ASTM D5154 D5154M-2018 Standard Test Method for Determining Activity and Selectivity of Fluid Catalytic Cracking (FCC) Catalysts by Microactivity Test.pdf

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1、Designation: D5154 10D5154/D5154M 18Standard Test Method forDetermining Activity and Selectivity of Fluid CatalyticCracking (FCC) Catalysts by Microactivity Test1This standard is issued under the fixed designation D5154;D5154/D5154M; the number immediately following the designation indicatesthe year

2、 of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers determining the activity and se

3、lectivity of either equilibrium or laboratory deactivated fluid catalyticcracking (FCC) catalysts. The activity is evaluated on the basis of mass percent conversion of gas oil feed in a microactivity unit.The selectivities are evaluated on the basis of mass percent yields of specifically defined pro

4、ducts resulting from the catalyticcracking of gas oil.oil feed.1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values given inparentheses are mathematical conversions to SI units that are provided for information only and are not considered

5、 stated in eachsystem may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from thetwo systems may result in non-conformance with the standard.1.2.1 ExceptionSI units have been retained in some of the figures.1.3 This standard does not purpo

6、rt to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.1.4 This internation

7、al standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.

8、2. Referenced Documents2.1 ASTM Standards:2D2887 Test Method for Boiling Range Distribution of Petroleum Fractions by Gas ChromatographyD3907 Test Method for Testing Fluid Catalytic Cracking (FCC) Catalysts by Microactivity TestD4463 Guide for Metals Free Steam Deactivation of Fresh Fluid Cracking C

9、atalystsD7964 Test Method for Determining Activity of Fluid Catalytic Cracking (FCC) Catalysts in a Fluidized BedE105 Practice for Probability Sampling of MaterialsE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE456 Terminology Relating to Quality and StatisticsE691 Practi

10、ce for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 activitycalculated as conversion divided by the difference of 100 minus conversion.3.1.2 ASTM reference catalystsa set of equilibrium FCC catal

11、ysts within the useful range of this test method is used toimprove the reproducibility of test results between different laboratories. Each catalyst has a consensus mean conversion valueassigned to it by Committee D32. Samples of the ASTM reference catalysts can be obtained through NIST.3.1.3 ASTM s

12、tandard feeda specific batch of gas oil that is used as feedstock in the described test method.31 This test method 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 April 1, 2010May 1,

13、 2018. Published May 2010May 2018. Originally approved in 1991. Last previous edition approved in 20052010 asD515405.10. DOI: 10.1520/D5154-10.10.1520/D5154_D5154M-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual B

14、ook of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available Formerly available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070,http:/www.nist.gov.This document is not an ASTM

15、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. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all

16、cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.4 catalyst/oil (C/O) ratiothe mass of catalyst used in the test divided b

17、y the mass of feed fed to the reactor. In practice,the mass of catalyst is usually maintained at a constant value and the total mass of feed is varied.3.1.5 contact timecalculated as 3600/(WHSV C/O). This is the delivery time, in seconds, during which feed is introducedto the reactor.3.1.6 HCOthe he

18、avy cycle oil product defined to have a minimum boiling point of 650F (343C).3.1.7 LCOthe light cycle oil product defined to have a boiling point range of 421 to 650F (216 to 343C).3.1.6 measured conversioncalculated as the difference between the mass of feed used and the mass of unconverted materia

19、ldivided by the mass of feed used times 100 %. The unconverted material is defined as all liquid product with a boiling point above42F (216C).216 C 421 F.3.1.7 gasolineC5 compounds through compounds boiling at 216 C 421 F.3.1.8 HCOthe heavy cycle oil product defined to have a minimum boiling point o

20、f 343 C 650 F.3.1.9 LCOthe light cycle oil product defined to have a boiling point range of 216 C to 343 C 421F to 650 F.3.1.10 liquid productall products formed in the catalytic reaction that can be condensed in the chiller bath afterward, usuallya combination of gasoline, LCO, and HCO, but can con

