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Contents lists available at ScienceDirect

Catalysis Today
journal homepage: www.elsevier.com/locate/cattod

Ethylene production via Oxidative Dehydrogenation of Ethane using

M1 catalyst
Anne M. Gaffney a,∗ , Olivia M. Mason a,b
a
Idaho National Laboratory, P.O. Box 1625m MS 2203, Idaho Falls, ID 83415, United States
b
Department of Chemical Engineering, Manhattan College, 4513 Manhattan College Parkway, Riverdale, NY 10471, United States

a r t i c l e i n f o a b s t r a c t

Article history: Ethylene is the top petrochemical produced worldwide with continuously growing production capacity.
Received 26 September 2016 Steam Pyrolysis of straight run hydrocarbons is the conventional technology for producing ethylene for
Received in revised form 10 January 2017 more than 50 years. Currently the feedstock of choice domestically is ethane or liquefied petroleum gas
Accepted 14 January 2017
(LPG). Oxidative Dehydrogenation of Ethane (C2-ODH) is an alternative catalytic technology for produc-
Available online xxx
ing ethylene using a natural gas feedstock. North American olefin plants have switched from a heavy
petroleum feedstock to a light ethane feedstock due to the shale revolution. The M1 catalyst, advanced
Keywords:
by co-author, Dr. Anne M. Gaffney, selectively and exothermically transforms ethane to ethylene under
Oxidative dehydrogenation
Mixed metal oxide
mild conditions (300–400 ◦ C, 4–7 atm). A comparison of the two technologies shows the energy and cost
Ethane savings of C2-ODH along with the promising future for oxidative dehydrogenation technology.
Ethylene Published by Elsevier B.V.
Natural gas
Conventional steam pyrolysis

1. Introduction
Oxidative dehydrogenation (ODH) catalysts for converting
ethane to ethylene began receiving attention in the late 1970s after
Journal of Catalysis published an article titled, “The Oxidative Dehy-
drogenation of Ethane over Catalyst Containing Mixed Oxide of
Molybdenum and Vanadium” followed by a prodigious amount of
advances in the 1980s; in part due to substantial research being
conducted on remote natural gas [1,2]. The selectivity and conver-
sion to ethylene are the two parameters commonly used to measure
the catalyst productivity. Fig. 1 displays a variety of catalysts for the
Oxidative Dehydrogenation of Ethane (C2-ODH) including the M1
catalyst. The original M1 catalyst was refined at ABB Lummus in the
early 2000s and achieved high selectivity at high conversion [3].
The discovery of an abundance of North American shale gas over
the past decade has resulted in an enormous growth in US tight oil
and shale gas production. A steep decrease in the US dependence
on foreign energy resources coupled with new opportunities for US
manufacturing is causing growth across the petrochemical indus-
Abbreviations: C2-ODH, Oxidative Dehydrogenation of Ethane; ODH, oxida-
tive dehydrogenation; CSP, conventional steam pyrolysis; FTM, facilitated transport
membrane; TEA, Techno-Economic Analysis; LCA, Life Cycle Analysis.
∗ Corresponding author.
E-mail addresses: anne.gaffney@inl.gov (A.M. Gaffney), olivia.mason@inl.gov
(O.M. Mason).
try [4]. Ethylene, the lightest olefin, is an organic intermediate used
for manufacturing many downstream chemicals such as polyethy-
lene, ethylbenzene, 1,2-dichloro-ethane, ethylene oxide, ethanol,
polyvinyl acetate and many more important chemicals. Polyethy-
lene, the most common plastic used worldwide, is the most notable
end product of ethylene accounting for nearly 60% of the capacity. In
the US, 90% of the manufactured ethylene is produced from natural
gas and accounts for 20% of the worlds capacity. Worldwide, con-
ventional steam pyrolysis (CSP) is the current means for producing
ethylene. CSP is a non-catalytic, high temperature, and low pres-
sure process that thermally cracks a feedstock of ethane, propane,
or liquid fuels. The choice of feedstock depends greatly on geo-
graphic location, cost, and availability of hydrocarbons. The process
is extremely energy and capital intensive, yielding many byprod-
ucts, requiring extensive separations and purification [5].The US
has transitioned mostly to a gas feedstock for crackers due to the
abundant supply of low cost ethane. In the US, ten additional ethane
cracker expansion projects are driving the steep increase in ethy-
lene capacity. Global ethylene capacity is 160 MTPA and is projected
to reach 179 MTPA by 2018 [5].
Aspen HYSYS is used to simulate and compare the respective CSP
and C2-ODH plant design. Preliminary Techno-Economic Analyses
(TEA) shows the superiority of C2-ODH over conventional meth-
ods for producing ethylene. Required netback (RNB) is an economic
approach commonly used for assessing the attractiveness of new vs
current technology (top cat paper ref). RNB is based on calculation

