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NASA NTRSDate not supplied

Scaling of Liquefaction Systems and the Effects of Gravity

Recent exploration initiatives both by NASA and others have produced interest in the liquefaction of fluids produced through in-situ processes on the surfaces of the Moon and Mars. Liquefaction of fluids in cryogenic temperatures is routinely done at large scale for terrestrial uses, but these processes do not necessarily scale down in an economical or technologically feasible manner for the anticipated rates of initial Lunar or Martian production plants. To understand appropriate processes and scaling parameters, various options should be considered. A multi-center team at NASA considered multiple different refrigeration cycles and refrigeration integration methodologies as well as how these might fit into early liquefaction plants. These studies resulted in the conclusion that integrating the tubing on the storage tank wall (for both structural and heat spreading reasons), preferably the tank which will actually use the fluid, is the nearest path forward. Given that assumption on the general framework of the liquefaction system, there are several different heat transfer mechanisms to consider from a scaling perspective. These include forced convection heat removal to the refrigeration system (or cryocooler), conduction through the tank wall heat exchanger, and condensation (with some natural convection) on the inner tank wall. Analysis of these mechanisms shows that while there is some sensitivity to gravitational level, that within the bounds of current interest (Lunar and Martian applications), this sensitivity does not dominate the liquefaction application. While there will be some effect, perhaps in a limiting manner as the tanks approach some high fill level, system level testing on the Earth should suffice for the performance prediction and demonstration of liquefaction operations as applicable to Lunar and Martian applications. However, as one approaches orbital conditions, this general approach to liquefaction will not be appropriate as the scaling of the heat transfer mechanisms is not appropriate. At this point, other approaches will need to be developed and demonstrated in the micro-gravity environment.

Cryogenics↗

NASA NTRSDate not supplied

Liquefaction of Cryogenic Fluids for Production and Storage of Commodities on Extra-Terrestrial Surfaces

The Cryogenic Fluid In-situ Liquefaction for Landers (CryoFILL) activity has been investigating concepts for the liquefaction of cryogenic fluids produced on the surface of the Moon and Mars. CryoFILL consists of four activities: liquid nitrogen liquefaction testing that was completed in 2019, liquid oxygen liquefaction testing planned to begin in early 2022, fiber-optic sensor temperature measurement system development, and lightweight vacuum jacketed systems designed for the atmosphere of Mars. Additional activities include the development and validation of numerical modeling systems at three stages: thermodynamic models of the liquefaction process for basic energy/mass estimates, nodal models to predict liquefaction tank system level performance, and computational fluid dynamics to assess fluid phenomena occurring within the tank, specifically condensation and stratification within the ullage. These developments form a combined liquefaction and storage solution to support Lunar and Martian exploration. Key testing results from liquid nitrogen testing as well as plans for liquid oxygen testing will be discussed including key sensitivities from analytical evaluation of completed test results. Progress on the development and improvements on fiber optic sensor testing and developments will also be provided. Finally, work on the progress of the lightweight vacuum jacketed systems being co-developed by NASA and industry will be summarized.

Liquefaction↗

NASA NTRS2023

Cryogenic Fluid In-Situ Liquefaction for Landers: Prototype Demonstration

As the advancement of In-Situ Resource Utilization concepts and systems continue to develop, applicable technology development and maturation continues in parallel. While there are many different ways to use the resources found on other bodies, one of the most prevalent suggested applications is the manufacturing of propellants. One of the key technologies for the eventual use of these propellant production based ISRU systems is the liquefaction and storage of the produced propellants. The most mentioned propellant combinations include oxygen-hydrogen and oxygen-methane. The liquefaction of oxygen in these systems will be different than oxygen liquefaction systems on Earth, which mainly revolves around the distillation of air. These systems have been developed conceptually and many of the components have been previously tested or are in development. However, the need to demonstrate the system level operations still exists. The demonstration of a prototypical oxygen liquefaction system using tube-on-tank broad area cooling was completed to better understanding system level operations during liquefaction activities. Demonstration testing included system performance determination, constant liquefaction demonstrations, and transient liquefaction demonstrations. The demonstrations showed the operational capabilities of the tube-on-tank system with an integrated cryocooler. Additional testing explored subsurface vs ullage introduction of the gaseous oxygen flow stream as well as demonstrating a novel fiber optic sensor that measured the temperature gradients along the fluid center line within the tank.

