CN107917999A - A kind of acid/base liquid corrodes the research method of reservoir rock dynamic characteristic - Google Patents
A kind of acid/base liquid corrodes the research method of reservoir rock dynamic characteristic Download PDFInfo
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Abstract
The invention discloses the research method that a kind of acid/base liquid corrodes reservoir rock dynamic characteristic, belong to Reservoir Development field.Research method includes：Etchant is configured, measures and records the pH value of the etchant；Weigh mineral samplers and record its quality m1, mineral samplers and etchant are mixed and are reacted in the reactor of sealing, after question response, measures and records the pH value of reaction mixture；Reaction mixture is stood, is filtered, obtains solid product, cleaning solid product is in neutrality up to filtrate, obtains remaining sample, then drying to constant weight by remaining sample, weighs and records the weight m of the remaining sample2；Reaction rate is calculated, reaction activity is calculated according to reaction rate, calculates the erosion ratio of reaction；Erosion effect of the etchant to mineral samplers is judged according to the size of erosion ratio and reaction activity.Invention has the advantages of high efficiency, cost is low, simple and practicable, has great importance to reservoir protection and its economic development.
Description
Technical field
Damaging the present invention relates to working fluid during reservoir reconstruction in Reservoir Development and reservoir protection to reservoir
Evaluation field, and in particular to a kind of acid/base liquid corrodes the research method of reservoir rock dynamic characteristic.
Background technology
With the continuous development of petroleum exploration and development technological means, more and more complicated fine and close oil-gas reservoir input exploitations,
Acid fracturing becomes the important technical of reservoir reconstruction.Due to the complexity of Reservoir Minerals the Nomenclature Composition and Structure of Complexes so that acid solution with
The reaction mechanism of reservoir rock is sufficiently complex, and causing acidizing design, there are larger blindness, the design and technique of acid formula
The optimization of parameter largely relies on field experience, has seriously affected the success rate and effective percentage of acidifying.For acid/base liquid
In terms of corroding reservoir rock dynamics, forefathers have done numerous studies work, and achieve great successes, but real indoors
Above proved recipe method, exist it is high to experimental facilities requirement, be limited to reservoir rock sample type, form and dosage, be limited to reality
The problems such as experimental group number that test fluid properties, can be carried out at the same time is few.
In view of this, it is special to propose the present invention.
The content of the invention
Existing in order to solve the problems, such as, the object of the present invention is to provide a kind of acid/base liquid to corrode reservoir rock power
The research method of feature is learned, its is efficient, cost is low, simple and practicable, has important meaning to reservoir protection and its economic development
Justice.
The technical solution that the present invention solves above-mentioned technical problem is as follows：
A kind of acid/base liquid corrodes the research method of reservoir rock dynamic characteristic, including：
(1) etchant is configured, measures and records the pH value of etchant；Weigh mineral samplers and record its quality m1, by ore deposit
Thing sample and etchant are mixed and reacted in the reactor of sealing, after question response, are measured and are recorded the pH of reaction mixture
Value；
(2) reaction mixture is stood, filtered, obtain solid product, cleaning solid product is in neutrality up to filtrate, obtains
Remaining sample, then by remaining sample, drying to constant weight, weighs and records the weight m of remaining sample2；
(3) reaction rate is calculated according to the pH value measured in step (1), reaction activity, root is calculated according to reaction rate
According to m1、m2Calculate the erosion ratio of reaction；Judge that etchant invades mineral samplers according to the size of erosion ratio and reaction activity
Effect is lost, so as to design the etchant of suitable different reservoir rock；Wherein,
(3.1) calculation formula of reaction rate is：
It is abbreviated as：J=KCm
In formula, the volume of the etchant of V-participation reaction, L；S-reaction surface surface area, cm2；The erosion of C-t moment
The concentration of liquid, mol/L；T- moment, s；K-reaction constant, (mol/L)1-m·s-1, represent reaction during reactant unit concentration
Speed；M-the order of reaction, dimensionless；J-reaction rate, mol/ (cm2·h)；
The calculation formula of reaction activity is：
In formula, K-rate constant, (mol/L)-ms-1；K0- frequency factor, (mol/L)-mL/ (cm2
s)；Ea-reaction activity, kcal/mol；R-mol gas constant, kcal/molk；T-thermodynamic temperature, kcal；
(3.2) calculation formula of erosion ratio is：
η=(m1-m2)/m1* 100%
In formula, η-erosion ratio, m1The quality of-mineral samplers；m2The quality of-solid product；m3The matter of-remaining sample
Amount.
