CN102816558B - Plugging agent for deep profile control and water plugging and preparation method thereof - Google Patents
Plugging agent for deep profile control and water plugging and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a plugging agent for deep profile control and water plugging and a preparation method thereof. The plugging agent comprises the following raw materials in percentage by weight: 0.10-0.30% of partially hydrolyzed polyacrylamide, 0.09-0.20% of potassium dichromate, 0.15-0.30% of sodium sulfite, 0.08-0.3% of hexamethylenetetramine, 0.06-0.24% of phenol, 0.04-0.14% of ammonium chloride and the balance of water. The invention also provides the preparation method of the plugging agent. The variation of the gelatinization strength of the plugging agent system along with time is in an obvious double-step trend. Thus, the plugging agent can be effectively prevented from leaking into a low-permeability layer in the injection process, and can effectively plug a high-permeability stratum when the plugging agent reaches the deep stratum.
Description
Technical field
The present invention relates to a kind of well deep part profile control and water plugging blocking agent and preparation method thereof, belong to technical field of oilfield chemistry.
Background technology
Profile control and water plugging, as increase oil-displacing agent sweep efficiency, improves an important technology of oil recovery factor, is widely used in oil field.Along with going deep into of oil-field development, water drive contradiction also strengthens thereupon, and in layer, non-homogeneous degree worsens further, needs the well of profile control and water plugging to increase year by year.When utilizing frozen glue to adjust stifled stratum, although metallic-ion crosslinking agent gelling strength is large, its crosslinking time is short, profile control and water plugging operating area is only limitted to immediate vicinity of wellbore, inject water and stream phenomenon seriously, cause the reserves of deep hyposmosis band to employ, action effect is limited; Although resol class linking agent crosslinking time is long, Initial Viscoelastic is poor, easily misses in injection process, causes the waste of blocking agent, and can damage hydrocarbon zone.
The depth profile control agent of current application mainly contains compound-ion profile-modifying agent, flow-gel etc.Compound-ion profile-modifying agent is made up of zwitterion polymkeric substance, phenol, oxalic acid, Resorcinol, and amendment cost is high, configuration is complicated; Flow-gel is made up of polymeric anion type polyacrylamide, Tiorco 677, thiocarbamide, and cost is low, but Weak Gels large usage quantity, construction period is longer.Such as, CN102559159A(CN201110417293.X) a kind of high-temperature resistant phenolic resin weak gel profile control plugging agent is provided, to be reacted the profile-controlling and plugging agent formed by its amide group and linking agent by partially hydrolyzed polyacrylamide, wherein, partially hydrolyzed polyacrylamide consumption is 0.25%-1.2%, linking agent (phenol etc. are made) 0.2%-1%, additive (ammonium chloride) 0.01%-1% and water.The water plugging rate of high-temperature resistant phenolic resin weak gel profile control plugging agent provided by the invention is greater than 80%, oil plugging rate is less than 30%, high temperature resistant property can reach more than 90 DEG C, the highest 85000mg/L(that can reach of resistance to salinity is in 80000mg/L sodium-chlor and 5000mg/L calcium chloride), gel-strength is high, break through strength ratio and improve 68% in the past, gelation time is adjustable, can reach the object of shutoff most permeable zone and deep adjustment profile-log of water injection in the earth formation.CN101892037A(CN201010233614.6) a kind of novel salt-resistant gel selective water shutoff agent is provided, mainly comprise: cationic polyacrylamide 0.54% ~ 0.64%, linking agent (vulkacit H) 0.8 ~ 1.6%, phenol 0.9 ~ 1.2%, conditioning agent (oxalic acid) 0.02 ~ 0.6%, NaCl 0 ~ 4%, surplus is water; Wherein, described per-cent is weight percentage.Novel salt-resistant gel selective water shutoff agent of the present invention is a kind of crosslinked polymeric system, temperature resistance, salt tolerant, and gelation time is adjustable, overcomes the problem of existing water-plugging technique to the poor selectivity of profit.Selective water shutoff agent water plugging rate of the present invention is greater than 95%; Oil plugging rate is less than 30%; Temperature resistance reaches 85 DEG C; Resistance to salinity (in sodium-chlor) the highest 40000mg/L(take seawater as dosing basis); Gel time is greater than 96 hours.Above-mentioned patent document solves corresponding technical problem, but also there is following what time needs and improve: adopt cation type polymer, consumption is large, can injection poor, cost is high and in stratum absorption seriously; Adopt anionic polymer, then spininess is cross-linked its structural single group, and polymkeric substance and dosage of crosslinking agent are greatly, less economical, and difficulty pumps into stratum; Conventional single group is cross-linked blocking agent system and adjusts in injection process and stifledly can not well to combine with the displacement of reservoir oil.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of deep profile controlling water blockoff blocking agent and preparation method thereof.
