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Development of vanadium-phosphate catalysts for methanol production by selective oxidation of methane. Quarterly technical progress report No. 6, July--September 1994

Description: This is the eighth quarterly technical progress report. During this quarter the project was initiated, after transfer via a novation agreement, at the Colorado School of Mines. Project initiation activities have included: set up of catalyst synthesis apparatus; training on x-ray diffraction and FTIR apparatus; set up of catalyst testing reactor; set up of reactor product analytical systems; and set up of method development for measuring catalyst acidity via FTIR. At the end of this quarter significant progress had been made towards completion of these initiation activities. Several catalyst syntheses have been performed and the catalysts characterized by x-ray diffraction and FTIR. The catalyst testing reactor system is operational. Reactor product analysis system is nearing completion. Initiation of this system was delayed by the unavailability of a Valco valve which has just recently arrived. Set up of the in-situ FTIR cell for catalyst acidity studies has begun. In this report the results of several catalyst syntheses are reported along with characterization results. In particular, impregnation of vanadyl pyrophosphate with potassim nitrate dramatically reduced the number of surface hydroxyl groups. Such groups may be important in the non-selective, total oxidation of hydrocarbons. Also, preliminary experimental results on FTIR spectra of adsorbed pyridine are presented. It is shown that pyridine adsorbed on the catalyst surface can be easily observed by the diffuse reflectance IR technique. We plan to apply this technique to measurement of the acid site strength of surfaces modified with promoters.
Date: January 10, 1995
Creator: McCormick, R.L.
Partner: UNT Libraries Government Documents Department

Development of vanadium-phosphate catalysts for methanol production by selective oxidation of methane. Quarterly technical progress report 11, October--December 1995

Description: Activities during this report period focused on testing of additional modified and promoted catalysts and characterization of these materials. Methanol oxidation studies were performed as a method of acid site characterization. Improvements to the product gas analysis system continued to be developed. These results are reported. Specific accomplishments include: (1) Obtaining and interpreting infrared spectra of modified catalysts prepared to enhance surface acidity. (2) Testing of these catalysts in methanol oxidation as a method of acid site characterization and to determine catalytic activity for conversion of this desired product. Catalysts were quite active for methanol conversion to dimethyl ether. Two of the modified catalysts prepared in this work exhibited the highest activity for this reaction, presumably because of their higher surface areas. (3) Determination that acidity modifications had no effect on activity for methane conversion.
Date: April 16, 1996
Creator: McCormick, R.L.
Partner: UNT Libraries Government Documents Department

Development of vanadium-phosphate catalysts for methanol production by selective oxidation of methane. Quarterly technical progress report No. 9, April 1995--June 1995

Description: This document is the ninth quarterly technical progress report under Contract No. DE-AC22-92PC92110 {open_quotes}Development of Vanadium-Phosphate Catalysts for Methanol Production by Selective Oxidation of Methane{close_quotes}. Activities were focused on fine tuning of the microreactor system by elimination of transport effects and improvements in the analytical system. Process variable studies were conducted on vanadyl pyrophosphate and screening studies were conducted on several modified catalyst. One additional catalyst was prepared and characterization studies continued. These results are reported.
Date: September 14, 1995
Creator: McCormick, R.L.
Partner: UNT Libraries Government Documents Department

Development of vanadium-phosphate catalysts for methanol production by selective oxidation of methane. Quarterly technical progress report 8, January--March, 1995

Description: Activities during this quarter focused on fine tuning of catalyst characterization and synthesis techniques. Improvements in catalyst activity test methods were also implemented but more remains to be done. Specific accomplishments include: improved characterization of vanadyl pyrophosphate (VPO) and Si promoted VPO by FTIR and FTIR of chemisorbed bases; several minor improvements in catalyst preparation technique resulting in enhanced catalyst yield, better control of catalyst composition, and generation of less waste; preliminary pulsed reaction data on methane oxidation were also acquired. Preliminary activity measurements for methane conversion (without oxygen) in a pulsed reactor over VPO indicate that the primary reaction product is CO. Carbon dioxide is also formed but selectivity to CO{sub 2} decreases with number of pulses. These results suggest that selectivity to partially oxidized products improves with catalyst reduction and suggest that some surface modification will be required to obtain oxidized hydrocarbon products. Note that catalyst activation (conversion from the precursor to VPO) has been carried out using air. For butane oxidation catalysts VPO is activated in a 1% butane/air mixture which produces a slightly reduced catalyst.
Date: May 25, 1995
Creator: McCormick, R.L.
Partner: UNT Libraries Government Documents Department

Development of vanadium-phosphate catalysts for methanol production by selective oxidation of methane. Quarterly technical progress report 10, July 1, 1995--September 31, 1995

