基于正交试验的半水磷石膏充填配比优化
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摘要
针对二水磷石膏充填存在充填成本高、水泥耗量大、固结体强度低等问题,以半水磷石膏替代胶凝材料,通过正交试验法确定半水磷石膏充填的最佳配方,并对其流动性和微观结构进行研究。结果表明:通过配方优化,半水磷石膏充填体3 d、7 d、28 d的强度可达到5.4 MPa、5.5 MPa、6.1 MPa,膏体坍落度为26 cm,扩展度为71cm。半水磷石膏充填配比中的3个影响因素为外加剂掺量、尾砂掺量和浆料浓度。对于3 d抗压强度影响最大的因素是外加剂掺量,对于7 d强度影响最大的因素是浆料浓度,对于28 d强度影响最大的因素是外加剂掺量,对于料浆流动性影响最大的是浆料浓度。半水磷石膏固结体由半水相转化为二水相,形成致密的晶体结构,表明以半水磷石膏制备的膏体料浆具备矿山充填的可行性。充填材料固体中废弃物用量占98%以上,成本较低,具有良好的经济效益和社会效益,推广应用前景良好。
In view of a series of dehydrate phosphogypsum filling problems, such as high filling cost, large consumption amount of cement, low strength of consolidation and so on, hemihydrate phosphogypsum was used as paste filling material in the paste filling research. Through orthogonal experiment method, the best prescription of hemihydrate phosphogypsum was determined, and the liquidity and micro structure were also studied. The results show that the filling strength of hemihydrate phosphogypsum in 3rd day, 7th day and 28 th day can reach to 5.4 MPa, 5.5 MPa and 6.1 MPa,respectively, and the paste collapsbillity is 26 cm, and the extension is 71 cm. The three factors that affect the filling ratio of hemihydrate phosphogypsum are admixture amount, slurry concentration and tailing amount. The most influential factor that affects the compressive strength of sample for 3rd day is the admixture amount. The most influential factor that affects the compressive strength of sample for 7th day is the slurry concentration. The most influential factor that affects the compressive strength of sample for 28th day is the admixture amount. The most influential factor that affects the slurry fluidity is the slurry concentration. Meanwhile, the hemihydrate phosphogypsum consolidation transforms from hemihydrate into dehydrate, then forms dense crystal structure and effectively solidifies the soluble phosphorus.Therefore, the paste slurry made with hemihydrate phosphogypsum can completely meet the requirement of filling process and performance index. Furthermore, the solid waste in the filling material accounts for more than 98%, and the cost is low, which has good economic and social benefits, also the popularization and application prospects are good and worth expecting.
In view of a series of dehydrate phosphogypsum filling problems, such as high filling cost, large consumption amount of cement, low strength of consolidation and so on, hemihydrate phosphogypsum was used as paste filling material in the paste filling research. Through orthogonal experiment method, the best prescription of hemihydrate phosphogypsum was determined, and the liquidity and micro structure were also studied. The results show that the filling strength of hemihydrate phosphogypsum in 3rd day, 7th day and 28 th day can reach to 5.4 MPa, 5.5 MPa and 6.1 MPa,respectively, and the paste collapsbillity is 26 cm, and the extension is 71 cm. The three factors that affect the filling ratio of hemihydrate phosphogypsum are admixture amount, slurry concentration and tailing amount. The most influential factor that affects the compressive strength of sample for 3rd day is the admixture amount. The most influential factor that affects the compressive strength of sample for 7th day is the slurry concentration. The most influential factor that affects the compressive strength of sample for 28th day is the admixture amount. The most influential factor that affects the slurry fluidity is the slurry concentration. Meanwhile, the hemihydrate phosphogypsum consolidation transforms from hemihydrate into dehydrate, then forms dense crystal structure and effectively solidifies the soluble phosphorus.Therefore, the paste slurry made with hemihydrate phosphogypsum can completely meet the requirement of filling process and performance index. Furthermore, the solid waste in the filling material accounts for more than 98%, and the cost is low, which has good economic and social benefits, also the popularization and application prospects are good and worth expecting.
