CN103234861A - Acid-rock reaction rate dynamic test device and calculation method - Google Patents
Acid-rock reaction rate dynamic test device and calculation method Download PDFInfo
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Abstract
The invention relates to an acid-rock reaction rate dynamic test device and a calculation method in the oil exploitation industry. The test device comprises a preheating liquid storage pot connected with a temperature sensor, and the lower part of the preheating liquid storage pot is connected to a reaction kettle. The reaction kettle is disposed in a heat-gathering type magnetic heating stirrer. The reaction kettle is connected to a temperature sensor, and a reaction product escape port in connection with a condenser pipe is arranged over the reaction kettle. An ultra low temperature circulating condensation system is employed to provide an ultra low temperature environment to the condenser pipe. The air outlet of a buffer device is communicated with a gas collecting bottle, a float type height sensor is placed on a liquid level of the gas collecting bottle, the top of which is equipped with a liquid inlet and the bottom of which is equipped with a liquid outlet connected to a T-shaped communicating vessel. A float type height sensor is placed on the liquid level of the T-shaped communicating vessel, the lower part of which is connected to a volume meter. Through volume meter readings, the hydrochloric acid concentration and acid-rock reaction rate at any time in a reaction process can be calculated.
Description
Technical field
The present invention relates to a kind of acid-rock reaction rate method of testing of field of petroleum exploitation, be specifically related to a kind of acid-rock reaction rate dynamic checkout unit and computing method.
Background technology
Acidifying is a kind of effective ways that make well production increment or water injection well stimulation.It is to inject a kind of acid solution or acid mixed solution by well in the stratum, utilize the chemical reaction of the part mineral in acid and the stratum, open pore in the corrosion reservoir or crack wall rock, increase the flow conductivity in hole and crack, thereby make a kind of technological measure of well production increment or water injection well stimulation.In acidization, acid-rock reaction rate should be suitable.It is more that acid-rock reaction rate can cause the immediate vicinity of wellbore corrosion faster, and the deep reservoir that need transform does not obtain transforming; Too slow acid-rock reaction rate then can cause bigger, the residual acid of long, acid liquid loss amount of engineering time to be detained reservoir is caused secondary pollution problems.Based on above requirement, need in the laboratory, to carry out simulated experiment preferred acid formula of liquid, measuring and calculating reaction time.Petroleum industry generally adopts rotation laccolite instrument to measure sour rock reaction dynamics parameter at present, but its operation is comparatively complicated, workload is bigger, and can not measure the reaction rate dynamic change situation in the entire reaction course easily, can't record the time that quantitative acid solution and capacity rock core fully react, so the invention provides a kind of acid-rock reaction rate dynamic checkout unit and computing method.
Summary of the invention
The object of the present invention is to provide a kind of acid-rock reaction rate dynamic checkout unit and computing method, its principle is the amount of gathering acid-gas that the rock reaction generates, thereby calculates the acid-rock reaction rate in a certain moment concentration of hydrochloric acid and unit interval.
A kind of acid-rock reaction rate dynamic checkout unit disclosed by the invention and computing method, its proving installation is characterised in that: proving installation comprises that preheating fluid reservoir (1), preheating fluid reservoir (1) upward connect temperature sensor (a); The lower end of preheating fluid reservoir (1) is connected with reactor (5), be connected with valve (2) and valve (3) on preheating fluid reservoir (1) and the pipeline that reactor (5) is connected, reactor (5) places heat collecting type magnetic force heating stirrer (4), reactor (5) to go up to connect temperature sensor (b); The outlet of reactor (5) connects condenser pipe (6), uses ultralow temperature circulating condensing system (7) to provide ultra-low temperature surroundings to condenser pipe (6).Be connected with valve (8) on condenser pipe (6) and the pipeline that snubber assembly (9) is connected, the air intake opening of snubber assembly (9) is a little less than the liquid level of snubber assembly, so that observe gas effusion speed; Be connected with valve (10) on snubber assembly (9) and the pipeline that gas bottle (11) is connected, the air intake opening in the gas bottle (11) is higher than the liquid level in the gas bottle (11), and the liquid level of gas bottle (11) is placed float-type height sensor (13); The top of gas bottle (11) is provided with filling opening (12), and the gas bottle top arranges temperature sensor (c); Be connected with valve (14) on gas bottle (11) and the pipeline that T type linker (16) is connected, the upper end liquid level of T type linker is placed float-type height sensor (15); Be connected with the sensitive valve (17) by float-type height sensor (15) control on T type linker (16) and the pipeline that volume gauger (18) is connected.
