Micro-scale chemical process simulation methods and apparatus useful for design of full scale processes, emergency relief systems and associated equipment

A method for pressure vessel emergency relief system design, useful to determine exothermicity and pressure generation during chemical reactions or pressure conditions which exist upon extraneously applied heat, comprising the steps of:

• confining a sample of the material to be evaluated on a micro-scale in a test vessel;
• positioning the confined sample of material in said vessel in a containment zone;
• monitoring the temperature conditions existing in the material within said vessel;
• monitoring the pressure conditions existing within the vessel and the containment zone;
• introducing fluid or exhausting fluid from the containment zone in response to the monitored pressure conditions as necessary to substantially maintain isobaric pressure conditions on the material within the vessel and in the containment zone;
• providing a source of guard heat within the containment zone physically and thermally spaced from the test vessel for controlling the temperature of the environment immediately surrounding the test vessel;
• providing thermal insulation between the source of guard heat and the test vessel;
• selectively maintaining the temperature of the environment immediately surrounding the vessel at a value relative to the temperature of the material in the vessel such that heat loss from the material to the environment surrounding the vessel is substantially prevented;
• and
• maintaining a phi factor defined by the thermal mass of the sample of material plus the thermal mass of the confinement vessel divided by the thermal mass of the sample at a value not significantly greater than about 1.1.

Equipment for micro-scale piloting of full-scale chemical reactions or chemical process conditions to be carried out in pressure vessels, comprising:

• a containment unit having an interior surface;
• a pilot vessel within the containment unit and having a thin-walled container, with side and bottom walls, for receiving a predetermined pilot proportion of the material(s) to be processed on a full-scale basis and in a manner simulating the full scale reaction or chemical process conditions,
• said pilot vessel being spaced from the interior surface of the containment unit;
• means for introducing said pilot proportion of the material(s) into the pilot vessel and to effect removal thereof;
• a guard energy device within the containment unit and spaced from the pilot vessel and the interior surface of the containment unit respectively for controlling the temperature of the environment immediately surrounding the pilot vessel;
• insulating means between the guard energy device and the test vessel;
• means for monitoring the temperature conditions existing in the material(s) in the pilot vessel;
• means for monitoring the pressure conditions existing within the pilot vessel and the containment unit;
• means for introducing fluid or exhausting fluid from the containment unit;
• means for comparing the monitored pressures for controlling the introduction or exhaustion of fluid from the containment unit as necessary to maintain substantially isobaric pressure conditions in the pilot vessel and the containment unit;
• and
• means responsive to the monitored temperature conditions and operably connected to the guard energy device for selectively controlling operation thereof to maintain the temperature of the environment around the pilot vessel at a value relative to the sensed temperature of the material(s) in said pilot vessel such that significant heat loss from the material(s) to the environment immediately surrounding the pilot vessel is prevented,
• the wall thickness of the pilot vessel being such that a phi factor defined by the thermal mass of the proportion of material(s) in the vessel plus the thermal mass of the pilot vessel divided by the thermal mass of the proportion of such material(s) is not significantly greater than about 1.1.

A method of micro-scale piloting of full-scale chemical reactions or chemical process conditions to be carried out in pressure vessels, said method comprising the steps of:

• confining a predetermined pilot proportion of the material(s) to be processed on a full-scale basis in a pilot vessel;
• positioning the pilot proportion of material(s) confined in said pilot vessel in a containment zone spaced from the vessel;
• providing a controllable supply of guard thermal energy within the containment zone physically and thermally spaced from the pilot vessel for controlling the temperature of the environment immediately surrounding the pilot vessel and the pilot materials therein;
• providing insulating means between the pilot vessel and the supply of guard thermal energy;
• monitoring the temperature conditions existing in the material(s) in the pilot vessel;
• monitoring the pressure conditions existing within the pilot vessel and the containment zone;
• selectively providing a supply of pressurized fluid to the containment zone;
• effecting selective removal of fluid from the containment zone;
• comparing the monitored pressures in the pilot vessel and containment zone for controlling introduction or exhaustion of fluid from the containment zone;
• and
• selectively maintaining the temperature of the environment immediately surrounding the pilot vessel at a value relative to the sensed temperature of the material(s) in said pilot vessel to prevent significant heat loss from the material(s) to the environment immediately surrounding the pilot vessel,
• the thermal mass of the pilot vessel being such that the phi factor defined by the thermal mass of the proportion of pilot material(s) plus the thermal mass of the pilot vessel divided by the thermal mass of the proportion of the pilot material(s) is not significantly greater than about 1.1.