造纸污泥灰煤矿充填胶凝材料配比试验研究
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摘要
以造纸污泥灰、硫铝酸盐水泥熟料配制煤矿充填胶凝材料,研究悬浮增稠剂、激发剂、料浆水固比对胶凝材料强度、保水性、流动性的影响,并利用X射线衍射、扫描电镜和能谱分析表征手段对水化产物进行微观分析。结果表明,当羟丙基甲基纤维素掺量0.2%～0.3%,碱性激发剂A掺量1.8%,脱硫石膏掺量4%,早强剂B掺量0.9%,水固比为1.3时,充填胶凝材料可同时满足泵送及强度要求。胶凝材料水化产物以针状钙矾石晶体,云朵状无定型水化硅(铝)酸钙凝胶及少量片状单硫型水化硫铝酸钙晶体为主,随龄期增长,钙矾石由细针状和纤维状发育成棒状和柱状,水化硅(铝)酸钙凝胶生成量不断增加并连接成整体,钙矾石及单硫型水化硫铝酸钙填充于凝胶孔隙中,使得充填试样微观结构更加紧凑,抗压强度进一步提高。
The given article is inclined to study the effect of the suspended thickener,the activator and slurry water-solid ratio on the strength,the water-retaining property and fluidity of the cementitious materials by using the paper mill sludge ash and the sulpho-aluminate cement clinker through the so-called single factor experiment and the orthogonal experiment.At the same time,it has also done an analysis of the mineral composition and micromorphology of the hydration products by X-ray diffraction,electronic scanning microscopy and energy spectrum recognition.The results of our experiment and analysis indicate that,when added with hydroxypropyl methyl cellulose at the percentage of 0.2%(0.3%,the alkali-activator A may tend to set up at 1.8%,while the flue gas desulfurization gypsum should be chosen at 4%with the early strength agent B being set up at 0.9% in a watersolid ratio of 1 to 3.It is just based on such a condition that the strengths of the cementitious materials for filling can be made to reach 0.87 MPa,1.77 MPa and 3.25 MPa,respectively,for the 1st,3rd and 28th day.At the same time,the bleeding rate can be made to reduce to no more than 3% and the expansion degree can be made to reach 148 mm.Furthermore,all the illustrated indicative parameters should be made to come up to meet the demands for pumping and strengthening simultaneously.Besides,the hydration products of the proposed cementitious material should be well-made by the needle-like ettringite crystal,the cloud-like amorphous calcium silicate(aluminate) hydrates gel with a little flake single sulfur hydrated calcium sulfoaluminate crystal.Besides,it is also necessary to point it out that the ettringite has to be formulated during the early stage of hydration reaction,which should also be demanded to make an outstanding contribution to the improvement of the early strength of filling materials.With the age-long increase,the shape of the ettringite may evolve and develop into rods and columns from fine needle shapes.However,with the consumption of gypsum dehydrate,part of ettringite may get decomposed into mono-sulfur hydrated calcium sulphoaluminate.Furthermore,catalyzed by the alkaline activator,a kind of reaction,tends to take place in large amounts of active Al_2O_3 and SiO_2 in the sludge ash glass phase with Ca2+ in the soluble state,so as to result in a constantly increasing form of calcium silicate(aluminate) hydrates gel and making them into an integrated entity.Hence,the ettringite and single sulfur hydrated calcium sulfoaluminate filled in gel pores may tend to make the microstructure of filling sample more compact and further enhance its compressive strength.
The given article is inclined to study the effect of the suspended thickener,the activator and slurry water-solid ratio on the strength,the water-retaining property and fluidity of the cementitious materials by using the paper mill sludge ash and the sulpho-aluminate cement clinker through the so-called single factor experiment and the orthogonal experiment.At the same time,it has also done an analysis of the mineral composition and micromorphology of the hydration products by X-ray diffraction,electronic scanning microscopy and energy spectrum recognition.The results of our experiment and analysis indicate that,when added with hydroxypropyl methyl cellulose at the percentage of 0.2%(0.3%,the alkali-activator A may tend to set up at 1.8%,while the flue gas desulfurization gypsum should be chosen at 4%with the early strength agent B being set up at 0.9% in a watersolid ratio of 1 to 3.It is just based on such a condition that the strengths of the cementitious materials for filling can be made to reach 0.87 MPa,1.77 MPa and 3.25 MPa,respectively,for the 1st,3rd and 28th day.At the same time,the bleeding rate can be made to reduce to no more than 3% and the expansion degree can be made to reach 148 mm.Furthermore,all the illustrated indicative parameters should be made to come up to meet the demands for pumping and strengthening simultaneously.Besides,the hydration products of the proposed cementitious material should be well-made by the needle-like ettringite crystal,the cloud-like amorphous calcium silicate(aluminate) hydrates gel with a little flake single sulfur hydrated calcium sulfoaluminate crystal.Besides,it is also necessary to point it out that the ettringite has to be formulated during the early stage of hydration reaction,which should also be demanded to make an outstanding contribution to the improvement of the early strength of filling materials.With the age-long increase,the shape of the ettringite may evolve and develop into rods and columns from fine needle shapes.However,with the consumption of gypsum dehydrate,part of ettringite may get decomposed into mono-sulfur hydrated calcium sulphoaluminate.Furthermore,catalyzed by the alkaline activator,a kind of reaction,tends to take place in large amounts of active Al_2O_3 and SiO_2 in the sludge ash glass phase with Ca2+ in the soluble state,so as to result in a constantly increasing form of calcium silicate(aluminate) hydrates gel and making them into an integrated entity.Hence,the ettringite and single sulfur hydrated calcium sulfoaluminate filled in gel pores may tend to make the microstructure of filling sample more compact and further enhance its compressive strength.
