Silazane Synthesis Using Self-Solvent to Eliminate Distillation

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Solution Overview

Problem

The existing methods for preparing silazane compounds require a large amount of solvent, which complicates the process due to the formation of a hydrogen halide salt that precipitates out, interfering with stirring and necessitating cumbersome distillation steps.

Innovation Solution

Using a silazane compound as both the reactant and solvent in the reaction between a halosilane compound and an amino-containing compound improves fluidity and reduces solvent requirements, eliminating the need for solvent distillation.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of operation

If a large amount of solvent is used to continue stirring during the reaction, then the stirring is maintained, but the process becomes cumbersome and requires additional distillation steps

Engineering Contradiction:
Improvestirring continuityVSAvoidprocess complexity
Core Design Contradiction:
Ease of operationVSDevice complexity

Solution Approach 1:

The patent introduces a specific solvent system comprising a first solvent (ether or esters) and a second solvent (aromatic hydrocarbon) that acts as an intermediary to dissolve the hydrogen halide salt precipitate. This solvent combination mediates between the reacting components and the precipitated salt, maintaining stirring continuity without requiring excessive solvent volumes or additional processing equipment.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Ease of operation

If a solvent is added to continue stirring during the reaction, then stirring is maintained, but the amount of solvent required is large

Engineering Contradiction:
Improvestirring continuityVSAvoidsolvent volume
Core Design Contradiction:
Ease of operationVSQuantity of substance

Solution Approach 1:

The patent optimizes the solvent composition parameters by specifying precise volume ratios (first solvent: second solvent in 1:3 to 1:10 range) and selecting specific chemical classes for each solvent. This parameter optimization allows the system to maintain adequate stirring with reduced total solvent volume compared to using a single solvent system.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs a composite solvent system combining two different types of solvents (ether/esters and aromatic hydrocarbons) that work synergistically. The first solvent provides initial dissolution capability while the second solvent enhances solubility of the hydrogen halide salt, together achieving effective stirring maintenance with optimized total volume.

Inventive Principle:
Principle #40Composite materials

3Productivity

If the hydrogen halide salt precipitates out during the reaction, then the reaction proceeds, but the precipitate interferes with stirring

Engineering Contradiction:
Improvereaction progressVSAvoidstirring efficiency
Core Design Contradiction:
ProductivityVSEase of operation

Solution Approach 1:

The patent introduces a specific solvent system comprising a first solvent (ether or esters) and a second solvent (aromatic hydrocarbon) that acts as an intermediary to dissolve the hydrogen halide salt precipitate. This solvent combination mediates between the reacting components and the precipitated salt, maintaining stirring continuity without requiring excessive solvent volumes or additional processing equipment.

Inventive Principle:
Principle #24Intermediary (Mediator)

4Ease of operation

If a large amount of solvent is used, then stirring is maintained, but the solvent must be distilled off when the target silazane compound is isolated

Engineering Contradiction:
Improvestirring continuityVSAvoiddistillation time
Core Design Contradiction:
Ease of operationVSLoss of time

Solution Approach 1:

The patent optimizes the solvent composition parameters by specifying precise volume ratios (first solvent: second solvent in 1:3 to 1:10 range) and selecting specific chemical classes for each solvent. This parameter optimization allows the system to maintain adequate stirring with reduced total solvent volume compared to using a single solvent system.

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 method efficiently prepares silazane compounds, useful as intermediates for paint additives, pharmaceuticals, and agricultural chemicals, by enhancing reaction fluidity and simplifying the process by eliminating the need for solvent distillation.

Implementation Method 1

When the same silazane compound as the target product is used as a solvent, the resulting slurry which contains a hydrogen halide salt of the amino-containing compound is improved in fluidity

Methodology Applied
Scientific EffectSolvation: Solvation

Implementation Method 2

silazane compounds are prepared by reaction of a halosilane compound with an amino-containing compound. In this reaction, not only the target silazane compound, but also a hydrogen halide by-product forms

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 3

The hydrogen halide reacts with the amino-containing compound to form a hydrogen halide salt of the amino-containing compound in stoichiometric amount

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 4

an alkaline aqueous solution is added to the reaction solution to dissolve the hydrogen halide salt of the amino-containing compound in the alkaline aqueous solution, thereby separating the amino-containing compound from an organic layer containing the silazane compound

Methodology Applied
Scientific EffectAcid-base reaction and dissolution: Solvation

Data Source

PatentEP2930177B1Preparation of silazane compound
Publication Date: 2018.04.25 SHIN ETSU CHEMICAL CO LTD
  • EP2930177B1 patent drawing
  • EP2930177B1 patent drawing
  • EP2930177B1 patent drawing

AI summary

A silazane compound useful as synthesis intermediates for paint additives, polymer modifiers, pharmaceuticals and agricultural chemicals is efficiently prepared by reaction of a halosilane compound with an amino-containing compound in a solvent which is the same silazane compound as the target product.