CN105987925A - Method for measuring oil length and/or oil content of oil-based drilling cuttings and application of method - Google Patents
Method for measuring oil length and/or oil content of oil-based drilling cuttings and application of method Download PDFInfo
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Abstract
The invention relates to a method for measuring the oil length and/or oil content of treated oil-based drilling cuttings. The method includes the following steps that 1, an organic reagent which does not contain hydrogen atoms is mixed with various types of oil-based drilling fluid base oil with different masses, nuclear magnetic resonance measuring is carried out, and the linear equation that Mi=k*Si+b of the T2 spectrum oil peak area (Si) and base oil mass (Mi) is established; 2, the treated oil-based drilling cuttings are weighed, the mass of the treated oil-based drilling cuttings is recorded as M1, and the treated oil-based drilling cuttings are poured into a vessel; 3, a carbon tetrachloride analytically-pure solution is measured, the volume of the carbon tetrachloride analytically-pure solution is recorded as V1, and the carbon tetrachloride analytically-pure solution is poured into the vessel in the step 2 for extraction; 4, a solution with the volume of V2 is measured from the vessel in the step 3 under the condition that V2<V1 and then is subjected to nuclear magnetic resonance measuring, and the T2 spectrum peak area is recorded as S2; 5, the oil content or oil length of the treated oil-based drilling cuttings is calculated according to a formula. The invention further relates to application of the measuring method.
Description
Technical field
The present invention relates to the measuring method of a kind of oil field, be specifically related to the measuring method of a kind of oil content and/or oil content.The invention still further relates to the application of this measuring method.
Background technology
Oil base drilling fluid is one of key technology of unconventionaloil pool horizontal well drilling.Along with continuing to increase of the unconventional energy resource exploration and development dynamics such as shale oil gas, tight sand oil gas, whole world drilling fluid service enters " oil base drilling fluid epoch ".Oil-based drill cuttings contains the pollutant such as petroleum hydrocarbon, heavy metal and Organic substance because of it, has been put into National Hazard garbage (National Hazard refuse register, HW08), if the most treated the most directly discharge, it will periphery ecological environment is caused serious harm.Oil base drilling fluid is used by China and research is started late, and the concrete Abgasgesetz about oil-based drill cuttings is still central in formulation.Therefore, the oil-based drill cuttings oil-containing measurement technique after process is oil base drilling fluid another important technology in addition to preparation.Current patent focuses primarily upon in the preparation of oil base drilling fluid and the process of oil-based drill cuttings, and open to the almost blank of the oil-based drill cuttings oil content Research on measuring technique after processing, the most any Patents and non-patent literature.
The technology measured based on landwaste oil content is a lot, and such as chromatograph (rock pyrolysis), spectrum (quantitative fluorescence), wave spectrum (nuclear magnetic resonance, NMR) etc., but these technology are not suitable for the oil-based drill cuttings after processing.This is because: one, use the well section of oil base drilling fluid to be the unconventional reservoir of tool nanoscale hole or be prone to the igneous rock formation etc. caved in, and creep into frequently with PDC drill bit or composite drill bit, resolution and the suitability to conventional nuclear magnetic resonance logging instrument propose challenge；Two is that oily mud shale is reservoir rock and hydrocarbon source rock, uses pyrolytic technique to measure oil-based drill cuttings residue oil content, is inevitably affected by parent rock organic matter.Three is that the oil content of oil-based drill cuttings may be higher, the range of linearity of quantitative fluorescence is the narrowest (20mg/l), needing by many times or could measure within being repeatedly diluted to its range of linearity, this inevitably introduces error, causes measurement result not accurate enough.Four is that the treatment technology of oil-based drill cuttings is varied, plants including materializing strategy, biological treatment etc. more than ten, and existing landwaste oil-containing measurement technique can not be the most applicable.There is a small amount of research to relate to oil content and/or the oil content analysis of oil base drilling fluid at present, but be not related to the oil content after oil base landwaste processes and/or oil-containing measurement technique.Therefore, this area need badly a kind of can the effectively oil content of oil-based drill cuttings after measurement processing and/or the side of oil content
Method.
Summary of the invention
Instant invention overcomes the deficiency in terms of current landwaste oil-containing measurement technique oil-based drill cuttings oil content measurement after treatment, provide oil content and/or the method for oil content of the oil-based drill cuttings after a kind of new measurement processing, it is easy by high-resolution fluid nuclear magnetic resonance technique, accurately measure process after oil-based drill cuttings oil content and/or oil content, provide a kind of effective Means of Ensuring for environmental protection with healthy.
