Characterization of the surfaces of single-walled carbon nanotubes using alcohols and hydrocarbons: a pulse adsorption technique

A pulse mass analyzer was used to study the vapor phase adsorption of organic compounds on single-walled carbon nanotubes and chemically modified/oxidized SWCNTs. The change in mass of a packed bed of adsorbent held at 200 °C was observed following the injection of a pulse of an organic compound from the series: ethanol, iso-propanol, cyclohexane, cyclohexene, benzene, or n-hexane. The relative strength of adsorption was obtained by the mass increase resulting from injection of the pulse and by the time required for desorption. This time was broken into the transit time to reach the end of the bed and the half-time for return from peak to baseline. Hexane was the most strongly held compound of the organic sequence. Oxidative purification of a raw nanotube sample produced a less hydrophobic surface. The effect of the purification was reversed by thermolysis at 700 °C, which removed oxygenated functional groups and increased the affinity for hydrocarbons. The amorphous carbon associated with the raw nanotube sample is a strong adsorbent for hydrocarbons. By comparison, an activated carbon had a greater affinity for hydrocarbons than any of the nanotube samples.     

Hydrothermal alteration of sedimentary organic matter in the presence and absence of hydrogen to tar then oil

Hydrothermal alteration (hydrous pyrolysis) experiments, in the absence and presence of H₂ (reductive), were conducted on organic matter from marine and lacustrine sediments. The experiments were carried out at discrete temperatures from 150 °C to 350 °C to assess the yields and compositions of the bitumen (tar) formed and subsequently at higher temperatures the oil generated. The yield of bitumen was observed to increase with increasing temperatures. Under hydrous pyrolysis conditions with hydrogen, the yield increases by an order of magnitude and immature lacustrine organic matter shows the highest yield. Bitumen, the extractable organic matter at temperatures below 250-300 °C, contains mainly polar compounds, an unresolved complex mixture (UCM) of branched and cyclic compounds, with low amounts of saturated hydrocarbons. The polar compounds include n-alkanoic acids, n-alkanedioic acids, n-alkanols, isoprenoid ketones and methyl alkanoates. At temperatures above 300 °C, the bitumens transform into petroleum products with saturated hydrocarbons (n-alkanes and biomarkers) and UCM as the major components (>95% of total yield). The degree of maturation of the generated oil increases with increasing temperature under both pyrolysis conditions to full maturity at >350 °C. Although, the bitumen yield is much higher under conditions with added hydrogen, the maturity of the generated oil is lower than with just hydrous pyrolysis.     

Synthesis and electrochemical properties of lithium-electroactive surface-stabilized silicon quantum dots

Highly lithium-electroactive Si quantum dots (n-Si), coated with an amorphous carbon layer, were prepared by of butyl-capped Si annealing at 700 or 900 °C. The ordering of the carbon layer structure increased with increasing annealing temperature while the thickness decreased to 1 from 2 nm due to the increased ordering of carbon. n-Si, annealed at 900 °C, had the same particle size (5 nm) as n-Si annealed at 700 °C. In contrast to Si nanocrystals with an average particle size of 30 nm that had a first charge capacity of 225 mAh/g with a very small coulombic efficiency of 4%, n-Si that annealed at 900 °C possessed a first charge capacity of 1257 mAh/g with a significantly enhanced coulombic efficiency of 71%. This improvement was due to the uniform distribution of n-Si with a carbon layer that prohibited n-Si aggregation during cycling.     

Improvement of oil yield and its distribution from coal extraction using sulfide catalysts

Extraction of Mae Moh lignite using toluene-tetralin mixture was performed in a batch reactor at a temperature range from 370 to 490 °C and under initial hydrogen pressure up to 12 MPa. Experiments were carried out to investigate the effects of temperature and initial hydrogen pressure on coal conversion, liquid yield and liquid composition. The effect of catalysts Fe₂S₃, Fe/Ni and Ni/Mo impregnated into activated carbon was also studied. In the absence of a catalyst, the oil yield decreased with temperature above 410 °C and the content of naphtha and kerosene increased while light gas oil and gas oil decreased with increasing temperature. The presence of catalyst would benefit the formation of lighter components, kerosene and light gas oil. Extraction in the presence of Ni/Mo catalyst, the liquid yield reached 64.6 wt% (daf) which included naphtha 2%, kerosene 72.8%, light gas oil 14.9%, gas oil 2.4% and long residue 7.9%. For GC-MS analysis, the fraction of kerosene was composed of tetralin, naphthalene, dodecamethyl-cycloheptasiloxane, methyl dodecanoate, tetradecamethyl-cycloheptasiloxane, ethyl dodecanoate, methyl tetradecanoate and dibutyl phthalate.     

