CN105987925B - The oil content of oil-based drill cuttings and/or the measuring method of oil content and its application - Google Patents
The oil content of oil-based drill cuttings and/or the measuring method of oil content and its application Download PDFInfo
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Abstract
The present invention relates to the oil content and/or oil-containing measuring method of the oil-based drill cuttings after a kind of processing, include the following steps：1) mixed with the not organic reagent of hydrogen atoms with a variety of oil base drilling fluid base oils of different quality, and carry out Nuclear Magnetic Resonance Measurement, establish T2Oily peak area (the S of spectrumi) and basic oil quality (Mi) linear equation：Mi=k × Si+b；2) oil-based drill cuttings after processing are weighed, are M by its quality record1, pour into container；3) measure carbon tetrachloride and analyze pure solution, its volume is denoted as V1, pour into the container described in step 2) and extract；4) volume V is measured from the container of step 3)2Solution, condition is V2<V1, Nuclear Magnetic Resonance Measurement is then carried out, records T2Spectral peak area is S2；5) oil content or oil content of the oil-based drill cuttings after being handled by formula calculating.The invention further relates to the application of the measuring method.
Description
Technical field
The present invention relates to a kind of measuring method of oil field, and in particular to the measurement of a kind of oil content and/or oil content
Method.The invention further relates to the application of the measuring method.
Background technology
Oil base drilling fluid is one of key technology of unconventionaloil pool horizontal well drilling.With shale oil gas, tight sand
The unconventional energy resource exploration and development dynamics such as oil gas continues to increase, and global drilling fluid service enters " oil base drilling fluid epoch ".
Oil-based drill cuttings have been put into National Hazard discarded object (country's danger because it contains the pollutants such as petroleum hydrocarbon, heavy metal and organic matter
Dangerous waste register, HW08), if just directly being discharged without processing, it will periphery ecological environment is caused to seriously endanger.China is to oil
Base drilling fluid use and research is started late, the specific Abgasgesetz on oil-based drill cuttings is still among formulation.Therefore, locate
Oil-based drill cuttings oil-containing measurement technique after reason is another important technology of oil base drilling fluid in addition to preparation.Current is special
Profit is focused primarily upon in the preparation of oil base drilling fluid and the processing of oil-based drill cuttings, and to the oil-based drill cuttings oil-containing measurement after processing
Technical research is almost blank, and also not any related patents and non-patent literature disclose.
Technology based on landwaste oil-containing measurement is very much, such as chromatography (rock pyrolysis), spectrum (quantitative fluorescence), wave spectrum (core
Magnetic resonance) etc., but these technologies are not suitable for the oil-based drill cuttings after processing.This is because：First, using the well of oil base drilling fluid
Section is that have igneous rock formation that the unconventional reservoir or be easy to of nanoscale hole caves in etc., and frequently with PDC drill bit or composite drill
Head drilling, challenge is proposed to the resolution ratio and applicability of conventional nuclear magnetic resonance logging instrument；Second, oily mud shale is both
Reservoir rock is hydrocarbon source rock again, oil-based drill cuttings residue oil content is measured using pyrolytic technique, inevitably by parent rock organic matter
Influence.Third, the oil content of oil-based drill cuttings may be higher, the range of linearity relatively narrow (20mg/l) of quantitative fluorescence is, it is necessary to pass through
More times or repeatedly it is diluted within its range of linearity and could measures, this inevitably introduces error, causes measurement result not
It is enough accurate.Fourth, the treatment technology of oil-based drill cuttings is varied, including materializing strategy, biological treatment etc. more than ten is planted, existing rock
Bits oil-containing measurement technique can not be applicable in completely.There are the oil content and/or oil-containing that a small amount of research is related to oil base drilling fluid at present
Amount analysis, but it is not related to oil content and/or oil-containing measurement technique after the processing of oil base landwaste.Therefore, this area there is an urgent need for
A kind of method of the oil content and/or oil content of oil-based drill cuttings that can be effectively after measurement processing.
The content of the invention
In terms of the present invention overcomes current landwaste oil-containing measurement technique after treatment oil-based drill cuttings oil-containing measurement not
Foot, there is provided the method for the oil content and/or oil content of the oil-based drill cuttings after a kind of new measurement processing, it passes through high-resolution stream
Body nuclear magnetic resonance technique is easy, accurately measures oil-based drill cuttings oil content and/or oil content after handling, is carried for environmental protection with health
For a kind of effective Means of Ensuring.
