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DOE OSTI2025

Experimental and fuel-surrogates modeling study of the high-pressure pyrolysis of specialty cetane number fuels: implications for fall-off in ethylene unimolecular dissociation

Single pulse shock tube experiments were conducted at 50 atm nominal pressure and 4 ms nominal reaction time over a temperature range of 900–1800 K, to study the pyrolysis speciation of a multi-component jet fuel, F-24, and six cetane number (CN) specialty fuels - CN30, CN35, CN40, CN45, CN50, and CN55. Gas chromatography (GC) was used to qualitatively and quantitatively analyze the post shock gases. The relationship between the formation of key pyrolysis species and the chemically controlled combustion propensity as reflected by the cetane number of each fuel was examined. A surrogate-based mechanism from the CRECK Modelling Group and chemical-functional group based optimized surrogates (CFGO) were used to simulate the pyrolysis speciation results. The model was able to capture the chemistry of most species except two important pyrolysis intermediates – ethylene and acetylene. Chemical kinetic analyses were performed to identify the important reactions which affect the chemistry of these species; however, the rate parameters of critical reactions were found to be unsuitable for simulating the present high-pressure studies. Here, to address this unsuitability, a theory-based fall-off analysis for three reactions representing the decomposition of ethylene and subsequent formation of acetylene was performed, and these are included in an updated version of the CRECK mechanism. This update resolves discrepancies between the experimental results and simulations for ethylene and acetylene. Reaction flux analyses using the updated surrogate model were also performed to identify the important reaction pathways responsible for the formation of crucial species and to provide an analysis of the chemistry of complex multi-component fuel systems. The fundamental reactions responsible for driving pyrolysis chemistry were greatly influenced by the chemical functional groups present in these fuels. In addition to updating the rate parameters of specific reactions to improve modeling, this study also emphasizes the effectiveness of the fuel-surrogate approach, where surrogates representing the chemical functional group composition of the parent fuel serve as a valuable tool for predicting the combustion chemistry of novel fuels.

Chemical Kinetics↗

DOE OSTI2025

Influence of functional additives, fillers, and pigments on thermal and catalytic pyrolysis of polyethylene for waste plastic upcycling

Pyrolysis offers a relatively green and economical method to convert waste plastics into valuable chemicals and fuels without the need for harmful solvents, toxic chemicals, or costly high-pressure reactors. Despite its popularity among chemical upcycling technologies, industrial adoption suffers from feedstock heterogeneity, low-quality products, and catalyst deactivation. Most plastics in our daily lives are formulated with functional additives, fillers, and colorants. These additives remaining in end-of-life waste streams increase feedstock heterogeneity, creating a challenging issue in recycling plastics. Still, the potential impacts of additives on the chemical upcycling of plastics have been poorly understood. In this study, polyethylene compounded with a range of widely used additives (antioxidants, stabilizers, pigments, fillers, slip agents, and flame retardants) was subjected to both thermal pyrolysis and catalytic pyrolysis in different catalyst-to-feedstock contact modes. It showed that many inorganic additives, such as talc, kaolin, CaCO 3 , TiO 2 , carbon black, and zinc stearate, facilitated polymer decomposition during pyrolysis, increasing light hydrocarbons while also promoting aromatic and carbon residue formation. Conversely, antioxidants and stabilizers inhibited depolymerization, favoring heavier hydrocarbons. During catalytic pyrolysis with HZSM-5 zeolite, additives strongly enhanced aromatic and catalytic coke formation, especially when there was direct contact between plastics and catalysts. Although certain additives seem beneficial in the short term by promoting polymer cracking and improving the selectivity of aromatics, the transport of the additives and their degradation products and increased carbon coking can contaminate products, deactivate or modify catalysts, and foul reactors. These findings address a critical knowledge gap in effectively converting waste plastics via a greener route.

42 ENGINEERING↗

NASA NTRS1971

Molecular configuration and pyrolysis reactions of phenolic-novolaks.