21、tain a trace of C4 and C4 minus compounds.3.1.11 normalized product yieldthe result obtained when each product yield has been corrected for non-perfect mass balances.For a run to be judged acceptable, the total recovery, wt %mass % of feed, should be in the range of 96 to 101 % prior tonormalization

22、. If the recovery is outside this range the test data should be discarded.3.1.12 product yieldone hundred times the mass of a specific product divided by the mass of feed used in the test.3.1.13 reaction severityan indication of the severity of the cracking reaction which allows a range of conversio

23、ns to beobtained from any particular catalyst without changing reactor temperature. Changing reaction severity is achieved by changingWHSV or C/O ratio or both.3.1.14 selectivitysame as yield. Selectivity generally refers to how much of a particular product, such as coke, is formedduring a chemical

24、reaction; selectivity is related to, but different from, conversion, which is the total amount of all products formedduring the reaction.3.1.15 weight hourly space velocity (WHSV)the oil feed rate in grams per hour divided by the mass of catalyst in grams. Unitsare hr-1.4. Summary of Test Method4.1

25、At least two samples of FCC catalysts, one of which is chosen as a reference, are separately contacted with gas oil feed(ASTM Standard Feed or other suitable feedstock) in a fixed bed reactor at a specified reaction temperature and at more than onereaction severity. Reaction products (liquid, gas, a

26、nd coke on catalyst) are analyzed. Conversion, activity, and product yields arecalculated for each experiment.4.2 Following analysis of the products, the total recovery (that is, mass balance) of the feed as converted and unconvertedproducts is determined. If the recovery is less than 96 % or greate

27、r than 101 %, the test is rejected as unsatisfactory.unsatisfactory(an outlier).4.3 For each catalyst tested, normalized product yields are plotted against conversion or activity to generate a yield curve. Thedata comprising the yield curve may be used to obtain the parameters of an appropriate math

28、ematical expression for the curve.Comparisons among catalysts can be made by interpolating the yield curves to obtain the product yields at some specifiedconversion.5. Significance and Use5.1 The microactivity test provides data to assess the relative performance of FCC catalysts. Because results ar

29、e affected bycatalyst pretreatment, feedstock characteristics, test equipment, and operating parameters, adherence to this test method is aprerequisite for correct interpretation of results. Apparatus, test conditions, and analytical procedures actually used should closelyresemble those described in

30、 this test method. Significant variations in apparatus, test conditions and/or analytical procedures mayresult in activity and selectivity data which do not correlate with data developed by other laboratories on identicalcatalyst/feedstock samples.5.2 The standard method reaction temperature is 960F

31、 (516C).516 C 960 F. Other reaction temperatures can be used;however, catalyst selectivity data developed at temperatures other than 960F (516C)516 C 960 F may not correlate withselectivity data developed at 960F (516C).516 C 960 F.Also, precision at other reaction temperatures may change comparedto

32、 data obtained at 960F (516C).516 C 960 F.D5154/D5154M 1826. Apparatus6.1 The apparatus of this test method is essentially that described inTest Method D3907, as shown in Figs. 1-4, with the additionof a gas collection system on the effluent gas vent line. In a typical gas collection system, a fluid

33、 water is displaced by the collectedgas and the volume of displaced liquidwater provides a quantitative measurement of the amount of gas collected. To minimize thesolubility of gases like H2 and H2S in the fluid, a saturated brine (NaCl) solution is recommended. Other gas collection systemscan be us

34、ed, such as the water-free gasometer (consisting of two gas chambers in series, each with a piston inside) which is moreideal for H2S quantification.4 Some publications have appeared which give example flow schematics and more detaileddescriptions of typical apparatus.5 Alternatively, there are seve

35、ral vendors as listed in Research Report RR:D32-10306 who canprovide specific equipment for performing this test. However, Committee D32 can only suggest and will not recommend nor certifyany specific vendor. Significant variations from the test apparatus of this method most likely will result in si

36、gnificantly differentactivity and selectivity data from identical catalyst samples.6.2 Chromatographic Equipment:6.2.1 Liquid product analyses should be performed using Test Method D2887 on a gas chromatograph (G.C.)(GC) equippedwith a flame ionization detector.6.2.2 Gas product analyses may be acco

