CN1346333A - 从硅和含硅材料生产非晶形硅石的方法和装置 - Google Patents
从硅和含硅材料生产非晶形硅石的方法和装置 Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 31
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Abstract
本发明涉及用含有至少50%元素硅的细粒材料生产非晶形硅石的方法,它是把含硅材料送入用油燃烧器或气体燃烧器加热的燃烧反应器中,并从燃烧反应器出口后面回收非晶形硅石。至少有一部分含硅材料是以水成淤浆的方式被送入燃烧反应器。本发明还涉及生产非晶形硅石的装置。
Description
发明领域
本发明涉及由含硅材料与空气、富氧空气或氧进行火焰燃烧,从硅和含硅材料生产非晶形硅石的方法。本发明还涉及生产非晶形硅石的装置。
背景技术
非晶形硅石颗粒小、表面积很大,现在的生产方法主要是将挥发性硅化合物,特别是四氯化硅与含氧气体在火焰中进行反应。被称为“雾化硅石”的该产品具有多种用途,特别是用作塑料和橡胶的填充剂。还知道类似的非晶形硅石产品可在等离子炉和电炉中生产,反应物是石英和碳或者硅石和石英。这些产品很贵,未见多用。
从欧洲专利EP-B-151490和美国专利4,755,368中知道硅的火焰燃烧方法,它是将细粒的硅例如空气或氧的气体中流化后送入反应器,在火焰中燃烧硅来制造SiO2微粒。
从挪威专利304366还知道一种用细粒的含硅材料生产非晶形硅石的方法,它是用含氧流化气体以流化方式,把细粒的硅送入燃烧反应器中,再加入补充的含氧气体,使细粒的硅燃烧成SiO2,而无需再加别的热能。
已知的用硅粉燃烧成非晶形SiO2的方法的缺点是难于均匀一致地生产。相信其主要原因是当硅粉在气体中流化时,很难均匀一致地向反应器中供料。另外,从挪威专利304355可以看出,该方法生产出的SiO2只能得到20m2/g的比表面积,而对很多用途来说,所要求的硅石的比表面积要高得多,达80m2/g或更高。
发明内容
本发明的目的是要提供出一种将含硅材料燃烧成SiO2的方法和装置,它能将硅非常均匀非常稳定地送入燃烧反应器,它所制得的非晶形硅石具有高得惊人的比表面积。
因此本发明是涉及用含有至少50%元素硅的细粒材料生产非晶形硅石的方法,它是把含硅材料送入用油燃烧器或气体燃烧器的热的燃烧反应器中,并从燃烧反应器出口后面回收非晶形硅石,该方法的特征在于,至少有一部分含硅材料是以水成淤浆的方式送入燃烧反应器的。
按照一个优选的实施方案,硅是以水成淤浆的方式被送入燃烧反应器中,该淤浆中以重量计含有20%~80%的含硅材料,优选含有以重量计40%~60%的含硅材料。
按照另一个优选的实施方案,在含有含硅材料的水成淤浆中还加入粘度调节剂、如无机酸或有机分散剂。
为了改进所生产的无晶形硅石的表面,可往水成淤浆中加入表面改性剂,例如铝盐,优选为硫酸铝。
按照又一个实施方案,可在燃烧反应器的出口区域加入水以使非晶形硅石骤冷。
令人惊喜地发现,借助于以水成淤浆的方式送入硅料可使反应室操作处于平衡状态,同时还能使生产出的非晶形硅石具有惊人高的比表面积达100m2/g以上。
作为含硅材料,可使用含有元素硅至少50%的细粒材料。这些材料的例子有:细粒状的冶金级硅;细粒状的高纯度硅;雾化硅;电子用和太阳能电池用硅片的锯屑;粉碎硅时所得到的滤粉;生产有机卤素硅烷和无机硅烷的反应器中的残留内。
本发明还涉及用含有以重量计至少50%元素硅的细粒材料生产无晶形硅石的装置,该装置包括一个加长的反应室,反应室一端有一个由燃烧器或气体燃烧器,在反应室侧壁上至少设有一个供应含硅材料水成淤浆的孔、一个无晶形硅石产品的出口孔;以及收集无晶形硅石的设施。
该反应室优选设有一个供应空气、富氧空气或氧的入口孔。
附图简述
图1示出本发明的装置的断面图。
图1中示出圆柱形的燃烧反应器1。燃烧反应器1包括有外部钢筒2,其内衬有耐火衬套3。在燃烧反应器1的一端装有一个油燃烧器或气体燃烧器4。燃烧反应器1的另一端设有一个出口孔。在钢筒2外面装有供冷却空气循环用的冷却套5。冷却套5上设有一个入口孔6。反应室1上还设有一个入口孔7,以供输入含硅材料的水成淤浆。
冷却空气通过入口孔6送入冷却套5,离开冷却套5后进入小室8,小室8借助于出口9与过滤器或类似物相连结,以收集生产出的非晶形硅石。还设有一个入口孔10,以便向反应器1输入空气、富氧空气或氧。
开始生产时,反应器1首先用油燃烧器或气体燃烧器4加热。随后开始输入硅,通过入口孔7输入含硅的水成淤浆并通过孔10输入空气、富氧空气或氧。进入反应器的硅粒将着火并在通过反应室1过程中被烧制成非晶形硅石。
实施例1
将从粉碎冶金级硅的工厂收集来的硅粉与水混合成含有以重量计60%硅的淤浆。该淤浆在如图1的反应器被预热到约1550℃时,从入口端送入反应室。淤浆是被泵入反应器的入口孔7的,流量率为0.2kg/min,同时还流入500l/min的氧。生产出的无晶形硅石则在与小室8的出口孔9相连结的过滤单元中被收集起来。
该非晶形硅石的比表面积按照DIN 66132(BET单点测量法)进行了测量。其比表面积为114.2m2/g。
为了测量该非晶形硅石的晶状硅石含量,使用了菲力浦PW1710 X-射线衍射机(它在X-射线管中有铜阳极)进行检验,结果没有发现晶状硅石。
实施例2
重复实施例1的试验,不同的只是送入反应器的淤浆量改为0.4kg/min。所生产出的非晶形硅石的比表面积为213.6m2/g。
实施例3
重复实施例1的试验,不同的只是使用含硅50重量%的淤浆。所生产出的非晶形硅石和比表面积为117.9m2/g。
实施例4
重复实施例1的试验,不同的只是所用的含硅材料是金刚石切割太阳能电池用硅片的切屑,该切屑已用球磨机研磨过15分钟。所生产出的非晶形硅石的比表面积为103.2m2/g。
