Static Reactor for Polysilazane Production

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Solution Overview

Problem

The high cost and complexity of polysilazane production, particularly in separating polysilazane resin from ammonia and waste ammonium halide salt, hinder efficient manufacturing due to the exothermic nature of the ammonolysis reaction, which can lead to over-pressurization and explosive risks, and the current batch process is inefficient and costly.

Innovation Solution

A system comprising a static reactor vessel with precise control of temperature, pressure, and flow rate, along with a mechanism for settling and removing ammonium chloride waste, and a method for recovering ammonia, where anhydrous ammonia is maintained at sufficient temperature and pressure to solubilize and ionize ammonium halide salt, creating an acidic environment for catalytic polymerization of silazanes and polysilazanes, allowing for continuous processing and efficient separation of products.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Temperature

If batch process ammonolysis is used to produce polysilazanes, then the exothermic reaction can be controlled through periodic cooling, but the process complexity increases and productivity decreases due to repeated cooling cycles and settling steps

Engineering Contradiction:
Improvereaction temperature controlVSAvoidproduction efficiency
Core Design Contradiction:
TemperatureVSProductivity

Solution Approach 1:

The patent implements a continuous process where chlorosilane is continuously fed into liquid ammonia in a reactor, and the reaction mixture continuously flows through a settling vessel and ammonia recovery system. This eliminates the need for repeated batch cooling cycles while maintaining temperature control through the continuous flow regime and heat exchange with incoming cold ammonia, thereby significantly improving productivity.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent combines multiple functions into integrated system components. The settling vessel simultaneously performs phase separation and preliminary ammonia recovery, while the ammonia recovery system handles both ammonia purification and salt removal. This merging of functions reduces the number of discrete steps and equipment needed, simplifying the overall process.

Inventive Principle:
Principle #5Merging (Combining)

2Manufacturing precision

If batch process with settling and decanting is used to separate polysilazane resin from ammonia and salt, then separation can be achieved, but the device complexity and time consumption increase

Engineering Contradiction:
Improveseparation efficiencyVSAvoidprocessing time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The patent replaces batch settling and decanting operations with a continuous flow system. The reaction mixture continuously passes through a settling vessel where phases separate, and the separated streams continuously flow to their respective destinations. This continuous operation eliminates idle time between batch cycles and maintains constant separation throughput, significantly reducing total processing time while maintaining separation efficiency.

Inventive Principle:
Principle #20Continuity of useful action

3Loss of substance

If ammonia evaporation/condensation is used for ammonia recovery, then ammonia can be reused, but energy consumption increases and the process becomes more complex

Engineering Contradiction:
Improveammonia recoveryVSAvoidenergy consumption
Core Design Contradiction:
Loss of substanceVSUse of energy by moving object

Solution Approach 1:

The patent utilizes the exothermic heat of the ammonolysis reaction itself to drive the ammonia recovery process. The reaction heat warms the reaction mixture, which then transfers heat to incoming cold liquid ammonia in a heat exchanger, causing the warm ammonia to vaporize and the cold ammonia to condense. This converts the reaction's harmful heat buildup into a useful energy source for ammonia recovery, eliminating the need for external heating and cooling utilities.

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

Solution Approach 2:

The system recovers and reuses ammonia within the process itself without requiring external energy inputs for evaporation and condensation. The heat exchange between reaction streams and fresh ammonia creates a self-sustaining thermal cycle that continuously recycles ammonia, making the process energy-self-sufficient.

Inventive Principle:
Principle #25Self-service

4Temperature

If chilled ammonia is used to control exothermic reaction, then temperature control is achieved, but over-pressurization risk increases when cooling is insufficient

Engineering Contradiction:
Improvereaction temperatureVSAvoidpressure control safety
Core Design Contradiction:
TemperatureVSReliability

Solution Approach 1:

The patent implements inherent feedback control through the continuous flow system. The reaction mixture temperature and pressure continuously influence the flow rates and heat exchange efficiency, which in turn adjust the cooling capacity. Additionally, the system design ensures that excess pressure can be safely managed through the continuous ammonia recovery and venting system, preventing dangerous pressure buildup.

Inventive Principle:
Principle #23Feedback

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 simplifies the polysilazane production process, reduces waste salt and ammonia recovery costs, and maintains a controlled reaction environment, enabling the production of polysilazanes with improved efficiency and safety by minimizing over-pressurization risks and allowing for the reuse of ammonia, thus lowering overall production costs.

Implementation Method 1

The ammonium halide salt is substantially ionized and solubilized in the anhydrous liquid ammonia, and as such, provides an acidic environment for catalytically preparing the novel silazane and polysilazane compounds

Methodology Applied
Scientific EffectIonization: Ionisation

Implementation Method 2

The ammonium halide salt is substantially ionized and solubilized in the anhydrous liquid ammonia

Methodology Applied
Scientific EffectSolvation: Solvation

Implementation Method 3

the exothermic nature of the ammonolysis reaction which can range between 2,600 to 4,400 btu/pound of product

Methodology Applied
Scientific EffectExothermic reaction: Exothermic Reaction

Implementation Method 4

a static reactor vessel which requires no moving parts, and adapted for precise control of reaction processing parameters including temperature, pressure, and flow rate

Methodology Applied
Scientific EffectHeat exchange: Heat Exchanger

Implementation Method 5

a mechanism for settling of the product phase from the salt ammonia phase and removing a significant portion of the ammonium chloride waste material

Methodology Applied
Scientific EffectSettling: Settling

Implementation Method 6

Other operations collect the ammonia by evaporation/condensation for subsequent reuse

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 7

Other operations collect the ammonia by evaporation/condensation for subsequent reuse

Methodology Applied
Scientific EffectCondensation: Condensation

Data Source

PatentUS12012486B2System and method for a semi-continuous process for producing polysilazanes
Publication Date: 2024.06.18 A G INNOVATION PARTNERS LTD
  • US12012486B2 patent drawing
  • US12012486B2 patent drawing
  • US12012486B2 patent drawing

AI summary

The present invention provides for a system comprising a static reactor vessel which requires no moving parts, and adapted for precise control of reaction processing parameters including temperature, pressure, and flow rate; a mechanism for settling of the product phase from the salt ammonia phase and removing a significant portion of the ammonium chloride waste material; a method for recovering essentially all of the process ammonia and a method for maintaining a reaction environment which is suitably ionic/acidic.