CN103555305B - Hyperbranched slow-swelling profile control particles and preparation method thereof - Google Patents
Hyperbranched slow-swelling profile control particles and preparation method thereof Download PDFInfo
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- CN103555305B CN103555305B CN201310530883.2A CN201310530883A CN103555305B CN 103555305 B CN103555305 B CN 103555305B CN 201310530883 A CN201310530883 A CN 201310530883A CN 103555305 B CN103555305 B CN 103555305B
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- 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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- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
- C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/516—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls characterised by their form or by the form of their components, e.g. encapsulated material
Abstract
The invention discloses hyperbranched slow-swelling profile control particles and a preparation method thereof. The profile control particles are prepared by drying, crushing and screening a functional skeleton monomer, an acrylamide monomer and a temperature-resistant and salt-resistant monomer by taking ammonium persulfate or azobisisobutylamidine as an initiating agent and adopting hydrogel prepared by a free radical copolymerization method, wherein the functional skeleton monomer is obtained by adopting methyl methacrylate to perform terminal group modification on polyamide-amine; the temperature-resistant and salt-resistant monomer is N-vinyl pyrrolidone, 2-acrylamide-2-sodium methylacrylsulfonate or sodium vinylsulfonate. The profile control particles disclosed by the invention take a hyperbranched skeleton unit as a core to form a three-dimensional network structure, and form hydrogel with high strength and strong toughness after water swelling to block a high-permeability layer to promote liquid flow diversion, so that the profile control particles can be used for deep profile control of an oil reservoir with the temperature of 60-120 DEG C and mineralization degree of 2*10<4>-20*10<4>mg/L. The preparation method of the profile control particles is reasonable in principle and simple and convenient in operation and has broad application prospects.
Description
Technical field
The present invention relates to one and be applicable to 60 DEG C～120 DEG C of reservoir temperatures, salinity 2 × 10
4mg/L～20 × 10
4the hyperbranched slow swelling property deep profile controlling particle of mg/L, belongs to oilfield chemistry field.
Background technology
In the oil field in waterflooding later stage, water drive form advantage passage obvious, once particularly interlayer, layer in particularly thorny oil reservoir water breakthrough, oil offtake will reduce rapidly, most crude oil be trapped in stratum is difficult to exploitation, deficiency in economic performance.For this type of oil reservoir, profile control and water plugging system can shutoff high permeability formation, impels fluid diversion, improves intake profile and is widely used in profile control and the water blockoff of high temperature and high salt oil deposit.At present, profile control and water plugging system mainly contains weak gelling system, colloidal dispersed gel, calcium soil-cement system, water glass-calcium chloride precipitation system, the crosslinked water blockoff system of polymerization in situ and pre-crosslinking swell particle.Wherein pre-crosslinking swell particle adopts that ground is synthetic, oven dry, pulverizing and screening be prepared from, and has effectively avoided the deficiencies such as underground not plastic, temperature resistant antisalt poor performance; The particle diameter range of choice of pre-crosslinking swell particle is wide, and all there is to good adaptability in the serious duct of nonuniformity and pervious course; Particle water-swelling flexible reinforced shows the characteristic of " amoeba " in the migration of porous medium, expands the sphere of action of profile control.Therefore, pre-crosslinking swell particle is widely used in the profile control of high temperature and high salt, high moisture, macropore oil reservoir.But the precrosslink particle taking acrylamide as host exists under fast, low mineralization of water-swelling time speed swollen, shutoff immediate vicinity of wellbore causes infusion pressure large, aging dehydration under the increase of expansion later stage fragility, high temperature and high salt, flexible deficiency, fluid diversion ability die down, and make profile control effect not obvious.The reason of searching to the bottom is N, the cross-linking reagent that N methylene-bisacrylamide (NMBA), polyvinyl alcohol (PEG) are representative is linear bifunctional monomer, form random two dimension (plane) network structure with main in the crosslinked process of acrylamide (AM), have obvious orientation and on the third dimension (solid) space, have the defect of network structure.Obtaining pre-crosslinking swell particle deep flooding fluid under the wide salinity scope of high temperature turns to, improving water driving technology must be from the three-dimensional net structure of design precrosslink particle, really realizes particle and under reservoir media, delays the overall targets such as swollen property, Gao Suoshui, obdurability.