Description of a statistical method for characterizing the structure of an average phenolic-novolak prepolymer molecule in terms of the total number of phenolic nuclei that compose the molecule and the number of these nuclei that are pendent. It is only necessary to resort to experimental pyrolysis to evaluate the thermokinetic parameters for pyrolysis for the ablator. In addition, the fraction of phenolic involved in the major pyrolysis reactions can be estimated in terms of the parameters previously evaluated. It is shown that the overlapping reactions which occur during pyrolysis of a phenolic-novolak can be resolved by pyrolyzing samples with different extents of cure. It is then possible to determine the kinetic parameters for pyrolysis for the major reactions by well-known methods which often fail when reactions are not well resolved.

Winkler, E. L.↗

NASA NTRS1974

Pyrolysis system evaluation study

An evaluation of two different pyrolysis concepts which recover energy from solid waste was conducted in order to determine the merits of each concept for integration into a Integrated Utility System (IUS). The two concepts evaluated were a Lead Bath Furnace Pyrolysis System and a Slagging Vertical Shaft, Partial Air Oxidation Pyrolysis System. Both concepts will produce a fuel gas from the IUS waste and sewage sludge which can be used to offset primary fuel consumption in addition to the sanitary disposal of the waste. The study evaluated the thermal integration of each concept as well as the economic impact on the IUS resulting from integrating each pyrolysis concepts. For reference, the pyrolysis concepts were also compared to incineration which was considered the baseline IUS solid waste disposal system.

Source record↗

NASA NTRS1978

Concentration-response data on toxicity of pyrolysis gases from six synthetic polymers

Concentration-response data are presented on the toxic effects of the pyrolysis gases from six synthetic polymers on Swiss Webster male mice, using a toxicity screening test method. The polymers consisted of one sample each of polycarbonate and polystyrene, and two samples each of polyethylene and acrylonitrile-butadiene-styrene (ABS). All six samples were evaluated using the rising temperature program, and three samples were evaluated using the fixed temperature program. The pyrolysis gases from polycarbonate, polyethylene, and ABS appeared to exhibit the concentration-response relationships commonly encountered in toxicology. The polystyrene sample gave variable results; probably due to poor reproducibility of the essentially anaerobic pyrolysis. Carbon monoxide seemed to be the principal toxicant in the pyrolysis gases from polycarbonate and polyethylene, but did not appear to be the principal toxicant in the pyrolysis gases from ABS.

Hilado, C. J.↗

NASA NTRS1985

A ceramic matrix composite based on polymerization and pyrolysis of ethynylated aromatics

A number of ethynylated aromatic monomers recently have been synthesized which thermally homopolymerize and copolymerize to produce rigid, highly cross-linked polymers with high thermal stability (Tg of about 450 C). On pyrolysis, these polymers lose few volatiles (more than 85 percent char yield) to yield carbon bodies of relatively low porosity. These properties render the ethynylated aromatics of significant interest as matrices for high temperature composites. Incorporation of a SiC particle filler in the matrix improves the rheology of the system and minimizes shrinkage during pyrolysis. Several unidirectional composites have been fabricated combining a graphite or boria-alumina-silica continuous reinforcement with an ethynylated aromatic polymer matrix and SiC filler. Thermogravimetric analysis of composite pyrolysis behavior was used to determine reaction kinetics and to establish a composite fabrication cycle. Composites retained 95 percent of their green weight on pyrolysis. Microstructure of the green and pyrolyzed composites is characterized for materials pyrolyzed at 600 C in vacuum and argon as well as for laminates heated at 1200 C in argon following pyrolysis.

