CN1431969A - 用于制备烷基或芳基卤代硅烷的硅粉末 - Google Patents
用于制备烷基或芳基卤代硅烷的硅粉末 Download PDFInfo
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- CN1431969A CN1431969A CN01810470A CN01810470A CN1431969A CN 1431969 A CN1431969 A CN 1431969A CN 01810470 A CN01810470 A CN 01810470A CN 01810470 A CN01810470 A CN 01810470A CN 1431969 A CN1431969 A CN 1431969A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 239000011863 silicon-based powder Substances 0.000 title claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 30
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000009826 distribution Methods 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 150000004756 silanes Chemical class 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 238000010908 decantation Methods 0.000 claims description 5
- 125000003118 aryl group Chemical group 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229910000676 Si alloy Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- -1 siloxanes Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 150000005826 halohydrocarbons Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229940050176 methyl chloride Drugs 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/16—Preparation thereof from silicon and halogenated hydrocarbons direct synthesis
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Developing Agents For Electrophotography (AREA)
Abstract
本发明涉及用于制备烷基或芳基卤代硅烷的一种硅粉末,其粒度分布小于350μm,并且含有小于3%,优选小于2%的粒度小于5μm的粒子。所述粉末可以提高合成反应的效率。
Description
发明领域
本发明涉及粒度小于350μm,特别适于希望用于硅氧烷合成的烷基或芳基卤代硅烷的制备的硅或硅合金粉末。
相关技术的状态
从1945年向E.G.ROCHOW授权专利US2380995以来,通过250-350℃下卤代烃,例如氯甲烷,在硅上的反应合成烷基或芳基卤代硅烷是已知的。
此反应在硅氧烷制备上已得以显著的工业开发,它通常在流化床反应容器中采用粉末形式的硅,最通常的是粒度小于350μm的粒子。多年来,通常使用粒度大约在50和350μm之间的级分,粒度小于50μm硅粒子的存在是材料损失和反应容器收率降低的原因。例如在如下文献中可以看到使用这样粒度分布的说明:由Union Carbide持有的,在1986年提交的EP0191502,该文献推荐48目(300μm)-325目(45μm)的分布,或由Pechiney Electrométallurgie持有,在1998年提交的EP 0893408,该文献在实施例1和2中说明了50-350μm分布。
发明目的
本发明涉及粒度小于350μm的用于制备烷基或芳基卤代硅烷的硅或硅合金粉末,包括小于3wt%,和优选小于2wt%的粒度小于5μm的粒子级分。
发明描述
本发明基于申请人的如下观察:在筛分以获得约50-350μm粒度分布的硅粉末中,存在不可忽略量的粒度小于5μm的粒子。出乎预料地,经验显示筛分粉末以提取小于50μm级分已证实在消除最细粒子,例如小于5μm的级分中是无效的。这些非常细的粒子可能在产物的包装期间产生并在显微镜下的观察粉末中确认它们的存在。
可以通过激光粒度测定法对它们的相对数量(重量)进行评估估值,不论它们的制备方法,总是发现在硅粉中约至少4wt%的粒度小于5μm的粒子级分。申请人还观察到这些非常细粒子含量的消除或降低使得可以改进Rochow反应产率。因此,为尽可能有效地使用基于硅粉末的接触物质,它构成卤代硅烷生产成本的显著部分,本发明由如下组成:将粒度小于5μm的粒子的含量降低到小于3%,和优选小于2%。
