CN108318370B - Device and method for measuring wax dissolution rate and recovery ratio of wax remover under pressure - Google Patents
Device and method for measuring wax dissolution rate and recovery ratio of wax remover under pressure Download PDFInfo
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- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
本发明涉及油井清防蜡实验设备领域，具体的是一种带压测定清蜡剂溶蜡速率与回收比率的装置及其测定方法。装置主要由活塞容器A、承压的溶蜡反应釜、恒温箱、活塞容器B、承压的计量罐、回收罐以及若干配套的阀门仪表管线组成。该装置可以实现对任意试剂的溶蜡率测试以及该试剂的回收率测试。解决了许多常温常压下为气态，油井实际工作状态下为液态的相态易改变试剂在实验室环境下无法测定试剂溶蜡率的问题。
The invention relates to the field of oil well wax removal and prevention experimental equipment, in particular to a device for measuring the wax dissolution rate and recovery ratio of a wax remover under pressure and a measurement method thereof. The device is mainly composed of a piston container A, a pressure-bearing wax-dissolving reactor, a constant temperature box, a piston container B, a pressure-bearing measuring tank, a recovery tank and a number of matching valve and instrument pipelines. The device can realize the test of the wax dissolution rate of any reagent and the test of the recovery rate of the reagent. It solves the problem that many reagents that are gaseous at normal temperature and pressure and liquid in the actual working state of the oil well can easily change the phase state and cannot measure the wax-dissolving rate of the reagents in the laboratory environment.
Description
Technical Field
The invention relates to the field of oil well wax removal and prevention experimental equipment, in particular to a device for measuring the wax dissolving rate and recovery ratio of a wax remover under pressure and a measuring method thereof.
Background
Three major problems exist in the oil extraction process: sand production, scaling and wax deposition, which bring many troubles to the extraction and construction of crude oil. In the process of exploitation, the waxy crude oil rises along an oil pipe, and paraffin molecules in the waxy crude oil are crystallized and separated out due to the fact that the dissolution balance is damaged along with the change of environmental conditions such as temperature, pressure, flow rate and water content, and are deposited on the inner wall of the oil pipe in a concentrated mode. The deposition of paraffin on the inner wall of the oil pipe inevitably causes the reduction of an oil flow channel and the increase of flow resistance, so that the productivity of the oil well is reduced, and even the production is stopped. In order to solve this problem, many coping methods have been developed, and among them, the chemical wax removal and prevention technology is well received and widely adopted due to its characteristics of wide adaptability, high efficiency, simple operation process, etc.
The chemical paraffin removing and preventing agent has many kinds, which are mainly divided into oil-based paraffin removing and preventing agent, water-based paraffin removing and preventing agent and emulsion type paraffin removing and preventing agent, and the common paraffin removing and preventing agent has a common defect of being unrecoverable, so that the use cost is increased. Therefore, a novel water-based paraffin removal and prevention agent which is in a gas state at low pressure and is converted into a liquid state at high pressure is developed, the function of the conventional common paraffin removal and prevention agent can be realized under the underground high-pressure working condition, and the low-pressure paraffin removal and prevention agent can be vaporized and is convenient to recover, so that the novel water-based paraffin removal and prevention agent has the excellent characteristics of being green, safe and recyclable. When the wax dissolution rate of the novel wax removal and prevention agent is measured in a laboratory environment, the device and the method for measuring the wax removal rate in the industry standard cannot be suitable because the test cannot be carried out under normal pressure. Therefore, it is important to invent a new device and method for determining the paraffin removal efficiency and recovery rate of the paraffin remover with changeable phase state.
The existing wax removal and prevention rate testing device and standard method can change the temperature through water bath and other modes, but the applicable pressure is normal pressure. When the paraffin removal rate is tested under normal pressure, a certain amount of reagent is directly introduced into a test tube with a plug, then the plug is covered, the temperature is stabilized, then a wax ball is added, and the paraffin removal rate of the reagent is measured by measuring the dissolving amount of the wax ball in a certain time. For new reagents with easily changeable phase, it is difficult to complete the experiment due to the inability to control the amount of reagent added to the test tube at normal pressure and the difficulty in controlling the phase of the reagent. Meanwhile, the conventional reagent and method do not have a function of recovering the reagent. In this regard, it is necessary to develop an experimental method capable of controlling the amount of a reagent to be added and controlling the phase state of the reagent, and an experimental apparatus and method capable of measuring the recovery rate of the reagent.