引文
[1]JIANG Juan,MA Xiaoqian.Experimental research of microwave pyrolysis about paper mill sludge[J].Applied Thermal Engineering.2011,31:3897-3903.
[2]CHEN Shan(陈珊),LIU Yan(刘妍),CHEN Qi(陈齐),et al.Effect of applied paper mill sludge on migration of Cd in soil-white radish system[J].Chinese Journal of Environmental Engineering(环境工程学报),2017,11(3):1907-1910.
[3]ZHANG Tuo(张拓),HAN Qing(韩卿),LI Xinping(李新平).Research progress on biorefining and filler utilization of papermaking sludge[J].Paper Science&Technology(造纸科学与技术),2017,36(4):86-90.
[4]HU Z S,DENG Y L.Supersaturation control in aragonite synthesis using sparingly soluble calcium sulfate as reactants[J].Colloid and Interface Science,2003,266(2):359-365.
[5]YUAN Yanyan(袁言言),HUANG Ying(黄瑛),ZHANG Dong(张冬).Energy utilization and pollutants emission in sewage sludge incineration[J].Chinese Journal of Environmental Engineering(环境工程学报),2017,39(3):12-15.
[6]WEI Guoxia(魏国侠),LIU Hanqiao(刘汉桥),XU Xian(徐仙).Glass-ceramics made by ash from sludge incinerator[J].China Ceramics(中国陶瓷),2015,51(5):46-49.
[7]JAMSHIDI M.Mechanical performance and capillary water absorption of sewage sludge ash concrete(SSAC)[J].International Journal of Sustainable Engineering,2012,5(3):227-228.
[8]MACPHEE D E,TAYLOR A H.Preliminary studies on the utilisation of blast-furnace slag(BFS)in mine backfill including an assessment of an air-quenched slag[J].Transactions of the Institution of Engineers,1991,33(4):299-302.
[9]WANG A L,Ma L Q,WANG Z W,et al.Soil and water conservation in mining area based on ground surface subsidence control:development of a high-water swelling material and its application in backfilling mining[J].Environmental Earth Sciences,2016,75:779-783.
[10]YI Hongwei(易宏伟),ZHOU Huaqiang(周华强),ZHANG Lianxin(张连信).Study on the basic properties of high water ash filling material[J].Ground Pressure and Strata Control(矿山压力与顶板管理),1991,4:13-17.
[11]LI Keqing(李克庆),FENG Lin(冯琳),GAO Shujie(高术杰).Preparation of cementitious materials for backfilling by using nickel slag[J].Chinese Journal of Engineering(工程科学学报),2015,37(1):1-6.
[12]WANG Youtuan(王有团),YANG Zhiqiang(杨志强),LI Maohui(李茂辉).Preparation of new backfill cementitious materials with unclassified tailings-rod milling sands[J].Chinese Journal of Materials Research(材料研究学报),2015,29(4):292-296.
[13]HUANG Di(黄迪),NI Wen(倪文),ZHU Liping(祝丽萍).Paste backfilling material prepared with red mud from sintering process and unclassified tailings[J].Journal of University of Science and Technology Beijing(北京科技大学学报),2012,34(3):246-249.
[14]ZHU Jian(朱健),WANG Ping(王平),LEI Mingjing(雷明婧).Adsorption behavior and characteristics of Cu2+,Zn2+,Mn2+onto diatomite in liquid/solid system[J].Acta Scientiae Circumstantiae(环境科学学报),2017,7(9):3370-3374.
[15]ZHAO Caizhi(赵才智).Study on coal mine new paste filling material properties and its application(煤矿新型膏体充填材料性能及其应用研究)[D].Xuzhou:China University of Mining and Technology,2008.
[16]WANG Peiming(王培铭),ZHAO Guorong(赵国荣),ZHANGGuofang(张国防).Mechanism on water retention and thickening of cellulose ethers in fresh mortars[J].Journal of the Chinese Ceramic Society(硅酸盐学报),2017,45(8):1190-1195.