37、mplished in two parts. First, an analysis using a G.C.a GC equipped with a thermalconductivity detector, employing Ndetector is needed2 as a carrier gas, andfor quantitative identification of H2 using aand N2 G.CH2 column that permits the separation and quantitative identification of HS can optional

38、ly be detected, but will not be quantitativein2 and Hunits that2S. collect gas by water displacement Second, an analysis using a G.C.GC equipped with a FID or TCD,employing He as a carrier gas and using a column that permits the separation and quantitative identification of methane, ethane,ethylene,

39、 propane, propylene, n-butane, iso-butane, 1-butene and iso-butene, cis-2-butene, and trans-2-butene, C5s (C5andsaturates, i.e., i-pentane and n-pentane) and a C5+ lump (including C5 olefins, i.e., i-pentenes and n-pentenes, and C6+, i.e., C6 toC9 ) that is not resolved. The C5s and the C5+ group ar

40、e included as part of the gasoline fraction.4 Ng, S.H., Shi,Y., Heshka, N.E., Zhang,Y., Little, E. “Laboratory Production of Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking Conversion”,J. Vis. Exp. e54390, doi:10.3791/54390.5 Campagna, R. J., Wick, J. P., Brady, M. F., and F

41、ort, D. L., “ Fresh FCC Catalyst Tests Predict Performance,” OGJ, March 24, 1986, p. 85.6 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D32-1030.NOTE 1This drawing is not to scale. For engineering details, see other drawings.F

42、IG. 1 Microactivity Flow ChartD5154/D5154M 1836.3 Carbon analysis of a representative sample of the spent catalyst (that is, the catalyst after the cracking reaction has beencompleted) reaction) may be accomplished using a commercially available carbon analyzer.analyzer if the microactivity unit bei

43、ngused does not have catalyst regeneration capability. If the microactivity unit is a model that does have regeneration capability, thenthe carbon on catalyst is back calculated from the CO2 evolved in the flue gas during the regeneration cycle.7. Sampling7.1 A sampling procedure is needed. Practice

44、 E105 is appropriate.8. Sample Preparation8.1 Equilibrium CatalystsDry samples or decoke, or both, and remove coke by heating a shallow (less than 10 mm thick) bedof catalyst in a porcelain crucible at 1094590 6 36F (59020 C 1094 6 20C)36 F for a length of time sufficient to removeFIG. 2 Microactivi

45、ty ReactorD5154/D5154M 184FIG. 3 Reactor Feed Tube InsertD5154/D5154M 185any coke. This typically requires approximately three hours.3 h. Sufficient air should be available in the furnace to burn the samplefree of coke. Insufficient decoking coke removal is indicated by a difference in color of the

46、top and bottom layers. The hot crucibleis cooled in a desiccator to prevent moisture pickup.NOTE 1Heavily coked samples may be damaged by sintering or deactivation if oxidation is allowed to occur too rapidly, leading to artificially lowcatalytic activity and surface area.8.2 Fresh CatalystsFresh ca

47、talyst samples should be steam treated prior to selectivity testing. Steaming procedures such asthose specified in Guide D4463 may be used. However, specific conditions (temperature, partial pressure of steam, and time)should be chosen such that the steamed catalyst properties (activity, zeolite and

48、 matrix surface areas, and unit cell size)approximate those found in equilibrium FCC catalysts of the same type.9. Procedure9.1 Reactor Preparation:9.1.1 Rinse feed line with acetone or other suitable solvent and dry with air. Periodic cleaning of the insert is recommended byair purge at 1022F (550C

49、)550 C 1022 F for one hour at least once every 12 tests.9.1.2 Wash the reactor and product receiver thoroughly with acetone or other suitable solvent and dry. If necessary, burn outany coke deposited in the reactor by heating in air at 960F (516C)516 C 960 F prior to washing.9.1.3 Insert a plug of quartz or borosilicate glass wool (about 20 mm length) until it reaches the constricted region of the reactor.Optionally, a reactor with a fritted disc may be used to position the catalyst.