The existing testing device can not meet the test of special reagents, such as a reagent which is in a gas state at normal pressure and then in a liquid state after being pressurized.
Disclosure of Invention
In order to solve the problem that an experimental device for measuring the paraffin removal rate and the recovery rate of a phase easily-changed reagent cannot be used in the prior art, the invention provides a device for measuring the paraffin dissolution rate and the recovery rate of the paraffin removal agent under pressure and a measuring method thereof, which are used for measuring the paraffin removal rate and the recovery rate of the phase easily-changed reagent and can realize measurement by controlling the phase of the reagent.
The specific technical scheme is as follows:
the device for measuring the wax dissolving rate and the recovery ratio of the paraffin remover under pressure comprises a wax dissolving reaction kettle, a piston container A, a piston container B and a recovery tank;
the upper part of the wax dissolving reaction kettle is connected with a tee joint A, the tee joint A is connected with the lower part of a piston container A through a needle valve O, and the tee joint A is also connected with the lower part of a piston container B through a needle valve A, a pressure gauge A and a needle valve B;
the lower part of the wax dissolving reaction kettle is connected with a recovery tank through a needle valve C and a tee joint B in sequence;
the upper parts of the piston container A and the piston container B, the wax dissolving reaction kettle, the recovery tank and the metering tank are respectively connected with a nitrogen bottle;
the lower part of the piston container A is connected with a reagent tank through a pressure gauge B and a needle valve D;
the upper part of the recovery tank is also communicated with the lower part of the piston container B through a tee joint B; the lower part of the recovery tank is connected with a needle valve E;
the lower part of the piston container B is also communicated with the metering tank through a needle valve F and a tee joint E; the lower part of the metering tank is connected with an external device through a needle valve G to recover the reagent;
the wax dissolving reaction kettle and the recovery tank are arranged in a thermostat with adjustable temperature.
Wherein, a needle valve H and a pressure regulating valve are connected on the nitrogen steel cylinder in sequence;
the upper part of the piston container A is connected with a pressure regulating valve through a needle valve I and a tee joint F to realize connection with a nitrogen steel cylinder so as to control the pressure in the piston container A;
the upper part of the piston container B is connected with a nitrogen steel cylinder through a needle valve J, a tee joint D, a needle valve K, a tee joint C, a pressure gauge C, a tee joint F and a connecting pressure regulating valve in sequence so as to control the pressure in the piston container B;
the upper part of the wax dissolving reaction kettle sequentially passes through a needle valve A, a four-way valve and a needle valve M, the needle valve M is connected with a pressure gauge C through a three-way valve C to realize connection with a nitrogen steel cylinder so as to control the pressure in the wax dissolving reaction kettle;
the upper part of the recovery tank is connected with a four-way valve through a needle valve N to realize connection with a nitrogen steel cylinder so as to control the pressure in the recovery tank;
needle valve L is connected through tee bend E in metering tank upper portion, and needle valve K is connected through tee bend D to needle valve L, realizes being connected with the nitrogen gas steel bottle to control metering tank internal pressure.
Furthermore, the upper part of the recovery tank is sequentially connected with a needle valve N and a four-way valve through a three-way valve B, and the four-way valve is connected with a pressure gauge A to realize communication with the lower part of a piston container B.
Specifically, the wax dissolving reaction kettle is a quartz glass cylinder, volume scales are arranged on the glass cylinder, a stainless steel sleeve is sleeved outside the glass cylinder, observation slits are formed in two sides of the stainless steel sleeve and used for observing the state in the quartz glass cylinder and reading the volume;
the upper flange of the wax dissolving reaction kettle is provided with a metal cover, a hook is arranged in the metal cover, one end of the thin line is connected with the wax ball, the other end of the thin line is connected with the iron sheet, the iron sheet is attracted outside the metal cover through a magnet, the wax ball is hung in the wax dissolving reaction kettle through the hook, and the hanging height of the wax ball is adjusted through adjusting the position of the iron sheet connected on the thin line.
