CN114354889A - Device and method for accurately measuring deep high-temperature acid rock reaction speed and kinetic parameters - Google Patents
Device and method for accurately measuring deep high-temperature acid rock reaction speed and kinetic parameters Download PDFInfo
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- CN114354889A CN114354889A CN202210016181.1A CN202210016181A CN114354889A CN 114354889 A CN114354889 A CN 114354889A CN 202210016181 A CN202210016181 A CN 202210016181A CN 114354889 A CN114354889 A CN 114354889A
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Abstract
The invention discloses a device and a method for accurately measuring deep high-temperature acid rock reaction speed and kinetic parameters. When the device is used for experimental determination, the rock sample box is driven to lift through the lifting assembly, after the temperature of the solution in the kettle rises to the experimental temperature, the rock sample box is lowered to the position below the liquid level for contact reaction, and the acid rock reaction starting time and the subsequent interval sampling time can be accurately controlled.
Description
Technical Field
The invention relates to the technical field of carbonate reservoir determination, in particular to a device and a method for accurately determining deep high-temperature acid rock reaction speed and kinetic parameters.
Background
The carbonate reservoir is a main reservoir of deep geothermal energy, and large-scale development and utilization of the carbonate reservoir have important significance for relieving energy pressure and assisting the realization of a double-carbon target. However, because natural fractures are very heterogeneous in development, development blocks and individual development wells are likely to be distributed in positions with poor pore permeation conditions, and cannot meet the requirement of large-scale development, reservoir modification is needed to improve the productivity, and acidification and acid fracturing are one of the most important ways to modify carbonate reservoirs.
The accurate measurement of acid rock reaction speed and kinetic parameters is the basis and key for correctly guiding the construction site acidification and acid fracturing design and optimization. Acid rock reaction influencing factors are numerous and mainly include: rock type, temperature, pressure, acid liquor type, acid liquor concentration, same ion effect, surface-to-rock system ratio, and the like. The indoor experiment is an optimal method for accurately obtaining the acid rock reaction rate and the kinetic parameters under the condition of controllable influence factors.
The conventional experiment methods for simulating the acid rock reaction are numerous, wherein the simplest operation and the most widely applied method are high-temperature high-pressure reaction kettles. Although relevant improvement measures aiming at the reaction kettle are reported at present, the following key problems still exist when the method is applied to acid rock reaction.
The acid rock reaction is rapid and violent, particularly for the acidification experiment of a carbonate reservoir, but at present, a reaction kettle generally has slow temperature rise, when the experiment temperature is set to be higher than the boiling point of acid liquor, the reaction kettle needs to be inflated and pressurized, so that a rock sample and the acid liquor need to be injected in advance, and the acid liquor in the reaction kettle reacts with the rock sample in the process of raising the temperature in the reaction kettle to the experiment set temperature.
In order to solve the problems, the conventional solution is to arrange at least two reaction kettles, one for placing the rock sample and the other for containing the acid liquid, and the acid liquid is injected into the reaction kettle containing the rock sample when the temperature of the acid liquid is raised to the experimental set temperature.
Disclosure of Invention
The invention aims to solve the technical problem of providing a device and a method for measuring the reaction of a carbonate reservoir and acid liquor under the condition of simulating a high-temperature high-pressure stratum so as to solve the problem that the existing measuring device cannot accurately control the starting time of the acid-rock reaction, the reaction speed and the measurement of kinetic parameters are inaccurate.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
deep high temperature acid rock reaction rate and kinetic parameter accurate measurement device, including reation kettle, the pressure-controlled subassembly of regulation and control reation kettle internal pressure, the temperature control assembly of regulation and control reation kettle internal temperature, stirring subassembly and the sampling tube that acid liquor stirred in to reation kettle, its characterized in that still including the rock sample box that is located reation kettle, rock sample box has the cavity that holds the rock sample and the breach that supplies acid liquor to get into, reation kettle's upper cover is connected with the lifting unit who drives the rock sample box and go up and down.
