CN103018147A - Method for measuring total porosity of shale - Google Patents
Method for measuring total porosity of shale Download PDFInfo
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- CN103018147A CN103018147A CN2012104768919A CN201210476891A CN103018147A CN 103018147 A CN103018147 A CN 103018147A CN 2012104768919 A CN2012104768919 A CN 2012104768919A CN 201210476891 A CN201210476891 A CN 201210476891A CN 103018147 A CN103018147 A CN 103018147A
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Abstract
The invention discloses a method for measuring the total porosity of shale, which is applied to laboratories for oil exploration, geological exploration and mineral exploration to perform a shale measurement. The method is characterized by comprising the following steps of: measuring the apparent volume of a shale sample; crushing the same sample used aforementioned to 100-200 meshes; performing drying treatment for 24-48 hours at 60-80 DEG C; performing cyclic crushing on the shale sample into fine particles which are 100-1000 nm in diameter by an auxiliary liquid, and measuring the volume of the consumed auxiliary liquid; and measuring the volume of the mixed liquid of the auxiliary liquid and the shale sample after the cyclic crushing, and calculating to obtain the total porosity of the shale sample. The method has the effects of being capable of measuring the total porosity of shale and high in measurement accuracy.
Description
Technical field
The present invention relates to oil, geology, mining industry exploratory development technical field, particularly a kind of mud shale that carries out in the laboratory is measured, and is a kind of method of measuring the mud shale total porosity.
Background technology
In the exploratory development process to shale oil gas, total porosity is to calculate oil shale fuel, shale gas stock number and formulate one of key parameter of recovery scheme.The total porosity of oil shale fuel and shale gas reservoir directly affects the stock number of oil shale fuel, shale gas, and is used for estimating the production cycle of oil shale fuel, shale gas well.The source bed of oil shale fuel and shale gas and reservoir are same set of mud shale, and sizable a part of hole is disconnected mutually in the mud shale, i.e. " stagnant pore ".The attached oil gas of depositing can be for exploitation through fracturing reform in this part mutual disconnected hole, therefore need to measure the total porosity of oil shale fuel gas reservoir, so that the stock number of shale oil gas is calculated, and the production cycle of oil shale fuel gas well is assessed.At present, the basic skills of measurement blowhole comprises: gas method, liquid processes.Gas method is that rock sample is put into obturator, is filled with gases at high pressure in device, asks for rock porosity according to Boyle law; Liquid processes is that rock sample is vacuumized saturated kerosene (perhaps saturated alcohol), utilizes the weight difference of the saturated kerosene of rock sample front and back to ask for factor of porosity.But these methods all can only be measured the hole that is interconnected in the rock, and can't measure the size of mutual nonconductive pore, namely can only measure net porosity, can't measure total porosity.Therefore, with the basic skills of measuring blowhole the oil shale fuel gas reservoir is estimated and to be made porosity value less than normal, can not truly reflect the total porosity of shale reservoir, and then affect that shale oil gas stock number is calculated and the production cycle of oil shale fuel gas well is assessed.
Those skilled in the art's immersion method commonly used is measured the apparent volume of mud shale sample.Can measure its volume with immersion method for the water insoluble sample in irregular shape that does not also absorb water.Testing sample all is submerged in water, and the volume differences of twice reading is the apparent volume of sample.Mud shale sample for suction can replace hydromining to measure its apparent volume with immersion method with fine powder (such as flour sand, flour etc.).
By patent retrieval, Chinese patent, 201110155601 applications for a patent for invention of having announced " method for measuring porosity of mud shale " (application publication number: CN 102252948A) have larger defective in principle: think mud shale pulverize before and pulverize after density identical, use the sample quality M after the pulverizing
1With density p before the pulverizing
bRatio ask for volume before pulverizing.In the mud shale crushing process, (be crushed to granularity less than the minimum non-open pore of sample, the grain size that is equivalent to Nano grade) can produce large calorimetric, water in the mud shale, wet goods fluid are discharged from the pulverizing sample because heating becomes gaseous state, change with the density of pulverizing rear mud shale sample before pulverizing like this.There is deviation in the mud shale factor of porosity that calculates like this.For this reason, the present invention adopts locking device to utilize circulation fluid (can play the effect of cooling, circulation) to pulverizings that circulate of mud shale sample, by before pulverizing and the volume change after the pulverizing ask for the mud shale factor of porosity and have higher precision.
