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

VSEngineering 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

Engineering Contradiction:
Improvedrying efficiencyVSAvoidcompound stability
Core Design Contradiction:
ProductivityVSReliability

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.

Inventive Principle:
Principle #1Segmentation

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.

Inventive Principle:
Principle #10Preliminary action

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

Engineering Contradiction:
Improvedrying system complexityVSAvoidcompound purity
Core Design Contradiction:
Device complexityVSManufacturing precision

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.

Inventive Principle:
Principle #35Parameter changes

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

Engineering Contradiction:
Improvedrying process complexityVSAvoidiodine liberation and corrosion
Core Design Contradiction:
Device complexityVSObject-generated harmful factors

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.

Inventive Principle:
Principle #1Segmentation

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.

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

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

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 2

The steps (i) and (ii) are performed under a reduced pressure

Methodology Applied
Scientific EffectReduced pressure: Depressurisation

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

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 4

The steps (i) and (ii) are performed under a reduced pressure

Methodology Applied
Scientific EffectReduced pressure: Depressurisation

Data Source

PatentEP2937338B1Production method and production device for halo-hydantoin compound, reuse system, and halo-hydantoin compound
Publication Date: 2019.07.10 NIPPON CHEMICALS CO LTD
  • EP2937338B1 patent drawingFigure 1
  • EP2937338B1 patent drawing
  • EP2937338B1 patent drawing

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).