the performance of RHA were deeply studied. The results showed that the pretreated rice husk burned well in the bench-scale fluidized bed and the bed material′s agglomeration was not happened. The obtained RHA consisted of 15-50 nm nanoparticles and had abundant mesoporous pores of about 4 nm, SiO_2 purity of higher than 98 wt.% and ultra-low residual carbon content of less than 0.08 wt.%. Acid pretreatment greatly eliminated the limitation of combustion temperature on RHA properties under low temperature condition, however, the temperature constraints gradually appeared when temperature above 800 ℃. In brief, the fluidized bed combustion of acid-pretreated rice husk could achieve the purpose of preparing high purity and high active RHA, and the pretreatment effect of sulfuric acid was better than citric acid.
引文
[1] PODE R. Potential applications of rice husk ash waste from rice husk biomass power plant[J]. Renewable and Sustainable Energy Reviews, 2016, 53: 1468. DOI: 10.1016/j.rser.2015.09.051
[2] 胡彦伟,程珙,李浩然,等.化学沉淀法制备纳米SiO2颗粒[J].化工学报, 2016, 67(s1): 379. DOI: 10.11949/j.issn.0438-1157.20160565 HU Yanwei, CHENG Gong, LI Haoran, et al. Synthesis of SiO2 nanoparticles by chemical precipitation[J]. CIESC Journal, 2016, 67(s1): 379. DOI: 10.11949/j.issn.0438-1157.20160565
[3] VENKATANARAYANAN H K, RANGARAJU P R. Effect of grinding of low-carbon rice husk ash on the microstructure and performance properties of blended cement concrete[J]. Cement and Concrete Composites, 2015, 55: 348. DOI: 10.1016/j.cemconcomp.2014.09.021
[4] LIU X, CHEN X, YANG L, et al. A review on recent advances in the comprehensive application of rice husk ash[J]. Research on Chemical Intermediates, 2016, 42(2): 893. DOI: 10.1007/s11164-015-2061-y
[5] LIU N, HUO K, MCDOWELL M T, et al. Rice husks as a sustainable source of nanostructured silicon for high performance Li-ion battery anodes[J]. Scientific Reports, 2013, 3(5): 1919. DOI: 10.1038/srep01919
[6] SUTAS J, MANA A, PITAK L. Effect of rice husk and rice husk ash to properties of bricks[J]. Procedia Engineering, 2012, 32: 1061. DOI: 10.1016/j.proeng.2012.02.055
[7] JEMBERE A L, FANTA S W. Studies on the synthesis of silica powder from rice husk ash as reinforcement filler in rubber tire tread part: replacement of commercial precipitated silica[J]. International Journal of Materials Science and Applications, 2017, 6(1): 37. DOI: 10.11648/j.ijmsa.20170601.16
[8] GU S, ZHOU J, YU C, et al. A novel two-staged thermal synthesis method of generating nanosilica from rice husk via pre-pyrolysis combined with calcination[J]. Industrial Crops and Products, 2015, 65: 1. DOI: 10.1016/j.indcrop.2014.11.045
[9] KRISHNARAO R V, SUBRAHMANYAM J, JAGADISH KUMAR T. Studies on the formation of black particles in rice husk silica ash[J]. Journal of the European Ceramic Society, 2001, 1: 99. DOI: 10.1016/S0955-2219(00)00170-9
[10]SARANGI M, BHATTACHARYYA S, BEHERA R C. Effect of temperature on morphology and phase transformations of nano-crystalline silica obtained from rice husk[J]. Phase Transitions, 2009, 82(5): 377. DOI: 10.1080/01411590902978502
[11]SHEN J, LIU X, ZHU S, et al. Effects of calcination parameters on the silica phase of original and leached rice husk ash[J]. Materials Letters, 2011, 65(8): 1179. DOI:10.1016/j.matlet.2011.01.034