为获得此结果,可以采用水洗涤研磨到小于350μm并且如需要筛分以得到的50-350μm的粒度分布的粉末。在此洗涤之后是选择性滗析,和随后滗析的粉末的干燥并且还有真空脱除以易于除去水。此技术使得可以获取严格的在5μm的粒度分布,粒度小于5μm的残余级分的最终比例可能达到0.5%。
为了最细粒子的选择性消除,也可以使用粉末在适度速度下的气流中的分散。气体速度选择为所需截止阈值的函数,总是在层流状态下操作的。对于气体,由于安全原因优选选择贫氧的空气。
实施例
实施例1
在电弧炉中制备满足卤代硅烷应用要求规格的化学级冶金硅。将合金浇铸,固化,和然后研磨到小于350μm的粒度。采集五个1kg的产物样品。
一般在设计用于评价其性能的装置中测试此类型的粉末。为进行此测试,将40g粉末与催化剂混合和将混合物放入直径为30mm装配有搅拌器的玻璃反应容器中。一气态CH3Cl流通过承载所述粉末的烧结玻璃盘送入。将气体流量保持恒定在3.6 10-3m3/hr。在加热反应介质和开始反应之后,将系统保持在300℃。在12小时反应之后,记录获得的二甲基二氯硅烷的平均流量,及此产物在所有反应产物中的含量。
为了样品No.1粉末粒度等级的评价,进行了两种类型的测量:
-激光粒度测定法;
-一种参照上述测试的简化测试,直接在测试粉末上不加入催化剂,在环境温度下,不采用加热,并将CH3Cl气体替换为氮气来进行。
激光粒度测定法检测到5.5%(按重量)粒度小于5μm的细粒。
在简化测试中,在12小时处理之后,将反应容器中的剩余产物取出和称重。在初始产物的40g中,仅剩余37.2g,即7%的损失。实施例2
将在实施例1开始时制备的样品No.2在50μm下筛分以提取粒度分布为0-50μm的级分。对以此方式筛分的样品,进行激光粒度测定和检测到4.5%的粒度小于5μm的细粒。移取40g粉末进行实施例1中的简化测试。在12小时处理之后,将反应容器中的剩余产物取出和称重。在初始产物的40g中,仅剩余37.8g,即5.5%的损失。实施例3
将在实施例1开始时制备的,粒度分布小于350μm的样品No.3在10升水中洗涤。然后允许获得的混合物滗析一小时和然后除去上层清液和将滗析的粉末取出和在红外灯下真空干燥。在以此方式洗涤的样品上,进行激光粒度测定和检测到0.5%的粒度小于5μm的细粒。
对所述洗涤了的样品No.3,移取40g粉末进行实施例1中的简化测试。在12小时处理之后,将在反应容器中的剩余产物取出和称重。在初始产物的40g中,仅剩余39.7g,即0.75%的损失。实施例4
将在实施例1开始时制备的样品No.4在10g每分钟的速率下,在直径为50mm和500mm高的管子顶部以规则投掷方式分散,采用一体积空气和两体积氮气组成的向上升气流通过该管,其中流量设定为60cm3每秒。
在管子顶部观察由气体夹带的细粉尘的去除。对在管子底部取出的粉末进行激光粒度测定并检测到2%的粒度小于5μm的细粒。
对所述样品No.4,移取40g粉末进行实施例1中的简化测试。在12小时处理之后,将在反应容器中的剩余产物取出和称重。在初始产物的40g中,仅剩余39.0g,即2.5%的损失。实施例5
将样品No.5在50μm下筛分以制备粒度分布为50-350μm的粉末,然后将它用于重复实施例4中所述的操作。
对在管子底部取出的粉末,进行进行激光粒度测定和检测到1%的粒度小于5μm的细粒。对这样处理的所述样品No.5,移取40g粉末进行实施例1中的简化测试。在12小时处理之后,将在反应容器中的剩余产物取出和称重。在初始产物的40g中,仅剩余39.4g,即1.5%的损失。
Claims (6)
1.粒度小于350μm的用于制备烷基或芳基卤代硅烷的硅或硅合金粉末,其特征为粒度小于5μm的粒子级分小于3wt%。
2.根据权利要求1的硅粉末,其特征为粒度小于5μm的粒子级分小于2wt%。
3.根据权利要求1或2任一项的粉末的制备方法,包括将粉末研磨到小于350μm的粒度,采用水洗涤,滗析和干燥。
4.根据权利要求3的粉末的制备方法,其特征在于将研磨到小于350μm的粉末筛分到50μm以获得50-350μm的粒度分布。
5.根据权利要求1或2任一项的粉末的制备方法,包括将粉末研磨到小于350μm的粒度,筛分以获得50-350μm的粒度分布并使所述粉末在层流状态下的气流中分散。
6.根据权利要求5的方法,其特征在于气体是贫氧的空气。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR00/06920 | 2000-05-30 | ||
FR0006920A FR2809719B1 (fr) | 2000-05-30 | 2000-05-30 | Poudre de silicium pour la preparation des alkyl - ou aryl-halogenosilanes |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1431969A true CN1431969A (zh) | 2003-07-23 |
CN1237003C CN1237003C (zh) | 2006-01-18 |
Family
ID=8850781
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB018104703A Expired - Fee Related CN1237003C (zh) | 2000-05-30 | 2001-05-29 | 用于制备烷基或芳基卤代硅烷的硅或硅合金粉末 |
