What Issues Should Be Noted During The Use Of Hydrothermal Synthesis Autoclave?
Feb 05, 2025
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Hydrothermal synthesis autoclave (usually referred to as hydrothermal synthesis reactor) is a reactor that synthesizes chemical substances under certain temperature and pressure conditions, and is widely used in scientific research experiments in new materials, energy, environmental engineering and other fields. In order to ensure the safety and success of the experiment and extend the service life of the equipment, a series of problems need to be paid attention to during use.
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Equipment inspection and preparation
Check the integrity of the reactor
Before use, it is necessary to carefully check whether the reactor body, cover, lining (such as PTFE or PPL), gaskets and other components are intact, and there are no deformation, cracks, wear and other problems.
Check whether the connection parts are tight to ensure the sealing of the reactor. A loose seal may lead to gas leakage during the reaction, affecting the experimental results and even causing danger.
Clean reactor
The reactor needs to be thoroughly cleaned before use to remove residues or impurities left over from the last experiment. This helps to ensure the accuracy and repeatability of the experiment.
When cleaning, you can use warm water and mild detergent, for difficult to remove stains, you can use appropriate chemical cleaning agent, but pay attention to the compatibility of cleaning agent and reactor material.
Prepare the reactants
According to the experimental requirements, accurately weigh the required reactants and ensure that its purity meets the experimental requirements.
If the reactant is corrosive, it needs to be placed in a corrosion-resistant liner (such as a teflon liner) to protect the reactor body from corrosion.
Precautions during operation
Loading reactants:
Pour the treated reactants into the teflon bushing or PPL bushing, and ensure that the feeding factor is less than 0.8 (generally recommended not to exceed 75% of the liner volume).
Be careful when loading to avoid spills or contamination of reactants to other parts of the reactor.
Tighten the reactor:
When tightening the reactor, the top wire should be loosened first, the kettle body and cover should be tightened with a wrench, and then the top wire should be tightened. Use even force to avoid component damage caused by excessive tightening.
Heating operation:
Before heating operations, be sure to read the reactor instructions carefully to understand its maximum temperature and heating rate limits.
Use suitable heating equipment, such as electric blast drying oven, and set the appropriate heating program according to the experimental requirements. The heating equipment should provide an independent working space and be equipped with special heating equipment that can withstand impact resistance.
Strictly control the temperature in the reactor to avoid exceeding the set temperature range. It can be monitored and adjusted using a thermometer or temperature control device. At the same time, when heating away from the heating equipment and work room, in case of danger.
Pressure control and safety measures:
Some reactions may produce gas, resulting in increased pressure in the reactor. Therefore, it is necessary to install appropriate pressure relief devices according to the specific situation, such as pressure reducing valves or explosion-proof membranes.
During operation, the pressure indicator should be checked regularly to ensure that the pressure is within a safe range. If the pressure is found to be abnormally high, corresponding measures should be taken immediately, such as stopping the heating and opening the pressure reducing valve.
Follow laboratory safety regulations and wear appropriate personal protective equipment, such as goggles, gloves, knee-length lab clothing, closed-foot shoes (non-mesh uppers), insulated gloves, impact-proof full-face covers, etc.
Watch the reaction closely:
During the reaction, the situation in the reactor should be closely observed, including temperature, pressure, color changes, etc. Record the experimental data and phenomena in time for subsequent analysis and summary.
Treatment after the reaction is over
Cooling and depressurization
After the reaction, turn off the heater and allow the reactor to cool naturally to room temperature. Be careful not to force cooling with water quenching or other methods, otherwise it may cause the reactor to crack or damage.
In the process of depressurization, attention should be paid to controlling the depressurization speed to avoid excessive depressurization resulting in severe solvent evaporation or reactor rupture.
Open the reactor
Before opening the reactor, make sure there is no pressure in the reactor. You can tell by looking at the pressure indicator or trying to gently rotate the kettle cover. It is strictly prohibited to forcibly disassemble, in case of danger.
When opening the kettle cover, use the appropriate tools and follow the operating procedures. Be careful to avoid burns from reaction products or steam.
Remove the reaction product
Remove the reaction product carefully to avoid spilling or getting on the skin. Toxic or harmful reaction products should be properly disposed of in accordance with laboratory regulations.
Cleaning and maintenance
Clean the reactor, including the reactor body, cover, lining and other parts. Use warm water and detergent when cleaning, and use appropriate chemical cleaning agents if necessary. Pay attention to the compatibility of cleaning agent and reactor material.
After cleaning, dry or dry the reactor and place it in a dry and ventilated place. Avoid direct sunlight and harsh temperature environments.
Special note
Material and temperature limits:
Different reactor liner materials (such as PTFE, PPL) have different temperature limits. For example, the external heating temperature of PTFE material is recommended not to exceed 230 ° C, and the PPL material is recommended not to exceed 260 ° C. Exceeding these temperature limits may cause the liner to deform or produce toxic gases.
Selection of reaction medium:
The choice of reaction solvent should be based on the needs of the experiment, generally 1/3 to 1/5 of the lining capacity. Special attention should be paid to the safety of the use of some strong oxidants (such as perchloric acid, hydrogen peroxide) to avoid violent reactions or explosions.
Overpressure and overtemperature use:
It is strictly forbidden to use the reactor over pressure and over temperature. Overpressure may cause the reactor to crack or explode, and overtemperature may cause the inner liner to deform or produce toxic gases. Therefore, before use, it should be ensured that the maximum value of the mixed steam pressure generated by the reaction system at the reaction temperature is lower than the design pressure of the reactor.
Equipment maintenance and maintenance:
Periodically check the sealing performance of the equipment and the integrity of each component, if any damage should be replaced in time. This helps to ensure the safety of the experiment and the reliability of the equipment.
The reactor that is not used for a long time should be properly stored and maintained regularly. This helps to extend the service life of the equipment and keep its performance stable.
Operator training:
The experimental personnel using hydrothermal synthesis reactor must be trained, familiar with the structure and performance of the reactor and proficient in equipment operation procedures. This helps ensure the safety and accuracy of the experiment.
Laboratory safety management:
The laboratory should be well ventilated and equipped with necessary safety facilities (such as fire extinguishers, eye washers, etc.). At the same time, a sound safety management system and operating procedures should be developed, and safety education and training should be conducted regularly for experimental personnel.