Technical scheme of the present invention is as follows:
A kind of deep profile controlling water blockoff blocking agent, feed composition is as follows by weight percentage:
Partially hydrolyzed polyacrylamide (HPAM) 0.10 ~ 0.30%, potassium bichromate 0.09 ~ 0.20%, sodium sulphite 0.15 ~ 0.30%, vulkacit H 0.08 ~ 0.3%, phenol 0.06 ~ 0.24%, ammonium chloride 0.04 ~ 0.14%, excess water.
Preferably, deep profile controlling water blockoff blocking agent, feed composition is as follows by weight percentage:
Partially hydrolyzed polyacrylamide 0.15 ~ 0.23%, potassium bichromate 0.09 ~ 0.12%, sodium sulphite 0.15 ~ 0.24%, vulkacit H 0.08 ~ 0.20%, phenol 0.06 ~ 0.16%, ammonium chloride 0.06 ~ 0.14%, excess water.
Preferred according to the present invention, described partially hydrolyzed polyacrylamide is viscosity-average molecular weight is 1000 ~ 1,900 ten thousand, degree of hydrolysis is the partially hydrolyzed polyacrylamide of 25 ~ 30%.
Preferred according to the present invention, described sodium sulphite and the mass ratio of potassium bichromate are 1.5 ~ 2.0:1.
Preferred according to the present invention, described water is salinity lower than the clear water of 500mg/L or tap water.
Each component in deep profile controlling water blockoff blocking agent of the present invention is commercially available prod, and described potassium bichromate, sodium sulphite, vulkacit H, phenol, ammonium chloride are preferably analytical pure.
According to the present invention, a kind of preparation method of deep profile controlling water blockoff blocking agent, step is as follows:
Each component is got by proportioning, partially hydrolyzed polyacrylamide is added in suitable quantity of water and stirs, be made into 5000mg/L solution, slaking 4 ~ 6h under normal temperature, partially hydrolyzed polyacrylamide mother liquor good for slaking is added the water of residual content, stir 0.5h, in the Partially Hydrolyzed Polyacrylamide Solution stirred after then potassium bichromate, sodium sulphite, vulkacit H, phenol, ammonium chloride being added dilution in proportion at 20 ~ 50 DEG C, stirring 0.5h at 20 ~ 30 DEG C, obtain deep profile controlling water blockoff blocking agent.
Deep profile controlling water blockoff blocking agent of the present invention, adapting to formation temperature is 55 ~ 90 DEG C.
Deep profile controlling water blockoff blocking agent of the present invention, adapts to stratum salinity < 30000mg/L.
Deep profile controlling water blockoff blocking agent of the present invention carries out the application in profile control and water plugging when oilfield exploitation, gelation time is at 4 ~ 200h, and it is controlled to realize gelation time by the dosage controlling different crosslinker component; Breakthrough pressure gradient > 6MPa/m; Reservoir core plugging rate is greater than 95%; Blocking agent is injected water through 10PV and is washed away, and sealing ratiod still keeps more than 90%, blocking agent good stability.
