• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    From a temperature (T1) of between 50 ° C and 120 ° C, the temperature of a rock sample is raised to a temperature (T2) of between 180 ° C and 220 ° C. This temperature (T2) is maintained for a predetermined duration. The temperature of the sample is raised to a temperature (T3) of between 330 ° C and 370 ° C. This temperature (T3) is maintained for a predetermined duration. The temperature of the sample is then raised to a temperature (T4) of between 630 ° C and 670 ° C. Three quantities Sh0, Sh1 and Sh2 representative of the quantity of hydrocarbon compounds released during the temperature change steps are measured, and at least one petroleum characteristic of the sample is deduced from these quantities. Application particularly to exploration and oil exploitation.
    公开号:FR3021749A1
    申请号:FR1460576
    申请日:2014-11-03
    公开日:2015-12-04
    发明作者:Daniel Pillot；Geremie Letort；Maria Romero-Sarmiento；Violaine Lamoureux-Var；Valerie Beaumont；Bruno Garcia
    申请人:IFP Energies Nouvelles IFPEN；
    IPC主号:
    专利说明:

    [0001] The present invention relates to the technical field of the petroleum industry, and more particularly to the field of exploration and exploitation of a geological formation potentially or actually producing hydrocarbons.
    [0002] Petroleum compounds, mainly hydrocarbons extracted by organic solvents, are formed by the transformation of insoluble organic matter (called kerogen) generated by the rise in temperature and pressure inherent in the burial of sediments in a pond. sedimentary. The sedimentary rocks that gave rise to oil are called mother rocks. Under certain conditions, the oil thus formed will be partly expelled from the bedrock, then will migrate to rocks called reservoir rocks in which it will accumulate. For a long time, source rocks have been considered as a source of unexploitable hydrocarbons. With the evolution of technologies, this is no longer the case. In fact, mother-rock hydrocarbons are now a new source of fossil energy. For this type of hydrocarbons, the source rock is also the reservoir rock, the hydrocarbons having remained trapped, disseminated within a rock very little permeable. The source rock hydrocarbons are categorized in the unconventional hydrocarbon family, their extraction requiring unconventional techniques compared to the techniques commonly used by the oil and gas industry. This type of bedrock is known as hydrocarbon source rock ("shale plays"). The knowledge of soluble organic matter (petroleum) on the one hand, and insoluble organic matter (kerogen) on the other, present in a rock sample is of great interest in oil exploration and exploitation. For example, it is known that: the amount of oil formed in sediments increases steadily with depth of burial. Therefore, it is possible to assess the degree of evolution of the organic matter contained in these sediments and, more particularly, the evolution interval which corresponds to the main phase of oil formation. the nature of the insoluble organic matter contained in the rocks conditions the petroleum potential of these rocks, that is to say their capacity more or less to produce oil.
    [0003] Thus, the knowledge of such information allows the drillers to perform the operations of coring or tank test, long operations, expensive and perilous, that wisely, especially when these results can be acquired simultaneously operations drilling.
    [0004] Prior Art The following documents will be cited in the description: Behar, F., Beaumont, V., B. Penteado, H.L., 2001. Rock-Eval 6 Technology: Performance and Developments. Oil & Gas Science and Technology 56, 111-134. Lafargue, E., Marquis, F., Pillot, D., 1998. Rock-Eval 6 applications in hydrocarbon exploration, production, and soil contamination studies. Oil & Gas Science and Technology - 15 Journal of the Institut Français du Pétrole, 53, 4, 421-437. The ROCK-EVAL® technique (IFP Energies nouvelles, France), developed by the applicant, and described in particular in documents FR2472754 and EP 0691540 B1, is known. This fast, almost automatic analysis technique has been developed for the characterization of organic matter and hydrocarbons contained in a rock sample from a geological formation. More specifically, this technique makes it possible to determine the presence, the nature and the degree of maturity of the organic matter contained in a rock sample. The ROCK-EVAL method also provides accurate information on the quantification of hydrocarbons, the amount of total organic carbon (TOC) and the amount of mineral carbon (MinC) contained in a rock sample. The ROCK-EVAL technique consists of pyrolysis in an inert (non-oxidizing) atmosphere and a predefined temperature sequence of a rock sample. The pyrolysis furnace cooperates with a device for detecting and measuring the amount of hydrocarbon compounds in the pyrolysis sample. The specific detection device comprises, for example, a flame ionization type detector, of conventional use in gas chromatographic analyzes. The detector delivers a signal representative of the quantities of hydrocarbon products measured. This signal can be transmitted to calculation, storage and display means in which a specific software program calculates, displays and stores the various parameters representative of the characteristics of the hydrocarbons in the presence. More details about the ROCK-EVAL technique are given in the documents mentioned above.
