CN103146370A - Scale inhibitor for presetting in oil reservoir - Google Patents
Scale inhibitor for presetting in oil reservoir Download PDFInfo
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- CN103146370A CN103146370A CN2013100604967A CN201310060496A CN103146370A CN 103146370 A CN103146370 A CN 103146370A CN 2013100604967 A CN2013100604967 A CN 2013100604967A CN 201310060496 A CN201310060496 A CN 201310060496A CN 103146370 A CN103146370 A CN 103146370A
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- trimethylene phosphonic
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Abstract
The invention discloses a scale inhibitor for presetting in an oil reservoir. The scale inhibitor for the presetting in the oil reservoir is nitroxotrimethylene triphosphonic acid and is a cationic scale inhibitor. By adopting the scale inhibitor, the problem of operation cost is taken into consideration, use amount of the scale inhibitor does not exceed 10% generally, the minimal effective concentration is lower than 20mg/L generally, production cost is low, and in addition subsequent treatment measures are not needed. The scale inhibitor disclosed by the invention focuses on environmental-friendliness, is nontoxic, can be recycled through refilling after wastewater treatment, and does not pollute environment. In combination with an oil reservoir presetting scale control technology, the scale inhibitor disclosed by the invention is simple in operation process; by presetting the scale inhibitor at stratum once, the scale inhibitor can be automatically and continuously released and is effective for long time; and the scale inhibitor not only can be used for preventing scaling on wellbore and scaling on ground pipeline, but also can be used for preventing scale inside near wellbore stratum.
Description
Technical field
The present invention relates to a kind ofly have preferably the oil reservoir of antiscaling effect and absorption-desorption performance preset and use scale inhibitor in oil reservoir.
Background technology
At mid-late oilfield development, along with the generally application of various raising recovery efficiency techniques, stratum and extraction scaling problem become increasingly conspicuous.Stratum and extraction scaling often cause oil reservoir injury, well wellbore and ground pipe laying choked flow, and the problems such as structure deteriorate cause the production fluid amount to descend, and have had a strong impact on the normal production in oil field.
Comprehensive antiscaling method both at home and abroad, mainly comprise: (1) chemical process antiscale has 2 kinds for the treatment of processs: acid adding or injection CO
2Prevent alkaline scale, with scale inhibitor; (2) physical method antiscale prevents the formation of dirt by physical means, comprise 5 kinds of methods: avoid inconsistent water to mix, keep pressure and prevent calcium carbonate scaling, the plastic paint antiscale, " sound field " and " electromagnetic field " antiscale reduces incrustation ion concentration in oil-field water.The use limitation that wherein adds chemical scale inhibition agent antiscaling method is minimum, and its antiscaling effect is obvious, cost is lower, is generally used by domestic and international oil field.
Scale inhibitor has in the using method in oil field: (1) for surface gathering system, can stand metering (turning oil), each well terminal manifold place adds scale inhibitor; (2) oil well pump and tail pipe fouling can or be lowered to solid scale inhibitor in the well head medicine-adding agent; (3) stratum, immediate vicinity of wellbore, down-hole fouling can adopt oil reservoir to preset scale inhibitor technology squeezing high density scale inhibitor.Wherein, inject continuously scale inhibitor, to having relatively high expectations of pump, and complicated operation, take more human and material resources; Throw in solid scale inhibitor, the dissolution rate of solid scale inhibitor is wayward; Oil reservoir presets the scale inhibitor technology and compares with aforesaid method, and have Automatic continuous and discharge, can realize by the nearly well band of recovery well → comprehensive antiscale of production pit shaft → surface pipeline and the advantage such as operating process is simple, be a preventing fouling with the potentiality that develop on a large scale very much.
The ultimate principle that oil reservoir presets the scale inhibitor technology is that scale inhibitor is got into around pit shaft in the stratum, and scale inhibitor can be stranded in porous medium by physical adsorption or precipitation, slowly is released in output water by desorb after opening well and making production, reaches the purpose of long lasting scale prevention.
At present, the research and development overwhelming majority of scale inhibitor concentrates on and improves on anti-scaling property and synthetic multi-functional scale inhibitor both at home and abroad, the rarely seen research that has the scale inhibitor of antiscale and adsorption-desorption performance in the stratum concurrently.