Country Status (14)
Country | Link |
---|---|
US (1) | US7108734B2 (zh) |
EP (1) | EP1292535B1 (zh) |
JP (1) | JP4782968B2 (zh) |
CN (1) | CN1237003C (zh) |
AT (1) | ATE321734T1 (zh) |
AU (1) | AU2001264040A1 (zh) |
BR (1) | BR0111189B1 (zh) |
CA (1) | CA2410639C (zh) |
DE (1) | DE60118365T2 (zh) |
FR (1) | FR2809719B1 (zh) |
NO (1) | NO20025733L (zh) |
RU (1) | RU2261839C2 (zh) |
WO (1) | WO2001092153A1 (zh) |
ZA (1) | ZA200209240B (zh) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104105543A (zh) * | 2011-12-19 | 2014-10-15 | 蓝星有机硅法国公司 | 烷基卤代硅烷的直接合成方法 |
US11072528B2 (en) * | 2019-04-22 | 2021-07-27 | Fei Company | Halogen generator |
Family Cites Families (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2466412A (en) * | 1946-02-21 | 1949-04-05 | Gen Electric | Method of preparation of hydrocarbon-substituted halosilanes |
US3133109A (en) * | 1960-11-28 | 1964-05-12 | Gen Electric | Silicon compound process and apparatus |
US4307242A (en) * | 1980-10-03 | 1981-12-22 | General Electric Company | Process for removing impurities from residual silicon powder |
JPS58145611A (ja) * | 1982-02-23 | 1983-08-30 | Shin Etsu Chem Co Ltd | シリコン粒子の粉砕、篩別方法 |
US4864044A (en) * | 1985-02-15 | 1989-09-05 | Union Carbide Corporation | Tin containing activated silicon for the direct reaction |
JPS62108727A (ja) * | 1985-11-07 | 1987-05-20 | Mitsubishi Mining & Cement Co Ltd | 疎水性微粒シリカの製造方法 |
JPH07100605B2 (ja) * | 1987-03-14 | 1995-11-01 | 三井東圧化学株式会社 | 高純度粒状珪素の製造方法 |
KR940006017B1 (ko) * | 1992-03-19 | 1994-07-02 | 재단법인 한국화학연구소 | 실리콘 입자의 제트분쇄방법 |
JPH06191817A (ja) * | 1992-12-22 | 1994-07-12 | Tonen Chem Corp | 粒状多結晶シリコンの製造方法 |
JP3679175B2 (ja) * | 1995-11-15 | 2005-08-03 | 東レ・ダウコーニング株式会社 | シリコーン系微粒子の分級方法 |
JP3159029B2 (ja) * | 1996-01-12 | 2001-04-23 | 信越化学工業株式会社 | シラン類の製造方法 |
US5728858A (en) * | 1996-10-10 | 1998-03-17 | Osi Specialties, Inc. | Activation of copper-silicon slurries for the direct synthesis of trialkoxysilanes |
JPH10279584A (ja) * | 1997-04-01 | 1998-10-20 | Shin Etsu Chem Co Ltd | アルキルハロシランの製造方法 |
JPH1129319A (ja) * | 1997-07-08 | 1999-02-02 | Kunimine Ind Co Ltd | 補強性充填剤 |
FR2766474B1 (fr) * | 1997-07-24 | 1999-09-03 | Pechiney Electrometallurgie | Procede de fabrication de poudre de silicium active pour la preparation des alkyl- ou aryl-halogenosilanes |