Hurwitz, F. I.↗

NASA NTRS1999

Methane Pyrolysis and Disposing Off Resulting Carbon

Sabatier/Electrolysis (S/E) is a leading process for producing methane and oxygen for application to Mars ISPP. One significant problem with this process is that it produces an excess of methane for combustion with the amount of oxygen that is produced. Therefore, one must discard roughly half of the methane to obtain the proper stoichiometric methane/oxygen mixture for ascent from Mars. This is a waste of hydrogen, which must be brought from Earth and is difficult to transport to Mars and store on Mars. To reduce the problem of transporting hydrogen to Mars, the S/E process can be augmented by another process which reduces overall hydrogen requirement. Three conceptual approaches for doing this are (i) recover hydrogen from the excess methane produced by the S/E process, (ii) convert the methane to a higher hydrocarbon or other organic with a lower H/C ratio than methane, and (iii) use a separate process (such as zirconia or reverse water gas shift reaction) to produce additional oxygen, thus utilizing all the methane produced by the Sabatier process. We report our results here on recovering hydrogen from the excess methane using pyrolysis of methane. Pyrolysis has the advantage that it produces almost pure hydrogen, and any unreacted methane can pass through the S/E process reactor. It has the disadvantage that disposing of the carbon produced by pyrolysis presents difficulties. The goals of a research program on recovery of hydrogen from methane are (in descending priority order): 1) Study the kinetics of pyrolysis to arrive at a pyrolysis reactor design that produces high yields in a confined volume at the lowest possible operating temperature; 2) Study the kinetics of carbon burnoff to determine whether high yields can be obtained in a confined volume at acceptable operating temperatures; and 3) Investigate catalytic techniques for depositing carbon as a fine soot which can be physically separated from the reactor. In the JPL program, we have made significant measurements in regard to goal 1, cursory measurements in regard to goal 2, and would plan to pursue goal 3 if additional resources are secured.

Sharma, P. K.↗

NASA NTRS2012

Volatile Analysis by Pyrolysis of Regolith for Planetary Resource Exploration

The extraction and identification of volatile resources that could be utilized by humans including water, oxygen, noble gases, and hydrocarbons on the Moon, Mars, and small planetary bodies will be critical for future long-term human exploration of these objects. Vacuum pyrolysis at elevated temperatures has been shown to be an efficient way to release volatiles trapped inside solid samples. In order to maximize the extraction of volatiles, including oxygen and noble gases from the breakdown of minerals, a pyrolysis temperature of 1400 C or higher is required, which greatly exceeds the maximum temperatures of current state-of-the-art flight pyrolysis instruments. Here we report on the recent optimization and field testing results of a high temperature pyrolysis oven and sample manipulation system coupled to a mass spectrometer instrument called Volatile Analysis by Pyrolysis of Regolith (VAPoR). VAPoR is capable of heating solid samples under vacuum to temperatures above 1300 C and determining the composition of volatiles released as a function of temperature.

Glavin, Daniel P.↗

NASA NTRS2013

Effects of Nonequilibrium Chemistry and Darcy-Forchheimer Pyrolysis Flow for Charring Ablator

The fully implicit ablation and thermal response code simulates pyrolysis and ablation of thermal protection materials and systems. The governing equations, which include energy conservation, a three-component decomposition model, and a surface energy balance, are solved with a moving grid.This work describes new modeling capabilities that are added to a special version of code. These capabilities include a time-dependent pyrolysis gas flow momentum equation with Darcy-Forchheimer terms and pyrolysis gas species conservation equations with finite rate homogeneous chemical reactions. The total energy conservation equation is also enhanced for consistency with these new additions. Two groups of parametric studies of the phenolic impregnated carbon ablator are performed. In the first group, an Orion flight environment for a proposed lunar-return trajectory is considered. In the second group, various test conditions for arcjet models are examined. The central focus of these parametric studies is to understand the effect of pyrolysis gas momentum transfer on material in-depth thermal responses with finite-rate, equilibrium, or frozen homogeneous gas chemistry. Results indicate that the presence of chemical nonequilibrium pyrolysis gas flow does not significantly alter the in-depth thermal response performance predicted using the chemical equilibrium gas model.