The measuring tank is of a double-layer structure and is a quartz glass cylinder sleeved with a stainless steel cylinder, volume scales are arranged on the quartz glass cylinder, and observation slits are formed in two sides of the stainless steel cylinder and used for observing the state in the quartz glass cylinder and reading the volume.
The invention also provides a related test method:
(1) the paraffin removal agent which is gaseous at normal pressure is liquefied and enters the reaction kettle through the pressure stabilization of the piston container A, and the temperature is controlled through the thermostat so as to measure the paraffin dissolution rate of the liquefied reagent.
(2) The paraffin removing agent in the reaction kettle is dissolved in the wax and then enters a recovery tank, and the gasified and liquefied reagent enters a metering tank for metering to determine the recovery rate of the reagent through temperature control of a thermostat and continuous pressure reduction and pressurization of a piston container B.
Firstly, the method for measuring the wax dissolving rate of the paraffin remover under pressure by using the device for measuring the wax dissolving rate and the recovery ratio of the paraffin remover under pressure comprises the following steps:
the method comprises the following steps: suspending a wax ball with the mass M in a wax dissolving reaction kettle before the start of an experiment;
step two: controlling the pressure in the wax-dissolving reaction kettle to be higher than the saturated vapor pressure of the reagent, so that the reagent filled in the wax-dissolving reaction kettle is in a liquid state and is filled to a proper amount, and adjusting the temperature of the thermostat to ensure that the temperature of the wax-dissolving reaction kettle is constant;
step three: dropping the wax ball into the reagent and starting timing;
step four: dissolving wax for a certain time, and displacing all reagents in the wax dissolving reaction kettle) under pressure into a recovery tank.
Step five: emptying to change the pressure in the wax dissolving reaction kettle to normal pressure, opening the wax dissolving reaction kettle, taking out the wax balls, drying and weighing, wherein the mass of the wax balls after reaction is m;
and (3) calculating: wax dissolution rate:
secondly, the method for measuring the recovery ratio of the paraffin remover under pressure measures the recovery ratio of the paraffin remover entering a recovery tank after the measurement of the paraffin dissolving rate is finished by using the device for measuring the paraffin dissolving rate and the recovery ratio of the paraffin remover under pressure, and the volume of the paraffin remover in the recovery tank is V, and comprises the following steps:
the method comprises the following steps: the pressure in the upper part of the piston container B is controlled to gradually reduce the pressure in the recovery tank, and the gasified reagent is extruded into the metering tank until the pressure in the recovery tank is reduced to the normal pressure;
step two: pressurizing to enable the pressure in the measuring tank to be higher than the steam pressure of the reagent, and reading the liquid amount v in the measuring tank;
and (3) calculating:
the device for determining the wax dissolving rate and the recovery ratio of the paraffin remover under pressure and the determination method thereof provided by the invention are suitable for a special reagent which is in a gas state at normal pressure and is in a liquid state after being pressurized, and can be used for determining the wax dissolving rate and determining the recovery ratio of the special reagent under pressure.
The invention has the following specific technical effects:
1 all devices are connected with a nitrogen cylinder, the nitrogen cylinder provides enough driving pressure and high-pressure environment for the whole experimental device, and the high-pressure environment in the piston container A and the wax dissolving reaction kettle can ensure that the phase state of the reagent is liquid.
2 dissolve wax reation kettle and a measurement section of thick bamboo and adopt the glass material to solve the problem that reagent dissolves the reation kettle material, overcoat stainless steel section of thick bamboo is in order to bear the high pressure, and stainless steel section of thick bamboo both sides are to slotting, so that observe the interior situation of reation kettle, read a liquid level height in the section of thick bamboo, thereby the volume of adding of control reagent.
