CN107976529A - A kind of multifunctional reaction still experimental system and experimental method - Google Patents
A kind of multifunctional reaction still experimental system and experimental method Download PDFInfo
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Abstract
A kind of multifunctional reaction still experimental system and experimental method, the system includes piston container, gas cylinder, cooler, valve one and mass flowmenter are connected to the top of piston container in turn, constant speed and constant pressure pump is connected by valve two with the bottom of piston container, branch is separately arranged at the top of piston container, by being divided into three branches after valve three, pass through valve four respectively, valve five and valve six and reaction kettle left upper portion, middle part is connected with lower part, reaction kettle right upper portion, middle part, lower part and bottom separate four branches respectively by valve seven, valve eight, valve nine, valve ten is connected with sampler, sampler bottom connection valve 11；The invention also discloses the experimental method of the system；The present invention is used to test conventional hydraulic fracturing fluid or CO2After the interaction of anhydrous fracturing fluid and reservoir, mineral ion concentration situation of change of taking a sample to research；Static test can be carried out and dynamic is tested, analyze mineral ion situation of change in the reaction solution of different level.
Description
Technical field
The present invention relates to oil and gas Development Engineering field, more particularly to a kind of multifunctional reaction still experimental system and
Experimental method.
Background technology
Current people's mini-frac liquid interacts mainly for the common hydrofrac fluid used in industry, example with reservoir
Such as gelled fracturing fluid, or the liquid fracturing fluid such as riverfrac treatment liquid.Actual fracturing fluid is in formation fracture relative to fracture faces
During flowing, the liquid sample single ionic concentration in crack is generally mainly influenced be subject to fracturing fluid ion concentration, general constant in the short time.
And rock sample and fracturing fluid sample are generally placed in a fixed container current line by experimental study in the industry, with fracturing fluid and storage
The progress of layer mineral chemistry effect, certain interior single ionic concentration of container are likely to change, this may be to fracturing fluid and reservoir phase
Interaction or the speed of reaction, power have an impact, it is impossible to which accurately analog study actual reservoir thing is believed, and research mineral ion
Concentration situation of change.
In recent years, a kind of new fracturing technique-carbon dioxide pressure break technology gradually warms up, and more and more people open
Beginning studies him；Wherein, carbon dioxide pressure break liquid is mainly made of carbon dioxide and the mixing of certain chemical reagent.For
Currently used CO2Anhydrous this kind of gas fracturing fluid of fracturing fluid, temporarily without mature equipment product simulation itself and reservoir Dynamic in industry
Interaction.
The content of the invention
In order to overcome problem existing in the prior art, object of the present invention is to provide a kind of experiment of multifunctional reaction still
System and experimental method, for testing conventional hydraulic fracturing fluid or CO2After the interaction of anhydrous fracturing fluid and reservoir, sampling
Study mineral ion concentration situation of change；Static test can be carried out and dynamic is tested, analyzed in the reaction solution of different level
Mineral ion situation of change.
In order to achieve the above object, the technical solution taken of the present invention is：
A kind of multifunctional reaction still experimental system, including piston container 5, gas cylinder 1, cooler 2, valve 1 and mass flow
Meter 4 is connected to the top of piston container 5 in turn, and constant speed and constant pressure pump 6 is connected by valve 27 with the bottom of piston container 5, piston
Branch is separately arranged at the top of container 5, by being divided into three branches after valve 38, respectively by valve 49, valve 5 10 and valve 6 11 and instead
22 left upper portion of kettle, middle part is answered to be connected with lower part, 22 right upper portion of reaction kettle, middle part, lower part and bottom separate four branches
It is connected respectively by valve 7 12, valve 8 13, valve 9 14, valve 10 with sampler 19,19 bottom connection valve 11 of sampler.
The top of the piston container 5 can open, convenient to inject liquid sample；Convenient test conventional hydraulic fracturing fluid and dioxy
Change carbon fracturing fluid (CO2With chemical reagent mixture) interaction under different temperatures, pressure, concentration conditions experiment.