[12]LIU X, BI X T. Removal of inorganic constituents from pine barks and switchgrass[J]. Fuel Processing Technology, 2011, 92(7): 1273. DOI: 10.1016/j.fuproc.2011.01.016
[13]SALAS A, DELVASTO S, GUTIERREZ R M D, et al. Comparison of two processes for treating rice husk ash for use in high performance concrete[J]. Cement and Concrete Research, 2009, 39(9): 773. DOI: 10.1016/j.cemconres.2009.05.006
[14]ALYOSEF H A, EILERT A, WELSCHER J, et al. Characterization of biogenic silica generated by thermo chemical treatment of rice husk[J]. Paticulate Science and Technology, 2013, 31(5): 524. DOI: 10.1080/02726351.2013.782931
[15]CHEN P, GU W, FANG W, et al. Removal of metal impurities in rice husk and characterization of rice husk ash under simplified acid pretreatment process[J]. Environmental Progress and Sustainable Energy, 2017, 36(3): 830. DOI: 10.1002/ep.12513
[16]李万海, 齐爱玖, 王红. 稻壳制备二氧化硅的研究[J]. 吉林化工学院学报, 2008, 25(3): 47. DOI: 10.3969/j.issn.1007-2853.2008.03.012 LI Wanhai, QI Aijiu, WANG Hong. Study on preparation of silicon dioxide from rice husk[J]. Journal of Jilin Institute of Chemical Technology, 2008, 25(3): 47. DOI: 10.3969/j.issn.1007-2853.2008.03.012
[17]YOON S J, SON Y I, KIM Y K, et al. Gasification and power generation characteristics of rice husk and rice husk pellet using a downdraft fixed-bed gasifier[J]. Renewable Energy , 2012, 42(1): 163. DOI: 10.1016/j.renene.2011.08.028
[18]MADHIYANON T, SATHITRUANGSAK P, SOPONRONNARIT S, et al. Combustion characteristics of rice-husk in a short-combustion-chamber fluidized-bed combustor (SFBC)[J]. Applied Thermal Engineering, 2010, 30(4): 347. DOI: 10.1016/j.applthermaleng.2009.09.014
[19]SAIDUR R, ABDELAZIZ E A, DEMIRBAS A, et al. A review on biomass as a fuel for boilers[J]. Renewable & Sustainable Energy Reviews, 2011, 15(5): 2262. DOI: 10.1016/j.rser.2011.02.015
[20]杜胜磊. 生物质热化学利用过程中无机矿物质转化规律及灰熔融特性研究[D]. 武汉: 华中科技大学, 2014 DU Shenglei. Fundamental study on transformation behavior of inorganic components during thermochemical conversion of biomass and ash fusion characteristics[D]. Wuhan: Huazhong University of Science and Technology, 2014
[21]HUANG S, JING S, WANG J, et al. Silica white obtained from rice husk in a fluidized bed[J]. Powder Technology, 2001, 117(3): 232. DOI: 10.1016/S0032-5910(00)00372-7
[22]WERTHER J, SAENGER M, HARTGE E U, et al.Combustion of agricultural residues[J]. Process in Energy and Combustion Science, 2000, 26(1): 1. DOI: 10.1016/S0360-1285(99)00005-2
[23]CHEN P, BIE H, BIE R. Leaching characteristics and kinetics of the metal impurities present in rice husk during pretreatment for the production of nanosilica particles[J]. Korean Journal of Chemical Engineering, 2018, 35(9): 1911. DOI: 10.1007/s11814-018-0103-z
[24]尚琳琳. 生物质流化床燃烧粘结特性及控制研究[D]. 北京: 中国科学院研究生院(工程热物理研究所), 2012 SHANG Linlin. Study on agglomeration characteristics and counteraction technology of biomass combustion in fluidized bed[D]. Beijing: Graduate University of Chinese Academy of Sciences, 2012
[25]SINGH R I, MOHAPATRA S K, GANGACHARYULU D. Studies in an atmospheric bubbling fluidized-bed combustor of 10 MW power plant based on rice husk[J]. Energy Conversion and Management, 2008, 49(11): 3086. DOI: 10.1016/j.enconman.2008.06.011
[26]陈佩. 稻壳预处理对稻壳灰的影响研究[D]. 哈尔滨: 哈尔滨工业大学, 2014 CHEN Pei. Effect of pretreatment on properties of rice husk ash[D]. Harbin: Harbin Institute of Technology, 2014
