APPARATUS FOR EXTRACTION AND EFFECTIVE DISTILLATION PROCES

Abstract

The smart Soxhlet extraction apparatus (101) designed to optimize the efficiency of solvent-based extractions. The apparatus features an improved condenser (102) with a spiral design made from high thermal conductivity alloy, a specially designed extraction chamber (103) with internal baffles and embedded sensors, and an innovative heating mantle (104) utilizing ceramic heating elements with aerogel insulation. The apparatus is equipped with a microprocessor-controlled system (105) for precise control and monitoring of extraction parameters, a unique solvent recovery mechanism (106) capable of recovering up to 95% of the solvent, and a modular design framework (107) for easy customization and maintenance. Advanced materials (108) such as corrosion-resistant alloys and fluoroelastomers ensure durability and performance. The method involves sample preparation, solvent selection, parameter programming, and automated extraction with data collection. This smart system enhances extraction efficiency and minimizes solvent consumption.

Specification

Description:The following is a step-by-step description of the invention, detailing the components, and their functionalities mentioned below:

The novel Soxhlet extraction apparatus of the present invention is now described in detail with reference to the embodiments illustrated in the accompanying drawings. It should be noted that while specific materials, dimensions, and configurations are mentioned, these are for illustrative purposes only and should not be considered limiting to the scope of the invention.

The apparatus (101) has a number of interlinked elements for the enhancement of particular stages in the process of extraction. The apparatus consists of an improved condenser (102) specifically designed to cool and condense vapour for the recovery of solvent. An extraction chamber (103), specifically designed to distribute solvent as uniformly as possible with all the opportunities for effective extraction of compounds, is used. A novel heating mantle (104) controls heating and realizes the possibilities of accurate regulation of temperature so that extraction conditions are best optimized. A microprocessor control system (105) is used for automated control of parameters such as temperature and timing and adjustments in the process itself, yielding a consistent outcome with as little operator intervention as possible. Loss of solvents is at a minimum in the unique solvent recovery mechanism (106). The entire system increases efficiency. Built on a modular design framework (107), the apparatus allows flexibility and ease in maintenance and scaling up for application to specific extraction needs. Advanced materials are used in its construction throughout, so that the chemical resistance, durability, and long-term reliability in operational behaviour, as built in modern extraction processes are guaranteed.

The condenser (102) is designed with a novel spiral configuration that significantly boosts cooling efficiency, enhancing its performance by 40% over traditional straight-tube condensers. Constructed from a high thermal conductivity copper-silver alloy (108), with a thermal conductivity rating of 400 W/(m·K), the condenser optimizes heat transfer, ensuring rapid and effective condensation. Its spiral design increases the surface area available for heat exchange, maximizing its ability to condense vapors efficiently. Additionally, the condenser features a double-wall design with a vacuum-insulated layer between the inner and outer walls. This design helps minimize heat loss to the environment while preventing condensation from forming on the exterior surface. The integration of microchannels within the walls, through which the coolant (typically water) flows, further improves the heat transfer efficiency, making this condenser a highly effective and energy-saving component in the extraction process.

The extraction chamber (103) is constructed from borosilicate glass, offering superior chemical resistance and transparency, allowing for clear visual monitoring during extraction. Its unique geometry, enhanced by internal baffles (103a), promotes a turbulent flow pattern, which significantly improves the contact between the solvent and sample, ensuring efficient extraction of target compounds. The chamber is highly versatile, with an adjustable capacity ranging from 100 mL to 5 L, making it adaptable to a variety of batch sizes and applications. Embedded within the chamber walls are temperature and pressure sensors (103b) that continuously provide real-time data on critical extraction conditions. This data is fed to the microprocessor-controlled system (105), which dynamically adjusts parameters like temperature and pressure to ensure optimal extraction efficiency. The chamber's base incorporates an advanced filtration system (103c), featuring a sintered glass disk with adjustable porosity. This innovative design ensures that solid particles are filtered out while allowing the solvent to percolate smoothly, facilitating a clean and efficient extraction process.