A further technical solution is that the lifting assembly comprises:
the screw is vertically arranged and is in threaded connection with a top cover of the reaction kettle; and
the connecting rope is made of acid-base-resistant and temperature-resistant materials, one end of the connecting rope is fixed with the lower end of the screw, and the other end of the connecting rope is fixed with the rock sample box.
The further technical proposal is that the connecting rope is made of polytetrafluoroethylene.
The technical scheme is that the screw comprises an outer sleeve and a rod part arranged in the outer sleeve, the outer sleeve can rotate relative to the rod part, and the lower end of the rod part extends out of the outer sleeve and is fixed with the connecting rope.
A further technical scheme is that the lower end of the connecting rope is divided into a plurality of sections of stay ropes, the tail ends of the stay ropes are fixed with the rock sample box, and the stay ropes are uniformly distributed around the outer edge of the rock sample box to suspend the rock sample box in a balanced manner.
A further technical scheme lies in, the sampling tube includes that the vertical first pipe portion that stretches into the reation kettle bottom and the second pipe portion that the level is located outside the reation kettle are equipped with the control valve on second pipe portion, have the detachable syringe in the end sealing connection of second pipe portion.
A further technical solution is that the voltage control component comprises:
the gas cylinder is communicated with the top of the reaction kettle through a gas pipe, and a pressure sensor, a constant pressure pump and a compressor are arranged on the gas pipe; and
the exhaust pipe is arranged at the top of the reaction kettle, and a safety valve is arranged on the exhaust pipe.
A further technical solution is that the temperature control assembly comprises:
the heating ring is coated on the side wall and the bottom of the reaction kettle, and a heat insulation layer is arranged outside the heating ring;
the temperature measuring tube is vertically arranged in the reaction kettle, the upper end of the temperature measuring tube is fixed with the upper cover of the reaction kettle, and the lower end of the temperature measuring tube is a blind end and extends into the bottom of the reaction kettle; and
and a temperature probe of the temperature sensor extends into the temperature measuring tube.
The stirring assembly comprises a magnetic stirrer, the magnetic stirrer comprises magnetic steel, a magnetic stirring rotor and a micro motor for driving the magnetic steel to rotate, the reaction kettle is positioned on the magnetic steel, and the magnetic stirring rotor is positioned at the bottom of an inner cavity of the reaction kettle; the lowest position of the lifting component for driving the rock sample box to descend is higher than the magnetic stirring rotor.
The method for accurately measuring the reaction speed and the kinetic parameters of the deep high-temperature acid rock is applied to the device for measurement and is operated according to the following steps:
a, selecting a stratum characteristic rock sample, crushing, weighing a certain weight, putting the rock sample into a rock sample box, grinding part of the rock sample into powder, and carrying out XRD (X-ray diffraction) test to obtain the mineral composition and proportion of the rock;
b, adding acid liquor into the reaction kettle, and screwing the upper cover of the reaction kettle to enable the rock sample box to be positioned above the acid liquor;
c, pressurizing the inside of the reaction kettle to a set pressure, and heating and stirring the acid liquor in the reaction kettle;
d, when the temperature of the acid liquor reaches a set value, the lifting assembly controls the rock sample box to descend until the rock sample box is completely immersed into the acid liquor;
e, the rock sample contacts with the reaction solution to start reaction, the reaction time is recorded, the reaction solution is quantitatively taken from the sampling pipe according to a set time interval to carry out ion test, pressure supplement is carried out in time, and the ion test result is used for calculating acid liquor reaction speed and kinetic parameters and researching the acid rock reaction mechanism;
and f, after the experiment is finished, regulating and controlling the pressure in the reaction kettle to the normal pressure, driving the rock sample box to rise to the liquid level, leaching the reaction solution on the rock sample box, and then opening the upper cover of the reaction kettle to clean the reaction kettle.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
the device drives the rock sample box to lift through the lifting component, and can drop the rock sample box to the liquid level for contact reaction after the temperature of the solution in the kettle rises to the experimental temperature, so that the acid rock reaction starting time and the subsequent interval sampling time can be accurately controlled.
During the reaction, the rock sample suspends in midair in reation kettle, does not contact with the magnetic stirring rotor of reation kettle bottom, can avoid the stirring to the broken influence of rock sample, has further promoted the accuracy of experimental determination.
