CN107271247B - A kind of separation method of Macerals of Hydrocarbon Source Rocks - Google Patents
A kind of separation method of Macerals of Hydrocarbon Source Rocks Download PDFInfo
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- CN107271247B CN107271247B CN201610214821.4A CN201610214821A CN107271247B CN 107271247 B CN107271247 B CN 107271247B CN 201610214821 A CN201610214821 A CN 201610214821A CN 107271247 B CN107271247 B CN 107271247B
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Abstract
The present invention relates to a kind of separation methods of Macerals of Hydrocarbon Source Rocks, it is 100-1600 mesh that the kerogen for the enriched organic matter separated from hydrocarbon source rock, which is crushed to granularity, it is gradually separated with the specific gravity liquid that density is incremented by again, the maceral of different densities range can be obtained.The specific gravity liquid that the method for the present invention is configured in first partition density point of the first Macerals using alcohol and heavy-fluid, increases the compatibility of component and specific gravity liquid to be separated, improves the separating effect of maceral.The separation of each Macerals in hydrocarbon source rock not only may be implemented in the method for the present invention, while can also obtain the accurate density range of each Macerals, to realize that the quick separating of a large amount of Macerals in hydrocarbon source rock is laid a good foundation.
Description
Technical field
The invention belongs to Macerals of Hydrocarbon Source Rocks separation technology fields, and in particular to organic aobvious in a kind of hydrocarbon source rock
The separation method of micro-group point.
Background technique
Hydrocarbon source rock is also oil source rock, is a kind of rich in organic matter, a large amount of generation oil gas and the rock that oil gas is discharged.By hydrocarbon source
Rock is milled into light thin slice, and identifiable organic principle is known as maceral under reflected light, transmitted light and fluorescence.Usual organic rock
Maceral is divided into sapropel group, chitin group, vitrinite, inertinite, animal organic debris group and secondary organic matter by Shi Xue
The classifications such as group, also include several specific maceral kinds in each group, and every kind of component has its form and photosensitiveness feature.
Since lipid contents are different inside different maceral its organism, hydrocarbon potentiality difference also compared with
Greatly, research thinks that sapropel group is the best maceral of hydrocarbon potentiality at present.But in fact, inside sapropel group, due to biology
Source is different, and hydrocarbon potentiality differ greatly.For example, planktonic algae cell wall be rich in lipides, and benthic algae cell wall by
Pectin and cellulose composition, lipid contents are seldom, basic content be no more than 3% (Harwood, J.L., Jones, A.L.,
1989.Lipid metabolism in algae.In:Callow,J.A.(Ed.),Advances in Botanical
Research,vol.16.Academic Press,London,pp.1-53).Only it is made of a certain single maceral
Hydrocarbon source rock is seldom, therefore, for the hydrocarbon potentiality of further accurate analysis different maceral, first have to by each maceral into
Row separating-purifying.
The research in terms of maceral separation is mainly for coal rock component both at home and abroad.Patent CN104258975A utilizes electricity
Floatation separates macerals.Different macerals are crushed by patent CN104280284A using crush method
It is separated to different-grain diameter.Lin Hualin proposes that coal is divided into vitrinite's enrichment coal using crush method and inertinite is enriched with coal.It applies
It builds fine jade and separation once was carried out to the maceral in coal with heavy-fluid method.VanKrevelen etc. proposes separation macerals
Heavy/floating technology.Dyrkacz and Horwitz has developed density gradient centrifugation isolation technics (DGC).Rake once utilized suddenly in the U.S.
Flotation column separates maceral in coal, and this method is suitable for large-scale separation.
At present report is had not yet to see for the separation of Macerals of Hydrocarbon Source Rocks, and above-mentioned provided in the prior art
Separation method is only applicable to separate maceral single in coal petrography, can not separate to its maceral kind.This
Outside, hydrocarbon source rock has the characteristics that following two compared with coal petrography: 1) abundance of organic matter is micro- group different well below coal in hydrocarbon source rock
Density variation between point is smaller, and separating difficulty is larger；2) maceral in hydrocarbon source rock is many kinds of, and every kind of maceral is wrapped again
Containing several specific maceral kinds, the difficulty of separation is further increased.
Therefore, presently, there are the problem of be to be badly in need of researching and developing the separation method of Macerals of Hydrocarbon Source Rocks a kind of.
Summary of the invention
The technical problem to be solved by the present invention is to solve the above shortcomings of the prior art and to provide organic in a kind of hydrocarbon source rock
The separation method of maceral.This method isolates kerogen from hydrocarbon source rock first, is made to be separated after handling kerogen
Component separated then according to the density variation of different maceral with the specific gravity liquid of different densities, by lighter component
It is enriched in supernatant, and heavier component is deposited in sediment, to achieve the purpose that Macerals separate.
For this purpose, the present invention provides a kind of separation methods of Macerals of Hydrocarbon Source Rocks comprising:
Step T1 carries out separating treatment to component to be separated with specific gravity liquid, and supernatant and sediment is made；
Supernatant is filtered, washs, is dried by step T2, and target product is made；
Sediment is filtered, washs, is dried by step T3, and pellet fraction is made；
Step T4, be 1 separation by step T1 to step T3 in terms of, n times separation is carried out, until organic aobvious in pellet fraction
Micro-group score is 0；
Wherein, the density of target product described in step T2 is less than the density of specific gravity liquid described in step T1；
As N=1, the component obtained after handling kerogen isolated in source rock sample is as wait divide
From component carry out separating treatment；As N >=2, separating treatment is carried out using pellet fraction as component to be separated；
As N >=2, the N-1 times density for separating specific gravity liquid used is less than the density of the separating obtained target product of n-th；
The density of the specific gravity liquid is gradually incremented by, density interval≤0.02g/mL.
