Tetraalkyl Bisphosphate Extraction from Aqueous Reaction Mixtures
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Solution Overview
Problem
Existing processes for preparing tetraalkyl bisphosphates are inefficient, leading to high impurity levels and low yields, making them unsuitable for industrial production due to the complexity of solvent use, multiple work-up operations, and difficulties in separating water-soluble products.
Innovation Solution
Reacting tetrachlorobisphosphates with alcohols and neutralizing the resulting hydrogen chloride with a base, followed by extraction from an aqueous reaction mixture to isolate tetraalkyl bisphosphates, which allows for better yields and easier purification of fully or partly water-soluble products.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Ease of manufacture
If traditional processes using pyridine and multiple solvents are used to prepare tetraalkyl bisphosphates, then the reaction can proceed, but the process becomes complex with multiple work-up operations and solvent removal steps
Solution Approach 1:
The invention extracts and removes the problematic pyridine solvent from the process by replacing it with water as the reaction medium. This eliminates the need for multiple solvent removal operations and simplifies the work-up procedure, directly resolving the contradiction between process execution and complexity
Solution Approach 2:
The invention changes the fundamental parameter of the reaction medium from organic solvent (pyridine) to water. This parameter change transforms the entire process from requiring multiple extraction and drying steps to a simplified aqueous-based procedure with single-phase reaction and simple product isolation
2Manufacturing precision
If multiple work-up operations and solvent washes are performed to purify tetraalkyl bisphosphates, then impurity levels decrease, but the number of操作步骤 increases and productivity decreases
Solution Approach 1:
The aqueous reaction medium performs multiple functions simultaneously: it serves as the reaction solvent, automatically neutralizes HCl byproducts through water dissolution, and facilitates direct product isolation without requiring sequential washing and drying operations. This self-service approach maintains high purity while maximizing productivity
3Manufacturing precision
If water washing is used to remove impurities from tetraalkyl bisphosphates, then acidic impurities are removed, but water-soluble products cannot be separated from the aqueous phase
Solution Approach 1:
Instead of using water to wash away impurities from the product phase (traditional approach), the invention inverts the approach by conducting the reaction directly in water. The product precipitates or separates from the aqueous phase, allowing impurities to remain dissolved in water while the pure product is recovered, eliminating product loss to aqueous washes
4Manufacturing precision
If pyridine is used to neutralize HCl and form pyridine hydrochloride, then the acid is neutralized, but pyridine residues remain in the product and require additional extraction steps
Solution Approach 1:
The invention replaces pyridine with water as the neutralizing agent. Water, being inexpensive and volatile, neutralizes HCl to form dissolved salts that remain in the aqueous phase, while the organic product separates cleanly. No additional extraction steps are needed to remove the 'neutralizing agent' since water evaporates completely or remains in the aqueous phase
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 results in higher yields and purer tetraalkyl bisphosphates with reduced impurities, particularly acidic and electrolytic impurities, making the process more industrially viable for both fully and partly water-soluble products.
Implementation Method 1
neutralizing the resultant hydrogen chloride with a base
Implementation Method 2
isolating the desired product from the reaction mixture by extraction
Data Source
AI summary
The present invention relates to a process for preparing tetraalkyl bisphosphates by reacting tetrachlorobisphosphates with alcohols, neutralizing the resultant hydrogen chloride with a base, and isolating the desired product from the reaction mixture by extraction.