Further, in preferred embodiments of the present invention, in step (1), reaction vessel is placed in 30-100 DEG C
Under the conditions of react 5-8h.Preferably, reaction vessel is placed under conditions of 60 DEG C and reacts 5h.Reaction time can be appropriately extended,
Reaction of being subject to fully carries out.
Further, in preferred embodiments of the present invention, research method further includes：Before the reaction, mineral samplers are dried
It is dry, until constant weight.
Further, in preferred embodiments of the present invention, research method further includes：To the mineral samplers after drying into
The measure of row chemical constituent and its content, to determine chemical composition main in mineral samplers.By to mineral samplers chemistry into
The measure divided, can specify mineral samplers Mineralss and its content, can be with comparative analysis different component for erosion ratio
Influence, the detection of ion concentration can be targetedly carried out to the solution after reaction, carrying out component to the solid phase after reaction contains
Amount detection.
Further, in preferred embodiments of the present invention, research method further includes：Mineral samplers after observation drying
Microscopic appearance, and the mineral samplers microscopic appearance feature after observing response.Observed, can measured by microscopic appearance
The arrangement form of mineral samplers each component under different eating conditions, summarizes the Erosion Law of soda acid etchant.
Further, in preferred embodiments of the present invention, research method further includes：To the mineral samplers powder after drying
It is broken.
Further, in preferred embodiments of the present invention, the material of reactor is acidproof and alkali corrosion resistance material, excellent
Selection of land, the material of reactor is polytetrafluoroethylene (PTFE).
Further, in preferred embodiments of the present invention, etchant is acid solution or lye.
The invention has the advantages that：
(1) the method for the present invention is simple, of less demanding to experimental facilities, cost is low.
(2) present invention is not only restricted to reservoir rock sample type, form and dosage, is not only restricted to Experimental Flowing Object property, fits
Ying Xingqiang, is conducive to promote.
(3) present invention can be not only used for the erosion experiments of actual reservoir mineral, can be used for studying each single mineral and more
The erosion experiment of kind Within Monominerals combination；Both it block rock sample can be used to be tested, the rock powder of different-grain diameter can also be used to carry out
Experiment.Selected experimental liquid is also unrestricted.Have great importance for further disclosing erosion mechanism.
(4) present invention can be carried out at the same time multigroup experiment, and work efficiency is high.For example, can be at the same time using more by the present invention
A independent polytetrafluoroethylene (PTFE) material, sealable reaction vessel, in digital display air dry oven (static state) or roller heating furnace
(dynamic) inner space can be carried out at the same time multigroup experiment in the case of allowing, and will not influence each other, and substantially increase experiment
Process and efficiency.
(5) during reservoir reconstruction, for corrosion formation mineral and the tamper of interstitial space, expanded hole
Gap space, improves seepage flow condition, general work on hand liquid (also known as etchant) is often the fluid of strong acid and strong base, of the invention
Using the container of polytetrafluoroethylene (PTFE) material, prolonged experiment and working solution invading for metal laboratory apparatus repeatedly are avoided
Erosion.
Brief description of the drawings
Fig. 1 (a) is the microscopic appearance figure before the kaolinite of the embodiment of the present invention 1 corrodes；
Fig. 1 (b) is the microscopic appearance figure before the kaolinite of the embodiment of the present invention 1 corrodes；
Fig. 1 (c) is the microscopic appearance figure before the kaolinite of the embodiment of the present invention 1 corrodes；
Fig. 1 (d) is the microscopic appearance figure before the kaolinite of the embodiment of the present invention 1 corrodes；
Fig. 2 (a) is the microscopic appearance figure after the kaolinite of the embodiment of the present invention 1 corrodes；
Fig. 2 (b) is the microscopic appearance figure after the kaolinite of the embodiment of the present invention 1 corrodes；
Fig. 2 (c) is the microscopic appearance figure after the kaolinite of the embodiment of the present invention 1 corrodes；
Fig. 2 (d) is the microscopic appearance figure after the kaolinite of the embodiment of the present invention 1 corrodes.