    [0005] Thus, the ROCK-EVAL technique makes it possible in particular to measure the amount of hydrocarbon compounds released throughout the pyrolysis. It is then possible to establish a pyrogram, which is a curve representing the evolution of the quantity of hydrocarbon compounds released, relative to the weight of the sample considered, as a function of time.
    [0006] A pyrogram typically has several peaks (see, for example, Figures 1A and 1B). The peaks are well differentiated and the area of each peak is calculated. This gives, for each peak, a magnitude representative of the amount of hydrocarbon compounds released during the temperature range surrounding the peak considered.
    [0007] Two main methods using two different temperature sequences have been developed: The "Basic method" (or "Bulk Rock method"), dedicated more particularly to the samples of source rocks, is described by For example in Lafargue et al (1998) and Behar et al (2001). The temperature sequence of this method is characterized by an initial temperature T1 of the pyrolysis furnace generally between 300 ° C and 350 ° C, which temperature is maintained for a predetermined time of a few minutes. It is during this phase that the free hydrocarbons initially contained in the rock sample are released. Their quantity is estimated by measuring the area of a first peak, noted Sl. Then, the pyrolysis temperature is gradually increased to a temperature T2, generally 550 ° C. During this phase, volatilization of very heavy hydrocarbon compounds and cracking of nonvolatile organic matter occur. The amount of hydrocarbon compounds released during this thermal cracking phase is estimated by measuring the area of a second peak, denoted S2. It corresponds to the amount of hydrocarbon compounds that would have been generated if the rock had reached a sufficient stage of ripening.
    [0008] The method "Reservoir" (referred to as "Reservoir method" in English), dedicated specifically to reservoir rock samples, is for example described in EP 0691540 B1. The temperature sequence of the "Tank" method is characterized by an initial temperature T1 of the pyrolysis furnace of less than 200 ° C. and preferably equal to 183 ° C. This temperature is maintained for a predetermined time and the amount of light hydrocarbon compounds is estimated by measuring the area of a first peak, noted Sir. Then the temperature of the pyrolysis furnace is raised to a second T2 temperature of about 370 ° C., a phase during which the amount of heavier hydrocarbons released is estimated via the estimation of the surface of a second peak, noted S2a. The temperature T2 corresponds substantially to the end of the thermovaporization of certain hydrocarbons and the beginning of cracking by pyrolysis of the heavy compounds. Thus, the family of hydrocarbon compounds corresponding to the Sir and S2a peaks of the "Reservoir" method is almost equivalent to the family of hydrocarbon compounds characteristic of the S1 peak of the "Basic" method. Then the pyrolysis temperature is again increased to a third temperature T3 of at most 800 ° C. The surface of a second peak, denoted S2b, representative of the heavy hydrocarbon compounds, is estimated during this third heating phase. This peak S2b can be considered as an equivalent of the S2 peak of the "Basic" method. Although initially developed for specific rock types (bedrock for the "Basics" method, reservoir rock for the "Reservoir" method), both methods can be applied to any type of rock. When applied to hydrocarbon source rock samples, it appears that both methods underestimate the area of the peak (s) corresponding to the free hydrocarbons contained in the sample under consideration. Indeed, as shown in Figures 1A and 1B showing the pyrograms resulting from the application respectively of the "Basic" method and the "Tank" method on the same sample of hydrocarbon source rock, the first peak is truncated. The quantification of its surface is therefore underestimated, as well as the amount of free hydrocarbon compounds contained in this rock. Thus, the temperature sequences of the "Basic" and "Reservoir" methods do not appear to be particularly suitable for hydrocarbon source rock samples.
    [0009] This is explained by the fact that, when these methods were developed, the source rocks were not then considered as exploitable oil reservoirs. Due to the growing interest in source rock hydrocarbons, there is a strong demand for an improvement in the ROCK-EVAL pyrolysis technique for reliably estimating the amount of free hydrocarbons in a rock. mother hydrocarbons, and more generally the amount of hydrocarbons potentially extractable from this type of rock.