The heating mantle (104) is designed with advanced ceramic heating elements arranged in a helical pattern around the extraction flask, providing uniform heat distribution across the entire surface. This configuration ensures rapid and precise temperature control, allowing the system to quickly adapt to changes in extraction conditions. The heating elements can achieve temperatures of up to 300°C, with a precision of ±0.1°C, enabling highly accurate thermal regulation for optimal extraction processes. Surrounding the heating elements is a layer of aerogel insulation (104a), which minimizes heat loss, making the heating mantle highly energy efficient. This insulation helps maintain the desired temperature within the chamber while preventing excess heat from dissipating into the environment. The outer layer of the mantle is constructed from a heat-resistant polymer that remains cool to the touch, ensuring operator safety during use and preventing accidental burns. This combination of advanced materials and design offers both efficiency and safety in high-temperature extraction operations.

The microprocessor-controlled system (105) serves as the brain of the apparatus, seamlessly overseeing and automating the entire extraction process. It includes a central processing unit (CPU), multiple input/output modules for capturing real-time data, and an intuitive high-resolution touchscreen display that allows users to interact with the system easily. The microprocessor constantly gathers input from a network of sensors, such as temperature sensors in both the heating mantle and extraction chamber, pressure sensors, and flow rate sensors in the solvent recovery system, ensuring that all operational parameters are closely monitored and precisely controlled. This intelligent system can automatically adjust critical parameters, such as temperature, pressure, and solvent flow rate, to maintain optimal extraction conditions throughout the process. Users can also program multi-stage extraction protocols with customizable settings for each stage, such as varying temperatures or flow rates. The integration of machine learning modules further enhances its capabilities, enabling the system to analyse historical performance data and refine extraction parameters for each sample, improving both efficiency and precision over time.

The solvent recovery mechanism (106) is a pivotal innovation that dramatically reduces solvent consumption and waste. It comprises a distillation column (106a), a condensation unit (106b), and a purified solvent reservoir (106c), all integrated seamlessly into the apparatus. After each extraction cycle, the used solvent flows through the distillation column, where impurities are separated. The purified solvent vapor then enters the condensation unit, which employs Peltier cooling elements for efficient and compact condensation. The recovered solvent is collected in the purified solvent reservoir, where it is stored for reuse in subsequent extraction cycles. This continuous recovery and purification process allows the system to reclaim up to 95% of the solvent, significantly reducing solvent consumption, operational costs, and environmental impact.

The modular design framework (107) of the apparatus offers flexible customization, easy maintenance, and scalability. Each component is engineered as a detachable module, allowing for quick disconnection and replacement. This design supports seamless reconfiguration to meet varying extraction needs; for instance, the extraction chamber can be replaced with one of a different size or material without affecting other system parts. Using standardized connections and interfaces, the modular system ensures compatibility across different configurations, supporting a wide range of extraction applications. Additionally, it simplifies maintenance and cleaning processes, making the apparatus suitable for compliance with current Good Manufacturing Practices (cGMP) in pharmaceutical production.

The apparatus incorporates advanced materials (108) to improve performance, durability, and chemical resistance. The condenser (102) and heating mantle (104) utilize high thermal conductivity alloys, such as copper-silver, for efficient heat transfer. Wetted parts are constructed from borosilicate glass, PTFE, and high-grade stainless steel, ensuring excellent chemical resistance and preventing contamination. Seals and gaskets are made from fluoroelastomers, which resist chemical degradation and retain their integrity over a wide temperature range, enhancing long-term reliability. The outer casing of the apparatus is made from a composite material that is lightweight yet strong, offering superior thermal insulation while maintaining structural integrity.

Method of extraction (200) and distillation using Soxhlet extraction apparatus involves the following steps:

Preparing a sample and loading it into the extraction chamber (201): The process incorporates preparing the sample material, ensuring it is ground to a uniform particle size, typically between 0.5 to 1 mm, to facilitate efficient extraction. Weigh an appropriate quantity of the sample, generally ranging from 5 to 20 grams, depending on the size of the extraction chamber. Place the weighed sample into a cellulose thimble, which is designed to hold the material while allowing the solvent to pass through easily, and load it into the extraction chamber.

