CN209356413U - A kind of experimental provision of quick measurement acid fluid system to the rejection ability of secondary precipitation - Google Patents
A kind of experimental provision of quick measurement acid fluid system to the rejection ability of secondary precipitation Download PDFInfo
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- CN209356413U CN209356413U CN201821759995.XU CN201821759995U CN209356413U CN 209356413 U CN209356413 U CN 209356413U CN 201821759995 U CN201821759995 U CN 201821759995U CN 209356413 U CN209356413 U CN 209356413U
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Abstract
The utility model discloses a kind of for quickly measuring acid fluid system to the experimental provision of the rejection ability of secondary precipitation.The experimental provision uses in Oil Field sandstone acidizing, and specifically include that thermostat, multiple closed reaction vessels and the one-to-one blender of the closed reaction vessel and the one-to-one test tube clamp of the closed reaction vessel and the one-to-one thermometer of the closed reaction vessel, the pipette for quantitatively pipetting liquid and the iron stand for experimental provision to be fixed, and the closed reaction vessel is made of resistant material.The utility model can relatively rapid can obtain experimental result to the complexing power of metal ion by Fast Evaluation complexing agent at high temperature.
Description
Technical field
The utility model relates to a kind of experimental provisions used in Oil Field sandstone acidizing, more particularly to one kind
Quickly experimental provision of the measurement complexing agent to complexing of metal ion ability.
Background technique
Sandstone acidizing refers to using the pollution near acid solution releasing oil-water well shaft bottom, restores or improve sandstone reservoir infiltration
One well production increment of rate, intensified injection of wells measure.Sandstone mineral composition is complicated, directly carries out corrosion with mud acid, usually generates
Serious secondary precipitation injury.There is no the standard for the evaluation of sandstone acidizing secondary precipitation rejection in petrochemical industry,
And secondary precipitation is related to fluoride, fluosilicate, fluoaluminate, hydroxide etc., many kinds of, complicated component.Currently, domestic
Rock core flowing and large-scale instrument is mainly taken to detect mutually matched method to study acid fluid system outside；Test procedure are as follows: setting
It counts under temperature and pressure, with the acid fluid system primarily determined, carries out acid/unvenile water solid phase reaction, measurement by different fluid injection programs
Different phase pressure, discharge capacity, the variation of core permeability before and after comparative test, in conjunction with the rock core analyzed with rock core electron-microscope scanning instrument
The variation of microstructure, the variation for the residual acid ion concentration analyzed with ICP instrument, the rock core analyzed with X-ray (X-ray) diffractometer
Variation of surface mineral ingredient etc. to acid solution carry out assessment and preferably, with verify acid/rock reaction mechanism or assessment acid fluid system pair
The adaptability on stratum is further improved, optimization acid formula.
However, each rock core composition can not be completely the same, and the amount and time for flowing out sampling are difficult cross in these research methods
To comparing, experimental period and span are very long, can not every kind of system of quantitative assessment inhibition secondary precipitation ability, limit correlation
System preferably and exploitation.
For " SY/T 6571-2012 acidification with ferrous stability method of evaluating performance " that petroleum industry generallys use,
It is to observe by the naked eye solution whether muddiness qualitatively judges titration end-point, and naked eyes are difficult to handle when titration end-point solution is micro- muddy
It holds, there is biggish experimental error, in addition, this method only proposes measurement complexing agent to the method for iron ion complexing power, application
Secondary precipitation complexing agent performance evaluation still has certain limitation during sandstone acidizing, also not it is proposed that measuring under high temperature
The method of complexing agent complexing power.Experimental implementation process is also complex, only single reaction system, cause conventional efficient compared with
It is low, inconvenience preferably is brought with evaluation to the quantitative of secondary precipitation during sandstone acidizing.
Utility model content
In order to overcome the above-mentioned deficiencies of the prior art, the utility model provides a kind of measurement complexing agent to metal ion network
The experimental provision of conjunction ability more can fast and accurately obtain experimental result.
