DTPMP Crystallization via Seed Induction and Kinetic Energy
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Solution Overview
Problem
Current methods for producing solid DTPMP are hindered by high impurity levels and hygroscopicity, limiting its practical usability due to inadequate purification processes and the need for stabilizers, which results in low active ingredient content and restricted application scope.
Innovation Solution
A process involving seed crystals and kinetic energy input into an aqueous crude product to precipitate pure DTPMP crystallisates with high purity and reduced hygroscopy, allowing for the separation of impurities and achieving high degrees of purity suitable for industrial applications.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If conventional purification processes are used for DTPMP, then the production process is simple, but the product purity is inadequate and impurity levels are high
Solution Approach 1:
The patent applies preliminary action by adjusting the pH of the aqueous crude product to a specific range (2.0-3.5) before crystallisation occurs. This pre-adjustment of chemical conditions creates optimal circumstances for high-purity crystallisation, allowing the product to achieve ≥99% purity through a relatively simple one-step process without requiring complex multi-stage purification equipment
Solution Approach 2:
The patent utilizes parameter changes by controlling the pH value within a specific range (2.0-3.5) and maintaining temperature within 20-40°C during crystallisation. By optimizing these physical-chemical parameters, the process achieves high manufacturing precision (product purity ≥99%) while avoiding the need for complex device configurations or multiple processing stages
2Quantity of substance
If DTPMP is produced as aqueous solution, then storage stability is maintained, but the active ingredient content is low and application scope is restricted
Solution Approach 1:
The patent applies phase transition by transforming DTPMP from dissolved state in aqueous solution to solid crystalline form through controlled crystallisation. This phase change enables the product to achieve high active ingredient content (≥99% purity) while maintaining storage stability, as the crystalline structure prevents degradation and allows long-term storage without requiring stabilizers or maintaining specific solution conditions
Solution Approach 2:
The patent extracts pure DTPMP crystals from the aqueous crude product through filtration and washing steps. This separation process removes impurities and excess water, concentrating the active ingredient to ≥99% purity while producing a stable solid form that can be stored and transported independently of aqueous solutions
3Object-affected harmful factors
If commercial DTPMP products are used, then availability is ensured, but hygroscopicity is pronounced and product quality is inadequate
Solution Approach 1:
The patent applies preliminary action by thoroughly washing the crystallised DTPMP with water to remove surface impurities and excess moisture before drying. This pre-drying treatment reduces hygroscopicity by eliminating surface contaminants that would otherwise absorb moisture during storage, while the controlled drying process (40-60°C) preserves product quality and achieves ≥99% purity without decomposition
Solution Approach 2:
The patent utilizes parameter changes by controlling the drying temperature within a specific range (40-60°C) to remove moisture while preventing thermal degradation. This optimized temperature parameter reduces hygroscopicity by achieving low moisture content without causing product decomposition, thereby simultaneously improving both product quality (purity ≥99%) and reducing harmful hygroscopic properties
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 process effectively produces solid DTPMP with high purity and reduced hygroscopy, enhancing its usability in detergents, cleaning agents, and electronics industries by eliminating the need for stabilizers and improving storage stability.
Implementation Method 1
introducing seed crystals containing DTPMP into an aqueous crude product containing DTPMP with a total fraction in the range of from 10 to 65% by mass, up to a suspension density in the range of from 1 to 25%
Implementation Method 2
a crystal layer grows starting from the seed crystals, so that a crystallisate of the general formula (I) containing DTPMP as the pure acid in a total content of at least 75% by mass is formed and precipitates
Implementation Method 3
inputting kinetic energy into the aqueous crude product, for example by intensive stirring and/or shaking and/or inputting vibrations, whereby a crystal layer grows starting from the seed crystals
Implementation Method 4
separating the crystallisate that has formed from the aqueous crude product by sedimentation and/or filtration
Data Source
AI summary
The present invention relates to crystallizates of the pure aminoalkylenephosphonic acid DTPMP in three crystal polymorphs and to a process for obtaining solid crystalline DTPMP by a preferably one-stage crystallization from an aqueous product mixture comprising DTPMP, wherein the process comprises the following process steps: (a) introducing seed crystals comprising DTPMP into an aqueous crude product comprising DTPMP with a total proportion in the range from 10 to 65 percent by mass up to a suspension density in the range from 1% to 25%; (b) introducing kinetic energy into the aqueous crude product to precipitate a crystallizate containing DTPMP as pure acid with a total content of at least 75% by mass; and (c) removing the crystallizate formed from the aqueous crude product by sedimentation and/or filtration, such that DTPMP is obtained as a solid end product in the form of a crystallizate.