Ethanol Dehydration Distillation Reflux Ratio

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Solution Overview

Problem

Existing methods for removing nitrogen-containing contaminants, such as acetonitrile, from ethanol feedstocks are inefficient and require additional process steps or lead to the need for replacing catalysts, as these contaminants can deactivate acid catalysts used in dehydration processes.

Innovation Solution

A process involving distillation of the ethanol feedstock with a reflux ratio of at least 20:1 to separate nitrogen-containing contaminants like acetonitrile from ethanol, reducing the nitrogen content to 50 ppmw or less, thereby minimizing catalyst deactivation and improving process efficiency.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If aqueous extraction or adsorption is used to remove nitrogen-containing contaminants from ethanol, then the level of contaminants is reduced, but additional process steps are required and the process becomes more complex

Engineering Contradiction:
Improvecatalyst performanceVSAvoidprocess complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent applies extraction by distillation to separate nitrogen-containing contaminants from ethanol feedstock. The distillation column extracts these contaminants into the overhead stream while purifying the ethanol in the bottom stream, eliminating the need for additional aqueous extraction or adsorption steps.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent changes the operating parameters of the dehydration process by using a heteropolyacid catalyst supported on silica gel with specific surface area and pore volume characteristics. The catalyst operates at optimized temperature and pressure conditions to achieve efficient dehydration while being resistant to nitrogen-containing contaminants.

Inventive Principle:
Principle #35Parameter changes

2Reliability

If adsorbent materials are used to remove nitrogen-containing contaminants, then contaminants are adsorbed, but the adsorbent materials need to be replaced frequently

Engineering Contradiction:
Improvecatalyst stabilityVSAvoidcatalyst replacement frequency
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

Instead of using expensive adsorbent materials that require frequent replacement, the patent employs a heteropolyacid catalyst supported on silica gel that is resistant to nitrogen-containing contaminants. This catalyst maintains its activity over extended periods without needing frequent replacement.

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

Solution Approach 2:

The patent uses a composite catalyst system consisting of heteropolyacid (such as phosphotungstic acid or silicotungstic acid) supported on silica gel. This composite material combines the acidic activity of heteropolyacid with the high surface area and stability of silica gel, creating a robust catalyst that resists deactivation by nitrogen-containing compounds.

Inventive Principle:
Principle #40Composite materials

3Reliability

If distillation with high reflux ratio is used to separate nitrogen-containing contaminants, then separation efficiency is improved, but energy consumption increases

Engineering Contradiction:
Improvefeedstock purityVSAvoiddistillation energy consumption
Core Design Contradiction:
ReliabilityVSUse of energy by moving object

Solution Approach 1:

The patent applies preliminary distillation to the ethanol feedstock before it enters the dehydration reactor. This pre-purification step removes nitrogen-containing contaminants that would otherwise poison the catalyst, ensuring that the main dehydration process operates efficiently without catalyst deactivation.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent replaces the need for complex multi-step purification mechanisms with a single distillation step followed by dehydration over a heteropolyacid catalyst. The catalyst system is designed to tolerate the simplified purification approach, substituting the need for multiple mechanical separation steps.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

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 effectively reduces the level of nitrogen-containing contaminants in the ethanol feedstock, enhancing the performance of acid catalysts and reducing the need for frequent catalyst replacement by achieving significant separation of acetonitrile from ethanol, even at low concentrations, thus improving the overall efficiency of the dehydration process.

Implementation Method 1

distilling an ethanol feedstock (101) comprising at least one nitrogen-containing contaminant to form an overhead stream (102) and a bottom stream comprising ethanol (103), wherein the distillation has a reflux ratio of at least 20:1

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 2

reacting the bottom stream in the presence of an acid catalyst to form a product stream comprising ethylene and/or diethyl ether

Methodology Applied
Scientific EffectCatalysis: Catalysis

Implementation Method 3

acid-catalysed dehydration of ethanol

Methodology Applied
Scientific EffectDehydration:

Data Source

PatentEP3087047B1Process for the acid-catalysed dehydration of ethanol
Publication Date: 2018.04.25 TECHNIP E&C LTD
  • EP3087047B1 patent drawingFigure 1

AI summary

A process for the acid-catalysed dehydration of ethanol, the process comprising the steps of distilling an ethanol feedstock (101) comprising at least one nitrogen-containing contaminant to form an overhead stream (102) and a bottom stream comprising ethanol (103), wherein the distillation has a reflux ratio of at least 20:1; and reacting the bottom stream in the presence of an acid catalyst to form a product stream comprising ethylene.