The technical scheme adopted by the utility model is one kind is in Oil Field sandstone acidizing for quickly measuring acid solution
Experimental provision of the system to the rejection ability of secondary precipitation, wherein the experimental provision includes: thermostat, multiple closed reactions
Container and the one-to-one blender of the closed reaction vessel and the one-to-one temperature of closed reaction vessel
Meter, the pipette for quantitatively pipetting liquid and the iron stand for experimental provision to be fixed；Wherein, described closed
Reaction vessel is made of resistant material, is fixed by iron stand, and immerses in thermostat；The stirring magneton and thermometer
It is respectively placed in reaction vessel.
Preferably, the experimental provision further includes spectrophotometer.
Preferably, the experimental provision includes 2-6 closed reaction vessels.
Preferably, the thermostat has the function of heating and magnetic agitation simultaneously, can be stirred while heating,
So that rapid reaction carries out, experimental result is more accurate.Temperature and revolving speed can be adjusted by operator, to meet difference
The requirement of experiment condition.
Preferably, each of described closed reaction vessel is designed with test tube clamp for fixing, convenient for operator and
When take out reaction vessel, observation experiment phenomenon.
Preferably, each of described closed reaction vessel is designed with the thermometer for measuring reacting liquid temperature, can be quasi-
The really temperature change in record experimentation, while the thermometer is able to satisfy the requirement of high temperature experiment condition.
Preferably, the pipette energy accurate quantitative analysis pipettes solution into reaction vessel, is used to quantitative assessment complexing agent
Complex performance.
Preferably, the stirring magneton for being stirred to react solution, institute are placed in each of described closed reaction vessel
The stirring magneton stated is stirred reaction solution using the magnetic interaction with thermostat, makes close to reaction container bottom
It must react more uniform.
Compared with prior art, the utility model has the advantage that
(1) the utility model has been put forward for the first time the complexing power that complexing agent is quickly measured under a kind of high temperature to metal ion
Experimental provision.
(2) can be used for simulated formation temperature to evaluate acid fluid system to complexing of metal ion ability, cover acid solution compared with
For complete application range.0~110 DEG C of temperature measuring range.
(3) it can be tested simultaneously in multiple reaction vessels, such as multiple groups parallel laboratory test can be carried out simultaneously, to mention
High conventional efficient saves experimental period.
(4) it is precipitated by using the absorbance of spectrophotometric determination reaction solution to determine whether generating, it can be more accurate
Judge whether precipitating generates, improve the reliability of experiment, be successfully applied to secondary precipitation inhibitor during sandstone acidizing
It is preferred that with evaluation.
Detailed description of the invention
Attached drawing described here is only used for task of explanation, and model disclosed by the utility model is limited without in any way
It encloses.In addition, shape and proportional sizes of each component in figure etc. are only schematically, to be used to help the reason to the utility model
Solution is not the specific shape and proportional sizes for limiting each component of the utility model.Those skilled in the art is practical new at this
Under the guidance of type, various possible shapes and proportional sizes can be selected to implement the utility model as the case may be.
Fig. 1 shows one group of combination feelings of the experimental provision that complexing agent is quickly measured under high temperature to complexing of metal ion ability
Condition, the present apparatus can have the such combination of multiple groups.
The figures above label: 1, thermostat；2, the first closed reaction vessel；3, the second closed reaction vessel；4,
One stirring magneton；5, the second stirring magneton；6, the first test tube clamp；7, the second test tube clamp；8, the first thermometer；9, second temperature
Meter；10, the first pipette；11, the second pipette；12, iron stand.
Fig. 2 is the specific implementation step flow chart of the utility model implementation process.
Complexing power of the different acid fluid systems to metal ion under Fig. 3 hot conditions.
Fig. 4 is to be added to the construction curve figure of the complex acid of 3% complexing agent 6 at the scene.