Catalytic hydrocracking of primary maceral concentrate extracts prepared in a flowing solvent reactor

Differences between the behaviour of coal macerals during liquefaction and catalytic hydrocracking were investigated. The liquefaction experiments were carried out in tetralin, using a flowing solvent reactor. The extracts were catalytically hydrocracked in a micro-bomb reactor, using a commercial catalyst. Extracts and hydrocracked products were characterised by size exclusion chromatography (SEC), UV-fluorescence spectroscopy (UV-F), probe-mass spectrometry and thermogravimetric analysis. Conversions of the vitrinite and the liptinite concentrates during liquefaction were high (∼89%), while inertinite samples yielded a little over 20% extract. For inertinites, the emerging picture was consistent with high cross-link density. Liptinite was extracted less completely at lower temperatures and more slowly at high temperatures compared to corresponding vitrinites and vitrinitic coals. Long chain aliphatics released from the liptinite concentrate between 340 and 390°C appeared likely to have originated in lower-molecular mass material occluded in the sample matrix and dissolving in tetralin prior to the onset of massive covalent bond scission. SEC chromatograms showed material of larger MMs in liptinite and vitrinite extracts than in the inertinite extract. The molecular mass distributions broadened with increasing extraction temperature. Catalytic hydrocracking experiments were carried out in a micro-bomb reactor for 10 and 120 min at 440°C, under 190 bar of hydrogen. In hydrocracking, the liptinite was the slowest extract to react at short reaction times (∼10 min). However, at longer reaction times, its products showed the smallest MM-distribution. Smaller differences were observed between the chromatograms of the 10 and 120 min hydrocracked products of the inertinite extract. Differences between spectra of the three extracts would strongly suggest the presence of larger (and apparently irreducible) polycyclic aromatic ring systems, in the hydrocracked products of the inertinite extract.     

Characterisation of insoluble charcoal in Weipa bauxite

The role of charcoal like components (also referred to as char) in soil organic matter reactivity has become increasingly evident. Recently we have demonstrated the role of such material in bauxite. Sodium hydroxide is used at elevated temperatures to separate aluminium hydroxide from ferric oxide in bauxite in the Bayer process and charcoal like material may interfere with the precipitation of aluminium hydroxide. In this paper we study the solubility, structure and composition of charcoal in the feed stockpile of bauxite ore by solubility, laser Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy, and pyrolysis gas chromatography mass spectrometry (py-GC/MS). The charcoal was treated under simulated Bayer process conditions of 245 °C in 5 M sodium hydroxide. The alkaline digestion test showed that a large fraction of the charcoal was insoluble (∼90%). Surprisingly, the spectroscopic characterisation revealed not only typical polycyclic aromatic networks expected for charcoals (aromaticity f_a = 0.64), but also showed an aliphatic character and that the sample contained alkyl chains ranging from nC₁₀ to nC₂₃ carbon chain lengths. The role of this material in bauxite refineries is discussed.     

Fischer-Tropsch synthesis: supercritical conversion using a Co/Al2O3 catalyst in a fixed bed reactor

Modeling of the supercritical fluid mixture indicated that an important increase in density occurs above a threshold of approximately 4 MPa for the reaction temperature of 220 °C studied. While transport parameters of the fluid are largely retained, the observed improvement in wax solubility was noteable.A cobalt catalyst (25%Co/γ-Al₂O₃) was used in a fixed bed reactor under a pressure/density tuned supercritical fluid mixture of n-pentane/n-hexane. By using inert gas as a balancing gas to maintain a constant pressure, the density of the supercritical fluid could be tuned near the supercritical point while maintaining constant space velocity within the reactor. The benefits of the mixture allowed for optimization of transport and solubility properties at an optimum reaction temperature for Fischer-Tropsch synthesis with a cobalt catalyst. Indeed, above 4 MPa, increases in wax yields from sampling and carefully controlled gas measurements using an internal standard demonstrated an important increase in conversion due to greater accessibility to active sites after extraction of heavy wax from the catalyst. Additional benefits included decreased methane and carbon dioxide selectivities. Decreased paraffin/(olefin+paraffin) selectivities with increasing carbon number were also observed, in line with extraction of the hydrocarbon from the pore. Faster diffusion rates of wax products resulted in lower residence times in the catalyst pores, and therefore, decreased probability for readsorption and reaction to the hydrogenated product. Even so, there was not an observable increase in the alpha value for higher carbon number products over that obtained with just the inert gas.     