3 dissolve wax reation kettle upper flange and for dismantling the metal covering, have the couple in the metal covering, can hang the wax ball through the fine rule. The metal sheet is bound on the thin wire, and the metal sheet can be attracted by the magnet outside the metal cover, so that the wax ball is suspended. The suspension height of the wax ball can be adjusted by adjusting the position of the metal sheet on the fine line, and the magnet is taken down after the reaction kettle is kept at a constant temperature to enable the wax ball to fall down and be suspended and immersed in the paraffin remover.
4 in the experiment of reagent recovery rate measurement, the wax dissolving agent after compression liquefaction enters the metering tank by heating the wax dissolving reaction kettle and continuously pumping and compressing the piston container B, thereby simulating multi-stage degassing in oil exploitation. The recovery rate of the reagent can be accurately measured through the experimental operation.
5 this set of experimental apparatus not only can satisfy the survey that the phase state easily changed reagent paraffin removal rate, can also be directly used for surveing the wax dissolution rate of various paraffin removal and prevention agents under different pressure, different temperature, different dissolved gas-oil ratios, is a new experimental apparatus of survey paraffin removal rate.
Drawings
Fig. 1 is a schematic structural view of the present invention.
FIG. 2 is a schematic view of the structure of a wax dissolving reaction kettle of the present invention;
fig. 3 is a schematic view of a wax ball fixing structure of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As shown in figure 1, the device for measuring the wax dissolving rate and the recovery ratio of the paraffin remover under pressure comprises a wax dissolving reaction kettle 12, a piston container A10, a piston container B24 and a recovery tank 15;
the upper part of the wax dissolving reaction kettle 12 is connected with a tee joint A30, the tee joint A30 is connected with the lower part of a piston container A10 through a needle valve O11, and the tee joint A30 is also connected with the lower part of a piston container B24 through a needle valve A6, a pressure gauge A21 and a needle valve B22;
the lower part of the wax dissolving reaction kettle 12 is connected with a recovery tank 15 through a needle valve C14 and a tee joint B31 in sequence;
the upper part of the piston container A10, the upper part of the piston container B24, the wax dissolving reaction kettle 12, the recovery tank 15 and the upper part of the metering tank 27 are respectively connected with a nitrogen bottle 1;
the lower part of the piston container A10 is connected with the reagent tank 5 through a pressure gauge B8 and a needle valve D4;
the upper part of the recovery tank 15 is also communicated with the lower part of a piston container B24 through a tee joint B31; the needle valve E17 is connected to the lower part of the recovery tank 15;
the lower part of the piston container B24 is also communicated with the metering tank 27 through a needle valve F25 and a tee joint E34; the lower part of the metering tank 27 is connected with an external device through a needle valve G28 to recover the reagent;
the wax dissolving reaction kettle 12 and the recovery tank 15 are placed in a thermostat 13 capable of adjusting the temperature.
Wherein, a needle valve H2 and a pressure regulating valve 3 are connected on the nitrogen steel cylinder 1 in sequence;
the upper part of the piston container A10 is connected with a pressure regulating valve 3 through a needle valve I9 and a tee joint F35 to realize connection with a nitrogen steel cylinder 1 so as to control the pressure in the piston container A10;
the upper part of the piston container B24 is connected with the nitrogen steel cylinder 1 through a needle valve J23, a tee joint D33, a needle valve K20, a tee joint C32, a pressure gauge C18, a tee joint F35 and a connecting pressure regulating valve 3 in sequence so as to control the pressure in the piston container B24;
the upper part of the wax dissolving reaction kettle 12 sequentially passes through a needle valve A6, a four-way valve 29 and a needle valve M19, the needle valve M19 is connected with a pressure gauge C18 through a three-way valve C32 to realize connection with a nitrogen steel cylinder 1 so as to control the pressure in the wax dissolving reaction kettle 12;
the upper part of the recovery tank 15 is connected with a four-way valve 29 through a needle valve N16 to realize the connection with the nitrogen steel cylinder 1 so as to control the pressure in the recovery tank 15;
the upper part of the measuring tank 27 is connected with a needle valve L26 through a tee joint E34, and the needle valve L26 is connected with a needle valve K20 through a tee joint D33 to realize connection with the nitrogen gas steel cylinder 1 so as to control the pressure in the measuring tank 27.