Chen, Yih-Kanq↗

NASA NTRS2016

Magnesium Sulfate as a Key Mineral for the Detection of Organic Molecules on Mars Using Pyrolysis

Pyrolysis of soil or rock samples is the preferred preparation technique used on Mars to search for organic molecules up today. During pyrolysis, oxichlorines present in the soil of Mars release oxidant species that alter the organic molecules potentially contained in the samples collected by the space probes.This process can explain the difficulty experienced by in situ exploration probes to detect organic materials in Mars soil samples until recently. Within a few months, the Curiosity rover should reach and analyze for the first time soils rich in sulfates which could induce a different behavior of the organics during the pyrolysis compared with the types of soils analyzed up today. For this reason, we systematically studied the pyrolysis of organic molecules trapped in magnesium sulfate, in the presence or absence of calcium perchlorate. Our results show that organics trapped in magnesium sulfate can undergo some oxidation and sulfuration during the pyrolysis. But these sulfates are also shown to protect organics trapped inside the crystal lattice and/or present in fluid inclusions from the oxidation induced by the decomposition of calcium perchlorate and probably other oxychlorine phases currently detected on Mars. Trapped organics may also be protected from degradation processes induced by other minerals present in the sample, at least until these organics are released from the pyrolyzed sulfate mineral (700C in our experiment). Hence, we suggest magnesium sulfate as one of the minerals to target in priority for the search of organic molecules by the Curiosity and ExoMars 2018 rovers.

Francois, P.↗

NASA NTRS2021

Pyrolysis Rate and Yield Strength Reduction Incarbon Fiber and Glass Fiber Composites Underreentry Heating Conditions

The behavior of composite materials, specifically carbon fiber reinforced plastic (CFRP) and glass fiber reinforced plastic (GFRP), under reentry conditions poses a problem for space debris reentry risk modeling. Since these materials pyrolyze rather than melt and their different components demise at different rates, modeling their destruction to determine ground impact risk is complex. Modern spacecraft are using these materials in ever-greater quantities owing to their superior strength-to-weight characteristics, and this has required that the orbital debris community improve its understanding of how these materials demise on reentry. The NASA Orbital Debris Program Office undertook an extensive test campaign to better understand the rate at which several types of GFRP and CFRP materials pyrolyze under reentry heating conditions and how that pyrolysis affects the ultimate strength of the material. GFRP with a polyester resin (G10/FR-4) and CFRP with epoxy, cyanate ester, vinyl ester, and phenolic resins were tested. The test campaign was carried out at the Inductively Coupled Plasma (ICP) Torch Facility at the University of Texas at Austin. Because the ICP facility operates in a shirt-sleeve environment, test samples can be changed within seconds or minutes, allowing many samples to be tested in a short period. Two heat flux rates, 20 W/m2 and 30W/m2, and two oxygen concentration conditions, 0% and 2% of atmospheric, were applied to all five types of material. To measure both the char rate and the effect of pyrolysis on the ultimate material strength, two types of test were carried out for each material: a char rate test on a ~10 mm thick sample of material and an in-situ bending stress test of a ~2 mm thick sample of material. Measurements of the char rate showed very similar average pyrolysis front velocity in epoxy resin CFRP as in G10 at 3.6 mm/min and 3.4 mm/min, respectively. However, the total mass loss rate in theG10 was nearly double that of the CFRP at 3.8 g/min and 2.2 g/min, respectively. This result represented a slow ablation rate of carbon fibers in the CFRP at the temperatures encountered in low Earth orbit reentry and a comparatively rapid removal of the glass fibers in G10 due to melting and spallation. Pyrolysis front velocity was more significantly affected by the type of plastic than the type of fiber, with the cyanate ester CFRP samples displaying an average pyrolysis front velocity of only 1.9 mm/min. Similarly, the effect of thermal exposure on the ultimate strength of the material depended heavily on the type of plastic and very little on the type of fiber in the material. Epoxy, vinyl ester, and polyester resins all behaved very similarly, with complete structural failure at between 400 J/g and 600 J/g of specific absorbed heat. Phenolic and cyanate ester resins, on the other hand, displayed a change in structural properties that was only barely measurable with the current apparatus even after the maximum exposure time tested. These data are being incorporated into a numerical model of the ablation and demise of composite materials that will be used to more accurately calculate the ground casualty risk of future spacecraft.