引文
[1]杨成军,杨敏,曹建新.半水/无水磷石膏复相胶凝材料水化硬化特性研究[J].非金属矿,2014,37(6):22-25.YANG Cheng-jun,YANG Ming,CAO Jian-xin.Study on hydration and hardening of duplex gypsum binder of hemihydrite phosphogypsum and anhydrite phosphogypsum[J].Non-Metallic Mines,2014,37(6):22-25.
[2]韩斌,吴爱祥,王贻明,王洪江,王少勇,江怀春.低强度粗骨料超细全尾砂自流胶结充填配合比优化及应用[J].中南大学学报(自然科学版),2012,43(6):2357-2362.HAN Bin,WU Ai-xiang,WANG Yi-ming,WANGHong-jiang,WANG Shao-yong,JIANG Huai-chun.Optimization and application of cemented hydraulic fill(CHF)with low strength aggregate and extra fine grain full tailings[J].Journal of Central South University(Natural Science Edition),2012,43(6):2357-2362.
[3]邓代强,姚中亮,朱永建,汪令辉.胶结充填体强度预测及水泥消耗量反演计算[J].中国矿业大学学报,2013,42(1):39-44.DENG Dai-qiang,YAO Zhong-liang,ZHU Yong-jian,WANG Ling-hui.Strength prediction of cemented filling body and back calculation of cement consumption[J].Journal of China University of Mining and Technology,2013,42(1):39-44.
[4]高术杰,倪文,祝丽萍,王中杰,王佳佳.脱硫石膏对赤泥-矿渣胶结充填料强度性能的影响[J].中南大学学报(自然科学版),2013,44(6):2259-2266.GAO Shu-jie,NI Wen,ZHU Li-ping,WANG Zhong-jie,WANG Jia-jia.Effect of desulphurization gypsum on the strength of red mud and slag cemented filling[J].Journal of Central South University(Natural Science Edition),2013,44(6):2259-2266.
[5]杨林,曹建新,刘亚明.半水磷石膏的晶型、形貌及胶凝性能的影响因素研究[J].人工晶体学报,2015,44(9):2460-2467.YANG Lin,CAO Jian-xin,LIU Ya-ming.Study on the influence factor of the crystalline,morphology and cementitious properties of hemi-hydrate phosphogypsum[J].Journal of Artificial Crystal,2015,44(9):2460-2467.
[6]韩伟明,李建锡,段正洋,郑书瑞,耿庆钰.缓凝剂对α半水磷石膏性能的影响[J].硅酸盐通报,2016,35(6):1958-1963,1969.HAN Wei-ming,LI Jian-xi,DUAN Zheng-yang,ZHENGShu-rui,GENG Qing-yu.Effect of retarder on properties ofα-hemihydrate gypsum[J].silicate bulletin,2016,35(6):1958-1963,1969.
[7]熊有为.基于半水磷石膏自胶凝充填材料膏体特性实验研究[J].矿业研究与开发,2018,38(1):15-19.XIONG You-wei.Experimental study on paste characteristics of selfgelling filling materials based on the semi-water phosphogypsum[J].Mining Research and Development,2018,38(1):15-19.
[8]陈嘉懿.预处理工艺对磷石膏性能的影响及作用机理研究[D].武汉:武汉理工大学,2012.CHEN Jia-yi.Effect of pretreatment process on phosphogypsum performance and its action mechanism[D].Wuhan:Wuhan University of Technology,2012.
[9]冯光明,丁玉,朱红菊,柏建彪.矿用超高水充填材料及其结构的实验研究[J].中国矿业大学学报,2010,39(6):813-819.FENG Guang-ming,DING Yu,ZHU Hong-ju,BAI Jian-biao.Experimental study on mineral superhigh water filling material and its structure[J].Journal of China University of Mining and Technology,2010,39(6):813-819.
