Condensed Phase Trisilylamine Synthesis Solvent Extraction
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Solution Overview
Problem
Current batch methods for synthesizing trisilylamine face challenges such as decomposition due to excessive reaction conditions, limited batch size, and the need for labor-intensive reactor cleaning, which affects yield and efficiency.
Innovation Solution
A condensed phase batch process involving the use of a solvent to facilitate low-temperature reactions between monohalosilane and ammonia, where ammonium halide salts are localized as a slurry, allowing for efficient separation and purification of trisilylamine without requiring reactor cleaning between batches.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Reliability
If batch reactor process is used to synthesize trisilylamine, then the reaction can be performed in a closed vessel, but the yield is reduced due to decomposition from excessive reaction conditions and contact with ammonium halide catalysts
Solution Approach 1:
The harmful ammonium halide catalyst is removed from the reaction system by using a solvent that selectively dissolves it, separating the catalyst from the trisilylamine product and preventing decomposition
Solution Approach 2:
A solvent is introduced as an intermediary substance that mediates between the reactants and the catalyst, allowing the reaction to proceed while preventing the catalyst from contacting and decomposing the product
2Quantity of substance
If all monohalosilane is charged into the reactor vessel at once, then the batch size is maximized, but the mixing efficiency decreases and reaction conditions become uneven
Solution Approach 1:
The solvent creates local microenvironments throughout the reactor where reactants can interact efficiently, ensuring uniform reaction conditions even in large batch sizes
3Productivity
If tubular flow gas phase reactor is used to produce high volumes of silylamines, then the yield efficiency is high, but the reactor requires opening and cleaning after each batch which is labor intensive and causes downtime
Solution Approach 1:
The ammonium halide byproduct is extracted into the solvent, allowing it to be removed along with the solvent after reaction, eliminating the need for labor-intensive cleaning of the reactor
Solution Approach 2:
The solvent performs multiple functions: it facilitates the reaction, dissolves the byproduct catalyst, and enables easy removal of contaminants, making the process suitable for continuous operation
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 process enhances trisilylamine formation, suppresses unwanted byproducts, and enables continuous operation by removing ammonium chloride salts as a slurry, improving yield and reducing downtime.
Implementation Method 1
condensing monohalosilane into the solvent to form a solution
Implementation Method 2
adding anhydrous ammonia into the solution to form a reaction mixture
Implementation Method 3
separating the silylamines, excess monohalosilane and TSA from the reaction mixture
Data Source
Figure 1
Figure 2
Figure 3~4
AI summary
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 downstream solids contamination and high-purity product from first-pass distillation.