Benton R. Greene↗

DOE OSTI2024

Pyrolysis of high-density polyethylene: Degradation behaviors, kinetics, and product characteristics

Pyrolysis is a promising technology for converting plastic waste into valuable raw materials while offering a potential solution to the global plastic pollution crisis. In this study, the thermal pyrolysis of high-density polyethylene (HDPE) is investigated in a drop tube reactor under nearly isothermal conditions. The impact of reaction temperature and gas/volatile residence time on carbon conversion and product distribution is examined across a range of 500–900°C and 3.6–32.2s, respectively. Non-condensable gas products detected by online mass spectrometry are H 2 , CH 4 , C 2 H 4 , C 2 H 6 , C 3 H 6 , and C 3 H 8 . At elevated temperatures and prolonged residence time, H 2 yield reaches as high as 8.6 wt% of the initial HDPE mass due to intensified cracking reactions of C 2 –C 3 hydrocarbons and long-chain aliphatic compounds. Consequently, pyrolysis tars consist mainly of polycyclic aromatic hydrocarbons (PAHs) with 5–7 rings, accompanied by visible coke deposition within the reactor. HDPE decomposition to volatiles is an endothermic process and it is complete at a temperature between 492°C and 525°C, depending on the heating rate employed, from non-isothermal thermogravimetric analysis and differential scanning calorimetry (TGA-DSC) measurements. The thermal degradation of HDPE pellets follows the two-dimensional nucleation growth model for conversion levels up to 0.8 with an apparent activation energy of 259–270 kJ/mol and a pre-exponential factor of 4.83 × 10 17 –1.37 × 10 19 min -1 , determined from various isoconversional methods such as Flynn-Wall-Ozawa (FWO), Kissinger-Akahira-Sunose (KAS), and Starink, along with Criado's master plots. Further, these findings provide valuable insights into optimizing process parameters and refining reactor design for pyrolysis, which can be integrated with gasification and reforming processes to enhance hydrogen production on a larger scale.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Process Feasibility Analysis of Waste Biomass Valorization to Biochar and Bio-Oil via Slow and Fast Pyrolysis

The United States has abundant biomass and waste feedstock to support the nation's energy addition and affordability targets. Pyrolysis, a thermochemical conversion process, decomposes lignocellulosic feedstocks into liquid, solid, and gaseous fuels that can contribute to the domestic production of biofuels, biopower, and bioproducts. Growing private sector interest in this technology is a key motivation for this comprehensive techno-economic process modeling analysis of a respective biorefinery that includes feedstock preprocessing, slow and fast pyrolysis, and product separation to bio-oil, biochar, and syngas hydrocarbons. Results show that biochar from slow pyrolysis could achieve minimum selling prices (MSPs) of $\$$188-$\$$260/t, competitive with reported market values, while bio-oil from fast pyrolysis is estimated to yield MSPs of $\$$6.49-$\$$9.68/GGE, approximately twice conventional fuel benchmarks. Sensitivity analysis identifies feedstock cost, product yield, and scale as primary cost drivers, while scenarios involving biochar carbon credits and high value applications may substantially improve economics. Overall, these results suggest that continued innovation in feedstock logistics, process integration, and market development will be critical to achieving economically viable and scalable bioproducts.

09 BIOMASS FUELS↗

DOE OSTI2025

Analysis of Tar and Oil Derived from Pyrolysis and Copyrolysis of Waste Plastics and Biomass

