CN104592524A - Selective water-plugging agent for super-molecular oil well and preparation method thereof - Google Patents

Selective water-plugging agent for super-molecular oil well and preparation method thereof Download PDF

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CN104592524A
CN104592524A CN201410844248.6A CN201410844248A CN104592524A CN 104592524 A CN104592524 A CN 104592524A CN 201410844248 A CN201410844248 A CN 201410844248A CN 104592524 A CN104592524 A CN 104592524A
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water
core
reaction
oil
plugging
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CN104592524B (en
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麻金海
孔淑玲
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Qingdao University
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Qingdao University
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Abstract

The invention relates to a selective water-plugging agent for a super-molecular oil well and a preparation method thereof. According to the water-plugging agent, a super-molecular structure is produced by utilizing self-assembly of a self-side chain group in a hydrophilic stratum of the oil well, so that the aim of selective water plugging of oil-water is fulfilled. According to the water-plugging agent, the problem of poor selectivity of the water-plugging agent is solved, the water content of crude oil produced by the oil well can be greatly reduced, the crude oil extraction efficiency is improved, and the crude oil extraction cost is reduced.

Description

A kind of supramolecule selective water shutoff agent for oil wells and preparation method thereof
Technical field
The invention belongs to oilfield oil extraction additive field, particularly relate to selective water shutoff agent for oil wells and preparation method thereof.
Background technology
In recent years, the most oil field of China has entered the tail period stage, and composite water cut sharply rises, and most oil reservoir composite water cut is more than 90%, drastically influence the normal production in oil field, well water has become the serious problems that waterflooding oil field faces.For this reason, oil well will carry out water blockoff usually, and its water ratio is reduced.The essence of water blockoff changes water flow direction in the earth formation, can keep producing energy by water blockoff, improves the sweep efficiency injecting water or other oil-displacing agent, thus the recovery ratio of crude oil is improved.
Existing various oilwell water shutoff agent at present, such as polyacrylamide-lignin sulfonate selective water shutoff agent (Zhejiang University's calendar year 2001 Master's thesis), the compound plugging agent of xanthan gum-AMPS-wilkinite (petrochemical complex Journal of Chinese Universities, in December, 2011), magnetic polymer composite microspheres profile-controlling and plugging agent (Beijing University of Chemical Technology's Master's thesis in 2012), CN 103013480 A, CN 103773338 A etc., but this area still needs good, the effective plugging agent of selectivity.Plugging agent of the present invention is applicable to oil field, oil and water well water plugging and profile controlling, has the advantages such as intensity is good, high temperature resistant, water plugging effect is good.
Summary of the invention
The present invention designs and has prepared the self-assembled supermolecular polymkeric substance of a kind of side chain containing beta-cyclodextrin and phenyl ring.First the present invention has synthesized a kind of main chain containing atom N, is then connected on main chain by the side chain containing beta-cyclodextrin and phenyl ring by grafting respectively, has prepared the polymkeric substance that side chain contains beta-cyclodextrin and phenyl ring simultaneously.This polymkeric substance, after oil well water-wet formation internal adsorption, can generate supramolecule by the self-assembly of the beta-cyclodextrin of side chain and phenyl ring, thus reach the object of the spontaneous water blockoff of oil well selectivity, overcome the problem of plugging agent oil-water selectivity difference in the past.
Embodiment
Embodiment 1
(1) beta-cyclodextrin that 0.45mol refines is added in the reaction vessel with whipping appts, and add 5.0mol ethanol, after abundant mixing, constant temperature 0.5h, uniformly solution in 65 DEG C, in reaction vessel, slowly 0.4mol epoxy chloropropane is dripped with dropping funnel, drip and finish, reaction solution is warming up to 70 DEG C ~ 75 DEG C, reaction 3h, add 0.5mol 1-chloromethylbenzene after reaction terminates, fully mix;
(2) 0.2mol diethylenetriamine is added the reaction vessel with whipping appts, add 3.0mol ethanol, be warming up to 70 DEG C, slowly drip 0.2mol epoxy chloropropane with dropping funnel, drip and finish, 70 DEG C of reaction 3h;
(3) slowly drop in step (2) gained mixture by step (1) gained mixed solution dropping funnel, drip and finish, be warming up to 90 DEG C ~ 95 DEG C, reaction 4h, obtains product.The molecular-weight average that mass spectroscopy records product is about 24100, and its polymerization degree is 17.1.
Embodiment 2