Embodiment
The principle of the present invention and feature are described with reference to embodiments, the given examples are served only to explain the present invention,
It is not intended to limit the scope of the present invention.The person that is not specified actual conditions in embodiment, suggests according to normal condition or manufacturer
Condition carries out.Reagents or instruments used without specified manufacturer, is the conventional products that can be obtained by commercially available purchase.
Before specific embodiment is introduced, first the calculation formula involved in the present invention is illustrated.
(1) reaction kinetics equation determines
It is theoretical to use for reference acid-rock reaction dynamics, acid solution erosion rate is calculated using reaction kinetics equation：
Then formula (4-1) is reduced to：
J=KCm (4-2)
In formula, the volume of the acid attack liquid of V-participation reaction, L；S-reaction surface surface area, cm2；K-reaction rate is normal
Number, (mol/L)1-m·s-1, represent reaction rate when reactant concentration is unit concentration；M-the order of reaction, represents reactant
Influence degree of the concentration to reaction speed；J-reaction rate (i.e. the unit interval flows through the amount of substance of unit rock area),
mol/(cm2·h)。
Formula (4-2) is reaction kinetics equation, and reaction speed is determined using the differential method, is depicted as relation curve, i.e.,：
Reaction kinetics equation is can obtain using power function fitting.
(2) reaction activity calculates
Temperature has a significant impact reaction rate.As a rule, its quantitative rule can by Arrhenius formula Lai
Description：
In formula, K-rate constant, (mol/L)-m·s-1；K0- frequency factor, (mol/L)-m·L/(cm2·s)；
Ea-reaction activity, kcal/mol；R-mol gas constant, kcal/molk；T-thermodynamic temperature, k.
Formula (4-4) can be write as：
Take the logarithm again on both sides：
Then, when other conditions are identical, static reaction reality is carried out at different temperatures with the etchant of same concentration
Test.It can obtain temperature T1, T2..., the reaction speed J under Tn1, J2..., Jn.Since lgJ and 1/T are linear relationship, with recurrence
Or mapping processing can obtain etchant etching reaction activation energy.
(3) calculation formula of erosion ratio：
η=(m1-m2)/m1* 100%
In formula, η-erosion ratio, m1The quality of-mineral samplers；m2The quality of-remaining sample.
By the reaction activity Ea and erosion ratio η calculated, the effect thus evaluated between etchant and mineral is closed
System, such as different etchant is to the erosion effect of mineral of the same race, or etchant of the same race is to the erosion effect of mineral not of the same race,
The optimal etchant of erosion effect is filtered out with this.Reaction activity Ea and erosion ratio η values are bigger, illustrate that reaction is more violent, invade
Erosion effect is better, conversely, then reacting weaker, erosion effect is poorer.
The acid/base liquid of the present invention corrodes the research method of reservoir rock dynamic characteristic, including：
(1) mineral or rock are broken into powder, pour into mortar and grind, until powder can be by giving mesh number scope
Sieve, such as 150 mesh, are then put into powder in air dry oven and are dried under conditions of 60 DEG C, spare.
(2) 600mL etchants are configured.In the present embodiment, etchant is mud acid solution, including hydrochloric acid and hydrofluoric acid.Survey
Determine and record the pH value of etchant；Weigh mineral samplers and record its quality m1.Mineral samplers and etchant are mixed and close
Reaction in the reactor of envelope, sets reaction temperature and reaction time.After question response, measure and record the pH of reaction mixture
Value.
(3) reaction mixture is stood, filtered, obtain solid product cleaning solid product until filtrate be in neutrality, remained
Remaining sample, then by remaining sample, drying to constant weight, weighs and records the weight m of remaining sample2；
(4) reaction rate is calculated according to the pH value measured in step (2), reaction activity, root is calculated according to reaction rate
According to m1、m2Calculate the erosion ratio of reaction.