Oil content and/or the oil content measuring method of the oil-based drill cuttings after a kind of process that the present invention provides comprise the steps:
1) mix with one or more oil base drilling fluid base oils of different quality with the not organic reagent of hydrogen atoms, and carry out Nuclear Magnetic Resonance Measurement, set up T2Spectrum oil peak area (Si) and base oil quality (Mi) linear equation: Mi=k × Si+b；
2) weigh the oil-based drill cuttings after process, be M by its quality record1, all pour in container after grinding；
3) measure the organic reagent of not hydrogen atoms, its volume is designated as V1, pour step 2 into) described in container in, shake up, stand, realize extraction；
4) from step 3) container measure volume V2Solution, condition is V2<V1, then carried out Nuclear Magnetic Resonance Measurement, recorded T2Spectral peak area is S2；
5) by following equation, the oil content of the oil-based drill cuttings after calculating process and/or oil content:
In oil-based drill cuttings, the signal area of remaining oil is:
In oil-based drill cuttings, the quality of remaining oil is: Mi=k × S1+ b,
Oil-based drill cuttings oil content after process is:
Oil-based drill cuttings oil content after process is:
Wherein, step 1) in, due to the described organic reagent not hydrogen atoms as organic extractant, this organic reagent does not has a NMR signal, thus T2Spectrum or T2-D is (by T2 T2The two-dimensional spectrum constituted with diffusion coefficient D) peak be the signal response of base oil such that it is able to use oil content and/or the oil content of the oil-based drill cuttings after technique scheme measurement processing easily.
Described oil-based drill cuttings is during with oil base drilling fluid drilling well, oil base drilling fluid carry and return out
Landwaste.Remaining oil described in oil-based drill cuttings is remaining oil after treatment, such as the remaining oil after burning disposal, wherein potentially includes the oil in stratum.
Described T2Oil peak area refers to oil peak spectral line and T2The area of axle institute envelope, base oil quality is the quality of the base oil weighed with instruments such as such as electronic balances.
Step 1) in use linear regression method commonly used in the art set up described linear equation.
Step 2) described in " all pouring into " refer to pour into as fully as possible in the zone of reasonableness of technical licensing, i.e. do not have not pour in described container in the zone of reasonableness of technical licensing by the oil-based drill cuttings after perception or measurable process.
Organic reagent of the present invention is analytical pure.
One of the present invention preferred embodiment in, step 1) described in oil base drilling fluid base oil be white oil, diesel oil, mineral oil, vegetable oil or its any mixture, preferably white oil, diesel oil or its mixture.
One of the present invention preferred embodiment in, step 1) described in the organic reagent of not hydrogen atoms be carbon tetrachloride, Carbon bisulfide or its any mixture, preferably carbon tetrachloride.Carbon tetrachloride is organic extractant, and not hydrogen atoms, because not having signal for measuring the nuclear magnetic resonance technique of hydrogen spectrum
One of the present invention preferred embodiment in, step 2) described in process as to process by one or more in burning method, ablution, solidification method, heat treating process, centrifuging and extraction.
One of the present invention preferred embodiment in, step 2) described in weigh as accurately weighing for the balance that service precision is 1/1000g or higher precision, it is preferable to use precision is that the balance of 1/10000g or higher precision accurately weighs.
One of the present invention preferred embodiment in, step 2) described in the sealing container that container is with closure, the preferably glass container of with closure, more preferably wide mouthed bottle or cuvette.
One of the present invention preferred embodiment in, step 2) described in grind as claying into power in mortar.
One of the present invention preferred embodiment in, step 3) described in the time of repose that stands be 5-15 minute, preferably 10 minutes.
It is a further object of the invention to provide and measuring according to above-mentioned method and/or processing the application in oil-based drill cuttings.One of the present invention preferred embodiment in, described oil-based drill cuttings comes from nano-pore stratum or is certainly conigenous storage stratum.
It is still another object of the present invention to provide and measuring according to above-mentioned method and/or processing the application in oil-based drill cuttings, it is characterised in that described oil-based drill cuttings uses PDC drill bit to exploit in recovery process.