http://dx.doi.org/10.1016/j.cattod.2017.01.020
0920-5861/Published by Elsevier B.V.

Please cite this article in press as: A.M. Gaffney, O.M. Mason, Ethylene production via Oxidative Dehydrogenation of Ethane using M1
catalyst, Catal. Today (2017), http://dx.doi.org/10.1016/j.cattod.2017.01.020
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Fig. 1. High selectivity and conversion catalyst for ethylene production.

Table 1
Tubular Bundle Feed Compositions.

Component Module-1 Module-2 Module-3 Module-4

Molar Feed Molar Feed Molar Feed Molar Feed
Composition Composition Composition Composition

Ethane 0.875 0.661 0.465 0.109

Oxygen 0.125 0.118 0.187 0.049
Ethylene 0.000 0.214 0.410 0.766
Water 0.000 0.214 0.410 0.766

of the Cost of Production (COP). COP is based on variable costs, fixed Activation energy 70,000 kJ/kmol
costs, cash costs, capital investment, capital recovery. The current
spot or contract prices are greater than the COP of new technolo- Selectivity 90% (original analysis)
gies then the new technology shows potential. If the COP of a new
technology is less than the cash costs of a current technology, then
shutdown economics are achieved [6]. 95% (current expected selectivity)

By-products up to 5% CO2; trace quantities of acetylene and

1.1. Options for the reactor and reaction specifics
From an engineering standpoint there are basically 3 options in
the design of a reactor to achieve the high yields and manage the
heat of reaction. The use of an adiabatic fixed bed reactor with a
cold feed was removed as an option due to the potential for safety
issues associated with the passive control of the exotherms. Con-
sequently, the main options studied with ASPEN-HYSYS to date are
listed below. The stoichiometry and activation energy input into the
model was determined from the patent literature. Temperature and
pressure were input into the model based on the laboratory data
reported in the patent examples. Assuming a pseudo-first order
reaction, the conditions used for the analysis are listed below.
Inlet temperature: 325C
Inlet pressure: 4 atm
Pre-exponential
parameter(A) 1e9
acetic acid used in the modeling
Sensitivity analyses using these numbers are easily accommo-
dated in the modeling work and are used to assess the viability of
the various case studies. The various options for reactor designs are
as follows:
a Packed tubular reactors in series
1. Tubes with internal diameters of 1–1.5 in. and 5–7 m in length
are packed with the M1 catalyst. The target is to achieve about
25% conversion of ethane within each reactor. Due to the fric-
tional pressure drop in each reactor, the partial pressure of
ethane will be decreased in subsequent reactors. Consequently,
the temperature will need to be higher to maintain the 25%
conversion target. Additionally, latter reactors may require a
more complex heat recovery system since the boiler feed water
coolant (BFW) may exceed the critical temperature and pressure.
A super critical water coolant system (SCWC) similar to that used