(1) beta-cyclodextrin that 0.5mol refines is added in the reaction vessel with whipping appts, add 5.0mol ethanol, abundant mixing, constant temperature 0.5h, uniformly solution in 65 DEG C, in reaction vessel, slowly 0.5mol epoxy chloropropane is dripped with dropping funnel, drip and finish, reaction solution is warming up to 70 DEG C ~ 75 DEG C, reaction 3.0h, add 0.5mol1-chloromethylbenzene after reaction terminates, fully mix;
(2) 0.3mol diethylenetriamine is added in the reaction vessel with whipping appts, add 3.0mol ethanol, be warming up to 70 DEG C, slowly drip 0.3mol epoxy chloropropane with dropping funnel, drip and finish, 70 DEG C of reaction 3h;
(3) slowly drop in step (2) gained mixture by step (1) gained mixed solution dropping funnel, drip and finish, be warming up to 90 DEG C ~ 95 DEG C, reaction 4h, obtains product.Mass spectroscopy records product molecular-weight average and is about 23060, and its polymerization degree is 16.4.
Embodiment 3
(1) beta-cyclodextrin that 0.55mol refines is added in the reaction vessel with whipping appts, add 5.0mol ethanol, fully mix, constant temperature 0.5h, uniformly solution in 65 DEG C.In reaction vessel, slowly drip 0.6mol epoxy chloropropane with dropping funnel, drip and finish, be warming up to 70 DEG C ~ 75 DEG C, reaction 3.0h, adds 0.5mol1-chloromethylbenzene after reaction terminates, fully mixes;
(2) 0.4mol diethylenetriamine is added in the reaction vessel with whipping appts, add 3.0mol ethanol, be warming up to 70 DEG C, slowly drip 0.4mol epoxy chloropropane with dropping funnel, drip and finish, 70 DEG C of reaction 3.0h;
(3) slowly drop in the mixture of step (2) gained by step (1) gained mixed solution dropping funnel, drip and finish, be warming up to 90 DEG C ~ 95 DEG C, reaction 4h, obtains product.Mass spectroscopy records product molecular-weight average and is about 21370, and its polymerization degree is 15.2.
Embodiment 4
Using the product in embodiment 1-3, by measuring the working substance content in the rear solution of self-assembly generation, indirectly can characterize the self-assembly speed of molecule.Result shows: under 30 DEG C, 60 DEG C and 90 DEG C of three kinds of temperature, the solution effective content of three kinds of products all showed anticlimax phenomenon after 0.5 day, and culminated after 2 days, in solution, effective constituent is 0.02%.
Embodiment 5
Use the product in embodiment 1-3, it is 2.5cm that assembling is prepared into diameter, and height is the right cylinder of 2.5cm, measures its ultimate compression strength after seasoning.The ultimate compression strength of three kinds of products is respectively 8.9MPa, 9.5MPa, 9.7MPa.
Embodiment 6
Be that the quartz sand of 0.1 ~ 0.6mm or reservoir sand and a certain amount of kaolin (200 order) mix by a certain percentage by particle diameter, load plexi-glass tubular (80cm × 5cm); Need in filling process to use perspex bar compacting, two ends seal with the metal cap that outlet aperture is 0.5cm respectively, prepare the artificial rock core of different permeability (high, medium and low).Then at 60 DEG C, the viscosity of a saturated rock core volume (1PV) is 200mPa.s crude oil, prepares saturated core; By the basket (1#) of a unsaturation crude oil, (saturated local water, salinity is 35000mg/L, CaCl 2type) and basket (2#) horizontal positioned in parallel of a saturated crude oil, for subsequent use; Forward passes into the local water that salinity is 350000mg/L, and after waiting two basket both sides pressure reduction stable, then the mass percent of inverse injection 1-6PV is the product in the embodiment 1 of 3%, arrest reaction some hours, measures 1# basket rate of permeation K 1with with 2# basket rate of permeation K 2, and respectively at 30 DEG C, at 60 DEG C and 90 DEG C of three kinds of temperature, measure the permeability variation before and after two kinds of rock core different treatment amounts (1-6PV) process.The results are shown in Table 1, table 2, table 3.
Ooze water wet core (1#) and oil-wet core (2#) for height, the product in the embodiment 1 of 3%, treatment capacity is respectively 1,2,3,4,5 and 6PV, along with the increase for the treatment of capacity, water plugging rate significantly rises, and along with the rising of temperature, water plugging rate slightly declines.When treatment capacity is 1PV, at three kinds of temperature, (30 DEG C, 60 DEG C, 90 DEG C) water plugging rate is all greater than 55%; When treatment capacity is 4PV, water plugging rate all reaches more than 80%, and oil plugging rate increases by a small margin along with the increase for the treatment of capacity and temperature all has.When treatment capacity is 1PV, at three kinds of temperature, (30 DEG C, 60 DEG C, 90 DEG C) oil plugging rate is less than 3%; When treatment capacity is 4PV, oil plugging rate has increased to about 12%.Result shows: this plugging agent has desirable oil, water selective shut-off capacity for the rock core of higher permeability.
Under table 1 30 DEG C of conditions, embodiment 1 product oozes sealing ratiod (48h) that is moisture, saturated core to height
Treatment capacity/PV 0 1 2 3 4 5 6
1# core permeability/DC 38.4 12.8 8.4 5.7 3.2 2.4 1.7
1# reservoir core plugging rate/% _ 66.7 78.1 85.2 91.7 94.8 95.6