[27]LIU Y, GUO Y, ZHU Y, et al. A sustainable route for the preparation of activated carbon and silica from rice husk ash[J]. Journal of Hazardous Materials, 2011, 186(2/3): 1314. DOI: 10.1016/j.jhazmat.2010.12.007
[28]GU S, ZHOU J, LUO Z, et al. A detailed study of the effects of pyrolysis temperature and feedstock particle size on the preparation of nanosilica from rice husk[J]. Industrial Crops and Products, 2013, 50(4): 540. DOI:10.1016/j.indcrop.2013.08.004
[2] 胡彦伟,程珙,李浩然,等.化学沉淀法制备纳米SiO2颗粒[J].化工学报, 2016, 67(s1): 379. DOI: 10.11949/j.issn.0438-1157.20160565 HU Yanwei, CHENG Gong, LI Haoran, et al. Synthesis of SiO2 nanoparticles by chemical precipitation[J]. CIESC Journal, 2016, 67(s1): 379. DOI: 10.11949/j.issn.0438-1157.20160565
[3] VENKATANARAYANAN H K, RANGARAJU P R. Effect of grinding of low-carbon rice husk ash on the microstructure and performance properties of blended cement concrete[J]. Cement and Concrete Composites, 2015, 55: 348. DOI: 10.1016/j.cemconcomp.2014.09.021
[4] LIU X, CHEN X, YANG L, et al. A review on recent advances in the comprehensive application of rice husk ash[J]. Research on Chemical Intermediates, 2016, 42(2): 893. DOI: 10.1007/s11164-015-2061-y
[5] LIU N, HUO K, MCDOWELL M T, et al. Rice husks as a sustainable source of nanostructured silicon for high performance Li-ion battery anodes[J]. Scientific Reports, 2013, 3(5): 1919. DOI: 10.1038/srep01919
[6] SUTAS J, MANA A, PITAK L. Effect of rice husk and rice husk ash to properties of bricks[J]. Procedia Engineering, 2012, 32: 1061. DOI: 10.1016/j.proeng.2012.02.055
[7] JEMBERE A L, FANTA S W. Studies on the synthesis of silica powder from rice husk ash as reinforcement filler in rubber tire tread part: replacement of commercial precipitated silica[J]. International Journal of Materials Science and Applications, 2017, 6(1): 37. DOI: 10.11648/j.ijmsa.20170601.16
[8] GU S, ZHOU J, YU C, et al. A novel two-staged thermal synthesis method of generating nanosilica from rice husk via pre-pyrolysis combined with calcination[J]. Industrial Crops and Products, 2015, 65: 1. DOI: 10.1016/j.indcrop.2014.11.045
[9] KRISHNARAO R V, SUBRAHMANYAM J, JAGADISH KUMAR T. Studies on the formation of black particles in rice husk silica ash[J]. Journal of the European Ceramic Society, 2001, 1: 99. DOI: 10.1016/S0955-2219(00)00170-9
[10]SARANGI M, BHATTACHARYYA S, BEHERA R C. Effect of temperature on morphology and phase transformations of nano-crystalline silica obtained from rice husk[J]. Phase Transitions, 2009, 82(5): 377. DOI: 10.1080/01411590902978502
[11]SHEN J, LIU X, ZHU S, et al. Effects of calcination parameters on the silica phase of original and leached rice husk ash[J]. Materials Letters, 2011, 65(8): 1179. DOI:10.1016/j.matlet.2011.01.034
[12]LIU X, BI X T. Removal of inorganic constituents from pine barks and switchgrass[J]. Fuel Processing Technology, 2011, 92(7): 1273. DOI: 10.1016/j.fuproc.2011.01.016
[13]SALAS A, DELVASTO S, GUTIERREZ R M D, et al. Comparison of two processes for treating rice husk ash for use in high performance concrete[J]. Cement and Concrete Research, 2009, 39(9): 773. DOI: 10.1016/j.cemconres.2009.05.006
[14]ALYOSEF H A, EILERT A, WELSCHER J, et al. Characterization of biogenic silica generated by thermo chemical treatment of rice husk[J]. Paticulate Science and Technology, 2013, 31(5): 524. DOI: 10.1080/02726351.2013.782931