Summary of the invention
The purpose of this invention is to provide a kind of oil reservoir that had not only had anti-scaling property preferably but also had an adsorption-desorption performance and preset and use scale inhibitor, this agent can have adsorption-desorption performance and antiscaling effect preferably at high-temperature stratum.
The objective of the invention is to be achieved through the following technical solutions:
A kind of oil reservoir presets uses scale inhibitor, it is nitrogen oxygen base trimethylene phosphonic that described oil reservoir presets with scale inhibitor, its synthesis condition is: in water bath with thermostatic control, the Amino Trimethylene Phosphonic Acid crystal is joined in reaction vessel, add distilled water, then regulating pH with the NaOH solution of massfraction 40% is 9 again; Slowly drip H after being cooled to room temperature
2O
2Stir Amino Trimethylene Phosphonic Acid: H
2O
2=1:2.5(mol ratio); Dropwise rear intensification, temperature of reaction is 60 ℃, and reaction 3h namely gets nitrogen oxygen base trimethylene phosphonic solution; Product is poured into while hot in the ethanol solution of preheating, standing after stirring, white crystal appears in the cooling rear bottom of solution, obtains nitrogen oxygen base trimethylene phosphonic crystal after suction filtration.
This scale inhibitor is cationic scale inhibitor.This scale inhibitor has three methylene phosphonic acid groups and a nitrogen oxygen groups, in the process of antiscale, methylene phosphonic acid group in molecular structure both can form inner complex with the fouling positively charged ion and reduce the cationic content of fouling in fluid, and the Sauerstoffatom in this group can be adsorbed on again and stops growing up of dirt on calcium carbonate crystal surface growth active site; And the nitrogen oxygen groups gives the scale inhibitor molecule weak positive polarity, can be electronegative formation material associative list and reveal the scale inhibitor adsorptivity good on the stratum.Because this scale inhibitor contains adsorption group and antiscale group simultaneously, so this agent can realize the function of in stratum Long-Term Sorption desorb and antiscale simultaneously, has long-lasting.
Main points of the present invention are to have reduced fouling cations in fluid adding of scale inhibitor, and occupy the accumulation of growing up that the brilliant surperficial active site of dirt stops the carbonic acid dirt; The scale inhibitor molecule is positive polarity, realizes adsorption-desorption effect preferably with reservoir formation.
The present invention considers the problem of operating cost, and this scale inhibitor consumption generally is no more than 10%, and minimal effective concentration is generally lower than 20mg/L, and production cost is low, and need not follow-up treatment measures.
The present invention pays attention to environmental protection, and scale inhibitor is nontoxic, and can realize recycling by re-injection after sewage disposal, and is free from environmental pollution.
The present invention presets preventing fouling in conjunction with oil reservoir, and to have an operating process simple, and preset once on the scale inhibitor stratum, and scale inhibitor can discharge by Automatic continuous, and is permanently effective; Except anti-pit shaft and surface pipeline fouling, also can prevent the dirt in stratum around the well.
Description of drawings
Fig. 1 is nitrogen oxygen base trimethylene phosphonic infrared spectrum;
Fig. 2 is the relation curve of scale inhibitor concentration and fouling time;
Fig. 3 is that the scale inhibitor static adsorbance is with the change in concentration relation curve;
Fig. 4 is the relation curve that scale inhibitor returns row's concentration and output volume;
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
1.1 nitrogen oxygen base trimethylene phosphonic is synthetic
In water bath with thermostatic control, Amino Trimethylene Phosphonic Acid (ATMP) crystal is joined in there-necked flask, then add distilled water, then use the NaOH regulator solution pH of massfraction 40%; Slowly drip H after being cooled to room temperature
2O
2Stir; Dropwise rear intensification, the reaction certain hour namely gets nitrogen oxygen base trimethylene phosphonic solution; Product is poured into while hot in the ethanol solution of preheating, standing after stirring, white crystal appears in the cooling rear bottom of solution, obtains nitrogen oxygen base trimethylene phosphonic crystal after suction filtration.
