Countercurrent Steam Stripping for Glyoxylic Acid Purification

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Solution Overview

Problem

Current methods for purifying glyoxylic acid from aqueous reaction media containing hydrochloric acid are inefficient, as they require high energy consumption or large amounts of materials, and fail to reduce hydrochloric acid concentrations below 5000 ppm, posing corrosion risks and being unsuitable for high glyoxylic acid concentrations.

Innovation Solution

A countercurrent steam stripping process is employed to separate glyoxylic acid from an aqueous reaction medium containing hydrochloric acid, operating under reduced pressure and with a controlled steam-to-medium ratio, effectively reducing hydrochloric acid concentrations to very low levels in the purified glyoxylic acid solution.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional techniques (evaporation, electrodialysis, ion exchange resins) are used to remove hydrochloric acid, then some purification is achieved, but energy consumption is high and hydrochloric acid content cannot be reduced below 5000 ppm

Engineering Contradiction:
Improvehydrochloric acid contentVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by moving object

Solution Approach 1:

The invention changes the operating parameters by conducting steam stripping under reduced pressure (vacuum conditions) rather than at atmospheric pressure. This parameter change allows the process to achieve lower hydrochloric acid removal levels (below 5000 ppm) while consuming less energy, as the vacuum condition facilitates more efficient mass transfer and reduces the energy required for water evaporation

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention utilizes phase transition of water from liquid to vapor through steam stripping. By introducing steam into the aqueous glyoxylic acid solution, water evaporates and carries away hydrochloric acid in the vapor phase, which is then condensed and separated. This phase transition mechanism enables effective removal of hydrochloric acid to levels below 5000 ppm with moderate energy consumption

Inventive Principle:
Principle #36Phase transitions

2Manufacturing precision

If conventional techniques are used to remove hydrochloric acid, then some purification is achieved, but large amounts of materials (resins, energy) are required

Engineering Contradiction:
Improvehydrochloric acid contentVSAvoidamount of resins and energy
Core Design Contradiction:
Manufacturing precisionVSQuantity of substance

Solution Approach 1:

The invention extracts hydrochloric acid from the aqueous glyoxylic acid solution through steam stripping. The steam acts as a carrier that selectively removes water and dissolved hydrochloric acid from the liquid phase, concentrating the glyoxylic acid while eliminating hydrochloric acid to levels below 5000 ppm. This extraction method avoids the need for large amounts of ion exchange resins or other material-intensive processes

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The steam stripping process is self-sustaining in that the steam generated from a portion of the feed solution is sufficient to drive the removal of hydrochloric acid throughout the column. The process uses the latent heat of vaporization and the mass transfer driven by the steam flow to achieve continuous purification without requiring external heating systems or large amounts of chemical additives

Inventive Principle:
Principle #25Self-service

3Manufacturing precision

If evaporation techniques are used to remove hydrochloric acid, then concentration is achieved, but an azeotropic hydrochloric acid-water mixture is formed, preventing further purification

Engineering Contradiction:
Improvehydrochloric acid contentVSAvoidazeotropic mixture formation
Core Design Contradiction:
Manufacturing precisionVSStability of the object's composition

Solution Approach 1:

The invention creates a vacuum environment (reduced pressure) during steam stripping, which effectively removes oxygen and other gases from the system. This inert environment prevents the formation of azeotropic mixtures that would occur at atmospheric pressure, allowing continuous removal of hydrochloric acid below the azeotropic concentration limit. The vacuum condition enables the system to operate beyond the azeotropic barrier

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

4Productivity

If glyoxylic acid concentration is increased to improve productivity, then yield is improved, but viscosity increases making hydrochloric acid removal more difficult

Engineering Contradiction:
Improveglyoxylic acid concentrationVSAvoidhydrochloric acid removal difficulty
Core Design Contradiction:
ProductivityVSEase of manufacture

Solution Approach 1:

The invention changes the temperature and pressure parameters during steam stripping to optimize mass transfer. By operating at elevated temperatures and reduced pressures, the process maintains effective heat and mass transfer even in highly concentrated (viscous) glyoxylic acid solutions. This allows the process to handle high productivity streams with minimal resistance from viscosity

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The steam stripping column operates continuously, with steam flowing upward through the packed bed and aqueous glyoxylic acid solution flowing downward. This continuous contact between steam and liquid maintains consistent mass transfer conditions throughout the column, preventing viscosity buildup from interfering with hydrochloric acid removal. The continuous operation allows high concentrations to be processed efficiently

Inventive Principle:
Principle #20Continuity of useful 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

This process significantly reduces hydrochloric acid concentrations to less than 50 ppm, making it suitable for high glyoxylic acid concentrations and reducing energy and material consumption, thus addressing industrial inefficiencies and corrosion issues.

Implementation Method 1

a step of countercurrent steam stripping of the reaction medium in order to obtain, on the one hand, a gas phase containing the volatile hydrochloric acid and, on the other hand, a liquid phase containing the purified glyoxylic acid

Methodology Applied
Scientific EffectSteam stripping: Pervaporation

Implementation Method 2

Glyoxylic acid is usually obtained by oxidation of glyoxal using nitric acid in the presence of an inorganic acid such as hydrochloric acid, in an aqueous medium

Methodology Applied
Scientific EffectOxidation: Oxidation

Data Source

PatentEP2244997B1Process of separation of glyoxylic acid from an aqueous reaction medium containing glyoxylic acid and hydrochloric acid
Publication Date: 2012.11.21 CLARIANT SPECIALTY FINE CHEMICALS (FRANCE)
  • EP2244997B1 patent drawing

AI summary

The invention relates to a process for separating glyoxylic acid starting from an aqueous reaction medium containing glyoxylic acid and hydrochloric acid, comprising a step of countercurrent steam stripping of the reaction medium in order to obtain, on the one hand, a gas phase containing the volatile hydrochloric acid and, on the other hand, a liquid phase containing the purified glyoxylic acid.