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Scheme 1. Block Flow of C2-ODH Process.
in nuclear reactor/power generators is being considered for that
function.
2. Feeds with ethane/ethylene and limiting pure oxygen feed deliv-
ered via inter-reactor injection
3. Ethane and ethylene serving as diluents. Ethylene is reported
to not undergo secondary reactions. By-products will track with
unreacted ethane to the next reactor in series.
4. The number of tubes is similar to that required in the conven-
tional ethylene oxide reactions, and be as many as 20,000 tubes.
This reactor system has been in-place and studied for decades.
b Short packed beds with intercoolers
1. Similar to the packed tubes, in this option oxygen is limiting and
is extinguished by the end of each stage. In this case the effluent
of each reactor stage is removed and cooled externally. Once the
heat of reaction is recovered the reactor stream is returned to
the reactor and enters the next reactor stage. This is continued
until the desired conversion is achieved. Again due to frictional
pressure drop, the partial pressures decrease towards the end
of the reactor and in order to maintain reactivity, temperatures
need to be increased and the SCWC system may be required.
c Cold shot reactors
1. This option is similar to the reactor design used for the con-
version of synthesis gas to methanol. Heat management is
accomplished by the injection of a cold stream containing addi-
tional oxygen at several positions during the axial run of the
reactor. A sparger may need to be imbedded in the catalyst bed
to distribute the reactants and avoid channeling. The heat trans-
fer mechanism is direct quench rather than indirect quench and
therefore the level (temperature) at which the energy will be
recovered will be lower and the overall plant will become less
efficient and may not reach the envisioned E-0 conditions.
Multiple trains are not included in the analysis because it is
expected that each reactor could provide several hundred millions
of pounds per year of product. Additionally, it should be scalable by
adjustment of the number of tubes. There are no other unit oper-
ations or equipment in the process that will be limiting. It will
probably be prudent to have several parallel reactors either as a
parallel unit to adjust the capacity as needed or perhaps as a spare.
2. Overview of C2-ODH
2.1. Chemistry
A gas stream of ethane and oxygen are reacted over the opti-
mized M1 catalyst and form ethylene, water, and traces of carbon
oxides at temperatures less than 400C and 1–2 atm3 . The catalysts
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3
disclosed in U.S. Pat. No. 4,250,346 include oxides of molybdenum:
Moa Xb Yc , where X = Chromium, Manganese, Niobium, Tantalum,
Titanium, Vanadium and/or Tungsten, Y = Bismuth, Cerium, Cobalt,
Copper, Iron, Potassium, Magnesium, Nickel, Lead, Antimony, Sili-
con, Tin, Thallium, and/or Uranium [7]. Catalyst preparation is key
to achieving high selectivity at high conversion to ethylene. Cat-
alyst preparation is described in World Patent No. 2010115108
The refined M1 catalyst has been demonstrated at a Technology
Readiness Level of 3 for over 1000 h of operation.
2.2. Process
Scheme 1 shows a block flow of the C2-ODH process. The pro-
cess has the potential to only contain 3-major sections as shown in
Scheme 1 – a heating & cooling network, a reactor, and a membrane.
Ethane is preheated to approximately 200C and fed with limited
oxygen to the ODH reactor. Pure oxygen is used rather than air to
avoid downstream removal of nitrogen. Ethane and ethylene are
used as diluents due to lack of secondary reactions with ethylene.
Inter-bed oxygen injections ensure operation occurs safely. Based
on the current Aspen HYSYS modeling of laboratory data, a tubu-
lar reactor design, similar to an Ethylene Oxide reactor, offers the
most potential for managing the heat generated by the exother-
mic gas phase reaction. The reactor effluent containing ethylene,
unreacted ethane, water, and carbon oxides are cooled and water
is recovered. This charge gas is sent to conventional separations
units. Novel membranes being developed by Compact Membrane
System have the ability to separate alkenes from alkanes and are
being considered for application [8]. If needed, carbon dioxide can
be scrubbed, or adsorbed from the reactor effluent. C2-ODH could
potentially be an add-on reactor unit to conventional ethylene plant
and existing distillation/fractionation columns could be used for
purification. The limited amount of byproducts and almost stoi-
chiometric chemistry of C2-ODH creates a grade of ethylene with
high enough purity that can be used downstream for processing for
example ethylbenzene.
2.3. Reactor design considerations
In order to manage the heat and provide conversion of ethane,
a tubular reactor in series, with a shell-side coolant is used. One to
four tubular reactors in series, with complete consumption of oxy-
gen per reactor, can be run isothermally using a shell-side coolant
to control the exotherm in the reactor. At the exit of each reac-
tor, oxygen is injected and ran to extinction in each set of bundles,
while also ensuring each module is operating safely outside of the
explosion limits. Oxygen consumption across the first bed is shown
in Fig. 2.
The first set of bundles is 4-m long with one thousand 1.25-in
tubes; the reactor length increases for each subsequent reactor to
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Scheme 2. CSP vs ODH unit operations.