Sampling in the experimental process, when the pressure in the kettle is normal, the external connection injector extracts quantitative reaction solution, when the pressure in the kettle is high, the control valve is slowly opened, the reaction solution can automatically flow out, and if the pressure in the kettle is reduced during sampling, the pressure needs to be supplemented in time. In the in-process of sample, reaction solution upwards flows out through one section vertical first pipe portion on the sampling tube, and the tiny rock granule falls because of the dead weight, can avoid tiny rock granule to flow out or block up the thief hole from the cauldron bottom.
After the experiment is completed, the rock sample box is lifted to the liquid level, the reaction solution on the rock sample box is completely sprayed, then the upper cover of the reaction kettle is opened to clean the reaction kettle, and the reaction platform can be prevented from being polluted during cleaning.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Fig. 1 is a schematic structural view of the apparatus of the present disclosure.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
As shown in fig. 1, the device for accurately determining the reaction speed and the kinetic parameters of deep high-temperature acid rock comprises a reaction kettle 10, a pressure control component for regulating and controlling the pressure in the reaction kettle 10, a temperature control component for regulating and controlling the temperature in the reaction kettle 10, a stirring component for stirring acid liquor in the reaction kettle 10, a sampling tube 121, and a rock sample box 111 located in the reaction kettle 10, wherein the rock sample box 111 has a cavity for accommodating a rock sample and a gap for allowing acid liquor to enter, preferably, the rock sample box 111 has a mesh cage structure, and the initial particle size of the rock sample is larger than the hole in the rock sample box 111. The upper cover of the reaction kettle 10 is connected with a lifting component for driving the rock sample box 111 to lift. The reaction kettle 10 and the rock sample box 111 can be made of hastelloy, are resistant to high temperature and high pressure and resistant to acid and alkali corrosion, and the upper cover of the reaction kettle is detachably and hermetically connected with the main body.
The method for accurately measuring the reaction speed and the kinetic parameters of the deep high-temperature acid rock is applied to the device for measurement and is operated according to the following steps:
a, selecting a stratum characteristic rock sample, crushing the rock sample to a particle size of 3-8mm generally, weighing a certain weight, putting the rock sample into a rock sample box 111, grinding part of the rock sample into powder, and performing XRD (X-ray diffraction) test to obtain the mineral composition and proportion of the rock;
b, adding acid liquor into the reaction kettle 10, wherein the concentration of the acid liquor is 15% or adjusting according to the test requirement, and screwing the upper cover of the reaction kettle 10 to enable the rock sample box 111 to be positioned above the acid liquor;
c, pressurizing the inside of the reaction kettle 10 to a set pressure, wherein the pressure is generally normal pressure to 40 MPa according to the test requirement, and heating and stirring the acid liquor in the reaction kettle 10 at the heating temperature of generally 200 ℃;
d, when the temperature of the acid liquor reaches a set value, the lifting assembly controls the rock sample box 111 to descend until the rock sample box is completely immersed into the acid liquor;
e, the rock sample contacts with the reaction solution to start reaction, the reaction time is recorded, the reaction solution is quantitatively received from the sampling tube 121 at a certain time interval to carry out ion test, and the sampling time for the sample with rapid reaction can be set to be 1min, 2min, 4min, 6min, 10min, 20 mm, 30min, 40min and 60min after the reaction starts; the sampling time of a sample with slow reaction can be set to 10min, 20min, 30min, 60min, 90min and 120min after the reaction starts, pressure supplement is carried out in time in the sampling process, and the ion test result is used for calculating acid liquor reaction speed and kinetic parameters and researching the acid rock reaction mechanism;
and f, after the experiment is finished, regulating and controlling the pressure in the reaction kettle 10 to the normal pressure, driving the rock sample box 111 to rise to the liquid level, leaching out the reaction solution on the rock sample box 111, and then opening the upper cover of the reaction kettle 10 to clean the reaction kettle 10.
