CN107057666A - A kind of sand prevention integrated chemical agent of supermolecule oilwell water shutoff and preparation method thereof - Google Patents
A kind of sand prevention integrated chemical agent of supermolecule oilwell water shutoff and preparation method thereof Download PDFInfo
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- CN107057666A CN107057666A CN201710304481.9A CN201710304481A CN107057666A CN 107057666 A CN107057666 A CN 107057666A CN 201710304481 A CN201710304481 A CN 201710304481A CN 107057666 A CN107057666 A CN 107057666A
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- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
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- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
- C08B37/0012—Cyclodextrin [CD], e.g. cycle with 6 units (alpha), with 7 units (beta) and with 8 units (gamma), large-ring cyclodextrin or cycloamylose with 9 units or more; Derivatives thereof
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Abstract
The present invention relates to a kind of sand prevention integrated chemical agent of supermolecule oilwell water shutoff and preparation method thereof, the preparation method comprises the following steps：1) after 0.45 0.55mol hydroxypropyl cyclodextrins and 5mol absolute ethyl alcohols being sufficiently mixed, the 2h of constant temperature 1.5 in 65 DEG C, form homogeneous solution, 0.4 0.6mol epichlorohydrins are slowly added dropwise into the solution, drop finishes, 70 75 DEG C of 3 5h of reaction are warming up to, reaction adds 0.5mol1 chloromethylbenzenes after terminating, is sufficiently mixed；2) 0.25 0.4mol diethylenetriamines and 3mol absolute ethyl alcohols are sufficiently mixed, are warming up to 70 DEG C, then 0.2 0.3mol epoxychloropropane is slowly added dropwise into the solution, drop finishes, in 70 DEG C of 4 5h of reaction；3) by step 1) gained mixed solution be slowly added dropwise to step 2) gained reaction product in, drop finish, by reaction system be warming up to 90 95 DEG C reaction 6h after final products.The sand prevention integrated chemical agent of supermolecule oilwell water shutoff of the present invention overcomes the problem of poor function of conventional water shutoff agent oil-water selectivity is single.
Description
Technical field
The present invention relates to a kind of sand prevention integrated chemical agent of supermolecule oilwell water shutoff and preparation method thereof.
Background technology
China oil field comes into the tail period production phase, and most oil reservoir comprehensive water cuts are more than 90%, and oil well goes out
Water has turned into the serious problems that waterflooding oil field is faced；Based on the exploitation actuality in current oil field, oil well will generally enter
Row plug water construction operation, reduces water ratio in oil well.The effect of the sand prevention integrated medicament of water blockoff is substantially to change water in the earth formation
Flow direction, stable loose stratum can keep stratum energy by the way that water blockoff is sand prevention integrated, improve injection water or
The swept volume of other oil displacement agents, on the premise of keeping formation physical property stable, the recovery ratio for improving crude oil extends the life of oil well
The production cycle.
Existing a variety of oilwell water shutoff agent, such as polyacrylamide-lignin sulfonate selective water shutoff agent (Zhejiang at present
University's Master's thesis in 2001), xanthans-AMPS- swelling soil composite water shutoff agent (petrochemical industry Journal of Chinese Universities, 2011
Year December), magnetic polymer composite microspheres profile-controlling and plugging agent (Beijing University of Chemical Technology's Master's thesis in 2012), CN 103013480
A, CN103773338 A etc., but still need in Middle-later Development Stage of Oilfield field good, the effective water blockoff sand control medicine of selectivity
Agent.The sand prevention integrated medicament of water blockoff of the present invention is applied to oil field, oil-water well water plugging and profile controlling, with intensity height, high temperature resistant, water blockoff
The advantages of effect is good.
The content of the invention
In order to solve the above technical problems, the present invention provide a kind of sand prevention integrated chemical agent of supermolecule oilwell water shutoff and its
Preparation method.