Each embodiment is carried out according to above-mentioned steps, its reaction condition is shown in Tables 1 and 2.
The etchant of 1 various concentrations of table
2 differential responses temperature of table
In addition to above-mentioned temperature, it is 30 DEG C or 100 DEG C that the other embodiment of the present invention, which also includes temperature,.Each embodiment
Measurement result be shown in Table 3 and table 4.
The corresponding experimental result of 3 various concentrations etchant of table
The corresponding experimental result of 4 different temperatures of table
From table 3 it can be seen that certain in reaction temperature, in the case of being 70 DEG C, Acid concentration is higher, every kind of Mineral pairs
The erosion ratio answered is bigger, illustrates that erosion effect is better, wherein, will to the erosion effect of montmorillonite, kaolinite and chlorite three
It is better than to illitic erosion effect.Thus it can be explained, the etchant being made of mud acid, be 70 in the case where temperature is certain
DEG C when, can corrode montmorillonite, kaolinite and chlorite well, and in mud acid solution hydrochloric acid concentration it is bigger, corrode effect
Fruit is better.
It is the mud acid of "+3% hydrofluoric acid of 15% hydrochloric acid " from table 4, it can be seen that in the case where Acid concentration is certain,
Reaction temperature is higher, and the corresponding erosion ratio of every kind of ore is bigger, illustrates that erosion effect is better, wherein, to montmorillonite and chlorite
Both erosion effects are better than the erosion effect to both illite and kaolinite.Thus can be explained, by mud acid " 15% salt
The etchant that sour+3% hydrofluoric acid " is formed, it can corrode montmorillonite and chlorite well, and reaction temperature is higher, invade
It is better to lose effect.
Therefore, according to the size of erosion ratio, optimum the etchant temperature and concentration of yield ores can be screened, is real
The reference frame that border application provides, avoids the blindness for corroding formula of liquid design.
In order to improve the accuracy of experimental method, the present invention also calculates the activation energy of every kind of ore.
The data measured according to table 3 and table 4, carry out linear fit, and the reaction kinetics equation of four kinds of ores is calculated
For：
J=0.0169C0.910(montmorillonite)；
J=0.0018C2.022(illite)；
J=0.0061C1.625(kaolinite)；
J=0.0013C2.585(chlorite).
Its corresponding activation energy equation is：
J=0.0169EXP (- 0.00315/8.314T) C0.910(montmorillonite)；
J=0.0018EXP (- 0.00268/8.314T) C2.022(illite)；
J=0.0061EXP (- 0.00119/8.314T) C1.625(kaolinite)；
J=0.0013EXP (- 0.00139/8.314T) C2.585(chlorite).
Thus, the activation energy calculated is：
Ea=0.00315 (KJ/mol) (montmorillonite)；
Ea=0.00268 (KJ/mol) (illite)；
Ea=0.00119 (KJ/mol) (kaolinite)；
Ea=0.00139 (KJ/mol) (chlorite).
The present invention also observes the pattern of the ore of embodiment 1-4 in experimentation, before it is corroded and invades
Microscopic appearance figure after erosion is respectively Fig. 1 (a)-(d) and Fig. 2 (a)-(d).
