Crystallization Device with Light Scattering Feedback Control

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Solution Overview

Problem

Current methods for producing isopulegol and menthol face challenges in efficiently recovering ligands, particularly due to the use of expensive catalysts and complex synthesis processes, leading to unsatisfactory yields and purities, and require precise control of crystallization conditions for complex molecular structures.

Innovation Solution

A device and method that uses electromagnetic radiation to detect the intensity of scattered crystals, regulating the solution temperature to achieve the desired seed crystal formation and growth, allowing for precise control of crystallization conditions and improved recovery of ligands through crystallization processes.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional crystallization methods are used for ligand recovery, then the process is simpler to operate, but the yield and purity of ligand recovery are unsatisfactory

Engineering Contradiction:
Improveyield and purity of ligand recoveryVSAvoidoperational complexity of crystallization control
Core Design Contradiction:
Manufacturing precisionVSEase of operation

Solution Approach 1:

The patent implements online monitoring of the crystallization process using light scattering technology to detect crystal formation in real-time. The system continuously measures the intensity of light scattered by forming crystals and uses this feedback to automatically adjust cooling rates and other process parameters, ensuring optimal crystallization conditions are maintained throughout the process. This closed-loop control system enables precise control of crystal growth while maintaining ease of operation through automation.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The patent replaces conventional mechanical or manual monitoring methods with optical detection technology. By using light scattering measurements to detect crystal formation and growth, the system substitutes direct mechanical observation or sampling with non-intrusive optical sensing, enabling continuous real-time monitoring without disrupting the crystallization process. This substitution allows for more precise control while simplifying the operational interface.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

2Reliability

If expensive catalyst complexes are used for citronellal cyclization, then the catalytic activity is sufficient, but the cost of production increases and catalyst recovery becomes difficult

Engineering Contradiction:
Improvecatalytic activityVSAvoidproduction cost and catalyst recovery
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The patent employs heterogeneous catalysts that can be easily separated from the reaction mixture through filtration or decantation. The catalyst design incorporates support materials that allow for simple physical separation, enabling the catalyst to be recovered, washed, and reused in subsequent reactions. This approach maintains high catalytic activity while dramatically reducing production costs by eliminating the need for expensive catalyst synthesis and complex recovery procedures associated with homogeneous catalysts.

Inventive Principle:
Principle #34Discarding and recovering

3Productivity

If the crystallization process is accelerated to reduce production time, then the productivity increases, but the crystal size and morphology become unsuitable for separation

Engineering Contradiction:
Improvecrystallization speedVSAvoidcrystal size and morphology control
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent implements dynamic control of the crystallization process by continuously adjusting cooling rates based on real-time monitoring of crystal formation. The system transitions from static, predetermined cooling schedules to adaptive dynamic control, where the cooling rate is automatically modified during the process to maintain optimal crystal growth conditions. This enables accelerated crystallization while preserving crystal quality through continuous parameter optimization.

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The patent utilizes real-time changes in process parameters (temperature, cooling rate, agitation speed) based on monitored crystal formation progress. By dynamically adjusting these parameters during crystallization rather than maintaining fixed conditions, the system achieves both high productivity and excellent crystal morphology. The ability to modify parameters on-the-fly allows the process to adapt to changing conditions and maintain optimal performance throughout.

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 enhances the efficiency and yield of isopulegol and menthol production by ensuring ideal crystal size and morphology, reducing the time required for separation, and facilitating the recovery of ligands with high purity, thus improving the economic viability of the process.

Implementation Method 1

with which electromagnetic radiation can be radiated into the solution and the intensity of the electromagnetic radiation scattered by crystals present in the solution can be detected

Methodology Applied
Scientific EffectLight scattering: Scattering

Implementation Method 2

a temperature control device for changing the temperature of the solution being introduced and/or the solution being introduced

Methodology Applied
Scientific EffectTemperature control: Heating

Implementation Method 3

Device for separating a substance by crystallization from a solution of the substance. The separation is carried out using a crystallization process

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentEP3919148B1Device for separating a substance from a solution
Publication Date: 2024.05.08 BASF SE
  • EP3919148B1 patent drawingFigure 1
  • EP3919148B1 patent drawingFigure 2
  • EP3919148B1 patent drawingFigure 3

AI summary

The present invention relates to a device for separating a substance from a solution of the substance by crystallization, comprising a crystallization vessel (1) which includes an opening for introducing the solution, a temperature control device (5, 7) for changing the temperature of the solution to be introduced and/or introduced, a temperature sensor (6, 8) for measuring the temperature of the solution to be introduced and/or introduced, a scattering light probe (9) which is arranged inside the crystallization vessel (1) and with which electromagnetic radiation can be radiated into the solution, wherein the electromagnetic radiation radiated into the solution has the form of a beam whose opening angle is greater than 5 degrees and is in the visible spectral range or is infrared radiation, and an intensity of the electromagnetic radiation scattered by crystals located in the solution can be detected, and a control unit (10).which is coupled to the temperature sensor (6, 8), the scattering light probe (9) and the temperature control device (5, 7), with which the temperature of the solution in the crystallization vessel (1) can be controlled, wherein the control unit (10) is designed such that, in order to set a desired quantity of seed crystals, the intensity of the electromagnetic radiation scattered by crystals in the solution is detected, the detected intensity is compared with a target intensity (Is), the temperature of the solution is controlled as a function of the difference between the detected intensity and the target intensity (Is) such that the magnitude of this difference decreases, and, if the magnitude of the difference between the detected intensity and the target intensity (Is) is less than a limit value, the desired quantity of seed crystals for the crystallization process is present and a crystallization process can be initiated.by which crystals of the substance are obtained, and a separation unit (11) for separating the obtained crystals.