US6057469A (en) | 1997-07-24 | 2000-05-02 | Pechiney Electrometallurgie | Process for manufacturing active silicon powder for the preparation of alkyl- or aryl-halosilanes |
US6019667A (en) * | 1998-05-26 | 2000-02-01 | Dow Corning Corporation | Method for grinding silicon metalloid |
US6258970B1 (en) * | 1999-04-19 | 2001-07-10 | General Electric Company | Method for promoting dialkyldihalosilane formation during direct method alkylhalosilane production |
-
2000
- 2000-05-30 FR FR0006920A patent/FR2809719B1/fr not_active Expired - Fee Related
-
2001
- 2001-05-29 AT AT01938359T patent/ATE321734T1/de not_active IP Right Cessation
- 2001-05-29 BR BRPI0111189-2A patent/BR0111189B1/pt not_active IP Right Cessation
- 2001-05-29 AU AU2001264040A patent/AU2001264040A1/en not_active Abandoned
- 2001-05-29 CN CNB018104703A patent/CN1237003C/zh not_active Expired - Fee Related
- 2001-05-29 EP EP01938359A patent/EP1292535B1/fr not_active Expired - Lifetime
- 2001-05-29 WO PCT/FR2001/001647 patent/WO2001092153A1/fr active IP Right Grant
- 2001-05-29 US US10/296,548 patent/US7108734B2/en not_active Expired - Fee Related
- 2001-05-29 RU RU2002135595/15A patent/RU2261839C2/ru not_active IP Right Cessation
- 2001-05-29 JP JP2001588132A patent/JP4782968B2/ja not_active Expired - Fee Related
- 2001-05-29 DE DE60118365T patent/DE60118365T2/de not_active Expired - Lifetime
- 2001-05-29 CA CA2410639A patent/CA2410639C/fr not_active Expired - Fee Related
-
2002
- 2002-11-13 ZA ZA200209240A patent/ZA200209240B/en unknown
- 2002-11-28 NO NO20025733A patent/NO20025733L/no unknown
Also Published As
Publication number | Publication date |
---|---|
ZA200209240B (en) | 2003-11-13 |
NO20025733D0 (no) | 2002-11-28 |
EP1292535B1 (fr) | 2006-03-29 |
EP1292535A1 (fr) | 2003-03-19 |
RU2261839C2 (ru) | 2005-10-10 |
BR0111189B1 (pt) | 2010-10-19 |
CN1237003C (zh) | 2006-01-18 |
DE60118365D1 (de) | 2006-05-18 |
FR2809719A1 (fr) | 2001-12-07 |
AU2001264040A1 (en) | 2001-12-11 |
FR2809719B1 (fr) | 2002-07-12 |
BR0111189A (pt) | 2003-06-10 |
US7108734B2 (en) | 2006-09-19 |
CA2410639A1 (fr) | 2001-12-06 |
US20030171606A1 (en) | 2003-09-11 |
ATE321734T1 (de) | 2006-04-15 |
WO2001092153A1 (fr) | 2001-12-06 |
NO20025733L (no) | 2003-01-30 |
JP2003535008A (ja) | 2003-11-25 |
CA2410639C (fr) | 2011-01-25 |
JP4782968B2 (ja) | 2011-09-28 |
DE60118365T2 (de) | 2006-11-02 |
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