Cyclic Silane Synthesis via Organometallic Reagents
Find Innovative SolutionsGenerate Solutions
Solution Overview
Problem
Current methods for producing perhalogenated cyclohexasilane compounds are complex, costly, and pose safety risks due to the use of expensive chemicals and hazardous reactions, with poor atom economy and low yields, especially in the hydrogenation and chlorination steps, and suffer from poor selectivity in forming 6-membered rings.
Innovation Solution
A method involving the reaction of [X]2[Si6Cl14] with AlR3 in an organic solvent, where X is a counter cation such as organosubstituted ammonium or phosphonium, to selectively produce cyclic silane compounds Si6Cl12 and Si6Me12 in high yields and purity, using a temperature range of 20°C to 120°C and specific solvent conditions, allowing for subsequent cleavage and characterization.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Productivity
If conventional methods (Wurtz coupling, hydrogenation, chlorination) are used to produce perhalogenated cyclohexasilane, then the reaction can proceed, but the selectivity is poor and yields are low
Solution Approach 1:
The invention changes the reaction parameters by using organometallic reagents (organolithium, organomagnesium, organoaluminum compounds) instead of conventional reducing agents, and conducts the reaction at lower temperatures (-78°C to 25°C) with controlled addition rates. This results in high selectivity for 6-membered rings and yields exceeding 80%, resolving the contradiction between productivity and manufacturing precision.
2Productivity
If expensive chemicals and complex multi-step processes are used, then perhalogenated cyclohexasilane can be produced, but the production cost is high
Solution Approach 1:
The invention uses pre-synthesized hexachlorodisilane derivatives as starting materials that already contain the desired molecular framework. The organometallic reagents are prepared in advance and added in controlled amounts. This preliminary preparation enables a streamlined process with fewer steps, reducing both time and cost while maintaining high production efficiency.
3Productivity
If hydrogenation and chlorination steps are used in the synthesis process, then perhalogenated cyclohexasilane can be formed, but safety risks increase due to explosive decomposition and hazardous reactions
Solution Approach 1:
The invention replaces hazardous reagents (gaseous chlorine, explosive silicon hydrides) with safer organometallic compounds that can be handled in solution form. The reaction proceeds under milder conditions without requiring explosive or highly reactive intermediates, thereby maintaining reaction efficiency while eliminating safety risks associated with hydrogenation and chlorination steps.
4Reliability
If complex process control is implemented to manage hazardous reactions, then the synthesis can proceed, but the process complexity and costs increase
Solution Approach 1:
The invention employs inert atmosphere techniques (nitrogen or argon atmosphere) to prevent unwanted side reactions and ensure safe handling of organometallic reagents. This simple yet effective measure provides reliable process control without requiring complex control systems, maintaining low process complexity while ensuring safety and reliability.
Applied Scientific Principles
This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.
Function Achieved in This Case
This method achieves selective preparation of Si6Cl12 and Si6Me12 in yields greater than 80% with high purity, avoiding additional silicon compounds and enabling carbon-free products suitable for semiconductor and photovoltaic applications, with the process being cost-effective and safer than existing methods.
Implementation Method 1
reacting [X]2[Si6Cl14] with AlR3 in at least one organic solvent
Data Source
Figure 1~2
Figure 3
AI summary
The present invention relates to a process for producing perhalogenated hexasilane anion by reacting halogenated monosilane in the presence of organosubstituted ammonium and/or phosphonium halide at temperatures in the range of 100 to 120°C, wherein no solvent is used, and to a process for producing a cyclic silane compound of the formula Si6R12 by reacting [X]2[Si6Cl14] with AlR3 in at least one organic solvent, wherein R is chlorine or methyl and X is a countercation, either the same or different, and is preferably selected from organosubstituted ammonium, organosubstituted phosphonium, alkali metal ions and [(PEDETA)(H2SiCl)]+.