[10]WU Ai-xiang,RUAN Zhu-en,WANG Yi-ming,YINSheng-hua,WANG Shao-yong,WANG Yong,WANGJian-dong.Simulation of long-distance pipeline transportation properties of whole-tailings paste with high sliming[J].Journal of Central South University,2018,25(1):141-150.
[11]GB 18599-2001.一般工业固体废物贮存、处置场污染控制标准[S].GB 18599-2001.Standard for pollution control on the storage and disposal site for general industrial solid wastes[S].
[12]GB/T 17671-1999,水泥胶砂强度检验方法(ISO法)[S].GB/T 17671-1999.Method of testing cements-Determination of strength[S].
[13]GB/T 1346-2011,水泥标准稠度用水量、凝结时间、安定性检验方法[S].GB/T 1346-2011.Test methods for water requirement of normal consistency,setting time and soundness of the Portland cement[S].
[14]李克庆,冯琳,高术杰.镍渣基矿井充填用胶凝材料的制备[J].工程科学学报,2015,37(1):1-6.LI Ke-qing,FENG Lin,GAO Shu-jie.Preparation of cementitious materials for backfilling by using nickel slag[J].Chinese Journal of Engineering,2015,37(1):1-6.
[15]苏金明,阮沈勇,王永利编.MATLAB工程数学[M].北京:电子工业出版社,2005:77-95.SU Jin-ming,RUAN Shen-yong,WANG Yong-li.MATLABengineering mathematics[M].Beijing:Electronic Industry Press,2005:77-95.
[16]李公成,王洪江,吴爱祥,于少峰,陈辉,王晓宁,严庆文.基于倾斜管实验的膏体自流输送规律[J].中国有色金属学报,2014,24(12):3162-3169.LI Gong-cheng,WANG Hong-jiang,WU Ai-xiang,YUShao-feng,CHEN Hui,WANG Xiao-ning,YAN Qing-wen.The law of the self flow of the paste based on the inclined tube experiment[J].The Chinese Journal of Nonferrous Metals,2014,24(12):3162-3169.
[17]张修香,乔登攀.粗骨料高浓度充填料浆的管道输送模拟及试验[J].中国有色金属学报,2015,25(1):258-266.Zhang Xiu-xiang,Qiao Deng-pan.Simulation and experiment of pipeline transportation of high density filling slurry with coarse aggregates[J].The Chinese Journal of Nonferrous Metals,2015,25(1):258-266.
[18]杨建,王新民,张钦礼,柯愈贤.含硫高黏性三相流态充填浆体管道输送性能[J].中国有色金属学报,2015,25(4):1049-1055.YANG Jian,WANG Xin-min,ZHANG Qin-li,KE Yu-xian.Pipeline transportation properties of high viscosity sulfur-content filling slurry in three-phase flow[J].The Chinese Journal of Nonferrous Metals,2015,25(4):1049-1055.
[19]张钦礼,刘奇,赵建文,刘贱刚.深井似膏体充填管道的输送特性[J].中国有色金属学报,2015,25(11):3190-3195.ZHANG Qin-li,LIU Qi,ZHAO Jian-wen,LIU Jian-gang.Pipeline transportation characteristics of filling paste-like slurry pipeline in deep mine[J].The Chinese Journal of Nonferrous Metals,2015,25(11):3190-3195.
[20]吴爱祥,程海勇,王贻明,王洪江,刘晓辉,李公成.考虑管壁滑移效应膏体管道的输送阻力特性[J].中国有色金属学报,2016,26(1):180-187.WU Ai-xiang,CHENG Hai-yong,WANG Yi-ming,WANGHong-jiang,LIU Xiao-hui,LI Gong-cheng.Transport resistance characteristic of paste pipeline considering effect of wall slip[J].The Chinese Journal of Nonferrous Metals,2016,26(1):180-187.
[21]林宗寿.胶凝材料学[M].武汉:武汉理工大学出版社,2014:20-37.LIN Zong-shou.Cementitious materials science[M].Wuhan:Wuhan University of Technology Press,2014:20-37.
