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Azeotropic distillation
Add substance that forms minimum boiling
azeotrope with one or both components.
Take azeotrope off top and separate bydecanting or by solvent extraction
May get binary or ternary azeotrope, either
homogeneous or heterogeneous
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Extractive distillation
Add non-volatile substance/entrainer that
modifies relative volatility of the other
components.
May reverse volatilities
However, leads to higher T in reboiler Must separate entrainer by decanting,
distillation or solvent extraction
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Extractive distillation - examples
Max boiling Azeotropes
Nitric acid/water or hydrochloric acid/water
extract water using sulphuric acid
Close Boilers
Toluene/methylcyclohexane add phenol to
dissolve toluene. Gives mch overhead distill
phenol/toluene
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Extractive distillation - examples
Reverse volatilities
Paraffins/aromatics add glycol to dissolve
aromatics recover glycol with water wash
Propene/propane in presence of nitrogen use
acrylonitrile to reverse the volatilities of propane
and propene. Propene dissolves in acrylonitrile
separate by flash followed by distillation
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Molecular DistillationFor those classes of chemical compounds
which decompose, polymerize, react or
are destroyed by conventional lowpressure distillation, efficient commercial
high vacuum distillation equipment is
available for those compounds
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By centrifugal force, the materialspreads in a film across the
heated disc which intimately faces
a large condensing surface.
The lighter compound evaporates
and condenses in a fraction of a
second. The heavier residue
which has not evaporatedslides off the outer edge of the disc
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NO HEAT DEGRADATION:Low pressure and a thermal residence timeof less than one second protects against decomposition.
HIGHER PRODUCT QUALITY:This process can remove objectionable
colors, odors, and excess reactants, adding value to product.
VALUABLE BY-PRODUCTS:Materials removed from product remainintact. These waste materials become potential marketable products.
LOW PROCESS COST: can be processed small or large volumes at lowcosts because stills use less energy, are very efficient and economical inoperation.
PROCESS SMALL OR LARGE VOLUMES: throughput ranging from
ounces to 2,000 pounds per hour
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Food Processing IndustriesProvide a method for refining edible oils that result in decolorized,deodorized, pure oil, separating valuable products such as vitamins,
sterols, fatty acids, and antioxidants. The centrifugal moleculardistillation process provides a gentle method for purifying and fractioningessential oils. Odors, colors, and flavors can be separated withoutdanger of hydrolysis, air oxidation or decomposition. Monoglycerides oremulsifiers can be more highly concentrated than with traditionalseparation techniques.
Cosmetic IndustriesThis type of distillation equipment is ideal for use in recovering lanolinfrom wool grease, the crude soft wax obtained from the hair of thesheep. Fragrance derived from fatty acids are also isolated through thissystem.
Pharmaceutical IndustriesGovernment requirements concerning enrichment of food with vitamins
have caused increased interest in centrifugal molecular distillation ofnatural vitamins A and E. Natural vitamins K-1 and K-2 are beingdistilled to replace synthetic K-3 and -4. Synthetic vitamin E also hasbeen distilled by Myers molecular distillation equipment. Stills are usedin a variety of purification and separation processes for many drugs,including tranquilizers.
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Paint and Varnish IndustryThe drying properties and firm hardness of polymerized oils such ascastor and linseed can be altered by distilling off low molecularweight compounds.
Epoxy Resin ManufacturesManufacturers of liquid epoxy resins have discovered that this
distillation technique results in desirable color reduction, loweredviscosity, and increased shelf life by removing the catalyst typicallyused in the formulation.
Tall Oil ProductionTall oil producers have benefited from Myers centrifugal moleculardistillation in two ways. First, the distillation reduces the problem of
tall oil pitch disposal. Secondly, the remaining fatty acids can berecovered in profitable quantities to be reused for emulsifiers,flotation agents, plasticizers, disinfectants, soaps, and cleaningagents.
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Silicon Producers
Myers molecular stills are ideal for the removal of either low orhigh molecular weight polymers from a mixture of polymers.
Wax ProducersCrude paraffin, beeswax carnauba, and certain microcrystallineand high melting point waxes are purified by the Myerscentrifugal molecular distillation system.
Basic ResearchMolecular distillation has been proven successful in separatingvarious isotopes, as well as many other research application.The Myers still is an effective tool for separating components ofhigh molecular weight and for concentrating components forquantitative or qualitative analysis. Surfactant ProducersSugar esters and poly-oxyalkylins glycol have been routinelypurified by Myers molecular distillation. Crude fatty acids andwax derivatives of fatty acids have been distilled in maximumpurity concentrations without thermal damage.
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Plastic IndustryThis method benefits plastics manufacturers. Plasticizers such asdi-octyl phthalate and di-octyl sebacate are purified with the Myersstills to remove excess reactants of estererification, moisture ofcondensation, objectionable color, odor, and traces of catalyst.