ISRU↗

NASA NTRSDate not supplied

Cryogenic Fluid In-Situ Liquefaction for Landers: Prototype Demonstration

ISRU↗

DOE OSTI2020

Hydrothermal liquefaction of Cyanidioschyzon merolae and Salicornia bigelovii Torr.: The interaction effect on product distribution and chemistry

Hydrothermal liquefaction (HTL) has proven to be a promising technology for processing wet biomass into valuable biofuel intermediates. We investigated the influence of HTL process parameters on the individual and co-liquefaction of Salicornia bigelovii Torr. (SL) and Cyanidioschyzon merolae (CM) biomass and their respective product properties and characteristics. SL and CM biomasses were subjected to HTL conditions of process temperatures (250–350 °C), 10 wt% solid loading, 30 min reaction time, and co-liquefaction ratios (80–20, 50–50, 20–80, CM-SL, respectively). The individual maximum HTL biocrude yields for CM (34.63 wt%) and SL (7.63 wt%) were obtained at 300 °C. In both cases, biocrude oils had a higher carbon and hydrogen content relative to those of the original biomass. The HHV (higher heating value) values for the biocrude samples ranged from 24.2 to 33.12 MJ/kg, which were significantly higher than those of the original biomasses. A positive synergistic effect was observed during the co-liquefaction of two biomasses, where the experimental yield of biocrude oil was higher than the theoretical value. During the co-liquefaction experiments, a maximum biocrude yield of 32.95 wt% was obtained at 300 °C and 80–20 CM-SL biomass mix ratio. Co-liquefaction led to an increase in the energy content of the co-liquefied biocrude oil and a higher energy recovery rate. Finally, the properties of HTL products and biomasses were determined with TGA, CHN elemental analyzer, GC/MS, bomb calorimeter, HACH Spectrophotometer, and ICP OES.

09 BIOMASS FUELS↗

NASA NTRSDate not supplied

Comparison of Oxygen Liquefaction Gaseous Oxygen Injection via Ullage and Dip Tube

The Cryogenic Fluid In-situ Liquefaction for Landers (CryoFILL) testing demonstrated constant and transient oxygen liquefaction in a scaled lander tank integrated with an industrial cryocooler. Early in the test series, two methods for injecting gaseous oxygen into the test tank were ran under similar constant liquefaction conditions for comparison. Gaseous oxygen was either injected directly from the lid into the ullage or bubbled up through the liquid using a dip tube that extends to the bottom of the test tank. The direct comparison of these gaseous oxygen injection methods for constant liquefaction indicated ullage injection provided a greater liquefaction rate than injection via a dip tube. Injection through the ullage was subsequently selected as the nominal injection method for the CryoFILL test series. The comparison of the two injection methods will be highlighted with a discussion of what may cause the variation in liquefaction rate.

Cryogenic Fluid Management↗

NASA NTRSDate not supplied

Cryogenic Fluid In-Situ Liquefaction for Landers: Prototype Demonstration

As the advancement of In-Situ Resource Utilization concepts and systems continue to develop, applicable technology development and maturation continues in parallel. While there are many different ways to use the resources found on other bodies, one of the most prevalent suggested applications is the manufacturing of propellants. One of the key technologies for the eventual use of these propellant production based ISRU systems is the liquefaction and storage of the produced propellants. The most mentioned propellant combinations include oxygen-hydrogen and oxygen-methane. The liquefaction of oxygen in these systems will be different than that on Earth, which mainly revolves around the distillation of air. These systems have been developed conceptually and many of the components have been previously tested or are in development. However, the need to demonstrate the system level operations still exists. The demonstration of a prototypical oxygen liquefaction system using tube-on-tank broad area cooling was completed to better understanding system level operations during liquefaction activities. Demonstration testing included system performance determination, constant liquefaction demonstrations, and transient liquefaction demonstrations. The demonstrations showed the operational capabilities of the tube-on-tank system with an integrated cryocooler. Additional testing explored subsurface vs ullage introduction of the gaseous oxygen flow stream as well as demonstrating a novel fiber optic sensor that measured the temperature gradients along the fluid center line within the tank.

