DFA III Crystallization pH Control

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Solution Overview

Problem

Current industrial processes for producing difructose dianhydride III (DFA III) face challenges in maintaining crystal yield due to decomposition of substances at high temperatures and acidic conditions, leading to impurities and reduced purity, with no established efficient method for industrial crystallization.

Innovation Solution

Maintaining the pH of DFA III solutions between 5 and 8, preferably 6 to 8, during concentration and crystallization steps, and using alkaline agents to adjust pH, along with chromatographic methods to remove acidic substances, ensures stable crystal yield and high purity by suppressing decomposition and inhibiting factors like fructose and sucrose.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If concentration and crystallization are performed at high temperatures and acidic conditions to improve productivity, then the production speed increases, but the crystal yield decreases due to decomposition of substances

Engineering Contradiction:
Improveproduction speedVSAvoidcrystal yield
Core Design Contradiction:
ProductivityVSLoss of substance

Solution Approach 1:

The patent applies parameter changes by adjusting the pH of the solution to 5 or more, transforming the chemical environment from acidic to weakly acidic or neutral conditions. This parameter change prevents decomposition of DFA III and other substances during concentration and crystallization, thereby maintaining high crystal yield while enabling efficient industrial production. The pH adjustment is a fundamental parameter modification that resolves the contradiction between production speed and substance preservation.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If purification steps are increased to improve product purity, then the purity of DFA III crystals increases, but the process complexity and production time increase

Engineering Contradiction:
Improvepurity of DFA III crystalsVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent applies preliminary action by adjusting the pH to 5 or more before concentration and crystallization steps. This preliminary pH adjustment creates optimal conditions that prevent decomposition and facilitate efficient crystallization in a single step. By preparing the solution in advance with the correct pH, the patent achieves high purity crystals without requiring multiple sequential purification steps, thus reducing process complexity while maintaining high manufacturing precision.

Inventive Principle:
Principle #10Preliminary action

3Productivity

If recycling of crystal syrups is implemented to improve productivity, then the production efficiency increases, but the crystal yield decreases over time due to accumulation of inhibitory substances

Engineering Contradiction:
Improveproduction efficiencyVSAvoidcrystal yield
Core Design Contradiction:
ProductivityVSLoss of substance

Solution Approach 1:

The patent applies parameter changes by maintaining the pH at 5 or more throughout the recycling process. This consistent pH parameter prevents the accumulation of inhibitory substances that would otherwise decompose DFA III and reduce crystal yield over time. By controlling this critical parameter, the system can continuously recycle crystal syrups indefinitely without loss of productivity or crystal yield, resolving the contradiction between production efficiency and substance preservation in long-term operation.

Inventive Principle:
Principle #35Parameter changes

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 approach allows for the efficient industrial production of DFA III crystals with maintained or increased crystal yield and high purity by controlling pH and removing inhibitory substances, overcoming previous limitations in DFA III crystallization.

Implementation Method 1

Maintaining the pH of DFA III solutions between 5 and 8, preferably 6 to 8, during concentration and crystallization steps

Methodology Applied
Scientific EffectpH control:

Implementation Method 2

using alkaline agents to adjust pH

Methodology Applied
Scientific EffectpH adjustment with alkaline agents:

Implementation Method 3

chromatographic methods to remove acidic substances

Methodology Applied
Scientific EffectChromatography: Chromatography

Implementation Method 4

concentrating the resulting filtrate for crude crystallization

Methodology Applied
Scientific EffectConcentration:

Implementation Method 5

crystallizing the concentrate, and separating the crystal syrup

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentUS8039615B2Process for producing difructose dianhydride III crystals
Publication Date: 2011.10.18 NIPPON BEET SUGAR MFG CO LTD
  • US8039615B2 patent drawing
  • US8039615B2 patent drawing
  • US8039615B2 patent drawing

AI summary

The invention provides a process for producing the crystals of difructose dianhydride III (DFA III), namely a indigestible disaccharide where two fructose molecules are bonded to each other at positions 1,2′ and 2,3′ (di-D-fructofuranose-1,2′,2,3′-dianhydride), where solutions containing DFA III are adjusted to and/or maintained at pH 5 or more, preferably pH 5 to 8, and more preferably 6 to 8. In accordance with the invention, DFA III can be produced industrially without lowering the crystal yield even when the crystallization thereof is done in a recycling system; additionally by adjusting the total fructose content in mother solutions for (crude) crystallization to 5% or less per a solid content basis and adjusting the fructose content to 1% or less, DFA III can more effectively be produced.