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
Engineering 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
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).
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.
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
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.
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.
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
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.
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
Implementation Method 2
concentrating the filtrate obtained in step 1) under reduced pressure and while heating to remove water
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
Data Source
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).


