Recovery column

The extract is vacuum-distilled ia the solvent recovery column, which is operated at low bottom temperatures to minimise the formation of polymer and dimer and is designed to provide acryUc acid-free overheads for recycle as the extraction solvent. A small aqueous phase in the overheads is mixed with the raffinate from the extraction step. This aqueous material is stripped before disposal both to recover extraction solvent values and minimise waste organic disposal loads. 

It is possible to dispense with the extraction step if the oxidation section is operated at high propylene concentrations and low steam levels to give a concentrated absorber effluent. In this case, the solvent recovery column operates at total organic reflux to effect a2eotropic dehydration of the concentrated aqueous acryflc acid. This results in a reduction of aqueous waste at the cost of somewhat higher energy usage. 

The bottoms from the solvent recovery (or a2eotropic dehydration column) are fed to the foremns column where acetic acid, some acryflc acid, and final traces of water are removed overhead. The overhead mixture is sent to an acetic acid purification column where a technical grade of acetic acid suitable for ester manufacture is recovered as a by-product. The bottoms from the acetic acid recovery column are recycled to the reflux to the foremns column. The bottoms from the foremns column are fed to the product column where the glacial acryflc acid of commerce is taken overhead. Bottoms from the product column are stripped to recover acryflc acid values and the high boilers are burned. The principal losses of acryflc acid in this process are to the aqueous raffinate and to the aqueous layer from the dehydration column and to dimeri2ation of acryflc acid to 3-acryloxypropionic acid. If necessary, the product column bottoms stripper may include provision for a short-contact-time cracker to crack this dimer back to acryflc acid (60). 

The oxidation reactor effluent and methanol ate sent to the esterification reactor, which operates at up to 250°C and a pressure sufficient to maintain the Hquid phase. This latter is about 2500 kPa (25 atm). The oxidation products are converted to methyl -toluate and dimethyl terephthalate without a catalyst. Excess methanol is suppHed, and steam and vaporized methanol ate removed and enter a methanol recovery column. The esterification products flow to a cmde ester column, which separates the toluate from the terephthalate. The overhead stream of methyl -toluate is returned to the oxidation reactor, and the bottoms stream of dimethyl terephthalate goes to a primary distillation. The distillate is dissolved in methanol, crystallized, and sohd dimethyl terephthalate is recovered. The dimethyl terephthalate can then be either recrystallized or distilled to yield the highly pure material needed for the polyesterification reaction. 

Eig. 4. Mobil—Badger process for ethylbenzene production H = heater Rx = reactor P = prefractionator BC = benzene recovery column ... 

VS = vent gas scrubber EC = ethylbenzene recovery column DC = diethylbenzene recovery column. 

In general, the sulfolane extraction unit consists of four basic parts extractor, extractive stripper, extract recovery column, and water—wash tower. The hydrocarbon feed is first contacted with sulfolane in the extractor, where the aromatics and some light nonaromatics dissolve in the sulfolane. The rich solvent then passes to the extractive stripper where the light nonaromatics are stripped. The bottom stream, which consists of sulfolane and aromatic components, and which at this point is essentiaHy free of nonaromatics, enters the recovery column where the aromatics are removed. The sulfolane is returned to the extractor. The non aromatic raffinate obtained initially from the extractor is contacted with water in the wash tower to remove dissolved sulfolane, which is subsequently recovered in the extract recovery column. Benzene and toluene recoveries in the process are routinely greater than 99%, and xylene recoveries exceed 95%. 

Fig. 7. Shell sulfolane extraction process. E, extraction ED, extractive distillation RC, recovery column.

As a starting point for identifying candidate solvents, all compounds having boiling points below that of any component in the mixture to be separated should be eliminated. This is necessary to yield the correct residue curve map for extractive distillation, but this process implicitly rules out other forms of homogeneous azeotropic distillation. In fact, compounds which boil as much as 50°C or more above the mixture have been recommended (68) in order to minimize the likelihood of azeotrope formation. On the other hand, the solvent should not bod so high that excessive temperatures are required in the solvent recovery column. 

Fig. 19. Separation of ethanol and water from an ethanol—water—benzene mixture. Bottoms and are water, B is ethanol, (a) Kubierschky three-column sequence where columns 1, 2, and 3 represent the preconcentration, azeotropic, and entrainer recovery columns, respectively, (b) Material balance lines from the azeotropic and the entrainer recovery columns, A and E, respectively, where represents the overall vapor composition from the azeo-column, 2 1SP Hquid in equiUbrium with overhead vapor composition from the azeo-column, Xj, distillate composition from entrainer...

Ydibierschky Three-Column Sequence. If only simple columns are used, ie, no side-streams, side-rectifiers/strippers etc, then the separation sequence can be completed by adding an entrainer recovery column, column 3 in Figure 19a, to recycle the entrainer, and a preconcentrator column (column 1) to bring the feed to the azeotropic column up to the composition of the binary azeotrope. 

