CN106771080B - Tight sand different existence state classification of crude oil extracts and scale new method - Google Patents

Tight sand different existence state classification of crude oil extracts and scale new method Download PDF

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Publication number
CN106771080B
CN106771080B CN201710022984.7A CN201710022984A CN106771080B CN 106771080 B CN106771080 B CN 106771080B CN 201710022984 A CN201710022984 A CN 201710022984A CN 106771080 B CN106771080 B CN 106771080B
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crude oil
hydro carbons
tight sand
extraction
methylene chloride
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CN106771080A (en
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王琪
马晓峰
邓秀芹
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Institute Of Exploration And Development Of Changqing Oilfield Branch China National Petroleum Corp
Lanzhou Center for Oil and Gas Resources of Institute of Geology and Geophysics of CAS
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Institute Of Exploration And Development Of Changqing Oilfield Branch China National Petroleum Corp
Lanzhou Center for Oil and Gas Resources of Institute of Geology and Geophysics of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/24Earth materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26Oils; viscous liquids; paints; inks
    • G01N33/28Oils, i.e. hydrocarbon liquids
    • G01N33/2823Oils, i.e. hydrocarbon liquids raw oil, drilling fluid or polyphasic mixtures

Abstract

The invention discloses a kind of extraction of tight sand different existence state classification of crude oil and scale new methods, this method combination temperature and pressure fluid controls instrument for crude oil carries out classification extraction in free state in tight sand, closing state, physical absorption state, chemical adsorption states, carbonate cements and in feldspar quartz altogether, and has carried out precise calibration according to different phase light hydrocarbons extent of damage difference and content ratio is demarcated.Static observations and Dynamic Extraction have been carried out effective combination by this method, it ensure that each quasi-oil extracts the accurate errorless of content by visual observation and Temperature-pressure Conditions control, by free state, the practical geological conditions of oil reservoir is separated in conjunction with closing state crude oil for the first time, and physical absorption state and chemical adsorption states crude oil have been carried out accurate extraction for the first time and content is demarcated.Accurate extraction of this method for different existence state crude oil in tight sand ensure that the reliability for subsequently changing Parameter analysis.

