Autoclave for laboratory (2)

(2) Technical parameters (different for each model)

Working pressure: 0.

Jacket working pressure: 0.

Working temperature: room temperature～300℃ (adjustable)

Stirring speed: 20～1000r/min (adjustable)

Heating method: Jacketed heat conduction oil electric heating tube

In the form of a stirring blade: Promoting type, paddle type, anchor type, turbine type and the like

The technical parameters of various autoclaves produced by various manufacturers are different, so please refer to the manual

(Three) use

Install, debug, feed, run, unload, and clean according to the instructions for different types of autoclaves

(4) Safety instructions

(1) Before operation, carefully check the kettle body for abnormalities.

(2) The measuring instrument should be calibrated regularly to ensure its accurate and reliable operation

(3) The heating rate should not be too fast, generally not more than 80°C/h; pressurization should also be carried out slowly, especially the stirring speed, which only allows a slow rise

(4) Rapid cooling is not allowed to prevent damage to the kettle body caused by excessive temperature difference and pressure

(5) When the reaction kettle is running, the water jacket between the coupling and the kettle cover must pass cooling water to control the working temperature of the magnet and avoid demagnetization

(6) It is strictly forbidden to knock and twist the bolt and nut joints under high pressure

(7) The blasting membrane will age and fatigue after a period of use, reduce the blasting pressure, and may also have medium adhesion, which affects sensitivity.

(8) The needle valve is line-sealed, and good sealing performance can be achieved by turning the valve needle lightly.

(9) When using a rubber tube to suck the reaction liquid containing RaneyNi, Pd/C, Pd(OH) ₂ and other catalysts in the autoclave , be careful not to evacuate the reaction liquid to avoid combustion caused by the flammable catalyst adsorbed on the inner wall of the tube and air friction , It is necessary to repeatedly flush the inner wall of the autoclave with the corresponding solvent and absorb it in time
.
The used rubber tube should not be thrown into the trash can casually.
It should be immersed in the water along with the filter paper, diatomaceous earth and wipes, and handed over to the administrator for disposal
.
The used rubber tube can also be rinsed with appropriate solvent or water, and it can be reused after confirming it is clean
.

(10) After use, all valves of the gas cylinder must be closed, adjust the pressure gauge to 0, and keep the surrounding environment clean and tidy
.

(11) The gas in the hydrogen cylinder cannot be empty.
When the pressure reading of the total gauge is lower than 2MPa, the hydrogen cylinder should be replaced
.

(12) For the catalytic hydrogenation reaction, two fire extinguishers and a fire blanket should be equipped in advance next to the autoclave when feeding and discharging materials for emergency use
.

(13) The autoclave and the controller must be grounded to ensure the safe operation of the autoclave
.
Correct and reasonable operation can ensure the safe operation of Yuli Vessel, because even if the design of the vessel fully meets the requirements, the quality of manufacturing and installation is excellent, if the operation is improper, it will also cause pressure vessel accidents
.

(14) To ensure the safe operation of the autoclave, the following aspects must be achieved:

① Smooth operation
.

During the operation of the pressure vessel, frequent changes and large fluctuations in pressure have a great effect on the fatigue resistance of the vessel
.
The operating pressure should be kept as stable as possible
.
At the same time, the container should also avoid sudden changes in shell temperature during operation to avoid excessive temperature stress
.
When the pressure vessel is loaded (increasing pressure, heating) and unloading (decreasing pressure, cooling), the speed should not be too fast, and it is necessary to prevent the pressure or temperature from changing rapidly in a short period of time to adversely affect the vessel
.

② Prevent overloading
.

To prevent overloading of pressure vessels, the main thing is to prevent overpressure
.
The reaction vessel should strictly control the feed volume and reaction temperature to prevent the reaction from running out of control and causing the vessel to overpressure
.
When the storage container is filled and fed, it is necessary to strictly measure, to prevent overfilling, and to prevent the material from being heated and expanding and causing the container to overpressure
.

③Status monitoring
.

Pressure vessel operators should constantly supervise the working conditions of the vessels during the operation period of the vessels, promptly discover abnormal conditions in the operation of the vessels, and take corresponding instructions to ensure safe operation
.
The supervision and control of the operating state of the container are mainly carried out from the aspects of process conditions, equipment conditions, and safety devices
.

a.
Process conditions
.
Mainly the operating pressure, temperature, liquid level in the range of the operating specifications; chemical composition within the vessel to meet the requirements of the working medium and the like
.

b.
Equipment condition
.
Mainly check whether the container body and the directly connected parts such as valves, flanges, pressure, temperature and liquid level meter nozzles are deformed, cracked, leaked, corroded and other defects or suspicious phenomena; whether the container and its connecting pipes and other equipment are present vibration, wear and tear; insulation equipment (cold) is intact and so on
.

c.
Safety device
.
Mainly check the integrity of all safety accessories and measuring instruments, such as whether the instruments are inaccurate, blocked, whether interlocking, alarms are reliably put into use, whether they are within the allowable use period, and whether the outdoor equipment is frozen in winter
.

(5) Emergency shutdown

When one of the following abnormal phenomena occurs in the pressure vessel, the operator should take emergency measures immediately and report to the administrator and the competent department in accordance with the prescribed procedures
.
These phenomena mainly include: ①The working pressure and the medium change drastically, and the medium temperature or wall temperature exceeds the allowable value, which cannot be effectively controlled after measures are taken; ②The main pressure components have cracks, bulges, deformation, leakage and other defects that endanger safety; ③ safety accessories fail to take over, fasteners damaged, it is difficult to ensure safe operation; ④ fire a direct threat to the safe operation of pressure vessels; ⑤ pressure vessels and piping severe shock, endangering the safe operation and so on
.

Related link: Autoclave for laboratory (1)