Specific embodiment
In conjunction with the description of attached drawing and specific embodiment of the present invention, the utility model can be clearly understood
Details.But specific embodiment of the present utility model described herein, it is only used for explaining the purpose of this utility model, without
It can understand in any way or limitations of the present invention.Under the guidance of the utility model, technical staff is contemplated that
Any possible deformation based on the utility model, these are regarded as belonging to the scope of the utility model.
What is introduced first is sandstone acidizing mechanism and basic acid-rock reaction.
(1) the initial primary first-order equation of soil acid acidizing
The acid solution used in sandstone acidizing at present is mainly mud acid, it is recognized that regular mud acid acidification mainly have following three bases
This reaction:
2HCl+CaCO3→CaCl2+CO2↑+H2O (1)
6HF+SiO2→H2SiF6+2H2O (2)
(6+x)HF+M-Al-Si-O+(4-x)H+→H2SiF6+AlFx (3-x)++M++H2O (3)
In primary first-order equation, the carbonate rocks such as Hydrochloric Acid Etching calcite, hydrofluoric acid corrosion quartz and clay.The reaction is oil
The purpose reaction of field acidification, reaches dissolution Reservoir Minerals, realizes the purpose for releasing blocking or injury.
(2) the secondary precipitation reaction under the conditions of residual acid
With the progress of acidification, almost all of hydrochloric acid has reacted, and acid solution pH value is 2~3, and the zwitterion in solution will
Generate following precipitating:
Ca2++2F-→CaF2↓ (4)
SiF6 2-+2K+→K2SiF6↓ (5)
AlF6 3-+3Na+→Na3AlF6↓ (6)
Fe3-+3OH-→Fe(OH)3↓ (7)
Above-mentioned only to list representative precipitation reaction, actually fluorine ion and bivalent metal ion can produce white
Fine powder fluoride precipitates (calcirm-fluoride, magnesium fluoride), and sodium, potassium, calcium and barium salt of fluosilicic acid and fluoaluminic acid etc. are also that white is heavy
It forms sediment.In acidization, after acid solution enters stratum by pipeline, can corrosion pipeline, dissolve the chlorite and green in formation rock
Mixed layer is covered, a large amount of iron ion is released, these ferric hydroxide receiving electrodes are also easy to produce, and are sent out in pH > 2.2
It is raw, it is often green or brownish red floccule.
(3) precipitation reaction three times under the conditions of residual acid:
With reaction further deeply, product fluoaluminate continues to react with clay etc., generates fluorine aluminium coordination valence object
AlF2+And silicic acid Si (OH)4With metasilicic acid H2SiO3Precipitating, further polycondensation is silica gel to silicic acid etc., can not be ejected by returning.
AlF2 ++M-Al-Si-O+2H++H2O→2AlF2++M++Si(OH)4↓ (8)
The production of silica gel is the long response time of a Step Condensation, if can be in secondary response, stable fluoaluminic acid well
Salt then can inhibit the generation of third-order reaction.Therefore, the inhibition of secondary precipitate is particularly important.
According to the above mechanism, we can choose these four mineral of calcirm-fluoride, potassium fluosilicate, cryolite and iron hydroxide
As primary standard substance, the dosage of metal ion when its precipitating occurs is measured, under the same conditions, the dosage of metal ion is more, and four
Kind mineral precipitation is less susceptible to generate, and the secondary precipitation rejection ability of the acid fluid system is better.
The present invention will be further described with reference to the accompanying drawing.
Referring to Fig.1 shown in, quickly measure complexing agent include: thermostat 1 to the experimental provision of complexing of metal ion ability, it is more
A closed reaction vessel 2 and 3, with the closed reaction vessel stir correspondingly magneton 4 and 5, with it is described closed
The one-to-one test tube clamp 6 and 7 of reaction vessel and the one-to-one thermometer 8 and 9 of the closed reaction vessel are used to determine
Measure pipette 10 and 11, the iron stand 12 for experimental provision to be fixed for pipetting liquid.