Technical characterstic of the present invention:
1, blocking agent of the present invention is double-basis group cross-linking system, makes full use of the characteristic of two crosslinked group on HPAM molecular structure, can realize secondary crosslinking, have " step " shape cross-linking curve (as Fig. 2);
2, the polymkeric substance of blocking agent system formulation of the present invention and crosslinker concentration lower (consumption is few), initial viscosity is suitable, is easy to pump into;
3, the present invention utilizes once weak being cross-linked plugging technology and technology of reservoir sweep to be coordinated to combine, and secondary is asynchronous crosslinked, completes once weak crosslinked, effectively reduce its leakage to low permeability layer, and have certain oil displacement efficiency in nearly well section; Deep formation completes secondary crosslinking, forms high strength blocking agent, effective shutoff most permeable zone, with in increasing, the sweep efficiency of low permeability layer.
Reaction mechanism of the present invention illustrates:
(1) molecular formula of partially hydrolyzed polyacrylamide (HPAM) is as follows:
HPAM molecular chain also exists jointly carboxyl (-COONa) and amide group (-CONH
2) two crosslinkable groups, wherein carboxyl can occur crosslinked, as redox system or Cr with transition metal ions linking agent
3+, Al
3+, Zr
4+deng chelating systems; Amide group can be cross-linked with phenolic resin crosslinking agent generation dehydrating condensation.
(2) because the inorganic metal cross-linking agents time is fast, be therefore once cross-linked as Cr
3+with being cross-linked of carboxyl.
1. the S-WAT in inorganic chromium cross-linking system is by the Cr in sodium dichromate 99
6+be reduced into Cr
3+, reaction formula is as follows:
Cr
2O
7 2-+3SO
3 2-+8H
+→2Cr
3++3SO
4 2-+4H
2O
2. Cr
3+through further hydration, hydrolysis and ol bridge effect:
3. Cr
3+polynuclear hydroxy bridge complex ion can with-the COO in HPAM
-coordination, form the frozen glue of network structure, its structure is as follows:
(3) resol class crosslinking time is slow, and therefore secondary crosslinking is resol and being cross-linked of amide group, and reaction formula is as follows:
1. phenol and formaldehyde carry out condensation reaction, and generate methylolphenol or resol, reaction formula is as follows:
2. HPAM and resol carry out dehydrating condensation, and reaction formula is as follows:
Excellent results of the present invention:
Deep profile controlling water blockoff blocking agent system provided by the invention is cross-linked at twice, and gelation time is fast for the first time, and gelling strength is weak, can ensure good injection, effectively can prevent again the leakage to low-permeability layer in its migration process; By linking agent and the additive of regulation system, control second time crosslinking time, enter after the predetermined depth of stratum until this system, it is crosslinked that system completes second time, and blocking agent plugging strength is high, good stability, can carry out effective shutoff at earth formation deep.This blocking agent system effectively improves the strength and stability of polymer gel, reduces polymer loading, and realizes timing, controlled delay cross linking, can meet Different Strata, different depths adjusts stifled requirement.
It is few that deep profile controlling water blockoff blocking agent of the present invention has drug dosage, and cost is low, preparation is simple, gelation time is long and controlled; The features such as gelling strength is high, good stability, can improve water flooding effect.
Accompanying drawing explanation
Fig. 1 is prior art vacuum breakthrough pressure method measuring apparatus schematic diagram; In figure, 1, colorimetric cylinder, 2, U-tube, 3, rubber tubing, 4, tensimeter, 5, filter flask, 6, vacuum pump.
Fig. 2 is embodiment 7 blocking agent system gelling strength change curve in time.X-coordinate is gelation time (h), and ordinate zou breaks through vacuum pressure (MPa).
Fig. 3 is embodiment 8 and existing displacement test device schematic flow sheet used in reference examples 3; In figure, 11, constant-flux pump, 12, intermediate receptacle, 13, six-way valve, 14, precision pressure gauge, 15, fill out sand tube, 16, oily water separation pipe.
