不同处理方法对冶金硅系产业回收微硅粉结构组成的影响
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摘要
为研究不同处理方法对微硅粉结构组成、元素存在状态的影响,以冶金硅系产业回收微硅粉为原料,采用水洗磁选、水流分级、微波酸浸、700℃煅烧自然冷却、700℃水淬急冷、800℃煅烧自然冷却、800℃水淬急冷对微硅粉进行实验处理,得到了不同处理条件下的微硅粉样品。通过XRD、SEM、TEM、XPS对微硅粉样品物相组成、微观形貌和元素存在状态进行了表征分析。结果表明:水洗磁选、水流分级和微波酸浸处理微硅粉只去除了微硅粉中部分Fe_3O_4、游离碳和金属氧化物杂质;高温煅烧微硅粉改变了微硅粉结晶状态,在800℃时,微硅粉由无定形的玻璃相转化为方石英相。通过对微硅粉元素拟合分析,发现微硅粉中除含有SiO_2外,还有化合物(SiO_2)_(0. 694)(Na_2O)_(0. 306)、(K,Ca)_2[Mg_(4. 3)Fe_(0. 7)][Si_(7. 2)Al_(0. 8)O_(22)](OH)_2、Mg_3H_2(SiO_3)_4,并存在少量CaO、MgO等矿化剂。
In order to study the effect of different treatment methods on the structure and elemental state of silica fume,the silica fume recovered from the metallurgical silicon industry was used as the raw material,using magnetic separation,flow classification,microwave acid leaching,natural cooling at 700℃ calcination,water quenching at 700 ℃,natural cooling at 800 ℃ calcination,and water quenching at800 ℃ were used for the experimental treatment of the silica fume. Samples under different treatment conditions were obtained. Characterization analysis of morphology,phase composition,compound element status of silica fume were made with adoption of XRD,SEM,TEM and XPS. The results show that the magnetic separation,flow classification and microwave acid leaching treatment of silica fume only remove some of the Fe_3O_4,free carbon and metal oxide impurities in the silica fume. In high temperature calcinations,silica fume changes crystalline state. At 800 ℃,silica fume converts from amorphous glass phase to cristobalite phase. Through fitting analysis of silica fume impurity,it is found out that in addition to SiO_2,silica fume also contain compounds like( SiO_2)_(0. 694)( Na_2 O)_(0. 306),( K,Ca)_2[Mg_(4. 3) Fe_(0. 7)][Si_(7. 2) Al_(0. 8) O_(22)]( OH)_2,Mg_3 H_2( SiO_3)_4 as well as small amount of CaO,MgO and other mineralizer.
In order to study the effect of different treatment methods on the structure and elemental state of silica fume,the silica fume recovered from the metallurgical silicon industry was used as the raw material,using magnetic separation,flow classification,microwave acid leaching,natural cooling at 700℃ calcination,water quenching at 700 ℃,natural cooling at 800 ℃ calcination,and water quenching at800 ℃ were used for the experimental treatment of the silica fume. Samples under different treatment conditions were obtained. Characterization analysis of morphology,phase composition,compound element status of silica fume were made with adoption of XRD,SEM,TEM and XPS. The results show that the magnetic separation,flow classification and microwave acid leaching treatment of silica fume only remove some of the Fe_3O_4,free carbon and metal oxide impurities in the silica fume. In high temperature calcinations,silica fume changes crystalline state. At 800 ℃,silica fume converts from amorphous glass phase to cristobalite phase. Through fitting analysis of silica fume impurity,it is found out that in addition to SiO_2,silica fume also contain compounds like( SiO_2)_(0. 694)( Na_2 O)_(0. 306),( K,Ca)_2[Mg_(4. 3) Fe_(0. 7)][Si_(7. 2) Al_(0. 8) O_(22)]( OH)_2,Mg_3 H_2( SiO_3)_4 as well as small amount of CaO,MgO and other mineralizer.
引文
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[2]铁生年,姜子炎,汪长安.矿热炉冶炼铁合金回收微硅粉粉体应用研究与发展现状[J].硅酸盐通报,2012,31(6):1491-1497.
[3] Medina N F,Barluenga G,Hernandez-Olivares F. Combined effect of polypropylene fibers and silica fume to improve the durability of concrete with natural pozzolans blended cement[J]. Construction and Building Materials,2015,96:556-566.
[4] Khater H M. Effect of silica fume on the characterization of the geopolymer materials[J]. International Journal of Advanced Structural Engineering,2013(5):12-22.
[5]陈超,夏扬,石莹,等.微硅粉的微观结构分析[J].商品混凝土,2016(7):39-42.
[6]唐建新,吕艳红,李传山.体废弃物微硅粉应用研究进展[J].现代陶瓷技术,2013(4):17-21.
[7] Lian T W,Kondo A,Kozawa T,et al. Effect of fumed silica properties on the thermal insulation performance of fibrous compact[J]. Ceramics International,2015,41(8):9966-9971.
[8]姜子炎,铁生年,汪长安.流化床法除去微硅粉游离碳工艺研究[J].硅酸盐通报,2013,32(1):19-24.
[9]铁生年,姜子炎,汪长安.微波酸浸提高微硅粉纯度工艺研究[J].人工晶体学报,2013,42(10):2183-2193.
[10]张韶红,铁生年.水流分级对非晶微硅粉除杂效果研究[J].人工晶体学报,2017,46(2):323-328.
[11]肖万生,陈晋阳,彭文世,等.方石英的亚稳态形成机制探讨[J].矿物岩石,200,23(4):5-10.
[12]徐常明,王士维,黄校先,等.方石英的析晶与无定形化[J].无机材料学报,2007,22(4):577-582.
[13] Mollah M Y,Promreuk S,Schennach R,et al. Cristobalite formation from thermal treatment of Texas lignite fly ash[J]. Fuel,1999(26):484-495.
[14] Jan M L,Peter Z K. Conventional and microwave sintering of condensed silica fume[J]. Communication,1994(7):2411-2414.
[15] Nanri H,Takeuch N,Ishida S,et al. Mineralizing action of iron in amorphous silica[J]. J Non-cryst Solids,1996(203):375-379.
[16] Moulder J F,Stickle W F,Sobol P E,et al. Handbook of X-ray photoelectro spectroscopy[M]. America:Perkin EImer Corp,1992:72-130.
[17]刘芬,赵志娟,邱丽美,等. XPS光电子峰和俄歇能谱峰峰位表[J].分析测试技术与仪器,2009,15(1):1-17.