CN101466463B - 生产甲硅烷的方法 - Google Patents

生产甲硅烷的方法 Download PDF

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CN101466463B
CN101466463B CN2006800356931A CN200680035693A CN101466463B CN 101466463 B CN101466463 B CN 101466463B CN 2006800356931 A CN2006800356931 A CN 2006800356931A CN 200680035693 A CN200680035693 A CN 200680035693A CN 101466463 B CN101466463 B CN 101466463B
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current reactor
reactor
product
trichlorosilane
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CN101466463A (zh
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P·阿德勒
R·索南谢因
Y·卡萨特金
A·佩特里克
L·施瓦茨曼
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Evonik Operations GmbH
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Evonik Degussa GmbH
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S203/00—Distillation: processes, separatory
    • Y10S203/06—Reactor-distillation

Abstract

本发明涉及通过催化歧化三氯硅烷来连续生产甲硅烷和四氯化硅的设备和方法，其中在根据权利要求1的设备中以一定操作温度和1-50bar绝压下操作，在权利要求1的设备中：三氯硅烷(A)在热交换器(7)中预热，并且将预热后的三氯硅烷进料到提供催化剂(3)的逆流反应器(1)中；在逆流反应器(1)中形成的产物混合物至少部分被冷凝器(5)冷凝，冷凝温度为-25至50℃之间，冷凝物流回到逆流反应器(1)中；冷凝器(5)中没有被冷凝的产物相进入到冷凝单元(8)中，其中该冷凝单元在温度为-40至-110℃下操作；来自冷凝单元(8)的挥发性产物相被进料到蒸馏塔9中，该塔的操作温度为-60至-170℃之间，并且甲硅烷(C)在蒸馏塔(9)的顶部排出；来自逆流反应器(1)的含SiCl4底部产物在蒸发单元(6)中被加热到60-110℃的温度范围；来自蒸发器(6)的底部产物经过热交换器(7)送入逆流反应器(1)的双壁(2)内，并且含SiCl4产物流(B)在反应器(1)的上部区域位置排出。

Description

生产甲硅烷的方法
技术领域
本发明涉及在催化剂存在下通过歧化三氯硅烷来生产甲硅烷和四氯化硅的连续方法。
背景技术
甲硅烷是一种制备太阳能用硅的重要原材料。
目前甲硅烷通常通过歧化三氯硅烷来制备(例如DE2162537、DE2507864、DE3925357、DE3311650、DE10017168、US3968199)。
在三氯硅烷(TCS，HSiCl3)的催化歧化中，甲硅烷(SiH4)与副产物四氯化硅(STC，SiCl4)一起生成，其中四氯化硅可以被用于例如SiO2的制备。在歧化反应中，二氯硅烷(DCS，H2SiCl2)和单氯硅烷(MCS，H3SiC)作为中间产物形成：
2HSiCl3
Figure 2006800356931_0
H2SiCl2+SiCl4          (I)
2H2SiCl2
Figure 2006800356931_1