Embodiment
For further illustrating the present invention, below enumerate specific embodiment, but institute of the present invention protection domain is not limited only to this.
In embodiment, polymkeric substance adopts anionic partially hydrolyzed polyacrylamide, viscosity-average molecular weight 1,600 ten thousand, degree of hydrolysis 25 ~ 30%.Water used is the tap water of salinity lower than 500mg/L.
Embodiment 1
Deep profile controlling water blockoff blocking agent, raw material forms:
Partially hydrolyzed polyacrylamide 0.15%, potassium bichromate 0.1%, sodium sulphite 0.2%, vulkacit H 0.15%, phenol 0.12%, ammonium chloride 0.1%, the water of surplus.
Preparation method:
Each component is got by proportioning, partially hydrolyzed polyacrylamide powder is added in suitable quantity of water and stirs, being made into concentration is 5000mg/L solution, slaking 5h under normal temperature, partially hydrolyzed polyacrylamide mother liquor good for slaking is joined in the water of residual content, stir 0.5h at 26 DEG C, obtain partially hydrolyzed polyacrylamide diluting soln; Then potassium bichromate, sodium sulphite, vulkacit H, phenol, ammonium chloride are added in partially hydrolyzed polyacrylamide diluting soln in proportion, stir 0.5h at 26 DEG C, obtain deep profile controlling water blockoff blocking agent.
Gained blocking agent test case: under 60 DEG C of conditions, this blocking agent system first time gelation time is 23h, and second time gelation time is about 148h; (rate of permeation is 1.06 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 7MPa/m; Reservoir core plugging rate is 95.3%; Inject water through 10PV to wash away, blocking agent is 90.6% to the sealing ratiod of rock core.
Embodiment 2
As described in Example 1, difference is, blocking agent raw material consists of:
Partially hydrolyzed polyacrylamide 0.20%, potassium bichromate 0.08%, sodium sulphite 0.16%, vulkacit H 0.10%, phenol 0.08%, ammonium chloride 0.10%, the water of surplus.
Gained blocking agent test case: under 60 DEG C of conditions, this blocking agent system first time gelation time is about 46h, and second time gelation time is about 285h; (rate of permeation is 1.11 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 10MPa/m; Reservoir core plugging rate is 97.1%; Inject water through 10PV to wash away, blocking agent is 92.8% to the sealing ratiod of rock core.
Embodiment 3
As described in Example 1, difference is, blocking agent raw material consists of:
Partially hydrolyzed polyacrylamide 0.25%, potassium bichromate 0.08%, sodium sulphite 0.16%, vulkacit H 0.10%, phenol 0.08%, ammonium chloride 0.10%, the water of surplus.
Gained blocking agent test case: under 60 DEG C of conditions, this blocking agent system first time gelation time is about 6h, and second time gelation time is about 150h; (rate of permeation is 1.08 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 12MPa/m; Reservoir core plugging rate is 98.8%; Inject water through 10PV to wash away, blocking agent is 93.4% to the sealing ratiod of rock core.
Embodiment 4
As described in Example 1, difference is, blocking agent raw material consists of:
Partially hydrolyzed polyacrylamide 0.20%, potassium bichromate 0.10%, sodium sulphite 0.20%, vulkacit H 0.10%, phenol 0.08%, ammonium chloride 0.12%, the water of surplus.
Gained blocking agent test case: under 60 DEG C of conditions, this blocking agent system first time gelation time is about 3.5h, and second time gelation time is about 175h; (rate of permeation is 1.01 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 11MPa/m; Reservoir core plugging rate is 97.7%; Inject water through 10PV to wash away, blocking agent is 92.6% to the sealing ratiod of rock core.
Embodiment 5
As described in Example 1, difference is, blocking agent raw material consists of:
Partially hydrolyzed polyacrylamide 0.15%, potassium bichromate 0.12%, sodium sulphite 0.18%, vulkacit H 0.20%, phenol 0.12%, ammonium chloride 0.10%, the water of surplus.