According to the method for the present invention, in step T2, Macerals number is 0 or 1 in the target product.
According to the method for the present invention, the specific gravity liquid is the mixed liquor of solution Q and heavy-fluid.
In some embodiments of the invention, the relative density of the heavy-fluid is 0.95-2.8g/mL；It is preferred that the heavy-fluid
Relative density be 2.0g/mL；It is preferred that the heavy-fluid is the aqueous solution of metatungstic acid iron or the ethanol solution of metatungstic acid iron.
In other embodiments of the invention, as N=1, the solution Q is the mixed liquor of dehydrated alcohol and water；Institute
The volume ratio for stating dehydrated alcohol and water is 1:(1-100)；It is preferred that the volume ratio of the dehydrated alcohol and water is 1:(2-50)；Work as N
When >=2, the solution Q is water.
According to the method for the present invention, in step T1, the granularity of the component to be separated is 100-1600 mesh.
In some embodiments of the invention, in step T1, the weight of the component to be separated and the specific gravity liquid
Volume ratio is 1:(5-20)；It is preferred that the w/v of the component to be separated and the specific gravity liquid is 1:(10-20).
In other embodiments of the invention, in step T1, the separating treatment is centrifuging treatment；It is described from
Heart separating treatment carries out in centrifuge；The revolving speed of the centrifuge is 4000-20000r/min；The time of the separating treatment
For 15-120min.
In other embodiments of the invention, in step T1, component to be separated is being carried out at separation with specific gravity liquid
It is ultrasonically treated before reason；The ultrasonic treatment carries out in Ultrasound Instrument；Power density >=0.3W/cm of the Ultrasound Instrument2；
The frequency of the ultrasonic treatment is 20-100Hz；The time of the ultrasonic treatment is 15-120min.
In some embodiments of the invention, the carrying out washing treatment agents useful for same is distilled water.
In other embodiments of the invention, the pH value of the carrying out washing treatment to filtrate is 6 pH≤7 <.
In other embodiments of the invention, the temperature of the drying process is 50-60 DEG C；The time of the drying process
For 0.5-2.0h.
Detailed description of the invention
It is next with reference to the accompanying drawing that invention is further described in detail.
Fig. 1 is the flow chart of the separation method of Macerals of Hydrocarbon Source Rocks of the present invention.
Specific embodiment
To keep the present invention easier to understand, below in conjunction with embodiment and attached drawing, the present invention will be described in detail, these realities
Apply example only serve it is illustrative, it is not limited to application range of the invention.
As previously mentioned, separation method in the prior art is only applicable to separate the single maceral in coal petrography,
Its maceral kind cannot be separated；And compared with coal petrography, density variation in hydrocarbon source rock between different maceral compared with
Small, every kind of maceral includes several specific maceral kinds again, and separating difficulty is larger.The present inventor studies hair
Existing, it is 100-1600 mesh that the kerogen for the enriched organic matter separated from hydrocarbon source rock, which is crushed to granularity, then is passed with density
The specific gravity liquid of increasing is gradually separated, and the maceral of different densities range can be obtained.The present invention is based on above-mentioned discovery
It makes.
Therefore, the separation method of Macerals of Hydrocarbon Source Rocks according to the present invention, comprising:
Step T1 carries out separating treatment to component to be separated with specific gravity liquid, and supernatant and sediment is made；
Supernatant is filtered, washs, is dried by step T2, and target product is made；
Sediment is filtered, washs, is dried by step T3, and pellet fraction is made；
Step T4, be 1 separation by step T1 to step T3 in terms of, n times separation is carried out, until organic aobvious in pellet fraction
Micro-group score is 0；
Wherein, the density of target product described in step T2 is less than the density of specific gravity liquid described in step T1；
As N=1, the component obtained after handling kerogen isolated in source rock sample is as wait divide
From component separated；As N >=2, separated pellet fraction as component to be separated；
As N >=2, the N-1 times density for separating specific gravity liquid used is less than the density of the separating obtained target product of n-th；
The density of the specific gravity liquid is gradually incremented by, density interval≤0.02g/mL.
The range that density interval of the present invention is limited by the way of "≤0.02g/mL " or " 0-0.02/mL " is not wrapped
Include the case where being divided into 0 between density.
Term " separating treatment " described in step T1 of the present invention refers to lock out operation；Term described in step T4 " separation " is
Refer to the complete separation process from step T1 to step T3.
It further include to source rock sample before step T1 as N=1 in the separation method of above-mentioned Macerals
In isolated kerogen handled the step of obtaining component to be separated:
I, according to the kerogen in GB/T 19144-2010 sedimentary rock in kerogen maceration method separation hydrocarbon source rock；
II carries out isolated kerogen using " measurement that SY/T 5118-2005 CHLORINE IN ROCKS imitates pitch " method
Extracting processing；The extracting processing solvent for use is common organic solvent, such as chloroform, methylene chloride, methylene chloride and ethyl alcohol
One of mixed liquor, n-hexane, benzene and toluene or a variety of；It is preferred that the solvent is chloroform.The time of the extracting processing
For 72h.