[22]侯玉芬.胶凝材料[M].北京:中国电力出版社,2012:93-94.HOU Yu-fen.Cementitious materials[M].Beijing:China Electric Power Press,2012:93-94.
[2]韩斌,吴爱祥,王贻明,王洪江,王少勇,江怀春.低强度粗骨料超细全尾砂自流胶结充填配合比优化及应用[J].中南大学学报(自然科学版),2012,43(6):2357-2362.HAN Bin,WU Ai-xiang,WANG Yi-ming,WANGHong-jiang,WANG Shao-yong,JIANG Huai-chun.Optimization and application of cemented hydraulic fill(CHF)with low strength aggregate and extra fine grain full tailings[J].Journal of Central South University(Natural Science Edition),2012,43(6):2357-2362.
[3]邓代强,姚中亮,朱永建,汪令辉.胶结充填体强度预测及水泥消耗量反演计算[J].中国矿业大学学报,2013,42(1):39-44.DENG Dai-qiang,YAO Zhong-liang,ZHU Yong-jian,WANG Ling-hui.Strength prediction of cemented filling body and back calculation of cement consumption[J].Journal of China University of Mining and Technology,2013,42(1):39-44.
[4]高术杰,倪文,祝丽萍,王中杰,王佳佳.脱硫石膏对赤泥-矿渣胶结充填料强度性能的影响[J].中南大学学报(自然科学版),2013,44(6):2259-2266.GAO Shu-jie,NI Wen,ZHU Li-ping,WANG Zhong-jie,WANG Jia-jia.Effect of desulphurization gypsum on the strength of red mud and slag cemented filling[J].Journal of Central South University(Natural Science Edition),2013,44(6):2259-2266.
[5]杨林,曹建新,刘亚明.半水磷石膏的晶型、形貌及胶凝性能的影响因素研究[J].人工晶体学报,2015,44(9):2460-2467.YANG Lin,CAO Jian-xin,LIU Ya-ming.Study on the influence factor of the crystalline,morphology and cementitious properties of hemi-hydrate phosphogypsum[J].Journal of Artificial Crystal,2015,44(9):2460-2467.
[6]韩伟明,李建锡,段正洋,郑书瑞,耿庆钰.缓凝剂对α半水磷石膏性能的影响[J].硅酸盐通报,2016,35(6):1958-1963,1969.HAN Wei-ming,LI Jian-xi,DUAN Zheng-yang,ZHENGShu-rui,GENG Qing-yu.Effect of retarder on properties ofα-hemihydrate gypsum[J].silicate bulletin,2016,35(6):1958-1963,1969.
[7]熊有为.基于半水磷石膏自胶凝充填材料膏体特性实验研究[J].矿业研究与开发,2018,38(1):15-19.XIONG You-wei.Experimental study on paste characteristics of selfgelling filling materials based on the semi-water phosphogypsum[J].Mining Research and Development,2018,38(1):15-19.
[8]陈嘉懿.预处理工艺对磷石膏性能的影响及作用机理研究[D].武汉:武汉理工大学,2012.CHEN Jia-yi.Effect of pretreatment process on phosphogypsum performance and its action mechanism[D].Wuhan:Wuhan University of Technology,2012.
[9]冯光明,丁玉,朱红菊,柏建彪.矿用超高水充填材料及其结构的实验研究[J].中国矿业大学学报,2010,39(6):813-819.FENG Guang-ming,DING Yu,ZHU Hong-ju,BAI Jian-biao.Experimental study on mineral superhigh water filling material and its structure[J].Journal of China University of Mining and Technology,2010,39(6):813-819.
[10]WU Ai-xiang,RUAN Zhu-en,WANG Yi-ming,YINSheng-hua,WANG Shao-yong,WANG Yong,WANGJian-dong.Simulation of long-distance pipeline transportation properties of whole-tailings paste with high sliming[J].Journal of Central South University,2018,25(1):141-150.