    [0010] The present invention relates to a pyrolysis method for improving the quantification of the hydrocarbon compounds contained in a sample of a rock. In particular, the temperature sequence described in the present invention is adapted to hydrocarbon source rock. In addition, certain petroleum characteristics, making it possible to evaluate the interest of exploring and / or exploiting a given geological formation, are predefined. The process according to the invention The invention relates to a method for evaluating at least one petroleum characteristic of a rock sample from a geological formation, wherein said sample is heated in an inert atmosphere in a sequence of temperatures. The process comprises the following steps: a) from a first temperature value (T1) between 50 ° C and 120 ° C, the temperature of said sample is raised to a first temperature gradient of between 1 ° C / min and 50 ° C / min, up to a second temperature value (T2) between 180 ° C and 220 ° C, and maintaining said sample at said second temperature value (T2) for a first predetermined duration; b) from said second temperature value (T2), the temperature of said sample is raised according to a second temperature gradient of between 1 ° C./min and 50 ° C./min, up to a third temperature value ( T3) between 330 ° C and 370 ° C, and said sample is maintained at said third temperature value (T3) for a second predetermined duration; C) from said third temperature value (T3), the temperature of said sample is raised according to a third temperature gradient of between 1 ° C./min and 50 ° C./min, up to a fourth temperature value (T4) between 630 ° C and 670 ° C; D) determining three quantities Sho, Shi and Sh2 representative of the measured amount of hydrocarbon compounds released respectively during steps a, b, and c; e) determining, from at least one of said three quantities Sho, Shi or Sh2, at least one petroleum characteristic of said sample.
    [0011] In one embodiment of the present invention, said rock sample may be from hydrocarbon source rock. According to an advantageous embodiment, said first temperature may be between 80 ° C and 120 ° C. According to another advantageous embodiment, said first temperature may be between 90 ° C and 110 ° C.
    [0012] Advantageously, at the beginning of step a), said sample can be maintained at said first temperature T1. According to a preferred embodiment, said second temperature may be between 190 ° C and 210 ° C.
    [0013] According to another preferred embodiment, said third temperature may be between 340 ° C. and 360 ° C. Advantageously, said fourth temperature may be between 640 ° C and 660 ° C.
    [0014] Preferably, said first and second durations may be between 2 and 4 minutes. Advantageously, said first, second and third temperature gradients can be between 20 ° C / minute and 30 ° C / min. According to an embodiment of the present invention, said oil characteristic of said sample calculated in step e) can be chosen from: a free hydrocarbon content index denoted HC ', t, a quality index of said hydrocarbons noted HQI , a production index written Plshale, the degree API, the parameter GOR, and the parameter GCR. According to an embodiment of the present invention, it is possible to calculate in step e) a free hydrocarbon content index HC'nt according to the following formula: HC 'nt = Sho + Shl with Sho, Shi and HC It is expressed in milligrams of hydrocarbon compounds per gram of rock. According to another embodiment of the present invention, it is possible to calculate in step e) a quality index of said HQI hydrocarbons according to the following formula: HQI = S + x100 Sho + Shi with Sho and Shi expressed in milligrams of hydrocarbon compounds per gram of rock and HQI expressed as a percentage by weight. According to a particular mode of implementation of the present invention, it is possible to calculate in step e) a PIShale production index according to the following formula: (Sho + S hi) 131 Shale - (c_L c_L) x100, "h0 M hi M Sh2) with Sho, Shi and Sh2 expressed in milligram of hydrocarbon compounds per gram of rock, and Plshale expressed as a percentage by weight.
    [0015] Advantageously, the calculation of said Plshale production index can be repeated for said samples from different sedimentary layers of said formation, and at least one sedimentary layer of said formation of interest for exploration can be determined and / or or an oil exploitation when said Plshale production index is greater by a factor A than the average of all Plshale production indices measured for said formation. Preferably, said factor λ can be between 1.1 and 1.5.
    [0016] BRIEF DESCRIPTION OF THE FIGURES Other features and advantages of the process according to the invention will become apparent on reading the description hereafter of nonlimiting examples of embodiments, with reference to the appended figures and described hereinafter.
    [0017] FIGS. 1A and 1B show the evolution of the amount of hydrocarbon compounds (Q) with time (t) during a pyrolysis established according to the "Basic" method and according to the "Reservoir" method for the same sample respectively. of hydrocarbon source rock. It should be noted that the abscissa axis, which represents time, is given as an indication: from one method to another, the position of the peaks with respect to the abscissa axis can not be directly compared because the temperature sequences are different. Figure 2 illustrates the temperature sequence of the process according to the invention.
    [0018] FIG. 3 illustrates the evolution of the amount of hydrocarbon compounds (Q) with time (t) during pyrolysis established according to the process according to the invention on a sample of hydrocarbon source rock, the sample being identical to that used to establish Figures 1A and 1B. It should be noted that the abscissa axis, which represents the time, is given as an indication: from one method to another, the position of the peaks by With respect to the x-axis 30 can not be directly compared because the temperature sequences are different.