Furthermore, the upper part of the recovery tank 15 is sequentially connected with a needle valve N16 and a four-way valve 29 through a three-way valve B31, and the four-way valve 29 is connected with a pressure gauge A21 to realize the communication with the lower part of a piston container B24.
As shown in fig. 2, specifically, the wax dissolving reaction kettle 12 is a quartz glass cylinder, the glass cylinder is provided with volume scales, and is externally sleeved with a stainless steel sleeve, and observation slits are formed on two sides of the stainless steel sleeve and used for observing the state in the quartz glass cylinder and reading the volume;
as shown in fig. 3, a metal cover 121 is flanged on the wax dissolving reaction kettle 12, a hook 122 is arranged in the metal cover 121, one end of a thin wire 123 is connected with a wax ball 125, the other end of the thin wire is connected with an iron sheet 124, the iron sheet 124 is attracted by a magnet outside the metal cover 121, the wax ball 125 is hung in the wax dissolving reaction kettle 12 through the hook 122, and the hanging height of the wax ball 125 is adjusted by adjusting the position of the iron sheet 124 connected on the thin wire 123.
The metering tank 27 is of a double-layer structure and is a quartz glass cylinder sleeved with a stainless steel cylinder, volume scales are arranged on the quartz glass cylinder, and observation slits are formed in two sides of the stainless steel cylinder and used for observing the state in the quartz glass cylinder and reading the volume.
The method for measuring the paraffin removal rate and the recovery rate of the special paraffin remover which is easy to change the phase state is introduced below, the special paraffin remover is changed into a gas state at normal temperature and normal pressure and is in a liquid state under the actual working condition of an oil well, the device for measuring the paraffin dissolving rate and the recovery rate of the paraffin remover under pressure is used, and the method for measuring the paraffin removal rate and the recovery rate of the special paraffin remover comprises the following steps:
① wax-dissolving rate determination experiment of wax remover
The method comprises the following steps: before the experiment is started, all valves are closed, a metal cover 121 of the wax dissolving reaction kettle 12 is opened, a fine wire 123 is hung at a hook 122 in the cover, a prepared wax ball 125 with the mass of M is hung at the lower end of the fine wire 123, an iron sheet 124 is bound on the fine wire 123, a magnet is placed outside the cover to enable the iron sheet 124 to be absorbed inside the cover, the wax ball 125 is hung at the top of the wax dissolving reaction kettle 12, and the metal cover 121 is covered.
Step two: opening the nitrogen cylinder 1, the needle valve H2 and the needle valve I9, regulating the pressure of the pressure regulating valve 3 to the pressure required by the experiment, such as 1.0MPa, filling the nitrogen gas into the upper part of the piston container A10, pushing the piston to the lower part of the container, and closing the needle valve I9. Opening a needle valve M19, a needle valve N16 and a needle valve A6 to make the pressure in the wax dissolving reaction kettle 12 and the recovery tank 15 reach the pressure required by the experiment, such as 1.0MPa, and closing the needle valve M19 and the needle valve N16.
Step three: the needle valve D4 and the needle valve I9 are opened, the reagent enters the piston container A10, the reading of a pressure gauge C18 is observed, and when the reading of the pressure gauge is not changed, the reading is recorded, and the needle valve D4 and the needle valve I9 are closed.
Step four: the needle valve O11 is opened to let the reagent enter the wax-dissolving reaction kettle 12, and the adding amount is controlled from the scale.
Step five: the needle valve M19 and the needle valve N16 are opened, the pressure regulating valve 3 is adjusted to make the pressure in the wax dissolving reaction kettle 12 and the recovery tank 15 larger than the saturated vapor pressure of the reagent after the subsequent temperature rise, for example, 2.0MPa, and the needle valve M19 and the needle valve N16 are closed. And (3) adjusting the temperature of the constant temperature box 13 to 45 ℃, and keeping the constant temperature to keep the temperature of the wax dissolving reaction kettle 12 constant.
Step six: after the temperature is kept constant for 1h, the magnet on the metal cover 121 of the wax dissolving reaction kettle 12 is taken out to enable the wax ball 125 to fall into the reagent, and the timing is started.