[15]CHEN P, GU W, FANG W, et al. Removal of metal impurities in rice husk and characterization of rice husk ash under simplified acid pretreatment process[J]. Environmental Progress and Sustainable Energy, 2017, 36(3): 830. DOI: 10.1002/ep.12513
[16]李万海, 齐爱玖, 王红. 稻壳制备二氧化硅的研究[J]. 吉林化工学院学报, 2008, 25(3): 47. DOI: 10.3969/j.issn.1007-2853.2008.03.012 LI Wanhai, QI Aijiu, WANG Hong. Study on preparation of silicon dioxide from rice husk[J]. Journal of Jilin Institute of Chemical Technology, 2008, 25(3): 47. DOI: 10.3969/j.issn.1007-2853.2008.03.012
[17]YOON S J, SON Y I, KIM Y K, et al. Gasification and power generation characteristics of rice husk and rice husk pellet using a downdraft fixed-bed gasifier[J]. Renewable Energy , 2012, 42(1): 163. DOI: 10.1016/j.renene.2011.08.028
[18]MADHIYANON T, SATHITRUANGSAK P, SOPONRONNARIT S, et al. Combustion characteristics of rice-husk in a short-combustion-chamber fluidized-bed combustor (SFBC)[J]. Applied Thermal Engineering, 2010, 30(4): 347. DOI: 10.1016/j.applthermaleng.2009.09.014
[19]SAIDUR R, ABDELAZIZ E A, DEMIRBAS A, et al. A review on biomass as a fuel for boilers[J]. Renewable & Sustainable Energy Reviews, 2011, 15(5): 2262. DOI: 10.1016/j.rser.2011.02.015
[20]杜胜磊. 生物质热化学利用过程中无机矿物质转化规律及灰熔融特性研究[D]. 武汉: 华中科技大学, 2014 DU Shenglei. Fundamental study on transformation behavior of inorganic components during thermochemical conversion of biomass and ash fusion characteristics[D]. Wuhan: Huazhong University of Science and Technology, 2014
[21]HUANG S, JING S, WANG J, et al. Silica white obtained from rice husk in a fluidized bed[J]. Powder Technology, 2001, 117(3): 232. DOI: 10.1016/S0032-5910(00)00372-7
[22]WERTHER J, SAENGER M, HARTGE E U, et al.Combustion of agricultural residues[J]. Process in Energy and Combustion Science, 2000, 26(1): 1. DOI: 10.1016/S0360-1285(99)00005-2
[23]CHEN P, BIE H, BIE R. Leaching characteristics and kinetics of the metal impurities present in rice husk during pretreatment for the production of nanosilica particles[J]. Korean Journal of Chemical Engineering, 2018, 35(9): 1911. DOI: 10.1007/s11814-018-0103-z
[24]尚琳琳. 生物质流化床燃烧粘结特性及控制研究[D]. 北京: 中国科学院研究生院(工程热物理研究所), 2012 SHANG Linlin. Study on agglomeration characteristics and counteraction technology of biomass combustion in fluidized bed[D]. Beijing: Graduate University of Chinese Academy of Sciences, 2012
[25]SINGH R I, MOHAPATRA S K, GANGACHARYULU D. Studies in an atmospheric bubbling fluidized-bed combustor of 10 MW power plant based on rice husk[J]. Energy Conversion and Management, 2008, 49(11): 3086. DOI: 10.1016/j.enconman.2008.06.011
[26]陈佩. 稻壳预处理对稻壳灰的影响研究[D]. 哈尔滨: 哈尔滨工业大学, 2014 CHEN Pei. Effect of pretreatment on properties of rice husk ash[D]. Harbin: Harbin Institute of Technology, 2014
[27]LIU Y, GUO Y, ZHU Y, et al. A sustainable route for the preparation of activated carbon and silica from rice husk ash[J]. Journal of Hazardous Materials, 2011, 186(2/3): 1314. DOI: 10.1016/j.jhazmat.2010.12.007
[28]GU S, ZHOU J, LUO Z, et al. A detailed study of the effects of pyrolysis temperature and feedstock particle size on the preparation of nanosilica from rice husk[J]. Industrial Crops and Products, 2013, 50(4): 540. DOI:10.1016/j.indcrop.2013.08.004