    [0019] DETAILED DESCRIPTION OF THE INVENTION The object of the present invention is a method for evaluating at least one petroleum characteristic of a rock sample from a geological formation, wherein said sample is heated in an inert atmosphere according to a particular temperature sequence. The present invention can be applied to any type of rock, such as for example a source rock, a reservoir rock or a hydrocarbon source rock. The advantages of the process according to the invention are demonstrated below in the context of an application to a rock sample from a hydrocarbon source rock. Thus, the present invention comprises at least the following steps: a) from a first temperature value (T1) between 50 ° C and 120 ° C, the temperature of said sample is raised according to a first temperature gradient included between 1 ° C / min and 50 ° C / min, up to a second temperature value (T2) between 180 ° C and 220 ° C, and maintaining said sample at said second temperature value (T2) for a first predetermined duration ; B) from said second temperature value (T2), the temperature of said sample is raised according to a second temperature gradient of between 1 ° C./min and 50 ° C./min, up to a third temperature value ( T3) between 330 ° C and 370 ° C, and said sample is maintained at said third temperature value (T3) for a second predetermined duration; C) from said third temperature value (T3), the temperature of said sample is raised according to a third temperature gradient of between 1 ° C / min and 50 ° C / min, up to a fourth temperature value ( T4) between 630 ° C and 670 ° C; d) determining three quantities Sho, Shi and Sh2 representative of the measured amount of hydrocarbon compounds released respectively during steps a, b, and c; e) determining, from at least one of said three quantities Sho, Shi or Sh2, at least one petroleum characteristic of said sample.
    [0020] Figure 2 illustrates the temperature sequence of the inert atmosphere pyrolysis operation of the process according to the invention. At the beginning of the process, the sample is introduced into the heated furnace at a first temperature (T1). This initial temperature value (T1) is between 50 ° C and 120 ° C. According to a preferred embodiment of the invention, the first temperature (T1) is between 80 ° C and 120 °. According to another embodiment of the present invention, the first temperature (T1) is between 90 ° C and 110 ° C.
    [0021] According to an embodiment of the present invention, the sample is maintained at the first temperature (T1) for a non-zero duration. This preliminary step of maintaining the sample at the first temperature (T1) allows the sample to be brought to temperature and / or the release of the very light hydrocarbon compounds present in a sample that is little or not damaged.
    [0022] Then the sample undergoes a programmed heating phase in which the rise in temperature is between 1 ° C / minute and 50 ° C / rinute (segment A), up to a temperature corresponding to a second temperature (T2), between 180 ° C and 220 ° C. Advantageously, a second temperature (T2) of between 190 ° C. and 210 ° C. is chosen. The temperature gradient is preferably between 20 ° C / minute and 30 ° C / minute. The sample is maintained at the second temperature (T2) for a first predetermined duration (segment B), non-zero, for example greater than half a minute and preferably between 2 and 4 minutes. This second temperature (T2) corresponds substantially to the end of the thermovaporization phase of the lighter hydrocarbons contained in the rock sample, and at the beginning of the cracking phase by pyrolysis of heavier hydrocarbons.
    [0023] Then, from the second temperature (T2), the temperature is high (segment C) to a temperature corresponding to a third temperature (T3), according to a temperature gradient of between 1 ° C./minute and 50 ° C. C / minte. The value of the third temperature (T3) is between 330 ° C and 370 ° C. Advantageously, a third temperature value is chosen between 340 ° C and 360 ° C. According to a preferred embodiment, the temperature gradient is between 20 ° C / minute and 30 ° C / minute. The third temperature (T3) is maintained (segment D) for a second predetermined duration, non-zero, for example greater than half a minute, and preferably between 2 and 4 minutes. This third temperature (T3) corresponds substantially to the end of the thermovaporization phase of the heavy hydrocarbons contained in the rock sample, and at the beginning of the pyrolysis cracking phase of the very heavy hydrocarbons.
    [0024] The pyrolysis is continued (segment E) so as to reach a fourth temperature (T4), according to a temperature gradient of between 1 ° C./minute and 50 ° C./minute. The value of the fourth temperature (T4) is between 630 ° C and 670 ° C, preferably between 640 ° C and 660 ° C. The temperature gradient and advantageously between 20 ° C / minute and 30 ° C / minute. This fourth temperature (T4) corresponds substantially to the end of the pyrolysis phase, that is to say at the end of the thermal cracking of the organic material present in the rock sample. Thus, the temperature sequence of the process according to the invention comprises a succession of three heating stages (ramps specified by segments A, C, and E in FIG. 2), separated by two stages of temperature maintenance (isothermal stages specified by FIG. segments B and D in Figure 2). Figure 3 shows the pyrogram resulting from the application of the process according to the invention applied to the same sample of hydrocarbon source rock as that considered to establish Figures 1A and 1B. It can be seen in this FIG. 3 that the pyrogram in question is characterized by the presence of three peaks: a first peak that is called a peak Sho, a second peak that is called a peak Shi, and a third peak that is call Sh2 peak.