Since coming out the eighties in 20th century, hyperbranched polymer is because the end group that has the highly branched unique molecular structure of 3 D stereo structure and can carry out in a large number finishing and modification becomes polymer science and the most active branch of engineering field.Hyperbranched polymer be described as after linear polymer, cross-linked polymer and branched polymer the 4th generation high molecular polymer, and show unique application prospect in fields such as slow releasing pharmaceutical carrier, information storage material, effective catalyst, nonlinear optical material, nano material, sewage disposal, separatory membrane, rheology modifier.Start hyperbranched polymer the earliest as research, polyamide-amide (PAMAM) is due to synthetic raw material (polyamine, methyl acrylate) commercialization, technique are simple, molecular structure strictly controlled, productive rate is high, whole generation upper end-blocking amido and half generation upper end-blocking the easy modification of ester group, be to study one of ripe, the most deep hyperbranched polymer.At present, the application of the PAMAM of process finishing and modification on oil field makes first appearance, as Chinese invention patent " a kind of Shearing Resistant Polymer and preparation method thereof " (patent No. ZL201210117149), the polymkeric substance that adopts maleic anhydride modified PAMAM skeleton monomer and acrylamide, vinylformic acid and dimethyl-allyl-N-alkyl ammomium chloride to prepare, shows good shear resistant and temperature resistant antisalt performance; The PAMAM of epoxy alkyl modification shows good interfacial activity, the dehydration rate of water-in-oil-type crude oil emulsion is exceeded to the post etc. that continues in 90%(week, the synthetic and performance of polymeric amide one amine Starlike polyether crude oil demulsifier, Speciality Petrochemicals, 2008,25 (5): 5-8); It is good flocculation agent that cationic monomer MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) carries out hyperbranched polymer prepared by terminal groups modification to PAMAM, can be used for the processing (Liu Lixin etc. of oilfield sewage, cation-modified and the flocculating property of over-branched polyamidoamine (PAMAM), chemical science and technology, 2011,19(1): 1-4).Therefore, the present invention obtains the hyperbranched functional large monomer of polymerisable polyfunctional group (two key) to PAMAM end group surface modification, the hyperbranched profile control particle that adopts free radical copolymerization method to prepare with acrylamide and temperature resistant antisalt monomer again, there is high-intensity 3 D stereo network structure, under reservoir condition, its slow swelling capacity, lock aqueous nature, temperature resistant antisalt and flexility organic unity, reach the effect of deep profile controlling.
Summary of the invention
The object of the present invention is to provide a kind of hyperbranched slow swollen property profile control particle, this profile control particle forms the network structure of 3 D stereo taking hyperbranched skeleton unit as core, water-swelling process is slow, can effectively advance to oil deposit deep part, after water-swelling, form the hydrogel of high strength, obdurability, shutoff high permeability formation, impels fluid diversion, has overcome the deficiency of pre existing cross-linked particles in deep profile controlling.
Another object of the present invention is also to provide the preparation method of above-mentioned hyperbranched slow swollen property profile control particle, and the method principle is reliable, easy and simple to handle, and the hyperbranched slow swelling property profile control particle of preparation, can be used for 60～120 DEG C of temperature, salinity 2 × 10
4～20 × 10
4the oil reservoir deep profile controlling of mg/L, has broad application prospects.
For reaching above technical purpose, the invention provides following technical scheme.
A kind of hyperbranched slow swollen property profile control particle, functionalization skeleton monomer (PAMAMM) and acrylamide (AM) monomer, temperature resistant antisalt monomer, taking ammonium persulphate or azo two NSC 18620 (V50) as initiator, the hydrogel that adopts free radical copolymerization method to prepare, forms through drying, pulverize, sieving.
Described functionalization skeleton monomer is to adopt methyl methacrylate (MMA) to carry out terminal groups modification to polyamide-amide (PAMAM), and the functionalization skeleton monomer of the progressively polymerization forming.
Described temperature resistant antisalt monomer is NVP (NVP), 2-acrylamide-2-methylpro panesulfonic acid sodium (AMPS-Na) or sodium vinyl sulfonate (SAS).
The present invention is synthesis of super branched skeleton monomer PAMAM(Tomalia et al.Dendrimers with hydrophobic cores and the formation of supramolecular dendrimer-surfactant assemblies first, Langmuir, 1997,13 (12): 3136-3141), adopt methyl methacrylate to carry out terminal groups modification to PAMAM and form the progressively functionalization skeleton monomer PAMAMM of polymerization.
