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Method for separating and enriching low-grade adamantane compounds in petroleum and hydrocarbon source rocks

A source rock and adamantane technology, which is applied in the field of separation and enrichment of low-level adamantane compounds from petroleum and source rocks, and can solve the problems of inability to enrich low-level adamantane compounds and single species of low-level adamantane

Active Publication Date: 2011-06-22
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the low-level adamantanes obtained by the above method are relatively single and suitable for systems with high concentrations, and cannot effectively enrich various low-level adamantanes from oil and source rocks with low content.

Method used

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  • Method for separating and enriching low-grade adamantane compounds in petroleum and hydrocarbon source rocks
  • Method for separating and enriching low-grade adamantane compounds in petroleum and hydrocarbon source rocks

Examples

Experimental program
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Effect test

Embodiment 1

[0019] 1 g of source rock samples crushed to 100 μm were placed in 25 mL of dichloromethane:methanol (1:1 v / v) solution for ultrasonic extraction for 24 hours. Filter the extract and pour it into a 100mL separatory funnel containing 25mL deionized water. The bottom aqueous phase was extracted three times with 10 mL of n-pentane:dichloromethane (2:1 v / v) solution, and the combined extracts were added with appropriate amount of sodium sulfate to remove water. Dry the sample with nitrogen at room temperature, dissolve it with a small amount of isooctane, and use isooctane as the eluent to remove normal saturated hydrocarbons and asphaltenes with a 6g ZSM-5 molecular sieve column, and then use n-hexane as the eluent to dissolve the sample The isooctane solution of the obtained isomeric saturated hydrocarbon component was obtained through a 12g silica gel column. The resulting solution was poured into 50 mL of an aqueous solution of β-cyclodextrin with a concentration of 5 mg / mL, ...

Embodiment 2

[0021] 1 g of source rock samples crushed to 100 μm were placed in 25 mL of dichloromethane:methanol (1:1 v / v) solution for ultrasonic extraction for 24 hours. Filter the extract and pour it into a 100mL separatory funnel containing 25mL deionized water. The bottom aqueous phase was extracted three times with 10 mL of n-pentane:dichloromethane (2:1 v / v) solution, and the combined extracts were added with appropriate amount of sodium sulfate to remove water. Dry the sample with nitrogen at room temperature and dissolve it with a small amount of cyclohexane, use cyclohexane as eluent, remove normal saturated hydrocarbons and asphaltenes with 6g ZSM-5 molecular sieve column, then use n-pentane as eluent, The n-hexane solution of the sample was passed through a 12g silica gel column to obtain isomeric saturated hydrocarbon components. The resulting solution was poured into 50 mL of 2 mg / mL β-cyclodextrin aqueous solution, and stirred rapidly for 4 hours. The resulting milky whit...

Embodiment 3

[0023] Take 100mg crude oil sample and dissolve it with a small amount of cyclohexane. Using cyclohexane as the eluent, use a 6g ZSM-5 molecular sieve column to remove normal saturated hydrocarbons and asphaltenes, and then use n-pentane as the eluent to pass the cyclohexane solution of the sample through a 12g silica gel column to obtain isomerization saturation hydrocarbon components. The resulting solution was poured into 50 mL of β-cyclodextrin aqueous solution with a concentration of 1 mg / mL, and stirred rapidly for 1 hour. The resulting milky white suspension was centrifuged for 20 minutes (3000 rpm) to obtain a precipitate, which was washed three times with 10 mL of n-pentane. The resulting precipitate was transferred to a glass bottle filled with 30 mL of 0.1 mol / L hydrochloric acid solution, sealed and placed in an oven at 80°C for 24 hours at a constant temperature. After the sample is cooled to room temperature, add 20 mL of n-pentane to extract the lower adamanta...

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Abstract

The invention relates to a method for separating and enriching low-grade adamantane compounds in petroleum and hydrocarbon source rocks, which comprises the following steps: extracting a hydrocarbon source rock sample with dichloromethane and methanol solution to obtain a hydrocarbon source rock extract; removing normal saturated hydrocarbons and asphaltene components in the hydrocarbon source rock extract or crude oil sample by using a ZSM-5 molecular sieve, passing through silicagel columns to obtain isomeric saturated hydrocarbon components, adding beta-cyclodextrin solution into the isomeric saturated hydrocarbon solution, and separating the suspension to obtain a precipitate; moving the precipitate into a hydrochloric acid solution, putting into a baking oven at 40-95 DEG C, and keeping the temperature; and after the acid-catalysis hydrolysis reaction of the beta-cyclodextrin finishes, cooling to room temperature, and extracting with a saturated hydrocarbon solvent to obtain the low-grade adamantane compounds. By using the method, the recovery rate of the single-adamantane compounds can maximally reach higher than 18%, the recovery rate of the double-adamantane compounds can maximally reach higher than 35%, and the recovery rate of the tertiary-adamantane compounds can maximally reach higher than 1.5%.

Description

technical field [0001] The invention relates to a method for separating and enriching lower adamantane compounds (monoadamantane, double adamantane, triamantane and their derivatives containing alkyl side chains) from petroleum and hydrocarbon source rocks. Background technique [0002] Adamantane compounds have a special lattice structure, and are not easily affected by factors such as organic matter type and depositional environment under most geological conditions, and have strong corrosion resistance, biodegradation resistance and thermal stability. In the field of oil and gas geochemistry research, it is a kind of ideal carbon and hydrogen isotope markers. In the field of oil and gas exploration, it can be used as the basis for identifying the source of oil and gas reservoirs and comparing natural gas with related crude oil and condensate. However, so far there are few studies on the application of adamantane compounds as stable isotope markers, mainly because there are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/615C07C13/64C07C7/10C07C7/152
CPCC07C2103/90C07C7/005C07C2603/90C07C13/64
Inventor 黄凌王汇彤张水昌魏彩云张文龙
Owner PETROCHINA CO LTD
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