Trialkoxysilane Synthesis via Inert Solvent Pulverization

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Solution Overview

Problem

The existing methods for synthesizing trialkoxysilane face challenges such as long induction periods, accumulation of impurities, and complexity in the synthesis process, leading to reduced productivity and increased costs, particularly due to the formation of oxide films on silicon surfaces and the need for additional purification steps.

Innovation Solution

The method involves pulverizing silicon into fine particles in a solvent environment to prevent oxide film formation, continuously feeding a suspension of silicon and alcohol to a reactor, and using a ceramic membrane filter to continuously remove impurities and supplement the solvent, ensuring consistent reaction conditions and high conversion rates.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Area of moving object

If silicon is pulverized in air to form fine particles, then particle size is reduced for increased surface area, but oxide film forms on silicon surface reducing reactivity

Engineering Contradiction:
Improvesurface area of silicon particlesVSAvoidoxide film formation
Core Design Contradiction:
Area of moving objectVSObject-generated harmful factors

Solution Approach 1:

The patent applies inert atmosphere by pulverizing silicon in a nitrogen-filled environment instead of air. This prevents oxygen from contacting and oxidizing the silicon surface during pulverization, thereby eliminating oxide film formation while still achieving fine particle size reduction for increased surface area.

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

Solution Approach 2:

The patent applies preliminary action by pre-pulverizing silicon into fine particles in an inert atmosphere before introducing it to the reaction system. This preliminary particle size reduction increases surface area and reactivity without allowing oxide film formation, as the pulverization occurs in nitrogen rather than air.

Inventive Principle:
Principle #10Preliminary action

2Temperature

If additional inert gas is added to dilute alcohol vapor in fluidized bed, then temperature peak is prevented, but production cost increases and trialkoxysilane loss increases

Engineering Contradiction:
Improvetemperature control in fluidized bedVSAvoidtrialkoxysilane and alcohol carryover
Core Design Contradiction:
TemperatureVSLoss of substance

Solution Approach 1:

The patent extracts and removes the harmful inert gas from the system by conducting the reaction in a closed system without adding external inert gases. Instead of using inert gas dilution to control temperature, the patent uses a solvent-based liquid-phase reaction system that inherently controls temperature without requiring additional gases, thereby eliminating carryover losses.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent introduces a solvent as an intermediary medium to control reaction temperature. The solvent acts as a heat transfer medium, allowing temperature control without requiring inert gas dilution. This intermediary approach eliminates the need for additional inert gases while maintaining temperature control effectiveness.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Manufacturing precision

If reaction is carried out under low pressure to improve synthesis indices, then conversion rate and selectivity increase, but reaction rate decreases and productivity deteriorates

Engineering Contradiction:
Improveconversion rate and selectivityVSAvoidreaction rate
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent changes the physical state parameter from gas-phase to liquid-phase reaction by introducing a solvent. This parameter change allows the reaction to proceed at lower pressures with improved conversion and selectivity, while the liquid phase maintains adequate reaction rates through enhanced molecular mobility and heat transfer characteristics of the solvent system.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses a solvent as an intermediary to mediate between pressure and reaction rate relationships. The solvent enables the reaction to proceed efficiently at lower pressures by providing an alternative reaction medium that maintains molecular interaction frequencies and energy transfer without requiring high pressure, thus decoupling the pressure-rate relationship.

Inventive Principle:
Principle #24Intermediary (Mediator)

4Reliability

If induction period is long due to oxide film on silicon surface, then reaction activation is delayed, but adding activation step increases process complexity and time

Engineering Contradiction:
Improvereaction activationVSAvoidprocess complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent applies preliminary action by pre-pulverizing silicon in an inert atmosphere before the reaction, which prevents oxide film formation during preparation. This eliminates the need for separate activation steps during the reaction process, as the silicon surface remains clean and reactive from the outset, thereby reducing overall process complexity while ensuring reliable reaction activation.

Inventive Principle:
Principle #10Preliminary action

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 significantly shortens the induction period, simplifies the synthesis process, maintains high conversion rates, and enables continuous production of trialkoxysilane, thereby maximizing productivity and economic efficiency by preventing oxide film formation and continuously removing impurities.

Implementation Method 1

removing impurities accumulated in a reactor in a manner of continuously bleeding a solvent using a ceramic membrane filter

Methodology Applied
Scientific EffectFiltration: Filter (physical)

Implementation Method 2

pulverizing silicon into fine particles in a solvent environment to prevent oxide film formation

Methodology Applied
Scientific EffectOxidation prevention: Oxidation

Implementation Method 3

the temperature of reaction mixture may be uniformly maintained to greatly reduce the possibility of overheating reaction environment

Methodology Applied
Scientific EffectThermal conduction: Conduction (thermal)

Implementation Method 4

in case of using a solvent, the temperature of reaction mixture may be uniformly maintained

Methodology Applied
Scientific EffectConvection: Convection

Data Source

PatentEP2754664B1Method for preparing trialkoxysilane
Publication Date: 2016.12.28 OCI CO LTD(KR)
  • EP2754664B1 patent drawingFigure 1
  • EP2754664B1 patent drawing
  • EP2754664B1 patent drawing

AI summary

The present invention relates to a method for preparing SiH(OR3)-type trialkoxysilane (wherein, R is a C1-C3 methyl, ethyl, propyl or isopropyl group), and more specifically, the method comprises the steps of: preventing the oxidation of a silicon surface by pulverizing raw silicon material in a solvent environment without contact with the air so that the initial induction period of the direct synthesis of trialkoxysilane is dramatically reduced; and removing impurities from a reaction environment by continuously selecting a part of the solvent through a membrane filter provided in a reactor body.