1.2 the synthesis condition discussion of nitrogen oxygen base trimethylene phosphonic
Investigate the impact (during static antiscaling rate experiment directly use product liquid state under, its test concentrations be 20mg/L) of each factor on static antiscaling rate in building-up process, determine at last optimum synthesis condition.
1. the impact of pH value on the static antiscaling rate of product
60 ℃ of temperature of reaction, reactant ratio are Amino Trimethylene Phosphonic Acid: H
2O
2=1:2(mol ratio), reaction times 2.5h investigates with the static antiscaling rate under the different pH values of 40%NaOH adjusting.Experimental result sees Table 1.
The relation of table 1pH value and static antiscaling rate
| pH | 8 | 9 | 10 |
| Static antiscaling rate (%) | 71.25 | 84.04 | 63.22 |
Experimental result shows, the pH value of solution affects the antiscaling effect of product, and the antiscaling effect of product is best when pH=9.This may be to be that under 9 condition, reactive behavior is maximum at pH due to ATMP, easily and H
2O
2Reaction, synthetic product.
2. the impact of reaction times on the static antiscaling rate of product
60 ℃ of temperature of reaction, reactant ratio are Amino Trimethylene Phosphonic Acid: H
2O
2=1:2, pH=9 investigates the static antiscaling rate under the different lower reaction times.Experimental result sees Table 2.
The relation of table 2 reaction times and static antiscaling rate
| Reaction times (h) | 2 | 2.5 | 3 | 3.5 |
| Static antiscaling rate (%) | 73.53 | 84.04 | 86.72 | 80.25 |
As shown in Table 2, when the reaction times is 3h, antiscaling effect is better, and static antiscaling rate reaches 86.72%.When the time was less than 3h, the reaction times was inadequate, and raw-material transforming degree is low, and synthetic active substance content is not high, so static antiscaling rate is not high; During more than 3h, the synthetic active variation of active substance part produces impurity when the reaction times, so antiscaling effect reduces.
3. the impact of temperature of reaction on the static antiscaling rate of product
Reactant ratio is Amino Trimethylene Phosphonic Acid: H
2O
2=1:2, pH=9, the reaction times is 3h, investigates the static antiscaling rate under different lower temperature of reaction.Experimental result sees Table 3.
The relation of table 3 differential responses temperature and static antiscaling rate
| Temperature of reaction (℃) | 55 | 60 | 65 | 70 |
| Static antiscaling rate (%) | 74.21 | 86.72 | 81.06 | 68.14 |
By experiment as can be known, temperature of reaction is too high and too lowly all the antiscaling effect of product is had a negative impact.Temperature is low, and speed of response is slow, and therefore the active substance content of its generation is low when termination reaction; Excess Temperature destroys the active substance structure that has generated, and causes activity decreased, the antiscaling effect variation.
4. the impact of material proportion on the static antiscaling rate of product
In the situation that above-mentioned condition is constant, adjust ATMP and H
2O
2Proportioning, to obtain to have the product of better antiscaling effect.Experimental result sees Table 4.
The relation of table 4 different material proportioning and static antiscaling rate
As shown in Table 4, work as Amino Trimethylene Phosphonic Acid: H
2O
2During=1:2.5, antiscaling effect is best, and static antiscaling rate has reached 90.27%.
Consider above factor, determine that the optimum synthesis condition of nitrogen oxygen base trimethylene phosphonic is as follows: temperature of reaction is 60 ℃, and the pH value is 9, Amino Trimethylene Phosphonic Acid: H
2O
2=1:2.5, the reaction times is 3h.The antiscaling effect of synthetic scale inhibitor is best with this understanding, and static antiscaling rate can reach 90.27%(20mg/L).
The structural characterization of embodiment 2 nitrogen oxygen base trimethylene phosphonics
Nitrogen oxygen base trimethylene phosphonic crystal after purifying is carried out Infrared spectroscopy, and its infrared spectra spectrogram is seen Fig. 1.On spectrogram, each peak may belong to and sees Table 5.
