HMTBA Metal Complex Powder via Spray Drying

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Solution Overview

Problem

Current processes for preparing metal salts of HMTBA are inefficient due to the use of supports or excipients, leading to clogging, reduced active ingredient content, and increased costs, and existing methods require multiple steps and additional drying operations, which reduce productivity and result in unsuitable particle sizes for animal feed applications.

Innovation Solution

A single-step process involving the direct contact of HMTBA with a mineral source of a metal in a spray drying tower, allowing for the formation and precipitation of stable powder complexes without the need for supports or excipients, enabling high dry extract and efficient particle formation.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Quantity of substance

If HMTBA is reacted with calcium source in highly concentrated aqueous solution, then the reaction medium becomes very viscous and sticky, but this makes it very difficult to homogenize in mixers or reactors equipped with conventional stirring systems

Engineering Contradiction:
Improveconcentration of HMTBA solutionVSAvoidhomogenization difficulty
Core Design Contradiction:
Quantity of substanceVSEase of manufacture

Solution Approach 1:

The patent uses a recycling stream of calcium salt product as an intermediary substance to modify the reaction medium properties. By introducing 10-50 wt% of the final calcium salt product back into the reaction medium, the viscosity and stickiness are reduced, enabling effective homogenization while maintaining high HMTBA concentration (70-90 wt%).

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent changes the physical parameters of the reaction medium by controlling the concentration of HMTBA (70-90 wt%) and the temperature (50-80°C), and by adjusting the composition through recycling of calcium salt product. These parameter changes transform the reaction medium from a viscous,难以混合 state to one that can be effectively homogenized while maintaining high productivity.

Inventive Principle:
Principle #35Parameter changes

2Ease of manufacture

If calcium salt is recycled from HMTBA to the calcium source before contacting it with HMTBA, then the consistency of the reaction medium improves, but this significantly reduces the productivity of an industrial plant and necessitates a substantial oversizing of the mixer/reactor

Engineering Contradiction:
Improveconsistency of reaction mediumVSAvoidindustrial plant productivity
Core Design Contradiction:
Ease of manufactureVSProductivity

Solution Approach 1:

The patent optimizes the recycling ratio parameter, using only 10-50 wt% of the calcium salt product in the reaction medium rather than the 20-80% range that causes productivity issues. This controlled parameter change maintains adequate consistency improvement while preserving industrial scalability and productivity.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent applies the recycling principle locally and controllably, introducing a specific proportion (10-50 wt%) of recycled calcium salt product at a specific stage in the process, rather than uniformly recycling large amounts throughout the entire system. This localized application maintains consistency benefits without excessive reactor sizing.

Inventive Principle:
Principle #3Local quality

3Ease of manufacture

If organic acid is deposited onto an inert support before adding calcium source, then the reaction can proceed, but the inert support is present in the dry finished product representing 30 to 50% by weight, which reduces the active ingredient content

Engineering Contradiction:
Improveprocessability of reactionVSAvoidactive ingredient content
Core Design Contradiction:
Ease of manufactureVSQuantity of substance

Solution Approach 1:

The patent extracts and eliminates the inert support from the process entirely. By reacting HMTBA directly in aqueous solution with calcium source without any inert support material, the final product contains only the active calcium salt of HMTBA and water, achieving 70-90 wt% active ingredient content in the concentrate.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent replaces the inert support (a permanent, space-consuming component) with a temporary aqueous medium that serves its purpose during reaction and is then completely removed through evaporation, leaving no residual inactive material in the final product.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

4Productivity

If a simple process using an extruder is used to prepare HMTBA salts, then rapid mixing is achieved, but this leads to the formation of vermicelli-like particles which are incompatible with the particle sizes required in the final applications

Engineering Contradiction:
Improvemixing speedVSAvoidparticle size and morphology
Core Design Contradiction:
ProductivityVSShape

Solution Approach 1:

The patent uses phase transition (evaporation of aqueous phase) to transform the reaction mixture from a liquid state during rapid mixing to a solid powder form in the final product. The controlled evaporation process produces fine, free-flowing particles with appropriate morphology for animal feed applications, rather than vermicelli-like structures.

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The patent replaces the mechanical extrusion system (which produces vermicelli shapes) with a chemical reaction followed by evaporation system. The rapid mixing is maintained through efficient contact between aqueous phases, and the particle morphology is controlled by the evaporation process rather than mechanical forcing through a die.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

5Shape

If two-step process with aqueous solution and spray drying is used, then salts in powder form with suitable particle size are produced, but this introduces a further drying step and does not allow for high dry extract of the reaction mixture

Engineering Contradiction:
Improveparticle size suitabilityVSAvoidnumber of processing steps
Core Design Contradiction:
ShapeVSDevice complexity

Solution Approach 1:

The patent merges the reaction step and the concentration step into a single integrated process. The HMTBA and calcium source are reacted in aqueous solution, and the water is evaporated in the same system to produce the final concentrated powder product (70-90 wt% dry matter), eliminating the need for separate spray drying equipment and steps.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent changes the concentration parameter during the process, starting with dilute aqueous solutions for efficient reaction, then progressively concentrating to 70-90 wt% dry matter through evaporation. This continuous parameter change allows high dry extract content to be achieved without clogging, as the system is designed to handle the concentration progression.

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

This process produces stable, homogeneous powder complexes with high amorphous content, suitable for animal feed applications, that can be directly handled and used, avoiding clogging and reducing production costs while maintaining high productivity.

Implementation Method 1

A single-step process involving the direct contact of HMTBA with a mineral source of a metal in a spray drying tower, allowing for the formation and precipitation of stable powder complexes

Methodology Applied
Scientific EffectSpray drying:

Implementation Method 2

spray drying tower, allowing for the formation and precipitation of stable powder complexes without the need for supports or excipients

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 3

contacting said acid with a mineral source of a metal in a spray drying tower to obtain the formation of said complex and to initiate its precipitation

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Data Source

PatentEP3214069B1Powdered compositions of a complex between hmtba and a metal and method for preparing same
Publication Date: 2020.12.16 INNOVIA 3I
  • EP3214069B1 patent drawingFigure 1
  • EP3214069B1 patent drawingFigure 2
  • EP3214069B1 patent drawingFigure 3~4

AI summary

The present invention relates to powdered compositions of a complex between an acid and a metal and their preparation process.