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Effect of Minerals on the Transformations of Organic Matter During Thermolysis in Benzene

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Effect of Minerals on the Transformations of Organic Matter During Thermolysis in Benzene Chemistry for Sustainable Development 13 (2005) 569–574 569 Effect of Minerals on the Transformations of Organic Matter During Thermolysis in Benzene V. V. SAVELIEV Institute of Petroleum Chemistry, Siberian Branch of the Russian Academy of Sciences, Pr. Akademicheskiy 3, Tomsk 634021 (Russia) E-mail: [email protected] (Received February 1, 2005; in revised form May 6, 2005) Abstract The effect of minerals (montmorillonite, calcite, quartz) on the formation of group components of liquid products during pyrolysis of the kerogen of sapropel nature in benzene was investigated. It was established that the maximal amount of liquid products (with the mass concentration above 60 mass %) is formed in the presence of quartz and montmorillonite. It was established that carbonate and clayish rocks promote generation of high-molecular compounds in the pyrolyzate. INTRODUCTION Cuonam formation of bituminous sediments of the siliceous-carbonate-clayish and clayish- Investigation of the interaction between carbonate compositions is situated in the basins inorganic and organic components in of the Olenek and Yudoma rivers (Yakutia) [5]. sedimentary rocks shows that in the majority The bituminological analysis of these sediments of cases the effect of minerals manifests itself showed that this horizon of the Cambrian age is as adsorption and catalytic effects [1, 2]. In generally bitumen maternal with high potential. particular, for thermal destruction of organic Kerogen was obtained form shale oil by matter (OM), these effects promote an increase means of consecutive separation of the in the yield of liquid products, a decrease in chloroform, alcohol-benzene and “bound” (after the concentration of tarry and pyrobitumen acidic treatment) bitumoids. In order to study substances, prevalence of thermodynamically the hydrocarbon components of shale oil, the stable isomers of hydrocarbons. In this situation, group composition of the chloroform-extracted as it was shown by the authors of [3], clayish bitumoid (the so-called bitumoid A) was minerals, especially montmorillonite and illite, determined. The yield of bitumoid A was 0.6 % as well as quartz under the conditions of dry of the weighed portion. The elemental o pyrolysis (T > 40 C), possess these properties to composition of kerogen is represented by the a larger extent than carbonate rocks do. At the following elements, concentration, mass %: same time, during thermolysis of OM in water, Ñ 72.29, H 7.61, O 11.41, S 7.02, N 1.67. The H/C intensive formation of the pyrolyzate occurs in atomic ratio is equal to 1.26, O/C – 0.12. On the presence of calcium carbonate [4]. the basis of atomic ratios of hydrogen and oxygen to carbon according to van Krevelen, EXPERIMENTAL the kerogen is related to type II [6]. The effect of the inorganic constituent of Kerogen of the shale oil of Cuonam horizon sedimentary rocks on the formation of liquid was chosen as the subject of investigation. The products during thermolysis of the sapropel OM 570 V. V. SAVELIEV was studied with montmorillonite TABLE 1 ⋅ (Na0.7Al3.3Mg0.7Si2O20(OH)4 nH2O), calcite Conversion of kerogen into liquid products during (CaCO3) and quartz (SiO2) as examples. These thermolysis, mass % minerals are among the main components Sample Regime incorporated into petroleum-enclosing rocks; Stationary Flow therefore, they provide substantial changes in Temperature, îÑ the petroleum natural substance. Montmorillonite is a representative of clayish 270 320 370 200–500 rocks playing the part of oil-proof covers. Kerogen 4.54 14.2 25.9 51.4 Carbonate and sandy rocks composed mainly Kerogen + calcite 5.40 13.8 25.6 51.7 of calcite and quartz, respectively, serve as Kerogen + montmorillonite 6.03 17.4 33.3 60.4 collectors of micropetroleum. Kerogen + quartz 5.47 18.1 38.2 61.7 Thermolysis of kerogen was carried out in the isothermal and non-isothermal regimes: in Pre-pyrobitumen insoluble in benzene under an autoclave and in a flow reactor, respectively. normal conditions were separated by filtering The organic matter and minerals were ground the pyrolyzate with paper filters. Pyrobitumen before experiments till the particle size of 0.063– was isolated with Golde cold procedure by o 0.2 mm and dried at T = 105 C for 1 h. The means of precipitation in hexane taken in ratio of kerogen to mineral mass was 1 : 1. excess. The components of the liquid product Thermal dissolution of samples in the steady soluble in hexane (petrolene) were separated regime was carried out in benzene in a sealed into tar and hydrocarbon groups (saturated, bomb made of stainless steel. The volumetric aromatic). Separation was carried out by means efficiency for benzene was 0.5. Benzene was of liquid adsorption chromatography on chosen as the solvent due to the assumption that aluminium oxide. Elution was carried out with a fatty solvent medium allows more adequate hexane, a