Summary of the invention
The objective of the invention is: a kind of method of measuring the mud shale total porosity is provided, realizes the accurate measurement to the mud shale total porosity.Overcome the deficiency that prior art, method are difficult to the total porosity of Measurement accuracy mud shale.Another object of the present invention is: a kind of device of measuring the mud shale total porosity is provided, has been used for realizing measuring the method for mud shale total porosity.
The technical solution used in the present invention is: measure the method for mud shale total porosity, it is characterized in that:
Step 1: with the apparent volume of immersion method or vernier caliper measurement mud shale sample, record apparent volume V
1, the unit of apparent volume is cm
3
Step 2: above-mentioned same a mud shale sample is crushed to 100～200 orders;
Step 3: the mud shale sample of above-mentioned pulverizing is carried out drying and processing under 60～80 ℃ of temperature, drying time is 24～48 hours, removes water and hydro carbons in the mud shale sample;
Step 4: mud shale sample and the auxiliary liquid of above-mentioned oven dry are mixed the pulverizing that circulates, the circulation of mud shale sample is crushed to the fine particle of diameter 100～1000nm; And the long-pending V of stoichiometric consumption auxiliary liquid
2, consume the long-pending V of auxiliary liquid
2Unit be mL;
Step 5: the mixing material cumulative volume V that measures auxiliary liquid and mud shale sample fine particle
3, measure the mixing material cumulative volume V that assists liquid and mud shale sample fine particle
3Unit be mL;
Step 6: according to the total porosity Φ of following formula calculating mud shale sample, the unit of the total porosity Φ of mud shale sample is %:
φ=(V
1-(V
3-V
2))/V
1×100%
When the right cylinder of mud shale sample shape rule, utilize vernier caliper measurement mud shale sample diameter and ask for highly again mud shale sample apparent volume; When the mud shale sample shape is non-cylinder, measure the apparent volume of mud shale sample with immersion method.
Auxiliary liquid can be alcohol, kerosene, distilled water etc.
The stoichiometric consumption auxiliary liquid amasss V
2Before will assisting liquid to add the circulation reducing mechanism with high precision measuring cylinder (the high precision measuring cylinder patent publication No.: CN202420600U) measure the volume of pouring auxiliary liquid into, this volume be the auxiliary liquid that consumes amass V
2, measurement volumes is accurate to 0.01mL.
Measure the mixing material cumulative volume V of auxiliary liquid and mud shale sample fine particle
3After end is pulverized in circulation, the mixing material of auxiliary liquid and mud shale sample fine particle is discharged from the circulation reducing mechanism, with high precision measuring cylinder (high precision measuring cylinder patent publication No.: CN202420600U) measure this mixeding liquid volume V
3, measuring accuracy reaches 0.01mL.
Described circulation is pulverized and is carried out in the circulation reducing mechanism.Described circulation reducing mechanism comprises the first valve (1), the second valve (2), the 3rd valve (3), upper U-shaped glass tube A, lower U-shaped glass tube D, micromill (B) and pony pump (C).Upper U-shaped glass tube A is relative respectively with the U-shaped mouth of lower U-shaped glass tube D; A port of upper U-shaped glass tube (A) links to each other by rubber hose with the discharging opening of micromill (B), and the charging aperture of micromill (B) links to each other by rubber hose with the port of lower U-shaped glass tube D; Another port of upper U-shaped glass tube (A) links to each other by rubber hose with the charging aperture of pony pump C, and the discharging opening of pony pump C links to each other by rubber hose with another port of lower U-shaped glass tube D; Top at upper U-shaped glass tube (A) is connected with the charging mouth of pipe, and the first valve 1 is arranged at the bottom of the charging mouth of pipe, at second valve 2 that has of upper U-shaped glass tube A; Bottom at lower U-shaped glass tube D is connected with the discharging mouth of pipe, is connected with the 3rd valve 3 on the discharging mouth of pipe.
