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Molecular Sieves:

Molecular Sieve Process Summary

This process uses two molecular sieves for the dehydration of the distilled (~95% v/v)
product. The sieves are cycled from the active dehydration bed to regenerated dehydration bed
when the active bed is spent to provide continuous product flow. While one sieve is in process
the other is regenerated and the sieves switch when the sieve in process has reached its capacity.
Degassed ethanol/water mix from the distiller product stream is superheated to a vapor and
transferred to one of two adiabatic molecular sieve (MS) bedded with 3 sphere Zeolite beds for
a few minutes in an exothermic adsorption process involving the water and Zeolite beads in the
feed. Part of the anhydrous ethanol from the fresh active adsorption bed is redirected and is used
to regenerate the other loaded (water-filled) bed. A vacuum is applied to induce condensation of
the water ethanol mix from the loaded bed and recycled back to the distillation process. The
exiting anhydrous ethanol (~99.98%) is condensed and transferred to the next point of
processing. The processs major energy requirement is the power consumption needed for the
vacuum pump and plant steam to superheat the feed.
Molecular Sieve Process Assumptions:

Process is considered isothermal due to the fast regeneration time.

Ethanol water vapor is an ideal gas
Only water is adsorbed
Axial pressure drop is neglected
Axial dispersed plug flow model is valid
Mass transfer rates are linear and in one direction
Radial gradients in the bed are negligible
Valve flow is isentropic

Important considerations in the design of molecular sieves are:

Sieve sizing

Type and specification of dehydration medium

Bed breakthrough time
Cycle time.

All of these aspects are interrelated and require and orchestrated approach to manage a
successful design. Sieve sizing is based on required maximum velocity medium specifications
and operational and hazard safety parameters. Bed breakthrough time which are governed by
bed isotherms and pressures determine the cycle times which drive the process. These
calculations and specifications are provided.
Half cycle Product Flow Process and Unit Operation Description
At present state B-MS-1 (sieve bed) is regenerated and B-MS-2 is spent and requires
regeneration (Please reference Fig. 7) The 37345 kg/hr ~ 95% ethanol/water stream from the
distillation section is preheated with product stream using heat exchanger (HE-MS-1) and
superheated and pressurized (440 K, 380 kPa) by heat exchanger (HE-MS-2) before enters the
top of the molecular sieve apparatus. The feed is vaporized to prevent liquid from damaging the
bedding. Two heat exchangers are used due the desire to integrate the enthalpy of the product
stream and the lack of heat duty of the product stream to product a super heated vapor. The
superheated feed (393K 440 kPa) is directed to B-MS-1 at a controlled rate by valve 1 (valve 5 is
open). All valves are closed unless referred to otherwise and at the end of each process event.
The vessel is pressurized and water is adsorped by the Zeolite bed producing ~99.98% ethanol.
The product stream rate is increased to ~ 54,000kg/hr using pump FP-MS-1 for the duration of
the regeneration cycle and is split (60/40) using timed valve switching and 60% of the anhydrous
ethanol is sent to storage which is condensed and depressurized by product heat exchanger (HEMS-3) and delivered as a liquid to designated atmospheric storage tanks. The exothermic

adsorption process generates an enthalpy. The sensible heat generated is utilized during the
subsequent regeneration of B-MS-1.
Simultaneously, B-MS- 2- valve 4 is opened at a controlled rate and the vacuum pump
(VP-MS-1) is engaged and produces a vacuum in the bed (~-202 Kpa) (Courtemanche)
Exhausted heated water (PE-MS-1) from valve 4 is directed to distillation to be recycled to the
rectifier recycle feed. Valve 6 is metered open to allow a small portion of anhydrous ethanol from
B-MS-1 to flow (counter current) and purge B-MS-2 of any remaining water. B-MS-2 pressure
is reduced to ~101 kPa and a temperature of ~308K. Bed 2 (B-MS-2) is in standby mode.
Before the breakthrough time ~24 min. is reached in the active product bed (B-MS-1), B-MS-2
valve 2 is opened in a controlled manner and B-MS-2 is pressurized (250 Kpa, 383K) by the
superheated distillation product stream. The breakthrough time is used to calculate the beds cycle
time. Because regeneration time of the loaded (spent) bed is two to three times less than the time
the active product bed is producing the required specification of anhydrous ethanol drives the
cycle. The regeneration time is ~7 minutes. The estimated cycle times will be optimized during
plant startup.
Heat Integration
Heat flow from the Heat exchanger HE-MS-3 product stream (HI-MS-3) that will heat HE-MS-1
which is used heat the product feed from the distiller (F-MS-1).

Table 2: Molecular Sieve Unit

Operation Data

Enthalpy and Tank Sizing Calculations

The following parameters were gathered and compared with other reasonable sources.
Calculations and parameters are based on the removal rate of 2090kg/h.of water from the feed
stream and the following assumptions.

The feed is a homogenous binary component system

Model sieve as a plug flow system
The fraction of ethanol adsorbed is insignificant
The active molecular sieve is
Process is adiabatic
Total mole change is negligible No accumulation within the system
Negligible axial dispersion

To ensure turbulent flow and maximum mass transfer characteristics the smallest diameter
possible will be used with the maximum velocity. Based on industrial standards, preliminary
flow calculations and cost control considerations a 20 minute cycle time with a 7 miniute
regeneration was established.
The minimum design dimensions (one equilibrium zone) of each molecular sieve calculated
(0.125 inch/3.17mm dia. Zeolite spheres)

Length (I.D.) 3.5m

Width (I.D.) 2.5m

This produced a break through time of ~19 min. Length of the equilibrium zone was
increased and the break through time recalculated to meet the desired operation cycle time of 20
min. and provide a tolerance to accommodate varying conditions.

Length (I.D.) 5.0m

Width (I.D.) 2.5m

The recalculated length of the Zeolite bed increased the break trough time to a more workable
time of 25.7 minutes.

As per this companys standard practices to ensure quality of product and safety the volume
of bedding will be doubled and an additional 10% added to the calculated length for support
bedding material. The final I.D. dimensions are as follows:

Length (I.D.) 11.0m

Width (I.D.) 2.5m