The device drives the rock sample box 111 to ascend and descend through the lifting assembly, and can descend the rock sample box 111 to the liquid level for contact reaction after the temperature of the solution in the kettle rises to the experimental temperature, so that the acid-rock reaction starting time and the subsequent interval sampling time can be accurately controlled.
After the experiment is completed, the rock sample box 111 is lifted to the liquid level, the reaction solution on the rock sample box 111 is completely sprayed, then the upper cover of the reaction kettle 10 is opened to clean the reaction kettle 10, and the reaction table can be prevented from being polluted during cleaning.
In the device for accurately measuring the acid rock reaction speed and the kinetic parameters, the lifting assembly comprises a screw 112 and a connecting rope 113. Screw rod 112 is vertical to be set up, and with reation kettle 10's top cap threaded connection, connect 113 to make by the material of acid and alkali resistance temperature, preferably adopt the polytetrafluoroethylene material, connect 113 upper ends of rope and screw rod 112's lower extreme fixed, the multistage stay cord is divided to the lower extreme, the end and the rock specimen box 111 of stay cord are fixed, many the stay cord evenly arranges around the outer fringe of rock specimen box 111, and balanced suspension rock specimen box 111 guarantees the stability that rock specimen box 111 suspends in midair before sour rock reaction.
This lifting unit adopts soft connection rope 113 to suspend in midair rock sample box 111, the buoyancy that the acidizing fluid can be overcome to rock sample box 111 is fallen into in the acidizing fluid to the dead weight, rock sample and acidizing fluid contact back, the violent reaction of acid rock, produce a large amount of bubbles, rock sample box 111 can take place to rock, the relative rock sample of acidizing fluid produces and flows, carry out the disturbance to the rock sample surface, the ion that can make the reaction go out diffusion with higher speed, rock sample box 111 rocks still to the effect that the middle part of solution produced the stirring, do benefit to going on of reaction, and the accuracy of sample analysis.
The lifting and locking of the rock sample box 111 can be realized by rotating the screw rod 112 forward or backward, the self weight is larger after the rock sample is filled in the rock sample box 111, and the rock sample can overcome the buoyancy of acid liquor after falling and is immersed in the acid liquor.
In order to avoid the rotation of the screw rod 112, the rock sample box 111 is driven to rotate, and the centrifugal force is generated to enable the time delay sample to collide with the rock sample box 111, the screw rod 112 in the device comprises an outer screw sleeve and a rod part arranged in the outer screw sleeve, the outer screw sleeve can rotate relative to the rod part and cannot be separated from the outer screw sleeve downwards, for example, the rod part is a T-shaped rod and is inserted into the outer screw sleeve, the diameter of the upper convex edge of the T-shaped rod is larger than the outer diameter of the outer screw sleeve, and the lower end of the rod part extends out of the outer screw sleeve and is fixed with the connecting rope 113.
The pressure control component comprises a gas cylinder 131 and an exhaust pipe 135, the gas cylinder 131 is communicated with the top of the reaction kettle 10 through a gas pipe, and the gas pipe is provided with a pressure sensor 132, a constant pressure pump 133 and a compressor 134. The exhaust pipe 135 is disposed at the top of the reaction vessel 10, and a safety valve 136 is disposed on the exhaust pipe 135. The gas cylinder 131 provides a gas source, if the reaction kettle 10 needs to be pressurized, the gas enters the kettle through the compressor 134 and the constant pressure pump 133, the pressure sensor 132 can be used for monitoring the pressure in the kettle, and after the pressure sensor 132 detects that the pressure value in the reaction kettle 10 reaches a set value, the compressor 134 and the constant pressure pump 133 work.
The temperature control assembly comprises a heating ring 141, a temperature measuring tube 142 and a temperature sensor 143, the heating ring 141 can be a resistance heating ring 141 or an infrared heating ring 141, the heating ring 141 is coated on the side wall and the bottom of the reaction kettle 10 and used for adjusting and controlling the temperature in the reaction kettle 10, a heat insulation layer is arranged outside the heating ring 141 and plays roles of heat preservation and scalding prevention. The temperature measuring tube 142 is vertically arranged in the reaction kettle 10, the upper end of the temperature measuring tube is fixed with the upper cover of the reaction kettle 10, and the lower end of the temperature measuring tube is a blind end and extends into the bottom of the reaction kettle 10. The temperature probe of the temperature sensor 143 extends into the thermo tube 142. The lower end of the temperature measuring tube 142 extends into the liquid surface of the kettle and is used for accurately monitoring the liquid temperature.
