Crystalline MGDA Salt Low Hygroscopicity Process

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Solution Overview

Problem

Hygroscopicity issues in granules and powders of methylglycine diacetate (MGDA) and its alkali metal salts lead to lump formation, water-mediated component deactivation, and yellowing, which are undesirable in care formulations.

Innovation Solution

A process involving a 35-60% aqueous solution of MGDA salt at 50-90°C, with the addition of 0.01-2% particulate solid having a specific pore volume, followed by crystallization and removal of crystalline MGDA, results in solid MGDA or its alkali metal salts with low hygroscopicity, forming powders or granules with controlled particle sizes.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Quantity of substance

If MGDA or its alkali metal salts are produced as granules or powders, then active ingredient content is high and shipping is economical, but the products become hygroscopic leading to lump formation and component deactivation

Engineering Contradiction:
Improveactive ingredient contentVSAvoidhygroscopicity
Core Design Contradiction:
Quantity of substanceVSReliability

Solution Approach 1:

The patent changes the physical and chemical parameters of the crystallization process, specifically controlling temperature (50-90°C), concentration (35-60% by weight), and pH conditions to produce a specific crystal form of MGDA salt that inherently exhibits low hygroscopicity while maintaining high active ingredient content

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent utilizes controlled phase transition from aqueous solution to solid crystalline form through temperature-controlled crystallization, transforming the MGDA salt from a hygroscopic state to a stable low-hygroscopicity crystalline state suitable for powder or granule formulations

Inventive Principle:
Principle #36Phase transitions

2Ease of manufacture

If MGDA or its alkali metal salts are produced as granules or powders, then shipping is economical, but water in the product creates a medium for component deactivation

Engineering Contradiction:
Improveshipping efficiencyVSAvoidcomponent deactivation
Core Design Contradiction:
Ease of manufactureVSObject-generated harmful factors

Solution Approach 1:

By optimizing crystallization parameters including temperature control during cooling, concentration levels, and pH conditions, the patent produces a crystalline product with minimal water content that does not create a medium for chemical reactions between incompatible components

Inventive Principle:
Principle #35Parameter changes

3Quantity of substance

If MGDA or its alkali metal salts are produced as granules or powders, then active ingredient content is high, but yellowing occurs when stored with percarbonate

Engineering Contradiction:
Improveactive ingredient contentVSAvoidyellowing
Core Design Contradiction:
Quantity of substanceVSObject-generated harmful factors

Solution Approach 1:

The patent employs specific crystallization conditions including temperature control (50-90°C), concentration management (35-60% by weight), and pH adjustment to produce a crystal form that is chemically stable and resistant to oxidation-induced yellowing when stored with percarbonate

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The crystallization process creates an environment that protects the MGDA salt from oxidation during production, and the resulting crystal structure inherently resists oxidation during storage, preventing yellowing even in the presence of percarbonate

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

4Productivity

If conventional crystallization processes are used, then MGDA crystals can be produced, but crystal removal from the crystallization vessel is tedious

Engineering Contradiction:
Improvecrystal productionVSAvoidcrystal removal
Core Design Contradiction:
ProductivityVSEase of manufacture

Solution Approach 1:

The patent optimizes temperature parameters during crystallization (cooling from 50-90°C to lower temperatures) to control crystal size and morphology, producing crystals that are easier to separate from the mother liquor through filtration or decantation, thereby simplifying removal from the crystallization vessel

Inventive Principle:
Principle #35Parameter changes

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 yields MGDA or its alkali metal salts as powders or granules with low hygroscopicity and stability, preventing lump formation and deactivation, and maintaining color integrity, suitable for use in laundry detergents and dishwashing formulations.

Implementation Method 1

adding 0.01 to 2% by weight of a particulate solid with a pore volume in the range of from 0.25 to 0.75 cm3/g

Methodology Applied
Scientific EffectAdsorption: Adsorption

Implementation Method 2

crystallizing (a)

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentUS11208375B2Process for making solid methylglycine diacetate (MGDA) alkali metal salt, and solid particles
Publication Date: 2021.12.28 BASF SE
  • US11208375B2 patent drawing
  • US11208375B2 patent drawing
  • US11208375B2 patent drawing

AI summary

Process for making solid methylglycine diacetate (MGDA) alkali metal salt (a), said process comprising the steps of (A) providing a 35 to 60% by weight aqueous solution of said MGDA salt having a temperature in the range of from 50 to 90° C., (B) adding 0.01 to 2% by weight of a particulate solid with a pore volume in the range of from 0.25 to 0.75 cm3/g, determined by nitrogen adsorption in accordance with 66134:1998-02 (b), the percentage referring to the content of (a), (C) crystallizing (a), (D) removing said crystalline (a) from the mother liquor.