Description

Tight sand different existence state classification of crude oil extracts and scale new method
Technical field
The invention belongs to chemical technology fields, and in particular to a kind of tight sand different existence state classification of crude oil extract and Scale new method.
Background technique
Fine and close oil refer to adsorb or free state preservation in oil source rock or with oil source rock alternating layers, adjacent fine and close sand It is a kind of non-conventional oil money without the oil accumulation of extensive long-distance migration in the reservoir rocks such as rock, dense carbonate Source.Compared with the low porosity and low permeability reservoir developed in the past, reservoiring mechanism is more complicated, pore throat is subtleer, chink content is higher, surveys It is bigger to visit difficulty.After Bakken group fine and close oil in the oil field Elmcoulee of the basin Williston in 2008 realizes scale development, The U.S. starts to pay much attention to fine and close exploration activity exploitation.2010, the fine and close oily producing well of United States was 2362 mouthfuls existing, individual well oil-producing 12t has added up oil-producing 3192 × 104T, it is contemplated that densification oil yield in the year two thousand twenty the whole America is up to 1.5 × 108t.Currently, China is causing Have good beginning in terms of close exploration activity, fine and close oil is found in 5 basins, illustrates good Exploration Potential, wherein E Er This more basin extension group take the lead in having built up the fine and close oily area of maturation of domestic first industrialized production, the cause of Sichuan Basin Jurassic system It is more than ten thousand tons of oil well that close reservoir, which has 146 mouthfuls of cumulative productions, is that domestic reality takes over fine and close oil area.
Crude oil occurrence status multiplicity in tight sand, the effective extraction and class test evaluation pair of different existence state crude oil Tight sand Hydrocarbon Accumulation mechanism study is formulated significant with development decision-making.Use in the prior art " sandstone substep is broken There are many deficiencies for broken soxhlet extraction methods ".
Summary of the invention
It is extracted the purpose of the present invention is to provide a kind of tight sand different existence state classification of crude oil and scale is new Method, this method combination temperature and pressure fluid control altogether instrument by free state in tight sand, closing state, physical absorption state, chemical adsorption states, Crude oil carries out classification extraction in carbonate cements and in feldspar quartz mineral particle, and is lost according to different phase light hydrocarbons Degree difference has carried out precise calibration and content ratio calibration.
Itself the specific technical proposal is:
Tight sand different existence state classification of crude oil extracts and scale new method, comprising the following steps:
Step 1, to by pretreated tight sand core column under normal temperature and pressure conditions with two that volume ratio is 93:7 Chloromethanes-methanol solvate soxhlet type obtains the free hydro carbons in the system of reservoir interconnected pore;
Step 2 by formation temperature of step 1 treated rock sample during crude oil development and is less than threshold pressure item The methylene chloride-methanol solvent for being 93:7 with volume ratio under part is controlled in instrument altogether in temperature and pressure fluid and obtains the free hydro carbons of two classes;
Step 3 keeps the temperature sample and boosts, the methylene chloride-first for being 93:7 with volume ratio under the conditions of being greater than threshold pressure Alcoholic solvent controls the physical absorption hydro carbons obtained in the following reservoir space of reservoir minimal flow pore throat radius in instrument in temperature and pressure fluid altogether;
Step 4 will complete the rock core cryogenic pulverization of step 3 to 1-2mm, the methylene chloride-methanol for being 93:7 with volume ratio Solvent soxhlet type obtains the closing hydro carbons in the non-interconnected dead-end pore system of reservoir;
Step 5 continues cryogenic pulverization sample to individual particles, is observed with microscope, to control separation degree, is used at any time The methylene chloride-methanol solvent soxhlet type that volume ratio is 93:7 obtains mineral surface chemistry and adsorbs hydro carbons;
Step 6 handles 6% hydrochloric acid solution of Within Monominerals sample of step 5 processing, and treated, and solution is extracted with solvent It takes, obtains the hydro carbons in carbonate cements;
Step 7, acid treated sample distilled water flushing to neutrality, the dichloromethane for being 93:7 using volume ratio after dry Alkane-methanol solvate soxhlet type obtains the remaining chemisorption hydro carbons of part mineral particle surface;
Step 8, with after rock sample of the potassium bichromate-concentrated sulfuric acid solution and dioxygen water process newly configured after step 7, use Rock sample, without hydro carbons, is then 10: 1 in volume ratio to surface by the methylene chloride-methanol solvent soxhlet type that volume ratio is 93:7 Methylene chloride-methanol solvent in it is levigate and obtain inclusion hydrocarbon component in individual particles with soxhlet type, to this six kinds of hydrocarbon After the completion of class extracting, Hydrocarbon type composition analysis is carried out respectively, and according to corresponding reservoir Crude Oil composition analysis as a result, carrying out lighter hydrocarbons school Just, horizontal in light hydrocarbons composition characteristic according to the lighter hydrocarbons degree difference correction lost in this six kinds of hydro carbons extraction process, and count Calculate six kinds of hydrocarbon content ratios.