[17]FENG Guorui(冯国瑞),REN Yafeng(任亚峰),ZHANG Xuyan(张绪言).The activating experimental research of fly ash for mining filling material in Tashan Mine[J].Journal of China Coal Society(煤炭学报),2011,36(5):272-275.
[18]DONG Jingliang(董晶亮),ZHANG Tingting(张婷婷),WANGLijiu(王立久).Alkali-activated modified steel slag/pishasandstone composites[J].Acta Materiae Compositae Sinica(复合材料学报),2016,33(1):132-135.
[19]SHI Di(史迪),ZHANG Wensheng(张文生),YE Jiayuan(叶家元).Effects of curing condition on properties,reaction products and microstructure of calcium silicate slag-based alkali-activated cementitious materials[J].Journal of the Chinese Ceramic Society(硅酸盐学报),2017,45(8):1080-1085.
[20]JIANG Guanzhao(姜关照),WU Aixiang(吴爱祥),WANGYiming(王贻明),et al.Effect of compound activator on copper slag activity and preparation of filling materials[J].Chinese Journal of Engineering(工程科学学报),2017,39(9):1305-1312.
[21]FENG Guangming(冯光明),DING Yu(丁玉),ZHU Hongju(朱红菊),et al.Experimental research on a super high-water packing material for mining[J].Journal of China University of Mining&Technology(煤炭学报),2010,39(6):813-819.
[22]LIAO Yishun(廖宜顺),LIU Chuming(刘楚明),KANG Shuang(康爽),et al.Effect of mineral admixtures on the hydration of sulphoaluminate cement under seawater condition[J].Bulletin of the Chinese Ceramic Society(硅酸盐通报),2017,36(4):1333-1336.
[23]WANG Peiming(王培铭),LI Nan(李楠),XU Linglin(徐玲琳).Hydration characteristics and strength development of sulphoaluminate cement cured at low temperature[J].Journal of the Chinese Ceramic Society(硅酸盐学报),2017,45(2):242-246.
[24]XU Linglin(徐玲琳),ZHOU Xiangyi(周向艺),LI Nan(李楠),Impact of calcium sulfate on hydration features of calcium sulfoaluminate cement[J].Journal of Tongji University:Natural Science(同济大学学报:自然科学版),2017,45(6):885-888.
[25]CHANG Jun(常钧),ZHANG Yangyang(张洋洋),SHANGXiaopeng(尚小朋).Effects of ah3 phase content and hydration degree on the strength of calcium sulfoaluminate cement[J].Journal of Building Materials(建筑材料学报),2016,19(6):1028-1031.
[26]GAO Shujie(高术杰),NI Wen(倪文),LI Keqing(李克庆),et al.Reparation and hydrated mechanism of mine filling material of water-granulated secondary nickel slag[J].Journal of the Chinese Ceramic Society(硅酸盐学报),2013,41(5):612-615.
[2]CHEN Shan(陈珊),LIU Yan(刘妍),CHEN Qi(陈齐),et al.Effect of applied paper mill sludge on migration of Cd in soil-white radish system[J].Chinese Journal of Environmental Engineering(环境工程学报),2017,11(3):1907-1910.
[3]ZHANG Tuo(张拓),HAN Qing(韩卿),LI Xinping(李新平).Research progress on biorefining and filler utilization of papermaking sludge[J].Paper Science&Technology(造纸科学与技术),2017,36(4):86-90.
[4]HU Z S,DENG Y L.Supersaturation control in aragonite synthesis using sparingly soluble calcium sulfate as reactants[J].Colloid and Interface Science,2003,266(2):359-365.
[5]YUAN Yanyan(袁言言),HUANG Ying(黄瑛),ZHANG Dong(张冬).Energy utilization and pollutants emission in sewage sludge incineration[J].Chinese Journal of Environmental Engineering(环境工程学报),2017,39(3):12-15.
[6]WEI Guoxia(魏国侠),LIU Hanqiao(刘汉桥),XU Xian(徐仙).Glass-ceramics made by ash from sludge incinerator[J].China Ceramics(中国陶瓷),2015,51(5):46-49.
[7]JAMSHIDI M.Mechanical performance and capillary water absorption of sewage sludge ash concrete(SSAC)[J].International Journal of Sustainable Engineering,2012,5(3):227-228.
[8]MACPHEE D E,TAYLOR A H.Preliminary studies on the utilisation of blast-furnace slag(BFS)in mine backfill including an assessment of an air-quenched slag[J].Transactions of the Institution of Engineers,1991,33(4):299-302.
[9]WANG A L,Ma L Q,WANG Z W,et al.Soil and water conservation in mining area based on ground surface subsidence control:development of a high-water swelling material and its application in backfilling mining[J].Environmental Earth Sciences,2016,75:779-783.