A kind of sand prevention integrated chemical agent of supermolecule oilwell water shutoff of the present invention, its feature structure can use below formula table
Show：
R1, R2 are respectively group (I), group (II) in formula, and m is 1,2 or 3；N is 15,16 or 17；
Wherein group (I), the feature structure of group (II) are represented by the formula：
A kind of preparation method of sand prevention integrated chemical agent of supermolecule oilwell water shutoff of the present invention, comprises the following steps：
1) after 0.45-0.55mol hydroxypropyl cyclodextrins and 5mol absolute ethyl alcohols being sufficiently mixed, the constant temperature 1.5- in 65 DEG C
2h, forms homogeneous solution, and 0.4-0.6mol epichlorohydrins are slowly added dropwise into the solution, and drop finishes, and is warming up to 70-75 DEG C of reaction 3-
5h, reaction adds 0.5mol1- chloromethylbenzenes after terminating, and is sufficiently mixed；
2) 0.25-0.4mol diethylenetriamines are sufficiently mixed with 3mol absolute ethyl alcohols, are warming up to 70 DEG C, then to the solution
In be slowly added dropwise 0.2-0.3mol epoxychloropropane, drop finishes, and 4-5h are reacted in 70 DEG C；
3) by step 1) gained mixed solution be slowly added dropwise to step 2) gained reaction product in, drop finish, by reaction system
Final products are obtained after being warming up to 90-95 DEG C of reaction 6h.
Beneficial effects of the present invention are compared with prior art：The sand prevention integrated chemistry of supermolecule oilwell water shutoff of the present invention
Medicament is self-assembled supermolecular polymer of the side chain containing hydroxypropyl cyclodextrin and phenyl ring, and the present invention has synthesized one kind and contained N first
Side chain containing hydroxypropyl cyclodextrin and phenyl ring, is then connected on main chain, prepared by the main chain of atom by grafting respectively
The side chain polymer containing beta-schardinger dextrin and phenyl ring simultaneously；After this polymer is adsorbed in oil well water-wet formation, it can pass through
Self assembly generates supermolecule, so as to reach the purpose of Selective Water Plugging sand control, overcomes conventional water shutoff agent oil-water selectivity
The problem of poor function is single.
Embodiment
With reference to embodiment, the embodiment to the present invention is described in further detail.Following examples are used for
Illustrate the present invention, but be not limited to the scope of the present invention.
Embodiment 1
A kind of preparation method of the sand prevention integrated chemical agent of supermolecule oilwell water shutoff, comprises the following steps：
1) hydroxypropyl cyclodextrin for refining 0.45mol is added in the reaction vessel with agitating device, and is added
5.0mol absolute ethyl alcohols, after being sufficiently mixed, in constant temperature 0.5h in 65 DEG C, into homogeneous solution, with dropping funel into reaction vessel
0.4mol epichlorohydrins are slowly added dropwise, drop finishes, and reaction solution is warming up into 70-75 DEG C, react 3h, reaction adds 0.5mol1- after terminating
Chloromethylbenzene, is sufficiently mixed；
2) 0.2mol diethylenetriamines are added into the reaction vessel with agitating device, adds 3.0mol absolute ethyl alcohols, risen
0.2mol epichlorohydrins are slowly added dropwise with dropping funel to 70 DEG C for temperature, and drop finishes, 70 DEG C of reaction 3h；
3) by step 1) gained mixed liquor be slowly added dropwise with dropping funel to step 2) gained mixture in, drop finish, heating
To 90-95 DEG C, 4h is reacted, product is obtained.The mean molecule quantity that mass spectrography measures product is about 24100, and its degree of polymerization is 17.1.
Embodiment 2
A kind of preparation method of the sand prevention integrated chemical agent of supermolecule oilwell water shutoff, comprises the following steps：
1) the hydroxypropyl basic ring paste refined 0.5mol is added in the reaction vessel with agitating device, adds 5.0mol anhydrous
Ethanol, is sufficiently mixed, and in constant temperature 0.5h in 65 DEG C, into homogeneous solution, is slowly added dropwise with dropping funel into reaction vessel
0.5mol epichlorohydrins, drop finishes, and reaction solution is warming up into 70-75 DEG C, reacts 3.0h, and reaction adds 0.5mol1- chloromethyls after terminating
Benzene, is sufficiently mixed；
2) 0.3mol diethylenetriamines are added in the reaction vessel with agitating device, add 3.0mol absolute ethyl alcohols,
70 DEG C are warming up to, 0.3mol epichlorohydrins are slowly added dropwise with dropping funel, drop finishes, 70 DEG C of reaction 3h；
3) by step 1) gained mixed liquor be slowly added dropwise with dropping funel to step 2) gained mixture in, drop finish is warming up to
90-95 DEG C, reaction 4h obtains product.It is about 23060 that mass spectrography, which measures product mean molecule quantity, and its degree of polymerization is 16.4.