Stirring assembly includes magnetic stirrers, and magnetic stirrers belongs to prior art, and magnetic stirrers includes magnet steel 151, magnetic stirring rotor 152 and the rotatory micro motor 153 of drive magnet steel 151, reation kettle 10 is located magnet steel 151, magnetic stirring rotor 152 is located the bottom of reation kettle 10 inner chamber, and the rationale rotates behind the micro motor 153 switch on to it is rotatory to drive magnet steel 151, and rotatory magnet steel 151 produces rotating magnetic field, makes the acidizing fluid in the rotatory stirring reation kettle 10 of magnetic stirring rotor 152.
The lowest position that lifting unit drive rock specimen box 111 descends is higher than magnetic stirring rotor 152, and during the reaction, the rock specimen suspends in midair in reation kettle 10, does not contact with the magnetic stirring rotor 152 of reation kettle 10 bottom, can avoid the stirring to the broken influence of rock specimen, has further promoted the accuracy of experimental determination.
In order to determine the reaction speed and the kinetic parameters of the acid rock, the reaction solution in the kettle needs to be taken regularly to determine the main ion content. This device is different from traditional reation kettle 10 and takes a sample at the bottom of the cauldron trompil, and sampling pipe 121 includes that vertical first pipe portion and the level that stretches into reation kettle 10 bottom are located reation kettle 10 outer, with the second pipe portion of first pipe portion upper end intercommunication in this device, is equipped with control valve 122 in second pipe portion, has the detachable syringe in the end sealing connection of second pipe portion.
Sampling in the experimental process, when the pressure in the kettle is normal, the external connection injector extracts quantitative reaction solution, when the pressure in the kettle is high, the control valve 122 is slowly opened, the reaction solution can automatically flow out, and if the pressure in the kettle is reduced during sampling, the pressure needs to be supplemented in time. In the in-process of sample, reaction solution upwards flows out through one section vertical first pipe portion on the sampling tube 121, and tiny rock particle falls down because of the dead weight, can avoid tiny rock particle to flow out or block up the thief hole from the cauldron bottom.
The above is only a preferred embodiment of the invention, and any simple modifications, variations and equivalents of the invention may be made by anyone in light of the above teachings and fall within the scope of the invention.
Claims (10)
1. Deep high temperature acid rock reaction rate and kinetic parameter accurate measurement device, including reation kettle (10), the pressure control assembly of regulation and control reation kettle (10) internal pressure, the temperature control assembly of regulation and control reation kettle (10) internal temperature, stirring subassembly and sampling tube (121) that the acidizing fluid carries out the stirring in reation kettle (10), its characterized in that still including rock sample box (111) that is located reation kettle (10), rock sample box (111) have the cavity that holds the rock sample and the breach that supplies the acidizing fluid to get into, the upper cover of reation kettle (10) is connected with the lifting unit who drives rock sample box (111) and go up and down.
2. The apparatus of claim 1, wherein the lift assembly comprises:
the screw rod (112) is vertically arranged and is in threaded connection with the top cover of the reaction kettle (10); and
the connecting rope (113) is made of acid-base-resistant and temperature-resistant materials, one end of the connecting rope is fixed with the lower end of the screw rod (112), and the other end of the connecting rope is fixed with the rock sample box (111).
3. The device according to claim 2, characterized in that said connecting string (113) is made of teflon.
4. The device according to claim 2, wherein the screw (112) comprises an outer sleeve, and a rod portion disposed in the outer sleeve, the outer sleeve being rotatable with respect to the rod portion, the rod portion having a lower end extending out of the outer sleeve and being fixed to the connecting cord (113).
