Solid Analysis Apparatus with Pressure Surge-Free Fluid Exchange

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Solution Overview

Problem

Existing methods for studying catalytic reactions on solid catalysts are limited to low pressures and temperatures, and are not suitable for examining reaction kinetics under conditions relevant to industrial processes.

Innovation Solution

A device and method that allow for controlled contact between solids and fluids at high pressures and temperatures, with a pressure surge-free exchange of fluids using a system of fluid channels and switching valves, enabling precise control of process conditions and minimization of disruptive processes.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Temperature

If traditional TAP methods are used to study catalytic reactions, then reaction kinetics can be analyzed, but the method is limited to low pressures below atmospheric pressure and Knudsen diffusion regime

Engineering Contradiction:
Improvereaction temperatureVSAvoidpressure range
Core Design Contradiction:
TemperatureVSStress or pressure

Solution Approach 1:

The patent changes the operating parameters of the reactor system to enable operation at high pressures (up to 200 barg) and temperatures (up to 500°C). This is achieved through a specialized reactor design with robust pressure control systems, temperature regulation mechanisms, and fluid exchange systems that maintain pressure surge-free operation despite the extreme conditions. The system allows kinetic studies to be conducted under industrially relevant conditions rather than being constrained to atmospheric or sub-atmospheric pressures.

Inventive Principle:
Principle #35Parameter changes

2Loss of information

If SSITKA method with isotopically labeled reactants is used, then information about surface interactions can be obtained, but changes of state of the catalyst due to step functions are excluded

Engineering Contradiction:
Improveinformation about surface interactionsVSAvoidability to study catalyst state changes
Core Design Contradiction:
Loss of informationVSAdaptability or versatility

Solution Approach 1:

The patent employs periodic pulse experiments where reactant gases are introduced in repeated cycles. This periodic action allows the catalyst to undergo repeated transitions between different states (e.g., oxidized and reduced states) while maintaining steady-state operating conditions. The pulsing mechanism enables the study of catalyst state changes over time without disrupting the overall steady-state environment, combining the benefits of both steady-state and transient analysis.

Inventive Principle:
Principle #19Periodic action

3Loss of information

If classical pulse experiments with temporary equilibrium change are conducted, then reaction networks can be investigated, but the method cannot be carried out at high pressures and temperatures used in technical processes

Engineering Contradiction:
Improveinformation about reaction networksVSAvoidprocess temperature
Core Design Contradiction:
Loss of informationVSTemperature

Solution Approach 1:

The patent modifies the operating parameters to achieve high temperatures (up to 500°C) and pressures (up to 200 barg) while maintaining the pulse experiment methodology. The reactor system incorporates advanced temperature control through heating elements and insulation, along with pressure regulation systems that allow rapid fluid exchange without pressure surges. These parameter changes enable kinetic network analysis under industrially relevant conditions.

Inventive Principle:
Principle #35Parameter changes

4Ease of operation

If fluid exchange is performed without pressure surge control, then simple fluid switching is possible, but disruptive pressure fluctuations occur that affect measurement accuracy

Engineering Contradiction:
Improvefluid exchange simplicityVSAvoidkinetic data accuracy
Core Design Contradiction:
Ease of operationVSMeasurement precision

Solution Approach 1:

The patent introduces pressure control systems as intermediary components between the fluid supply and the reactor. These include pressure regulators, flow controllers, and damping elements that mediate the fluid exchange process. The system uses controlled pressure equalization and surge suppression mechanisms to enable rapid fluid switching while maintaining stable pressure conditions within the reactor. This intermediary control ensures that fluid exchange does not create disruptive pressure fluctuations that would compromise kinetic measurements.

Inventive Principle:
Principle #24Intermediary (Mediator)

Data Source

PatentEP3960286B1Method and apparatus for analyzing solids
Publication Date: 2023.08.16 HTE-AKTIENGESELLSCHAFT THE HIGH THROUGHPUT EXPERIMENTATION COMPANY
  • EP3960286B1 patent drawingFigure 1
  • EP3960286B1 patent drawingFigure 2
  • EP3960286B1 patent drawingFigure 3

AI summary

The present invention relates to an apparatus and a method for the analysis of solids, wherein the apparatus comprises two or more fluid supply units (13, 15, 17, ...), a bypass line (61), at least one flow cell (33, 33', 33", ...) with a supply line (31) and outlet (35), a pressure regulator (64), and an online analysis unit (40). The apparatus includes several fluid supply units that are operatively connected to one or more switching valves (53, 55, 57, ...) via fluid channels (43, 45, 47, ...). By means of the method, different fluids are alternately introduced in pulsed form into the flow cell (33, 33', 33", ...) loaded with solids, and the fluids exiting the flow cell (33, 33', 33", ...) are subjected to analytical characterization.