Organosoluble semi-alicyclic polyimides derived from 3,4-dicarboxy-1,2,3,4-tetrahydro-6-tert-butyl-1-naphthalene succinic dianhydride and aromatic diamines: Synthesis,characterization and thermal degradation investigation

Semi-alicyclic polyimides (PI-1–PI-4) have been prepared from a newly-developed alicyclic dianhydride, 3,4-dicarboxy-1,2,3,4-tetrahydro-6-tert-butyl-1-naphthalene succinic dianhydride (TTDA) and various aromatic diamines. The asymmetrical alicyclic tetralin structure in TTDA endowed the derived PI resins good solubility in various organic solvents. They were soluble not only in polar aprotic solvents but also in solvents with low boiling points including dichloromethane and tetrahydrofuran. Flexible and tough PI films were successfully cast from their N-methyl-2-pyrrolidone (NMP) solution except PI-1 derived from TTDA and 4,4′-oxydianiline (ODA). The PI films exhibited good optical transparency in the ultraviolet and visible light region with optical transmittances around 80% at a wavelength of 400 nm. The PI films showed good thermal stability up to 400 °C in nitrogen, after that they thermally decomposed rapidly. The thermal degradation behaviors of the PIs were investigated by means of thermogravimetric analysis-mass spectrometry (TG-MS), thermogravimetric analysis-Fourier transform infrared spectrometry (TG-FTIR) and the real time FTIR spectra (RT-FTIR) analysis techniques. The results revealed that the decomposition of PI-1 (as a representative) took place mainly in the range of 450–550 °C. The major degradative fragments at 500 °C were clearly identified as the tert-butyl-substituted tetralin moiety and its dealkylation products. Therefore, it can be deduced that for the TTDA-PIs, the single bond bridge attached the maleic anhydride and tetralin anhydride units in TTDA moiety might break first during the heating; thus producing the tetralin fragments.     

Py-MS Study of Sulfur Behavior during Pyrolysis of High-sulfur Coals under Different Atmospheres

In this study sulfur pyrolysis behavior of two Chinese high sulfur coals and their treated coal samples was investigated by Py-MS at a heating rate of 5 °C/min from room temperature to 1025 °C under hydrogen, helium and 2% O₂-He. It is found that the internal and external hydrogen do not show hydrogenation ability at temperature below 400 °C, due to no H₂S formation at this temperature region for all the coal samples. At temperature higher than 400 °C, not only the indigenous hydrogen but also indigenous oxygen can react with sulfur-containing radicals to form H₂S or SO₂. The evolution of H₂S and SO₂ displays the same profiles in pyrolysis of ZY pyrite-free coal under He, further revealing that after the breakage of C-S bond in the organic sulfur structure in coal to form sulfur-containing radicals, which can equally react with indigenous hydrogen and oxygen. The similar tendency between evolution of CO₂ and SO₂ and the same ending temperature also shows that not only C-S but also C-C bond can be broken in pyrolysis of ZY coals under 2% O₂-He atmosphere. However, unlike SO₂ evolution, CO₂ emission increases in the temperature ranging from 500 °C to 800 °C in LZ raw and deashed coals, implying the breakage of C-C bond at high temperature, which might be related to their low coal rank and high pyrite content.     

Fractionation of brown coal by sequential high temperature solvent extraction

Separation of brown coal into fractions having rather uniform structure is believed to be one of the promising pretreatment methods for effective utilization of brown coal. The authors have recently presented a new coal fractionation method that can separate a bituminous coal into several fractions having different molecular weight compounds without decomposing the coal. The method extracts coal using a flowing stream of non-polar solvent such as tetralin or 1-methylnaphthalene by increasing the extraction temperature stepwise up to 350 °C. In this study the fractionation method was applied to fractionate a brown coal. Water was used as an extracting solvent in addition to tetralin and 1-methylnaphthalene by intending to utilize inherent water of brown coal as the extraction solvent. An Australian brown coal was successfully fractionated into six fractions by any solvents, but the properties of the fractions were significantly different depending on the extraction solvent. This is because tetralin, 1-methylnaphthalene, and water interacted significantly with the brown coal in different ways even at less than 350 °C. The difference in chemical structure and thermal properties of the fractions were examined in detail through ultimate analysis, ¹³C NMR, molecular weight distribution, and thermogravimetric and thermomechanical analyses.     

