GB2355674A - High-pressure multi-cell reactor - Google Patents

Abstract

A multi-cell reactor for parallel reactions comprises an annular array of reactor vessels mounted into a carousel having upper and lower plates. The upper plate seals to each vessel by an O-ring and is held in place, when sealed, by a rotary ring having keyhole slots which engage, on rotation, with undercut portions at the top of an annular array of retaining posts. The upper plate has a high-pressure gas connection to each cell, fed from a common manifold. Jacking posts having threaded upper ends are used, in conjunction with wing nuts, to press the upper plate initially against the vessels, before the locking plate is rotated, the wing nuts being thereafter released. The locking plate and pressure supply are mechanically interlocked to prevent wrong operation. The reactor is of a sized to fit on a conventional laboratory magnetic stirrer.

Description

2355674 Hi%!h Pressure Multi - Cell Reactor

Description Drawiniz No. A3.SO0049

Many researchers and chemists require to carry out parallel reactions on a new material or product. Frequently this involves pressurisation of a small (typlicallv 5 to 50ml of fluid) sample with a variety of gases and stirring of the liquid.

In the past this work has been carried out in high pressure reactors where a single sample has been placed in an autoclave and sealed prior to being reacted. Frequently the vessel would require the use of special tools or spanners and the use of leak detection fluids to ensure the vessel is satisfactorily sealed. Parallel reactions were carried out in other reactors or remat tests were made in the same reactor. In addition to the time factor involved with repetitive testing, this procedure introduced the difficulty of always accurately reproducing the same test conditions.

The new Multi-cell reactor overcomes these problems by incorporating a number of vessels (typically 10 but may be more), and testing samples in these simultaneously under identical temperature and pressure conditions.

The cells or vessels are set into a fixed carousel comprising an upper and lower plate. All vessels are attached to the lower plate, and all covers are attached to the upper plate. (As shown in drawing).

A single manifold is provided on top of the assembly with a distribution pipe to each cover vessel. The manifold also has a aas inlet valve, gas outlet valve, pressure gauge and a pressure relief valve, all as shown in section A - A of the drawing.

Attached to the lower plate is a series of retaining posts each with a shoulder near to the top. The upper plate has corresponding holes for the posts to pass through. On top of the upper plate is a locking ring, which has a series of keyhole slots arranged to align with the retaining posts. The shouldered part of the posts will just pass through the larger portion of the keyhole slots, and when in position the ring is rotated thereby locating the smaller part of the keyhole under the shoulder and preventing removal of the retaining post. With the locking ring in the locked position the posts secure the upper and lower plates and therefore the covers, containing the pressure inside the vessels. The locking ring is operated by means of an Operating arm as shown in section C-C of the drawing.

To prevent accidental unlocking of the unit when charged with pressure a mechanical interlock is provided between the locking valve, connected to the manifold, and an operating arm fixed to the locking ring (see section C-C of the drawing). The handle on the locking valve and the operating arm interface in such a way that:- a) With the locking valve in the 'vent' or open position, the unit can be locked or unlocked. b) With the locking valve in the 'closed' position, the unit remains in the locked or operating position. c) When the operating lever is in the open position the cells cannot be pressurised.

U the vessel / cover Joints are sealed by an '0' ring in a piston / cylinder arrangement see -,ection A-A of the drawing. This closure requires only an active (closing) force to bring the two parts together. The closing (and removing) force is sufficiently low to be applied by intep i - nuts. (See section C-C of the drawini I I ral wing g, and the operating instructions) The unit is designed for low viscosity media where aggressive stirring is not essential.

The u it is desi I I I I ru 1 gned to fit on a commercially available sing e position hot plate / stirrer with a small spin bar in each vessel.

High Pressure Multi - Cell Reactor Operating Instructions See Drawinz A3. S00050 The multi - cell reactor consists of two sub-assemblies, the top 'half consisting of principally the upper plate., locking ring, manifold, distribution tubes, covers, wing nuts and interlock valve.

The lower'half includes the lower plate, vessels, retaining posts andjacking posts.

1. To complete the assembly of the unit, the top 'half is aligned above the lower half as shown on the drawine so that the wina nuts are aliened vertically above the Jacking posts. The top 'half is then lowered carefully onto the lower 'half so that the covers fit into the respective vessels, and the retaining posts pass through the respective holes in the upper plate and locking ring. (The top 'half may be rotated horizontally through 180' before locating with the lower 'half, i.e. either wing nut can be aligned with either jacking post).

2. With the top 'half sitting loosely on the lower 'half, the wing nuts are turned clockwise (finger-tight) to engage the Jacking: posts. This action simultaneously locates the covers in the respective vessels and the '0' rings in position. (Total time up to this point is about 15 seconds).

At this stage both the locking valve and the locking ring are in the open or vent positions.

4. The operating arm is then rotated clockwise to the stop position causing the locking ring, to engage the retaininLy posts. To transfer the full load onto the retaining posts the wing nuts are turned anticlockwise to take up the slack. Finally the locking valve is rotated clockwise to the stop or locked position. The multi-cell is now ready for charging, pressurising and heating.

5. Heating / cooling may be by partial immersion in a liquid bath, or by electrical band heaters on individual vessels.

6. On completion of the reaction, the pressure is removed through the gas outlet valve and the unit cooled if necessary. The reactor can then be opened.

7. This is done by 1) turning the locking valve anti-clockv4'se to the open position ii) moving the operating arm to the open position iii) removing the wing nuts by turning them anti-clockwise iv) lifting the top 'half free of the lower 'half.

8. The samples may then be removed from the unit, and the unit cleaned, if necessary, before reloading and re-testing.

3 r High Pressure Multi - Cell Reactor

Claims (8)

Claims

1. The Baskerville High Pressure Multi - Cell Reactor incorporates a number of vessels (up to 10 or more) into a single unit with simultaneously rapid closure (approximately 15 seconds) of all the vessels without the use of spanners or tools. See operating instructions.

2. The multi - cell reactor is designed to operate at above ambient temperature and pressure. Heating can be ap lied by immersion in a water or oil bath. or p I - I alternatively by electrical band heaters on individual vessels.

The footprint is sufficiently small that 10 vessels (of 20 mm bore and 95mm deep) will sit on a single position magnetic stirrer typically of 140mm. diameter.

4. Each cell designed to take removable glass or PTFE liners.

5. Common gas supply line allows for a single gas inlet connection.

6. Alternative smaller cell sizes can be retro-fitted.

7. Options are available for cell sampling or catalyst injection at low pressure.

8. Options are available for insertion of a temp, probe into each cell.

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