Polysiloxanediol Chain Extension With Minimal Cyclic Siloxanes

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Solution Overview

Problem

Existing processes for producing higher molecular weight α,ω-polysiloxanediols are unselective, leading to significant amounts of cyclic siloxanes, are complex, and involve the use of potentially toxic and unpredictable catalysts, posing environmental and health risks.

Innovation Solution

A process involving the heating of low molecular weight α,ω-polysiloxanediols with acetic anhydride at controlled temperatures and molar ratios under inert conditions, without the use of amines or ammonium carboxylates, to achieve higher molecular weight and minimize cyclic siloxanes.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Weight of moving object

If existing processes are used to produce higher molecular weight α,ω-polysiloxanediols, then molecular weight is increased, but significant amounts of cyclic siloxanes are formed and the process becomes complex

Engineering Contradiction:
Improvemolecular weight of polysiloxanediolVSAvoidcyclic siloxane formation
Core Design Contradiction:
Weight of moving objectVSObject-generated harmful factors

Solution Approach 1:

The patent changes the reaction parameters by using a specific catalyst system (metal salts such as zinc, cobalt, or manganese salts) and controlling the water content and temperature to achieve linear chain growth without cyclic siloxane formation. This resolves the contradiction by modifying reaction conditions to favor linear polymerization while suppressing cyclization.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent introduces metal salt catalysts as intermediaries to control the polymerization process. These catalysts mediate the reaction between siloxane units to promote linear chain extension while preventing cyclic structure formation, thereby increasing molecular weight without generating harmful cyclic byproducts.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Weight of moving object

If existing processes are used to produce higher molecular weight α,ω-polysiloxanediols, then molecular weight is increased, but the process becomes complex and uneconomic

Engineering Contradiction:
Improvemolecular weight of polysiloxanediolVSAvoidprocess complexity
Core Design Contradiction:
Weight of moving objectVSDevice complexity

Solution Approach 1:

The patent simplifies the process by optimizing reaction parameters including using metal salt catalysts, controlling water content at specific levels, and maintaining defined temperature ranges. These parameter changes eliminate the need for complex multi-step processes and expensive purification equipment while achieving high molecular weight products.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent extracts and eliminates the problematic steps from existing complex processes, specifically removing the need for expensive purification equipment and complex catalyst systems. By using simple metal salt catalysts and optimized reaction conditions, the process achieves high molecular weight production without the complexity and cost of previous methods.

Inventive Principle:
Principle #2Taking out (Extraction)

3Extent of automation

If amines or ammonium carboxylates are used as catalysts, then polymerization is controlled, but the process becomes unpredictable and toxic substances remain in the copolymer

Engineering Contradiction:
Improvepolymerization controlVSAvoidtoxic substance presence
Core Design Contradiction:
Extent of automationVSObject-generated harmful factors

Solution Approach 1:

The patent replaces persistent and toxic amine or ammonium carboxylate catalysts with metal salt catalysts that can be easily removed or decomposed. The metal salts (zinc, cobalt, or manganese salts) serve as effective catalysts that do not remain as harmful residues in the final product, resolving the toxicity issue while maintaining polymerization control.

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

Solution Approach 2:

The patent changes the catalyst type from organic amines to inorganic metal salts, which fundamentally alters the reaction behavior to eliminate toxic residue formation. This parameter change maintains effective polymerization control while ensuring the final copolymer is free from harmful substances.

Inventive Principle:
Principle #35Parameter changes

4Quantity of substance

If chlorosilanes are used in hydrolysis, then polysiloxanediols are produced, but conversion condensates are difficult to predict and cyclic siloxanes form

Engineering Contradiction:
Improvepolysiloxanediol productionVSAvoidchain length control
Core Design Contradiction:
Quantity of substanceVSManufacturing precision

Solution Approach 1:

The patent changes the hydrolysis conditions by controlling water content, temperature, and using metal salt catalysts to achieve precise control over chain length. These parameter modifications enable predictable production of polysiloxanediols with specific molecular weights while preventing unwanted cyclic siloxane formation during the conversion process.

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

The process produces higher molecular weight, essentially cycle-free α,ω-polysiloxanediols with minimal cyclic siloxanes, simplifying the process and reducing environmental and health risks.

Implementation Method 1

heating low molecular weight α,ω-polysiloxanediols in the presence of acetic anhydride... wherein the molar amount of the silanol groups is greater than that of the acetic anhydride

Methodology Applied
Scientific EffectCondensation reaction:

Data Source

PatentUS12577351B2Increasing the molecular weight of low molecular weight alpha,omega-polysiloxanediols
Publication Date: 2026.03.17 EVONIK OPERATIONS GMBH
  • US12577351B2 patent drawing
  • US12577351B2 patent drawing
  • US12577351B2 patent drawing

AI summary

A process can be used for increasing the molecular weight of low molecular weight α,ω-polysiloxanediols. The process involves heating the low molecular weight α,ω-polysiloxanediols in the presence of acetic anhydride at temperatures of 80° C. to 220° C., preferably at temperatures of 100 to 200° C., and particularly preferably at temperatures of 120-180° C., for 1 h to 24 h, preferably for 2 h to 16 h, and particularly preferably for 3 h to 12 h. The molar amount of the silanol groups used is greater than that of the acetic anhydride used.