Two-Step Vacuum Drying for Halohydantoin Purity
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Solution Overview
Problem
Halohydantoin compounds are unstable at normal temperatures, decompose when suspended in water or mixed solvents, leading to purity loss and equipment corrosion, with existing methods failing to achieve high purity and prevent decomposition during drying.
Innovation Solution
A method involving a two-step drying process in a dryer under reduced pressure, first removing the organic solvent at 15-50°C and then water and elemental halogen at up to 90°C, with temperature and pressure settings adjusted to prevent decomposition and achieve high purity.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Productivity
If halohydantoin compound is dried at high temperature to remove solvents efficiently, then productivity is improved, but the halohydantoin compound decomposes and liberates iodine causing purity loss and equipment corrosion
Solution Approach 1:
The drying process is divided into two distinct stages: first removing organic solvent at lower temperature (15-50°C), then removing water at higher temperature (up to 90°C). This segmentation prevents decomposition by avoiding high temperature exposure when organic solvent is present, while still achieving complete drying and high productivity.
Solution Approach 2:
The organic solvent is removed first at lower temperature before the halohydantoin compound is exposed to higher drying temperatures. This preliminary removal of the organic solvent prevents subsequent decomposition reactions that would occur if high temperature drying was applied directly to the wet material containing organic solvent.
2Device complexity
If halohydantoin compound is dried under atmospheric pressure, then equipment complexity is reduced, but manufacturing precision and purity are compromised due to decomposition
Solution Approach 1:
The drying process utilizes reduced pressure (vacuum) conditions to lower the boiling points of solvents, enabling removal of organic solvent and water at lower temperatures. This parameter change prevents thermal decomposition while maintaining manufacturing precision and compound purity.
3Device complexity
If single-step drying is used to simplify the process, then device complexity is reduced, but the halohydantoin compound decomposes and liberates iodine causing harmful effects
Solution Approach 1:
The drying process is segmented into two temperature stages with distinct objectives: first stage removes organic solvent at 15-50°C, second stage removes water at up to 90°C. This prevents iodine liberation and equipment corrosion by avoiding high temperature exposure during the presence of organic solvent, while still achieving complete drying.
Solution Approach 2:
The invention converts the potential harm of high temperature drying (decomposition and iodine liberation) into a benefit by using reduced pressure conditions. The vacuum environment allows water removal at lower temperatures, transforming what would be a harmful high-temperature process into a gentle low-temperature drying process that preserves compound integrity.
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 method effectively stabilizes halohydantoin compounds, preventing decomposition and maintaining high purity, while also avoiding equipment corrosion, allowing for efficient production and storage.
Implementation Method 1
removing the organic solvent from the composition, at a temperature in a range of not less than 15°C and not greater than 50°C
Implementation Method 2
The steps (i) and (ii) are performed under a reduced pressure
Implementation Method 3
removing the at least one of the water and the elemental halogen from the composition refined in the step (i) at a temperature in a range of not greater than 90°C
Implementation Method 4
The steps (i) and (ii) are performed under a reduced pressure
Data Source
Figure 1

AI summary
A method of the present invention for producing a halohydantoin compound by refining, in a dryer (1), a composition containing at least one of water and elemental halogen, an organic solvent, and the halohydantoin compound, the method includes the steps of: (i) removing the organic solvent from the composition; and (ii) removing the at least one of the water and the elemental halogen from the composition refined in the step (i).