    [0025] The area of the peak Sho, given for example in milligram of hydrocarbon compounds per gram of rock, corresponds to the quantity of hydrocarbon compounds obtained between the first temperature (T1) and the second temperature (T2), more precisely obtained during the segments. A and B of Figure 2. This magnitude, which is called Sho magnitude, is representative of the lighter thermosaporizable hydrocarbons. The area of the peak Shi, given for example in milligram of hydrocarbon compounds per gram of rock, corresponds to the quantity of hydrocarbon compounds obtained between the second temperature (T2) and the third temperature (T3), more precisely obtained during the segments. C and D in Figure 2. This quantity, called size Shi, is representative of heavy thermovaporizable hydrocarbons.
    [0026] The area of the peak Sh2, given for example in milligram of hydrocarbon compounds per gram of rock, corresponds to the amount of hydrocarbon compounds obtained between the third temperature (T3) and the fourth temperature (T4), more precisely obtained during the segment. E of Figure 2. This quantity, which is called size Sh2, is representative of very heavy thermovaporizable hydrocarbons.
    [0027] It can be seen in FIG. 3 that the method according to the invention makes it possible to obtain a first peak (peak Sho) complete, not truncated, unlike the "basic" methods (peak S1 in FIG. 1A) and "reservoir" (peak Sir in Figure 1B). The method according to the invention therefore allows a more exhaustive recording of the free hydrocarbons contained in a sample, and therefore, in general, a better quantification of the hydrocarbon compounds contained in a sample. In addition, the method according to the invention allows a better separation of the last peak (peak Sh2) than in the case of the "reservoir" method (peak S2b in Figure 1 B) or that in the case of the "basic method "(Peak S2 in Figure 1A).
    [0028] Thus, the advantages of the process according to the invention demonstrated in the example above can be explained by the temperature sequence characteristic of the process according to the invention. Since the temperature sequence starts at a first low temperature (T1) compared to the methods of the prior art, the process according to the invention makes it possible to measure more completely the amount of free hydrocarbon compounds present in a sample. In addition, the method according to the invention comprises, between two heating stages (ramps A, C, and E in FIG. 2), temperature maintenance steps (isothermal stages B and D in FIG. 2) of at least one duration. greater than half a minute, these 3021749 13 levels ensure the end of the thermovaporization of hydrocarbon compounds of interest in the temperature range considered. From at least one of these three quantities, at least one petroleum characteristic of the parent rock sample under consideration is calculated. According to one embodiment of the present invention, a free hydrocarbon content index HC'nt is calculated according to the following formula: HC = Sho + S h 'with Sho, Shi and HCcont expressed in milligram of hydrocarbons per gram of rock. According to another embodiment of the present invention, a quality index of said HQI hydrocarbons is calculated according to the following formula: ## EQU1 ## with Sho and Sn, expressed in milligrams per gram of rock. HQI represents the proportion, given as a percentage by weight, of very light hydrocarbons with respect to the thermovaporizable fraction. Advantageously, a production index PlShale is calculated according to the following formula: (S ho + S hi) 131 Shale X100, (0 ho m Hi + S h2) with Sho, Shi and Sh2 expressed in milligrams per gram of rock. The Plshale index, expressed as a percentage by mass, represents the size of the light hydrocarbon fraction relative to all the pyrolyzable hydrocarbons (thermovaporizable hydrocarbons to which are added those which begin to be thermocracked). According to an embodiment of the present invention in which the Plshale index estimate is repeated for rock samples from different sedimentary layers of a geological formation, the sedimentary layer (s) of the geological formation having the an interest for exploration and / or oil exploitation when their Plshale production index is one factor A higher than the average of all Plshale production indices measured for the geological formation considered. According to a preferred mode of implementation of the invention, a value is chosen for the factor A of between 1.1 and 1.5. According to one embodiment of the present invention, it is also possible to calculate, from said three quantities, a petroleum characteristic of the parent rock sample considered