ISRU↗

DOE OSTI2023

Techno-economic assessment and life cycle assessment of three potential pathways for biomass liquefaction

Biomass liquefaction can enhance corn-stover slurry transportation by reducing yield stress and overall viscosity, easing biomass handling, especially for slurries at high solids loading (≥30 % (w/v). Implementing a liquefaction process at the front-end of the biorefinery could reduce downtime caused by equipment fouling. Furthermore, liquefaction reduces process complexity by transforming high fiber mass into a pumpable slurry. Three scenarios for liquefaction of corn stover pellets: enzyme process, enzyme mimetic process, and a combined process of enzyme and enzyme mimetic were assessed. The ideal process will have the best performance-to-cost ratio, with minimal impact on the environment. Techno-economic and life-cycle analyses were used to understand the economic and environmental effects of the three liquefaction scenarios and to determine if one or more can achieve cost parity. Here, results show that the enzyme process had the best performance in terms of cost and emissions (gCO 2 -equivalent/kg slurry)compared to the other scenarios.

09 BIOMASS FUELS↗

DOE OSTI2021

Oregon Roadway CSZ Liquefaction and Landslide Impact Screening Analysis

The roadway transportation routes and the surrounding environments in Oregon will be subject to ground acceleration and potential associated deformation due to the propagation of waves of energy during a Cascadia Subduction Zone (CSZ) earthquake. Linear features such as highways may be subject to partial or complete disruption of their function resulting from ground deformations at and along the roadway. A potential source of these disruptions associated with a CSZ event are landslides and liquefaction in the soils along and beneath the highways and local roadways. The construction of the Oregon roadway system and urban development have occurred largely along the banks of the rivers—those along the Pacific coast, and along the valleys throughout the Oregon Coast Range and Cascade Mountains. These locations also represent areas where landslides and liquefaction have occurred historically, or may potentially occur in the future, presenting a significant vulnerability for the roadway system and dependent post-CSZ earthquake emergency response and recovery effort. Many of the Oregon areas with landslide- and liquefaction-prone soils have the potential to impact roadway transportation routes after a major earthquake causing delays in establishing routes to transport emergency response personnel and resources to impacted areas and communities. This report presents methods used to project the impacts that CSZ earthquake-induced landslides and liquefaction may have on roadways across Oregon. First, this report presents an approach for estimating the risk of landslides to Oregon roadways, and determining approximate reopening times. Second, this report presents a similar approach for estimating the risk of liquefaction-induced ground displacements to roadway pavements, also resulting in approximate reopening times for roadway segments. The outcomes of these two ground failure analyses serve as inputs to a broader analysis of CSZ earthquake impacts to Oregon’s surface transportation system and its ability to support post-disaster response and recovery activities, as part of the Oregon Transportation Systems Regional Resiliency Assessment Program project (CISA 2021).

58 GEOSCIENCES↗

NASA NTRS2019

Liquid Nitrogen Testing of ISRU Liquefaction Methods in Unsteady Applications

To enable NASA’s planned long duration missions, the agency is putting emphasis on reusable cryogenic systems. Such systems will require replenishing of cryogens on-orbit via a cryogenic tanker or refueling depot, and potentially on the lunar or Martian surfaces with the utilization of in-situ resources. Surface replenishing requires the in-situ production of gaseous oxygen (and hydrogen if on the lunar surface), followed by liquefaction and storage. Funded by NASA’s Advanced Exploration Systems, and managed under the Advanced Cis-Lunar Space Capability Project, the Cryogenic Fluid In-Situ Liquefaction for Landers (CryoFILL) multi center team was formed to develop a liquefaction and storage system that is efficient, reliable and scalable. This presentation will demonstrate the liquefaction and storage of “In-Situ like” propellant via a Tube-On-Tank Heat Exchanger integrated with Active Cooling (cryocooler) (verify proof of concept and obtain relevant data for model validation) and gather lessons learned from “brassboard” testing which will be applied to future liquefaction system prototype testing, then eventually to an end-to-end demonstration.