III, will through extracting, treated that kerogen carries out pulverizing processing after natural drying, handled by sieving, it is obtained to
Isolated component.It is described pulverize processing instrument can be according to the granularity requirements to component to be separated in this field routine instrument
It is selected in device (agate grinds body or planetary ball mill instrument).For example, to obtain granularity larger (if granularity is 100-400 mesh)
Component to be separated grinds body using agate and carries out pulverizing processing；To obtain the to be separated of granularity smaller (such as more than 400 mesh)
Component carries out pulverizing processing using planetary ball mill instrument.Component to be separated is quickly prepared to realize, preferably using row in the present invention
Celestial body mill instrument carries out pulverizing processing.
The granularity of heretofore described component to be separated is 100-1600 mesh, the granularity of the preferably described component to be separated
For 1600 mesh, Macerals can be made to separate as far as possible with inorganic mineral, and Macerals can be dispersed into single
Granular state could separate the Macerals of different densities in this way in centrifugal separation processes.If Macerals are also
It is attached on inorganic mineral, its inevitable density will receive influence, to influence separating effect.
In the separation method of above-mentioned Macerals, in step T1, the specific gravity liquid is the mixing of solution Q and heavy-fluid
Liquid.The selection principle of heavy-fluid of the present invention is that any physical-chemical reaction does not occur between component to be separated.It is preferred that institute
State the ethanol solution of aqueous solution or metatungstic acid iron that heavy-fluid is metatungstic acid iron；The more preferable heavy-fluid is the water-soluble of metatungstic acid iron
Liquid.The relative density of the heavy-fluid is 0.95-2.8g/mL；It is preferred that the relative density of the heavy-fluid is 2.0g/mL.
In the present invention, the aqueous solution of the metatungstic acid iron is also known as ZY-1 type heavy-fluid.
Heretofore described term " relative density of heavy-fluid " refers to density (1.0g/mL) of the heavy-fluid relative to water.
In the separation method of above-mentioned Macerals, works as N=1, that is, carry out 1st time point of the first Macerals
From when, the solution Q be dehydrated alcohol and water mixed liquor；It is preferred that the volume ratio of the dehydrated alcohol and water is 1:(1-100)；
The volume ratio of the more preferable dehydrated alcohol and water is 1:(2-50)；The volume ratio of the further preferred dehydrated alcohol and water is
1:2.As N >=2, the solution Q is water.
The present invention is when carrying out the 1st separation of the first Macerals, using the mixing of dehydrated alcohol and heavy-fluid
Liquid increases the compatibility of component and specific gravity liquid to be separated as specific gravity liquid, the addition of dehydrated alcohol, to improve micro-
The separating effect of component.
Heretofore described term " dehydrated alcohol " refers to the ethyl alcohol of ethanol content > 99.7%.
Heretofore described term " water " refers both to distilled water unless otherwise instructed.
In the separation method of above-mentioned Macerals, in step T1, the component to be separated and the specific gravity liquid
W/v be 1:(5-20) (i.e. in component 1g to be separated be added 5-20mL specific gravity liquid)；It is preferred that the group to be separated
Dividing with the w/v of the specific gravity liquid is 1:(10-20) (i.e. 10-20mL specific gravity liquid is added in component 1g to be separated)；More
It is preferred that the w/v of the component to be separated and the specific gravity liquid is that (i.e. 10mL is added in component 1g to be separated in 1:10
Specific gravity liquid).
In the separation method of above-mentioned Macerals, in step T1, the separating treatment is centrifuging treatment；Institute
Centrifuging treatment is stated to carry out in centrifuge；The revolving speed of the centrifuge is 4000-20000r/min；The separating treatment
Time is 15-120min.
The effect of heretofore described separating treatment is to separate the Macerals of different densities, and density is small to be had
Machine maceral can on float on specific gravity liquid, and the big Macerals of density are then sunk in specific gravity liquid.
The present invention needs for centrifuge tube to be symmetrically disposed in centrifuge when processing is centrifuged.
In the separation method of above-mentioned Macerals, in step T1, component to be separated is being carried out with specific gravity liquid
It is ultrasonically treated before separating treatment；The ultrasonic treatment carries out in Ultrasound Instrument；The power density of the Ultrasound Instrument >=
0.3W/cm2；The power of the ultrasonic treatment is 20-100Hz；The time of the ultrasonic treatment is 15-120min.
Macerals particle can scatter by heretofore described ultrasonic treatment.Different maceral particles is close
Degree is different, and maceral is only dispersed into individual particle state as far as possible, could preferably separate the maceral of different densities
It opens.
In the separation method of above-mentioned Macerals, the carrying out washing treatment agents useful for same is distilled water.
In the separation method of above-mentioned Macerals, the pH value of the carrying out washing treatment to filtrate is 6 pH≤7 <.
It by the pH value that carrying out washing treatment controls filtrate is 6 pH≤7 < in the present invention, it can be as far as possible by acid separation weight
Liquid is cleaned, and the instrument for the later period not being separated and being tested impacts.