maintain conversion. The conversion achieved per bed is 25%. The
feed compositions for each bundle is listed in Table 1.
The reactants are modelled using first order kinetics with the
assumption that ethylene does not undergo secondary reactions.
This assumption is based on initial data for the M1 catalyst. The
M1 catalyst allows for a mixed C2 feed due to the refractory nature
of ethylene. A tubular design allows for high temperature energy
recovery from the heat of reaction; avoiding large exotherms and
inter reactor cooling. The residence time in each of the tube bundles
is approximately 5 s. The inlet pressure is approximately 900 kPa
with a tubeside pressure drop of 70–100 kPa. As more ethane is
consumed, the rate of reaction decreases as the pressure drops in
each series of packed tubes. In order to maintain the rate of reaction,
the temperature of the shell-side coolant is increased as shown in

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Scheme 3. Map of CPI coupling ODH with Conventional Technologies.

2.4. Heat management options

An advantage of a shell-and-tube design is the energy level is

maintained in the system by using a coolant and therefore expen-
sive intercooling is not needed. BFW-steam systems are typical
coolants but are not viable due to the critical temperature of water,
374C. If one set of bundles is used with a large recycle, steam could
be created on the shell-side and recovered. If two sets of bundles
are used, a heat transfer oil such as, Dowtherm A, could be used
but has a maximum cooling temperature of 400 ◦ C. After two-three
bundles, the coolant temperature is expected to exceed 400 ◦ C,
requiring a coolant able to run above that temperature. Above
400 ◦ C, supercritical steam, used for cooling in nuclear reactors, is
an option. The design follows similar to SCWC where circulating
Fig. 2. Oxygen Consumption Module 1. water pumps pressurize water above its critical pressure, which are
fed to the shell side of the reactor, heated, and serves as a coolant.
A turbine may then be used in a modified Rankine Cycle to convert
Table 2 captured heat. Other options include, thermoelectric coolers, heat
Shell-side coolant temperatures for each module.
pumps, and molten salt but all are expensive. Additionally, molten
Tubular Module Shell-Side Tube-Side salt is difficult to manage as it requires expertise to avoid freeze-ups
Coolant Temperature Inlet Temperature Exit Temperature
and line ruptures.
If a packed bed reactor design is used, cold shots or intercooling
1 345 174 357
could be used to control the exothermic reaction. Heat can be recov-
2 345 347 384
3 390 367 390 ered and integrated but energy levels are lost. The exotherms and
4 470 404 471 temperatures needed to maintain the reaction are too high for C2-
ODH therefore requiring a large recycle. A tubular reactor with shell
side cooling maintains the energy level by running isothermally and
controlling the shell side coolant.
Table 2 for each reactor, along with the packed tubes inlet and outlet
temperatures.
The first bed has a coolant temperature of 345C to initiate the 3. Process intensification of C2-ODH
reaction by raising the temperature in the packed tubes. The tem-
perature needed to maintain the reaction rate in the fourth bed The processing for C2-ODH is minimal compared to that of CSP.
gets too high and therefore separations and a recycle stream can Across the CPI, the separation and purification of products account
be used after the second or third module. If less modules are used for a majority of the energy consumed by chemical and manu-
and a recycle stream is added, the temperature of the coolant can facturing plants. Approximately half of the US industrial energy
be kept relatively low and less expensive coolants may be used. usage is due to chemical separations [9]. The high selectivity and

Table 3
Energy Metrics CSP vs ODH.