Specifically, thermostat 1 is used to carry out reaction solution heating and stirring action, meets high temperature experiment condition, make simultaneously
It must react more abundant, improve the accuracy and reliability of experiment.
Closed reaction vessel 2,3 is the cylindrical container of polytetrafluoroethylene (PTFE) material, there is thread seal at an upper portion thereof
Cap carries out it closed.It should be multiple, and preferably 2-6.Closed reaction vessel 2,3 is dipped into thermostat 1, and is led to
Cross the fixation of iron stand 12 that the side of thermostat is set.It is able to achieve acid solution and is isolated from the outside, and reduces acid solution and was heating up
Because losing caused by volatilization in journey, the experimental provision in the utility model can carry out multiple groups experiment simultaneously.It can not only accelerate reality
Test efficiency, moreover it is possible to while multiple groups parallel laboratory test is carried out, to improve the accuracy of experiment.
The bottom of reaction vessel 2,3 is respectively placed in for the magneton 4,5 of magnetic agitation, the band after thermostat 1 generates magnetic field
Dynamic magneton 4,5 does circumferential cycle movement, to achieve the purpose that be stirred to react liquid.
The clamping end of test tube clamp 6 and 7 clamps reaction vessel 2,3, and the other end is fixed on thermostat 1, the position point of clamping
Not under the sealing screw thread of closed reaction vessel 2,3 at 2-3cm, in order to which operator takes out reaction vessel in time, observation
Experimental phenomena.
Thermometer 8,9 is inserted in reaction solution, and is fixed among the seal cap of reaction vessel 2,3.Its energy Accurate Determining is anti-
The temperature for answering liquid reflects the temperature condition of this experiment, to improve the accuracy and reliability of experimental result.
The setting of pipette 10,11 is square on the reaction vessel, is fixed on iron stand by cross clamp.It can accurately be pipetted
A certain amount of standard ionomer salting liquid meets the requirement of quantitative assessment experiment, also further improves the reliability of experiment.
Spectrophotometer is separately provided relative to experimental provision.Spectrophotometric determination absorbance is used in the utility model
Variation rather than visually observe to judge whether generate precipitating in reaction solution, whether precipitating is generated with accurate judgement, increases reality
The reliability tested.
In the present embodiment, reaction vessel is made of polytetrafluoroethylene material, and to realize corrosion-resistant effect, this is practical new
The test temperature of type can achieve 110 DEG C or so, be able to satisfy high temperature requirement of experiment.It is secondary for current oil field sandstone acidization
For the evaluation of precipitating inhibitor is preferred, above-mentioned experimental provision and method cover more complete application range.
Compared with prior art, the utility model has the advantage that
(1) the utility model has very strong wide spectrum applicability.Difference is complexed at a temperature of being used to measure Different Strata
Complexing power of the agent to different metal ions.
(2) it can be tested simultaneously in multiple reaction vessels, improve conventional efficient, save experimental period.
(3) the utility model has been put forward for the first time the complexing power that complexing agent is quickly measured under a kind of high temperature to metal ion
Experimental provision and method.
(4) it is precipitated by using the absorbance of spectrophotometric determination reaction solution to determine whether generating, it can be more accurate
Judge whether precipitating generates, improve the reliability of experiment, be successfully applied to secondary precipitation inhibitor during sandstone acidizing
It is preferred that with evaluation.
(5) use " closed " reaction vessel for the first time, this be under measurement high temperature complexing agent to the complexing power of metal ion
Provide enforceable condition.Reaction vessel is made of polytetrafluoroethylene material, and stirring uses magnetic agitation mode, heat-conducting medium
For silicone oil.
