Butanol Extraction from Hydroalcoholic Solutions

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Solution Overview

Problem

The separation of water and ethanol in hydroalcoholic solutions is hindered by the formation of azeotropes, and the presence of butanol complicates this process further, especially in the Lebedev process where butanol accumulation reduces butadiene yield and increases energy consumption and equipment size.

Innovation Solution

A process involving a water-ethanol separation step with a distillation column, a demixing step using a settling tank, and a butanol separation step, allowing for the partial extraction of butanol to produce effluents rich in ethanol and water, which can be recycled without significant ethanol loss, and a practically pure butanol effluent.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If distillation is used to separate water and ethanol, then ethanol can be recovered, but the formation of water-ethanol azeotrope limits the recovery of pure ethanol

Engineering Contradiction:
Improveethanol purityVSAvoidseparation efficiency
Core Design Contradiction:
Manufacturing precisionVSReliability

Solution Approach 1:

The separation process is divided into multiple stages: first distillation column for preliminary separation, then liquid-liquid extraction stage, followed by second distillation column for final purification. This segmentation allows each stage to address specific separation challenges, overcoming the azeotrope limitation by combining multiple separation mechanisms

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

An organic solvent is introduced as an intermediary substance in the liquid-liquid extraction stage. This solvent selectively extracts ethanol from the water-ethanol mixture, breaking the azeotropic relationship and enabling pure ethanol recovery that cannot be achieved by distillation alone

Inventive Principle:
Principle #24Intermediary (Mediator)

2Adaptability or versatility

If butanol is present in the water-ethanol mixture, then the mixture can be treated, but separation is complicated by formation of water-butanol azeotrope

Engineering Contradiction:
Improvemixture treatment capabilityVSAvoidseparation process complexity
Core Design Contradiction:
Adaptability or versatilityVSDevice complexity

Solution Approach 1:

Butanol is selectively removed from the mixture in the liquid-liquid extraction stage using an organic solvent. The solvent preferentially extracts butanol due to its chemical properties, separating it from the water-ethanol system before the final distillation stage, thus simplifying the overall separation process

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The process utilizes differences in chemical parameters (solubility, polarity) rather than just physical parameters (boiling point). By changing the separation mechanism from thermal distillation to chemical extraction, the process can handle complex multi-component mixtures including azeotropes that are difficult to separate by traditional distillation

Inventive Principle:
Principle #35Parameter changes

3Productivity

If butanol is recycled with ethanol in the Lebedev process, then butanol can be reused, but butanol accumulates and reduces catalyst selectivity

Engineering Contradiction:
Improvebutadiene yieldVSAvoidcatalyst performance
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

Butanol is selectively extracted and separated from the recycled stream using liquid-liquid extraction. The purified ethanol is recovered for recycling to the reactor, while butanol is removed from the recycle loop. This prevents butanol accumulation that would otherwise poison the catalyst, while still allowing ethanol recycling to maintain productivity

Inventive Principle:
Principle #34Discarding and recovering

4Use of energy by moving object

If butanol is removed without significant energy consumption, then energy efficiency is improved, but pollution of water effluent may occur

Engineering Contradiction:
Improveenergy consumptionVSAvoidwater effluent pollution
Core Design Contradiction:
Use of energy by moving objectVSObject-generated harmful factors

Solution Approach 1:

An organic solvent serves as an intermediary extraction medium that selectively removes butanol from the aqueous stream at low energy cost. The solvent forms a separate organic phase containing butanol, leaving the aqueous phase relatively clean. This avoids high-energy distillation while preventing water pollution through selective phase separation

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

This process enhances ethanol concentration for recycling, reduces energy consumption, and minimizes butanol accumulation in the Lebedev process, improving catalyst selectivity and overall butadiene yield while reducing equipment size and utility consumption.

Implementation Method 1

a water-ethanol separation step, comprising a water-ethanol separation section comprising a distillation column

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 2

a demixing step comprising: a mixing section of said hydroalcoholic solution withdrawn in step a) with the water/butanol/ethanol fraction withdrawn in step c); a settling section of the preceding mixture comprising a settling flask in which the pressure is less than or equal to 6 bar absolute, said settling section producing a heavy phase comprising mainly water and a light phase

Methodology Applied
Scientific EffectDensity gradient separation: Density Gradient

Data Source

PatentEP3802472B1Partial extraction of butanol from an aqueous solution containing ethanol and butanol
Publication Date: 2024.12.11 IFP ENERGIES NOUVELLES
  • EP3802472B1 patent drawingFigure 1
  • EP3802472B1 patent drawingFigure 2

AI summary

The invention relates to a method for treating a hydroalcoholic feedstock comprising ethanol and butanol to produce an ethanol-rich effluent, a water-rich effluent and a butanol-rich effluent, comprising a) a water-ethanol separation step comprising a distillation column supplied with said hydroalcoholic feedstock and comprising at least 14 theoretical plates, a molar reflux ratio of less than or equal to 1.2, a side stream in the butanol accumulation region and two injections of recycled flows from steps b) and c); b) a demixing step comprising a section for mixing the flow drawn off in step a) and the fraction drawn off in step c), and a settling section, the heavy phase being recycled to the distillation column of step a); c) a butanol separation step comprising a distillation column supplied by the light phase from step b), comprising a side stream of a water/butanol/ethanol fraction recycled to the mixing section of step b) and producing a butanol-rich effluent and an ethanol-water distillate recycled to the distillation column of step a). Said method appears to be particularly useful for treating hydroalcoholic effluent in the context of the Lebedev method.