A kind of acid-rock reaction rate dynamic checkout unit and computing method, its computing method are characterised in that: use the drainage collection gas method, acid in the acquisition units time-rock reaction generates the amount (being the reading of volume gauger) of gas, the temperature of being measured by temperature sensor c, can from accompanying drawing 8, find the gas compressibility factor under this temperature, thereby calculate concentration of hydrochloric acid and the acid-rock reaction rate of any time in the entire reaction course according to following formula, the data that it is calculated that out can be made concentration of hydrochloric acid variation relation figure and acid-rock reaction rate variation relation figure in time in time.
A kind of acid-rock reaction rate dynamic checkout unit and computing method, the computing formula of described concentration of hydrochloric acid is:
In the formula: the concentration of hydrochloric acid in x-course of reaction, %;
V
Acid solutionThe volume of acid solution in the-adding reactor, mL;
The compressibility factor of gas under k-certain temperature can be found from subordinate list 8.
A kind of acid-rock reaction rate dynamic checkout unit and computing method, the acid-rock reaction rate computing formula is in the described unit interval:
In the formula: v-acid-rock reaction rate, g/cm
2Min;
S-rock sample surface area, cm
2
T-unit interval, min;
The compressibility factor of gas under k-certain temperature can be found from subordinate list 8.
Described preheating fluid reservoir adopts polytetrafluoroethylmaterial material as liner.
On described preheating fluid reservoir and the reactor temperature sensor is housed.
Described reactor diameter is 3～4cm, and it is liner that reactor adopts organic glass.
The liquid level of described gas bottle and T type linker is placed height sensor.
Described T type linker below arranges the sensitive switch by height sensor control.
Described gas bottle top arranges temperature sensor c, the gas temperature of collecting with mensuration.
The present invention has the following advantages owing to adopt above technical scheme: 1, the present invention is owing to adopt polytetrafluoroethylmaterial material as the liner of preheating fluid reservoir, and its surface is neither hydrophilic, also oleophylic not, and acid solution flows out easily and is not detained.2, there are two pipelines to be communicated with between preheating fluid reservoir and the reactor, are conducive to that acid solution all flows into rapidly in the reactors and blocking pipe not.3, add small amount of liquid in the snubber assembly, a little is advisable with the submergence mouth of pipe, so that observe gas effusion speed intuitively.4, the sensitive valve that employing T type linker connection gas bottle, and employing is controlled by the float-type height sensor is controlled the liquid level in gas bottle and the T type linker, can keep the pressure in the gas bottle consistent with atmospheric pressure, makes measurement result accurate.Principle of the present invention is simple, and energy consumption is low, and data collection point is intensive, and it measures the foundation that data can be used as acid solution prescription screening in the laboratory.
Description of drawings
Fig. 1 is a kind of acid-rock reaction rate dynamic checkout unit synoptic diagram of the present invention.
Fig. 2 is the concentration of hydrochloric acid change curve in time that utilizes in hydrochloric acid-rock core course of reaction that a kind of acid-rock reaction rate dynamic checkout unit of the present invention measures.
Fig. 3 is the hydrochloric acid-rock core course of reaction rock reaction rate change curve in time that utilizes a kind of acid-rock reaction rate dynamic checkout unit of the present invention to measure.
Fig. 4 utilizes in gel acid-rock core course of reaction that a kind of acid-rock reaction rate dynamic checkout unit of the present invention measures concentration of hydrochloric acid change curve in time.
Fig. 5 utilizes in gel acid-rock core course of reaction that a kind of acid-rock reaction rate dynamic checkout unit of the present invention measures rock reaction rate change curve in time.
Fig. 6 is that the cleaning of utilizing a kind of acid-rock reaction rate dynamic checkout unit of the present invention to measure turns to the acid concentration change curve in time in acid-rock core course of reaction.
Fig. 7 is that the cleaning of utilizing a kind of acid-rock reaction rate dynamic checkout unit of the present invention to measure turns to the rock reaction rate change curve in time in acid-rock core course of reaction.
Fig. 8 is the gas compressibility factor diagram.