After from Fig. 1 (a)-(d) and Fig. 2 (a)-(d) as can be seen that corroding, the grain shape of ore substantially changes,
Occur some little particle impurity in kaolin crystal, there is new product to generate.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of acid/base liquid corrodes the research method of reservoir rock dynamic characteristic, it is characterised in that including：
(1) etchant is configured, measures and records the pH value of the etchant；Weigh mineral samplers and record its quality m1, by described in
Mineral samplers and the etchant mix simultaneously to react in the reactor of sealing, after question response, measures and to record product molten
The pH value of liquid；
(2) by the reaction mixture stand, filtering, obtain solid product, clean the solid product until filtrate be in neutrality, obtain
To remaining sample, then by the remaining sample, drying to constant weight, weighs and records the weight m of the remaining sample2；
(3) reaction rate is calculated according to the pH value measured in step (1), reaction activity, root is calculated according to the reaction rate
According to m1、m2Calculate the erosion ratio of reaction；Judge the etchant to institute according to the size of the erosion ratio and the reaction activity
The erosion effect of mineral samplers is stated, so as to design the etchant of suitable different reservoir rock；Wherein,
(3.1) calculation formula of reaction rate is：
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It is abbreviated as：J=KCm
In formula, the volume of the etchant of V-participation reaction, L；S-reaction surface surface area, cm2；The etchant of C-t moment it is dense
Degree, mol/L；T- moment, s；K-reaction constant, (mol/L)1-m·s-1, represent reaction rate during reactant unit concentration；
M-the order of reaction, dimensionless；J-reaction rate, mol/ (cm2·h)；
The calculation formula of reaction activity is：
<mrow>
<mi>K</mi>
<mo>=</mo>
<msub>
<mi>K</mi>
<mn>0</mn>
</msub>
<mi>E</mi>
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<mi>P</mi>
<mrow>
<mo>(</mo>
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<mfrac>
<msub>
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</msub>
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<mi>R</mi>
<mi>T</mi>
</mrow>
</mfrac>
<mo>)</mo>
</mrow>
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<mrow>
<mi>J</mi>
<mo>=</mo>
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<mi>exp</mi>
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In formula, K-rate constant, (mol/L)-ms-1；K0- frequency factor, (mol/L)-mL/ (cm2·s)；
Ea-reaction activity, kcal/mol；R-mol gas constant, kcal/molk；T-thermodynamic temperature, k；
(3.2) calculation formula of erosion ratio is：
η=(m1-m2)/m1* 100%
In formula, η-erosion ratio, m1The quality of-mineral samplers；m2The quality of-remaining sample.
2. acid/base liquid according to claim 1 corrodes the research method of reservoir rock dynamic characteristic, it is characterised in that
In step (1), 5-8h is reacted under conditions of reaction vessel is placed in 30-100 DEG C.
3. acid/base liquid according to claim 1 corrodes the research method of reservoir rock dynamic characteristic, it is characterised in that
The research method further includes：Before the reaction, mineral samplers are dried, until constant weight.
4. acid/base liquid according to claim 3 corrodes the research method of reservoir rock dynamic characteristic, it is characterised in that
The research method further includes：Mineral samplers after drying are carried out with the measure of chemical constituent and its content, to determine mineral sample
Main chemical composition in product.
5. acid/base liquid according to claim 3 corrodes the research method of reservoir rock dynamic characteristic, it is characterised in that
The research method further includes：The microscopic appearance of mineral samplers after observation drying, and the mineral sample after observing response
Product microscopic appearance feature.
6. acid/base liquid according to claim 3 corrodes the research method of reservoir rock dynamic characteristic, it is characterised in that
The research method further includes：Mineral samplers after drying are crushed.
7. corroding the research method of reservoir rock dynamic characteristic according to claim 1-6 any one of them acid/bases liquid, it is special
Sign is that the material of the reactor is acidproof and alkali corrosion resistance material, it is preferable that the material of reactor is polytetrafluoroethylene (PTFE).
8. corroding the research method of reservoir rock dynamic characteristic according to claim 1-6 any one of them acid/bases liquid, it is special
Sign is that the etchant is acid solution or lye.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109738313A (en) * | 2019-01-28 | 2019-05-10 | 中国科学院武汉岩土力学研究所 | A kind of method for testing and analyzing of rocky erosion depth and mechanical property degradation |
| CN113533691A (en) * | 2021-07-15 | 2021-10-22 | 云南地矿国际矿业股份有限公司 | Method for evaluating ore content of titanium mineral |
-
2017
- 2017-08-22 CN CN201710726386.8A patent/CN107917999A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 佘继平: "巧岩井周地层-封诸带系统突变失稳机", 《中国博士学位论文全文数据库（电子期刊）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109738313A (en) * | 2019-01-28 | 2019-05-10 | 中国科学院武汉岩土力学研究所 | A kind of method for testing and analyzing of rocky erosion depth and mechanical property degradation |
| CN113533691A (en) * | 2021-07-15 | 2021-10-22 | 云南地矿国际矿业股份有限公司 | Method for evaluating ore content of titanium mineral |
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