The volume of the volumetric ratio reaction kettle 22 of the piston container 5 is 5-20 times big, for convenience with liquid successively, carries out multiple
Test operation.
22 both sides of reaction kettle are designed with the multiple inflow branches in upper, middle and lower position and upper, middle and lower, bottom outflow branch
Road, needs to select to open according to experiment.
The reaction kettle 22 is placed in inside temperature-controlled box 21, and the top of reaction kettle 22 is equipped with blender 15, and bottom has and can hold
The pallet 17 of rock sample 16 is held in the palm, 17 bottom of pallet is network, so that 16 bottom of rock sample cannot be contacted with fracturing fluid sample.
The volume of the sampler 19 is less than the volume of reaction kettle 22, convenient in experimentation, anti-in reaction kettle 22
Ying Hou, the liquid sample test analysis of taking-up at any time from upper, middle and lower, bottom different layers position.
The experimental method of the multifunctional reaction still experimental system,
1) when mini-frac liquid is CO2During anhydrous fracturing fluid：
First, all valves are closed, open piston container 5, by the chemical reagent needed with fracturing fluid injection wherein；So
Afterwards, valve 1 is opened, the CO in gas cylinder 12Gas once flows to piston container 5 by cooler 2, valve 1, mass flowmenter 4
In, and the CO flowed in piston container 5 is measured by mass flowmenter 42Gaseous mass, with reference to being injected into piston container 5
The quality of chemical reagent, calculates the mass concentration of the chemical reagent in piston container 5 in fracturing fluid, and calculation formula is：Chemistry
The mass concentration of reagent=chemical reagent quality/(CO in chemical reagent quality+injection 52Gaseous mass) × 100%), Ran Houguan
Valve closing 1；
Valve 27 and constant speed and constant pressure pump 6 are opened, by the CO in piston container 52Anhydrous fracturing fluid is pressurized to target experimental pressure
Condition；
Reaction kettle 22 is opened by above the pallet 11 in 16 portion disposed within of rock sample, closes reaction kettle 22；Then temperature control is adjusted
Case 21 is to target experimental temperature；
Valve 27 is then shut off, opens valve 38, is opened for one in selector valve 49, valve 5 10 and valve 6 11, to reaction kettle 22
In fill fracturing fluid, it is ensured that 16 surface of rock sample can touch fracturing fluid；As needed, after at interval of preset time, selection is beaten
One of valve opening 7 12, valve 8 13, valve 9 14 and valve 10 so that 22 inside liquid sample of reaction kettle is flowed into sampler 19, is surveyed
Examination analysis；
Inject fracturing fluid concentration control method：Injection CO is measured by mass flowmenter 42Amount and injection piston container 5
Chemical reagent amount control；
(1) during static test：It is selective after reacting a period of time with rock sample 16 after fracturing fluid fills reaction kettle 22
Mineral ion situation of change in from the reaction solution of the upper, middle and lower of reaction kettle 22 and bottom sampling and testing analysis different level；
(2) when dynamic is tested：After fracturing fluid fills reaction kettle 22, after reacting a period of time with rock sample 16, selector valve four
9th, an opening in valve 5 10, valve 6 11, continues to input liquid oxygen from one of upper, middle and lower portion of reaction kettle 22；At the same time from reaction kettle
Mineral ion situation of change in the reaction solution of 22 upper, middle and lower and bottom sampling and testing analysis different level, is analyzed to the greatest extent different
Mineral ion situation of change in the reaction solution of aspect；
Change experimental temperature, pressure, fracturing fluid concentration conditions, carry out the test under next experiment condition；Experiment test knot
Shu Hou, opens valve 10 and valve 11, sample discharge recycling；
2) when mini-frac liquid is liquid fracturing fluid：
Before experiment starts by liquid fracturing fluid injection piston container 5, that is, experiment test need to only be started, be simply not required to
Inject CO2Gas, other methods are constant, opposite to test CO2The method of fracturing fluid is simpler.
16 rock sample can be the duckpin rock sample or sillar of a certain size particle either definite shape.Described 15
Blender can be opened when rock sample is reacted with fracturing fluid as needed, to promote fully reaction.
