Dioxolane Process Phase Separation Methanol Recovery

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Solution Overview

Problem

Existing processes for preparing dioxolane result in high losses of the valuable product and require significant amounts of auxiliary substances that need to be purified or discharged, leading to inefficiencies and waste.

Innovation Solution

A process involving a reaction distillation device where ethylene glycol and formaldehyde are reacted in the presence of a catalyst, with a phase separation unit and organic extracting agent to enhance separation, recycle the extracting agent, and withdraw a side stream containing methanol to prevent accumulation, thereby increasing dioxolane yield and purity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If benzene is used as an extracting agent to break the azeotrope in dewatering column, then water removal efficiency is improved, but the process requires additional purification steps and generates waste that must be discharged

Engineering Contradiction:
Improvewater removal efficiencyVSAvoidwaste discharge
Core Design Contradiction:
ProductivityVSLoss of substance

Solution Approach 1:

The invention extracts and removes benzene from the process by introducing a side stream withdrawal unit that specifically removes benzene from the distillation column output. This extracted benzene is then recycled back to the dewatering column, eliminating waste discharge while maintaining the azeotrope-breaking function.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

Instead of discharging benzene-containing waste, the invention recovers benzene through the side stream withdrawal unit and recycling system. The benzene is discarded from the waste stream and recovered for reuse, transforming a waste disposal problem into a resource recovery solution.

Inventive Principle:
Principle #34Discarding and recovering

2Manufacturing precision

If multiple distillation columns are used to purify dioxolane, then product purity is improved, but part of the valuable dioxolane product is lost due to necessary discharge from the top of the purification column

Engineering Contradiction:
Improvedioxolane purityVSAvoiddioxolane loss
Core Design Contradiction:
Manufacturing precisionVSLoss of substance

Solution Approach 1:

The invention implements a feedback mechanism where the distillate from the purification column, which contains dioxolane, is not discharged but instead recycled back to the dewatering column. This closed-loop feedback system maintains product purity while preventing valuable dioxolane loss.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The invention ensures continuous useful action by recycling the dioxolane-containing distillate back into the process rather than discontinuing it through discharge. This continuous circulation maintains both purity requirements and minimizes product loss.

Inventive Principle:
Principle #20Continuity of useful action

3Reliability

If a side stream containing methanol is withdrawn from the waste water column, then methanol accumulation is prevented, but an additional process step is required

Engineering Contradiction:
Improvestable operationVSAvoidprocess steps
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The invention applies preliminary action by proactively withdrawing methanol through the side stream before it can accumulate to problematic levels. This preventive measure ensures stable operation by maintaining methanol concentrations within safe operating parameters throughout the process.

Inventive Principle:
Principle #10Preliminary action

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 achieves high purity of dioxolane with minimal product loss and complete recycling of the extracting agent, ensuring stable and efficient operation by efficiently separating components and removing side products like methanol.

Implementation Method 1

transferring a distillate stream containing raw product from the top of the reaction distillation device to a phase separation unit, wherein an organic extracting agent is present in the phase separation unit

Methodology Applied
Scientific EffectLiquid-liquid extraction: Liquid-Liquid Extraction

Implementation Method 2

transferring an organic fraction stream from the phase separation unit to an upper part of a purification column, withdrawing a bottom product stream containing dioxolane from the purification column

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 3

reacting ethylene glycol and formaldehyde in aqueous solution in the presence of at least one catalyst to obtain a raw product which comprises water, dioxolane and methanol

Methodology Applied
Scientific EffectCatalysis: Catalysis

Data Source

PatentEP3793986B1Process for preparing dioxolane
Publication Date: 2023.12.20 BASF SE
  • EP3793986B1 patent drawingFigure 1
  • EP3793986B1 patent drawingFigure 2
  • EP3793986B1 patent drawingFigure 3

AI summary

The present invention relates to a process for preparing dioxolane by reacting ethylene glycol with an aqueous solution of formaldehyde in the presence of an acid catalyst. The raw product comprising water, dioxolane and methanol is fed to a phase separation unit (20) wherein an organic extracting agent is present. An organic fraction stream from the phase separation unit is transferred to an upper part of a purification column (30) from which dioxolane is withdrawn as a bottom product while the distillate stream of the purification column is recycled to the phase separation unit. An aqueous fraction stream from the phase separation unit is transferred to a waste water column (40), withdrawing a waste water stream from the bottom of the waste water column, recycling a distillate stream (42) from the waste water column to the phase separation unit, and withdrawing a side stream (43) containing methanol from a stage below the feed stage of the waste water column.