The entrainer recovery column takes the distillate stream, from the azeo-column and separates it into a bottoms stream of pure water, and a ternary distillate stream for recycle to column 2. The overall material balance line for column 3 is shown in Figure 19b. This sequence was one of two original continuous processes disclosed in 1915 (106). More recendy, it has been appHed to other azeotropic separations (38,107,108). 

Extensive design and optimization studies have been carried out for this sequence (108). The principal optimization variables, ie, the design variables that have the largest impact on the economics of the process, are the redux ratio in the azeo-column the position of the tie-line for the mixture in the decanter, determined by the temperature and overall composition of the mixture in the decanter the position of the decanter composition on the decanter tie-line (see Reference 104 for a discussion of the importance of these variables) and the distillate composition from the entrainer recovery column. 

Fig. 20. Three sets of material balance lines for the Kubierschky three-column sequence where design 1 corresponds to the upper tie-line having Tmin = 8.78 design 2, to the subcooled upper tie-line having = 12.23 and design 3, to the lower tie-line having = 17.31 represents overall decanter composition , the overall feed composition to the azeo-column , the distillate composition from the entrainer recovery column and O, the...

Figure 3-3. Flow diagram of a delayed coking unit (1) coker fractionator, (2) coker heater, (3) coke drum, (4) vapor recovery column.

Figure 8-4. A flow diagram for the hydration of propylene to isopropanol (1) propylene recovery column, (2) reactor, (3) residual gas separation column, (4) aqueous - isopropanol azeotropic distillation column, (5) drying column, (6) isopropyl ether separator, (7) isopropyl ether extraction.

Figure 10-2. The Badger process for producing ethylbenzene (1) reactor, (2) fractionator (for recovery of unreacted benzene), (3) EB fractionator, (4) polyethylbenzene recovery column.

For the operating conditions, the set-points of EC and DMC compositions at the top and bottom are 0.01 and 0.2996, respectively, and the bottom temperature should not exceed 140°C to prevent the decomposition of reactants. From these plots, it can be concluded that the MPC outperforms the PI controller in terms of response speed in disturbance rejection, maintaining the variables at set points, and optimization capability. Especially, the PI controller failed to maintain the DMC composition set-point due to the slow long-term dynamics caused by the interaction between the RD column and azeotropic recovery column. 

Balance over reactor-filter-dryer sub-system gives flows to recovery column. 

Purge from the water recycle stream, to waste treatment, 10 per cent of the flow leaving the methanol recovery column. 

Recovery column diameter 1 m, vessel overall height 20 m, 35 sieve plates, vessel and plates stainless steel, operating pressure 1 bar. 

Solvent recovery column plate column, diameter 0.6 m, height 6 m, 10 stainless steel sieve plates, design pressure 2 bar, column material carbon steel. 

Recovery column condenser double-pipe, heat transfer area 1.5 m2, design pressure 2 bar, materials carbon steel. 

The mixture leaving the bottom of the reactor consists of unreacted propylene and water, IPA, and diisopropyl ether (DIPE). In subsequent steps it is cooled, depressurized, and waterwashed. The unreacted propylene and by-product DIPE are flashed off and separated in a propylene recovery column. The unreacted propylene is compressed and recycled. 

IPA in concentrations of 91% or 99% is recovered in the same manner described in the indirect hydration route. Approximately 5% DIPE forms as a by-product in this process and comes out the bottom of the propylene recovery column. 

The crude C4 mixture is charged to a 70 tray extractive distillation column T-l that employs acetonitrile as solvent. Trays are numbered from the bottom. Feed enters on tray 20, solvent enters on tray 60, and reflux is returned to the top tray. Net overhead product goes beyond the battery limits. Butadiene dissolved in acetonitrile leaves at the bottom. This stream is pumped to a 25-tray solvent recovery column T-2 which it enters on tray 20. Butadiene is recovered overhead as liquid and proceeds to the BDS reactor. Acetonitrile is the bottom product which is cooled to 100°F and returned to T-l. Both columns have the usual condensing and reboiling provisions. 

The extract is pumped from the bottom of D-l to a stripper D-2 with 35 trays. The stripped solvent is cooled with water and returned to D-l. An isoprene-acetonitrile azeotrope goes overhead, condenses, and is partly returned as top tray reflux. The net overhead proceeds to an extract wash column D-3 with 20 trays where the solvent is recovered by countercurrent washing with water. The overhead from D-3 is the finished product isoprene. The bottoms is combined with the bottoms from the raffinate wash column D-4 (20 trays) and sent to the solvent recovery column D-5 with 15 trays. 

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