The beneficial effects of the present invention is:
The present invention could be used without the not hydrogen atoms of NMR signal organic reagent extraction oil-based drill cuttings in remaining oil, by Monitoring lower-cut can reach 20mg/l, the upper limit can to 100% high-resolution low-field nuclear magnetic resonance technology realize oil-based drill cuttings process after remain oil content quick, accurately analyze.Instant invention overcomes conventional nuclear magnetic resonance technique, pyrolysis analysis analysis, quantitative fluorescence technology etc. to nano-pore stratum, PDC drill bit, be certainly conigenous the incomplete adaptability of storage stratum, different base oil classification, different oil-based drill cuttings processing methods etc., method is easy, reliable, and easily operates.The present invention is easy by high-resolution fluid nuclear magnetic resonance technique, accurately measure process after oil-based drill cuttings oil content, can detect whether oil-based drill cuttings has reached the standard of environmental protection (such as, the HSE management regulation relevant to oilfield enterprise), provide a kind of effective Means of Ensuring for environmental protection with healthy.
Accompanying drawing explanation
Fig. 1 is T2Compose the graph of a relation between peak area and oil quality that oils.
Fig. 2 is the T of carbon tetrachloride2Spectrum and T2-D two-dimensional spectrum.Wherein, Fig. 2 A is the T of carbon tetrachloride2Spectrum, because carbon tetrachloride is contained in vial, has faint signal, and amplitude is less than 0.35, for noise；Fig. 2 B is the two-dimensional spectrum of carbon tetrachloride, and also without 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, the T after Fig. 3 A is carbon tetrachloride and addition crude oil2Spectrum, it can be seen that the noise of carbon tetrachloride and sample bottle is suppressed；Fig. 3 B is the T after carbon tetrachloride adds crude oil2-D two-dimensional spectrum, noise is the most suppressed.
Fig. 4 be different lithology difference drill bit process after oil-based drill cuttings, carbon tetrachloride extraction liquid T2Spectrum.
Fig. 5 is the oil-based drill cuttings of different disposal method, carbon tetrachloride extraction liquid T2Spectrum.
Detailed description of the invention
Below by way of specific embodiment, the present invention is further detailed.It should be noted that following example are illustrative, and the scope of protection of present invention is not constituted any restriction.It will be understood by those skilled in the art that any improvement for detailed description below or change, in the case of without departing from the spirit and scope of the invention, all in the scope of protection of present invention.
Embodiment 1: the oil content of the oil-based drill cuttings after measurement processing and the method for oil content
Mix with the multiple oil base drilling fluid base oil of different quality with carbon tetrachloride solution, and carry out Nuclear Magnetic Resonance Measurement (oil quality of the multiple oil base drilling fluid base oil of different quality and the oil sample peak area recorded see table 1), set up T2Spectrum oil peak area (Si) and base oil quality (Mi) linear equation: Mi=0.2248Si+ 6.3755 (see Fig. 1).Due to described organic solvent not hydrogen atoms, this organic reagent does not has a NMR signal (see Fig. 2), thus T2Spectrum or T2The peak of-D is signal response (see Fig. 3) of base oil.
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 the oil-based drill cuttings 10000mg after the electronic balance of 1/10000g accurately weighs process, all put in glass container after mortar is pulverized, add the analytically pure carbon tetrachloride of 50ml, after soaking 10min, take 5ml extract and carry out nuclear magnetic resonance spectroscopy, signal area (the i.e. T recorded2Spectral peak area) be 152.121251, then:
In oil-based drill cuttings, the signal area of remaining oil is:
In oil-based drill cuttings, the quality of remaining oil is: Mi=0.2248 × S1+ 6.3755=342.60612mg
Oil content after oil-based drill cuttings processes is:
Oil content after oil-based drill cuttings processes is:
Oil-based drill cuttings oil content after i.e. processing is 3.4261%.
Embodiment 2:
The method described in embodiment 1 of employing, respectively to nano-pore tight sand formation (stone wheel drill bit), certainly come from storage shale formation (PDC drill bit), be certainly conigenous the oil-based drill cuttings after storage shale formation (rifler) processes and carry out the measurement of oil content and oil content.Oil-based drill cuttings after the process of these different lithology difference drill bits, carbon tetrachloride extraction liquid T2Spectrum different lithology and the oil-based drill cuttings of different bite type, T after carbon tetrachloride organic solvent extracts after process2Spectrum is shown in Fig. 4.
It can be seen that the method for the present invention is applicable to different lithology and different types of drill bit exploits the oil-based drill cuttings obtained.