It is as follows that PAMAM terminal groups modification obtains the reaction mechanism of functionalization skeleton monomer PAMAMM:
Adopt free radical copolymerization method with acrylamide and temperature resistant antisalt monomer on this basis, thereby prepare hyperbranched profile control particle.
The preparation method of described hyperbranched slow swollen property profile control particle, comprises the following steps successively:
(1) prepare functionalization skeleton monomer: 2.65g methyl methacrylate (MMA) 15g dimethyl formamide (DMF) dilution is formed to A solution, again 5.45g polyamide-amide (PAMAM) is dissolved in to formation B solution in 25g dimethyl formamide (DMF), then under cooling bath condition, A solution is dropwise added in B solution, underpressure distillation is except the methyl alcohol generating in dereaction, reaction continues 12h, by acetone wash products repeatedly, oven drying at low temperature obtains yellow solid and is functionalization skeleton monomer (PAMAMM);
(2) prepare hyperbranched slow swollen property profile control particle: by acrylamide 20～22.5g, temperature resistant antisalt monomer 4.2～4.5g, functionalization skeleton monomer 0.03～0.035g, deionized water 75～85g adds in there-necked flask, and sodium hydroxide solution regulates pH=5～7, logical N
2after 30min, add 0.055g ammonium persulphate or 0.025g azo two NSC 18620 as initiator, heat up subsequently, at 50～55 DEG C, react 4～6h, obtain translucent hydrogel, through drying, pulverize, sieving, obtain the profile control particle of different-grain diameter.
Profile control particle of the present invention forms the network structure of 3 D stereo taking hyperbranched skeleton unit as core, compound with regular structure, water-swelling process is slow, can effectively advance to oil deposit deep part, after water-swelling, form the hydrogel of high strength, obdurability, shutoff high permeability formation, impel fluid diversion, be applicable to reservoir condition and be temperature 60 C～120 DEG C, salinity 2 × 10
4mg/L～20 × 10
4the oil reservoir deep profile controlling of mg/L, has overcome the crosslinked profile control particle water suction of pre existing speed swollen, and shutoff immediate vicinity of wellbore expands that later stage fragility increases, aging dehydration under high temperature and high salt, deep flooding fluid steering capability is poor wait not enough.
Compared with prior art, beneficial effect of the present invention is as follows:
1. the density of profile control particle is almost suitable with the density of clear water, and suspension is good, is beneficial to infusion;
2. hyperbranched particle has high-intensity 3 D stereo network structure, compound with regular structure, water-swelling process is slow, can effectively migrate to oil deposit deep part, after water suction, water molecules and hyperbranched amide group form hydrogen bond and are strapped in the cavity of 3 D stereo network structure, form the hydrogel particle of high strength, obdurability;
3. hyperbranched particle effective shutoff high permeability formation under the reservoir temperature of wide region, salinity condition, impels fluid diversion, starts Middle-Low Permeability Reservoirs, reaches the ability that increases oil control water;
4. principle of design is reliable, and method is easy, Yi Hang.
Brief description of the drawings
Fig. 1 is that the hyperbranched slow swollen property particle deep profile controlling of the present invention impels fluid diversion schematic diagram.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further described.
One, the preparation of hyperbranched slow swollen property profile control particle
Embodiment 1
Take PAMAM5.45g and put into beaker, add 25gDMF stirring and dissolving, after treating that PAMAM dissolves completely, solution is transferred in the 250ml three-necked bottle that is equipped with decompression Rotary Evaporators, agitator and cooling bath; Pipette 2.65gMMA and put into beaker, add 15gDMF dilution, solution is transferred in constant pressure funnel; Slowly drip MMA solution to filling in the three-necked bottle of PAMAM solution, start agitator and decompression Rotary Evaporators (it is 0.5 normal atmosphere that vacuum tightness is set) simultaneously, except the methyl alcohol generating in dereaction, whole process is carried out under cooling bath condition, continues 12h; Acetone is cleaning reaction product repeatedly, and oven drying at low temperature obtains yellow solid and is functionalization skeleton monomer PAMAMM.
Take 21.5gAM, temperature resistant antisalt monomer 4.25g, PAMAMM0.0312g, is dissolved in 75g deionized water.Sodium hydroxide solution is transferred in there-necked flask after regulating pH=6, logical N
2after 30min, add 0.055g ammonium persulphate or 0.025gV50, heat up subsequently, at 50～55 DEG C, react 4～6h, obtain translucent hydrogel, through drying, pulverize, sieving, obtain the profile control particle of different-grain diameter.