Compared to the prior art compared with the present invention has the following advantages：
(1) conventional hydraulic fracturing fluid and carbon dioxide pressure break liquid (CO can be tested2With a small amount of chemical reagent mixture),
Interaction under different temperatures, pressure, fracturing fluid concentration conditions with rock sample.
(2)CO2The concentration of fracturing fluid, can be by injecting CO2Amount (being measured with mass flowmenter 4) and injection piston hold
The chemical reagent amount control of device 5.The concentration of common hydrofrac fluid is injected in 5 piston containers one after directly preparing.
(3) reaction kettle 22 is designed with three entrances, and four outlets, and test mini-frac liquid is in different temperatures, pressure, pressure
When splitting under liquid concentration conditions the interaction with rock sample, different layer position injections, and different levels can be conveniently studied
Take out fracturing fluid sample analysis in position.
(4) it is designed with 19 volume of sampler and is much smaller than reaction kettle 22, it is convenient in experimentation, reacted in reaction kettle 22
Afterwards, from the liquid sample test analysis of taking-up at any time of upper, middle and lower, bottom different layers position.
(5) 17 bottom of pallet is network, it is ensured that rock sample bottom can come into full contact with fracturing fluid sample, it is ensured that no
Influence the precision of reaction and experiment.
Brief description of the drawings
Fig. 1 is multifunctional reaction still experimental system figure of the present invention.
Embodiment
The present invention is described in further details with reference to the accompanying drawings and detailed description.
As shown in Figure 1, a kind of multifunctional reaction still experimental system of the present invention, including piston container 5, gas cylinder 1, cooler 2,
Valve 1 and mass flowmenter 4 are connected to the top of piston container 5 in turn, and constant speed and constant pressure pump 6 passes through valve 27 and piston container 5
Bottom is connected, and branch is separately arranged at the top of piston container 5, by being divided into three branches after valve 38, passes through valve 49, valve five respectively
10 and valve 6 11 be connected with 22 left upper portion of reaction kettle, middle part and lower part, 22 right upper portion of reaction kettle, middle part, lower part and bottom
Part go out four branches be connected respectively by valve 7 12, valve 8 13, valve 9 14, valve 10 with sampler 19,19 bottom of sampler
Portion's connection valve 11.
22 both sides of reaction kettle are designed with the multiple inflow branches in upper, middle and lower position and upper, middle and lower, bottom outflow branch
Road, needs to select to open according to experiment.
As the preferred embodiment of the present invention, the top of the piston container 5 can open, convenient to inject liquid sample；Side
Just conventional hydraulic fracturing fluid and carbon dioxide pressure break liquid (CO are tested2With chemical reagent mixture) in different temperatures, pressure, concentration
Under the conditions of interaction experiment.
As the preferred embodiment of the present invention, the volume of the volumetric ratio reaction kettle 22 of the piston container 5 is 5-20 times big,
For convenience with liquid successively, multiple test operation is carried out.
As the preferred embodiment of the present invention, the reaction kettle 22 is placed in inside temperature-controlled box 21, and the top of reaction kettle 22
Equipped with blender 15, the pallet 17 for being capable of support rock sample 16 is arranged at bottom, and 17 bottom of pallet is network, so that rock sample 16
Bottom cannot be contacted with fracturing fluid sample.
As the preferred embodiment of the present invention, the volume of the sampler 19 is less than the volume of reaction kettle 22, conveniently exists
In experimentation, after being reacted in reaction kettle 22, the liquid sample test analysis of taking-up at any time from upper, middle and lower, bottom different layers position.
