ASTM D7206/D7206M-19
(Guide)Standard Guide for Cyclic Deactivation of Fluid Catalytic Cracking (FCC) Catalysts with Metals
Standard Guide for Cyclic Deactivation of Fluid Catalytic Cracking (FCC) Catalysts with Metals
SIGNIFICANCE AND USE
4.1 This guide describes techniques of deactivation that can be used to compare a series of cracking catalysts at equilibrium conditions or to simulate the equilibrium conditions of a specific commercial unit and a specific catalyst.
SCOPE
1.1 This guide covers the deactivation of fluid catalytic cracking (FCC) catalyst in the laboratory as a precursor to small scale performance testing such as catalyst activities (Test Method D3907) or activities plus selectivities (Test Methods D5154 and D7964). FCC catalysts are deactivated in the laboratory in order to simulate the aging that occurs during continuous use in a commercial fluid catalytic cracking unit (FCCU). Deactivation for purposes of this guide constitutes hydrothermal deactivation of the catalyst and metal poisoning by nickel and vanadium. Hydrothermal treatment is used to simulate the physical changes that occur in the FCC catalyst through repeated regeneration cycles. Hydrothermal treatment (steaming) destabilizes the faujasite (zeolite Y), resulting in reduced crystallinity and surface area. Further decomposition of the crystalline structure occurs in the presence of vanadium, and to a lesser extent in the presence of nickel. Vanadium is believed to form vanadic acid in a hydrothermal environment resulting in destruction of the zeolitic portion of the catalyst. Nickel’s principle effect is to poison the selectivity of the FCC catalyst. Hydrogen and coke production is increased in the presence of nickel, due to the dehydrogenation activity of the metal. Vanadium also exhibits significant dehydrogenation activity, the degree of which can be influenced by the oxidation and reduction conditions prevailing throughout the deactivation process. The simulation of the metal effects that one would see commercially is part of the objective of deactivating catalysts in the laboratory. Catalyst deactivation by hydrothermal treatment only is addressed in Guide D4463/D4463M.
1.2 The two basic approaches to laboratory-scale simulation of commercial equilibrium catalysts described in this guide are as follows:
1.2.1 Cyclic Propylene Steaming (CPS) Method, in which the catalyst is impregnated with the desired metals via an incipient wetness procedure (Mitchell method)2 followed by a prescribed steam deactivation.
1.2.2 Crack-on Methods, in which fresh catalyst is subjected to a repetitive sequence of cracking (using a feed with enhanced metals concentrations), stripping, and regeneration in the presence of steam. Two specific procedures are presented here, a procedure with alternating metal deposition and deactivation steps and a modified Two-Step procedure, which includes a cyclic deactivation process to target lower vanadium dehydrogenation activity.
1.3 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used independently of the other, and values from the two systems shall not be combined.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D7206/D7206M − 19
Standard Guide for
Cyclic Deactivation of Fluid Catalytic Cracking (FCC)
1
Catalysts with Metals
This standard is issued under the fixed designation D7206/D7206M; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
2
1. Scope incipient wetness procedure (Mitchell method) followed by a
prescribed steam deactivation.
1.1 This guide covers the deactivation of fluid catalytic
1.2.2 Crack-onMethods,inwhichfreshcatalystissubjected
cracking (FCC) catalyst in the laboratory as a precursor to
to a repetitive sequence of cracking (using a feed with
small scale performance testing such as catalyst activities (Test
enhancedmetalsconcentrations),stripping,andregenerationin
Method D3907) or activities plus selectivities (Test Methods
the presence of steam. Two specific procedures are presented
D5154 and D7964). FCC catalysts are deactivated in the
here, a procedure with alternating metal deposition and deac-
laboratory in order to simulate the aging that occurs during
tivation steps and a modified Two-Step procedure, which
continuous use in a commercial fluid catalytic cracking unit
includesacyclicdeactivationprocesstotargetlowervanadium
(FCCU). Deactivation for purposes of this guide constitutes
dehydrogenation activity.
hydrothermal deactivation of the catalyst and metal poisoning
by nickel and vanadium. Hydrothermal treatment is used to 1.3 The values stated in either SI units or inch-pound units
simulate the physical changes that occur in the FCC catalyst are to be regarded separately as standard. The values stated in
through repeated regeneration cycles. Hydrothermal treatment each system are not necessarily exact equivalents; therefore, to
(steaming) destabilizes the faujasite (zeolite Y), resulting in ensure conformance with the standard, each system shall be
reduced crystallinity and surface area. Further decomposition used independently of the other, and values from the two
of the crystalline structure occurs in the presence of vanadium, systems shall not be combined.
and to a lesser extent in the presence of nickel. Vanadium is
1.4 This standard does not purport to address all of the
believed to form vanadic acid in a hydrothermal environment
safety concerns, if any, associated with its use. It is the
resulting in destruction of the zeolitic portion of the catalyst.