Referring to Fig. 1, this slow swollen property profile control particle forms the network structure of 3 D stereo taking hyperbranched skeleton unit as core, compound with regular structure, and in the process of injection oil reservoir, particle preferentially enters high aquifer formation and is dispersion state that (Fig. 1 is a); Enter imbibition in the process of migration behind stratum, because granuloplastic three-dimensional net structure is regular, water-swelling process is slow, and under lower injection pressure, expanded granular advances to oil deposit deep part in the mode of " amoeba " that (Fig. 1 b); After water-swelling, water molecules and hyperbranched amide group form hydrogen bond and are strapped in the cavity of 3 D stereo network structure, form the hydrogel of high strength, obdurability, and shutoff high permeability formation, impels fluid diversion, and (Fig. 1 c) to adjust intake profile.
Two, the performance measurement of hyperbranched slow swollen property profile control particle
(1) expansion character evaluation
Experiment takes 0.250～0.255g and is designated as W
09 parts of precrosslink particles, are divided into 3 parts, are placed in and fill Dagang Oilfield king 44 injected waters (salinity 25120mg/L, divalent ion Ca
2+, Mg
2+concentration 75mg/L), long celebrating oilfield injection water (salinity 112147mg/L, divalent ion Ca
2+, Mg
2+concentration 1050mg/L), Xi Daliya local water (salinity 191036mg/L, divalent ion Ca
2+, Mg
2+concentration 11324mg/L) wide-mouth vial in, sealing, is put in 60 DEG C, 90 DEG C, 120 DEG C constant temperature ovens, regularly takes out, and measures the water-swelling quality W of particle
t, according to formula S
f=(W
t-W
0)/W
0, obtain the water-swelling multiple S of particle
f, experimental result is as shown in table 1.
The hyperbranched slow swollen property particle water-swelling experiment of table 1
As known from Table 1, at 60～120 DEG C, 25000mg/L～200000mg/L condition, hyperbranched particle imbibition is slow, illustrates in on-the-spot injection process, and less injection pressure just can effectively enter deep oil reservoir; 60 DEG C, 100 DEG C conditions, hyperbranched gel particle reaches the maximum value of expansion multiple substantially at 30d, in the investigation process in later stage, do not change; 120 DEG C of conditions, hyperbranched gel particle is suitable at the expansion multiple of 30d and 20d, 30 times of left and right, in the weathering process in later stage, there is degraded and dehydration in part water-absorption particle, and expansion multiple decreases, and the expansion multiple after 60d still reaches 25 times.Water-swelling is tested and is shown, hyperbranched gel particle has good hot salt-stable, and after imbibition, hyperbranched 3 D stereo network structure has good " lock water " ability.
(2) toughness is measured
With three class oil fields inject (stratum) water by 30～45 orders not water-absorption particle be mixed with the suspension of mass concentration 0.25%, under 100 DEG C of conditions after water-swelling 15d, by in 40ml suspension filling sieve webmaster, and make it pass through 3 layer of 20 object screen cloth, survey corresponding pressure reduction △ p
1and flow Q (MPa)
1(ml), the 40ml suspension of outflow is reloaded to intermediate receptacle, repeat to inject screen casing, mensuration system flows through the pressure reduction △ p of screen cloth for the second time
1and flow Q (MPa)
1(ml), according to formula
calculate the tough factor of precrosslink particle.Result is as shown in table 2.
The hyperbranched slow swollen property particle of table 2 is at the tough factor of 100 DEG C of aging 15d
| Water quality type | King 44 | Long celebrating oil field | Xi Daliya |
| Tough factor f tay | 0.83 | 0.91 | 0.95 |
As known from Table 2, f
taylarger, toughness is higher, lower salinity (king's 44 injected waters), particle coefficient turgidity is high, and toughness declines to some extent, under the degree of high ore deposit (long celebrating oil field stratum water, Xi Daliya injected water), hyperbranched grain expansion is slow, slow swollen performance is obvious, shows unique anti-salt property, and the tough factor of aging 15d is more than 0.9.