Pyrolysis has been proposed as a potential technology for managing the growing volume of plastic waste generated worldwide. Co-pyrolysis of plastic waste with biomass is a promising technology for generating fuel and chemical products. However, this process generates tar as a waste product. The chemical properties of this tar have yet to be thoroughly analyzed. Further, this study presents the results of gas chromatography–mass spectrometry (GC–MS), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) of oil and tar obtained from the pyrolysis of pure plastics including high-density polyethylene (HDPE), low-density polyethylene (LDPE), polyethylene (PE), polystyrene (PS), and plastic-biomass mixtures. GC–MS analysis revealed the presence of C 7 –C 37 carbon-containing hydrocarbons, which include alkanes and alkenes as the dominant products. FTIR data revealed the presence of various functional groups, including alcohols, aldehydes, ketones, and carboxylic acids, indicating the complexity of the pyrolysis and copyrolysis oil obtained from waste plastics and biomass. TGA data show that tar from all four plastics has a higher decomposition rate, suggesting the presence of heavier hydrocarbons compared with their corresponding oils. This research will be of interest to researchers looking to advance the study of plastic and biomass waste management.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

A Kinetic Model-Driven Techno-Economic Analysis of Plastic Pyrolysis: Linking Process Dynamics to Economic Viability

This study employs a kinetic model integrated into Aspen Plus to predict pyrolysis product distribution under various conditions. A techno-economic assessment calculated the minimum selling price (MSP) of pyrolysis oil under different operating conditions for the baseline capacity of 100 kta, and across eight processing capacities ranging from 30 to 150 kta. The lowest MSP under the baseline capacity is estimated at $\$$420/ton, which is 33% lower than the 2023 average US crude oil price ($\$$74.6/bbl, equivalent to $\$$634/ton based on the density of pyrolysis oil). Under Monte Carlo simulation, accounting for variability in key economic and technical parameters, the mean MSP is estimated at $\$$1137/ton. The economic viability depends on feedstock price remaining below $\$$320/ton, defining the break-even feedstock price threshold. Sensitivity analysis further identifies capital investment and transportation cost as key economic drivers. Capacities beyond 90 kta show limited economies of scale benefits. Reducing product storage time cuts capital costs by 7% but raises operational risk. Uncertainty analysis suggests the economic feasibility of pyrolysis oil is unlikely to compete with crude oil without policy incentives.

petrochemicals↗

DOE OSTI2025

Pyrolysis Reactions of (2-Chloroethyl)benzene

Pyrolysis of polyvinyl chloride (PVC) is considered an alternative to traditional, mechanical methods of recycling. However, there is insufficient research conducted on the thermal decomposition pathways of PVC, particularly the fate of chlorinated hydrocarbons generated during the chemical recycling process. One significant product from the pyrolysis of PVC is (2- chloroethyl)benzene. Using a hyperthermal tubular reactor and matrix-isolation FTIR techniques, the pyrolysis products of gasphase (2-chloroethyl)benzene were identified. Following pyrolysis at 1400 K, the FTIR spectra indicated the formation of HCl, styrene, phenylacetylene, benzene, vinylacetylene, acetylene, propyne, ethylene, and propargyl radical.

Aromatic compounds↗

NASA NTRSDate not supplied

Analysis of Pyrolysis Products from Ablative Thermal Protection Systems

NASA’s state-of-the-art ablative materials are composed of a three-dimensional network of carbon fibers impregnated with polymers that dissipate thermal energy through pyrolysis. A fundamental understanding of the decomposition mechanisms and pyrolysis product distributions of various classes of polymers is instrumental in the design of new ablative materials. Furthermore, innovative experiments are essential to the continuous modernization of material response models by providing high-fidelity data. Thus, an apparatus has been designed to measure pyrolysis products from polymers and composite materials by implementing in-situ mass spectrometric techniques. Initial results from experiments performed on siloxane resins and a common phenolic resin will be discussed. Both classes of polymers exhibit heating-rate-dependent decomposition mechanisms. At the onset of heating, phenolic polymers decompose through competitive reactions to form gaseous products and a carbonaceous char. Gas phase products of phenolic resins are typically composed of molecular hydrogen, water, and aromatic hydrocarbons. Pyrolysis products from siloxane polymers include molecular hydrogen, small molecules, and cyclic oligomers from the polymer backbone.

Pyrolysis↗

NASA NTRSDate not supplied

Analysis of Pyrolysis Products from Ablative TPS

Pyrolysis↗