Filtration treatment and carrying out washing treatment sequence, and mistake in no particular order in term " being filtered, washed processing " of the present invention
Filter processing and carrying out washing treatment can repeat.For example, in some embodiments of the invention, it, can be to upper in step T2
Floating object is filtered, washs, refiltering, washing again, refiltering processing.In other embodiments of the invention, in step T3
In, sediment can be washed, be filtered, being washed again, refiltering processing.
In the separation method of above-mentioned Macerals, it is being filtered, after carrying out washing treatment, is further including being dried
The step of；The temperature of the drying process is 50-60 DEG C；The time of the drying process is 0.5-2.0h；It is preferred that the drying
The time of processing is 2h.
In some embodiments of the invention, after supernatant is dried, target product is made；The target
Macerals number is 0 or 1 in product.
In the present invention, due to including several specific macerals in hydrocarbon source rock, each maceral includes several again
A specific maceral kind, therefore, the density range of each maceral kind be likely to be it is discontinuous, i.e., have by one kind
Machine maceral is kept completely separate out in the separation process before a kind of rear, lower Macerals are separated, it may appear that on
The case where Macerals are not collected into floating object, Macerals number is 0 in target product at this time.
In the present invention, when carrying out the separation of a certain Macerals, from be initially separated out the maceral to this
During the separating for several times that maceral is kept completely separate out, Macerals number is in gained target product after separation every time
1。
Term " density " of the present invention refers to density range, rather than a specific density values.
The number of types that term " Macerals number " of the present invention refers to Macerals, it is aobvious especially by optics
Micro mirror determines.Since the form of different types of maceral under an optical microscope is different from optical characteristics, in optics
Form number under microscope is Macerals number.
Term " Macerals kind " of the present invention refers to the specific type under Macerals.For example, sapropel
Group includes grape ball algae and lamalginite, then grape ball algae and lamalginite are the specific type of sapropel group.
In the separation method of above-mentioned Macerals, before carrying out Macerals separation, it is necessary first to determine
Macerals type in component to be separated determines first then according to the substantially density range of Macerals
The first partition density point d of kind maceral1(density of i.e. the first maceral the 1st time separation specific gravity liquid used), with head
Based on a partition density point, set suitable density spacing value, the specific gravity liquid being gradually incremented by using density by density range from
It is small to be separated one by one to big component.
In some embodiments of the invention, when separating the first maceral, it is thus necessary to determine that first separation is close
Point (density of i.e. the first maceral the 1st time separation specific gravity liquid used) is spent, the specific method is as follows: according to various documents
Investigation, the density of Macerals is substantially all between 1.0-1.6g/mL, and therefore, based on 1.0g/mL, setting is appropriate
Density interval (such as 0.02g/mL), 1st time point is carried out to component to be separated with the specific gravity liquid that density is 1.02g/mL first
From.After separation, the Macerals number in supernatant in gained target product is judged with optical microscopy, if organic aobvious
Micro-group score is 1, then the density is first partition density point；If Macerals number >=2, need to turn density interval down,
Gained target product in supernatant is continued to separate, until Macerals number is in gained target product in supernatant
1, then the density that last time separates specific gravity liquid used is first partition density point；If not being collected into after separation
Machine maceral sets suitable density interval, repeats the above steps then based on 1.02g/mL, until gained in supernatant
Macerals number is 1 in target product, then the density that last time separates specific gravity liquid used is first partition density point.
In the separation method of above-mentioned Macerals, the density interval of specific gravity liquid can be according to gained target in supernatant
Macerals number is arbitrarily chosen within the scope of 0-0.02g/mL in product.For example, being used up if being divided into 0.02g/mL between density
Learn microscope judge in supernatant obtained by Macerals number >=2 in target product, then need to turn down at density interval (such as close
0.015g/mL is divided between degree), and the mixture of target product and sediment is re-used as to component to be separated, if using optics
Microscope judges in supernatant Macerals number >=2 in gained target product, then needs again to turn density interval down, weight
Multiple above-mentioned steps, until with optical microscopy judge in supernatant obtained by Macerals number is 1 in target product, then for most
Suitable density spacing value.By adjusting density interval in the present invention, so that in each separation of a certain Macerals
Macerals number is 1 in the target product obtained afterwards.
In the separation method of above-mentioned Macerals, after being kept completely separate out by a kind of Macerals, carry out
A kind of separation of lower Macerals.Since the density range of each maceral kind may be discontinuous, in 0-0.02g/
Density spacing value is chosen within the scope of mL, it may appear that the case where Macerals number is 0 in gained target product in supernatant.Example
Such as, the density of the specific gravity liquid used of separation for the last time is during being kept completely separate out by the first Macerals
d5, and be (d with density5+ density interval) specific gravity liquid of g/mL is when carrying out a kind of separation of lower component, gained target in supernatant
Macerals number is 0 in product, then separation next time is with (d5+ density interval) based on g/mL, with (d5+ density interval+close
Degree interval) specific gravity liquid of g/mL separated, until Macerals number is 1 in gained target product in supernatant, that is, divided
Separate out a kind of lower Macerals.