Stephens, J. R.↗

DOE OSTI2020

The effect of moisture on hydrocarbon-based solvent liquefaction of pine, cellulose and lignin

In this report we examined the effect of moisture on the solvent liquefaction of loblolly pine, cellulose, and lignin in tetralin at 280 °C and pressures ranging from 15 to 70 bar. Solvent liquefaction experiments were conducted in a quasi-batch reactor capable of continuous pressure control and external vapor condensation. Moisture was varied by the controlled addition of de-ionized water. Control over the system pressure subsequently impacted the removal of water vapor from the reactor. Liquid yield decreased by 25, 21, and 35 wt%, for pine, cellulose, and lignin, respectively, when moisture content was increased from 1 to 50 wt% at 42 bar. Humins were observed in the solid residue from liquefaction of wet cellulose. Wet lignin yielded a substantial amount of solid residue compared to dry lignin with a corresponding decrease in total phenolic monomer production. It was concluded that the ionic dissociation of water was an important factor in loss of liquid yield in the presence of water. Although water was less than 20 wt% of the solvent loading in these experiments, it strongly influenced the liquefaction of biomass and biomass components.

09 BIOMASS FUELS↗

NASA NTRS2017

Comparison of Oxygen Liquefaction Methods for Use on the Martian Surface

In order to use oxygen that is produced on the surface of Mars from In-Situ production processes in a chemical propulsion system, the oxygen must first be converted from vapor phase to liquid phase and then stored within the propellant tanks of the propulsions system. There are multiple ways that this can be accomplished, from simply attaching a liquefaction system onto the propellant tanks to carrying separate tanks for liquefaction and storage of the propellant and loading just prior to launch (the way that traditional rocket launches occur on earth). A study was done into these various methods by which the oxygen (and methane) could be liquefied and stored on the Martian surface. Five different architectures or cycles were considered: Tube-on-Tank (also known as Broad Area Cooling or Distributed Refrigeration), Tube-in-Tank (also known as Integrated Refrigeration and Storage), a modified Linde open liquefaction/refrigeration cycle, the direct mounting of a pulse tube cryocooler onto the tank, and an in-line liquefier at ambient pressure. Models of each architecture were developed to give insight into the performance and losses of each of the options. The results were then compared across eight categories: Mass, Power (both input and heat rejection), Operability, Cost, Manufacturability, Reliability, Volumility, and Scalability. The result was that, given the current state of technology maturity, Tube-on-Tank architectures were the most attractive solution, closely followed by Tube-in-Tank. As a result of this technical analysis and other factors, NASA has determined to focus its Martian surface liquefaction activities and technology development on Tube-on-Tank liquefaction cycles.