5. The device according to claim 2, characterized in that the lower end of the connecting rope (113) is divided into a plurality of segments of stay ropes, the ends of the stay ropes are fixed with the rock sample box (111), and the plurality of stay ropes are uniformly arranged around the outer edge of the rock sample box (111) to suspend the rock sample box (111) in a balanced manner.
6. The device as claimed in claim 1, wherein the sampling tube (121) comprises a first tube part vertically extending into the bottom of the reaction vessel (10) and a second tube part horizontally located outside the reaction vessel (10), a control valve (122) is provided on the second tube part, and a detachable syringe is hermetically connected to the end of the second tube part.
7. The apparatus of claim 1, wherein the voltage controlled component comprises:
the gas cylinder (131) is communicated with the top of the reaction kettle (10) through a gas pipe, and a pressure sensor (132), a constant pressure pump (133) and a compressor (134) are arranged on the gas pipe; and
the exhaust pipe (135) is arranged at the top of the reaction kettle (10), and a safety valve (136) is arranged on the exhaust pipe (135).
8. The apparatus of claim 1, wherein the temperature control assembly comprises:
the heating ring (141) is coated on the side wall and the bottom of the reaction kettle (10), and a heat insulation layer is arranged outside the heating ring (141);
the temperature measuring tube (142) is vertically arranged in the reaction kettle (10), the upper end of the temperature measuring tube is fixed with the upper cover of the reaction kettle (10), and the lower end of the temperature measuring tube is a blind end and extends into the bottom of the reaction kettle (10); and
and a temperature sensor (143) with a temperature probe extending into the temperature measuring tube (142).
9. The device of claim 1, wherein the stirring assembly comprises a magnetic stirrer, the magnetic stirrer comprises magnetic steel (151), a magnetic stirring rotor (152) and a micro motor (153) for driving the magnetic steel (151) to rotate, the reaction kettle (10) is positioned on the magnetic steel (151), and the magnetic stirring rotor (152) is positioned at the bottom of the inner cavity of the reaction kettle (10); the lowest position of the lifting component for driving the rock sample box (111) to descend is higher than the magnetic stirring rotor (152).
10. The method for accurately measuring the reaction speed and kinetic parameters of deep high-temperature acid rock is characterized by comprising the following steps of:
a, selecting a stratum characteristic rock sample, crushing, weighing a certain weight, putting the rock sample into a rock sample box (111), grinding part of the rock sample into powder, and carrying out XRD (X-ray diffraction) test to obtain the mineral composition and proportion of the rock;
b, adding acid liquor into the reaction kettle (10), and screwing the upper cover of the reaction kettle (10) to enable the rock sample box (111) to be positioned above the acid liquor;
c, pressurizing the inside of the reaction kettle (10) to a set pressure, and heating and stirring the acid liquor in the reaction kettle (10) at the same time;
d, when the temperature of the acid liquor reaches a set value, the lifting assembly controls the rock sample box (111) to descend until the rock sample box is completely immersed into the acid liquor;
e, the rock sample contacts with the reaction solution to start reaction, the reaction time is recorded, the reaction solution is quantitatively taken from the sampling tube (121) according to a set time interval to carry out ion test, and the result is used for calculating acid liquor reaction speed and kinetic parameters and researching the acid rock reaction mechanism;
and f, after the experiment is finished, regulating and controlling the pressure in the reaction kettle (10) to the normal pressure, driving the rock sample box (111) to rise to the liquid level, completely spraying the reaction solution on the rock sample box (111), and then opening the upper cover of the reaction kettle (10) to clean the reaction kettle (10).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115112551A (en) * | 2022-06-24 | 2022-09-27 | 中国核动力研究设计院 | Acid corrosion resistant dissolution kinetic reaction device and experimental method thereof |
| CN117054284A (en) * | 2023-10-12 | 2023-11-14 | 西南石油大学 | Acid rock reaction rate prediction device and method |
| CN117054617A (en) * | 2023-10-12 | 2023-11-14 | 西南石油大学 | High-temperature high-pressure acid rock reaction rate measuring device |
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| CN117054284A (en) * | 2023-10-12 | 2023-11-14 | 西南石油大学 | Acid rock reaction rate prediction device and method |
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