Silica Masterbatch Production via Silane Hydrophobation

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Solution Overview

Problem

Current methods for producing silica-filled rubber masterbatches using the solution process are inefficient and unable to achieve homogeneous mixing of silica with rubber, leading to poor performance in tire compounds due to incomplete dispersion and processing issues.

Innovation Solution

A process involving the hydrophobation of silica using a silane coupling agent in a reflux method, followed by mixing with solution-made rubber and controlled coagulation to achieve uniform dispersion and binding of silica within the rubber matrix, allowing for the production of silica-filled rubber masterbatches with improved properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If the dry mixing process is used to incorporate silica into rubber, then the silica can be hydrophobated and blended into the rubber, but the process is time-consuming and energy-intensive, greatly reducing the efficiency of the mixing operation

Engineering Contradiction:
Improvedispersion homogeneityVSAvoidmixing efficiency
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The silica is hydrophobated with silane compounds before being incorporated into the rubber compound. This preliminary treatment modifies the silica surface to improve compatibility with rubber, enabling better dispersion without requiring extensive mixing time in the rubber mixer.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

Silane compounds act as intermediary agents between silica and rubber. The silane forms a coupling layer on the silica surface that facilitates bonding with rubber molecules, achieving good dispersion and interfacial adhesion without prolonged mechanical mixing.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Manufacturing precision

If the dry mixing process is used to incorporate silica into rubber, then the silica can be blended into the rubber, but the process requires a great deal of time, capital and operating and maintenance expense

Engineering Contradiction:
Improvedispersion homogeneityVSAvoidprocess cost
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The silica is pre-hydrophobated with silane compounds before rubber compounding. This preliminary surface modification reduces the need for extensive mixing operations, thereby lowering operating costs, reducing capital equipment requirements, and minimizing maintenance expenses associated with prolonged mixing processes.

Inventive Principle:
Principle #10Preliminary action

3Device complexity

If ethanol from the silane is not removed in the mixing step, then the mixing process can proceed without additional equipment, but environmental standards cannot be met

Engineering Contradiction:
Improveequipment requirementVSAvoidenvironmental compliance
Core Design Contradiction:
Device complexityVSObject-affected harmful factors

Solution Approach 1:

The process extracts and removes ethanol from the silane treatment step before incorporating the modified silica into the rubber compound. This extraction eliminates the harmful environmental factor (ethanol emissions) while maintaining the beneficial effects of silane hydrophobation, avoiding the need for additional ethanol removal equipment in the mixing line.

Inventive Principle:
Principle #2Taking out (Extraction)

4Quantity of substance

If untreated silica is added to an emulsion of styrene-butadiene rubber, then the silica can be incorporated into the rubber, but the silica does not completely incorporate and separates as fines when coagulated

Engineering Contradiction:
Improvesilica incorporationVSAvoiddispersion stability
Core Design Contradiction:
Quantity of substanceVSStability of the object's composition

Solution Approach 1:

The silica is pre-hydrophobated with silane compounds before being added to the rubber emulsion. This preliminary surface modification ensures complete incorporation of silica into the rubber matrix and prevents separation as fines during coagulation, achieving both high incorporation and stable dispersion.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

Silane compounds serve as intermediary agents that bridge silica and rubber phases. The silane-modified silica surface is compatible with the rubber emulsion, ensuring complete incorporation and preventing fines formation during subsequent coagulation and processing steps.

Inventive Principle:
Principle #24Intermediary (Mediator)

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 results in fully-dispersed, fully-hydrophobated silica throughout the rubber matrix, enhancing properties such as wet traction and rolling resistance, and facilitating the incorporation of difficult-to-process rubbers and high-surface-area silica, thereby improving the quality and efficiency of tire compounds.

Implementation Method 1

the silica is hydrophobated with a silane compound

Methodology Applied
Scientific EffectHydrophobation: Chemisorption

Implementation Method 2

A desired type of silane is added into the suspension and then the mixture is heated to the boiling temperature of the solvent. Agitation is provide during this reflux period which lasts a couple to a few hours.

Methodology Applied
Scientific EffectSilane coupling: Chemical Bonding

Implementation Method 3

the mixture is heated to the boiling temperature of the solvent. Agitation is provide during this reflux period which lasts a couple to a few hours.

Methodology Applied
Scientific EffectReflux: Heating

Implementation Method 4

A dispersant soluble in the solvent of choice is later added to prevent the silica from clumping together.

Methodology Applied
Scientific EffectDispersion: Dispersion (of waves)

Implementation Method 5

The mixture is later coagulated in a manner similar to the coagulation of an emulsion rubber latex.

Methodology Applied
Scientific EffectCoagulation: Coagulation

Data Source

PatentUS11098169B2Processes for making masterbatches of rubber and silica
Publication Date: 2021.08.24 DYNASOL ELASTOMEROS S A DE

AI summary

A process is provided for making a silica masterbatch, that contains silica and solution-made rubber. The silica masterbatch has physical properties similar to those found in a comparable dry-mixed composition, but the silica masterbatch can be incorporated more easily and less expensively into tires and other rubber products than the dry-mixed composition. A process is also provided for making a masterbatch of silica, a solution-made rubber and an emulsion-made rubber.