The oil content and/or oil-containing measuring method of oil-based drill cuttings after a kind of processing provided by the invention include following step
Suddenly：
1) mixed with the not organic reagent of hydrogen atoms with one or more oil base drilling fluid base oils of different quality, and
Nuclear Magnetic Resonance Measurement is carried out, establishes T2Oily peak area (the S of spectrumi) and basic oil quality (Mi) linear equation：Mi=k × Si+b；
2) oil-based drill cuttings after processing are weighed, are M by its quality record1, all poured into after grinding in container；
3) organic reagent of not hydrogen atoms is measured, its volume is denoted as V1, pour into the container described in step 2), shake
It is even, stand, to realize extraction；
4) volume V is measured from the container of step 3)2Solution, condition is V2<V1, then carried out nuclear magnetic resonance survey
Amount, records T2Spectral peak area is S2；
5) following equation, the oil content and/or oil content of the oil-based drill cuttings after calculating processing are passed through：
The signal area of remaining oil is in oil-based drill cuttings：
The quality of remaining oil is in oil-based drill cuttings：Mi=k × S1+ b,
Oil-based drill cuttings oil content after processing is：
Oil-based drill cuttings oil content after processing is：
Wherein, in step 1), due to the organic reagent as organic extractant, hydrogen atoms, the organic reagent do not have
There are NMR signal, thus T2Spectrum or T2- D is (by lateral relaxation time T2With diffusion coefficient D form two-dimensional spectrum) peak be
The signal response of base oil, so as to use the oil content of the oil-based drill cuttings after above-mentioned technical proposal easily measurement processing
And/or oil content.
The oil-based drill cuttings are the rock that is carried by oil base drilling fluid and returned out during with oil base drilling fluid drilling well
Bits.Remaining oil described in oil-based drill cuttings is remaining oil after treatment, such as the remaining oil after burning disposal, wherein can
It can include the oil in stratum.
The T2Oily peak area refers to oily peak spectral line and T2The area of axis institute envelope, basic oil quality are to use such as electronics day
The quality for the base oil that equality instrument weighs.
The linear equation is established using linear regression method commonly used in the art in step 1).
" all pouring into " described in step 2) refers to pour into as fully as possible in the zone of reasonableness of technical licensing, i.e.,
Can not perceive or measurable processing after oil-based drill cuttings do not poured into the container in the zone of reasonableness of technical licensing.
Organic reagent of the present invention is that analysis is pure.
In the preferred embodiment of the present invention, oil base drilling fluid base oil described in step 1) is white oil, bavin
Oil, mineral oil, vegetable oil or its any mixture, are preferably white oil, diesel oil or its mixture.
In the preferred embodiment of the present invention, the organic reagent of hydrogen atoms is not tetrachloro described in step 1)
Change carbon, carbon disulfide or its any mixture, be preferably carbon tetrachloride.Carbon tetrachloride is organic extractant, and not hydrogen atoms,
Because there is no signal for the nuclear magnetic resonance technique of measurement hydrogen spectrum
In the preferred embodiment of the present invention, the processing described in step 2) is with burning method, ablution, consolidates
One or more in change method, heat treating process, centrifugal process and extraction are handled.
In the preferred embodiment of the present invention, weighing to be 1/ for service precision described in step 2)
1000g or the balance of higher precision are accurately weighed, it is preferable to use precision is 1/10000g or the balance of higher precision
Accurately to be weighed.
In the preferred embodiment of the present invention, the container described in step 2) holds for the sealing of with closure
Device, is preferably the glass container of with closure, more preferably wide-mouth bottle or cuvette.
In the preferred embodiment of the present invention, grinding to clay into power in mortar described in step 2).
In the preferred embodiment of the present invention, the time of repose stood described in step 3) is 5-15 minutes,
Preferably 10 minutes.
It is a further object of the invention to provide according to above-mentioned method measure and/or handle oil-based drill cuttings in
Using.In the preferred embodiment of the present invention, the oil-based drill cuttings come from nano-pore stratum or are born from storage ground certainly
Layer.
It is still another object of the present invention to provide according to above-mentioned method measure and/or handle oil-based drill cuttings in
Using, it is characterised in that the oil-based drill cuttings are exploited in recovery process using PDC drill bit.
The beneficial effects of the present invention are：
The present invention could be used without the residue in the organic reagent extraction oil-based drill cuttings of the not hydrogen atoms of NMR signal
Oil, can reach 20mg/l, the upper limit by Monitoring lower-cut can realize oil to 100% high-resolution low-field nuclear magnetic resonance technology
Quick, the accurate analysis of remaining oil content after base disposal of cuttings.The present invention overcomes conventional nuclear magnetic resonance technique, pyrolysis analysis point
Analysis, quantitative fluorescence technology etc. to nano-pore stratum, PDC drill bit, be born from storage stratum certainly, different base oil classification, different oil bases bore
Consider the endless full adaptability of processing method etc. to be worth doing, method is easy, reliable and easy to operate.The present invention passes through high-resolution fluid core
Mr techniques are easy, accurately measure the oil-based drill cuttings oil content after processing, can detect whether oil-based drill cuttings have reached ring
The standard (for example, with the relevant HSE management regulations of oilfield enterprise) of guarantor, a kind of effective guarantee hand is provided for environmental protection and health
Section.
