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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 hydrocarbon source rocks, can solve the problems of inability to enrich low-level adamantane compounds and single species of low-level adamantane, Achieving the effect of good guidance and simple operation steps

Active Publication Date: 2013-04-24
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

Examples

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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, then use n-pentane as the eluent, 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 adamantane com...

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Abstract

Disclosed is a method for separating and enriching lower diamondoid compounds from petroleum and source rock, which includes: extracting the source rock sample with a solution of dichloromethane and methanol to give a source rock extract; removing normal saturated hydrocarbons and asphaltic components from the source rock extract or a crude oil sample with ZSM-5 molecular sieve, obtaining isomeric saturated hydrocarbons components through silica-gel column; adding a solution of ß-cyclodextrin into the solution of the isomeric saturated hydrocarbons, separating the mixed suspension to obtain a deposit, adding the deposit into a solution of hydrochloric acid, maintaining the temperature from 40 to 95? in an oven, cooling to room temperature after the hydrolysis of ß-cyclodextrin catalyzed by an acid is completed, and extracting with a saturated hydrocarbon solvent to obtain lower diamondoid compounds. In this method, the rate of recovery of mono-diamondoid compounds is up to 18%, the rate of recovery of di-diamondoid compounds is up to 35%, and the rate of recovery of tri-diamondoid compounds is up to 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 Patents(China)
IPC IPC(8): C07C13/615C07C13/64C07C7/10C07C7/152
CPCC07C2103/90C07C7/005C07C2603/90
Inventor 黄凌王汇彤张水昌魏彩云张文龙
Owner PETROCHINA CO LTD
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