In some embodiments of the invention, the separation method of the Macerals of Hydrocarbon Source Rocks, comprising:
(1) kerogen isolated from source rock sample is handled, component S to be separated is made1；It sees under the microscope
Examine component S to be separated1In Macerals number (for example, Macerals number be 3), i.e., component S to be separated1In
Contain Macerals A, B and C；
(2) first partition density point (i.e. the density of specific gravity liquid) d is determined1, it is d with density1Specific gravity liquid to group to be separated
Divide S1Processing is centrifuged, supernatant and sediment is made；
(3) supernatant is filtered, washed, be dried, it is D that target product-density, which is made,1Component, micro-
It is under the microscope D to density1Component in Macerals number be 1, and density be D1Group be divided into Macerals A；
(4) sediment is filtered, washed, be dried, pellet fraction is made, observes precipitating under the microscope
Macerals number is 2 in object component, i.e. Macerals B and C；At this point, Macerals A is kept completely separate out
Come, using pellet fraction as component S to be separated2；
It (5) is d with density2Specific gravity liquid to component S to be separated2Processing is centrifuged, supernatant and precipitating is made
Object；
(6) supernatant is filtered, washed, be dried, it is D that target product-density, which is made,2Component, micro-
It is under the microscope D to density2Component in Macerals number be 1, and density be D2Group be divided into Macerals B；
(7) sediment is filtered, washed, be dried, pellet fraction is made；Precipitating is observed under the microscope
Macerals number is 2 in object component, i.e. Macerals B and C；At this point, Macerals B is kept completely separate not yet
Out, it needs to continue to separate, using pellet fraction as component S to be separated3；
It (8) is d with density3Specific gravity liquid to component S to be separated3Processing is centrifuged, supernatant and precipitating is made
Object；
(9) supernatant is filtered, washed, be dried, it is D that target product-density, which is made,3Component, micro-
It is under the microscope D to density3Component in Macerals number be 1, and density be D3Group be divided into Macerals B；
(10) sediment is filtered, washed, be dried, pellet fraction is made；It is heavy to observe under the microscope
Macerals number is 1 in starch component, i.e. Macerals C；At this point, Macerals B is kept completely separate out
Come, using pellet fraction as component S to be separated4；
It (11) is d with density4Specific gravity liquid to component S to be separated4Processing is centrifuged, supernatant is made and sinks
Starch；
(12) supernatant is filtered, washed, be dried, it is D that target product-density, which is made,4Component, aobvious
Observe that density is D under micro mirror4Component in Macerals number be 1, i.e. Macerals C；
(13) sediment is filtered, washed, be dried, pellet fraction is made；It is heavy to observe under the microscope
Macerals number is 0 in starch component, at this point, Macerals C is kept completely separate out, density D4Component
As Macerals C；So far, separation terminates.
In the separation method of above-mentioned Macerals of Hydrocarbon Source Rocks, D1< d1< D2< d2< D3< d3< D4< d4；0 <
d2-d1≤0.02g/mL；0 < d3-d2≤0.02g/mL；0 < d4-d3≤0.02g/mL.It, will be all organic aobvious after separation
Micro-group divides A, B and C to collect respectively.For example, only including density is D for component A1Component；For component B, packet
Including density is D2Component and density be D3Component；For component C, including density is D4Component.
In the present invention, if in certain component a certain Macerals account for observe under an optical microscope it is all organic
Relative amount >=95% of maceral, then it is assumed that Macerals number is 1 in the component；If a certain organic in certain component
Maceral accounts for the relative amount < 5% for all Macerals observed under an optical microscope, then it is assumed that this is organic
Maceral number is 0.The percentage contents value of Macerals can by under optical microscopy different shape it is micro-
The gray value of component is calculated by Leica QWin-V3 image processing software.
Since different maceral has different form and optical characteristics under an optical microscope, the present invention exists
Every time after separation, form and the optics for observing and recording the maceral in gained target product under an optical microscope are special
Property, form and the identical maceral of optical characteristics are collected, that is, it is rich to can reach Macerals of Hydrocarbon Source Rocks separation
The purpose of collection.
The separation method of Macerals of Hydrocarbon Source Rocks provided by the invention is sample separation method.In practical application
In, it is first for different hydrocarbon source rocks due to type and the number difference of different Macerals of Hydrocarbon Source Rocks
Sample separation first is carried out according to the method for the present invention, determines the accurate density range of each maceral, so that it is determined that each separation is close
Spend point (i.e. the density of specific gravity liquid) d1, d2……dN, then when carrying out full-page proof separation, directly matched according to each partition density point
The quick and precisely separation of each Macerals can be realized in specific gravity liquid processed.
The species number of Macerals of Hydrocarbon Source Rocks of the invention and the percentage contents of maceral use Leica
DM4500P optical microscope inspection, and be calculated by Leica QWin-V3 image processing software.
The density of heretofore described specific gravity liquid is measured using electronic densitometer.
