L-Glufosinate Ammonium Purification by pH-Controlled Precipitation
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Solution Overview
Problem
Existing methods for producing optically pure L-glufosinate ammonium are inefficient, costly, and lack effective downstream purification routes, particularly in biocatalytic processes, leading to low recovery rates and product purity.
Innovation Solution
A method involving biocatalytic transformation, calcium sulfate precipitation, zinc salt precipitation, pH adjustment, and recrystallization in ethanol or acetone solutions to obtain high-purity L-glufosinate ammonium powder, with byproducts being recycled for value-added products.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Ease of manufacture
If biocatalytic transformation is used to produce L-glufosinate ammonium, then the process is simpler and uses fewer additives, but the downstream purification is insufficient leading to low product purity and recovery rate
Solution Approach 1:
The purification process is divided into multiple sequential steps: calcium salt precipitation to remove gluconic acid, zinc salt precipitation to remove residual ammonium sulfate, pH adjustment, and recrystallization. Each step targets specific impurities, progressively improving product purity while maintaining process simplicity
Solution Approach 2:
The process utilizes pH adjustment as a key parameter to control precipitation and crystallization. By adjusting pH to specific ranges (4.5-5.5 for calcium precipitation, then adjusting to precipitate zinc salt, finally adjusting to pH 2-3 for product crystallization), the method selectively separates different components, achieving high purity without complex equipment
2Manufacturing precision
If conventional chemical synthesis methods are used, then purification can be achieved through esterification and hydrolysis, but the process is more complex and costly
Solution Approach 1:
The invention replaces complex chemical synthesis and purification steps with biocatalytic transformation followed by simple precipitation and crystallization. Instead of using esterification reagents, hydrolysis enzymes, and multiple chemical treatment steps, the method uses enzymatic resolution followed by pH-controlled precipitation, significantly simplifying the process while maintaining high purity
Solution Approach 2:
The method uses pH adjustment as the primary control parameter throughout the process, replacing the need for complex chemical reactions. By controlling pH at different stages, the process achieves selective precipitation of impurities and final product crystallization, eliminating the need for multiple chemical treatment steps required in conventional methods
3Manufacturing precision
If ion exchange or membrane filtration is used for purification, then some separation can be achieved, but the recovery rate remains low and costs increase
Solution Approach 1:
The invention utilizes phase transition from dissolved state to precipitated state through pH adjustment. By adjusting pH to specific ranges, the product and impurities transition from soluble to insoluble forms, allowing easy separation by filtration. This phase transition approach achieves both high purity and high recovery rate, avoiding the losses associated with membrane filtration and ion exchange
Solution Approach 2:
The invention converts the harmful effect of gluconic acid byproduct (which forms equilibrium with gluconolactone and complicates purification) into a beneficial separation mechanism. By adjusting pH to 4.5-5.5, gluconic acid precipitates as calcium gluconate, allowing easy removal. The same pH adjustment later causes the desired product to crystallize, turning the purification challenge into a simple precipitation-crisstallization process
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
The method is simple, economical, and achieves high recovery rates and product purity, with recyclable additives promoting sustainable development.
Implementation Method 1
adding calcium hydroxide or calcium oxide to react with the ammonium sulfate to produce calcium sulfate precipitates
Implementation Method 2
adding zinc salt, adjusting pH to 5.5-6.8 to produce glufosinate ammonium zinc salt precipitates
Implementation Method 3
adding a solvent to dissolve the glufosinate ammonium zinc salt precipitates collected in step (3), and adjusting pH of a solution to 2-2.5 to produce L-glufosinate ammonium precipitates
Implementation Method 4
recrystallizing the L-glufosinate ammonium precipitates obtained in step (4) to obtain purified L-glufosinate ammonium powder
Data Source
AI summary
The present invention discloses a method for preparing L-glufosinate ammonium powder. The method includes the following steps: (1) obtaining a transformation solution for performing biocatalytic transformation to prepare L-glufosinate ammonium, and filtering out bacteria to obtain a filtrate; (2) detecting the amount of ammonium sulfate in the filtrate obtained in step (1), adding calcium hydroxide or calcium oxide to react with the ammonium sulfate to produce calcium sulfate precipitates, and filtering out the calcium sulfate precipitates to obtain a filtrate; (3) detecting the amount of glufosinate ammonium in the filtrate obtained in step (2), adding zinc salt, adjusting pH to 5.5-6.8 to produce glufosinate ammonium zinc salt precipitates, and filtering and collecting the glufosinate ammonium zinc salt precipitates; (4) adding a solvent to dissolve the glufosinate ammonium zinc salt precipitates collected in step (3), and adjusting pH of a solution to 2-2.5 to produce L-glufosinate ammonium precipitates; and (5) recrystallizing the L-glufosinate ammonium precipitates obtained in step (4) to obtain purified L-glufosinate ammonium powder. The method provided by the present invention is simple to operate and low in cost, and has a better industrialization prospect.