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
Engineering 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
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%).
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.
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
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.
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.
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
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.
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.
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
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.
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.
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
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.
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.
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
Implementation Method 2
spray drying tower, allowing for the formation and precipitation of stable powder complexes without the need for supports or excipients
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
Data Source
Figure 1
Figure 2
Figure 3~4
AI summary
The present invention relates to powdered compositions of a complex between an acid and a metal and their preparation process.