The ownership of the main absorption peak of table 5 nitrogen oxygen base trimethylene phosphonic infrared spectra
| Absorption peak position (wave number/cm -1） | The ownership of absorption peak |
| 951，1060 | Phosphonyl group (PO 3H 2) absorption peak |
| 1220 | The C-N vibration peak |
| 1440 | The N-O absorption peak |
| 2870，2950 | -CH 2-stretching vibration peak |
As can be seen from Figure 1,951,1060cm
-1Appearance-the PO of place
3H
2Absorption peak; 1220cm
-1The C-N vibration peak appears in the place; 1440cm
-1The N-O absorption peak appears in the place; 2870,2950cm
-1Appearance-the CH of place
2-absorption peak.Therefore can determine that synthetic effect is better, product is target product nitrogen oxygen base trimethylene phosphonic.Can judge that its product structure formula is formula (3-4).
The performance evaluation of embodiment 3 synthetic products
Amino Trimethylene Phosphonic Acid (being designated as substance A) and nitrogen oxygen base trimethylene phosphonic (being designated as substance B) all carry out following experimental study with pressed powder state after its purification suction filtration.
3.1 the results and analysis of compatibleness experiment
The compatibleness experimental result of substance A and B and battalion's 11 blocks (an oil recovery block of Dongxing oil fields in Shengli, formation temperature is 127 ℃) local water sees Table 6.
The compatibleness experimental result of table 6A and B and local water
Experimental result shows, after modification, substance B can be realized in wider concentration range and local water consistency preferably.
3.2 the results and analysis of static antiscaling rate experiment
Substance A and B(experimental concentration are 20mg/L) static antiscaling rate experimental result see Table 7.
The static antiscaling rate experimental result of table 7
| Medicine | A | B |
| Static antiscaling rate (%) | 90.24 | 95.32 |
By experimental result as can be known, substance A and B its static antiscaling rate after purification is apparently higher than its solution form, and after modification, the static antiscaling rate of substance B is higher than substance A, and antiscaling effect increases compared with before-improvement.
3.3 the results and analysis of dynamic minimum effective antiscale concentration (MIC) experiment
Dynamically minimal effective concentration (MIC) experimental result as shown in Figure 2.
As shown in Figure 2, the blank fouling time is 57 minutes, and the fouling time of substance A and B increases along with the increase of its concentration.Wherein, when minimum effective working concentration of substance A was 20mg/L, the fouling time reached 193 minutes; When minimum effective working concentration of substance B was 15mg/L, the fouling time reached 191 minutes.This shows, its anti-scaling property of the substance B after improvement is better than substance A.
3.4 scale inhibitor Staticadsorption experiment results and analysis
Measure substance A and the static adsorbance of B under different concns.Experiment is all adopted battalion's 11 block operating modes with oil-sand, experimental temperature and experimental water.Its Staticadsorption experiment results is seen Fig. 3.
As shown in Figure 3, the static adsorbance of scale inhibitor A and B rises along with the increase of scale inhibitor concentration, and adsorptive capacity is substantially constant after arriving finite concentration, reaches adsorption equilibrium; The equilibrium adsorption concentration of substance A and B is 10
5Mg/L; Under the same conditions the substance B after modification in the adsorptive capacity of sandstone surface greater than substance A.Its adsorption mechanism can be analyzed by the dissociation equilibrium that reaches the quartz sand surface existence in substance A and B nature.
Quartz sand part in the aqueous solution exists to generate the silanol form, and this material exists dissociation equilibrium suc as formula (3-5) in water.When silanol dissociates H
+After, quartz sand surface is electronegativity.Greater than 2 the time, along with moving to right of dissociation equilibrium, surface negative charge increases when the pH value, but when the pH value less than 6 the time, its surface negative charge is still relatively low
[51]And substance A is phosphonic acids type scale inhibitor, and such scale inhibitor can be adsorbed onto rock surface by Van der Waals force when the pH value is low, simultaneously, and phosphonyl group [PO (HO)
2] on hydrogen atom and electronegative property rock formation hydrogen bond and being adsorbed on rock; Along with the pH value raises gradually, scale inhibitor A molecule dissociates, and the dissociation equilibrium of existence is suc as formula advancing to the right shown in (3-6), and quartz sand surface negative charge and scale inhibitor liberation degree all increase, and the scale inhibitor that is molecularity reduces, [SI.H
Num-m]
m-With the also corresponding enhancing of repulsion of quartz sand surface, so the ability that A is adsorbed on quartz sand surface reduces, and the scale inhibitor adsorptive capacity is reduced.Substance B has stronger and sandstone adsorption, and this may be relevant with its molecular structure (seeing formula (3-4)), this material due to adding of Sauerstoffatom whole molecule be positive polarity, therefore can with the chemical bond form a large amount of and SiO
-In conjunction with, therefore having stronger adsorptive power, adsorptive capacity is larger.