Cryogenic propellants↗

NASA NTRSDate not supplied

Analysis of Oxygen Liquefaction with Transient Flow Rates for ISRU Systems

Human occupation of lunar and Martian surfaces requires in-situ resource utilization (ISRU) to create a sustainable environment with the limited resources available in space. Fuel and oxidizer generation is essential for developing a refueling capability for spacecraft, significantly reducing the propellant mass required for landing. Liquefaction systems are a key step in producing and storing cryogenic liquids such as oxygen, hydrogen, and methane. All those fluids are critical to propulsion, life support, and other spacecraft systems. NASA has previously confirmed the presence of water on the Moon and an electrolysis process can be used to separate the oxygen from the hydrogen molecules. Oxygen has also been found within lunar regolith and can be separated through ISRU processes. The extracted oxygen gas can then be liquefied inside a storage tank with tube-on-tank heat exchangers for future use as an oxidizer for propellants. While steady state liquefaction performance is easy to model, power limitations and cyclical environments caused by the change in Sun exposure between day and night periods potentially call for transient operations. The following analysis was performed using the Thermal Desktop software to investigate how various transient gaseous oxygen (GOX) flow rates impact the production and storage of liquid oxygen (LOX) in a 1-g liquefaction system. Variations of sinusoidal and exponential step functions were selected to model potential GOX flow rates that could be experienced by ISRU systems on lunar or Martian surfaces. This early computational analysis provides some insight on how transient operations impact oxygen liquefaction systems and helps illustrate operational questions to explore experimentally throughout the design process.

Cryogenic Fluid Management↗

NASA NTRSDate not supplied

Transient Liquefaction on the Lunar or Martian Surface Operational Demonstration

As developments of local production of cryogenic fluids on the Lunar or Martian Surface progress, it is important to understand transient system responses to help with the balancing of process plant power and understanding system level operations. During the Cryogenic Fluid In-situ Liquefaction for Landers (CryoFILL) testing, a series of transient oxygen liquefaction tests were completed. These tests included varying liquefaction flow rate, environmental temperature, tank fill level, and effective cryocooler lift while allowing the tank pressure to respond to the input controls. An additional transient test was run at the 90% fill level to determine the impact of injecting the gaseous oxygen at the bottom of the tank, allowing the vapor to bubble up through the liquid. Tests were run in a cyclical nature varying one variable at a time. The control variable was set in a manner to increase tank pressure for a period of time and then subsequently changed in a manner to decrease the tank pressure back to its original value with multiple cycles run for all tests. Tank pressure and system temperature responses were tracked as a function of time with an emphasis on repeatability. Results indicate that of the four variables tested, the environmental temperature is the least important. As expected, the bubbling of the liquefaction gas significantly decreased the pressurization and depressurization rates in the tank at the 90% full level.

Liquefaction↗

DOE OSTI2021

Microalgae to biofuels through hydrothermal liquefaction: Open-source techno-economic analysis and life cycle assessment

Hydrothermal liquefaction is a promising conversion technology in algae biofuel research due to its ability to agnostically convert proteins, carbohydrates, and lipids to biocrude. The high-temperature conditions that define this conversion process require the material to maintain a subcritical liquid state, which complicates the assessment of accurate thermochemical properties due to the required pressure. To clarify this issue, this work compares the estimated performance of algal hydrothermal liquefaction between different thermodynamic models. A process model was developed in Aspen Plus from a robust assessment of current literature. Techno-economic assessment and life-cycle assessment metrics are derived from this model and used as key performance indicators. The baseline fuel price contribution of hydrothermal liquefaction is $0.45 per liter gasoline equivalent. Independently decreasing the temperature from 350 °C to 260 °C while maintaining yield reduces the conversion cost by 19%, illustrating the importance of understanding the high-temperature thermodynamics of the system. Different thermodynamic property models can vary fuel conversion cost results by $0.07 per liter gasoline equivalent. The baseline global warming potential is +23 g CO 2 eq MJ -1 and the net energy ratio is 0.30. Environmental metrics beyond global warming potential and net energy ratio are also discussed for the first time. Uncertainties in conversion performance are bounded through a scenario analysis that manipulates parameters such as product yield and nutrient recycle to produce a range of economic and environmental metrics. The report is supplemented with an open source model to support future hydrothermal liquefaction assessments and accelerate the development of commercial-scale systems.

09 BIOMASS FUELS↗

NASA NTRS1996

Liquefaction Of Coal With Surfactant And Disposable Catalyst

Fuels derived from coal more competitive with petroleum products. Improved coal-liquefaction process exploits synergistic effects of disposable iron oxide catalyst and cheap anionic surfactant. Efficiency of conversion achieved in significantly higher than efficiencies obtained with addition of either surfactant or catalyst alone. No costly pretreatment necessary, and increase in conversion achieved under processing conditions milder than those used heretofore in liquefaction of coal. Quality of distillates obtained after liquefaction in process expected superior to distillates obtained after liquefaction by older techniques.