The calculation formula of the rate of recovery of every kind of Macerals is as follows in the present invention:
The quality of the component (as N=1) of the actual recovered quality of the Macerals of the rate of recovery=every kind/to be separated ×
100%
The separation method of Macerals of Hydrocarbon Source Rocks provided by the invention has the advantages that
(1) heavy-fluid and various reagents used in method provided by the invention are nontoxic, to no damage to human body；
(2) a small amount of dehydrated alcohol that method provided by the invention is added in the 1st separation of the first maceral increases
Kerogenic hydrophily is added, and ethyl alcohol is dissolved in water, can quickly volatilize, be equivalent to surfactant, has not had to kerogen sample
Have an impact；In conjunction with using ultrasonic dispersion technique dispersion effect good, separative efficiency is improved；
(3) method provided by the invention carries out kerogen preparation to hydrocarbon source rock first, eliminates inorganic mineral, has realized
The enrichment of machine matter, to reduce separating difficulty；
(4) it is 100-1600 mesh that kerogen is crushed to granularity by method provided by the invention, can be by different maceral point
Individual particle state is dissipated into, provides guarantee for the separation of Macerals；
(5) separation of each Macerals in hydrocarbon source rock not only may be implemented in method provided by the invention, while may be used also
To obtain the accurate density range of each Macerals, to realize that the quick separating of a large amount of Macerals in hydrocarbon source rock is established
Basis is determined.
Embodiment
Embodiment 1
The hydrocarbon source rock of the present embodiment is Jilin Huadian third system oil shale BTZ-2, and the TOC% of the oil shale is 24.81%.
The separation methods of Macerals in the hydrocarbon source rock specifically includes the following steps:
(1) preparation of component to be separated
BTZ-2 rock sample 100g is taken, being crushed to granularity is 40 mesh, is then deposited according to GB/T 19144-2010
Kerogen maceration method carries out kerogen preparation in rock；The kerogen 5g prepared is taken to place it in after chloroform 72h
Naturally dry in draught cupboard；Then it is pulverized, is sieved with planetary ball mill instrument, it is 1600 purposes component S to be separated that granularity, which is made,1。
Component S to be separated is observed under the microscope1, observe sapropel group, two kinds of macerals of vitrinite, i.e. three kinds of maceral kinds
(grape ball algae, lamalginite and vitrinite) (note: grape ball algae, lamalginite belong to sapropel group, and vitrinite belongs to mirror matter
Group)；Its percentage contents is respectively 81.0%, 6%, 13%.
(2) first partition density point d is determined1
The specific gravity liquid for being first 1.02g/mL with density is to component S to be separated1Carry out the 1st separation.After separation,
It is not collected into Macerals number in supernatant, then based on 1.02g/mL, 0.02g/mL is divided between density, continues pair
Hypostasis (i.e. pellet fraction) after drying is separated；After separation, Macerals number is in gained supernatant
1, then 1.04g/mL is first partition density point d1。
(3) partition density is D1Maceral
It determines that partition density point is 1.04g/mL, alcohol and water is configured to mixed liquor according to volume ratio for 1:2, then will be upper
It states the ZY-1 type heavy-fluid that mixed liquor is 2.0g/mL with relative density and is configured to the specific gravity liquid that density is 1.04g/mL.Specific gravity liquid
Concrete configuration method is as follows: ZY-1 type heavy-fluid and mixed liquor is weighed on an electronic balance with 250mL volumetric flask, after the two is mixed
It shakes up, constant volume, and with the density of the matched specific gravity liquid of electronics densimeter measurement.Such as not up to required density, is added heavy-fluid or distillation
Water is finely adjusted, until reaching required density range.
Taking the granularity crushed is that 1600 purposes component 2.22g to be separated is divided into 2 parts, be respectively placed in 50mL from
In heart pipe, and the specific gravity liquid of 11.1mL is added into each centrifuge tube respectively, covers centrifuge tube lid.Centrifuge tube is sufficiently rocked, and
It is put into Ultrasound Instrument and carries out ultrasonic disperse, power density >=0.3W/cm of Ultrasound Instrument2, it is ultrasonically treated 15min, until to be separated
Component is uniformly dispersed.Centrifuge tube is then taken out, above-mentioned 2 centrifuge tubes symmetrically are put into a centrifuge and are carried out at centrifugation
Reason, the revolving speed of centrifuge are 4000r/min, after centrifugal treating 15min, above-mentioned centrifuge tube are taken out, is layered after standing.
Supernatant in centrifuge tube is poured into the triangular funnel for be placed with quantitative filter paper and is filtered, with distilled water repeated flushing three
Supernatant in the funnel of angle, and with the pH value of pH test paper detection filtrate, the pH up to being flushed to filtrate is 6 pH≤7 <.By filter paper
On separation and concentration object carefully taken out together with filter paper, be placed in surface plate, be placed in 60 DEG C of constant temperature oven dry
0.5-2h, until sample drying, then isolated target product-density is D1Maceral, in optical microscopy
Macerals number is 1 in lower observation target product, and the Macerals are grape ball algae.