Embodiment 3
A kind of preparation method of the sand prevention integrated chemical agent of supermolecule oilwell water shutoff, comprises the following steps：
1) hydroxypropyl basic ring paste that will be refined 0.55mol is added in the reaction vessel with agitating device, add 5.0mol without
Water-ethanol is sufficiently mixed, in constant temperature 0.5h formation homogeneous solution in 65 DEG C.It is slowly added dropwise with dropping funel into reaction vessel
0.6mol epichlorohydrins, drop finishes, and is warming up to 70-75 DEG C, reacts 3.0h, and reaction adds 0.5mol1- chloromethylbenzenes after terminating, fully
Mixing；
2) 0.4mol diethylenetriamines are added in the reaction vessel with agitating device, 3.0mol is without ethanol and rises for addition
0.4mol epichlorohydrins, 70 DEG C of reaction 3.0h are slowly added dropwise with dropping funel to 70 DEG C for temperature；
3) by step 1) gained mixed liquor be slowly added dropwise with dropping funel to step 2) obtained by mixture in, drop finish, rise
Temperature reacts 4h, obtains product to 90-95 DEG C.It is about 21370 that mass spectrography, which measures product mean molecule quantity, and its degree of polymerization is 15.2.
, can be indirect by determining the substance content after self assembly generation in solution using the product in embodiment 1-3
Characterize the self assembly speed of molecule.As a result show：At a temperature of 30 DEG C, 60 DEG C and 90 DEG C three kinds, the solution of three kinds of products is effective
Content showed anticlimax phenomenon after 0.5 day, by 2 days after culminate, active ingredient is 0.015-0.2% in solution.
Using the product in embodiment 1-3, assembling is prepared into a diameter of 2.5cm, and a height of 2.5cm cylinder is done naturally
Its compression strength is determined after dry.The compression strength of three kinds of products is respectively 9.0MPa, 9.5MPa, 9.7Mpa.
Implement 1
Particle diameter is mixed by a certain percentage for 0.1-0.6mm quartz sand or reservoir sand and a certain amount of kaolin (200 mesh)
It is even, load lucite tube (100cm × 5cm)；Need to be compacted with perspex bar during filling, outlet aperture is used at two ends respectively
Sealed for 0.5cm metal cap, prepare the artificial rock core of different permeability (high, medium and low).Then at 60 DEG C, saturation one
The viscosity of rock core volume (1PV) is 200mPa.s crude oil, prepares saturated core；By the basket (1#) of a unsaturated crude oil
The basket (2#) of (saturation stratum water, salinity is 45000mg/L, CaCl2 types) and saturation crude oil horizontal positioned in parallel,
It is standby；Forward direction is passed through the stratum water that salinity is 350000mg/L, after waiting two basket both sides pressure differences stable, then inverse injection
1-6PV mass percent is the product in 3% embodiment 1, arrest reaction some hours, determines 1# basket permeabilities K1
With with 2# basket permeability K2, and at a temperature of 30 DEG C, 60 DEG C and 90 DEG C three kinds determine two kinds of rock core different disposal amounts
The permeability variation of (1-6PV) before and after the processing.It the results are shown in Table 1, table 2, table 3.
For hypertonic water-wet core (1#) and oil-wet core (2#), the product in 3% embodiment 1, treating capacity is respectively
1st, 2,3,4,5 and 6PV, with the increase for the treatment of capacity, water plugging rate is substantially increased, and with the rise of temperature, water plugging rate is slightly decreased.
When treating capacity is 1PV, (30 DEG C, 60 DEG C, 90 DEG C) water plugging rate is all higher than 55% at a temperature of three kinds；When treating capacity is 4PV, water plugging rate
More than 80% has been reached, and oil plugging rate increases by a small margin as the increase for the treatment of capacity and temperature has.When treating capacity is 1PV,
(30 DEG C, 60 DEG C, 90 DEG C) oil plugging rate is less than 3% at a temperature of three kinds；When treating capacity is 4PV, oil plugging rate has increased to 12% or so.
As a result show：The water shutoff agent has preferably oil, water selective closure sand control energy for the rock core of higher permeability
Power.
