Type II Crystalline Topramezone Sodium Salt Hydrate for Granulation

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Solution Overview

Problem

The anhydrous topramezone sodium salt is prone to agglomeration during jet pulverization and has limited application due to difficulties in granulation, and its aqueous preparation is limited by solubility, requiring costly long-time crystallization at low temperatures for the more stable hydrate form.

Innovation Solution

A type II crystalline topramezone sodium salt hydrate with 0.5-2.0 moles of water is developed, characterized by specific X-ray powder diffraction patterns and prepared through methods involving heating and filtration, which reduces energy consumption and processing challenges, and a herbicidal composition incorporating this form is created.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Quantity of substance

If anhydrous topramezone sodium salt is used for preparation, then the active ingredient content is high, but the material is prone to agglomeration during jet pulverization and difficult to granulate

Engineering Contradiction:
Improveactive ingredient contentVSAvoidgranulation processability
Core Design Contradiction:
Quantity of substanceVSEase of manufacture

Solution Approach 1:

The patent changes the hydration state parameter of topramezone sodium salt from anhydrous to hydrate form (0.5-2.0 moles of water per mole of salt). This parameter change fundamentally alters the material's physical properties, making it suitable for granulation while maintaining high active ingredient content (70-90% in WG preparations).

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent utilizes the phase transition between anhydrous and hydrate forms of topramezone sodium salt. By controlling the crystallization process to form the hydrate phase instead of the anhydrous phase, the material gains improved processability for granulation and jet pulverization while retaining high potency.

Inventive Principle:
Principle #36Phase transitions

2Reliability

If type I topramezone sodium salt hydrate is prepared to improve stability and processing, then the preparation stability is improved, but long-time crystallization at low temperature is required

Engineering Contradiction:
Improvepreparation stabilityVSAvoidcrystallization time
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The patent identifies and characterizes a new crystal form (type II hydrate with 0.5-2.0 moles water) that differs from type I hydrate. This parameter change in crystal structure allows for dramatically reduced crystallization time (from 10-48 hours at -10°C to room temperature crystallization) while maintaining or improving preparation stability.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs a pre-concentration step before crystallization, where the aqueous solution is concentrated to a specific solid content range (10-50%). This preliminary action prepares the solution in an optimal state for rapid crystallization at room temperature, eliminating the need for long-time low-temperature crystallization.

Inventive Principle:
Principle #10Preliminary action

3Ease of operation

If aqueous preparation is used to improve solubility and processing, then the processability is improved, but the active ingredient content is limited by solubility

Engineering Contradiction:
ImproveprocessabilityVSAvoidactive ingredient content
Core Design Contradiction:
Ease of operationVSQuantity of substance

Solution Approach 1:

The patent utilizes the phase transition from dissolved state to crystalline hydrate form during the preparation process. By concentrating the aqueous solution and inducing crystallization of the hydrate form, the patent achieves both high processability (through aqueous handling) and high active ingredient content (70-90% in the final WG preparation) in the solid product.

Inventive Principle:
Principle #36Phase transitions

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 type II crystalline hydrate offers improved stability and processing advantages over the anhydrous form, reducing costs and energy consumption, and the herbicidal composition effectively controls undesired plant growth with enhanced stability and solubility.

Implementation Method 1

stirring an aqueous solution of topramezone sodium salt while heating the solution to dissolve the topramezone sodium salt completely

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 2

concentrating the filtrate obtained in step 1) under reduced pressure and while heating to remove water

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 3

suspending a mixture of an anhydrous substance of topramezone sodium salt and the type II crystalline topramezone sodium salt in water of a co-solvent

Methodology Applied
Scientific EffectSuspension: Suspension

Data Source

PatentUS12162869B2Type II crystalline topramezone sodium salt hydrate, preparation method therefor and use thereof
Publication Date: 2024.12.10 ALBAUGH LLC
  • US12162869B2 patent drawing
  • US12162869B2 patent drawing
  • US12162869B2 patent drawing

AI summary

A type II crystalline topramezone sodium salt hydrate, a preparation method of the type II crystalline topramezone sodium salt hydrate and the use thereof in herbicidal compositions is provided. An X-ray powder diffraction pattern of the hydrate recorded by Cu-Ka radiation at 25° C. shows at least 3 of the following reflections at 2θ values:2θ=9.63±0.2°  (1)2θ=11.00±0.2°  (2)2θ=11.97±0.2°  (3)2θ=13.13±0.2°  (4)2θ=14.36±0.2°  (5)2θ=15.37±0.2°  (6)2θ=17.24±0.2°  (7)2θ=18.01±0.2°  (8)2θ=19.12±0.2°  (9)2θ=19.65±0.2°  (10)2θ=22.03±0.2°  (11)2θ=23.20±0.2°  (12)2θ=25.29±0.2°  (13)2θ=27.29±0.2°  (14)2θ=27.93±0.2°  (15)2θ=28.90±0.2°  (16).