Sediment in centrifuge tube is cleaned with distilled water, after then being filtered with triangular funnel, is placed in surface plate, is placed in
Dry 0.5-2h obtains pellet fraction until sample drying in 60 DEG C of constant temperature oven；It sees under an optical microscope
Examining Macerals number in the pellet fraction is 3, is grape ball algae, lamalginite and vitrinite respectively；By sediment
Component is as component S to be separated2。
(4) partition density is D2Maceral
It determines that partition density point is 1.06g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (3), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.06g/mL
Liquid.Isolated target product-density is D2Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are grape ball algae；Pellet fraction is made simultaneously, sees under an optical microscope
Examining Macerals number in the pellet fraction is 2, is lamalginite and vitrinite respectively；Using pellet fraction as to
Isolated component S3。
(5) partition density is D3Maceral
It determines that partition density point is 1.08g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.08g/mL
Liquid.Isolated target product-density is D3Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are lamalginite；Pellet fraction is made simultaneously, under an optical microscope
Observing Macerals number in the pellet fraction is 2, is lamalginite and vitrinite respectively；Using pellet fraction as
Component S to be separated4。
(6) partition density is D4Maceral
It determines that partition density point is 1.10g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.10g/mL
Liquid.Isolated target product-density is D4Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are lamalginite；Pellet fraction is made simultaneously, under an optical microscope
Observing Macerals number in the pellet fraction is 2, is lamalginite and vitrinite respectively；Using pellet fraction as
Component S to be separated5。
(7) partition density is D5Maceral
It determines that partition density point is 1.12g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.12g/mL
Liquid.Isolated target product-density is D5Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are lamalginite, while pellet fraction is made, under an optical microscope
Observing in the pellet fraction Macerals number is 2, is lamalginite and vitrinite respectively, using pellet fraction as
Component S to be separated6。
(8) partition density is D6Maceral
It determines that partition density point is 1.14g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.14g/mL
Liquid.Isolated target product-density is D6Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are lamalginite；Pellet fraction is made simultaneously, under an optical microscope
Observing in the pellet fraction Macerals number is 2, is lamalginite and vitrinite respectively, using pellet fraction as
Component S to be separated7。
(9) partition density is D7Maceral
It determines that partition density point is 1.16g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.16g/mL
Liquid.Isolated target product-density is D7Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are lamalginite；Pellet fraction is made simultaneously, under an optical microscope
Observing Macerals number in the pellet fraction is 1, and is vitrinite, using pellet fraction as next density section wait divide
From component S8。
(10) partition density is D8Maceral
It determines that partition density point is 1.18g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.18g/mL
Liquid.It is D that target product-density is not obtained in supernatant after separation8Maceral, i.e., it is organic micro- in target product
Number of components is 0；Pellet fraction is made simultaneously, observing Macerals number in the pellet fraction under an optical microscope is
1, and be vitrinite, using pellet fraction as component S to be separated9。
(11) partition density is D9Maceral
It determines that partition density point is 1.20g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.20g/mL
Liquid.It is D that target product-density is not obtained in supernatant after separation9Maceral, i.e., it is organic micro- in target product
Number of components is 0；Pellet fraction is made simultaneously, observing Macerals number in the pellet fraction under an optical microscope is
1, and be vitrinite, using pellet fraction as component S to be separated10。
(12) partition density is D10Maceral
It determines that partition density point is 1.22g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.22g/mL
Liquid.It is D that target product-density is not obtained in supernatant after separation10Maceral, i.e., it is organic micro- in target product
Number of components is 0；Pellet fraction is made simultaneously, observing Macerals number in the pellet fraction under an optical microscope is
1, and be vitrinite, using pellet fraction as component S to be separated11。
(13) partition density is D11Maceral
It determines that partition density point is 1.24g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.24g/mL
Liquid.It is D that target product-density is not obtained in supernatant after separation11Maceral, i.e., it is organic micro- in target product
Number of components is 0；Pellet fraction is made simultaneously, observing Macerals number in the pellet fraction under an optical microscope is
1, and be vitrinite, using pellet fraction as component S to be separated12。
(14) partition density is D12Maceral
It determines that partition density point is 1.26g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.26g/mL
Liquid.It is D that target product-density is not obtained in supernatant after separation12Maceral, i.e., it is organic micro- in target product
Number of components is 0；Pellet fraction is made simultaneously, observing Macerals number in the pellet fraction under an optical microscope is
1, and be vitrinite, using pellet fraction as component S to be separated13。
(15) partition density is D13Maceral
It determines that partition density point is 1.28g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.28g/mL
Liquid.Isolated target product-density is D13Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are vitrinite；Pellet fraction is made simultaneously, observes under an optical microscope
Macerals number is 1 in the pellet fraction, and is vitrinite, using pellet fraction as component S to be separated14。
(16) partition density is D14Maceral
It determines that partition density point is 1.30g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.30g/mL
Liquid.Isolated target product-density is D14Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are vitrinite；Pellet fraction is made simultaneously, observes under an optical microscope
Macerals number is 1 in the pellet fraction, and is vitrinite, using pellet fraction as component S to be separated15。
(17) partition density is D15Maceral
It determines that partition density point is 1.32g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.32g/mL
Liquid.Isolated target product-density is D15Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are vitrinite；Pellet fraction is made simultaneously, observes under an optical microscope
Macerals number is 1 in the pellet fraction, and is vitrinite, using pellet fraction as component S to be separated16。
(18) partition density is D16Maceral
It determines that partition density point is 1.34g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.30g/mL
Liquid.Isolated target product-density is D16Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are vitrinite；Pellet fraction is made simultaneously, observes under an optical microscope
Macerals number is 1 in the pellet fraction, and is vitrinite, using pellet fraction as component S to be separated17。
(19) partition density is D17Maceral
It determines that partition density point is 1.36g/mL, i.e., is divided into 0.02g/mL between density, the same step of separation method (4), only
The specific gravity that the density that the ZY-1 type heavy-fluid that specific gravity liquid is changed to distilled water and relative density is 2.0g/mL is configured to is 1.36g/mL
Liquid.Isolated target product-density is D17Maceral, observe under an optical microscope organic in the target product
Maceral number is 1, and the Macerals are vitrinite；Pellet fraction is made simultaneously, observes under an optical microscope
Macerals number is 0 in the pellet fraction, then separating step terminates.