The use of circulation reducing mechanism.Before the mud shale sample is pulverized in circulation, need to open the first valve (1), the second valve (2) and the 3rd valve (3), pour auxiliary liquid into by the charging mouth of pipe of upper U-shaped glass tube (A) and the circulation reducing mechanism is carried out wetting, the wetting auxiliary liquid that consumes is not counted in the long-pending V of the auxiliary liquid that consumes
2In the circulation crushing process, close the second valve (2) and the 3rd valve (3), pour the good mud shale sample of drying and processing and the auxiliary liquid of part into by upper U-shaped glass tube (A) the upper end charging mouth of pipe, opening the second valve (2) continues to pour auxiliary liquid into by upper U-shaped glass tube (A) upper end charging aperture, when auxiliary liquid is full of upper U-shaped glass tube (A) and lower U-shaped glass tube D soon, stop to add auxiliary liquid, close the first valve (1); Open micromill (B) and small-sized electric pump (C), the mud shale sample is circulated pulverize and the degree of grinding of adjusting micromill (B).Mud shale sample circulation pulverizing is the fine particle of diameter 100～1000nm; Close micromill (B) and small-sized electric pump (C), open the first valve (1) and the 3rd valve (3), under the discharging mouth of pipe of lower U-shaped glass tube D bottom, collect the mixed liquor of auxiliary liquid and mud shale fine particle with container, and pour auxiliary liquid clean cycle reducing mechanism into by the charging mouth of pipe of upper U-shaped glass tube (A) upper end, the auxiliary liquid of the residual mud shale fine particle in the clean cycle reducing mechanism is also flowed out by the discharging mouth of pipe of lower U-shaped glass tube D bottom and uses surface vessel and collect together, at last metering except wetting circulating device the auxiliary liquid that consumes amass V
2
Beneficial effect of the present invention: the present invention measures the method for mud shale total porosity, realized the accurate measurement to the mud shale total porosity, and this measuring method expense is cheap, simple to operate, and measured mud shale reservoir total porosity is necessary important evaluating in the exploration and development of shale oil gas.
Description of drawings
Fig. 1 is the method flow synoptic diagram that the present invention measures the mud shale total porosity.
Fig. 2 is circulation reducing mechanism structural representation.
Among the figure, 1-the first valve, 2-the second valve, 3-the 3rd valve, the upper U-shaped glass tube of A-, B-micromill, C-pony pump, U-shaped glass tube under the D-.
Embodiment
Embodiment 1: take the method for one-shot measurement mud shale total porosity as example, the present invention is described in further detail.
Consult Fig. 2.The circulation reducing mechanism comprises the first valve (1), the second valve (2), the 3rd valve (3), upper U-shaped glass tube A, lower U-shaped glass tube D, micromill (B) and pony pump (C).The model of micromill B is ZM 200; The model of pony pump C is WT3000-1JA.
The internal diameter of upper U-shaped glass tube A and lower U-shaped glass tube D is 40mm.Upper U-shaped glass tube A is relative respectively with the U-shaped mouth of lower U-shaped glass tube D; A port of upper U-shaped glass tube (A) links to each other by rubber hose with the discharging opening of micromill (B), and the charging aperture of micromill (B) links to each other by rubber hose with the port of lower U-shaped glass tube D; Another port of upper U-shaped glass tube (A) links to each other by rubber hose with the charging aperture of pony pump C, and the discharging opening of pony pump C links to each other by rubber hose with another port of lower U-shaped glass tube D; Top at upper U-shaped glass tube (A) is connected with the charging mouth of pipe, and the first valve 1 is arranged at the bottom of the charging mouth of pipe, at second valve 2 that has of upper U-shaped glass tube A; Bottom at lower U-shaped glass tube D is connected with the discharging mouth of pipe, is connected with the 3rd valve 3 on the discharging mouth of pipe.Capacity 2500mL in the circulation reducing mechanism.
Consult Fig. 1.Measure the method for mud shale total porosity:
Step 1: with the apparent volume of immersion method measurement mud shale sample, the apparent volume of mud shale sample is 25.14 cubic centimetres.Record apparent volume V
125.14 cubic millimeter;
Step 2: the mud shale sample of above-mentioned measurement apparent volume is crushed to 150 orders;
Step 3: the mud shale sample of above-mentioned pulverizing is carried out drying and processing under 70 ℃ of temperature, drying time is 48 hours, removes water and hydro carbons in the mud shale sample;
Step 4: mud shale sample and the auxiliary liquid of above-mentioned oven dry are mixed the pulverizing that circulates, the circulation of mud shale sample is crushed to the fine particle of diameter 800nm; And the long-pending V of stoichiometric consumption auxiliary liquid
2, consume the long-pending V of auxiliary liquid
2It is 1834.25 milliliters;
Step 5: the mixing material cumulative volume V that measures auxiliary liquid and mud shale sample fine particle
3Measure the mixing material cumulative volume V of auxiliary liquid and mud shale sample fine particle
3It is 1850.32 milliliters;
Step 6: according to the total porosity Φ of following formula calculating mud shale sample, the unit of the total porosity Φ of mud shale sample is %:
φ=(V
1-(V
3-V
2))/V
1×100%
At last, the total porosity Φ that calculates the mud shale sample that this detection obtains is 3.61%
The kerosene that auxiliary liquid uses.
