公开(公告)号：WO2013052673A2

公开(公告)日：2013-04-11

申请号：PCT/US2012/058764

申请日：2012-10-04

Applicant: VOLTAIX, INC.

Inventor： RITTER, Cole, J.

IPC: C01B21/068 ,  B01J8/00 ,  B01J19/18

CPC classification number: C01B21/087

Abstract: The present invention is directed to a condensed phase batch process for synthesis of trisilylamine (TSA). An improved synthesis method that incorporates a solvent to help promote a condensed-phase reaction between ammonia gas (or liquid) and liquified monochlorosilane (MCS) in good yields is described. This method facilitates the removal of the byproduct waste with little to no reactor down time, substantial reduction of down-stream solids contamination and high-purity product from first-pass distillation.

Abstract translation: 本发明涉及用于合成三甲硅烷基胺（TSA）的缩合相批料方法。 描述了一种改进的合成方法，其包含溶剂以帮助促进氨气（或液体）和液化一氯甲硅烷（MCS）之间的冷凝相反应，产率良好。 这种方法有利于在几乎没有反应器停机时间的情况下去除副产物废物，大大减少下游固体污染物和来自首过蒸馏的高纯度产物。

公开(公告)号：WO2006107880A2

公开(公告)日：2006-10-12

申请号：PCT/US2006/012324

申请日：2006-04-03

Applicant: VOLTAIX, INC. ,  HAZELTINE, Bruce

Inventor： HAZELTINE, Bruce

IPC: C01B33/04

CPC classification number: C01B33/04 ,  Y10T428/2962 ,  Y10T428/2995 ,  Y10T428/31663

Abstract: A method for making a higher silane from a lower silane comprises heating a lower silane containing stream without exposing it to temperatures more than 2O°C more than the maximum temperature of a first reaction temperature range. The heated lower silane containing stream is introduced into a first reaction zone and allowed to react. Unreacted lower silanes are recycled to the earlier heating step. Preferably the average residence time is low to prevent decomposition and formation of undesired silane byproducts. A method for making a higher than higher silane from a lower silane comprises mixing a first gaseous mixture from the first reaction zone with a higher silane containing stream and introducing the mixed streams into a second reaction zone operating within a second reaction temperature range. A second gaseous mixture exiting the second reaction zone is separated into various streams. One stream containing unreacted lower silanes is recycled to an earlier heating step and first reaction zone. Another stream, the higher silane containing stream is mixed with the first gaseous mixture.

Abstract translation: 从下硅烷制备较高硅烷的方法包括加热含硅烷的流，而不将其暴露于比第一反应温度范围的最高温度高出多于20℃的温度。 将加热的含较低硅烷的流引入第一反应区并使其反应。 未反应的较低硅烷再循环至较早的加热步骤。 优选地，平均停留时间低，以防止分解和形成不需要的硅烷副产物。 从下硅烷制备高于高级硅烷的方法包括将来自第一反应区的第一气态混合物与较高含硅烷的物流混合，并将混合物流引入在第二反应温度范围内运行的第二反应区。 离开第二反应区的第二气体混合物被分离成各种流。 含有未反应的下硅烷的一股料流再循环至较早的加热步骤和第一反应区。 另一条流，较高的含硅烷的料流与第一种气体混合物混合。

公开(公告)号：WO2013052673A3

公开(公告)日：2013-07-11

申请号：PCT/US2012058764

申请日：2012-10-04

Applicant: VOLTAIX INC

Inventor： RITTER COLE J

IPC: C01B21/068 ,  B01J8/00 ,  B01J19/18

CPC classification number: C01B21/087

Abstract: The present invention is directed to a condensed phase batch process for synthesis of trisilylamine (TSA). An improved synthesis method that incorporates a solvent to help promote a condensed-phase reaction between ammonia gas (or liquid) and liquified monochlorosilane (MCS) in good yields is described. This method facilitates the removal of the byproduct waste with little to no reactor down time, substantial reduction of down-stream solids contamination and high-purity product from first-pass distillation.