Mineral Oil Production
High temperature lubricating oils and greases are commonlydistilled from the C/35 - C/100 fractions of petroleum bottoms. Lubeoils purified by Myers molecular distillation are more stable andprotected from decomposition. Resins and bitumin are separated bythe method as well.
Oil Reclamation
With the rising cost of oils and fluids, recovery of these materials bythe Myers molecular distillation process is highly practical,profitable, and environmentally compatible by reducing disposablewaste.
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INTRODUCTION
Reactive distillation is a process where thechemical reactoris also the still.
Separation of the product from the reactionmixture does not need a separate distillationstep, which saves energy (for heating) andmaterials.
This technique is especially useful forequilibrium-limited reactions such asesterification and esterhydrolysis reactions.
http://en.wikipedia.org/wiki/Reactorhttp://en.wikipedia.org/wiki/Stillhttp://en.wikipedia.org/wiki/Distillationhttp://en.wikipedia.org/wiki/Esterificationhttp://en.wikipedia.org/wiki/Hydrolysishttp://en.wikipedia.org/wiki/Hydrolysishttp://en.wikipedia.org/wiki/Esterificationhttp://en.wikipedia.org/wiki/Distillationhttp://en.wikipedia.org/wiki/Stillhttp://en.wikipedia.org/wiki/Reactor7/31/2019 Azeo Extra Mole Reac Distillation
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Reactive distillation can be used with a
wide variety of chemistries, including the
following:Acetylation
Aldol condensation
Alkylation
Amination
Dehydration
Esterification
Etherification
Hydrolysis
Isomerization
Oligomerization
http://en.wikipedia.org/wiki/Acetylationhttp://en.wikipedia.org/wiki/Aldol_condensationhttp://en.wikipedia.org/wiki/Alkylationhttp://en.wikipedia.org/wiki/Aminationhttp://en.wikipedia.org/wiki/Dehydrationhttp://en.wikipedia.org/wiki/Esterificationhttp://en.wikipedia.org/wiki/Etherhttp://en.wikipedia.org/wiki/Hydrolysishttp://en.wikipedia.org/wiki/Isomerhttp://en.wikipedia.org/wiki/Oligomerizationhttp://en.wikipedia.org/wiki/Oligomerizationhttp://en.wikipedia.org/wiki/Isomerhttp://en.wikipedia.org/wiki/Hydrolysishttp://en.wikipedia.org/wiki/Etherhttp://en.wikipedia.org/wiki/Esterificationhttp://en.wikipedia.org/wiki/Dehydrationhttp://en.wikipedia.org/wiki/Aminationhttp://en.wikipedia.org/wiki/Alkylationhttp://en.wikipedia.org/wiki/Aldol_condensationhttp://en.wikipedia.org/wiki/Acetylation7/31/2019 Azeo Extra Mole Reac Distillation
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PROBLEM STATEMENT
To study a proposed method of production of
methyl acetate. The acetic acid is to be reacted
with methanol in a catalyst filled semi batch
reactor.
To simulate the reaction and see if reactive
distillation is a better option than without.
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HAc
MeOH
MeAc
H2O
STRIPPING
COLUMN
CONDENSER
REBOILER
DISTILLATION
COLUMN
EXTRACTIVE
REACTIVE
RECYCLE
SIMPLIFIED FLOWDIAGRAM OF PRODUCTION OF METHYL ACETATE
MeOH
HAc
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CHAc
CMeAc
CMeOH
CH2O
T I M E
M
O
L
E
S
Y
X
300
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n-butyl acetate
C4H9OH + CH3COOH CH3COOC4H9 + H2O
Market price (India): Rs.54/kg
Global demand: 600,000 tpa (growth: 2-3%pa)
Indian producers: Laxmi Organics, VAM
Organics, RK Chemicals, Sterling Solvents etc.
International producers: BASF, Celanese, DOW,
Eastman Chemicals etc.
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Literature survey and process
selection Conventional process
homogeneously catalyzed (H2SO4)
problems of corrosion effluent treatment (tin octoate)
vapor phase
Heterogeneous catalysis Catalyst selection
ion-exchange resin
zeolites HPAs
Reactive distillation
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Reaction & Distillation ProcessBA
AA
Reactor
Condensor
Reboiler
Waste
Stream
Product
Stream
Dis
tillation
Co
lumn
Mixer / Heater
Reflux
Drum
Product Cooler
Recycle
Stream
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Reactive Distillation Column
ProcessCondensor
Reboiler
Effluent
Stream
Product
Stream
RD
Column
Decanter
Product Cooler
HAc
BuOH
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ADVANTAGES:
Increased speed and improved efficiency.
Lower costs reduced equipment use, energy
use and handling.
Less waste and fewer byproducts.
Improved product quality reducing opportunity
for degradation because of less heat exposure.
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DIFFICULTIES:
The performance of the reactive column is not
optimal when equated to a chemical reactoranda distillation column seperately.
It is not feasible to use a reactive distillationcolumn when the optimum process parameters(temp,pressure etc) differ too much.
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Thank you!
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