Metric CSP ODH Units

Compression Energy 60 10 BHP/million PPY

Furnace Energy 30 0 MJ/kg ethylene product
Endothermic Exothermic
Overall Energy Efficiency 2700 1300 kJ/kg

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conversion of the ODH reaction limits the byproducts created Table 4

Economics of CSP vs C2-ODH.
which reduces the number of separation unit operations needed.
Scheme 2 shows the unit operations of conventional plants and of Economics CSP ODH Units
a C2-ODH plant. Gas crackers reduce the number of unit operations Capacity 1 1 MTPA
by 30% compared to liquid crackers. C2-ODH reduces the amount Plant Capital Cost 1530 695 $$ MM USD
of unit operations by 80% compared liquid crackers. Capital Recovery 0.38 0.17 $ USD/kg C2 H4
C2-ODH plant aligns well with conventional technologies, Fixed Cost 0.14 0.07 $ USD/kg C2 H4
Variable Cost 0.23 0.17 $ USD/kg C2 H4
allowing for easy adoption and application. If a C2-ODH reac-
Cost of Production 765 421 $ USD/T C2 H4
tor is built as an add-on unit for conventional plants, traditional Economic Margin 435 779 $ USD/T C2 H4
separations units, such as distillation, may be used while further
separations are developed.
A comparison of CSP and C2-ODH energy efficiency and pro-
ductivity are displayed in Table 3. A significant increase in energy Aspen HYSYS. This required netback is a cost of production and is
efficiency is in part due to the elimination of unit operations, reduc- used to compare the price of ethylene versus the current spot price
tion in separations needed, and moderate operating temperatures. or contract price.
The overall energy efficiency of ODH indicates a 50% improvement Cost of production is based on variable, fixed, and cash costs.
over CSP. As C2-ODH is an exothermic reaction, the furnace energy Variable costs are the raw material and utilities costs; they depend
for the endothermic conventional process is eliminated. The com- on the amount of ethylene produced. Fixed costs are costs sus-
pression energy needed for CSP is reduced by 83% for C2-ODH due tained regardless the amount of ethylene produced. The fixed costs
to better yields and component state. include labor, supervision, foremen, maintenance materials, insur-
Rather than traditional distillation, the ethane-ethylene separa- ance, direct overhead, and plant overhead. Cash costs are the sum
tion is could be done via a membrane at near ambient temperatures. of fixed and variable costs. Capital recovery corresponds to the total
Compact Membrane Systems is developing a facilitated transport cost to cover cash costs and a profit, using a certain rate of return
membrane (FTM) for separating alkenes from alkanes. A facilitated (13.5% ATROI). Table 4 shows the economics and potential savings
silver transport membrane has the potential to cut energy, capi- that can be achieved by building a C2-ODH plant [10].
tal, and operating costs as conventional olefin/paraffin cryogenic Shutdown economics of emerging technologies is used by indus-
distillation separations are extremely energy and cost inten- tries to lower risk associated with building plants with new
sive. Olefin/paraffin membrane separations have been studied for technology. Shutdown economics occurs when new technology is
decades with increasing interest and developments in increasing so economically attractive that the capital recovery is less than
selectivity and stability of ion-exchange membranes. The construc- the cash costs of an existing plant. Therefore, the existing plants
tion of propane dehydrogenation units around the world has led are unable to pay for cash costs because the new technology can
to recent developments pertaining to propane/propylene separa- achieve a profit at a lower price. As a result, the shutdown of the
tions. Ethane/ethylene separations. The silver particles facilitate the existing plant occurs. Shutdown economics are achieved for C2-
transport of soluble olefins across the membrane with high selec- ODH with or without using conventional separations units coupled
tivity yielding a high purity olefin permeate. The C2-ODH reactor with an ODH reactor.
effluent compositions are synergistic with optimal membrane feed
compositions; water saturation has shown increased permeability 5. Further studies and applications
ratio of ethylene to ethane [8].
If a membrane is used, minimal, if any, separations are needed Further experiments proving the refractory nature of ethylene
before the reactor effluent enters the membrane because the is important as it plays a role as a diluent in the reactor. Oxygen
reactor effluent composition integrates well with the desired mem- flammability studies must be conducted to ensure safety in the
brane feed composition. It operates at near ambient temperatures design of the reactor. ODH using an M1 catalyst has further appli-
and is capable of separating out high purity products (90+%) which cations to a multitude of hydrocarbons other than ethane [4,11,12].
has significant economic impact on energy savings compared to Additional studies on the application of ODH using the M1 catalyst
cryogenic distillation. An ethane recycle may be added for optimal [6] are listed below:
recovery.