responsibility of the user of this standard to establish appro-
Nickel’s principle effect is to poison the selectivity of the FCC
priate safety, health, and environmental practices and deter-
catalyst. Hydrogen and coke production is increased in the
mine the applicability of regulatory limitations prior to use.
presence of nickel, due to the dehydrogenation activity of the
1.5 This international standard was developed in accor-
metal. Vanadium also exhibits significant dehydrogenation
dance with internationally recognized principles on standard-
activity,thedegreeofwhichcanbeinfluencedbytheoxidation
ization established in the Decision on Principles for the
and reduction conditions prevailing throughout the deactiva-
Development of International Standards, Guides and Recom-
tionprocess.Thesimulationofthemetaleffectsthatonewould
mendations issued by the World Trade Organization Technical
see commercially is part of the objective of deactivating
Barriers to Trade (TBT) Committee.
catalysts in the laboratory. Catalyst deactivation by hydrother-
mal treatment only is addressed in Guide D4463/D4463M.
2. Referenced Documents
3
1.2 The two basic approaches to laboratory-scale simulation
2.1 ASTM Standards:
of commercial equilibrium catalysts described in this guide are
D3907 Test Method for Testing Fluid Catalytic Cracking
as follows:
(FCC) Catalysts by Microactivity Test
1.2.1 Cyclic Propylene Steaming (CPS) Method, in which
D4463/D4463M Guide for Metals Free Steam Deactivation
the catalyst is impregnated with the desired metals via an
2
Mitchell, B. R., Industrial and Engineering Chemistry Product Research and
1
This guide is under the jurisdiction ofASTM Committee D32 on Catalysts and Development, 19, 1980, p. 209.
3
is the direct responsibility of Subcommittee D32.04 on Catalytic Properties. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2019. Published April 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2006. Last previous edition approved in 2013 as D7
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D7206/D7206M − 06 (Reapproved 2013) D7206/D7206M − 19
Standard Guide for
Cyclic Deactivation of Fluid Catalytic Cracking (FCC)
1
Catalysts with Metals
This standard is issued under the fixed designation D7206/D7206M; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1
ε NOTE—Editorially changed 8.2.1.1 in March 2013.
1. Scope
1.1 This guide covers the deactivation of fluid catalytic cracking (FCC) catalyst in the laboratory as a precursor to small scale
performance testing. testing such as catalyst activities (Test Method D3907) or activities plus selectivities (Test Methods D5154
and D7964). FCC catalysts are deactivated in the laboratory in order to simulate the aging that occurs during continuous use in
a commercial fluid catalytic cracking unit (FCCU). Deactivation for purposes of this guide constitutes hydrothermal deactivation
of the catalyst and metal poisoning by nickel and vanadium. Hydrothermal treatment is used to simulate the physical changes that
occur in the FCC catalyst through repeated regeneration cycles. Hydrothermal treatment (steaming) destabilizes the faujasite
(zeolite Y), resulting in reduced crystallinity and surface area. Further decomposition of the crystalline structure occurs in the
presence of vanadium, and to a lesser extent in the presence of nickel. Vanadium is believed to form vanadic acid in a hydrothermal
environment resulting in destruction of the zeolitic portion of the catalyst. Nickel’s principle effect is to poison the selectivity of
the FCC catalyst. Hydrogen and coke production is increased in the presence of nickel, due to the dehydrogenation activity of the
metal. Vanadium also exhibits significant dehydrogenation activity, the degree of which can be influenced by the oxidation and
reduction conditions prevailing throughout the deactivation process. The simulation of the metal effects that one would see
commercially is part of the objective of deactivating catalysts in the laboratory. Catalyst deactivation by hydrothermal treatment
only is addressed in Guide D4463/D4463M.
1.2 The two basic approaches to laboratory-scale simulation of commercial equilibrium catalysts described in this guide are as
follows:
1.2.1 Cyclic Propylene Steaming (CPS) Method, in which the catalyst is impregnated with the desired metals via an incipient
2
wetness procedure (Mitchell method) followed by a prescribed steam deactivation.
1.2.2 Crack-on Methods, in which fresh catalyst is subjected to a repetitive sequence of cracking (using a feed with enhanced
metals concentrations), stripping, and regeneration in the presence of steam. Two specific procedures are presented here, a
procedure with alternating metal deposition and deactivation steps and a modified Two-Step procedure, which includes a cyclic
deactivation process to target lower vanadium dehydrogenation activity.
1.3 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each
system mayare not benecessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used
independently of the other. Combiningother, and values from the two systems may result in non-conformance with the
standard.shall not be combined.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
1
This guide is under the jurisdiction of ASTM Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.04 on Catalytic Properties.
Current edition approved March 1, 2013April 1, 2019. Published March 2013April 2019. Originally approved in 2006. Last previous edition approved in 20122013 as
ɛ1
D7206/D7206M–06(2012)D7206/D7206M–06(2013) e1. DOI: 10.1520/D7206_D7206M-06R13E01.10.1520/D
...
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