The experimental method of multifunctional reaction still experimental system of the present invention,
1) when mini-frac liquid is CO2During anhydrous fracturing fluid：
First, all valves are closed, open piston container 5, by the chemical reagent needed with fracturing fluid injection wherein；So
Afterwards, valve 1 is opened, the CO in gas cylinder 12Gas once flows to piston container 5 by cooler 2, valve 1, mass flowmenter 4
In, and the CO flowed in piston container 5 is measured by mass flowmenter 42Gaseous mass, with reference to being injected into piston container 5
The quality of chemical reagent, calculates the mass concentration of the chemical reagent in piston container 5 in fracturing fluid, and calculation formula is：Chemistry
The mass concentration of reagent=chemical reagent quality/(CO in chemical reagent quality+injection 52Gaseous mass) × 100%), Ran Houguan
Valve closing 1；
Valve 27 and constant speed and constant pressure pump 6 are opened, by the CO in piston container 52Anhydrous fracturing fluid is pressurized to target experimental pressure
Condition；
Reaction kettle 22 is opened by above the pallet 11 in 16 portion disposed within of rock sample, closes reaction kettle 22；Then temperature control is adjusted
Case 21 is to target experimental temperature；
Valve 27 is then shut off, opens valve 38, is opened for one in selector valve 49, valve 5 10 and valve 6 11, to reaction kettle 22
In fill fracturing fluid, it is ensured that 16 surface of rock sample can touch fracturing fluid；As needed, after at interval of preset time, selection is beaten
One of valve opening 7 12, valve 8 13, valve 9 14 and valve 10 so that 22 inside liquid sample of reaction kettle is flowed into sampler 19, is surveyed
Examination analysis；
Inject fracturing fluid concentration control method：Injection CO is measured by mass flowmenter 42Amount and injection piston container 5
Chemical reagent amount control；
(1) during static test：It is selective after reacting a period of time with rock sample 16 after fracturing fluid fills reaction kettle 22
Mineral ion situation of change in from the reaction solution of the upper, middle and lower of reaction kettle 22 and bottom sampling and testing analysis different level；
(2) when dynamic is tested：After fracturing fluid fills reaction kettle 22, after reacting a period of time with rock sample 16, selector valve four
9th, an opening in valve 5 10, valve 6 11, continues to input liquid oxygen from one of upper, middle and lower portion of reaction kettle 22；At the same time from reaction kettle
Mineral ion situation of change in the reaction solution of 22 upper, middle and lower and bottom sampling and testing analysis different level, is analyzed to the greatest extent different
Mineral ion situation of change in the reaction solution of aspect；
Change experimental temperature, pressure, fracturing fluid concentration conditions, carry out the test under next experiment condition；Experiment test knot
Shu Hou, opens valve 10 and valve 11, sample discharge recycling；
2) when mini-frac liquid is liquid fracturing fluid：
Before experiment starts by liquid fracturing fluid injection piston container 5, that is, experiment test need to only be started, be simply not required to
Inject CO2Gas, other methods are constant, opposite to test CO2The method of fracturing fluid is simpler.
Claims (7)
- A kind of 1. multifunctional reaction still experimental system, it is characterised in that：Including piston container (5), gas cylinder (1), cooler (2), Valve one (3) and mass flowmenter (4) are connected to the top of piston container (5) in turn, constant speed and constant pressure pump (6) by valve two (7) with The bottom of piston container (5) is connected, and branch is separately arranged at the top of piston container (5), by being divided into three branches after valve three (8), It is connected respectively by valve four (9), valve five (10) and valve six (11) with reaction kettle (22) left upper portion, middle part and lower part, is reacted Kettle (22) right upper portion, middle part, lower part and bottom separate four branches respectively by valve seven (12), valve eight (13), valve nine (14), Valve ten (18) is connected with sampler (19), sampler (19) bottom connection valve 11 (20).
- A kind of 2. multifunctional reaction still experimental system according to claim 1, it is characterised in that：The piston container (5) Top can open, it is convenient to inject liquid sample；Convenient test conventional hydraulic fracturing fluid and carbon dioxide pressure break liquid different temperatures, Interaction experiment under pressure, concentration conditions.
- A kind of 3. multifunctional reaction still experimental system according to claim 1, it is characterised in that：The piston container (5) Volumetric ratio reaction kettle (22) volume it is 5-20 times big, for convenience with liquid successively, carry out multiple test operation.
- A kind of 4. multifunctional reaction still experimental system according to claim 1, it is characterised in that：The reaction kettle (22) two Side is designed with the multiple inflow branches in upper, middle and lower position and upper, middle and lower, bottom outflow branch, needs selection to open according to experiment Open.