Hydrothermal dewatering of lower rank coals. 2. Effects of coal characteristics for a range of Australian and international coals

A range of lower rank coals from Australia, Indonesia, and the USA have been dried under hydrothermal dewatering conditions at 320 °C for 30 min in a 500 ml autoclave using a 1:3 dry coal/water mixture. The hydrothermally dewatered (HTD) products were characterised by elemental analysis (both organic and inorganic components), volatile matter determinations, moisture holding capacity, calorific value and mercury porosimetry. The total organic carbon (TOC) and the concentrations of inorganics in the waste waters were also determined. The coals fell into two broad groups, the lower rank Australian brown coals with gross calorific values in the range 10-16 MJ/kg (afm) and the higher rank Indonesian and US coals with gross calorific values in the range 18-25.5 MJ/kg (afm). Rank was the major factor influencing the properties of the HTD products but lithotype was also important. TOC values of the waste water from drying of the low rank Australian coals were much higher than those of the waste water from the higher rank coals. Important variations in the amount of leached calcium, magnesium, and iron were noted.     

An extremely rapid, convenient and mild coal desulfurization new process: Sodium borohydride reduction

The present work describes the desulfurization of coal using mildly reductive method. Both a Yanzhou and a Yanshan coal (referred to as YZ and YS coal, respectively), were treated in an aqueous media employing sodium borohydride (NaBH₄) as reducing agent, which is a well known hydrogen storage. Reaction variables investigated include concentration of reductant, time, pH of initial media, temperature, stirring rate and particle size. The calorific values and ignition temperatures of the coal samples before and after treatment were determined. Results show that the total sulfur removal improved with the increase in the concentration of NaBH₄, shaking rate and temperature and with the decrease in the particle size. Meanwhile, decreasing the particle size from − 250 to − 109 μm increased the organic sulfur removal by more than six times for either of the coal samples. Considering economic rationality and operational convenience, the desulfurization conditions determined were 1.6 mM of NaBH₄ concentration, − 109 μm of particle size, neutral pH of initial media, 1 min of treated time, 100 rpm of shaking rate, 30 °C of temperature. This led to 23.8% and 59.0% reduction in the pyritic, 70.4% and 100% reduction in the sulfate, and 11.0% and 15.0% reduction in the organic sulfur, giving 31.3% and 40.8% reduction in the total sulfur for the YZ coal and the YS coal, respectively. Moreover, this resulted in the increase in the calorific values by 3.4-6.9% and the decrease in the ignition temperatures by 2-21 °C for the coal samples. The desulfurization method described here is extremely rapid, convenient, inexpensive and mild, and therefore, has considerable technological interest.     

Dry catalytic partial oxidation of diesel-fuel distillates into syngas

Volatile compounds distilled below 205 °C from diesel fuel are reformed into synthesis gas by dry catalytic partial oxidation using porous membrane reactors, eliminating complex liquid-fuel injectors and fuel-air mixers, greatly simplifying reformers for applications with solid-oxide fuel cells and NO_x traps. For distillates utilizing 20 wt% of the diesel fuel, 88 mol% of the carbon is converted into CO and 75 mol% of the hydrogen into H₂. Rationale is as follows: Long-chain n-alkanes such as n-hexadecane, with normal boiling point, 286.5 °C, but autoignition temperature, 205 °C, are the least thermally stable hydrocarbons in diesel fuel. If attempts are made to vaporize diesel fuel under oxygen-lean conditions without precautions, long-chain n-alkanes crack at autoignition temperatures forming radicals that initiate polymerization. By eliminating more troublesome compounds by distillation, and by effusing cooler air through porous ceramic membranes to react radicals with oxygen, carbon deposition is largely suppressed. A perovskite catalyst, fed pre-heated air at >900 °C, provides a reservoir of mobile lattice oxygen to react with adsorbed carbon. In continuous runs of 72 h, carbon deposition was negligible in the reactor, on the catalyst, and in the exhaust, except for minor graphite deposited onto walls near the catalytic hot zone.     