Step seven: after timing t (such as 30min), opening the needle valve M19 and the needle valve C14, pressurizing to make all the reagents in the wax-dissolving reaction kettle 12 enter the recovery tank 15, and closing the needle valve C14 and the needle valve H2.
Step eight: and (3) opening a needle valve K20 to be empty, changing the pressure of the wax dissolving reaction kettle 12 to normal pressure, closing a needle valve M19, a needle valve A6 and a needle valve K20, opening a metal cover 121 of the wax dissolving reaction kettle 12, taking out the wax ball 125, drying and weighing, wherein the mass of the wax ball 125 after reaction is M.
Remarking: by utilizing the device and the method, the wax dissolving rates of different paraffin cleaners can be measured so as to perform comparative evaluation on the wax dissolving effects of the different paraffin cleaners.
Wax dissolution rate:
② test for determining recovery rate of paraffin remover after dissolving wax
This experiment is intended to measure the recovery rate of the volume V of the paraffin remover introduced into the recovery tank 15 after the measurement of the paraffin dissolution rate is completed.
The method comprises the following steps: opening the nitrogen cylinder 2 valve and adjusting the pressure regulating valve 3 to the pressure required by the experiment such as 1.0MPa, opening the needle valve J23, the needle valve F25 and the needle valve G28, releasing the pressure at the lower part of the piston container B24, pushing the piston to the bottom of the container, enabling the pressure at the upper part of the piston to reach the pressure required by the experiment, and closing the needle valve J23, the needle valve F25 and the needle valve G28. The needle valve L26 is opened to make the pressure in the measuring tank 27 reach the pressure required by the experiment, such as 1.0MPa, and then the needle valve L26 is closed.
Step two: the incubator 13 is adjusted to the appropriate temperature X ℃ and recorded.
Step three: needle-off valve H2. Needle valve N16, needle valve B22, needle valve J23, and needle valve K20 was opened slowly to release pressure from the upper part of piston container B24. Reading the indication Y of the pressure gauge A21 after a certain time interval1MPa and record, needle-off valve K20, needle valve B22.
Step four: after a needle valve H2 is opened, a piston container B24 is pressurized and the pressure reaches the vapor pressure at the temperature of X.degree.C.for recovering the reagent, a needle valve F25 is opened, the paraffin remover is liquefied and then introduced into the measuring cylinder 27, and a needle valve F25 is closed. Reading the volume v of the recovered reagent from the measuring cylinder 27 after the temperature has stabilized1And (3) ml. Obtain a set of data X temperature Y1The amount recovered under pressure is v1。
Step five: and repeating the third step and the fourth step. And obtaining and recording a plurality of groups of data until the pressure gauge A21 becomes 0.1MPa, wherein the total liquid volume v in the metering cylinder 27 is the final recovered liquid volume of the paraffin remover.
Step six: the open needle valve G28 recovered the reagent and the experiment was stopped.
The above description is only exemplary of the invention and should not be taken as limiting the scope of the invention, so that the invention is intended to cover all modifications and equivalents of the embodiments described herein. In addition, the technical features, the technical schemes and the technical schemes can be freely combined and used.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810011732.9A CN108318370B (en) | 2018-01-05 | 2018-01-05 | Device and method for measuring wax dissolution rate and recovery ratio of wax remover under pressure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810011732.9A CN108318370B (en) | 2018-01-05 | 2018-01-05 | Device and method for measuring wax dissolution rate and recovery ratio of wax remover under pressure |
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| Publication Number | Publication Date |
|---|---|
| CN108318370A CN108318370A (en) | 2018-07-24 |
| CN108318370B true CN108318370B (en) | 2020-04-21 |
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| CN102393344B (en) * | 2011-10-17 | 2014-08-20 | 中国石油化工股份有限公司 | Device for measuring solubility of gas in liquid with higher boiling point and method |
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| CN203519587U (en) * | 2013-10-24 | 2014-04-02 | 中国石油天然气股份有限公司 | Paraffin removal rate measuring device for paraffin remover |
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