2# core permeability/DC 23.5 23.1 22.6 22.0 21.2 21.0 20.8
2# reservoir core plugging rate/% _ 1.7 3.8 6.8 9.8 10.6 11.5
Under table 2 60 DEG C of conditions, embodiment 1 product oozes sealing ratiod (48h) that is moisture, saturated core to height
Treatment capacity/PV 0 1 2 3 4 5 6
1# core permeability/DC 38.2 14.6 9.2 6.2 4.8 3.5 2.1
1# reservoir core plugging rate/% _ 61.8 70.7 83.8 87.4 90.8 94.5
2# core permeability/DC 20.8 20.2 19.6 19.0 18.7 18.4 18.2
2# reservoir core plugging rate/% _ 2.9 5.8 8.7 10.1 11.6 12.5
Under table 3 90 DEG C of conditions, embodiment 1 product oozes sealing ratiod (48h) that is moisture, saturated core to height
Treatment capacity/PV 0 1 2 3 4 5 6
1# core permeability/DC 38.4 16.1 12.5 9.8 6.8 4.5 3.0
1# reservoir core plugging rate/% _ 58.1 67.5 74.5 82.3 88.3 92.2
2# core permeability/DC 20.1 19.5 18.8 18.1 17.7 17.5 17.4
2# reservoir core plugging rate/% _ 3.0 6.5 10.0 11.9 12.9 13.4
Embodiment 7
Centering oozes the selective water shut-off performance evaluation of oil-containing and moisture rock core.By the selective blocking outlet capacity of the product centering rate of permeation oil-containing in the instrument in embodiment 6, materials and methods Evaluation operation example 2 and moisture rock core.The results are shown in Table 4, table 5, table 6.
For in ooze water wet core (1#) and oil-wet core (2#), the product in the embodiment 2 of 3%, treatment capacity is respectively 1,2,3,4,5 and 6PV, along with the increase for the treatment of capacity, water plugging rate also significantly rises, and along with the rising of temperature, water plugging rate slightly declines.When treatment capacity is 1PV, at three kinds of temperature, (30 DEG C, 60 DEG C, 90 DEG C) water plugging rate is greater than 70%, and when treatment capacity is 4PV, water plugging rate all reaches 90%.And oil plugging rate along with treatment capacity and temperature increase all have and increase by a small margin.When treatment capacity is 1PV, at three kinds of temperature, (30 DEG C, 60 DEG C, 90 DEG C) oil plugging rate is less than 3%, and when treatment capacity is 4PV, oil plugging rate has increased to about 12%.Result shows, this plugging agent has desirable oil, water selective shut-off capacity equally for medium infiltrative rock core.
Under table 4 30 DEG C of conditions, embodiment 2 product centering oozes sealing ratiod (48h) that is moisture, saturated core
Treatment capacity/PV 0 1 2 3 4 5 6
1# core permeability/DC 2.66 0.67 0.30 0.19 0.11 0.075 0.040
1# reservoir core plugging rate/% _ 74.8 88.7 92.8 95.8 97.2 98.5
2# core permeability/DC 1.82 1.77 1.75 1.69 1.65 1.63 1.61
2# reservoir core plugging rate/% _ 2.7 3.8 7.1 9.3 10.4 11.5
Under table 5 60 DEG C of conditions, embodiment 2 product centering oozes sealing ratiod (48h) that is moisture, saturated core
Treatment capacity/PV 0 1 2 3 4 5 6
1# core permeability/DC 2.84 0.74 0.40 0.27 0.18 0.12 0.090
1# reservoir core plugging rate/% _ 73.9 85.9 90.5 93.7 95.8 96.8
2# core permeability/DC 1.60 1.55 1.53 1.48 1.44 1.43 1.41
2# reservoir core plugging rate/% _ 3.0 4.4 7.5 10.0 10.6 11.9
Under table 6 90 DEG C of conditions, embodiment 2 product centering oozes sealing ratiod (48h) that is moisture, saturated core
Treatment capacity/PV 0 1 2 3 4 5 6
1# core permeability/DC 2.75 0.78 0.47 0.32 0.20 0.17 0.14
1# reservoir core plugging rate/% _ 71.6 82.9 88.4 92.7 93.8 94.9
2# core permeability/DC 1.68 1.62 1.60 1.55 1.51 1.50 1.48
2# reservoir core plugging rate/% _ 33.6 4.8 7.7 10.1 10.7 11.9
Embodiment 8
To the selective water shut-off performance evaluation of hypotonic oil-containing and moisture rock core.By the product of the instrument in embodiment 6, materials and methods Evaluation operation example 3 to the selective blocking outlet capacity (see table 7, table 8, table 9) of low permeability oil-containing and moisture rock core.
Result shows: this plugging agent has desirable oil, water selective shut-off capacity equally to low-permeability water wet core.
Under table 7 30 DEG C of conditions, embodiment 3 product is to the sealing ratiod (48h) of hypotonic moisture, saturated core
Treatment capacity/PV 0 0.5 1.0 1.5 2.0 2.5 3.0
1# core permeability/× 10 -3DC 638 237 93 61 40 32 10
1# reservoir core plugging rate/% _ 62.9 85.4 90.4 93.7 95.0 98.4
2# core permeability/× 10 -3DC 445 428 422 408 398 395 390
2# reservoir core plugging rate/% _ 3.8 5.2 8.3 10.6 11.2 12.4
Under table 8 60 DEG C of conditions, embodiment 3 product is to the sealing ratiod (48h) of hypotonic moisture, saturated core
Treatment capacity/PV 0 0.5 1.0 1.5 2.0 2.5 3.0
1# core permeability/× 10 -3DC 680 284 146 112 85 49 38
1# reservoir core plugging rate/% _ 58.2 78.5 83.5 87.5 92.8 94.4
2# core permeability/× 10 -3DC 426 408 402 388 380 378 374
2# reservoir core plugging rate/% _ 4.2 5.6 8.9 10.8 11.3 12.2
Under table 9 90 DEG C of conditions, embodiment 3 product is to the sealing ratiod (48h) of hypotonic moisture, saturated core
Treatment capacity/PV 0 0.5 1.0 1.5 2.0 2.5 3.0
1# core permeability/× 10 -3DC 635 270 147 114 88 57 40
1# reservoir core plugging rate/% _ 57.5 76.9 82.0 86.1 91.0 93.7
2# core permeability/× 10 -3DC 382 364 358 346 340 336 334
2# reservoir core plugging rate/% _ 4.7 6.3 9.4 11.0 12.0 12.6