Each mark is as follows in apparatus of the present invention structural representation: 1 preheating fluid reservoir, 2,3,8,10, sensitive valve, 18 volume gaugers, a, b, the c of 14 valves, 4 heat collecting type magnetic force heating stirrers, 5 reactors, 6 condenser pipes, 7 ultralow temperature condenser systems, 9 buffer systems, 11 gas bottles, 12 filling openings, 13,15 float-type height sensors, 16T type linker, the control of 17 float-type height sensors are temperature sensor.
Embodiment
The present invention will be further described below in conjunction with specific embodiment, and following examples adopt hydrochloric acid, gel acid, cleaning to turn to acid to react with rock core with one deck position respectively, to estimate time and the speed that dissimilar acid solutions and specific formation core react.But the present invention is not limited to following examples, and the condition that experimentizes also is not limited to condition selected among the embodiment, and the acid solution prescription that adopts also is not limited to acid solution prescription selected in following examples.
Embodiment 1: rock core is polished into the rule bulk that length is respectively 2cm, 1cm, 1cm, and 100 ℃ of baking 2h, standby; Connect the pipeline of device, close all valves; Getting the ratio of 3mL acid solution in every square centimeter of rock core, is that 20% hydrochloric acid is poured in the preheating fluid reservoir (1) with the 30mL massfraction of measuring, and is warming up to and specifies 70 ℃; Rock core is put into reactor; Open heat collecting type magnetic force heating stirrer (4), the temperature in the reactor (5) is risen to 70 ℃; Open ultralow temperature condensing unit (7), make condenser pipe 6 keep ultra-low temperature surroundings; In gas bottle (11), add liquid by filling opening (12), and can not the submergence air intake opening, open valve (14), make liquid level and the liquid level in the T type linker (16) in the gas bottle (11) maintain an equal level, with rubbery stopper jam-pack filling opening (12), open valve (2) and valve (3) simultaneously, acid solution in the preheating fluid reservoir (1) flows into back valve-off in the reactor (5), pick up counting, and open valve (10) rapidly, valve (14) and valve (17), the reading of a volume gauger of per minute record is till the volume gauger reading no longer increases.
Embodiment 2: rock core is polished into the rule bulk that length is respectively 2cm, 1cm, 1cm, and 100 ℃ of baking 2h, standby; Connect the pipeline of device, close all valves; Getting the ratio of 3mL acid solution in every square centimeter of rock core, is that 20% gel acid is poured in the preheating fluid reservoir (1) with the 30mL hydrochloric acid massfraction of measuring, and is warming up to and specifies 70 ℃; Rock core is put into reactor; Open heat collecting type magnetic force heating stirrer (4), the temperature in the reactor (5) is risen to 70 ℃; Open ultralow temperature condensing unit (7), make condenser pipe 6 keep ultra-low temperature surroundings; In gas bottle (11), add liquid by filling opening (12), and can not the submergence air intake opening, open valve (14), make liquid level and the liquid level in the T type linker (16) in the gas bottle (11) maintain an equal level, with rubbery stopper jam-pack filling opening (12), open valve (2) and valve (3) simultaneously, acid solution in the preheating fluid reservoir (1) flows into back valve-off in the reactor (5), pick up counting, and open valve (10) rapidly, valve (14) and valve (17), the reading of a volume gauger of per minute record is till the volume gauger reading no longer increases.
Embodiment 3: rock core is polished into the rule bulk that length is respectively 2cm, 1cm, 1cm, and 100 ℃ of baking 2h, standby; Connect the pipeline of device, close all valves; Getting the ratio of 3mL acid solution in every square centimeter of rock core, is that 20% cleaning turns to acid to pour in the preheating fluid reservoir (1) with the 30mL hydrochloric acid massfraction of measuring, and is warming up to and specifies 70 ℃; Rock core is put into reactor; Open heat collecting type magnetic force heating stirrer (4), the temperature in the reactor (5) is risen to 70 ℃; Open ultralow temperature condensing unit (7), make condenser pipe 6 keep ultra-low temperature surroundings; In gas bottle (11), add liquid by filling opening (12), and can not the submergence air intake opening, open valve (14), make liquid level and the liquid level in the T type linker (16) in the gas bottle (11) maintain an equal level, with rubbery stopper jam-pack filling opening (12), open valve (2) and valve (3) simultaneously, acid solution in the preheating fluid reservoir (1) flows into back valve-off in the reactor (5), pick up counting, and open valve (10) rapidly, valve (14) and valve (17), the reading of a volume gauger of per minute record is till the volume gauger reading no longer increases.