[10]YI Hongwei(易宏伟),ZHOU Huaqiang(周华强),ZHANG Lianxin(张连信).Study on the basic properties of high water ash filling material[J].Ground Pressure and Strata Control(矿山压力与顶板管理),1991,4:13-17.
[11]LI Keqing(李克庆),FENG Lin(冯琳),GAO Shujie(高术杰).Preparation of cementitious materials for backfilling by using nickel slag[J].Chinese Journal of Engineering(工程科学学报),2015,37(1):1-6.
[12]WANG Youtuan(王有团),YANG Zhiqiang(杨志强),LI Maohui(李茂辉).Preparation of new backfill cementitious materials with unclassified tailings-rod milling sands[J].Chinese Journal of Materials Research(材料研究学报),2015,29(4):292-296.
[13]HUANG Di(黄迪),NI Wen(倪文),ZHU Liping(祝丽萍).Paste backfilling material prepared with red mud from sintering process and unclassified tailings[J].Journal of University of Science and Technology Beijing(北京科技大学学报),2012,34(3):246-249.
[14]ZHU Jian(朱健),WANG Ping(王平),LEI Mingjing(雷明婧).Adsorption behavior and characteristics of Cu2+,Zn2+,Mn2+onto diatomite in liquid/solid system[J].Acta Scientiae Circumstantiae(环境科学学报),2017,7(9):3370-3374.
[15]ZHAO Caizhi(赵才智).Study on coal mine new paste filling material properties and its application(煤矿新型膏体充填材料性能及其应用研究)[D].Xuzhou:China University of Mining and Technology,2008.
[16]WANG Peiming(王培铭),ZHAO Guorong(赵国荣),ZHANGGuofang(张国防).Mechanism on water retention and thickening of cellulose ethers in fresh mortars[J].Journal of the Chinese Ceramic Society(硅酸盐学报),2017,45(8):1190-1195.
[17]FENG Guorui(冯国瑞),REN Yafeng(任亚峰),ZHANG Xuyan(张绪言).The activating experimental research of fly ash for mining filling material in Tashan Mine[J].Journal of China Coal Society(煤炭学报),2011,36(5):272-275.
[18]DONG Jingliang(董晶亮),ZHANG Tingting(张婷婷),WANGLijiu(王立久).Alkali-activated modified steel slag/pishasandstone composites[J].Acta Materiae Compositae Sinica(复合材料学报),2016,33(1):132-135.
[19]SHI Di(史迪),ZHANG Wensheng(张文生),YE Jiayuan(叶家元).Effects of curing condition on properties,reaction products and microstructure of calcium silicate slag-based alkali-activated cementitious materials[J].Journal of the Chinese Ceramic Society(硅酸盐学报),2017,45(8):1080-1085.
[20]JIANG Guanzhao(姜关照),WU Aixiang(吴爱祥),WANGYiming(王贻明),et al.Effect of compound activator on copper slag activity and preparation of filling materials[J].Chinese Journal of Engineering(工程科学学报),2017,39(9):1305-1312.
[21]FENG Guangming(冯光明),DING Yu(丁玉),ZHU Hongju(朱红菊),et al.Experimental research on a super high-water packing material for mining[J].Journal of China University of Mining&Technology(煤炭学报),2010,39(6):813-819.
[22]LIAO Yishun(廖宜顺),LIU Chuming(刘楚明),KANG Shuang(康爽),et al.Effect of mineral admixtures on the hydration of sulphoaluminate cement under seawater condition[J].Bulletin of the Chinese Ceramic Society(硅酸盐通报),2017,36(4):1333-1336.
[23]WANG Peiming(王培铭),LI Nan(李楠),XU Linglin(徐玲琳).Hydration characteristics and strength development of sulphoaluminate cement cured at low temperature[J].Journal of the Chinese Ceramic Society(硅酸盐学报),2017,45(2):242-246.
[24]XU Linglin(徐玲琳),ZHOU Xiangyi(周向艺),LI Nan(李楠),Impact of calcium sulfate on hydration features of calcium sulfoaluminate cement[J].Journal of Tongji University:Natural Science(同济大学学报:自然科学版),2017,45(6):885-888.
[25]CHANG Jun(常钧),ZHANG Yangyang(张洋洋),SHANGXiaopeng(尚小朋).Effects of ah3 phase content and hydration degree on the strength of calcium sulfoaluminate cement[J].Journal of Building Materials(建筑材料学报),2016,19(6):1028-1031.
[26]GAO Shujie(高术杰),NI Wen(倪文),LI Keqing(李克庆),et al.Reparation and hydrated mechanism of mine filling material of water-granulated secondary nickel slag[J].Journal of the Chinese Ceramic Society(硅酸盐学报),2013,41(5):612-615.