Claims (2)

1. a supramolecule selective water shutoff agent for oil wells, is characterized in that its structure can represent with following general formula:
R in formula 1, R 2be respectively group (I), group (II), m is 1,2 or 3; N is 15,16 or 17.
。
2. the preparation method of a kind of supramolecule selective water shutoff agent for oil wells according to claim 1, is characterized in that implementing as follows:
The first step, after 0.45 ~ 0.6mol beta-cyclodextrin is fully mixed with 5mol dehydrated alcohol, constant temperature 0.5 ~ 2h in 65 DEG C, uniformly solution, in this solution, slowly drip 0.4 ~ 0.6mol epoxy chloropropane, drip and finish, be warming up to 70 DEG C ~ 75 DEG C reaction 3 ~ 5h, add 0.5mol1-chloromethylbenzene after reaction terminates, fully mix;
Second step, fully mixes 0.2 ~ 0.4mol diethylenetriamine with 3mol dehydrated alcohol, is warming up to 70 DEG C, more slowly drips 0.2 ~ 0.4mol epoxy chloropropane in this solution, drips and finishes, in 70 DEG C of reaction 3 ~ 5h;
3rd step, slowly drops to the first step gained mixing solutions in second step gained reaction product, drips and finishes, and reaction system is warming up to 90 DEG C ~ 95 DEG C reaction 4 ~ 6h, obtains the finished product.
CN201410844248.6A 2014-12-23 2014-12-23 A kind of supermolecule selective water shutoff agent for oil wells and preparation method thereof Active CN104592524B (en)

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CN107057666A (en) * 2017-05-03 2017-08-18 林林 A kind of sand prevention integrated chemical agent of supermolecule oilwell water shutoff and preparation method thereof
CN107474817A (en) * 2017-06-08 2017-12-15 西南石油大学 A kind of Supramolecular self assembly fracturing fluid

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CN107057666A (en) * 2017-05-03 2017-08-18 林林 A kind of sand prevention integrated chemical agent of supermolecule oilwell water shutoff and preparation method thereof
CN107474817A (en) * 2017-06-08 2017-12-15 西南石油大学 A kind of Supramolecular self assembly fracturing fluid
CN107474817B (en) * 2017-06-08 2019-04-02 西南石油大学 A kind of Supramolecular self assembly fracturing fluid

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