Sealing ratiod (48h) of the product of embodiment 1 to hypertonic aqueous saturated core under the conditions of 1 30 DEG C of table
The product of embodiment 1 is to hypertonic aqueous, saturated core sealing ratiod (48h) under the conditions of 2 60 DEG C of table
| Treating capacity/PV | 0 | 1 | 2 | 3 | 4 | 5 | 6 |
| 1# core permeabilities/DC | 38.2 | 14.6 | 9.2 | 6.2 | 4.8 | 3.5 | 2.1 |
| 1# reservoir core pluggings rate/% | _ | 61.8 | 70.7 | 83.8 | 87.4 | 90.8 | 94.5 |
| 2# core permeabilities/DC | 20.8 | 20.2 | 19.6 | 19.0 | 18.7 | 18.4 | 18.2 |
| 2# reservoir core pluggings rate/% | _ | 2.9 | 5.8 | 8.7 | 10.1 | 11.6 | 12.5 |
The product of embodiment 1 is to hypertonic aqueous, saturated core sealing ratiod (48h) under the conditions of 3 90 DEG C of table
| Treating capacity/PV | 0 | 1 | 2 | 3 | 4 | 5 | 6 |
| 1# core permeabilities/DC | 38.4 | 16.1 | 12.5 | 9.8 | 6.8 | 4.5 | 3.0 |
| 1# reservoir core pluggings rate/% | _ | 58.1 | 67.5 | 74.5 | 82.3 | 88.3 | 92.2 |
| 2# core permeabilities/DC | 20.1 | 19.5 | 18.8 | 18.1 | 17.7 | 17.5 | 17.4 |
| 2# reservoir core pluggings rate/% | _ | 3.0 | 6.5 | 10.0 | 11.9 | 12.9 | 13.4 |
Example 2
The sand prevention integrated performance evaluation of the selective water plugging of oil-containing and aqueous rock core is oozed in centering.By the instrument in example 1, material
Material and method evaluate the selective blocking outlet capacity of the product centering permeability oil-containing and aqueous rock core in embodiment 2.It the results are shown in Table
4th, table 5, table 6.
The product in water-wet core (1#) and oil-wet core (2#), 3% embodiment 2 is oozed in, treating capacity is respectively
1st, 2,3,4,5 and 6PV, with the increase for the treatment of capacity, water plugging rate is also substantially increased, with the rise of temperature, water plugging rate slightly under
Drop.When treating capacity is 1PV, (30 DEG C, 60 DEG C, 90 DEG C) water plugging rate is more than 70%, when treating capacity is 4PV, water blockoff at a temperature of three kinds
Rate has reached 90%.And oil plugging rate increases by a small margin as the increase for the treatment of capacity and temperature has.When treating capacity is 1PV,
(30 DEG C, 60 DEG C, 90 DEG C) oil plugging rate is less than 3%, when treating capacity is 4PV at a temperature of three kinds, and it is left that oil plugging rate has increased to 12%
It is right.As a result show, the water shutoff agent equally has preferably oil, water selective shut-off capacity for medium infiltrative rock core.
Aqueous, saturated core sealing ratiod (48h) is oozed in the product centering of embodiment 2 under the conditions of 4 30 DEG C of table
| Treating capacity/PV | 0 | 1 | 2 | 3 | 4 | 5 | 6 |
| 1# core permeabilities/DC | 2.66 | 0.67 | 0.30 | 0.19 | 0.11 | 0.075 | 0.040 |
| 1# reservoir core pluggings rate/% | _ | 74.8 | 88.7 | 92.8 | 95.8 | 97.2 | 98.5 |
| 2# core permeabilities/DC | 1.82 | 1.77 | 1.75 | 1.69 | 1.65 | 1.63 | 1.61 |
| 2# reservoir core pluggings rate/% | _ | 2.7 | 3.8 | 7.1 | 9.3 | 10.4 | 11.5 |
Aqueous, saturated core sealing ratiod (48h) is oozed in the product centering of embodiment 2 under the conditions of 5 60 DEG C of table
| Treating capacity/PV | 0 | 1 | 2 | 3 | 4 | 5 | 6 |
| 1# core permeabilities/DC | 2.84 | 0.74 | 0.40 | 0.27 | 0.18 | 0.12 | 0.090 |
| 1# reservoir core pluggings rate/% | _ | 73.9 | 85.9 | 90.5 | 93.7 | 95.8 | 96.8 |
| 2# core permeabilities/DC | 1.60 | 1.55 | 1.53 | 1.48 | 1.44 | 1.43 | 1.41 |
| 2# reservoir core pluggings rate/% | _ | 3.0 | 4.4 | 7.5 | 10.0 | 10.6 | 11.9 |
Aqueous, saturated core sealing ratiod (48h) is oozed in the product centering of embodiment 2 under the conditions of 6 90 DEG C of table