[11]GB 18599-2001.一般工业固体废物贮存、处置场污染控制标准[S].GB 18599-2001.Standard for pollution control on the storage and disposal site for general industrial solid wastes[S].
[12]GB/T 17671-1999,水泥胶砂强度检验方法(ISO法)[S].GB/T 17671-1999.Method of testing cements-Determination of strength[S].
[13]GB/T 1346-2011,水泥标准稠度用水量、凝结时间、安定性检验方法[S].GB/T 1346-2011.Test methods for water requirement of normal consistency,setting time and soundness of the Portland cement[S].
[14]李克庆,冯琳,高术杰.镍渣基矿井充填用胶凝材料的制备[J].工程科学学报,2015,37(1):1-6.LI Ke-qing,FENG Lin,GAO Shu-jie.Preparation of cementitious materials for backfilling by using nickel slag[J].Chinese Journal of Engineering,2015,37(1):1-6.
[15]苏金明,阮沈勇,王永利编.MATLAB工程数学[M].北京:电子工业出版社,2005:77-95.SU Jin-ming,RUAN Shen-yong,WANG Yong-li.MATLABengineering mathematics[M].Beijing:Electronic Industry Press,2005:77-95.
[16]李公成,王洪江,吴爱祥,于少峰,陈辉,王晓宁,严庆文.基于倾斜管实验的膏体自流输送规律[J].中国有色金属学报,2014,24(12):3162-3169.LI Gong-cheng,WANG Hong-jiang,WU Ai-xiang,YUShao-feng,CHEN Hui,WANG Xiao-ning,YAN Qing-wen.The law of the self flow of the paste based on the inclined tube experiment[J].The Chinese Journal of Nonferrous Metals,2014,24(12):3162-3169.
[17]张修香,乔登攀.粗骨料高浓度充填料浆的管道输送模拟及试验[J].中国有色金属学报,2015,25(1):258-266.Zhang Xiu-xiang,Qiao Deng-pan.Simulation and experiment of pipeline transportation of high density filling slurry with coarse aggregates[J].The Chinese Journal of Nonferrous Metals,2015,25(1):258-266.
[18]杨建,王新民,张钦礼,柯愈贤.含硫高黏性三相流态充填浆体管道输送性能[J].中国有色金属学报,2015,25(4):1049-1055.YANG Jian,WANG Xin-min,ZHANG Qin-li,KE Yu-xian.Pipeline transportation properties of high viscosity sulfur-content filling slurry in three-phase flow[J].The Chinese Journal of Nonferrous Metals,2015,25(4):1049-1055.
[19]张钦礼,刘奇,赵建文,刘贱刚.深井似膏体充填管道的输送特性[J].中国有色金属学报,2015,25(11):3190-3195.ZHANG Qin-li,LIU Qi,ZHAO Jian-wen,LIU Jian-gang.Pipeline transportation characteristics of filling paste-like slurry pipeline in deep mine[J].The Chinese Journal of Nonferrous Metals,2015,25(11):3190-3195.
[20]吴爱祥,程海勇,王贻明,王洪江,刘晓辉,李公成.考虑管壁滑移效应膏体管道的输送阻力特性[J].中国有色金属学报,2016,26(1):180-187.WU Ai-xiang,CHENG Hai-yong,WANG Yi-ming,WANGHong-jiang,LIU Xiao-hui,LI Gong-cheng.Transport resistance characteristic of paste pipeline considering effect of wall slip[J].The Chinese Journal of Nonferrous Metals,2016,26(1):180-187.
[21]林宗寿.胶凝材料学[M].武汉:武汉理工大学出版社,2014:20-37.LIN Zong-shou.Cementitious materials science[M].Wuhan:Wuhan University of Technology Press,2014:20-37.
[22]侯玉芬.胶凝材料[M].北京:中国电力出版社,2012:93-94.HOU Yu-fen.Cementitious materials[M].Beijing:China Electric Power Press,2012:93-94.