such that: the degree API: this is a scale well known to those skilled in the art, for accounting for the density of a crude oil; thus, the lighter a crude oil is, the lower its density, and the higher its API degree. Most crude oils have API degrees between 20 ° (very heavy) and 60 ° (very light); the parameter GOR ("Gas Oil Ratio"): this is a measure well known to those skilled in the art, accounting for the amount of gas recovered at the well's head compared to the quantity of gas oil ; the parameter GCR ("Gas Condensate Ratio"): this is a measure well known to those skilled in the art, accounting for the amount of condensates (or light hydrocarbons) relative to the amount of gas. Examples of Application Table 1 compares the results obtained by the process according to the invention (denoted "Method 1") and by the "Reservoir" method (denoted "Method 2") on three rock samples (noted sample A, B, and C) from different hydrocarbon source rock types. In the case of the "Reservoir" method, equivalences denoted HC * cont, HQI * 25 and Prshale of the petroleum characteristics HC'nt, HQI and Plshale defined above for the process according to the invention were calculated as follows: HCc * ', = Sir + S2a; HQI * = Sir X100; S lr + S 2a PI s * bale = (Sir + S 2a) X100. (Sir + S 2a + S2b) According to this table, it can be seen that, whatever the sample considered, the value of the oil characteristic HC 'n obtained by the process according to the invention is greater than its value. equivalent HC * cont obtained by the method "Tank". Indeed, as shown in Table 1, the HC'nt characteristic is 30% greater than its HC * cont equivalent in the case of sample A, 40% in the case of sample B, and 28% in the case of the sample C. This means that the method according to the invention makes it possible to measure a larger amount of free hydrocarbons contained in the sample in question. Thus, thanks to a sequence of temperatures starting at a lower temperature than that of the "Tank" method, the method according to the invention allows a better estimate of the amount of free hydrocarbons present in a rock sample originating from a hydrocarbon source rock that the prior art. With respect to the HQI and Plsnale petroleum characteristics, there is no systematic observable trend from one sample to another. This is explained by the fact that these characteristics depend on the proportion of hydrocarbon types (free, thermovaporizable, thermocrackable) present in the sample considered relative to each other.
    [0029] Table 2 compares the measured quantities Sho, Shi and Sh2 (respectively corresponding to the areas of the peaks Sho, Shi and Sh2) as well as certain petroleum characteristics (HC'nt, HQI and PIshale) obtained by the process according to the invention applied to a rock sample containing bedrock hydrocarbons, implemented with the values of the following first, second, third and fourth temperatures: 25 cases 1: T1 = 100 ° C, T2 = 200 ° C, T3 = 350 ° C and T4 = 650 ° C; case 2: T1 = 80 ° C, T2 = 200 ° C, T3 = 350 ° C and T4 = 650 ° C; case 3: T1 = 100 ° C, T2 = 180 ° C, T3 = 350 ° C and T4 = 650 ° C; case 4: T1 = 100 ° C, T2 = 220 ° C, T3 = 350 ° C and T4 = 650 ° C.
    [0030] It is observed in Table 2 that the oil characteristic HC 'n is equivalent (to within 1.7%, which is the order of magnitude of the measurement uncertainty) in cases 1 or 2. This demonstrates that the free hydrocarbons contained in a rock sample are recovered in an equivalent manner, whether the process according to the invention is carried out with the central temperature or with the minimum temperature of the first preferential temperature range relating to the first temperature T1. It can also be seen in Table 2 that the measured quantity Sho strongly varies in cases 3 and 4. Thus, the value of the second temperature T2, corresponding to the end of the first heating ramp and the first temperature level of the temperature sequence described in the present invention has a significant impact on the size Sho. Indeed, at 180 ° C, all light hydrocarbons have not yet been thermovaporised (Sho is 1.59 mg / g of rock) while at 220 ° C, some of the 10 heavier free hydrocarbons began to be thermovaporised (Sho is 2.5 mg / g of rock). On the other hand, again, the value of the oil characteristic HC'nt is equivalent in cases 3 and 4 (to 0.01 mg / g of rock, which is lower than the uncertainty on the measurement). This demonstrates that the free hydrocarbons contained in a rock sample are recovered in an equivalent manner, whether the process according to the invention is carried out with the minimum temperature or with the maximum temperature of the temperature range relative to the second temperature T2.