mixture of hexane with benzene at reflection of the processes of petroleum a ratio of 3 : 1, tar species were consecutively formation and organic substance maturing. The washed out with a mixture of ethanol with bomb was placed in a thermostat furnace and benzene (1 : 1). The eluates were combined in kept there for 4 h at a temperature of 270, groups on the basis of Rf values determined o 320 and 370 C. The resulting pyrolyzate was by means of thin layer chromatography with separated from the solid residue by filtering and Silufol plates with a UV 254 luminophor and washing with hot benzene. on the basis of UV spectral data. Thermolysis of the samples in the flow regime was carried out with a set-up described in [7]. A sample of OM was heated in the reactor RESULTS AND DISCUSSION from the room temperature to 500 oC at the heating rate of 2.5 oC/min, pressure in the Thermolysis of OM at a temperature of o system was 150 atm, benzene flow rate was 270 C in the steady regime results in 6–7 cm3/min. Liquid products of thermolysis insignificant generation of liquid products by were sampled at a temperature within the range kerogen: not more than 6 mass % (Table 1). from 200 to 500 oC with a step equal to 25 oC. Evidently, this is connected with rather mild Liquid products of each sample were united in thermolysis conditions under which destruction three fractions (200–325, 325–450 and 450– of the kerogen matrix proceeds only to a small 500 oC) on the basis of characteristic regions extent. The presence of minerals causes only of the curve of pyrolyzate formation. Gaseous insignificant increase in the formation of liquid products formed in thermal decomposition of products. Temperature rise to 320 oC causes a kerogen were not investigated. 3 times increase in the conversion of kerogen The resulting fractions were separated on the into liquid products, while rise up to 370 oC – basis of solubility into kerogen pseudo- more than 6 times. The largest yield of liquid components: pre-pyrobitumen (a mixture of products is observed in the presence of quartz carbenes and carboids), pyrobitumen, tar, oil. and montmorillonite. High conversion of the OM EFFECT OF MINERALS ON THE TRANSFORMATIONS OF ORGANIC MATTER DURING THERMOLYSIS IN BENZENE 571 into liquid products in the presence of quartz 450 oC. Mass concentration of the liquefied is likely to be connected with the fact that kerogen within this range is 67.6–81.7 mass % quartz, within the row of minerals chosen, (Table 2). This region of kerogen decomposition possesses the lowest thermal capacity (0.80 kJ/ is the most interesting one for the investigation (kg ⋅ K)). In the case of calcite and of petroleum formation processes because it is montmorillonite, the corresponding values are this temperature range that embraces the 0.88 and 0.92 kJ/(kg ⋅ K), respectively [8]. generation of the main portion of liquid Evidently, low thermal capacity and chemical products (the so-called petroleum window). inertness of quartz distributed within the bulk According to the data of thermogravimetric OM ensure more rapid heating of the system, analysis of this kerogen, the maximal which causes early generation of liquid products. temperature of its decomposition is 440 oC, the Forming local heating sites, quartz promotes coefficient of sample mass loss KΠ is 47 %. additional dissolution of kerogen in the newly However, we established experimentally that formed micropetroleum. In the case of a clayish the maximum of OM decomposition shifts by mineral, the catalytic effect on thermal 40–50 oC to the low-temperature range for destruction of kerogen is exhibited. It is known thermolysis in the flow regime in benzene [10]. that due to negatively charged centres and Van Low conversion of kerogen within other der Waals forces the surface of natural temperature ranges is explained by the absence aluminosilicates actively adsorbs organic of clearly expressed destructive processes in carbocations; hydrogen disproportionation, the kerogen matrix. It is probable that the low- hydrogenation, isomerisation can proceed on the temperature region involves desorption of the surface of clayish minerals. This also results in components formed during the formation of the an increase in the yield of the liquid part of biogeopolymer kerogen. Under the conditions of the pyrolyzate [9]. flow thermolysis, benzene is in the supercritical An increased (by more than 60 %) formation state, which promotes additional release of of the pyrolyzate in the presence of the clayish natural bitumoid from kerogen. Insignificant and sandy components of sedimentary rocks is yield of liquid products within the high- observed also in the flow regime. temperature region is due to depletion of the It should be noted that the degree of generation potential of the matter under generation of oil-like substances from the initial investigation, that is, the major part of labile kerogen and from a mixture of kerogen with OM has already been transformed into liquid calcite is almost the same in the stationary products, so further temperature rise leads only regime and in the flow one.
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