- A kind of 5. multifunctional reaction still experimental system according to claim 1, it is characterised in that：The reaction kettle (22) is put It is internal in temperature-controlled box (21), and blender (15) is housed at the top of reaction kettle (22), the pallet for being capable of support rock sample (16) is arranged at bottom (17), pallet (17) bottom is network, so that rock sample (16) bottom cannot be contacted with fracturing fluid sample.
- A kind of 6. multifunctional reaction still experimental system according to claim 1, it is characterised in that：The sampler (19) Volume is less than the volume of reaction kettle (22), convenient in experimentation, in reaction kettle (22) after reaction, from upper, middle and lower, bottom The liquid sample test analysis of taking-up at any time of portion different layers position.
- 7. the experimental method of claim 1 to 6 any one of them multifunctional reaction still experimental system, it is characterised in that：1) when mini-frac liquid is CO2During anhydrous fracturing fluid：First, all valves are closed, open piston container (5), by the chemical reagent needed with fracturing fluid injection wherein；Then, Valve one (3) is opened, the CO in gas cylinder (1)2Gas once flows to piston by cooler (2), valve one (3), mass flowmenter (4) In container (5), and the CO flowed in piston container (5) is measured by mass flowmenter (4)2Gaseous mass, with reference to being injected into The quality of chemical reagent in piston container (5), calculates the mass concentration of the chemical reagent in piston container (5) in fracturing fluid, It is then shut off valve one (3)；Valve two (7) and constant speed and constant pressure pump (6) are opened, by the CO in piston container (5)2Anhydrous fracturing fluid is pressurized to target experiment pressure Power condition；The pallet (11) in rock sample (16) portion disposed within above, is closed reaction kettle (22) by opening reaction kettle (22)；Then adjust Temperature-controlled box (21) is to target experimental temperature；It is then shut off valve two (7), opens valve three (8), opened for one in selector valve four (9), valve five (10) and valve six (11), to anti- Answer in kettle (22) and fill fracturing fluid, it is ensured that rock sample (16) surface can touch fracturing fluid；As needed, at interval of preset time Afterwards, one of valve seven (12), valve eight (13), valve nine (14) and valve ten (18) are opened in selection so that the internal liquid sample stream of reaction kettle (22) Enter in sampler (19), carry out test analysis；Inject fracturing fluid concentration control method：Injection CO is measured by mass flowmenter (4)2Amount and injection piston container (5) Chemical reagent amount controls；(1) during static test：It is selective after reacting a period of time with rock sample (16) after fracturing fluid fills reaction kettle (22) Mineral ion situation of change in from the reaction solution of the upper, middle and lower of reaction kettle (22) and bottom sampling and testing analysis different level；(2) when dynamic is tested：After fracturing fluid fills reaction kettle (22), after reacting a period of time with rock sample (16), selector valve four (9), an opening in valve five (10), valve six (11), continues to input liquid oxygen from one of upper, middle and lower portion of reaction kettle (22)；At the same time Mineral ion situation of change in from the reaction solution of the upper, middle and lower of reaction kettle (22) and bottom sampling and testing analysis different level, to the greatest extent And analyze mineral ion situation of change in the reaction solution of different level；Change experimental temperature, pressure, fracturing fluid concentration conditions, carry out the test under next experiment condition；After experiment test, Open valve ten (18) and valve 11 (20), sample discharge recycling；2) when mini-frac liquid is liquid fracturing fluid：By in liquid fracturing fluid injection piston container (5), that is, experiment test need to only be started before experiment starts, simply need not Inject CO2Gas, other methods are constant, opposite to test CO2The method of fracturing fluid is simpler.
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| CN110412221A (en) * | 2019-08-01 | 2019-11-05 | 中国石油大学(华东) | It is a kind of simulate reservoir home state frothy gel prepare evaluating apparatus and its application method |
| CN113903236A (en) * | 2021-10-22 | 2022-01-07 | 中铁二院工程集团有限责任公司 | Intelligent temperature and pressure control difference water-rock action contrast monitoring experimental device and experimental method thereof |
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