H3SiCl+HSiCl3         (II)
2H3SiCl
Figure 2006800356931_2
SiH4+H2SiCl2           (III)
—————————————————
4HSiCl3→SiH4+3SiCl4            (IV)
作为歧化作用的催化剂，通常由离子交换剂制成，例如胺功能化聚苯乙烯(DE10057521)、胺功能化无机载体(EP0474265，EP0285937)或有机多分子硅氧烷催化剂(DE3925357)。这些催化剂可以作为层状(US5338518，US5776320)的整个床(DE2507864)、或以编织网结构(WO90/02603)直接引入塔中。作为一种选择，催化剂可以容纳在一个或多个外部反应器中，所述外部反应器具有与蒸馏塔不同部分相连的入口和出口(US4676967、EP 0 474 265、EP 0 285 937、DE 37 11 444)。
由于表1中列举的硅烷的物理属性和在歧化反应中通常处于化学平衡的非常不利的位置，蒸馏反应和进行通常作为整个工艺进行操作。
表1：氯硅烷和甲硅烷的物理数据
  材料   甲硅烷   MCS   DCS   TCS   STC
  临界温度(℃)   -3.5   123   176   206   234
  大气压下的沸点(℃)   -112   -30   8.3   31.8   57.1
  5bar下的沸点(℃)   -78   15   60   87   117
  25bar下的沸点(℃)   -28   85   137   170   207
因此，DE19860146公开了一种生产甲硅烷的连续方法，该方法在反应蒸馏塔中进行TCS的催化歧化，蒸馏塔的压力为1-50bar绝压，通过该方式得到的产物混合物在-25至50℃之间的温度下暂时性冷凝(塔中的液相回流)，而未冷凝的含甲硅烷的产物相在冷凝器中冷凝，其中冷凝器位于反应蒸馏塔的顶部，并且被冷凝的产物作为最终产物排出。另外，在该方法的反应蒸馏塔中SiCl4作为高沸点底部产物形成，并通过热交换器从系统中排出。
另外，在所述方法中得到的氯硅烷作为位于反应蒸馏塔底部的冷凝器中的含甲硅烷产物流冷凝物的底部馏分，可以至少部分回流到塔的反应/蒸馏反应区中。
为了弥补所述反应蒸馏的低反应率的缺点，该问题通常通过附加具有一个或多个副反应器来加大催化剂体积的高代价方式来解决。基于硅的甚至更高非常高的产量是非常需要的。另外，通过所述方法得到的甲硅烷的纯度大约为98％。
发明内容
因此本发明的一个目的是提供用于生产甲硅烷的另一种方法。具体目的是基本上避免上述的缺点。
以上目的通过本发明以权利要求中提出的方式来实现。
因此，已经发现通过催化歧化三氯硅烷以相对简单和经济的方式，可以连续性制得具有高纯度的甲硅烷，例如99.5％的纯度，基于硅的产量高达化学计量可能的产量的98.6％，并且具有副产物四氯硅烷，其中歧化在一定操作温度和压力下进行，压力为1-50bar绝压、优选2-20bar绝压、更优选3-15bar绝压、更优选为4-10bar绝压，如图1和2所图示的：
三氯硅烷(A)在热交换器(7)中预热，优选预热到55-65℃的温度，尤其预热到约60℃，压力如上所述为1-10bar绝压，并且将预热后的三氯硅烷进料到提供催化剂(3)的逆流反应器(1)中；
在逆流反应器(1)中形成的产物混合物至少部分被冷凝器(5)冷凝，冷凝温度为-25至50℃之间，优选-25至-15℃之间，并且冷凝物流回到逆流反应器(1)中；
冷凝器(5)中没有被冷凝的产物相进入到冷凝单元(8)中，其中该冷凝单元在温度为-110至-40℃下操作；
来自冷凝单元(8)的挥发性产物相被进料到蒸馏塔9中，该塔的操作温度为-60至-170℃之间，并且优选具有约99.5％纯度的甲硅烷(C)在蒸馏塔(9)的顶部排出；
来自逆流反应器(1)的含SiCl4底部产物在蒸发单元(6)中被加热到60-110℃的温度范围，优选70-90℃之间；和
来自蒸发器的底部产物经过热交换器(7)被送入逆流反应器(1)的双壁(2)内，并且含SiCl4产物流(B)在反应器(1)的上部区域位置排出。