In the above-described embodiments, adopt hydrochloric acid, gel acid, cleaning to turn to acid and same reservoir core to react respectively, probe temperature is 70 ℃, and initial reaction rate is designated as 0, and checking in the gas compressibility factor is 0.92.
Hydrochloric acid in above-described embodiment adopts analyzes pure hydrochloric acid; Additive formulations is in the gel acid: the slow auxiliary agent of 1% diversion agent+2～3% jelling agents+1.5% Fe stabilizer+2% corrosion inhibiter+1.5% cleanup additive+1%; Cleaning turns to the additive formulations of acid to be: 5% cleaning turns to sour host+1.5% Fe stabilizer+2% corrosion inhibiter.
Fig. 2 as a result, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7 according to recording can draw following result:
Hydrochloric acid and rock core reaction rate are very fast, namely finish reaction in 20 minutes, and initial reaction stage speed is very fast, and along with the prolongation of time, reaction rate descends until being tending towards 0;
Gel acid and rock core reaction rate are slower, and reaction is tending towards finishing in the time of about 140 minutes, and initial reaction stage speed is very fast, but the speed that its speed is reacted much smaller than hydrochloric acid-rock core, along with the prolongation of time, reaction rate descends until being tending towards 0;
Cleaning turns to acid and rock core reaction rate to present the waveform variation, and initial reaction stage speed is slower; Along with the carrying out of reaction, reaction rate descends; Along with reaction is further carried out, after reaction rate rose to peak, reaction rate descended until being tending towards 0, and reaction is about 200 minutes T.T..
Comparison diagram 3, Fig. 5, Fig. 7, Fig. 3 is consistent with the curvilinear trend of Fig. 5 as can be seen, and is very fast in the reaction rate of initial reaction stage, and along with the carrying out in reaction time, reaction rate is dull decline all, and the acid solution of the type is suitable for the acidizing treatment of immediate vicinity of wellbore; Fig. 7 has occurred and Fig. 3 and the visibly different trend of Fig. 5, and reaction rate is also not non-constant, is not monotone variation yet, but the undulate variation, the acid solution of the type is favourable for causing remote acid-etched fracture.
As seen, by the disclosed experimental provision of the embodiment of the invention and method, the situation of change of reaction rate in the course of reaction that can visually see records the situation of change of acid-rock reaction rate in reaction time and the course of reaction, and optimizes the acid solution prescription that is suitable at specific stratum.
Energy consumption of the present invention is low, and test result is intuitively simple and clear, can make in the foundation of the preceding laboratory of acidifying inner evaluation acid liquid performance.
Claims (10)
1. an acid-rock reaction rate dynamic checkout unit is characterized in that, proving installation comprises that preheating fluid reservoir (1), preheating fluid reservoir (1) upward connect temperature sensor (a); The lower end of preheating fluid reservoir (1) is connected with reactor (5), be connected with valve (2) and valve (3) on preheating fluid reservoir (1) and the pipeline that reactor (5) is connected, reactor (5) places heat collecting type magnetic force heating stirrer (4), reactor (5) to go up to connect temperature sensor (b); The outlet of reactor (5) connects condenser pipe (6), uses ultralow temperature circulating condensing system (7) to provide ultra-low temperature surroundings to condenser pipe (6).Be connected with valve (8) on condenser pipe (6) and the pipeline that snubber assembly (9) is connected, the air intake opening of snubber assembly (9) is a little less than the liquid level of snubber assembly, so that observe gas effusion speed; Be connected with valve (10) on snubber assembly (9) and the pipeline that gas bottle (11) is connected, the air intake opening in the gas bottle (11) is higher than the liquid level in the gas bottle (11), and the liquid level of gas bottle (11) is placed float-type height sensor (13); The top of gas bottle (11) is provided with filling opening (12), and the gas bottle top arranges temperature sensor (c); Be connected with valve (14) on gas bottle (11) and the pipeline that T type linker (16) is connected, the upper end liquid level of T type linker is placed float-type height sensor (15); Be connected with the sensitive valve (17) by float-type height sensor (15) control on T type linker (16) and the pipeline that volume gauger (18) is connected.
