Continuous Flow Siloxane Synthesis Process

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Solution Overview

Problem

Existing batch processes for siloxane synthesis, such as octaphenylcyclotetrasiloxane production, are slow, require significant downtime for cleaning, and use excessive methanol, leading to increased processing times and costs.

Innovation Solution

A continuous flow system for siloxane synthesis that mixes chlorosilane and solvent with an acid scavenger in a first reactor, separates waste products, and reacts the product with methanol in a second reactor, using a caustic methanol and polar aprotic solvent to produce diphenyl cyclic siloxanes with reduced methanol usage and improved efficiency.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If a batch process is used for siloxane synthesis, then the process can be operated with simple equipment, but the processing time is slow and downtime is significant

Engineering Contradiction:
Improveprocessing speedVSAvoiddowntime for cleaning
Core Design Contradiction:
ProductivityVSLoss of time

Solution Approach 1:

The patent implements a continuous flow process where reactants are continuously fed through reactors and separation units, eliminating the need to stop between batches. The system operates continuously from feedstock introduction to product collection, removing downtime associated with cleaning and setup between batch operations.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The continuous process is divided into multiple functional modules including a first reactor for chlorosilane hydrolysis, a separation unit for removing waste products, and a second reactor for cyclic siloxane formation. This segmentation allows each unit to operate continuously while maintaining overall process efficiency.

Inventive Principle:
Principle #1Segmentation

2Loss of substance

If a batch process is used for siloxane synthesis, then equipment complexity is low, but the amount of methanol used is large and expensive

Engineering Contradiction:
Improvemethanol consumptionVSAvoidcontinuous flow system complexity
Core Design Contradiction:
Loss of substanceVSDevice complexity

Solution Approach 1:

The patent changes the operational parameters from batch to continuous mode, which fundamentally alters how methanol is consumed. In continuous operation, methanol is added in controlled amounts at specific rates rather than in large excess for suspension, reducing overall consumption while maintaining reaction effectiveness.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The continuous flow system incorporates flow meters and controllers that monitor and adjust methanol addition rates in real-time based on process conditions. This feedback control ensures optimal methanol usage by adding only the amount needed for the reaction, preventing excessive consumption.

Inventive Principle:
Principle #23Feedback

3Productivity

If chemical B is isolated after removal from the first batch reactor, then the reaction can be completed, but processing time increases

Engineering Contradiction:
Improvesynthesis efficiencyVSAvoidisolation and processing time
Core Design Contradiction:
ProductivityVSLoss of time

Solution Approach 1:

Instead of isolating chemical B between steps, the continuous process feeds the reaction mixture directly from the first reactor to the separation unit and then to the second reactor without interruption. This eliminates isolation time while maintaining product formation continuity.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent merges the hydrolysis step and cyclic siloxane formation step into a single continuous process flow. The output of the first reactor is directly fed to the second reactor, combining two previously separate batch operations into one integrated continuous system, thereby eliminating intermediate processing time.

Inventive Principle:
Principle #5Merging (Combining)

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

The continuous flow system significantly reduces processing time, minimizes downtime, and lowers methanol consumption by 66%, while maintaining high product purity and yield, and allows for real-time control of reaction parameters.

Implementation Method 1

reacting, in the first reactor of the continuous flow system, the chlorosilane-solvent mixture and an acid scavenger substance to form a first reaction product

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

providing, into a separator, the first reaction product to remove one or more waste products from the first reaction product

Methodology Applied
Scientific EffectSeparation:

Implementation Method 3

reacting, in the second reactor of the continuous flow system, the first reaction product and the methanol substance to form a diphenyl cyclic siloxane product

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Data Source

PatentUS11993621B1Continuous flow process for siloxane synthesis
Publication Date: 2024.05.28 HONEYWELL FEDERAL MANUFACTURING & TECHNOLOGIES LLC
  • US11993621B1 patent drawing
  • US11993621B1 patent drawing
  • US11993621B1 patent drawing

AI summary

Methods, systems, and computer-readable media for providing a continuous flow synthesis process including two or more multiphase reactions for producing a diphenyl siloxane product. Reactants and supporting substances are continuously added in-line of the continuous flow path to eliminate downtime associated with batch processes and increase the overall yield of the synthesis over time.