另外，本方法非常有利，并且根据本发明，提供装置的的设备费用相对较低。
需要特别指出的是底部产物(四氯化硅)能量的有效利用：该能量可用来预热进料流(三氯硅烷)、催化剂区域(逆流反应器的反应区)和低于催化剂的区域的额外加热和目标温度设定，和与其相关的优点：与甲硅烷隔离的冷凝氯硅烷液流的循环。
这样，采用这种独特的有利方式，催化歧化三氯硅烷产生用来生产太阳能用硅需要的甲硅烷等级的单阶段连续方法能够在产物质量和经济方面得到明显改进。
因此本发明提供了通过催化歧化三氯甲烷来连续性生产甲硅烷和四氯硅烷的设备，该设备在一定温度和压力下操作，压力为1-50bar绝压，该设备基于以下单元：
·具有双壁(2)的逆流反应器(1)；
·至少一个位于逆流反应器(1)内并且提供了催化剂(3)的催化剂床(4)；
·位于逆流反应器(1)顶部的冷凝器(5)；
·位于逆流反应器(1)底部的蒸发单元(6)
·至少一个三氯硅烷进料管线(A)，用于将三氯硅烷(7.1，7.2)引入逆流反应器(1)内；
·热交换器(7)，通过管线(7.1，7.2)三氯硅烷首先被传送通过热交换器(7)并在其中预热，并且用于预热的目的，来自蒸发单元(6)的底部产物通过管线(6.1，6.2)通过热交换器(7)，并且在逆流反应器(1)相对低部分的高度进入双壁(2)内，并在逆流反应器(1)的上部部分的高度排出(2.1)双壁(2)，即四氯化硅(B)的排出；
·安装在单元(5)下游的冷凝器单元(8)和
·随后的蒸馏塔(9)
·具有甲硅烷(C)的出口。
在本发明的设备中，通过一个或多个进料单元有利地实现了三氯甲烷(A)的导入，优选在逆流反应器(1)的中间区域或反应区导入。
因此，三氯硅烷(A)的入口优选设置在低于固定催化剂床和/或催化剂床的中间高度的区域。
在本发明的装置中，催化剂床(4)可以被设计成就其本身已知的固定床形式，例如图2中所示的，并且如在开始时描述的，提供催化剂。因此，一个或多个固定床(4)可以在反应器(1)中叠置。
然而，已经发现，根据本发明的逆流反应器(1)配置催化剂床(4)是非常有利的，其中催化剂床(4)包括至少一根管状元件(4.1)，优选3-6400根管状元件，更优选7-1600根，最优选13-400根管状元件，如图1中所述的元件(4.1)。在此，该管状元件(4.1)适合具有大于50mm的直径，优选100-300mm，管壁的厚度为例如2-4mm。管状元件可以由与反应器相应的材料制备。适合制备进行歧化反应的反应器的材料为已知的。管状元件的壁可以是穿孔的固体，例如在壁上提供多个小孔或裂缝或切口，或具有网孔结构。具体而言，每个管状元件的流入和流出侧根据如下设计：首先，管状元件可以容纳催化剂，其次，反应混合物从反应器进入管状单元并再次流出时没有相对大的流阻。适当的流体力学解决方案对本领域技术人员来说是已知的。因此，例如，管状元件的流入和流入侧可以由金属丝网提供。这种管状元件(4.1)可以成束或单个悬挂在反应器(1)中。也可以在反应器中悬挂一个或多个管束。
在根据本发明的装置中，尤其从基于硅的产量来讲是非常有利的，因为在冷凝单元(8)的底部得到的富含氯硅烷的冷凝物通过管线(8.2)回流到逆流反应器(1)的上部。
此外，在根据本发明的设备中可以具有另一优点：在逆流反应器(1)的一个或多个区域设置分离板(10)和/或分离填料(11)。同样地，反应蒸馏塔(9)可以优选设置本领域已知的分离板(10)和/或分离填料。
根据本发明的设备的优选实施方式如图1和2所述的流程图。另外，可以以本领域技术人员已知的方式使用泵、控制装置和调整装置，这些装置根据本发明的方法可以实现操作。
本发明还提供了通过催化歧化三氯甲烷来连续性生产甲硅烷和四氯化硅的方法，该方法在根据本发明的设备中在一定操作温度和压力下操作，压力为1-50bar绝压，其中：
三氯硅烷(A)在热交换器(7)中预热，并且将预热后的三氯硅烷进料到提供催化剂(3)的逆流反应器(1)中；
在逆流反应器(1)中形成的产物混合物至少部分被冷凝器(5)冷凝，冷凝温度为-25至50℃之间，冷凝物流回到逆流反应器(1)中；
在冷凝器(5)中没有被冷凝的产物相进入到冷凝单元(8)中，该冷凝单元的操作温度为-40至-110℃之间；
