Spray-Drying Complexing Agent Salts for Powder Crystallinity

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Solution Overview

Problem

Existing processes for producing glycine-N,N-diacetic acid derivatives, such as methylglycine-N,N-diacetic acid (MGDA) salts, face challenges with thermal lability in alkaline media, leading to low yields and high by-product formation, and result in powders with high residual moisture that are prone to clumping, requiring additional costly granulation steps.

Innovation Solution

A spray-drying process is employed using an aqueous solution of complexing agent salts with the addition of crystalline fine dust having smaller particle diameters than the desired powder, allowing for increased crystallinity and controlled particle size, achieving powders with 7-14% residual moisture and improved storage and processing properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If spray-drying is used to produce powder from aqueous solution, then production cost is reduced and processing is simplified, but the powder has high residual moisture and poor storage properties

Engineering Contradiction:
Improveproduction cost and process simplicityVSAvoidstorage stability and flowability
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The invention changes the residual moisture parameter from the conventional low range (<5%) to an optimized range of 5-15% through controlled spray-drying conditions. This parameter change improves storage stability and prevents caking while maintaining production efficiency and avoiding costly granulation steps

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention performs preliminary concentration of the aqueous solution to 40-70% solids content before spray-drying. This preliminary action ensures optimal drying performance and prevents excessive residual moisture, thereby improving storage stability without requiring additional granulation processing

Inventive Principle:
Principle #10Preliminary action

2Ease of operation

If conventional spray-drying produces amorphous powder with low residual moisture, then flowability is improved, but storage stability deteriorates due to caking

Engineering Contradiction:
ImproveflowabilityVSAvoidstorage stability
Core Design Contradiction:
Ease of operationVSReliability

Solution Approach 1:

The invention optimizes the residual moisture parameter to 5-15% and controls the degree of crystallinity through spray-drying parameters. This creates a powder that maintains both good flowability and storage stability, eliminating the trade-off between these properties

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention produces a composite powder structure with controlled crystalline and amorphous phases. The crystalline portion provides storage stability while the amorphous portion maintains flowability, achieving both desirable properties simultaneously

Inventive Principle:
Principle #40Composite materials

3Reliability

If additional granulation step is added to improve storage properties, then storage stability is improved, but production cost and process complexity increase

Engineering Contradiction:
Improvestorage stabilityVSAvoidprocess steps
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The invention combines the drying and granulation steps into a single spray-drying operation. By optimizing the spray-drying parameters, the process simultaneously achieves moisture removal, particle formation, and storage stability improvement, eliminating the need for separate granulation equipment and operations

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The invention extracts the granulation function from the conventional two-step process and integrates it into the spray-drying step. This reduces process complexity by removing the additional granulation equipment and operational steps while maintaining storage stability

Inventive Principle:
Principle #2Taking out (Extraction)

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 produces powders with enhanced crystallinity and storage properties, reducing clumping issues and eliminating the need for costly granulation steps, while maintaining flowability and ease of processing.

Implementation Method 1

in a spray-drying process, comprising an atomization step and a drying step

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 2

with the addition of crystalline fine dust of the same complexing agent salt(s) as are present in the aqueous solution

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentUS9540597B2Process for the preparation of a powder comprising one or more complexing agent salts
Publication Date: 2017.01.10 BASF SE
  • US9540597B2 patent drawing
  • US9540597B2 patent drawing
  • US9540597B2 patent drawing

AI summary

A process for the preparation of a powder comprising one or more complexing agent salts of the general formulacomprises atomizing an aqueous solution comprising the one or more complexing agent salts in the presence of a crystalline fine dust of the same complexing agent salts and a drying step, wherein the concentration of the one or more complexing agent salt is from 10 to 80% by weight, based on the total weight of the aqueous solution, with an upper limit for the average particle diameter of the crystalline fine dust which is lower by at least a factor of 2 than the lower limit of the average particle diameter of the powder obtained after the process, and the fraction of the crystalline fine dust is from 0.1 to 20% by weight, based on the weight of the powder obtained after the process.