Rotating Vessel Vacuum Sublimation for Thermally Sensitive Materials

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Current sublimation processes for high-value organic and organometallic compounds in organic electronics are inefficient, leading to low sublimation rates and significant decomposition, especially due to poor heat input and thermal conductivity issues, limiting their scalability and purity.

Innovation Solution

A sublimation process under high vacuum conditions using a rotating vessel with a ferrofluidic or mechanical face seal rotation coupling, allowing for efficient sublimation with reduced thermal stress and decomposition, enabling the purification of larger amounts of thermally sensitive materials.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If standard sublimation is used to purify thermally sensitive materials, then purification is achieved, but sublimation rates are very low and decomposition occurs

Engineering Contradiction:
Improvesublimation rateVSAvoiddecomposition
Core Design Contradiction:
ProductivityVSObject-affected harmful factors

Solution Approach 1:

The invention applies dynamic motion by rotating the sublimation vessel at controlled speeds (5-500 rpm). This rotation dynamically distributes the material across the heating surface, continuously exposing fresh material to heat while preventing localized overheating and decomposition, thereby increasing sublimation rate without causing thermal damage

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The invention changes the operational parameters by implementing controlled rotation speed as a new variable parameter. By adjusting rotation speed between 5-500 rpm, the system optimizes the balance between heat input efficiency and thermal stress on the material, enabling high sublimation rates while preventing decomposition of thermally sensitive compounds

Inventive Principle:
Principle #35Parameter changes

2Productivity

If heating is increased to improve sublimation rate, then sublimation efficiency improves, but thermal stress causes decomposition

Engineering Contradiction:
Improvesublimation rateVSAvoidthermal stress
Core Design Contradiction:
ProductivityVSTemperature

Solution Approach 1:

Rotation dynamically distributes thermal energy across the material bed, preventing localized heat accumulation. The continuous motion ensures uniform temperature distribution and reduces thermal stress peaks, allowing higher overall heating while preventing decomposition

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The rotating vessel creates periodic exposure of different material portions to the heating surface. This periodic action prevents continuous thermal stress on any single location, enabling sustained high-temperature operation without causing decomposition

Inventive Principle:
Principle #19Periodic action

3Productivity

If the path from sublimation zone to condensation zone is blocked by material, then material containment is maintained, but sublimation rate decreases

Engineering Contradiction:
Improvesublimation rateVSAvoidmaterial containment
Core Design Contradiction:
ProductivityVSStability of the object's composition

Solution Approach 1:

Rotation prevents material from settling and blocking the condensation path. The dynamic motion keeps the material distributed and prevents accumulation in the condensation zone, maintaining open pathways for vapor transport while containing material within the vessel

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The rotating vessel serves multiple functions simultaneously: it contains the material, distributes heat uniformly, prevents blocking of condensation pathways, and controls sublimation rate. This multi-functionality resolves the contradiction between containment and sublimation efficiency

Inventive Principle:
Principle #6Universality (Multi-functionality)

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 process significantly increases sublimation rates, reduces material loss, and prevents decomposition, making it suitable for industrial-scale purification of high-purity compounds, including those that decompose in standard processes.

Implementation Method 1

The apparatus operates under high vacuum conditions with a vacuum pump system comprising a roughing pump and a high vacuum pump

Methodology Applied
Scientific EffectVacuum: Vacuum

Implementation Method 2

The sublimation material is heated in the sublimation zone and converted into the vapor phase

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 3

the sublimation material is heated in the sublimation zone and converted into the vapor phase

Methodology Applied
Scientific EffectSublimation: Sublimation

Implementation Method 4

The vapor phase material is then converted back into the solid or liquid phase in a condensation zone

Methodology Applied
Scientific EffectCondensation: Condensation

Data Source

PatentUS10391418B2Apparatus for vacuum purification
Publication Date: 2019.08.27 MERCK PATENT GMBH
  • US10391418B2 patent drawing
  • US10391418B2 patent drawing
  • US10391418B2 patent drawing

AI summary

The present invention relates to a process for the vacuum purification of chemical compounds and to an apparatus for carrying out this process.