The stoichiometric consumption auxiliary liquid amasss V
2Before will assisting liquid to add the circulation reducing mechanism with high precision measuring cylinder (the high precision measuring cylinder patent publication No.: CN202420600U) measure the volume of pouring auxiliary liquid into, this volume be the auxiliary liquid that consumes amass V
2, measurement volumes is accurate to 0.01mL.
Measure the mixing material cumulative volume V of auxiliary liquid and mud shale sample fine particle
3After end is pulverized in circulation, the mixing material of auxiliary liquid and mud shale sample fine particle is discharged from the circulation reducing mechanism, with high precision measuring cylinder (high precision measuring cylinder patent publication No.: CN202420600U) measure this mixeding liquid volume V
3, measuring accuracy reaches 0.01mL.
Described circulation is pulverized and is carried out in the circulation reducing mechanism.
Claims (2)
1. method of measuring the mud shale total porosity is characterized in that:
Step 1: with the apparent volume of immersion method or vernier caliper measurement mud shale sample, record apparent volume V
1, the unit of apparent volume is cm
3
Step 2: above-mentioned same a mud shale sample is crushed to 100～200 orders;
Step 3: the mud shale sample of above-mentioned pulverizing is carried out drying and processing under 60～80 ℃ of temperature, drying time is 24～48 hours, removes water and hydro carbons in the mud shale sample;
Step 4: mud shale sample and the auxiliary liquid of above-mentioned oven dry are mixed the pulverizing that circulates, the circulation of mud shale sample is crushed to the fine particle of diameter 100～1000nm; And the long-pending V of stoichiometric consumption auxiliary liquid
2, consume the long-pending V of auxiliary liquid
2Unit be mL;
Step 5: the mixing material cumulative volume V that measures auxiliary liquid and mud shale sample fine particle
3, measure the mixing material cumulative volume V that assists liquid and mud shale sample fine particle
3Unit be mL.
Step 6: according to the total porosity Φ of following formula calculating mud shale sample, the unit of the total porosity Φ of mud shale sample is %:
φ=(V
1-(V
3-V
2))/V
1×100%
When the right cylinder of mud shale sample shape rule, utilize vernier caliper measurement mud shale sample diameter and ask for highly again mud shale sample apparent volume; When the mud shale sample shape is irregular, measure the apparent volume of mud shale sample with immersion method.
Auxiliary liquid can be alcohol, kerosene, distilled water etc.
The stoichiometric consumption auxiliary liquid amasss V
2Before will assisting liquid to add the circulation reducing mechanism, pour the volume of auxiliary liquid into high precision measuring cylinder measurements, this volume be the auxiliary liquid that consumes amass V
2, measurement volumes is accurate to 0.01mL.
Measure the mixing material cumulative volume V of auxiliary liquid and mud shale sample fine particle
3After end is pulverized in circulation, the mixing material of auxiliary liquid and mud shale sample fine particle is discharged from the circulation reducing mechanism, measure this mixeding liquid volume V with high precision measuring cylinder
3, measuring accuracy reaches 0.01mL.
2. the method for measurement mud shale total porosity according to claim 1 is characterized in that: described circulation is pulverized and is carried out in the circulation reducing mechanism.Described circulation reducing mechanism comprises the first valve (1), the second valve (2), the 3rd valve (3), upper U-shaped glass tube A, lower U-shaped glass tube D, micromill (B) and pony pump (C), and upper U-shaped glass tube (A) is relative respectively with the U-shaped mouth of lower U-shaped glass tube D; A port of upper U-shaped glass tube (A) links to each other by rubber hose with the discharging opening of micromill (B), and the charging aperture of micromill (B) links to each other by rubber hose with the port of lower U-shaped glass tube D; Another port of upper U-shaped glass tube (A) links to each other by rubber hose with the charging aperture of pony pump C, and the discharging opening of pony pump C links to each other by rubber hose with another port of lower U-shaped glass tube D; Top at upper U-shaped glass tube (A) is connected with the charging mouth of pipe, and the first valve 1 is arranged at the bottom of the charging mouth of pipe, at second valve 2 that has of upper U-shaped glass tube A; Bottom at lower U-shaped glass tube D is connected with the discharging mouth of pipe, is connected with the 3rd valve 3 on the discharging mouth of pipe.