Description: This document is the tenth quarterly technical progress report under Contract No. DE-AC22-92PC92110 {open_quotes}Development of Vanadium-Phosphate Catalysts for Methanol Production by Selective Oxidation of Methane{close_quotes}. Activities focused on testing of additional modified and promoted catalysts and characterization of these materials. Attempts at improving the sensitivity of our GC based analytical systems were also made with some success. Methanol oxidation studies were initiated. These results are reported. Specific accomplishments include: (1) Methane oxidation testing of a suite of catalysts promoted with most of the first row transition metals was completed. Several of these materials produced low, difficult to quantify yields of formaldehyde. (2) Characterization of these materials by XRD and FTIR was performed with the goal of correlating activity and selectivity with catalyst properties. (3) We began to characterize catalysts prepared via modified synthesis methods designed to enhance acidity using TGA measurements of acetonitrile chemisorption and methanol dehydration to dimethyl ether as a test reaction. (4) A catalyst prepared in the presence of naphthalene methanol as a structural disrupter was tested for activity in methane oxidation. It was found that this material produced low yields of formaldehyde which were difficult to quantify. (5) Preparation of catalysts with no Bronsted acid sites. This was accomplished by replacement of exchangeable protons with potassium, and (6) Methanol oxidation studies were initiated to provide an indication of catalyst activity for decomposition of this desired product and as a method of characterizing the catalyst surface.
Date: December 7, 1995
Creator: McCormick, R.L.
Partner: UNT Libraries Government Documents Department

Results of the 2007 B100 Quality Survey

Description: In a 2007 analysis of samples from 52% of U.S. biodiesel (B100) producers, 90% met ASTM and other specifications for critical engine performance properties and for elements that harm emission controls.
Date: March 1, 2008
Creator: Alleman, T. L. & McCormick, R. L.
Partner: UNT Libraries Government Documents Department

2008 B20 Survey Results (Presentation)

Description: Describes results of a sample survey of the quality of B20, a biodiesel blend, collected from U.S. public pumps and fleets as part of a joint effort by NREL, the NBB, and engine manufacturers.
Date: February 2, 2009
Creator: Alleman, T. L. & McCormick, R. L.
Partner: UNT Libraries Government Documents Department

Empirical Study of the Stability of Biodiesel and Biodiesel Blends: Milestone Report

Description: The objective of this work was to develop a database that supports specific proposals for a stability test and specification for biodiesel and biodiesel blends. B100 samples from 19 biodiesel producers were obtained in December of 2005 and January of 2006 and tested for stability. Eight of these samples were then selected for additional study, including long-term storage tests and blending at 5% and 20% with a number of ultra-low sulfur diesel fuels.
Date: May 1, 2007
Creator: McCormick, R. L. & Westbrook, S. R.
Partner: UNT Libraries Government Documents Department

Development of Vanadium Phosphaate Catalysts for Methanol Production by Selective Oxidation of Methane.

Description: This DOE sponsored study of methane partial oxidation was initiated at Amax Research and Development in Golden, CO in October of 1993. Shortly thereafter the management of Amax closed this R&D facility and the PI moved to the Colorado School of Mines. The project was begun again after contract transfer via a novation agreement. Experimental work began with testing of vandyl pyrophosphate (VPO), a well known alkane selective oxidation catalyst. It was found that VPO was not a selective catalyst for methane conversion yielding primarily CO. However, promotion of VPO with Fe, Cr, and other first row transition metals led to measurable yields for formaldehyde, as noted in the summary table. Catalyst characterization studies indicated that the role of promoters was to stabilize some of the vanadium in the V{sup 5+} oxidation state rather than the V{sup 4+} state formally expected for (VO){sub 2}P{sub 2}O{sub 7}.
Date: October 1, 1997
Creator: McCormick, R.L.
Partner: UNT Libraries Government Documents Department

Development of vanadium-phosphate catalysts for methanol production by selective oxidation of methane

Description: Amax R D will perform laboratory scale development of a promising, practical catalyst for the selective oxidation of methane to methanol. The primary component of this catalyst is vanadium-phosphate (VPO) which has shown good activity and selectivity in the partial oxidation of n-butane and propane but has not been studied in detail for methane oxidation. The goal of the project is to develop a catalyst which allows methane oxidation to methanol to be conducted at high conversion and selectivity. A low CH[sub 4]/O[sub 2] ratio will be employed with air as the source of oxygen. Temperatures below 600[degrees]C and pressures up to 20 atm are to be investigated. The use of steam in the feed gas will also be investigated. The catalyst development strategy will be to utilize promoters and supports to improve the activity and selectivity of the unmodified VPO catalyst. The catalyst testing reactor system was used to perform blank (empty) reactor runs over a wide range of temperatures, pressure, and flow rates. No methane conversion was observed at temperatures of 500[degrees]C or lower in any of the tests. At higher temperatures, significant methane conversion to carbon dioxide was observed. At 550[degrees]C, 300 psig, and the highest flow rate studied, reactor ignition was observed. Based on the results of these blank runs, we conclude that catalyst testing should be performed at temperatures not to exceed 500[degrees]C.
Date: March 4, 1993
Creator: McCormick, R.L. & Jha, M.C.
Partner: UNT Libraries Government Documents Department