Further, the size of tight sand core column described in step 1 is 25 × 25mm.
Compared with prior art, beneficial effects of the present invention:
Technical solution of the present invention combination temperature and pressure fluid controls instrument for free state, closing state, physical absorption in tight sand altogether State, chemical adsorption states, crude oil carries out classification extraction in carbonate cements and in feldspar quartz, and light according to different phase crude oil Hydrocarbon extent of damage difference has carried out precise calibration and content ratio calibration.This method is had static observations and Dynamic Extraction Effect combines, and ensure that each quasi-oil extracts the accurate errorless of content by visual observation and Temperature-pressure Conditions control, for the first time will Free state practical geological conditions of oil reservoir in conjunction with closing state crude oil is separated, for the first time by physical absorption state and chemical adsorption states Crude oil has carried out accurate extraction and content calibration.Accurate extraction of this method for different existence state crude oil in tight sand, It ensure that the reliability for subsequently changing Parameter analysis, compensate for and crude oil Filling process is only analyzed by hydrocarbon inclusion in mineral Deficiency is analyzed the filling timing of different existence state crude oil (hydro carbons) in tight sand comprehensively and is contributed at hiding, and opens to be subsequent The formulation of temperature and pressure parameter provides important references in hair measure.
Detailed description of the invention
Fig. 1 is that tight sand different existence state classification of crude oil of the present invention extracts and the process of scale new method is illustrated Figure.
Specific embodiment
Technical solution of the present invention is described in more detail with specific embodiment with reference to the accompanying drawing.
Referring to Fig.1, the extraction of tight sand different existence state classification of crude oil and scale new method, including following step It is rapid: 1. to use methylene chloride-methanol (body under normal temperature and pressure conditions to by pretreated tight sand core column (25 × 25mm) Product than 93:7) solvent soxhlet type obtain reservoir interconnected pore system in free hydro carbons (abbreviation free hydrocarbon);2. by above-mentioned Formation temperature during crude oil development of treated rock sample and it is less than under the conditions of threshold pressure and uses methylene chloride-methanol (body Product than 93:7) solvent temperature and pressure fluid controlled in instrument altogether obtain two classes dissociate hydro carbons;It boosts 3. being kept the temperature to sample, is being greater than boundary pressure Acquisition reservoir minimal flow pore throat in instrument is controlled altogether in temperature and pressure fluid with methylene chloride-methanol (volume ratio 93:7) solvent under the conditions of power Absorption hydro carbons (abbreviation physical absorption hydrocarbon) in the following reservoir space of radius;4. by the rock core cryogenic pulverization of complete process 3. to 1- 2mm obtains the closing in the non-interconnected dead-end pore system of reservoir with methylene chloride-methanol (volume ratio 93:7) solvent soxhlet type Hydro carbons (referred to as closing hydrocarbon);5. continuing cryogenic pulverization sample to individual particles (to be observed at any time with microscope, to control separation journey Degree), mineral surfaces, which are obtained, with methylene chloride-methanol (volume ratio 93:7) solvent soxhlet type adsorbs hydro carbons (abbreviation chemisorption Hydrocarbon);6. handling 5. 6% hydrochloric acid solution of Within Monominerals sample that step is handled, solution solvent extraction that treated is obtained Hydro carbons (abbreviation cement hydrocarbon) in calcite cement;7. acid treated sample distilled water flushing is to neutrality, after dry The remaining chemisorption hydrocarbon of part mineral particle surface is obtained using methylene chloride-methanol (volume ratio 93:7) solvent soxhlet type Class;8. using dichloromethane after rock sample of the potassium bichromate-concentrated sulfuric acid solution and dioxygen water process newly configured after 7. step Alkane-methanol (volume ratio 93: 7) solvent soxhlet type is to surface without hydro carbons.Then by rock sample in methylene chloride-methanol (volume ratio 10: 1) levigate in solvent and obtain inclusion hydrocarbon component in individual particles (abbreviation inclusion hydrocarbon) with soxhlet type.To this six After the completion of kind hydrocarbon extraction, Hydrocarbon type composition analysis is carried out respectively, and according to corresponding reservoir Crude Oil composition analysis as a result, carrying out light Hydrocarbon correction, it is horizontal in light hydrocarbons composition characteristic according to the lighter hydrocarbons degree difference correction lost in this six kinds of hydro carbons extraction process, And calculate six kinds of hydrocarbon content ratios.
The foregoing is only a preferred embodiment of the present invention, the scope of protection of the present invention is not limited to this, it is any ripe Know those skilled in the art within the technical scope of the present disclosure, the letter for the technical solution that can be become apparent to Altered or equivalence replacement are fallen within the protection scope of the present invention.