Brief description of the drawings
Fig. 1 is T2Compose the graph of a relation to oil between peak area and oil quality.
Fig. 2 is the T of carbon tetrachloride2Spectrum and T2- D two-dimensional spectrums.Wherein, Fig. 2A is the T of carbon tetrachloride2Spectrum, because carbon tetrachloride fills
In vial, there is faint signal, amplitude is no more than 0.35, is noise；Fig. 2 B are the two-dimensional spectrum of carbon tetrachloride, are not had equally
There is signal, the signal in the lower right corner is noise.
Fig. 3 is carbon tetrachloride and the mixed nuclear magnetic resoance spectrum of crude oil.Wherein, after Fig. 3 A is carbon tetrachloride and addition crude oil
T2Spectrum, it can be seen that the noise of carbon tetrachloride and sample bottle is suppressed；Fig. 3 B are that carbon tetrachloride adds the T after crude oil2- D two dimensions
Spectrum, noise are equally suppressed.
Fig. 4 be different lithology difference drill bit processing after oil-based drill cuttings, carbon tetrachloride extraction liquid T2Spectrum.
Fig. 5 be different disposal method oil-based drill cuttings, carbon tetrachloride extraction liquid T2Spectrum.
Embodiment
The present invention is further detailed below by way of specific embodiment.It should be noted that following implement
Example is illustrative, and does not form any restriction to the scope of protection of present invention.It will be understood by those skilled in the art that
, any improvement or change for detailed description below, in situation without departing from the spirit and scope of the invention
Under, in the scope of protection of present invention.
Embodiment 1：The oil content of oil-based drill cuttings after measurement processing and the method for oil content
Mixed with carbon tetrachloride solution with a variety of oil base drilling fluid base oils of different quality, and carry out Nuclear Magnetic Resonance Measurement
(oil quality of a variety of oil base drilling fluid base oils of different quality and the oil sample peak area measured see the table below 1), establishes T2Spectrum
Oily peak area (Si) and basic oil quality (Mi) linear equation：Mi=0.2248Si+ 6.3755 (see Fig. 1).Due to described organic
Hydrogen atoms, the organic reagent do not have NMR signal (see Fig. 2), thus T to solvent2Spectrum or T2The peak of-D is base oil
Signal respond (see Fig. 3).
Table 1
| Oil sample peak area | Oil quality, mg |
| 40.80362 | 12.9 |
| 103.891 | 28.3 |
| 149.4742 | 40.6 |
| 235.4325 | 60.6 |
| 309.432 | 78.9 |
| 363.5208 | 89.6 |
| 437.4061 | 105.9 |
| 515.7525 | 121.9 |
| 591.2319 | 137.4 |
| 640.0383 | 148.9 |
Service precision is that the electronic balance of 1/10000g accurately weighs the oil-based drill cuttings 10000mg after processing, in mortar
All it is put into after pulverizing in glass container, adds the analytically pure carbon tetrachloride of 50ml, after soaking 10min, takes 5ml extracts
Carry out nuclear magnetic resonance spectroscopy, signal area (the i.e. T measured2Spectral peak area) be 152.121251, then：
The signal area of remaining oil is in oil-based drill cuttings：
The quality of remaining oil is in oil-based drill cuttings：Mi=0.2248 × S1+ 6.3755=342.60612mg
Oil-based drill cuttings processing after oil content be：
Oil-based drill cuttings processing after oil content be：
Oil-based drill cuttings oil content after handling is 3.4261%.
Embodiment 2：
Using the method described in embodiment 1, respectively to nano-pore tight sand formation (stone wheel drill bit), come from storage shale certainly
Stratum (PDC drill bit), be born from the oil-based drill cuttings after storage shale formation (rock bit) processing and carry out oil content and oil content certainly
Measurement.Oil-based drill cuttings after the processing of these different lithology difference drill bits, carbon tetrachloride extraction liquid T2Compose different lithology and different brills
The oil-based drill cuttings of head type, the T after processing after the extraction of carbon tetrachloride organic solvent2Spectrum is shown in Fig. 4.
As can be seen that the oil base brill that the method for the present invention is suitable for different lithology and different types of drill bit is exploited
Bits.
Embodiment 3
Using the method described in embodiment 1, respectively to the oil-based drill cuttings after the processing of centrifugal process, extraction and ablution into
The measurement of row oil content and oil content.Oil-based drill cuttings after the processing of these distinct methods are after the extraction of carbon tetrachloride organic solvent
T2Spectrum is shown in Fig. 5.
As can be seen that the method for the present invention is suitable for the oil-based drill cuttings after the processing of different disposal method.