1) Ethylbenzene to Styrene Monomer

4. Economics 2) 2-Methyl-2-Butene to Isoprene
3) Mixed C4’s to 1,3-Butadiene
A standard required netback analysis was performed for CSP and 4) Isobutane to Isobutene
ODH technologies using the processing information provided from 5) Propylene and Ammonia to Acrylonitrile and Acetonitrile

Table 5
Scheme 3 Stream Definitions.

Stream Master Component (s) Stream Master Component (s)

1 Ethane 12 Isoprene
2 Ethylene 13 Polymer-grade Propylene
3 Polymer-grade Ethylene 14 Acrylonitrile and Acetonitrile
4 Mixed C4’s 15 Isobutane
5 Propylene 16 C7 Alkylate
6 Ethylbenzene 17 Isobutene
7 Styrene-Monomer 18 C8 Alkylate
8 1,3-Butadiene 19 Butane
9 Styrene-Butadiene Rubber 20 Benzene
10 Propylene and 2-Methyl-2-Butene 21 Oxygen
11 Cumene 22 Ammonia

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The US market for producing specialty petrochemicals is grow-
ing and gaps are forming from the transition from liquid crackers
to gas crackers. Scheme 3 is a list of possible end products, cou-
pling conventional technology with ODH technology, revealing a
new CPI [4,11,12]. Table 5 is a list of components associated with
the streams labeled in Scheme 3.
6. Conclusions
Ethylene is a commodity chemical with a growing capacity
worldwide. CSP is the current method for producing ethylene from
an either gas or liquid feedstock depending on location. The eco-
nomics for CSP expressed, as margins, are extremely attractive
yet C2-ODH shows potential for achieving shutdown economics
of current CSP plants. C2-ODH uses the M1 catalyst to selectively
dehydrogenate ethane and produce ethylene at low temperatures
and pressures. The moderate conditions, nearly stoichiometric
yields, and membrane separation of C2-ODH contribute to lowering
the capital, operating, and energy costs. The chemical processing
industry accounts for a large portion of the world’s carbon foot-
print; C2-ODH has the potential to drastically reduce the carbon
footprint of the top petrochemical produced globally. C2-ODH is a
simple, highly selective, exothermic process with the potential to
revolutionize the chemical processing industry (CPI).
Funding
This research did not receive any specific grant from funding
agencies in the public, commercial, or not-for-profit sectors.
Acknowledgement
The authors are grateful for the contribution and help of Dr. Gen-
naro J. Maffia, Chemical Engineering Professor at Manhattan College
and former/current colleague of Dr. Anne M. Gaffney.
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7
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