来自冷凝单元(8)的挥发性产物相被进料到蒸馏塔(9)中，该塔的操作温度为-60至-170℃之间，而甲硅烷(C)在蒸馏塔(9)的顶部排出；
来自逆流反应器(1)的含SiCl4底部产物在蒸发单元(6)中被加热到60-110℃的操作温度，优选70-90℃之间；和
蒸发器(6)的底部产物经过热交换器(7)被送入逆流反应器(1)的双壁(2)内，并且含SiCl4产物流(B)在反应器(1)的上部区位置排出。
可以在本方法中使用纯三氯硅烷。然而，在本发明的方法中也能够并且优选使用工业级三氯硅烷，例如具有98.8％-99.5％的纯度。
本发明方法的逆流反应器(1)，优选催化床区域(4)在70-90℃的温度和1-10bar绝压下操作，且歧化反应进行过程中放热并促使反应连续进行。在既有的条件下，气态产物混合物在逆流反应器(1)中上升，而主要含有四氯化硅的液态相下降到反应器的底部区。
而且，在本发明的工艺中的逆流反应器(1)中形成的产物混合物被冷凝器(5)部分冷凝，冷凝器优选在-10至-25℃温度之间和1-10bar绝压下操作，优选在-15至-20℃温度之间和1-10bar绝压下操作。
在冷凝器(5)中没有冷凝的产物相优选具有≥60至80％重量的甲硅烷含量。
在本发明方法的其它过程，冷凝单元(8)优选在-40至-100℃之间温度和1-10bar绝压下操作，优选在≤-60℃和1-10bar绝压下操作，更优选在-95℃和1-10bar绝压下操作。
冷凝器(8)中得到的含氯硅烷冷凝物优选回流到逆流反应器(1)中。冷凝物优选回流到反应器(1)的上部，合适地低于反应器的顶部，具体位于温度在约20℃温度区。
在本发明的方法中，来自冷凝单元(8)的挥发性产物相优选具有≤1％重量的氯硅烷含量，并且单元(8)优选在5-10bar绝压下操作。该挥发物相在进料到单元(9)之前通过泵适当压缩。
根据本发明，蒸馏塔(9)优选在-90至-110℃温度下、尤其优选在大约-100℃和1-10bar绝压下操作。随后可以有利地在蒸馏塔(9)顶部得到具有99.5％-99.8％纯度的甲硅烷，并通过管线(9.1)将其排出。
副产物四氯甲烷在反应器(1)的底部，即蒸发器(6)中作为热产物相得到。
在本发明的方法中，来自蒸发器(6)的热底部产物优选经过管线(6.1)、热交换器(7)和管线(6.2)被传送到逆流反应器(1)的双壁(2)中，其中在反应器的较低区位置送入，并且主要含有四氯化硅的产物流(B)在反应器(1)的上部区位置排出，具体为刚好低于反应器的顶部(5)的位置。在此得到的四氯化硅可以有利地用于生产硅，尤其是氧化硅。
总的来说，本发明的方法可以如下所述进行：
在根据本发明的装置中，例如在图1或2中看到的，预热三氯硅烷，并在1-50bar绝压下进料到提供催化剂并在一定温度下操作的逆流反应器中。为了预热进料流，优选可以使用来自反应器底部的热产物流。另外，得到的SiCl4产物中的能量/热量可以优选用来通过双壁额外加热逆流反应器，尤其是催化剂床区。在逆流反应器中的歧化反应中形成的产物混合物可以在反应器的顶部部分冷凝，其中大部分氯硅烷以液体形式流回反应器中。未冷凝的产物相有利地进入到另一冷凝单元中，冷凝单元优选在过压和温度为-40至-110℃之间操作。在此得到的含氯硅烷冷凝物有利地回流到逆流反应器的上部。来自冷凝器之后的挥发产物相随后可以进入到蒸馏塔中，其中甲硅烷可以从蒸馏塔中作为具有相对高产量和相对高纯度的顶部产物排出。
通过以下实施例举例说明本发明，但是并不限制本发明的范围。
实施例
在生产条件下在设备中检测本发明的方法，其中作为优选实施方式在图1中大体上示出了所述设备，并且其优选的操作方式已经在上面描述出。工业级三氯硅烷(98.8％)用作原料。阴离子交换树脂Amberlyst 21用作催化剂。三氯硅烷的消耗量为700kg/小时。
根据本发明的操作方式使得硅回收率从化学计量可能值的98.2％增加到98.6％。这种方式得到的甲硅烷具有99.5％的纯度。另外，采用根据本发明的操作方式，生成消耗可以降低2-2.2倍。

Claims (17)