Hickey, Gregory S.↗

DOE OSTI2021

Supplemental dietary full-fatted and defatted Desmodesmus sp. exerted similar effects on growth performance, gut health, and excreta hydrothermal liquefaction of broiler chicks

This study determined effects of full-fatted (C046, 41% crude protein) and lipid extracted (LEA, 39% crude protein) microalgae Desmodesmus sp. on growth performance, gut health, and excreta hydrothermal liquefaction of broiler chickens. Two experiments were conducted by feeding day-old Cornish male chicks: 1) a corn-soybean meal basal diet (control) 2) control +5% C046, or 3) control +5% LEA for 2 weeks. Growth performance was measured weekly in both experiments. Blood, liver, and duodenum samples of chickens were collected for biochemical analyses, and excreta samples were collected for hydrothermal liquefaction (300 °C, 60 min) at the end of Experiment 2. Compared with the control, supplemental dietary C046 and LEA enhanced average daily gain (13% to 40%, p < 0.05) in both experiments, and improved feed efficiency (15% and 11%, p < 0.01) in Experiment 2. The C046 and LEA diets enhanced the duodenum (19% to –2 fold, p < 0.05), but decreased the liver (17 to 78%, p < 0.05) mRNA abundances of interleukins-1, 6 and 8 and (or) tumor necrosis factor-α, respectively, compared with the controls. Meanwhile, the two types of biomass enhanced the protein amounts of claudin-1 in the duodenum (5–34%, p < 0.05) than the controls. Hydrothermal liquefaction of the excreta derived from the three diets showed no major differences in total bio-crude oil (average of 23%), hydrochar yield (average of 12%), or elemental compositions. However, the heating values of the resultant two bio-crude oils from the microalgae-fed chicken excreta (average of 34 MJ/kg) were 16% greater than those from the control chickens (29 MJ/kg). In conclusion, supplementing the full- and de-fatted Desmodesmus sp. microalgal biomass in the starter diets for broiler chickens produced largely similar improvements of growth performance, gut health, and excreta-derived oil quality.

09 BIOMASS FUELS↗

DOE OSTI2021

Use of a Lewis acid, a Brønsted acid, and their binary mixtures for the hydrothermal liquefaction of lignocellulose

The main objective of the present study is to investigate the effect of a Lewis acid, Brønsted acid, and their combined use on the hydrothermal liquefaction of lignocellulosic biomass. Hydrothermal liquefaction of teak wood was conducted at 250, 300 and 350 °C for 15, 30 and 60 min. Hydrothermal liquefaction of teak wood was carried out at 300 °C for 30 min (the best optimum conditions) without and with the use of Mg(ClO 4 ) 2 , HClO 4 , and HClO 4 /Mg(ClO 4 ) 2 at various loadings (2–10 mmol/15 g wood). The highest bio-oil yield was obtained with the non-catalytic run. All tested catalysts have negative effect on bio-oil yields. The bio-oil yields generally decreased with increasing the catalyst loadings. The deoxygenation degree in bio-oils changed depending on the type of catalyst and loading. A high degree of de-oxygenation took place with Mg(ClO 4 ) 2 catalysts. An increased catalyst loading led to decreased aromatic contents of bio-oils catalyzed by either Mg(ClO 4 ) 2 or HClO 4 . The use of a catalyst increased total naphtha fractions in bio-oils. The highest heating value of the bio-oil was estimated to be approximately 30 MJ/kg. Gas chromatography–mass spectrometry analysis revealed that the bio-oils from the non-catalytic and catalytic runs contained aldehydes, ketones, phenols, acids, esters and alcohols. Furthermore, the relative yields of the oxygenated compounds were affected by catalyst type.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