Dialkylaminosilane Synthesis Solvent System

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Solution Overview

Problem

Current methods for producing dialkylaminosilane face challenges such as hydrolysis of the product, limited structural versatility, and high halogen content due to the formation of dialkylamine hydrochloride, which complicates solid-liquid separation and reduces yield.

Innovation Solution

A method involving the use of a mixed solvent system comprising an aprotic polar solvent and a straight-chain or branched hydrocarbon, where the aprotic polar solvent has high solubility in dialkylamine hydrochloride and metal chloride by-products, and the hydrocarbon solvent reduces halogen content and facilitates efficient separation.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If a dialkylamine reacts with a chlorosilane to produce dialkylaminosilane, then the objective product is obtained, but a large amount of dialkylamine hydrochloride is produced as a by-product requiring solid-liquid separation

Engineering Contradiction:
Improveproduction efficiency of dialkylaminosilaneVSAvoidcomplexity of solid-liquid separation operation
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The invention changes the physical state parameter of the by-product dialkylamine hydrochloride from solid to dissolved state by selecting an appropriate solvent system. The solvent keeps the hydrochloride in dissolved state during reaction and allows easy separation through filtration or decantation, eliminating complex solid-liquid separation operations while maintaining high production efficiency

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention introduces a solvent as an intermediary substance that mediates between the reaction components and the by-product. The solvent dissolves dialkylamine hydrochloride, preventing it from forming solid precipitates that would require complex filtration, thereby simplifying the separation process while maintaining productivity

Inventive Principle:
Principle #24Intermediary (Mediator)

2Ease of operation

If an alkaline aqueous solution is used to dissolve dialkylamine hydrochloride, then the hydrochloride is extracted into aqueous layer, but the dialkylaminosilane is hydrolyzed resulting in significant reduction of yield

Engineering Contradiction:
Improveease of by-product separationVSAvoidyield of dialkylaminosilane
Core Design Contradiction:
Ease of operationVSProductivity

Solution Approach 1:

The invention uses an inert organic solvent system instead of alkaline aqueous solution to create a non-hydrolyzing environment for the dialkylaminosilane. The solvent dissolves the by-product hydrochloride without causing hydrolysis of the sensitive amino-silane product, thereby maintaining high yield while still enabling easy separation through filtration or decantation

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

Solution Approach 2:

The invention employs a simple organic solvent that can be easily removed after reaction, replacing the complex alkaline aqueous system. The solvent serves its purpose of dissolving by-products during reaction and can be readily eliminated, leaving the pure product without causing hydrolysis

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

3Ease of manufacture

If conventional solvents like hexane or ether are used, then the reaction proceeds, but the volumetric efficiency is reduced due to large amount of solvent required

Engineering Contradiction:
Improvefeasibility of reactionVSAvoidvolumetric efficiency of reaction mixture
Core Design Contradiction:
Ease of manufactureVSVolume of moving object

Solution Approach 1:

The invention changes the solvent selection parameter from conventional low-polarity solvents (hexane, ether) to a specific organic solvent system with appropriate solubility characteristics. This parameter change enables the solvent to dissolve by-products effectively at lower volumes, improving volumetric efficiency while maintaining reaction feasibility and ease of manufacture

Inventive Principle:
Principle #35Parameter changes

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 approach enhances volumetric efficiency, reduces the load of solid-liquid separation, and allows for the stable production of high-purity dialkylaminosilane with low halogen content, improving yield and reducing production costs.

Implementation Method 1

an aprotic polar solvent having high solubility in dialkylamine hydrochloride and metal chloride each produced as a by-product

Methodology Applied
Scientific EffectSolvation: Solvation

Implementation Method 2

a solvent of straight-chain or branched hydrocarbon that has high solubility in dialkylaminosilane and is hard to dissolve a halogen compound therein

Methodology Applied
Scientific EffectDifferential solubility:

Data Source

PatentEP3275886B1Method for producing dialkylaminosilane
Publication Date: 2020.03.11 JNC CORP
  • EP3275886B1 patent drawingFigure 1
  • EP3275886B1 patent drawing
  • EP3275886B1 patent drawing

AI summary

In a method for synthesizing dialkylaminosilane from a reaction of dialkylamine with chlorosilane as the method for producing dialkylaminosilane, a large amount of dialkylamine hydrochloride is produced as a by-product, in addition to objective dialkylaminosilane. Therefore, upon obtaining objective dialkylaminosilane, reduction of volumetric efficiency caused by a large amount of a solvent is prevented, and dialkylaminosilane is produced at a low cost and in a large amount. Dialkylaminosilane having a small halogen content is produced with high volumetric efficiency by using, as a solvent upon allowing dialkylamine to react with chlorosilane, an aprotic polar solvent having high solubility in dialkylamine hydrochloride and metal chloride each produced as a by-product by the reaction, and straight-chain or branched hydrocarbon having high solubility in dialkylaminosilane and hard to dissolve a halogen compound therein.