Crosslinking of PET through solid state functionalization with alkoxysilane derivatives

A new way for crosslinking poly(ethylene terephthalate) (PET) films and fibers is described using solid state functionalization of the PET end groups (alcohol and acid) with two reagents, respectively, 3-isocyanatopropyltriethoxysilane (IPTESI) or/and 3-glycidoxypropyltrimethoxysilane (GOPTMSI). This functionalization is then followed by hydrolysis-condensation reactions of PET-alkoxysilane end groups leading to the PET crosslinking.First of all, the functionalization reactions were investigated on model compounds by ¹H NMR spectroscopy in a range of temperature 80-160 °C. Furthermore, the diffusion of reagents in solid PET, depending on the initial degree of PET crystallinity, was characterized in the same temperature range through the variation of sample mass. On the other hand, this method allowed us to determine the diffusion coefficients and the solubility of the reagents in solid PET at different temperatures and initial crystallinity degrees.End groups functionalized PET films and fibers by alkoxysilane were then crosslinked by immersion of the samples in hot water. The crosslinking density was characterized by measuring the insoluble fraction of PET in good solvent constituted by a mixture of trifluoroacetic acid and dichloromethane (50/50 vol.). An insoluble fraction close to 70% was obtained by the functionalization treatment of amorphous PET film (8% crystallinity) by a mixture of GOPTMSI + IPTESI (50/50 M) at 155 °C for 1 h followed by hydrolysis-condensation reactions at 80 °C for 72 h. Thermomechanical and thermal properties of films and fibers were observed and found to be considerably enhanced in comparison to the untreated samples. The tensile properties of these partially crosslinked samples were maintained up to 320 °C.     

Synthesis of polyynes in a submerged electric arc in organic solvents

The products formed by the electric arc between graphite electrodes submerged in organic solvents like acetonitrile, n-hexane and methanol consist of a series of polyynes having the general chemical structure: H(CC)_mH (with m an integer 1,2,3,…m). The polyynes were separated through liquid chromatography (HPLC) and identified through their characteristic electronic absorption spectra recorded by a diode-array detector. When acetonitrile was arced at −40 °C, the entire polyynes series to m=9 (chain with 18 carbon atoms) were produced. Instead, at room temperature the entire polyynes series to m=8 (chain with 16 carbon atoms) were obtained. Similar results were obtained by arcing graphite electrodes in n-hexane and in methanol. The purest polyynes mixture is obtained in methanol while in n-hexane and in acetonitrile by-products are formed together with the polyynes series. In particular, in acetonitrile, a series of monocyanopolyynes was detected together with the normal polyynes series.The polyynes are formed by the vaporization of the elemental carbon from the graphite electrodes and dissolved in the solvent where the electrodes are submerged. The demonstration that the polyynes series H(CC)_mH is hydrogen-capped is based on several experimental data from electronic and FT-IR spectroscopy as well as their reactivity with a specific reagent for terminal acetylenes. Some chemical properties of the polyynes solutions (hydrogenation, oxidation) are also treated and discussed.     

Metal-ion pillared clays as hydrocracking catalysts (I): Catalyst preparation and assessment of performance at short contact times

A set of pillared clay catalysts based on montmorillonite (a natural clay) and laponite (a synthetic clay) have been prepared. The new catalysts have been pillared with tin, chromium and aluminium pillars as well as layered double hydroxides based on polyoxo-vanadate and -molybdate. The activities of these novel catalysts have been compared with that of a commercial supported NiMo/Al₂O₃ catalyst and with sulphided Mo(CO)₆ during short (10 min) contact runs. A coal extract sample was reacted at 440 °C in a microbomb reactor in the presence of tetralin and 19 MPa hydrogen. Products were compared by size exclusion chromatography, using NMP as eluent, and by UV-fluorescence. Boiling point distributions of hydrocracked products were determined by a TGA based method; ‘conversions’ were defined as the decrease in the fraction of material with boiling points >450 °C during the reaction. Previous work at 440 °C and 19 MPa H₂ indicates extensive thermal (pyrolytic) cracking during the first 10 min; in the absence of catalyst recombination reactions rapidly take over. Results with several of the new catalysts did not show any improvement compared to the absence of catalyst with ∼39% conversion. The highest conversion (∼70%) was obtained with the Sn laponite pillared clay. The Cr montmorillonite catalyst, pre-calcined at 500 °C, gave the greatest overall shift to smaller molecular masses even though the observed conversion of >450 °C boiling material was relatively poor.     