2. acid-rock reaction rate dynamic rate computing method, it is characterized in that, use the drainage collection gas method, acid in the acquisition units time-rock reaction generates the amount (being the reading of volume gauger) of gas, the temperature of being measured by temperature sensor c, can from accompanying drawing 8, find the gas compressibility factor under this temperature, thereby calculate concentration of hydrochloric acid and the acid-rock reaction rate of any time in the entire reaction course according to following formula, the data that it is calculated that out can be made concentration of hydrochloric acid variation relation figure and acid-rock reaction rate variation relation figure in time in time.
3. concentration of hydrochloric acid computing formula as claimed in claim 2 is:
In the formula: the acid concentration in x-course of reaction, %;
V
Acid solutionThe volume of acid solution in the-adding reactor, mL;
The compressibility factor of gas under k-this temperature can be found from subordinate list 8.
4. as right 2 described acid-rock reaction rate computing formula be:
In the formula: v-acid-rock reaction rate, g/cm
2Min;
The reading difference of-unit interval inner volume meter, mL;
S-rock sample surface area, cm
2
T-unit interval, min;
The compressibility factor of gas under k-this temperature can be found from subordinate list 8.
5. preheating fluid reservoir as claimed in claim 1 adopts polytetrafluoroethylmaterial material as liner.
6. on preheating fluid reservoir as claimed in claim 1 and the reactor temperature sensor is housed.
7. reactor diameter as claimed in claim 1 is 3～4cm, and it is liner that reactor adopts organic glass.
8. the liquid level of gas bottle and T type linker is placed height sensor according to claim 1.
9. T type linker below setting as claimed in claim 1 is by the sensitive switch of height sensor control.
10. gas bottle as claimed in claim 1 or 2 top arranges temperature sensor c, the gas temperature of collecting with mensuration, thus check in the gas compressibility factor.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104597219A (en) * | 2014-12-26 | 2015-05-06 | 西南交通大学 | Water-rock chemical dynamic reaction double-system test unit |
| CN105628549A (en) * | 2016-01-14 | 2016-06-01 | 太原理工大学 | Method for directly, quickly and full-automatically determining content of desorbing gas in coal seam |
| CN109490071A (en) * | 2017-09-12 | 2019-03-19 | 中国石油天然气股份有限公司 | Acid fluid system integrates optimization experiment evaluation method |
| CN114660224A (en) * | 2022-03-29 | 2022-06-24 | 西南石油大学 | Device and method for measuring reaction kinetic parameters of acid rock in high-viscosity liquid |
| CN115561189A (en) * | 2022-10-20 | 2023-01-03 | 西南石油大学 | Method for testing reaction rate of authigenic acid rock |
| RU2791215C1 (en) * | 2022-04-19 | 2023-03-06 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Уфимский государственный нефтяной технический университет" | Method for determining the reaction rate of hydrochloric acid with carbonate rock and a device for its implementation |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104597219A (en) * | 2014-12-26 | 2015-05-06 | 西南交通大学 | Water-rock chemical dynamic reaction double-system test unit |
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| CN105628549A (en) * | 2016-01-14 | 2016-06-01 | 太原理工大学 | Method for directly, quickly and full-automatically determining content of desorbing gas in coal seam |
| CN105628549B (en) * | 2016-01-14 | 2019-03-26 | 太原理工大学 | A kind of coal seam can desorbing mash gas content direct quickly full-automatic measuring method |
| CN109490071A (en) * | 2017-09-12 | 2019-03-19 | 中国石油天然气股份有限公司 | Acid fluid system integrates optimization experiment evaluation method |
| CN109490071B (en) * | 2017-09-12 | 2021-03-30 | 中国石油天然气股份有限公司 | Acid liquor system comprehensive optimization experimental evaluation method |
| CN114660224A (en) * | 2022-03-29 | 2022-06-24 | 西南石油大学 | Device and method for measuring reaction kinetic parameters of acid rock in high-viscosity liquid |
| RU2791215C1 (en) * | 2022-04-19 | 2023-03-06 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Уфимский государственный нефтяной технический университет" | Method for determining the reaction rate of hydrochloric acid with carbonate rock and a device for its implementation |
| CN115561189A (en) * | 2022-10-20 | 2023-01-03 | 西南石油大学 | Method for testing reaction rate of authigenic acid rock |
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Application publication date: 20130807 |