Compendium of Experimental Cetane Number Data

Description: In this report, we present a compilation of reported cetane numbers for pure chemical compounds. The compiled database contains cetane values for 299 pure compounds, including 156 hydrocarbons and 143 oxygenates. Cetane number is a relative ranking of fuels based on the amount of time between fuel injection and ignition. The cetane number is typically measured either in a combustion bomb or in a single-cylinder research engine. This report includes cetane values from several different measurement techniques - each of which has associated uncertainties. Additionally, many of the reported values are determined by measuring blending cetane numbers, which introduces significant error. In many cases, the measurement technique is not reported nor is there any discussion about the purity of the compounds. Nonetheless, the data in this report represent the best pure compound cetane number values available from the literature as of August 2004.
Date: September 1, 2004
Creator: Murphy, M. J.; Taylor, J. D. & McCormick, R. L.
Partner: UNT Libraries Government Documents Department

2006 B100 Quality Survey Results: Milestone Report

Description: In 2006, the National Renewable Energy Laboratory conducted a nationwide quality survey of pure biodiesel (B100) intended to be used as a blendstock. The study collected random samples throughout the United States and analyzed them for quality against the current and proposed ASTM D6751 fuel quality specifications.
Date: May 1, 2007
Creator: Alleman, T. L.; McCormick, R. L. & Deutch, S.
Partner: UNT Libraries Government Documents Department

St. Louis Metro Biodiesel (B20) Transit Bus Evaluation: 12-Month Final Report

Description: The St. Louis Metro Bodiesel Transit Bus Evaluation project is being conducted under a Cooperative Research and Development Agreement between NREL and the National Biodiesel Board to evaluate the extended in-use performance of buses operating on B20 fuel. The objective of this research project is to compare B20 and ultra-low sulfur diesel buses in terms of fuel economy, veicles maintenance, engine performance, component wear, and lube oil performance.
Date: July 1, 2008
Creator: Barnitt, R.; McCormick, R. L. & Lammert, M.
Partner: UNT Libraries Government Documents Department

Effect of B20 and Low Aromatic Diesel on Transit Bus NOx Emissions Over Driving Cycles with a Range of Kinetic Intensity

Description: Oxides of nitrogen (NOx) emissions for transit buses for up to five different fuels and three standard transit duty cycles were compared to establish whether there is a real-world biodiesel NOx increase for transit bus duty cycles and engine calibrations. Six buses representing the majority of the current national transit fleet and including hybrid and selective catalyst reduction systems were tested on a heavy-duty chassis dynamometer with certification diesel, certification B20 blend, low aromatic (California Air Resources Board) diesel, low aromatic B20 blend, and B100 fuels over the Manhattan, Orange County and UDDS test cycles. Engine emissions certification level had the dominant effect on NOx; kinetic intensity was the secondary driving factor. The biodiesel effect on NOx emissions was not statistically significant for most buses and duty cycles for blends with certification diesel, except for a 2008 model year bus. CARB fuel had many more instances of a statistically significant effect of reducing NOx. SCR systems proved effective at reducing NOx to near the detection limit on all duty cycles and fuels, including B100. While offering a fuel economy benefit, a hybrid system significantly increased NOx emissions over a same year bus with a conventional drivetrain and the same engine.
Date: October 1, 2012
Creator: Lammert, M. P.; McCormick, R. L.; Sindler, P. & Williams, A.
Partner: UNT Libraries Government Documents Department

Biodiesel Fuel Property Effects on Particulate Matter Reactivity

Description: Controlling diesel particulate emissions to meet the 2007 U.S. standard requires the use of a diesel particulate filter (DPF). The reactivity of soot, or the carbon fraction of particulate matter, in the DPF and the kinetics of soot oxidation are important in achieving better control of aftertreatment devices. Studies showed that biodiesel in the fuel can increase soot reactivity. This study therefore investigated which biodiesel fuel properties impact reactivity. Three fuel properties of interest included fuel oxygen content and functionality, fuel aromatic content, and the presence of alkali metals. To determine fuel effects on soot reactivity, the performance of a catalyzed DPF was measured with different test fuels through engine testing and thermo-gravimetric analysis. Results showed no dependence on the aromatic content or the presence of alkali metals in the fuel. The presence and form of fuel oxygen was the dominant contributor to faster DPF regeneration times and soot reactivity.
Date: June 1, 2010
Creator: Williams, A.; Black, S. & McCormick, R. L.
Partner: UNT Libraries Government Documents Department