    [0031] Method 1 Sho Shi Sh2 HCbont PIShale HQI (mg / g) (mg / g) (mg / g) (mg / g) (mass%) (mass%) Sample A 1.72 3.03 2.39 4.75 36.21 66.53 Sample B 5.03 7.50 96.04 12.53 40.14 11.54 Sample C 0.91 2.75 6.33 3.66 24.86 36.64 Method 2 Sir S2a S2b HC * cont HQI * HQI * (mg / g) (mg / g) (mg / g) (mg / g) (mass%) (mass%) Sample A 1.25 2.04 1 , 3.29 37.99 72.47 Sample B 3.33 4.29 95.70 7.62 43.70 7.38 Sample C 0.70 1.93 6.97 2.63 26.62 27, 40 Table 1 3021749 ShO Shi. Sh2 HCcont HOI Pishale (mg / g) (rnO / O) (rnO / O) (mg / g) (mass%) (mass%) Case 1 1.94 2.85 2.51 4.79 40, 50 65.62 Case 2 1.89 2.82 2.44 4.71 40.13 65.87 Case 3 1.59 3.31 2.54 4.90 32.45 65.86 Case 4 2.50 2 , 41 2.53 4.91 50.92 65.99 Table 2 Other Embodiments According to a particular embodiment of the present invention, a rock sample from a geological formation is heated in a non-oxidizing atmosphere according to the invention. a temperature sequence as defined in the process according to the invention, and the quantity of hydrocarbon compounds released during said heating is continuously measured from a first detector, and, from a second detector, the amount of CO2 and CO contained by the effluent resulting from said heating. According to an embodiment of the present invention, from the continuous measurements of 002, the amount of CO 2 of organic origin and the quantity of CO 2 of mineral origin are determined. According to another embodiment of the present invention, from the continuous measurements of CO 2 and CO, the amount of oxygen of organic origin and the quantity of oxygen of mineral origin are determined. According to another embodiment of the present invention, the residues resulting from the heating are placed in a non-oxidizing atmosphere in another furnace, where they are heated in an oxidizing atmosphere. According to an embodiment of the present invention, the heating in an oxidizing atmosphere can be programmed in temperature so as to go from a temperature of about 400 ° C. to a temperature of 850 ° C. by a gradient. temperature between 10 and 30 ° C / minute. According to one embodiment of the present invention, the amount of CO2 and / or CO contained by the effluent resulting from the oxidizing heating is continuously measured. According to an embodiment of the present invention, from the continuous measurements of CO2 in an oxidizing atmosphere, the amount of CO 2 of organic origin and the amount of CO 2 of mineral origin are determined. According to another embodiment of the present invention, the amount of total organic carbon contained in the sample is determined from the CO2 and CO measurements obtained as a result of heating sequences in non-oxidizing and oxidizing atmospheres. According to one embodiment of the present invention, the device used for the implementation of the present invention comprises a single furnace, allowing heating in an oxidizing atmosphere and heating in a non-oxidizing atmosphere.
    权利要求:
    Claims (16)
    [0001]
    REVENDICATIONS1. A method for evaluating at least one petroleum characteristic of a rock sample from a geological formation, wherein said sample is heated in an inert atmosphere in a temperature sequence, characterized in that: a) from a first temperature value (T1) of between 50 ° C. and 120 ° C., the temperature of said sample is raised according to a first temperature gradient of between 1 ° C./min and 50 ° C./min, up to a second a temperature value (T2) between 180 ° C and 220 ° C, and maintaining said sample at said second temperature value (T2) for a first predetermined duration; b) from said second temperature value (T2), the temperature of said sample is raised according to a second temperature gradient of between 1 ° C./min and 50 ° C./min, up to a third temperature value (T3 ) between 330 ° C and 370 ° C, and said sample is held at said third temperature value (T3) for a second predetermined duration; c) from said third temperature value (T3), the temperature of said sample is raised according to a third temperature gradient of between 1 ° C / min and 50 ° C / min, up to a fourth temperature value (T4). ) between 630 ° C and 670 ° C; d) three quantities Sho, Shi and Sh2 are determined representative of the measured amount of hydrocarbon compounds released respectively during steps a, b, and c; e) determining, from at least one of said three quantities Sho, Shi or Sh2, at least one petroleum characteristic of said sample.
    [0002]
    2. Method according to the preceding claim, wherein said rock sample comes from a hydrocarbon source rock.
    [0003]
    3. Method according to one of the preceding claims, wherein said first temperature is between 80 ° C and 120 ° C. 3021749 20
    [0004]
    4. Method according to one of the preceding claims, wherein said first temperature is between 90 ° C and 110 ° C.
    [0005]
    5. Method according to one of the preceding claims, wherein, at the beginning of step 5 a), said sample is maintained at said first temperature II.
    [0006]
    6. Method according to one of the preceding claims, wherein said second temperature is between 190 ° C and 210 ° C. 10
    [0007]
    7. Method according to one of the preceding claims, wherein said third temperature is between 340 ° C and 360 ° C.
    [0008]
    The process of one of the preceding claims, wherein said fourth temperature is from 640 ° C to 660 ° C. 15
    [0009]
    9. Method according to one of the preceding claims, wherein said first and second times are between 2 and 4 minutes.
    [0010]
    The process of one of the preceding claims, wherein said first, second and third temperature gradients are from 20 ° C / minute to 30 ° C / minute.