Gained blocking agent test case: under 60 DEG C of conditions, this blocking agent system first time gelation time is about 7h, and second time gelation time is about 120h; (rate of permeation is 1.03 μm to rock core
2) breakthrough pressure gradient is 8MPa/m; Reservoir core plugging rate is 96.1%; Inject water through 10PV to wash away, blocking agent is 91.2% to the sealing ratiod of rock core.
Embodiment 6
As described in Example 1, difference is, blocking agent raw material consists of:
Partially hydrolyzed polyacrylamide 0.20%, potassium bichromate 0.10%, sodium sulphite 0.15%, vulkacit H 0.15%, phenol 0.12%, ammonium chloride 0.06%, the water of surplus.
Gained blocking agent test case: under 60 DEG C of conditions, this blocking agent system first time gelation time is about 4h, and second time gelation time is about 112h; (rate of permeation is 1.06 μm to rock core
2) breakthrough pressure gradient (blocking agent injection rate is 0.3PV) is 10.5MPa/m; Reservoir core plugging rate is 96.9%; Inject water through 10PV to wash away, blocking agent is 92.0% to the sealing ratiod of rock core.
Embodiment 7, blocking agent secondary crosslinking gelling strength are tested
Test sample: as described in Example 1, difference is, blocking agent raw material consists of: partially hydrolyzed polyacrylamide 0.20%, potassium bichromate 0.10%, sodium sulphite 0.20%, vulkacit H 0.10%, phenol 0.08%, ammonium chloride 0.10%, the water of surplus.
Experimental technique: poured in ampoule by the blocking agent solution stirred and seal, is placed in water bath with thermostatic control under 60 DEG C of conditions, then surveys the gelling strength of this blocking agent by vacuum breakthrough pressure method at different time.Vacuum breakthrough pressure method experimental installation (as shown in Figure 1), experimental result as shown in Figure 2.
This blocking agent system increased along with the time as seen from Figure 2, and gelling strength presents two comparatively significantly " steps ", and namely gelling strength is first increased to one and comparatively keeps certain hour after low strength, and then is increased to a higher-strength gradually.When first " step ", blocking agent gelling strength is lower, ensures the normal injection of blocking agent, and effectively prevents blocking agent to the leakage of low permeability layer; When blocking agent arrives earth formation deep, gelling strength increases, and is conducive to the effective shutoff high-permeability reservoir of blocking agent.
Embodiment 8, blocking agent Oil Displacing Capacity are tested
Test sample: with embodiment 7.
Experimental technique: displacement test
Adopt displacement test device first to saturation water in fill out sand tube, then saturated oil, carry out water drive after the aging 24h of normal temperature and reach 98% to water ratio, calculate waterflood recovery efficiency factor; Then inject the blocking agent system of 0.3PV, and then filled drive reaches 98% to water ratio, calculate blocking agent system and improve recovery ratio value.Experimental result is as shown in table 1.
The Oil Displacing Capacity of table 1 blocking agent system
| Water surveys rate of permeation, μm 2 | Porosity, % | Waterflood recovery efficiency factor, % | Cross-linking system drives recovery ratio, % | Recovery ratio increased value, % |
| 1.18 | 28.1 | 61.7 | 80.9 | 19.2 |
As can be seen from Table 1, blocking agent system, on the basis of water drive irreducible oil, can improve recovery ratio 19.2%.
Reference examples 1 adopts anionic partially hydrolyzed polyacrylamide (viscosity-average molecular weight 1,600 ten thousand, degree of hydrolysis 25 ~ 30%), and potassium bichromate, sodium sulphite, ammonium chloride are configured to the aqueous solution by the preparation method of embodiment 1.Wherein, filling a prescription is: partially hydrolyzed polyacrylamide 0.25%, potassium bichromate 0.10%, sodium sulphite 0.20%, ammonium chloride 0.10%, excess water.