Adsorption of thiophene and toluene on NaY zeolites exchanged with Ag(I), Ni(II) and Zn(II)

The present study evaluates the adsorption capacity of thiophene and toluene and their competitive behaviour on zeolite NaY exchanged with transition metals (5 wt% Ni, Zn and Ag). The headspace chromatography technique was used to obtain monocomponent apparent adsorption isotherms of thiophene and toluene with NaY, NiY, ZnY and AgY using isooctane as an inert solvent at 30 and 60 °C. Selectivity between toluene and thiophene at saturation capacities were also measured at 30 °C. The adsorption capacity for thiophene increased for the studied adsorbents as follows: NaY < ZnY < NiY < AgY at 30 °C and NaY < NiY < ZnY < AgY at 60 °C. Toluene is less adsorbed, but within the same order of magnitude as thiophene and following the same sorbent order. All adsorbents were moderately selectivity for toluene. Nevertheless, the sulfur content was successfully reduced in the presence of aromatics and olefins in immersion tests with a model fuel mixture. These results show the importance of inserting transitions metals in the zeolitic structure to enhance the adsorption of both aromatic and sulfur containing compounds in organic liquid mixtures, which shows promise to meet environmental standards in transportation fuels.     

Effect of drying catalysts on the properties of thermal copolymers from conjugated linseed oil–styrene–divinylbenzene

The effect of addition of a varying concentration of a drying catalyst (cobalt salt as primary drier) and a combination of catalysts such as cobalt, zirconium (secondary drier) and calcium (auxiliary drier) in a fixed concentration (1%) to a 50:20:30 compositions of 87% conjugated linseed oil, styrene (ST), and divinylbenzene (DVB) has been studied by characterizing the resulting polymers from thermal polymerization with various techniques such as soxhlet extraction, ¹H NMR (¹H nuclear magnetic resonance) spectroscopy, dynamic mechanical analysis (DMA), mechanical and thermogravimetric analysis. The thermal polymerization is performed in the temperature range of 85–160 °C. By soxhlet extraction, it is observed that the polymers contain approximately 64–77% crosslinked materials and the crosslinked insoluble fraction increases with an increase in cobalt catalyst concentration. For fixed concentration (1%) of catalysts, the insoluble fraction from the soxhlet extraction is maximum for the cobalt–zirconium mixture and minimum for the cobalt–calcium mixture. The micro-composition of these polymers obtained from the ¹H NMR spectroscopy indicates that the crosslinked materials are composed of both soft oily and hard aromatic phases. The polymers with varying cobalt concentrations up to 0.6 wt% exhibit two separate glass transition temperatures, indicating the presence of two separate phases, one soft rubbery phase with sharp glass transition temperature of −50 °C and a hard brittle plastic phase of broadened glass transition temperature of 70–120 °C. On the other hand, instead of sharp peaks, the polymers with 0.8 and 1.0% cobalt salts exhibit two humps and a distinct peak in between the humps in the tan δ plots, indicating the presence of an additional phase comprised of a copolymer of linseed oil–styrene and DVB. For fixed concentration (1%) of catalysts, the cobalt–calcium combination follows the similar trend in the tan δ as that for the polymers with 0.8–1.0% cobalt whereas other combinations exhibit two phases. These polymers possess crosslink densities of 0.63–0.91 × 10⁴ mol/m³ and compressive strengths of 2.0–26.6 MPa. The catalyzed polymers are thermally stable below 300 °C and exhibit a major thermal degradation with a maximum degradation of 82–88% at a temperature of 500 °C.     

Effect of preparation conditions on the properties of a coal-derived activated carbon honeycomb monolith

Activated carbon honeycomb (ACH) monoliths were prepared by extruding of a mixture of bituminous coal and organic additives and subsequent carbonization and steam activation. Preparation parameters that were varied were carbonization temperature and activation time. The carbonization conditions were 500, 650 and 800 °C for 1 h and the steam activation conditions were 850 °C for 2, 4 and 6 h. The monoliths at various states were characterized by SEM, XRD, nitrogen adsorption and compression test. It was found that carbonization temperature has significant effects on pore size distribution and mechanical strength of ACH monoliths. The ACH monoliths prepared from high carbonization temperatures exhibited lower values of the BET surface area and total pore volume and higher value of the mechanical strength than those of the ACH monoliths prepared from low carbonization temperatures. This was attributed to the effect of high temperature carbonization that results in the formation of relatively less defective structures.     

Solubility and diffusivity of solvents by packed column inverse gas chromatography

Inverse gas chromatography was used with solid polymer particles in packed columns to measure polymer-solvent solubility and diffusion. A new model for this IGC technique has been developed and used to obtain experimental results for n-pentane, isopentane, 1-hexene, n-hexane, and 1-octene solvents in polymer beads of polyethylene. The conditions were measured for solvents at infinite dilution, and experimental data were obtained for the binary polymer-solvent systems in a temperature range from 70 to 100 °C.