Claims (16)
1. a kind of oil content of the oil-based drill cuttings after processing and/or the measuring method of oil content, include the following steps：
1) mixed, and carried out with one or more oil base drilling fluid base oils of different quality with the not organic reagent of hydrogen atoms
Nuclear Magnetic Resonance Measurement, establishes T2Oily peak area (the S of spectrumi) and basic oil quality (Mi) linear equation：Mi=k × Si+ b, wherein k and
B is constant；
2) oil-based drill cuttings after processing are weighed, are M by its quality record1, all poured into after grinding in container；
3) organic reagent of not hydrogen atoms is measured, its volume is denoted as V1, pour into the container described in step 2), shake up, it is quiet
Put, to realize extraction；
4) volume V is measured from the container of step 3)2Solution, condition is V2<V1, Nuclear Magnetic Resonance Measurement is then carried out, is remembered
Record T2Spectral peak area is S2；
5) following equation, the oil content and/or oil content of the oil-based drill cuttings after calculating processing are passed through：
The signal area of remaining oil is in oil-based drill cuttings：
The quality of remaining oil is in oil-based drill cuttings：Mi=k × S1+ b,
Oil-based drill cuttings oil content after processing is：
Oil-based drill cuttings oil content after processing is：
The processing is with the one or more in burning method, ablution, solidification method, heat treating process, centrifugal process and extraction
Handled.
2. according to the method described in claim 1, it is characterized in that, oil base drilling fluid base oil described in step 1) for white oil,
Diesel oil, mineral oil, vegetable oil or its any mixture.
3. according to the method described in claim 2, it is characterized in that, the base oil is white oil, diesel oil or its mixture.
4. according to the method described in claim 1, it is characterized in that, not hydrogen atoms described in step 1) and step 3) it is organic
Reagent is carbon tetrachloride, carbon disulfide or its any mixture.
5. according to the method described in claim 4, it is characterized in that, not hydrogen atoms described in step 1) and step 3) it is organic
Reagent is carbon tetrachloride.
6. according to the method described in any one in claim 1-5, it is characterised in that weighing to use described in step 2)
Precision is accurately weighed for 1/1000g or the balance of higher precision.
7. according to the method described in claim 6, it is characterized in that, weighing as service precision described in step 2) is 1/
10000g or the balance of higher precision are accurately weighed.
8. according to the method described in any one in claim 1-5, it is characterised in that the container described in step 2) is with close
The sealing container of capping.
9. according to the method described in any one in claim 1-5, it is characterised in that the container described in step 2) is with close
The glass container of capping.
10. according to the method described in any one in claim 1-5, it is characterised in that described in step 2) grind for
Clay into power in mortar.
11. according to the method described in any one in claim 1-5, it is characterised in that the standing stood described in step 3)
Time is 5-15 minutes.
12. according to the method for claim 11, it is characterised in that the time of repose of the standing is 10 minutes.
13. application of the method in measuring and/or handling oil-based drill cuttings according to any one in claim 1-12.
14. application according to claim 13, it is characterised in that the oil-based drill cuttings are bored in recovery process using PDC
Head exploitation.
15. method according to any one in claim 1-12 measure and/or handle come from nano-pore stratum or
Application from the oil-based drill cuttings for being born from storage stratum.
16. application according to claim 15, it is characterised in that the oil-based drill cuttings are bored in recovery process using PDC
Head exploitation.
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| CN106442599B (en) * | 2016-08-31 | 2018-12-25 | 中国石油天然气股份有限公司 | Rock determination method for oil content and device |
| CN106841269B (en) * | 2017-01-12 | 2018-09-25 | 西南石油大学 | A method of it is separated by solid-liquid separation using nuclear magnetic resonance evaluation rejected well drilling liquid |
| CN109386282B (en) * | 2017-08-09 | 2022-02-15 | 中国石油化工股份有限公司 | Identification method for drilling oil layer under mixed oil drilling fluid condition |
| CN108645883B (en) * | 2018-05-11 | 2020-11-03 | 苏州纽迈分析仪器股份有限公司 | Method for rapidly detecting water content of crude oil in oil field |
| CN110107285A (en) * | 2019-05-06 | 2019-08-09 | 中国石油集团渤海钻探工程有限公司 | The method of the petrogenesis attribute on stratum is quickly judged according to the element composition that landwaste is returned out in shaft bottom |
| CN113533156B (en) * | 2021-06-30 | 2024-02-02 | 西安石油大学 | Shale oil reservoir microscopic pore structure characteristic and multi-class pore fluid identification method |
| CN113970500B (en) * | 2021-10-27 | 2023-08-29 | 北京新风航天装备有限公司 | Rapid determination method for oil content of greasy dirt solid waste |
| CN113945444A (en) * | 2021-10-28 | 2022-01-18 | 科正检测(苏州)有限公司 | Solvent extraction method for hydrocarbon substances in trace rock sample |
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