Polishing Reactor Hydrogenation for Aromatic Amine Purity

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Solution Overview

Problem

In continuous catalytic hydrogenation processes for aromatic nitrocompounds, achieving complete hydrogenation while minimizing side reactions and maintaining product quality is challenging due to variations in residence time and the risk of over-hydrogenation, leading to reduced yields and contamination by tar-like constituents.

Innovation Solution

A two-reactor system is employed, where the overflow from a main hydrogenation reactor enters a smaller polishing reactor equipped with a gas recirculation device to ensure complete hydrogenation of residual feed material and intermediates without adding fresh feed, using a gas recirculation and distribution mechanism to enhance the hydrogenation process.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If the residence time in a single CSTR hydrogenator is increased to achieve complete hydrogenation, then the conversion of nitro compounds improves, but the risk of over-hydrogenation and side reactions increases leading to reduced yield

Engineering Contradiction:
Improvehydrogenation completenessVSAvoidproduct yield
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The continuous hydrogenation process is divided into multiple CSTRs connected in series, each operating at optimized conditions. This segmentation allows the reaction to proceed through distinct stages, achieving complete hydrogenation in each step while controlling residence time to prevent over-hydrogenation and side reactions, thus maintaining high product yield

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The process uses a pre-reactor before the main CSTR hydrogenator to perform initial hydrogenation of nitro compounds. This preliminary action converts a portion of the feed material before it enters the main reactor, reducing the burden on the main reactor and allowing optimization of residence time and conditions to achieve complete conversion without excessive side reactions

Inventive Principle:
Principle #10Preliminary action

2Productivity

If catalyst amount, hydrogen pressure and/or reaction temperature are increased to minimize residual feed material, then the reaction rate improves, but the risk of over-hydrogenation and side reactions increases

Engineering Contradiction:
Improvereaction rateVSAvoidside reactions and tar formation
Core Design Contradiction:
ProductivityVSObject-generated harmful factors

Solution Approach 1:

By dividing the hydrogenation process into multiple CSTRs, each reactor can operate at moderate catalyst loading, hydrogen pressure, and temperature conditions. This segmentation distributes the reaction burden across multiple units, achieving high overall reaction rate while maintaining conditions that minimize over-hydrogenation and side reactions in each individual reactor

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The process optimizes reaction parameters (catalyst amount, hydrogen pressure, temperature) specifically for multi-CSTR operation, where each reactor operates at parameter sets that balance reaction rate with selectivity. This allows achieving high productivity while controlling harmful side reactions through coordinated parameter optimization across the reactor series

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If multiple reactors in series are used to increase product output, then the complete hydrogenation improves, but the device complexity increases

Engineering Contradiction:
Improvehydrogenation completenessVSAvoidnumber of reactors
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

Multiple CSTRs are merged into a unified continuous hydrogenation system with coordinated feed and product streams. The reactors operate in series but are integrated as a single process unit, achieving complete hydrogenation through the combined effect while managing complexity through unified process control and material flow management

Inventive Principle:
Principle #5Merging (Combining)

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 increases the yield of high-quality aromatic amines by ensuring complete hydrogenation of residual materials in the polishing reactor, reducing side reactions, and improving product purity, as demonstrated by test results showing increased TDA production with minimal intermediates and tar formation.

Implementation Method 1

catalytic hydrogenation of the corresponding nitrocompounds

Methodology Applied
Scientific EffectCatalysis: Catalysis

Implementation Method 2

hydrogenation of nitrobenzene (NB) to produce aniline (AN) and the hydrogenation of dinitrotoluene (DNT) to produce toluenediamine (TDA)

Methodology Applied
Scientific EffectHydrogenation: Hydrogenation

Data Source

PatentEP3102559B1Method for hydrogenation of aromatic nitrocompounds for the production of aromatic amines, and a system therefore
Publication Date: 2019.08.07 CHEMATUR TECH
  • EP3102559B1 patent drawingFigure 1
  • EP3102559B1 patent drawingFigure 2

AI summary

The present invention relates to a process for the preparation of amines by hydrogenation of aromatic nitrocompounds in liquid phase, which comprises supplying a first reactor (2) comprising at least one catalyst with a feed (9) of gaseous hydrogen and a feed (8) of liquid aromatic nitrocompounds; hydrogenation in the first hydrogenation reactor (2) by contracting the gaseous phase with the liquid phase to obtain a product containing aromatic amines; forwarding the liquid and gaseous phases present in the first reactor (2) to a second polishing reactor (13); and contacting gaseous phase material present in the polishing reactor (13) with the liquid phase to allow further hydrogenation of any remaining aromatic nitrocompounds and/or intermediates, wherein the polishing reactor (13) is fed liquid phase and gaseous phase material forwarded from the first reactor. The present invention further relates to a system therefore.