D,L-Methionine Crystallization via CO2 Neutralization

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Solution Overview

Problem

Current industrial processes for producing D,L-methionine face challenges in achieving high bulk density and purity, particularly due to issues with crystallization and filtration, leading to energy inefficiencies and impurity incorporation.

Innovation Solution

A process involving alkaline hydrolysis of 5-(2-methylmercaptoethyl)hydantoin, followed by neutralization with carbon dioxide at elevated temperatures and crystallization in the presence of seed crystals, allowing for controlled crystal growth and separation of D,L-methionine with high bulk density and purity without the need for recrystallization.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If methionine is precipitated from process solution using conventional carbonation at low temperature, then methionine product is obtained, but the crystals form as very flat leaflets that are difficult to handle and slowly separate from mother liquor

Engineering Contradiction:
Improvefiltration speedVSAvoidcrystal shape
Core Design Contradiction:
ProductivityVSShape

Solution Approach 1:

The patent applies parameter changes by conducting carbonation at elevated temperatures (65-95°C) instead of conventional low temperatures, and by adding seed crystals to control nucleation. These parameter changes transform the crystal morphology from flat leaflets to more compact, filterable crystals that separate quickly from mother liquor.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs preliminary action by adding seed crystals before the carbonation reaction to control crystal nucleation and growth. This pre-seeding approach directs the formation of crystals with favorable morphology and size, preventing the formation of difficult-to-filter flat leaflets and improving subsequent filtration performance.

Inventive Principle:
Principle #10Preliminary action

2Manufacturing precision

If recrystallization is performed to obtain sufficient purity and quality, then methionine purity is improved, but energy consumption increases and processing time is extended

Engineering Contradiction:
Improvemethionine purityVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by moving object

Solution Approach 1:

The patent achieves high purity (exceeding 99% methionine content) by optimizing carbonation parameters including elevated temperature (65-95°C), turbulent mixing conditions, and controlled cooling rates. These parameter changes enable direct crystallization from concentrated process solution without requiring energy-intensive recrystallization steps.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent extracts impurities from the process solution during the controlled crystallization process, allowing direct filtration of high-purity methionine crystals. This approach eliminates the need for separate recrystallization purification steps, reducing both energy consumption and processing time while maintaining purity exceeding 99%.

Inventive Principle:
Principle #2Taking out (Extraction)

3Manufacturing precision

If recrystallization steps are performed to improve product quality, then purity is enhanced, but processing complexity and time are increased

Engineering Contradiction:
Improveproduct purityVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent merges the carbonation reaction and crystallization steps into a single integrated process. By conducting carbonation at elevated temperatures with turbulent mixing followed by controlled cooling in the presence of seed crystals, the process achieves both complete neutralization and high-purity crystal formation in one operation, eliminating separate recrystallization steps and simplifying the overall process flow.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent applies preliminary action by adding seed crystals before carbonation to control crystal growth from the beginning. This pre-seeding approach ensures that crystals form with the desired morphology and purity directly during the carbonation reaction, eliminating the need for subsequent recrystallization operations and reducing process complexity.

Inventive Principle:
Principle #10Preliminary action

4Productivity

If process solution is highly concentrated to improve productivity, then output increases, but impurity interference and crystallization difficulties arise

Engineering Contradiction:
Improveoutput concentrationVSAvoidcrystallization performance
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent successfully processes highly concentrated methionine solutions (up to 3000 ppm and higher) by changing the carbonation temperature parameter to elevated levels (65-95°C) and applying turbulent mixing conditions. These parameter changes prevent impurity interference and ensure reliable crystallization even at high concentrations, maintaining both productivity and crystallization performance.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs preliminary action by adding seed crystals to highly concentrated process solutions before carbonation. This pre-seeding approach provides nucleation sites that guide crystal growth, preventing the interference of impurities and ensuring reliable crystallization performance even at high concentrations, thereby maintaining both productivity and product quality.

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 a high bulk density of up to 600 g/L and purity exceeding 99% methionine content, improving filtration performance and reducing energy consumption by avoiding recrystallization steps, while allowing for more concentrated processing without interference from impurities.

Implementation Method 1

neutralizing the alkali methioninate solution at a temperature of between 65° C. and 95° C. by turbulent mixing with carbon dioxide

Methodology Applied
Scientific EffectNeutralization reaction: Chemical Bonding

Implementation Method 2

crystallizing the D,L-methionine product in the presence of D,L-methionine seed crystals by cooling the process solution to a temperature range of between 25° C. and 35° C.

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 3

cooling the process solution to a temperature range of between 25° C. and 35° C.

Methodology Applied
Scientific EffectCooling: Cooling

Implementation Method 4

an alkali methioninate solution is obtained by alkaline hydrolysis of 5-(2-methylmercaptoethyl)hydantoin

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Implementation Method 5

neutralizing the alkali methioninate solution at a temperature of between 65° C. and 95° C. by turbulent mixing with carbon dioxide

Methodology Applied
Scientific EffectTurbulence: Turbulence

Data Source

PatentUS12195422B2Process for the preparation of D,L-methionine
Publication Date: 2025.01.14 EVONIK OPERATIONS GMBH
  • US12195422B2 patent drawing
  • US12195422B2 patent drawing
  • US12195422B2 patent drawing

AI summary

The invention relates to a single cycle process for preparing D,L-methionine from an alkali methioninate solution obtained by alkaline hydrolysis of 5-(2-methylmercaptoethyl)hydantoin, in which the D,L-methionine is obtained by neutralizing the alkali methioninate solution with carbon dioxide at elevated temperature and subsequently crystallizing D,L-methionine in the presence of seed crystals.