All Macerals are collected respectively: grape ball algae includes that density is D1Component and density be D2Group
Point；Lamalginite includes that density is D3Component, density D4Component, density D5Component, density D6Component and
Density is D7Component；Vitrinite includes that density is D13Component, density D14Component, density D15Component, density be
D16Component and density be D17Component.With the quality of electronic balance weighing difference Macerals, the rate of recovery, knot are calculated
Fruit is shown in Table 1.
The separating resulting of 1 Macerals of Hydrocarbon Source Rocks of table
| Maceral | Density | Quality/g | The rate of recovery/% |
| Grape ball algae | 1.02g/cm3< ρGrape ball algae< 1.06g/cm3 | 0.09 | 4.05 |
| Lamalginite | 1.06g/cm3< ρLamalginite< 1.16g/cm3 | 1.69 | 76.13 |
| Vitrinite | 1.26g/cm3< ρVitrinite< 1.36/cm3 | 0.20 | 9.01 |
| It amounts to | - | 1.98 | 89.19 |
From table 1 it follows that isolated two kinds of Macerals from Jilin Huadian third system oil shale BTZ-2
(i.e. three kinds of Macerals kinds) are grape ball algae (1.02g/cm respectively3< ρGrape ball algae< 1.06g/cm3), lamalginite
(1.06g/cm3< ρLamalginite< 1.16g/cm3) and vitrinite (1.26g/cm3< ρVitrinite< 1.36/cm3), each organic micro- group
Dividing the rate of recovery of kind is respectively: 4.05%, 76.13%, 9.01%；The overall recovery of Macerals is 89.19%.
It should be noted that embodiment described above for explaining only the invention, is not constituted to of the invention any
Limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that word used in it is descriptive
With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation
Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it relates to
And specific method, material and embodiment, it is not intended that the present invention is limited to particular case disclosed in it, on the contrary, this hair
It is bright to can be extended to other all methods and applications with the same function.
Claims (12)
1. a kind of separation method of Macerals of Hydrocarbon Source Rocks comprising:
Step T1 carries out separating treatment to component to be separated with specific gravity liquid, and supernatant and sediment is made；
Supernatant is filtered, washs, is dried by step T2, and target product is made；
Sediment is filtered, washs, is dried by step T3, and pellet fraction is made；
Step T4, by step T1 to step T3 be 1 time separation in terms of, carry out n times separation, until pellet fraction in organic micro- group
Score is 0；
Wherein, the density of target product described in step T2 is less than the density of specific gravity liquid described in step T1；
As N=1, the component obtained after handling kerogen isolated in source rock sample is as to be separated
Component carries out separating treatment；As N >=2, separating treatment is carried out using pellet fraction as component to be separated；
As N >=2, the N-1 times density for separating specific gravity liquid used is less than the density of the separating obtained target product of n-th；
The density of the specific gravity liquid is gradually incremented by, density interval≤0.02g/mL,
Wherein in step T1, the granularity of the component to be separated is 100-1600 mesh.
2. the method according to claim 1, wherein in step T2, organic micro- group in the target product
Score is 0 or 1.
3. method according to claim 1 or 2, which is characterized in that
The specific gravity liquid is the mixed liquor of solution Q and heavy-fluid；
The relative density of the heavy-fluid is 0.95-2.8g/mL；
As N=1, the solution Q is the mixed liquor of dehydrated alcohol and water；The volume ratio of the dehydrated alcohol and water is 1:(1-
100)；As N >=2, the solution Q is water.
4. according to the method described in claim 3, it is characterized in that, the heavy-fluid is the aqueous solution or metatungstic acid iron of metatungstic acid iron
Ethanol solution.
5. according to the method described in claim 3, it is characterized in that, the volume ratio of the dehydrated alcohol and water is 1:(2-50).
6. method according to claim 1 or 2, which is characterized in that in step T1, the component to be separated with it is described
The w/v of specific gravity liquid is 1:(5-20).
7. according to the method described in claim 6, it is characterized in that, in step T1, the component to be separated and the ratio
The w/v of heavy-fluid is 1:(10-20).
8. method according to claim 1 or 2, which is characterized in that in step T1, the separating treatment is centrifuge separation
Processing；The centrifuging treatment carries out in centrifuge；The revolving speed of the centrifuge is 4000-20000r/min；Described point
Time from processing is 15-120min.
9. method according to claim 1 or 2, which is characterized in that in step T1, with specific gravity liquid to group to be separated
Divide and be ultrasonically treated before separating treatment；The ultrasonic treatment carries out in Ultrasound Instrument；The power of the Ultrasound Instrument is close
Degree >=0.3W/cm2；The frequency of the ultrasonic treatment is 20-100Hz；The time of the ultrasonic treatment is 15-120min.
10. method according to claim 1 or 2, which is characterized in that the carrying out washing treatment agents useful for same is distilled water.
11. method according to claim 1 or 2, which is characterized in that the pH value of the carrying out washing treatment to filtrate is 6 < pH
≤7。
12. method according to claim 1 or 2, which is characterized in that the temperature of the drying process is 50-60 DEG C；It is described
The time of drying process is 0.5-2.0h.
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