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Title: Hydrogen Production via a Commercially Ready

Abstract

The commercial stainless steel (SS) porous substrate (i.e., ZrO{sub 2}/SS from Pall Corp.) was evaluated comprehensively as substrate for the deposition of the CMS membrane for hydrogen separation. The CMS membrane synthesis protocol we developed originally for the ceramic substrate was adapted here for the stainless steel substrate. Unfortunately no successful hydrogen selective membranes had been prepared during Yr I of this project. The characterization results indicated two major sources of defect present in the stainless steel substrate, which may contribute to the poor CMS membrane quality. They include (i) leaking from the crimp boundary of the stainless steel substrate, and (ii) the delamination of the ZrO{sub 2} layer deposited on the stainless steel substrate during CMS membrane preparation. Recently a new batch of the stainless steel substrate (as the 2nd generation product) was received from the supplier. Our characterization results confirm that leaking of the crimp boundary no longer exists. The thermal stability of the ZrO{sub 2}/stainless steel substrate under the CMS membrane preparation condition will be evaluated during the remaining period of the project. Our goal here is to determine the suitability of the 2nd generation ZrO{sub 2}/SS as substrate for the preparation of the CMS membrane formore » hydrogen separation by the end of this project period.« less

Authors:
Publication Date:
Research Org.:
Media & Process Technology
Sponsoring Org.:
USDOE
OSTI Identifier:
909179
DOE Contract Number:
FC26-03NT41852
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 08 HYDROGEN; CERAMICS; DEFECTS; DEPOSITION; HYDROGEN; HYDROGEN PRODUCTION; MEMBRANES; STABILITY; STAINLESS STEELS; STEELS; SUBSTRATES; SYNTHESIS

Citation Formats

Paul K. T. Liu. Hydrogen Production via a Commercially Ready. United States: N. p., 2007. Web. doi:10.2172/909179.
Paul K. T. Liu. Hydrogen Production via a Commercially Ready. United States. doi:10.2172/909179.
Paul K. T. Liu. 2007. "Hydrogen Production via a Commercially Ready". United States. doi:10.2172/909179. https://www.osti.gov/servlets/purl/909179.
@article{osti_909179,
title = {Hydrogen Production via a Commercially Ready},
author = {Paul K. T. Liu},
abstractNote = {The commercial stainless steel (SS) porous substrate (i.e., ZrO{sub 2}/SS from Pall Corp.) was evaluated comprehensively as substrate for the deposition of the CMS membrane for hydrogen separation. The CMS membrane synthesis protocol we developed originally for the ceramic substrate was adapted here for the stainless steel substrate. Unfortunately no successful hydrogen selective membranes had been prepared during Yr I of this project. The characterization results indicated two major sources of defect present in the stainless steel substrate, which may contribute to the poor CMS membrane quality. They include (i) leaking from the crimp boundary of the stainless steel substrate, and (ii) the delamination of the ZrO{sub 2} layer deposited on the stainless steel substrate during CMS membrane preparation. Recently a new batch of the stainless steel substrate (as the 2nd generation product) was received from the supplier. Our characterization results confirm that leaking of the crimp boundary no longer exists. The thermal stability of the ZrO{sub 2}/stainless steel substrate under the CMS membrane preparation condition will be evaluated during the remaining period of the project. Our goal here is to determine the suitability of the 2nd generation ZrO{sub 2}/SS as substrate for the preparation of the CMS membrane for hydrogen separation by the end of this project period.},
doi = {10.2172/909179},
journal = {},
number = ,
volume = ,
place = {United States},
year = 2007,
month = 3
}

Technical Report:

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  • The porous stainless steel substrate commercially available from Pall offers great potential for large-scale membrane based high temperature gas separations. Our proposed project involves the deposition of the M&P carbon molecular sieve-based hydrogen membrane on AccuSep substrate as a membrane to reactor water-gas-shift reaction. However, the AccuSep substrate was originally designed for liquid phase applications . During the 1st half, this commercial substrate has been modified and improved with regard to its surface topography and end seals. The substrate is now suitable for the deposition of the CMS membrane for hydrogen separation according to the characterization we preformed. In addition,more » 40{angstrom} Al{sub 2}O{sub 3} membrane layers have been deposited on the improved AccuSep substrate successfully. The SEM, EDX and pore size distribution analysis indicate that the 40{angstrom} membrane is extremely thin, and defect free with a narrow pore size distribution around 40{angstrom} primarily. As the above results suggest, we have made significant progress in preparing a high quality nominal 40{angstrom} (actually 50{angstrom}) layer on the Pall substrate. During the 2nd half of Year 1, we will (1) continue this development work with a focus on eliminating the high pore size peak and (2) begin the CMS layer deposition on the 40{angstrom} deposited AccuSep.« less
  • During the 2nd half of Year I, we continued the development of the microporous ceramic layer as a transition layer for the deposition of the carbon molecular sieve membrane on the stainless steel substrate offered by Pall Corp. Based upon the positive result from the feasibility study conducted in the 1st half of Year I, our activities in this period focused on eliminating the high pore size peak and the minimization of defect. A microporous ceramic layer with 40A pore size and <1% initial flow have been successfully prepared. Further, this modified membrane has demonstrated excellent thermal stability, <1% initialmore » flow after the 5 thermal cycles. In addition we began the CMS layer deposition on the AccuSep with the ceramic transition layer. The CMS membranes fired at the low temperature range demonstrate an excellent hydrogen permeance, up to >5 m{sup 3}/m{sup 2}/hr/bar, with the selectivity of {approx}20 for H{sub 2}/N{sub 2}. The extremely high permeance is indicative of the extremely thin CMS membrane layer, which becomes possible as a result of the uniform and defect free transition layer. This could be an ideal membrane for hydrogen recovery applications where the hydrogen permeance is the primary concern. Presently we are actively pursuing the intermediate temperature firing to enhance the selectivity to above this range without sacrificing too much permeance.« less
  • Single stage low-temperature-shift water-gas-shift (WGS-LTS) via a membrane reactor (MR) process was studied through both mathematical simulation and experimental verification in this quarter. Our proposed MR yields a reactor size that is 10 to >55% smaller than the comparable conventional reactor for a CO conversion of 80 to 90%. In addition, the CO contaminant level in the hydrogen produced via MR ranges from 1,000 to 4,000 ppm vs 40,000 to >70,000 ppm via the conventional reactor. The advantages of the reduced WGS reactor size and the reduced CO contaminant level provide an excellent opportunity for intensification of the hydrogen productionmore » process by the proposed MR. To prepare for the field test planned in Yr III, a significant number (i.e., 98) of full-scale membrane tubes have been produced with an on-spec ratio of >76% during this first production trial. In addition, an innovative full-scale membrane module has been designed, which can potentially deliver >20 to 30 m{sup 2}/module making it suitable for large-scale applications, such as power generation. Finally, we have verified our membrane performance and stability in a refinery pilot testing facility on a hydrocracker purge gas. No change in membrane performance was noted over the >100 hrs of testing conducted in the presence of >30% H{sub 2}S, >5,000 ppm NH{sub 3} (estimated), and heavy hydrocarbons on the order of 25%. The high stability of these membranes opens the door for the use of our membrane in the WGS environment with significantly reduced pretreatment burden.« less
  • One of the technical barriers for ceramic membranes is its scale up potential. The conventional ceramic membranes/modules originally developed for liquid phase applications are costly and not suitable for high temperature applications. One of the objectives under this project is the development of a ceramic membrane/module, which is economical and suitable for high temperature applications proposed under this project (200-300 C). During this period, we initiated the fabrication of a prototype ceramic membrane module which can be (1) qualified for the proposed application temperature, and (2) cost acceptable for large scale applications. A prototype ceramic membrane bundle (3-inch diameter andmore » 35-inch L) has been prepared, which passes the temperature stability requirement. It also meets the low end of the burst pressure requirement, i.e., 500-750 psi. In the next period, we will continue the improvement of this prototype module to upgrade its burst pressure to 1000 to 1500 psi range. In addition, bench-top experimental study has been conducted in this period to verify satisfactorily the simulated results for the process scheme developed in the last report, which took into the consideration of streamlining the pre- and post-treatment. The sensitivity analysis indicates that membrane surface area requirement is a key operating parameter based upon the criteria of the CO conversion, hydrogen recovery and CO impurity level. A preliminary optimization study has been performed in this period based upon the key operating parameters determined above. Our result shows that at 40 bar feed pressure a nearly complete CO conversion and >95% hydrogen recovery can be achieved with the CO impurity level at {approx}3500 ppm. If the hydrogen recovery ratio is lowered, the CO impurity level can be reduced further. More comprehensive optimization study will be performed in the 2nd half of Yr III to focus on the reduction of the CO impurity level with a reasonable hydrogen recovery ratio.« less