Using above-mentioned experimental provision, measurement of the acid fluid system to the rejection ability of secondary precipitation is carried out using following methods:
(1) the certain density acid fluid system equipped with complexing agent is prepared；
(2) prepared acid fluid system in a certain amount of step (1) is added into closed reaction vessel, and stirring magnetic is added
Son；
(3) acid fluid system in closed reaction vessel is carried out by thermostat being heated to preset temperature；
(4) a certain amount of standard ionomer salting liquid (such as CaCl is measured with pipette2Solution, AlCl3Solution, FeCl3Solution,
(NH4)2SiF6Solution), it is added into closed reaction vessel, under the stirring action of magneton, so that reactant sufficiently reacts.
(5) using the variation of spectrophotometer comparison reaction front and back solution absorbance to determine whether generating precipitating.Pass through
The endpoint quantification that precipitating generates judges the acid fluid system to the complexing power of metal ion.
(6) change condition of different temperatures, repeat above-mentioned experimental procedure, measure under condition of different temperatures complexing agent to metal from
The complexing power of son, so that complexing agent is carried out preferably and be evaluated.
The complexing agent is as follows to the endpoint method of complexing of metal ion ability:
1) acid fluid system that 5ml is furnished with complexing agent is quantitatively measured with pipette；
2) three groups of parallel laboratory tests are carried out, the standard ionomer salting liquid V of the 1mol/L of standard is separately added into1Ml (such as CaCl2It is molten
Liquid, AlCl3Solution, FeCl3Solution, (NH4)2SiF6Solution), 10V1ml、100V1ml；
3) with the Na of saturation2CO3Solution/saturation K2CO3Solution adjusts the pH value of acid solution, is slowly added to pH value of solution
=7, the range that observation precipitating generates；
Theorem is forced according to folder, the intermediate value of standard ionomer salting liquid volume is added when precipitating being taken to generate, until V2To produce just
The volume number of standard ionomer salting liquid is added when raw precipitating, the specific judgment method of titration end-point is as follows.
A) as addition V1When the standard ionomer salting liquid of volume generate precipitating, that is, illustrate the complexing agent to the metal ion without
Apparent complexing power, can also be in 0~V1Between take intermediate value V2=V1/ 2, repeat above-mentioned experimental procedure 2), 3), until V is added2
Precipitating is generated just when the standard ionomer salting liquid of volume.
B) as addition 10V1Precipitating is generated when the standard ionomer salting liquid of volume, in V1~10V1Between take intermediate value V2=
11V1/ 2, repeat above-mentioned experimental procedure 2), 3), until V is added2Precipitating is generated just when the standard ionomer salting liquid of volume.
C) as addition 100V1Precipitating is generated when the standard ionomer salting liquid of volume, in 10V1~100V1Between take intermediate value V2
=110V1/ 2, repeat above-mentioned experimental procedure 2), 3), until V is added2Precipitating is generated just when the standard ionomer salting liquid of volume.
Because indoor discovery grind select the content of HCl in system number the performance of complexing agent complexation of metal ions will not be made
At influence, and the generation of fluoride secondary precipitation during the more identical live sandstone acidizing of 3%HF is added, therefore chooses certain oil
Field scene sandstone acidizing system and corresponding complexing agent measure sandstone acidizing complexing acid fluid system indoors and exist under laboratory condition
(90 DEG C of conditions) is to metal ion (Ca under high temperature2+、Al3+、Fe3+、K+) complexing power, to evaluate different complexing agents to difference
The complexing power of metal ion, further preferably complexing acid fluid system.It is walked using mentioned-above experimental provision and measuring method
Suddenly it is tested, experimental result is shown in Table shown in 1.