    [0011]
    11. Method according to one of the preceding claims, wherein said oil characteristic of said sample calculated in step e) is chosen from: a free hydrocarbon content index denoted HC ', t, a quality index of said hydrocarbons noted HQI, a Plshale production index, the API degree, the GOR parameter, and the GCR parameter.
    [0012]
    12. The process according to claim 11, wherein said free hydrocarbon content index HC 'n is calculated according to the following formula: ## EQU2 ## with Sho, Shi and HC'nt expressed in milligram of hydrocarbon compounds per gram of rock. 5
    [0013]
    13. The method of claim 11, wherein said quality index of said hydrocarbons HQI is calculated according to the following formula: HQI = S h ° x100 ShO + S hl with Sho and Shi expressed in milligrams of hydrocarbon compounds per gram of rock and HQI expressed as a percentage by mass. 10
    [0014]
    14. The method according to claim 11, wherein said Plshale production index is calculated according to the following formula: Sho + S hi) 131 Shale c_c X100, (0 ho m k_, h1 h2 S h2) with Sho, Shi and Sh2 expressed in milligram of hydrocarbon compounds per gram of rock, and PIshale expressed as a percentage by mass.
    [0015]
    15. The method according to claim 14, wherein the calculation of said Plshale production index is repeated for said samples from different sedimentary layers of said formation, and wherein at least one sedimentary layer of said formation of interest is determined for an oil exploration and / or exploitation when said Plshale production index is greater by a factor A than the average of all of said Plshale production indices measured for said formation. 25
    [0016]
    The method of claim 15, wherein said factor λ is between 1.1 and 1.5.
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    同族专利:
    公开号 | 公开日
    FR3021749B1|2016-09-02|
    US20150346179A1|2015-12-03|
    US20180106776A1|2018-04-19|
    US10302617B2|2019-05-28|
    FR3021748A1|2015-12-04|
    FR3021748B1|2016-09-02|
    US10088465B2|2018-10-02|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    EP0691540A1|1994-07-05|1996-01-10|Institut Français du Pétrole|Improved method for the rapid determination of at least one petrological characteristic of a sample of rock and its application to strata containing heavy oil|
    EP0829719A1|1996-09-12|1998-03-18|Institut Francais Du Petrole|Method and device for avaluating a pollution characteristic of a soil sample.|FR3072173A1|2017-10-09|2019-04-12|IFP Energies Nouvelles|METHOD FOR ESTIMATING THE QUANTITY OF FREE HYDROCARBONS IN A SEDIMENTARY ROCK SAMPLE|
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    US10578600B2|2017-08-17|2020-03-03|Saudi Arabian Oil Company|Decontaminating rock samples by thermovaporization|
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    FR3079935B1|2018-04-05|2020-03-27|IFP Energies Nouvelles|PROCESS FOR SIMULATING THE QUANTITY AND QUALITY OF THE HYDROCARBONS OF A SEDIMENTARY BASIN|
    FR3083316B1|2018-06-29|2020-06-12|IFP Energies Nouvelles|PROCESS FOR THE QUANTIFICATION OF PYRITIC SULFUR AND ORGANIC SULFUR FROM A SAMPLE OF ROCK|
    CN110940790A|2018-09-21|2020-03-31|中国石油化工股份有限公司|Method and device for identifying efficient hydrocarbon source rock|
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    2015-11-05| PLFP| Fee payment|Year of fee payment: 2 |
    2015-12-04| PLSC| Publication of the preliminary search report|Effective date: 20151204 |
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    2017-11-28| PLFP| Fee payment|Year of fee payment: 4 |
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    2020-11-26| PLFP| Fee payment|Year of fee payment: 7 |
    2021-11-26| PLFP| Fee payment|Year of fee payment: 8 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1455009A|FR3021748B1|2014-06-03|2014-06-03|METHOD FOR EVALUATING AT LEAST ONE PETROLEUM CHARACTERISTIC OF A ROCK SAMPLE|
    FR1460576A|FR3021749B1|2014-06-03|2014-11-03|METHOD FOR EVALUATING AT LEAST ONE PETROLEUM CHARACTERISTIC OF A ROCK SAMPLE|FR1460576A| FR3021749B1|2014-06-03|2014-11-03|METHOD FOR EVALUATING AT LEAST ONE PETROLEUM CHARACTERISTIC OF A ROCK SAMPLE|
    US14/725,483| US10302617B2|2014-06-03|2015-05-29|Method of assessing at least one petroleum characteristic of a rock sample|
    US15/845,710| US10088465B2|2014-06-03|2017-12-18|Method for determining quantities of hydrocarbon compounds contained in rock from a geological sample|
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