(3) residual resistance factor and sealing ratiod
With Dagang Oilfield king 44 injected waters by 30～45 orders not water-absorption particle be mixed with the suspension of mass concentration 0.25%, in 100 DEG C of constant temperature ovens, place after 2 days, particle water-swelling is also dispersed in solution, and constant voltage constant speed pump (model ES-V) is surveyed rate of permeation (K with the different water of 1ml/min flow velocity displacement
b) artificial sand rock rock core (2.5cm × 7.1cm), (△ is p) after pressure-stabilisation, to record displacement pressure
pand volumetric flow rate q (MPa)
p(ml), count particles enters the rate of permeation K after rock core
f, according to formula
and η=(1-K
f/ K
bthe residual resistance factor RRF of) × 100% count particles and sealing ratiod η.Result is as shown in table 3.
Residual resistance factor and the sealing ratiod of the hyperbranched slow swollen property particle of table 3
As known from Table 3, hyperbranched profile control particle has very strong migration ability and shut-off capacity, and sealing ratiod is up to more than 91%.This is main because particle preferentially enters macropore in the process of migration, water suction deliquescing, toughness increase, can in porous medium, migrate forward in the mode of " amoeba ", enter earth formation deep, shutoff high permeability formation, impel fluid diversion, adjust intake profile, start low-permeability layer.
Claims (2)
1. a hyperbranched slow swollen property profile control particle, it is characterized in that, this profile control particle is functionalization skeleton monomer and acrylamide monomer, temperature resistant antisalt monomer, taking ammonium persulphate or azo two NSC 18620 as initiator, the hydrogel that adopts free radical copolymerization method to prepare, forms through drying, pulverize, sieving; Described functionalization skeleton monomer is to adopt methyl methacrylate to carry out terminal groups modification to polyamide-amide, and the functionalization skeleton monomer of the progressively polymerization forming; Described temperature resistant antisalt monomer is NVP, 2-acrylamide-2-methylpro panesulfonic acid sodium or sodium vinyl sulfonate.
2. the preparation method of hyperbranched slow swollen property profile control particle as claimed in claim 1, comprises the following steps successively:
(1) prepare functionalization skeleton monomer: the dilution of 2.65g methyl methacrylate 15g dimethyl formamide is formed to A solution, again 5.45g polyamide-amide is dissolved in and in 25g dimethyl formamide, forms B solution, then under cooling bath condition, A solution is dropwise added in B solution, underpressure distillation is except the methyl alcohol generating in dereaction, reaction continues 12h, by acetone wash products repeatedly, oven drying at low temperature obtains yellow solid and is functionalization skeleton monomer;
(2) prepare hyperbranched slow swollen property profile control particle: by acrylamide 20～22.5g, temperature resistant antisalt monomer 4.2～4.5g, functionalization skeleton monomer 0.03～0.035g, deionized water 75～85g adds in there-necked flask, sodium hydroxide solution regulates pH=5～7, logical N
2after 30min, add ammonium persulphate or azo two NSC 18620 as initiator, heat up subsequently, at 50～55 DEG C, react 4～6h, obtain translucent hydrogel, through drying, pulverize, sieving, obtain the profile control particle of different-grain diameter.
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| CN105368417A (en) * | 2015-12-11 | 2016-03-02 | 西安奥力石油工程有限责任公司 | High-strength supramolecular crack rapid blocking agent |
| CN108504342A (en) * | 2018-04-09 | 2018-09-07 | 王建东 | A kind of preparation method of water shutoff agent |
| CN110885433B (en) * | 2019-05-24 | 2022-07-19 | 武汉金发科技有限公司 | Hyperbranched polyester and synthesis method thereof, and thermoplastic resin composition and preparation method thereof |
| CN112322268B (en) * | 2020-11-02 | 2023-06-30 | 中国石油天然气股份有限公司 | Stretchable slow-expansion acrylic resin and preparation process and application thereof |
| CN114478935A (en) * | 2020-11-12 | 2022-05-13 | 中国石油化工股份有限公司 | Temperature-resistant salt-resistant shape memory material particle system and preparation method thereof |
| CN114437689B (en) * | 2022-01-21 | 2023-05-16 | 中海石油(中国)有限公司 | High-strength double-network micro-nano particle composite gel for plugging large pore channels of oil reservoirs and preparation method thereof |
| CN114790295B (en) * | 2022-06-02 | 2023-04-11 | 东北石油大学 | Hydrogel and preparation method and application thereof |
| CN116004206B (en) * | 2023-01-31 | 2023-12-15 | 中海石油(中国)有限公司 | Novel deep profile control gel based on tree-core polymer and preparation method and application thereof |
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