SiO-H+H
2O→SiO
-+H
3O
+ （3-5）
SI.H
num+mH
2O→[SI.H
num-m]
m-+mH
3O
+ （3-6）
3.5 absorption-desorption experimental result and analysis
The concentration of being worked as can be known substance A and B by 3.4 experimental results is 10
5Can realize its maximal absorptive capacity during mg/L, so the experimental concentration of absorption-desorption experiment adopts 10
5Mg/L, its result such as Fig. 4.
Experimental data by Fig. 4 can be found out, the row's of returning Similar Broken Line of two kinds of scale inhibitors, and the initial stage density loss is very fast in the row of returning, and with the increase of output volume, change in concentration tends to be steady.Wherein the row of returning early stage, the row's of returning concentration of substance A is higher than substance B, and this is because substance B more is trapped in rock core because being adsorbed on sandstone; In the row's of returning later stage, the row's of returning density loss of substance A is very fast, and it is long-pending during for 370PV that it effectively returns isostere, substance B return isostere long-pending during for 425PV concentration remain on the 20mg/L left and right, this value is still higher than the minimal effective concentration (15mg/L) of this scale inhibitor.Therefore, substance B has absorption-desorption performance preferably than A as shown in this experiment, can be detained for a long time in rock core, obtains long work-ing life.
3.6 brief summary
Obtain Nitrogen in Products oxygen base trimethylene phosphonic after existing scale inhibitor ATMP is improved, this material possesses following character (after purifying) compared with before-improvement:
(1) ATMP is 10 at working concentration
5During mg/L, the crystal deposition phenomenon appears in the time of between standing 36 ~ 48h; And nitrogen oxygen base trimethylene phosphonic still shows in wider working concentration scope and seek 11 block local waters consistency preferably, and solution is limpid.
(2) the static antiscaling rate of nitrogen oxygen base trimethylene phosphonic is higher than ATMP, and minimum effective working concentration is lower than ATMP, and this shows that the antiscaling effect after medicament improves is good compared with before-improvement.
(3) isostere of effectively returning of nitrogen oxygen base trimethylene phosphonic is amassed as 425PV improves than the 370PV of ATMP, and is more approaching with the effectively row of the returning volume cost of scale inhibitor SA1320.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improve and conversion all should belong to the protection domain of claims of the present invention.
Claims (1)
1. an oil reservoir presets and uses scale inhibitor, it is characterized in that, it is nitrogen oxygen base trimethylene phosphonic that described oil reservoir presets with scale inhibitor, its synthesis condition is: in water bath with thermostatic control, the Amino Trimethylene Phosphonic Acid crystal is joined in reaction vessel, add distilled water, then regulating pH with the NaOH solution of massfraction 40% is 9 again; Slowly drip H after being cooled to room temperature
2O
2Stir Amino Trimethylene Phosphonic Acid: H
2O
2=1:2.5(mol ratio); Dropwise rear intensification, temperature of reaction is 60 ℃, and reaction 3h namely gets nitrogen oxygen base trimethylene phosphonic solution; Product is poured into while hot in the ethanol solution of preheating, standing after stirring, white crystal appears in the cooling rear bottom of solution, obtains nitrogen oxygen base trimethylene phosphonic crystal after suction filtration.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200063260A (en) * | 2017-10-25 | 2020-06-04 | 세인트-고바인 세라믹스 앤드 플라스틱스, 인크. | Composition for the material removal process and its composition method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200063260A (en) * | 2017-10-25 | 2020-06-04 | 세인트-고바인 세라믹스 앤드 플라스틱스, 인크. | Composition for the material removal process and its composition method |
| KR102447589B1 (en) | 2017-10-25 | 2022-09-28 | 세인트-고바인 세라믹스 앤드 플라스틱스, 인크. | Composition for material removal process and method of composition thereof |
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Application publication date: 20130612 |