| Treating capacity/PV | 0 | 1 | 2 | 3 | 4 | 5 | 6 |
| 1# core permeabilities/DC | 2.75 | 0.78 | 0.47 | 0.32 | 0.20 | 0.17 | 0.14 |
| 1# reservoir core pluggings rate/% | _ | 71.6 | 82.9 | 88.4 | 92.7 | 93.8 | 94.9 |
| 2# core permeabilities/DC | 1.68 | 1.62 | 1.60 | 1.55 | 1.51 | 1.50 | 1.48 |
| 2# reservoir core pluggings rate/% | _ | 33.6 | 4.8 | 7.7 | 10.1 | 10.7 | 11.9 |
As a result show：The water shutoff agent equally has preferably oily, water selective closure to hypotonicity water-wet core and anti-
Sand ability.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, some improvement and modification can also be made, these improvement and modification
Also it should be regarded as protection scope of the present invention.
Claims (1)
1. a kind of sand prevention integrated chemical agent of supermolecule oilwell water shutoff, it is characterised in that its feature structure can use below formula
Represent：
R1, R2 are respectively group (I), group (II) in formula, and m is 1,2 or 3；N is 15,16 or 17；
Wherein group (I), the feature structure of group (II) are represented by the formula：
A kind of preparation method of sand prevention integrated chemical agent of supermolecule oilwell water shutoff of the present invention, comprises the following steps：
1) after 0.45-0.55mol hydroxypropyl cyclodextrins and 5mol absolute ethyl alcohols being sufficiently mixed, the constant temperature 1.5-2h in 65 DEG C,
Homogeneous solution is formed, 0.4-0.6mol epichlorohydrins are slowly added dropwise into the solution, drop finishes, 70-75 DEG C of reaction 3-5h is warming up to, instead
0.5mol1- chloromethylbenzenes are added after should terminating, are sufficiently mixed；
2) 0.25-0.4mol diethylenetriamines are sufficiently mixed with 3mol absolute ethyl alcohols, are warming up to 70 DEG C, then delay into the solution
Slow that 0.2-0.3mol epoxychloropropane is added dropwise, drop finishes, and 4-5h is reacted in 70 DEG C；
3) by step 1) gained mixed solution be slowly added dropwise to step 2) gained reaction product in, drop finish, reaction system is heated up
Final products are obtained after to 90-95 DEG C of reaction 6h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113831457A (en) * | 2021-09-26 | 2021-12-24 | 中国海洋石油集团有限公司 | Preparation method of supramolecular material for oil well sand prevention |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102102012A (en) * | 2010-12-24 | 2011-06-22 | 中国石油天然气股份有限公司 | Selective plugging agent for horizontal well and preparation method thereof |
| CN104592524A (en) * | 2014-12-23 | 2015-05-06 | 青岛大学 | Selective water-plugging agent for super-molecular oil well and preparation method thereof |
| CN105331344A (en) * | 2015-10-23 | 2016-02-17 | 陕西省石油化工研究设计院 | High-strength selective water-plugging profile-modifying agent for low-permeability reservoir and preparation method thereof |
-
2017
- 2017-05-03 CN CN201710304481.9A patent/CN107057666A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102102012A (en) * | 2010-12-24 | 2011-06-22 | 中国石油天然气股份有限公司 | Selective plugging agent for horizontal well and preparation method thereof |
| CN104592524A (en) * | 2014-12-23 | 2015-05-06 | 青岛大学 | Selective water-plugging agent for super-molecular oil well and preparation method thereof |
| CN105331344A (en) * | 2015-10-23 | 2016-02-17 | 陕西省石油化工研究设计院 | High-strength selective water-plugging profile-modifying agent for low-permeability reservoir and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113831457A (en) * | 2021-09-26 | 2021-12-24 | 中国海洋石油集团有限公司 | Preparation method of supramolecular material for oil well sand prevention |
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