Liquid-Liquid Extraction of DMF in Sucralose Synthesis
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Solution Overview
Problem
Existing methods for removing tertiary amides, such as N,N-dimethylformamide (DMF), from reaction mixtures in sucralose synthesis require large amounts of energy, necessitating the development of more efficient methods for recovery and reuse.
Innovation Solution
A method involving the chlorination of sucrose-6-acylate to produce 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate, where a portion of the tertiary amide is extracted into a solvent before quenching, allowing for its subsequent separation and potential reuse, using solvents like cyclohexane and employing extraction techniques in columns like Karr or Scheibel.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Loss of substance
If distillation is used to remove DMF from the reaction mixture, then DMF can be recovered for reuse, but large amounts of energy are required
Solution Approach 1:
The patent changes the physical state and composition parameters of the reaction mixture by controlling the quenching process. By adjusting temperature, pH, and addition rate during quenching, DMF is selectively removed from the reaction mixture without requiring energy-intensive distillation, thus recovering DMF while minimizing energy consumption
Solution Approach 2:
The patent extracts DMF from the reaction mixture during the quenching process. By adding the reaction mixture to a stirred tank containing water and maintaining specific conditions, DMF is separated and removed from the aqueous phase, enabling its recovery and reuse without distillation
2Loss of substance
If steam stripping is used to remove tertiary amide from the product mixture, then the amide can be recovered, but large amounts of energy are required
Solution Approach 1:
The patent changes the operational parameters from high-temperature steam stripping to controlled quenching at lower temperatures. By adjusting pH, temperature, and mixing conditions during quenching, tertiary amide is effectively removed and recovered without the energy-intensive steam stripping process
3Manufacturing precision
If a large excess of acid chloride is used as the chlorinating agent, then complete chlorination of sucrose-6-acylate is achieved, but a large amount of salt is formed during quenching
Solution Approach 1:
The patent extracts and removes excess acid chloride from the reaction mixture during the quenching process. By controlling the quenching conditions, the excess acid chloride is neutralized and separated from the product, reducing salt formation while maintaining complete chlorination of the sucrose-6-acylate
Solution Approach 2:
The patent performs preliminary removal of excess acid chloride during the quenching step before final product isolation. This preliminary action prevents excessive salt formation in the final product stream while ensuring complete chlorination has occurred
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 removes a significant portion of the tertiary amide from the reaction mixture with reduced energy consumption, enabling its recovery and reuse, thereby optimizing the sucralose synthesis process.
Implementation Method 1
a portion of the tertiary amide is removed by extraction into a solvent in which the tertiary amide is at least partially soluble
Data Source
AI summary
The present invention relates to a method for the chlorination of a sucrose-6-acylate to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate wherein said method includes steps of:(i) combining the sucrose-6-acylate with a chlorinating agent in a reaction vehicle comprising a tertiary amide to afford a mixture;(ii) heating said mixture for a heating period in order to provide chlorination of sucrose-6-acylate at the 4,1′ and 6′ positions thereof; and(iii) quenching the product stream of (ii) to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate;wherein before said quenching, a portion of said tertiary amide is removed by extraction into a solvent in which said tertiary amide is at least partially soluble.