To complexing of metal ion merit rating under the different acid fluid systems of table 1.
| Acid fluid system | Calcium ion (ml) | Aluminium ion (ml) | Iron ion (ml) | Potassium ion (ml) |
| Complexing agent 1+3%HF | 0.1 | 0.1 | 0.1 | 3 |
| Complexing agent 2+3%HF | 0.1 | 0.1 | 0.1 | 2 |
| Complexing agent 3+3%HF | 0.1 | 0.1 | 0.1 | 0.5 |
| Complexing agent 4+3%HF | 4 | 0.5 | 0.5 | 1.5 |
| Complexing agent 5+3%HF | 0.1 | 0.1 | 0.1 | 2 |
| Complexing agent 6+3%HF | 5 | 0.5 | 1 | 3.5 |
For the ease of analyzing experimental result, the above experiment is made into histogram as shown in Figure 3 and is analyzed, by tables of data
With histogram it can be seen that under the high temperature conditions, complexing agent 6 is best to the complexing power of four metal ion species.Therefore, it can push away
The scene of recommending uses complexing agent 6 complexing acid systems.
It is acidified in the oil field using the complexing acid system for being added to 3% complexing agent 6, uses front in construction cup
The invention experimental provision is tested with measuring method step, is measured it and is reached 75% to the inhibiting rate of secondary precipitation, applies
The well restores water filling, injection rate 3.7m after work3/ H, injection pressure 0.17MPa, stratum injectivity index is than increasing 11 before acidification
Times, site operation figure is referring to fig. 4.
All the embodiments in this specification are described in a progressive manner, the highlights of each of the examples are with
The difference of other embodiments, the same or similar parts between the embodiments can be referred to each other.
The above embodiments are only for explaining the technical ideas and features of the present invention, and its object is to allow those skilled in the art
Member can understand the content of the utility model and implement accordingly, not limit the protection scope of the present invention.All
According to equivalent change or modification made by the spirit of the present invention essence, should be covered within the scope of the utility model.
Claims (9)
1. a kind of for measuring acid fluid system to the experimental provision of the rejection ability of secondary precipitation, wherein the experimental provision is in oil
It is used in the sandstone acidizing of field scene；Wherein the experimental provision include: thermostat, multiple closed reaction vessels, with it is described close
The one-to-one blender of the reaction vessel closed, with the one-to-one thermometer of the closed reaction vessel, for quantitatively moving
Take the pipette of liquid and the iron stand for experimental provision to be fixed；And wherein the closed reaction vessel by
Resistant material is made.
2. experimental provision according to claim 1, wherein the closed reaction vessel is fixed by the iron stand, institute
Pipette is stated to be fixed on the iron stand by cross clamp.
3. experimental provision according to claim 1, wherein the experimental provision further includes spectrophotometer.
4. experimental provision according to any one of claim 1-3, wherein each closed reaction vessel is designed with test tube
The clamping end of folder, the test tube clamp clamps the reaction vessel, and the other end is fixed on the thermostat.
5. experimental provision according to any one of claim 1-3, wherein the closed reaction vessel is by it
The thread seal cap in portion is closed, and the thermometer is fixed in the thread seal cap of the closed reaction vessel
Between.
6. experimental provision according to any one of claim 1-3, wherein the experimental provision includes 2-6 described closed
Reaction vessel.
7. experimental provision according to any one of claim 1-3, wherein the thermostat is equipped with magnetic stirring apparatus.
8. experimental provision according to any one of claim 1-3, wherein being corresponded with the closed reaction vessel
Blender be magnetic stirring apparatus.
9. experimental provision according to any one of claim 1-3, wherein the thermostat is able to maintain that up to 110 is Celsius
The temperature of degree.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109374818A (en) * | 2018-10-29 | 2019-02-22 | 中国海洋石油集团有限公司 | Quickly device and method of the measurement complexing agent to complexing of metal ion ability |
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2018
- 2018-10-29 CN CN201821759995.XU patent/CN209356413U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109374818A (en) * | 2018-10-29 | 2019-02-22 | 中国海洋石油集团有限公司 | Quickly device and method of the measurement complexing agent to complexing of metal ion ability |
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