Selecting an appropriate solvent (202): Choose a solvent or solvent mixture that is suitable for the target compounds in your sample. Common solvents used in pharmaceutical extractions include ethanol, methanol, and ethyl acetate. The selection should consider the solubility of the desired compounds and the extraction efficiency required for the specific application.

Programming extraction parameters using the microprocessor-controlled system (203): Use the intuitive touchscreen interface of the microprocessor-controlled system to set up the extraction protocol. Program essential parameters such as the heating rate, target temperature(generally 10°C above the boiling point of the solvent), extraction time (usually 4 to 8 hours), solvent flow rate (typically between 3 to 5 mL/min), and the number of extraction cycles (usually 15 to 30). This setup allows for precise control over the extraction conditions.

Initiation and Monitoring of the Extraction Process (204): Initiate the extraction process via the microprocessor-controlled system, which will automate the heating of the solvent and control the extraction cycles. During this phase, the system continuously monitors process parameters, such as temperature and flow rates, displaying real-time data on the touchscreen interface. This enables the user to ensure optimal conditions are maintained throughout the extraction.

Collecting the extract and analysing the extraction data (205): Upon completing the programmed extraction cycles, allow the apparatus to cool before collecting the extract from the distillation flask. Analyse the collected extract to determine the concentration of target compounds and evaluate the efficiency of the extraction process. This data can be utilized to refine future extraction protocols and enhance overall extraction performance.




Method of Performing of the Invention:

The operation of the novel Soxhlet extraction apparatus begins with the user loading the sample into the extraction chamber (103) and selecting the appropriate extraction protocol via the touchscreen interface of the microprocessor-controlled system (105).

The heating mantle (104) brings the solvent in the distillation flask to boiling point. The microprocessor continually adjusts the heating power to maintain the optimal temperature throughout the extraction process.

As the solvent vapor rises, it enters the improved condenser (102) where it is efficiently cooled and liquefied. The condensed solvent then drips into the extraction chamber (103), where it percolates through the sample, extracting the desired compounds.

When the solvent level in the extraction chamber reaches a certain point, it is automatically siphoned back into the distillation flask through the novel filtration system (103c), carrying the extracted compounds with it

This cycle repeats automatically, with each cycle concentrating the extract in the distillation flask. The microprocessor-controlled system (105) monitors the process parameters and makes adjustments as needed to maintain optimal extraction conditions.

Simultaneously, the unique solvent recovery mechanism (106) continuously purifies and recycles the solvent, significantly reducing solvent consumption.

The modular design (107) allows for easy customization of the setup for different extraction needs, while the use of advanced materials (108) throughout ensures durability and optimal performance.

Upon completion of the extraction, the microprocessor-controlled system (105) automatically shuts down the heating and initiates a cooling cycle. The extracted solution can then be easily collected from the distillation flask for further processing.

This novel Soxhlet extraction apparatus thus provides a highly efficient, flexible, and controlled extraction process, addressing the key limitations of traditional extractors and meeting the evolving needs of the pharmaceutical industry.


Sample Preparation:

• Begin by grinding the sample material to a uniform particle size, typically within the range of 0.5-1 mm. This uniformity enhances the extraction efficiency.
• Weigh an appropriate amount of the sample, usually between 5-20 g, depending on the size of the extraction chamber (103).
• Place the prepared sample into a cellulose thimble and load it into the extraction chamber.

Solvent Selection:

• Choose an appropriate solvent or solvent mixture for the target compounds. Common solvents for pharmaceutical extractions include ethanol, methanol, or ethyl acetate, as they effectively dissolve a wide range of active compounds.

Apparatus Setup:

• Assemble the modular components (107) of the apparatus according to the specific extraction requirements. Ensure that all connections are secure and that the system is completely leak-free.
Protocol Programming:

• Utilize the touchscreen interface of the microprocessor-controlled system (105) to set up the extraction protocol. Program the following parameters:
• Heating Rate and Target Temperature: Typically set to 5°C/min until reaching a final temperature that is 10°C above the solvent's boiling point.
• Extraction Time: Usually between 4-8 hours, depending on the specific sample characteristics.
• Solvent Flow Rate: Typically around 3-5 mL/min.
• Number of Extraction Cycles: Generally between 15-30 cycles to ensure thorough extraction.

