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00 Institution of Chemical Engineers 2005

A fire in a fluidized bed catalyst drier

Tony Fishwick

Summary
A fluidized bed drier was in use for drying palladium on carbon catalyst. A batch of catalyst had been partially dried and left overnight. Shortly after the batch had been put back into the drier the next day, and drying restarted, a fire and minor explosion occurred inside the drier. The supervisor stopped the drier fan and operated the fire alarm. The Local Authority Fire Brigade, together with the Works Fire Team, extinguished the fire. No one was injured and the only damage was to combustibles inside the drier (filter bag and rubber seals), the drier pan and some loss of catalyst.

Background and investigation

There had been a similar incident at another of the companys sites and there was a general history of such fires involving carbon and other active catalysts at the time of the incident (mid-1970s). The investigating committee took all of this into account and ordered the suspension of catalyst production operations until repairs to the drier had been completed and their initial findings made known and acted on. Their specific conclusion was that a slow current of air had been carried by convection through the bed of carbon, as it stood overnight. This had caused some heating up to occur so that ignition took place when fluidization resumed. The initial reaction was probably catalysed by the presence of palladium metal/palladium oxide. A probable contributory factor was the presence of residual acetone in the catalyst. After the catalyst was prepared, it was washed with water but final washed catalyst still contained acetone from earlier stages of the process. The acetone probably contributed significantly to the rate of heating and final temperature in the catalyst bed, and its vapours were the likely cause of the explosion.

Whenever possible, batches of catalyst should be fully dried in one operation thus removing the risk of heating up of the carbon between separate drying periods. Where this is not possible, the following precautions should be taken: cool the drier pan down by blowing cold air through for about 30 minutes with the heating off, before removal from the oven; check that the carbon temperature is below 30oC after removal of the pan from the oven; keep the pan covered, to prevent convected air being drawn through the carbon bed, for as long as it is outside the oven; before re-introducing the pan back into the oven, check that the carbon temperature is still below 30C and that the pan is cold; after resumption of drying, keep a careful check on operations to ensure that the rate of heating up is normal. Consider the use of a continuous flow process for acetone removal. The more acetone that is removed, the less likely is the heating of carbon by slow oxidation. Make the hazards associated with activated carbon, whether catalyst impregnated or not, more widely known.

Authors note
It is worth noting some of the general hazards associated with heat transfer in fluidized beds, whatever they are being used for. In order to ensure good, uniform heat transfer between the bed itself, the fluidizing gas and the reactor vessel and mechanical parts, it is essential that the bed and gas are in homogenous contact with each other at all times. This is particularly true where a strongly exothermic reaction is being carried out, or where the use of high energy external or internal heating is necessary in order to carry out an endothermic reaction. If parts of the bed become static they can rapidly heat up to dangerous levels and the reaction can run out of control. Consequences of this can include fire, explosion, serious damage to reaction vessels, and

Recommendations
The recommendations for avoidance of recurrence of similar incidents were:

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over-pressurization, with the possibility of dangerous materials being released to the working area and beyond. The fluidized bed must be a homogenous, well-mixed mass for it to be truly safe. This incident shows what can happen when a fluidized bed reaction is suspended and the bed left static in a potentially reactive state. Localized areas of an operating fluidizing bed can pose similar hazards if they are not fully mobile.

Sophisticated systems of temperature measurement and control of the bed and the reactor vessel are necessary in order to prevent temperature excursions that might lead to incidents. When a reaction has to be suspended before it is complete, it is good practice (if practicable) to keep the bed fluidizing by the use of an inert gas, for example nitrogen, to ensure that the homogeneity of the bed is maintained.

Change of specification for adsorbent carbon

In order to reduce acetone emissions to atmosphere, solvent-laden air from a drier was passed through a carbon adsorption unit. The acetone was adsorbed on to the carbon and solvent-free air discharged to atmosphere. The acetone was removed from the carbon by counterflow steaming and sent for recovery. After having operated successfully for several years, the carbon adsorption unit caught fire during a normal adsorption cycle. The investigation revealed that the Purchasing Department, acting on their own initiative, had found a cheaper supply of carbon. This carbon had a different specification and had a higher activity than normal. In other words, it acted as a catalyst for the thermal decomposition/oxidation of the acetone. This generated sufficient heat to start the fire.

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