Under 60 DEG C of conditions, this blocking agent system gelation time is 3h; (rate of permeation is 1.00 μm to rock core
2) breakthrough pressure gradient is 10MPa/m; Reservoir core plugging rate is 92.3%; Inject water through 10PV to wash away, blocking agent is 80.1% to the sealing ratiod of rock core.
Reference examples 2 adopts anionic partially hydrolyzed polyacrylamide (viscosity-average molecular weight 1,600 ten thousand, degree of hydrolysis 25 ~ 30%), and vulkacit H, phenol are configured to the blocking agent aqueous solution by embodiment 1 preparation method.Wherein, filling a prescription is: partially hydrolyzed polyacrylamide 0.25%, tetramine 0.10%, phenol 0.08%, excess water.
Under 60 DEG C of conditions, this blocking agent system is cross-linked into weak frozen glue, and gelation time is 260h; (rate of permeation is 1.13 μm to rock core
2) breakthrough pressure gradient is 6MPa/m; Reservoir core plugging rate is 87.7%; Inject water through 10PV to wash away, blocking agent is 68.2% to the sealing ratiod of rock core.
Reference examples 3 polymer flooding is tested:
Adopt anionic partially hydrolyzed polyacrylamide (viscosity-average molecular weight 1,600 ten thousand, degree of hydrolysis 25 ~ 30%), be directly mixed with the aqueous solutions of polymers of 0.25%.Adopt the experimental technique identical with embodiment 8, calculate polymkeric substance and improve recovery ratio effect.Experimental result is in table 2.
The Oil Displacing Capacity of table 2 polymkeric substance (partially hydrolyzed polyacrylamide)
| Water surveys rate of permeation, μm 2 | Porosity, % | Waterflood recovery efficiency factor, % | Polymer flooding recovery ratio, % | Recovery ratio increased value, % |
| 1.03 | 26.6 | 59.9 | 72.4 | 12.5 |
As can be seen from table 1 and table 2, partially hydrolyzed polyacrylamide polymkeric substance, on the basis of water drive irreducible oil, can improve recovery ratio 12.5%, lower than the recovery ratio increased value (19.2%) of the blocking agent system of the present invention containing partially hydrolyzed polyacrylamide same concentrations.
Claims (1)
1. a deep profile controlling water blockoff blocking agent, is characterized in that feed composition is as follows by weight percentage:
Partially hydrolyzed polyacrylamide 0.15 ~ 0.23%, potassium bichromate 0.09 ~ 0.12%, S-WAT 0.15 ~ 0.24%, vulkacit H 0.08 ~ 0. 20%, phenol 0.06 ~ 0.16%, ammonium chloride 0.06 ~ 0.14%, excess water;
Described S-WAT and the mass ratio of potassium bichromate are 1.5 ~ 2.0:1;
Be prepared from according to the following steps:
Each component is got by proportioning, partially hydrolyzed polyacrylamide is added in suitable quantity of water and stirs, be made into 5000mg/L solution, slaking 4 ~ 6h under normal temperature, partially hydrolyzed polyacrylamide mother liquor good for slaking is added the water of residual content, stir 0.5h, in the Partially Hydrolyzed Polyacrylamide Solution stirred after then potassium bichromate, S-WAT, vulkacit H, phenol, ammonium chloride being added dilution in proportion at 20 ~ 50 DEG C, stir 0.5h at 20 ~ 30 DEG C, obtain deep profile controlling water blockoff blocking agent.
2. deep profile controlling water blockoff blocking agent as claimed in claim 1, it is characterized in that described partially hydrolyzed polyacrylamide refers to that viscosity-average molecular weight is 1000 ~ 1,900 ten thousand, degree of hydrolysis is the partially hydrolyzed polyacrylamide of 25 ~ 30%.
3. deep profile controlling water blockoff blocking agent as claimed in claim 1, is characterized in that described water is salinity lower than the clear water of 500mg/L or tap water.
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