1.一种通过催化歧化三氯甲烷连续性生产甲硅烷和四氯硅烷的装置，该设备在一定操作温度和1-50bar绝压下操作，该设备基于以下单元：
·具有双壁(2)的逆流反应器(1)；
·至少一个位于逆流反应器(1)内并且提供了催化剂(3)的催化剂床(4)；
·位于逆流反应器(1)顶部的冷凝器(5)；
·位于逆流反应器(1)底部的蒸发单元(6)
·至少一个三氯硅烷进料管线，用于将三氯硅烷引入逆流反应器(1)内；
·热交换器(7)，三氯硅烷通过管线(7.1，7.2)首先被传送通过热交换器(7)并在其中预热，为实现预热目的，来自蒸发单元(6)的底部产物通过管线(6.1，6.2)经过热交换器(7)，并且在逆流反应器(1)较低部分的位置进入双壁(2)内，并在逆流反应器(1)的上部位置排出双壁(2)；
·安装在冷凝器(5)下游的冷凝单元(8)和
·随后的蒸馏塔(9)
·具有甲硅烷(C)的出口。
2.根据权利要求1的装置，特征在于至少一根管状元件(4.1)作为催化剂床(4)。
3.根据权利要求1或2的装置，特征在于具有一个或多个三氯硅烷进料管线导入逆流反应器(1)的中间区或反应区。
4.根据权利要求3的装置，特征在于三氯硅烷(A)的入口设置在低于固定催化剂床和/或催化剂床的中间高度位置上。
5.根据权利要求1或2的装置，特征在于管线(8.2)从冷凝单元(8)的底部导入逆流反应器(1)的上部。
6.根据权利要求1或2的装置，特征在于分离板(10)和/或分离填料(11)设置在逆流反应器(1)的一个或多个区域。
7.根据权利要求1或2的装置，特征在于蒸馏塔设置有分离板(10)和/或分离填料(11)。
8.一种通过催化歧化三氯甲烷连续性生产甲硅烷和四氯化硅的方法，该方法在根据权利要求1的设备中以一定操作温度和压力操作，操作压力为1-50bar绝压，其中：
三氯硅烷(A)在热交换器(7)中预热，并且将预热后的三氯硅烷进料到提供催化剂(3)的逆流反应器(1)中；
在逆流反应器(1)中形成的产物混合物至少部分被冷凝器(5)冷凝，操作温度为-25至50℃，冷凝物回流到逆流反应器(1)中；
在冷凝器(5)中没有冷凝的产物相进入到冷凝单元(8)中，该冷凝单元的操作温度为-40至-110℃之间；
来自冷凝单元(8)的挥发性产物相进料到蒸馏塔(9)中，该塔的操作温度为-60至-170℃，甲硅烷(C)在蒸馏塔(9)的顶部排出；
来自逆流反应器(1)的含SiCl4底部产物在蒸发单元(6)中被加热到60-110℃的操作温度范围；和
蒸发器(6)的底部产物经过热交换器(7)送入逆流反应器(1)的双壁(2)内，并且含SiCl4产物流(B)在反应器(1)的上部区排出。
9.根据权利要求8的方法，特征在于：该方法的操作压力为1-10bar绝压。
10.根据权利要求8或9的方法，特征在于逆流反应器在催化剂床(4)区操作温度为70-90℃和1-10bar绝压下进行操作。
11.根据权利要求8或9的方法，特征在于：在逆流反应器(1)中形成的产物混合物部分被冷凝器(5)冷凝，冷凝温度为-25至-10℃之间，压力为1-10bar绝压。
12.根据权利要求8或9的方法，特征在于：在冷凝器(5)中没有冷凝的产物相具有≥60％重量的甲硅烷含量。
13.根据权利要求8或9的方法，特征在于：冷凝单元(8)在-40至-110℃和1-10bar绝压下操作。
14.根据权利要求8或9的方法，特征在于：在冷凝单元(8)中得到的含氯硅烷的冷凝物回流到逆流反应器(1)中。
15.根据权利要求8或9的方法，特征在于：来自冷凝单元(8)的挥发性产物相具有≤1％重量的氯硅烷含量，并且冷凝单元(8)在5-10bar绝压下操作以压缩挥发性产物相。
16.根据权利要求8或9的方法，特征在于：蒸馏塔(9)在-90至-110℃温度下和1-10bar绝压下操作。
17.根据权利要求8或9的方法，特征在于：来自蒸发器(6)的底部热产物经过管线(6.1)、热交换器(7)和另外的管线(6.2)传送到逆流反应器(1)的双壁(2)中，送入位置在反应器的较低区位置，并且主要含有四氯化硅的产物流(B)在反应器(1)的上部区位置排出。
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