实施例1~4显示出,按照本发明的方法所得到的非晶形硅石,比挪威专利304366所生产的非晶形硅石的比表面积高得多。
Claims (12)
1.一种用含有至少50%元素硅的细粒材料生产非晶形硅的方法,其中含硅材料是被送入用油燃烧器或气体燃烧器加过热的燃烧反应器中,而非晶形硅石是在从燃烧反应器的出口以后被回收,其特征在于,至少有一部分含细粒硅材料是以水成淤浆的方式被送入燃烧反应器的。
2.权利要求1的方法,其特征在于,硅是以含有20重量%~80重量%的含硅材料的水成淤浆方式被送入燃烧反应器的。
3.权利要求2的方法,其特征在于,硅是以含有40重量%~60重量%的含硅材料的水成淤浆方式被送入燃烧反应器的。
4.权利要求1的方法,其特征在于,往含有含硅材料的水成淤浆中加入了粘度调节剂。
5.权利要求4的方法,其特征在于,往水成淤浆中加入了无机酸。
6.权利要求4的方法,其特征在于,往水成淤浆中加入了有机分散剂。
7.权利要求1的方法,其特征在于,往水成淤浆中加入了表面改性剂。
8.权利要求7的方法,其特征在于以铝盐作为表面改性剂加入水成淤浆中。
9.权利要求8的方法,其特征在于以硫酸铝作为表面改性剂加入水成淤浆中。
10.权利要求1的方法,其特征在于,在燃烧反应器的出口区域加入水以使非晶形硅石骤冷。
11.一种用含有至少50%元素硅的细粒材料生产非晶形硅石的装置,其特征在于,该装置包括一个加长的反应室(1),其一端有一个油燃烧器或气体燃烧器(4),沿燃烧反应器(1)的侧壁设有至少一个供应含硅材料水成淤浆的孔、一个非晶形硅石产品的出口孔、以及收集非晶形硅石的设施。
12.权利要求11的装置,其特征在于,燃烧反应器(1)上有一个供应空气、富氧空气或氧的入口孔(10)。
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NO19991521 | 1999-03-29 | ||
NO19991521A NO310142B1 (no) | 1999-03-29 | 1999-03-29 | Fremgangsmåte for fremstilling av amorft silica fra silisium og fra silisiumholdige materialer |
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CN100473605C CN100473605C (zh) | 2009-04-01 |
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EP (2) | EP1518826B1 (zh) |
JP (1) | JP3780166B2 (zh) |
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CN (1) | CN100473605C (zh) |
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AU (1) | AU3336700A (zh) |
BR (1) | BR0009412A (zh) |
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UA (1) | UA50882C2 (zh) |
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CZ20013454A3 (cs) | 2002-03-13 |
AU3336700A (en) | 2000-10-16 |
CA2366449A1 (en) | 2000-10-05 |
NO310142B1 (no) | 2001-05-28 |
PL350794A1 (en) | 2003-02-10 |
JP3780166B2 (ja) | 2006-05-31 |
UA50882C2 (uk) | 2002-11-15 |
KR100479564B1 (ko) | 2005-04-06 |
ATE465973T1 (de) | 2010-05-15 |
EP1175373A1 (en) | 2002-01-30 |
NO991521L (no) | 2000-10-02 |
KR20020024576A (ko) | 2002-03-30 |
PL197800B1 (pl) | 2008-04-30 |
BR0009412A (pt) | 2001-12-26 |
RU2195427C1 (ru) | 2002-12-27 |
DE60044309D1 (de) | 2010-06-10 |
WO2000058214A1 (en) | 2000-10-05 |
CA2366449C (en) | 2005-07-05 |
EP1518826A1 (en) | 2005-03-30 |
EP1518826B1 (en) | 2010-04-28 |
CZ295051B6 (cs) | 2005-05-18 |
US6702994B1 (en) | 2004-03-09 |
JP2002540054A (ja) | 2002-11-26 |
NO991521D0 (no) | 1999-03-29 |
ZA200106990B (en) | 2002-11-25 |
CN100473605C (zh) | 2009-04-01 |
ES2344561T3 (es) | 2010-08-31 |
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