Embodiment 3
The method described in embodiment 1, the oil-based drill cuttings after respectively method by centrifugation, extraction and ablution being processed is used to carry out the measurement of oil content and oil content.The oil-based drill cuttings after the process of these distinct methods T after carbon tetrachloride organic solvent extracts2Spectrum is shown in Fig. 5.
It can be seen that the method for the present invention is applicable to the oil-based drill cuttings after different disposal method processes.
Claims (10)
1. the oil content of the oil-based drill cuttings after processing and/or a measuring method for oil content, comprise the steps:
1) mix with one or more oil base drilling fluid base oils of the organic reagent of not hydrogen atoms with different quality
Close, and carry out Nuclear Magnetic Resonance Measurement, set up T2Spectrum oil peak area (Si) and base oil quality (Mi) linear
Equation: Mi=k × Si+ b, wherein k and b is constant；
2) weigh the oil-based drill cuttings after process, be M by its quality record1, all pour in container after grinding；
3) measure the organic reagent of not hydrogen atoms, its volume is designated as V1, pour step 2 into) described in appearance
In device, shake up, stand, realize extraction；
4) from step 3) container measure volume V2Solution, condition is V2<V1, then carried out
Nuclear Magnetic Resonance Measurement, records T2Spectral peak area is S2；
5) by following equation, the oil content of the oil-based drill cuttings after calculating process and/or oil content:
In oil-based drill cuttings, the signal area of remaining oil is:
In oil-based drill cuttings, the quality of remaining oil is: Mi=k × S1+b,
Oil-based drill cuttings oil content after process is:
Oil-based drill cuttings oil content after process is:
Method the most according to claim 1, it is characterised in that step 1) described in oil base drilling fluid base
Plinth oil is white oil, diesel oil, mineral oil, vegetable oil or its any mixture, preferably white oil, diesel oil or its mix
Compound.
Method the most according to claim 1 and 2, it is characterised in that step 1) and step 3) in institute
The organic reagent stating not hydrogen atoms is carbon tetrachloride, Carbon bisulfide or its any mixture, preferably four chlorinations
Carbon.
4. according to the method described in any one in claim 1-3, it is characterised in that step 2) described in
Process as by the one or many in burning method, ablution, solidification method, heat treating process, centrifuging and extraction
Plant and process.
5. according to the method described in any one in claim 1-4, it is characterised in that step 2) described in
The balance for service precision is 1/1000g or higher precision that weighs accurately weigh, it is preferable to use essence
Degree accurately weighs for the balance of 1/10000g or higher precision.
6. according to the method described in any one in claim 1-5, it is characterised in that step 2) described in
The sealing container that container is with closure, the preferably glass container of with closure.
7. according to the method described in any one in claim 1-6, it is characterised in that step 2) described in
Grind as claying into power in mortar.
8. according to the method described in any one in claim 1-7, it is characterised in that step 3) described in
The time of repose stood is 5-15 minute, preferably 10 minutes.
9. measuring according to the method described in any one in claim 1-8 and/or processing in oil-based drill cuttings
Application, preferably comes from nanometer according to the method described in any one in claim 1-8 in measurement and/or process
Stratum, hole or certainly be conigenous storage stratum oil-based drill cuttings in application.
10. measuring according to the method described in any one in claim 1-8 and/or processing in oil-based drill cuttings
Application, it is characterised in that described oil-based drill cuttings uses PDC drill bit to exploit in recovery process.
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| CN106841269A (en) * | 2017-01-12 | 2017-06-13 | 西南石油大学 | A kind of method that utilization nuclear magnetic resonance evaluates rejected well drilling liquid separation of solid and liquid |
| CN108645883A (en) * | 2018-05-11 | 2018-10-12 | 苏州纽迈分析仪器股份有限公司 | A kind of method that crude oil water content is quickly detected in oil field |
| CN109386282A (en) * | 2017-08-09 | 2019-02-26 | 中国石油化工股份有限公司 | Bored under the conditions of a kind of oil emulsion drilling fluid meet oil reservoir sentence knowledge method |
| 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 |
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| CN113533156A (en) * | 2021-06-30 | 2021-10-22 | 西安石油大学 | Identification method for microscopic pore structure characteristics and multi-type pore fluid of shale oil reservoir |
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| CN113970500A (en) * | 2021-10-27 | 2022-01-25 | 北京新风航天装备有限公司 | Method for rapidly measuring oil content of oil stain solid waste |
| 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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