Claims (2)

1. a kind of tight sand different existence state classification of crude oil extracts and scale new method, which is characterized in that including with Lower step:
Step 1, the dichloromethane for being under normal temperature and pressure conditions 93:7 with volume ratio to the pretreated tight sand core column of process Alkane-methanol solvate soxhlet type obtains the free hydro carbons in the system of reservoir interconnected pore;
Step 2 by formation temperature of step 1 treated rock sample during crude oil development and is less than under the conditions of threshold pressure The methylene chloride-methanol solvent for being 93:7 with volume ratio is controlled in instrument altogether in temperature and pressure fluid and obtains the free hydro carbons of two classes;
Step 3 keeps the temperature sample and boosts, and the methylene chloride-methanol for being 93:7 with volume ratio under the conditions of being greater than threshold pressure is molten The physical absorption hydro carbons obtained in the following reservoir space of reservoir minimal flow pore throat radius in instrument is controlled in agent in temperature and pressure fluid altogether;
Step 4 will complete the rock core cryogenic pulverization of step 3 to 1-2mm, the methylene chloride-methanol solvent for being 93:7 with volume ratio Soxhlet type obtains the closing hydro carbons in the non-interconnected dead-end pore system of reservoir;
Step 5 continues cryogenic pulverization sample to individual particles, is observed at any time with microscope, to control separation degree, uses volume Mineral surface chemistry, which is obtained, than the methylene chloride-methanol solvent soxhlet type for 93:7 adsorbs hydro carbons;
Step 6 is handled 6% hydrochloric acid solution of Within Monominerals sample of step 5 processing, solution solvent extraction that treated, Obtain the hydro carbons in carbonate cements;
Step 7, acid treated sample distilled water flushing to neutrality, the methylene chloride-for being 93:7 using volume ratio after dry Methanol solvate soxhlet type obtains the remaining chemisorption hydro carbons of part mineral particle surface;
Step 8, with after rock sample of the potassium bichromate-concentrated sulfuric acid solution and dioxygen water process newly configured after step 7, use volume Than the methylene chloride-methanol solvent soxhlet type for 93:7 to surface without hydro carbons, then by rock sample in two that volume ratio is 10: 1 It is levigate and obtain inclusion hydrocarbon component in individual particles with soxhlet type in chloromethanes-methanol solvate, it is taken out to this seven kinds of hydro carbons After the completion of mentioning, Hydrocarbon type composition analysis is carried out respectively, and according to corresponding reservoir Crude Oil composition analysis as a result, carry out lighter hydrocarbons correction, It is horizontal in light hydrocarbons composition characteristic according to the lighter hydrocarbons degree difference correction lost in this seven kinds of hydro carbons extraction process, and calculate Seven kinds of hydrocarbon content ratios.
2. tight sand different existence state classification of crude oil according to claim 1 extracts and scale new method, It is characterized in that, the size of tight sand core column described in step 1 is 25 × 25mm.
CN201710022984.7A 2017-01-12 2017-01-12 Tight sand different existence state classification of crude oil extracts and scale new method Expired - Fee Related CN106771080B (en)

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CN110058000B (en) * 2018-01-15 2022-03-01 中国石油天然气股份有限公司 Method and device for obtaining volume coefficient of crude oil
CN108982286B (en) * 2018-08-28 2021-09-03 同济大学 Separation and quantification method for soluble organic matters in different occurrence states in shale
CN111577265B (en) * 2020-02-17 2023-08-01 中国石油化工股份有限公司 Method for quantitatively restoring reservoir fluid filling process
CN113740454A (en) * 2021-09-02 2021-12-03 中国石油大学(北京) Pre-treatment method for analyzing primitiveness of precambrian biomarker compound
CN117949548A (en) * 2022-10-19 2024-04-30 中国石油天然气股份有限公司 Shale oil occurrence evaluation method and shale oil geological recoverable reserve evaluation method

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