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Cited By (11)
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| CN103674802A (en) * | 2013-11-05 | 2014-03-26 | 中国石油天然气股份有限公司 | Rock closed porosity determination method |
| CN103760082A (en) * | 2014-01-08 | 2014-04-30 | 中国石油天然气股份有限公司 | Shale layer system tight reservoir crude oil effective movable space determination method and device |
| CN103822866A (en) * | 2014-03-21 | 2014-05-28 | 中国石油大学(华东) | Method for evaluating porosity of mud shale at objective layer segment |
| CN104729971A (en) * | 2015-04-08 | 2015-06-24 | 中国石油大学(华东) | Rock nano CT pore calibration method |
| CN105092448A (en) * | 2015-07-01 | 2015-11-25 | 中国石油天然气股份有限公司 | Method for testing pore size distribution of tight reservoir rock pores |
| CN105445161A (en) * | 2015-11-16 | 2016-03-30 | 中国石油大学(北京) | Characterizing method for pore volumes of full apertures of shale |
| CN108872045A (en) * | 2018-08-06 | 2018-11-23 | 四川杰瑞泰克科技有限公司 | A kind of measurement method of the broken sample total porosity of shale |
| CN111537390A (en) * | 2020-06-11 | 2020-08-14 | 中国石油大学(华东) | Method for evaluating increment of organic porosity of reservoir during shale oil thermal upgrading exploitation |
| CN111650108A (en) * | 2020-06-19 | 2020-09-11 | 中国石油天然气股份有限公司 | Method and device for measuring effective porosity of shale rock |
| CN112345694A (en) * | 2020-10-20 | 2021-02-09 | 西北农林科技大学 | Method for measuring tightness of string-shaped fruits |
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| CN103674802B (en) * | 2013-11-05 | 2017-01-18 | 中国石油天然气股份有限公司 | Rock closed porosity determination method |
| CN103674802A (en) * | 2013-11-05 | 2014-03-26 | 中国石油天然气股份有限公司 | Rock closed porosity determination method |
| CN103760082A (en) * | 2014-01-08 | 2014-04-30 | 中国石油天然气股份有限公司 | Shale layer system tight reservoir crude oil effective movable space determination method and device |
| CN103760082B (en) * | 2014-01-08 | 2015-12-02 | 中国石油天然气股份有限公司 | Shale layer system tight reservoir crude oil effective movable space determination method and device |
| CN103822866A (en) * | 2014-03-21 | 2014-05-28 | 中国石油大学(华东) | Method for evaluating porosity of mud shale at objective layer segment |
| CN103822866B (en) * | 2014-03-21 | 2016-04-20 | 中国石油大学(华东) | A kind of evaluation objective interval mud shale porosity method |
| CN104729971A (en) * | 2015-04-08 | 2015-06-24 | 中国石油大学(华东) | Rock nano CT pore calibration method |
| CN104729971B (en) * | 2015-04-08 | 2017-02-22 | 中国石油大学(华东) | Rock nano CT pore calibration method |
| CN105092448A (en) * | 2015-07-01 | 2015-11-25 | 中国石油天然气股份有限公司 | Method for testing pore size distribution of tight reservoir rock pores |
| CN105092448B (en) * | 2015-07-01 | 2018-02-02 | 中国石油天然气股份有限公司 | Method for testing pore size distribution of tight reservoir rock pores |
| CN105445161A (en) * | 2015-11-16 | 2016-03-30 | 中国石油大学(北京) | Characterizing method for pore volumes of full apertures of shale |
| CN105445161B (en) * | 2015-11-16 | 2018-07-27 | 中国石油大学(北京) | The characterizing method of shale full aperture pore volume |
| CN108872045A (en) * | 2018-08-06 | 2018-11-23 | 四川杰瑞泰克科技有限公司 | A kind of measurement method of the broken sample total porosity of shale |
| CN111537390A (en) * | 2020-06-11 | 2020-08-14 | 中国石油大学(华东) | Method for evaluating increment of organic porosity of reservoir during shale oil thermal upgrading exploitation |
| CN111650108A (en) * | 2020-06-19 | 2020-09-11 | 中国石油天然气股份有限公司 | Method and device for measuring effective porosity of shale rock |
| CN111650108B (en) * | 2020-06-19 | 2022-12-16 | 中国石油天然气股份有限公司 | Method and device for measuring effective porosity of shale rock |
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| CN112504933A (en) * | 2020-11-19 | 2021-03-16 | 王云帅 | Porosity measuring device for predicting shale oil geological desserts |
| CN112504933B (en) * | 2020-11-19 | 2023-09-26 | 西安润丰源石化科技有限公司 | Porosity measuring device for shale oil geological dessert prediction |
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