Abstract translation: 本发明涉及用于合成三甲胺（TSA）的冷凝相间歇方法。 描述了一种改进的合成方法，其包括溶剂以帮助促进氨气（或液体）和液化的一氯硅烷（MCS）之间的冷凝相反应，产率良好。 该方法有助于在几乎没有反应器停机的时间内除去副产物废物，大大减少下游固体污染物和来自一次蒸馏的高纯度产物。

公开(公告)号：WO2010057073A1

公开(公告)日：2010-05-20

申请号：PCT/US2009/064537

申请日：2009-11-16

Applicant: VOLTAIX INC. ,  MILLER, Gary, D.

Inventor： MILLER, Gary, D.

IPC: C01G17/00

CPC classification number: B01J20/18 ,  B01J20/28083 ,  B01J20/3078 ,  B01J2220/56 ,  C01B3/56

Abstract: A process and system for the purification of germane containing phosphine to provide a purified germane product. One aspect of the present invention is a process for making a purified germane product containing less than 50 ppb of phosphine which comprises providing a phosphine contaminated germane gas hydrogen gas mixture; passing the germane gas hydrogen gas mixture through an adsorbent which selectively adsorbs phosphine and withdrawing therefrom a purified germane gas hydrogen mixture; and separating the purified germane gas from the hydrogen germane gas mixture.

Abstract translation: 用于纯化含锗的膦以提供纯化的锗烷产物的方法和系统。 本发明的一个方面是制备含有少于50ppb磷化氢的纯化的锗烷产物的方法，其包括提供磷化氢污染的锗烷气体氢气混合物; 使锗烷气体氢气混合物通过吸附剂，该吸附剂选择性地吸附膦并从中提取纯化的锗烷氢气混合物; 并将纯化的锗烷气体与氢气锗烷混合物分离。

公开(公告)号：WO2006107880A3

公开(公告)日：2006-12-21

申请号：PCT/US2006012324

申请日：2006-04-03

Applicant: VOLTAIX INC ,  HAZELTINE BRUCE

Inventor： HAZELTINE BRUCE

IPC: C01B33/04

CPC classification number: C01B33/04 ,  Y10T428/2962 ,  Y10T428/2995 ,  Y10T428/31663

Abstract: A method for making a higher silane from a lower silane comprises heating a lower silane containing stream without exposing it to temperatures more than 2O°C more than the maximum temperature of a first reaction temperature range. The heated lower silane containing stream is introduced into a first reaction zone and allowed to react. Unreacted lower silanes are recycled to the earlier heating step. Preferably the average residence time is low to prevent decomposition and formation of undesired silane byproducts. A method for making a higher than higher silane from a lower silane comprises mixing a first gaseous mixture from the first reaction zone with a higher silane containing stream and introducing the mixed streams into a second reaction zone operating within a second reaction temperature range. A second gaseous mixture exiting the second reaction zone is separated into various streams. One stream containing unreacted lower silanes is recycled to an earlier heating step and first reaction zone. Another stream, the higher silane containing stream is mixed with the first gaseous mixture.

Abstract translation: 由较低硅烷制备较高硅烷的方法包括加热含较低硅烷的物流而不将其暴露于比第一反应温度范围的最高温度高20℃以上的温度。 将加热的含较低硅烷的料流引入第一反应区并使其反应。 未反应的低级硅烷再循环到较早的加热步骤。 优选平均停留时间低以防止不希望的硅烷副产物的分解和形成。 由较低硅烷制备高于高硅烷的方法包括将来自第一反应区的第一气体混合物与含较高硅烷的物流混合并将混合物流引入在第二反应温度范围内操作的第二反应区。 离开第二反应区的第二气体混合物被分离成各种物流。 将含有未反应的低级硅烷的一股料流循环至较早的加热步骤和第一反应区。 另一种物流，即含较高硅烷的物流与第一种气体混合物混合。