Extraction Process:

• Initiate the extraction process via the control system. The apparatus will automatically heat the solvent, manage the extraction cycles, and oversee the solvent recovery process.
• Continuously monitor the extraction parameters on the touchscreen display for real-time feedback.

Post-Extraction:

• Once the programmed extraction cycles are complete, allow the system to cool down before handling.
• Collect the extract from the distillation flask for further analysis or application.
• Utilize the built-in cleaning cycle to clean the apparatus thoroughly.

Data Analysis:

• Retrieve the extraction data log from the microprocessor-controlled system (105) post-extraction.
• Analyze this data to optimize future extraction processes for similar sample types, improving efficiency.

Solvent Recovery:

• Assess the solvent recovery rate within the solvent recovery mechanism (106) to ensure efficient solvent reuse.
• If necessary, top up the purified solvent reservoir (106c) to prepare for subsequent extractions.

Maintenance:

• After each extraction, run the automated cleaning cycle to prevent cross-contamination between samples.
• Periodically inspect the modular components (107) and replace any worn or damaged parts to maintain operational efficiency.

Safety Considerations:

• Always operate the apparatus in a well-ventilated area or under a fume hood to ensure safety from solvent vapors.
• Wear appropriate personal protective equipment (PPE) when handling solvents and samples to protect against exposure.
• Regularly check the integrity of all seals and connections to prevent potential solvent leaks, ensuring a safe working environment.
This method leverages the innovative features of the apparatus, maximizing extraction efficiency while minimizing solvent consumption and reducing the need for operator intervention.
, Claims:1. A smart extraction using Soxhlet extraction apparatus (101), the apparatus comprising:
a) an improved condenser (102) with a spiral design, and constructed from a high thermal conductivity alloy;
b) a specially designed extraction chamber (103) with internal baffles (103a), and embedded sensors (103b);
c) an innovative heating mantle (104) with ceramic heating elements, and aerogel insulation (104a);
d) a microprocessor-controlled system (105) for regulating extraction parameters;
e) a unique solvent recovery mechanism (106) including a distillation column (106a), condensation unit (106b), and purified solvent reservoir (106c); and
f) a modular design framework (107) allowing for easy customization and maintenance;
wherein, the apparatus components are constructed using advanced materials (108) for improved performance and durability.

2. A method (200) of performing extraction using Soxhlet extraction apparatus, comprising the steps of:
a) preparing a sample and loading it into the extraction chamber (201);
b) selecting an appropriate solvent (202);
c) programming extraction parameters using the microprocessor-controlled system (203);
d) initiating and monitoring the extraction process (204);
e) collecting the extract and analysing the extraction data (205).

3. The smart extraction apparatus as claimed in claim 1, wherein the improved condenser (102) features a double-wall design with a vacuum-insulated layer and microchannels for coolant flow.

4. The smart extraction apparatus as claimed in claim 1, wherein the extraction chamber (103) incorporates a novel filtration system (103c) consisting of a sintered glass disk with controllable porosity.

5. The smart extraction apparatus as claimed in claim 1, wherein the heating mantle (104) is capable of reaching temperatures up to 300°C with a precision of ±0.1°C.

6. The smart extraction apparatus as claimed in claim 1, wherein the microprocessor-controlled system (105) incorporates machine learning modules for optimizing extraction parameters.

7. The smart extraction apparatus as claimed in claim 1, wherein the solvent recovery mechanism (106) is capable of recovering up to 95% of the solvent used in the extraction process.

8. The smart extraction apparatus as claimed in claim 1, wherein the modular design framework (107) uses standardized connections and interfaces for easy reconfiguration.

9. The smart extraction apparatus as claimed in claim 1, wherein the advanced materials (108) include high thermal conductivity alloys, corrosion-resistant materials, and advanced fluoroelastomers for seals and gaskets.

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