CN102504793B - Core-shell polymer microsphere profiling/flooding agent and preparation method thereof - Google Patents
Core-shell polymer microsphere profiling/flooding agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a core-shell polymer microsphere profile control and oil displacement agent for oil reservoir profile control and displacement and increase of water drive recovery factor and a preparation method of the core-shell polymer microsphere profile control and oil displacement agent, which can solve the technical problems of difficulty in injection and poor temperature resistance and salt resistance. The invention adopts a technical scheme as follows: the profile control and oil displacement agent is made from the following raw materials in parts: 15 to 20 of a hydrophobic monomer (such as styrene or a styrene derivative or an acrylate ester), 2 to 10 of a hydrophilic monomer (such as acrylic acid or an acrylate salt or acrylamide), 60 to 85 of deionized water, divinylbenzene as core-phase cross-linking agent, N,N'-methylene-bis-acrylamide as shell-phase cross-linking agent, and a sulfate salt as initiator. The method comprises the following steps of: adding the shell-phase cross-linking agent and acrylic acid into a three-necked flask with water, adding the core-phase cross-linking agent and styrene after dissolving completely, introducing nitrogen gas (30 DEG C to 75 DEG C), adding the initiator, and allowing reactions to take place for 6 to 8 hours under stirring, to obtain the polymer microsphere profile control and oil displacement agent. The polymer microsphere profile control and oil displacement agent is suitable for middle/low-permeability oil reservoirs, can be applied to high-permeability oil reservoirs in combination with other profile control agents, and can greatly increase the crude oil recovery ratio.
Description
Technical field
The present invention relates to hud typed polymer microballoon adjusting driving agnet and the preparation method of a kind of transfer drive for petroleum industry oil field high temperature and high salt oil deposit, raising waterflood recovery efficiency factor.
Background technology
The water-retaining capacity of most permeable zone or high permeability zone is strong after the water drive, and oil displacement efficiency is high, and a little less than the water-retaining capacity of low permeability layer or hyposmosis band, oily unstart or development degree are very low.Improve recovery ratio, need improve mobility ratio, improve the sweep efficiency of water.Adopt and inject suitable amendment, adjust the intake profile of high low permeability layer or height permeable belt, the water-retaining capacity of most permeable zone or high permeability zone is reduced, the water-retaining capacity of low permeability layer or hyposmosis band strengthens or obtains to a certain degree starting, make follow-up water enter in a large number low permeability layer or hyposmosis band, oil displacement efficiency increases, and reaches the section adjustment, realizes the purpose of steady oil control water.For 90～130 ℃ of high temperature 5～10 * 10
4The oil reservoir of the high salt of mg/L, the use of conventional transfer drive material is restricted, thereby needs novel heat and salinity tolerance transfer drive material.
The particle adjusting driving agnet mainly is to adopt water-soluble poly legal at present, with the water-absorbing material of hydrophilic monomer copolymerzation with cross-linking preparation and the composite absorbent material of the compound preparation of adding inorganic materials, is prepared into gel particle through technological processs such as granulation, oven dry, pulverizing, screenings.This two classes material granule is larger, be adapted at higher infiltration oil reservoir transfer drive, and injection is relatively poor in middle low-permeability oil pool, is difficult to effective application.And the former high temperature and high salinity situation stability inferior is relatively poor, and the latter is difficult for migrating to earth formation deep because the combined strength bination increase causes flexible the reduction, is difficult to reach the effect of deep transfer drive.
Summary of the invention
The objective of the invention is: become glue and HPAM in the abominable bad situation of reservoir condition stability inferior for weak gel difficulty under abominable reservoir condition, preparation is injected difficulty, can't realize that slug is processed, heat-resistant salt-resistant is poor and conventional gel particle adjusting driving agnet is difficult to just really arrive the technical barriers such as earth formation deep that the spy provides a kind of hud typed polymer microballoon adjusting driving agnet and preparation method.
In order to achieve the above object, the present invention is by the following technical solutions: a kind of hud typed polymer microballoon adjusting driving agnet, it is characterized in that: this adjusting driving agnet content raw materials used and each component is, the unit of its quality is gram or kilogram, hydrophobic monomer 15～20th, vinylbenzene or alpha-methyl styrene or a kind of in styryl phenyl or the acrylate; Hydrophilic monomer is 2～10th, mixes with the derivative of acrylamide or acrylamide or one or both monomers of vinylformic acid or acrylate or 2-acrylamide-2-methyl propane sulfonic salt or dimethyl diallyl ammonium chloride; Deionized water 60～85; Shell phase linking agent is that linking agent 1 is 0.00005～0.00015th, uses N, N '-methylene-bisacrylamide; The nuclear phase linking agent is that linking agent 2 is 0.00005～0.00015th, uses Vinylstyrene; Initiator 0.01～1st is used a kind of of ammonium persulphate or Potassium Persulphate or hydrogen peroxide-ferrous sulfate or Potassium Persulphate-sodium bisulfite.
The polymer microballoon adjusting driving agnet is to be that the first monomer is as the nuclear phase material cell by hydrophobic monomer vinylbenzene, alpha-methyl styrene, to styryl phenyl, take hydrophilic monomer acrylamide, vinylformic acid as the second monomer as shell phase material unit, with N, N ＇-methylene-bisacrylamide is that shell phase linking agent is linking agent 1, be linking agent 2 take Vinylstyrene as the nuclear phase linking agent, under initiator and suitable temperature, in aqueous media, carry out emulsifier-free emulsion polymerization and make.
A kind of preparation method of hud typed polymer microballoon adjusting driving agnet, it is characterized in that: first in the three-necked bottle that 60～85g deionized water is housed, add 0.00005～0.00015g linking agent, 1 N, the mixture of N '-methylene-bisacrylamide and 2～10g acrylamide or its derivative or vinylformic acid or acrylate, fully after the dissolving, add again 0.00005～0.00015g linking agent, 2 Vinylstyrenes and 10～15g vinylbenzene or styrene derivatives, be warmed up to 30～75 ℃, logical nitrogen protection, add initiator 0.01～1g, stirring velocity is controlled at 300～400rpm, reaction 6～8h, make hud typed polymer emulsion, obtain the polymer microballoon adjusting driving agnet solution of median size 300～800nm; This polymer emulsion does not generally need to separate, and being diluted to needs to be directly used in transfer drive under the concentration.
Polymer emulsion is by centrifugal break milk separation, absolute ethanol washing is purified three times, get the hud typed polymer microballoon of clean product after the vacuum-drying, the strength ratio of infrared analysis hydrophilic group and hydrophobic group stretching vibration peak can illustrate the ratio of the quantity of hydrophilic monomeric units and hydrophobic monomer unit in the copolymerization microsphere qualitatively, to confirm to have nucleocapsid structure.In temperature was 90～130 ℃ of scopes, salinity was 10 * 10
4Mg/L NaCl+5 * 10
3Mg/L CaCl
2Measure rate of expansion in the situation.Stirring velocity is different, can obtain the gel particle of different-grain diameter, can satisfy middle low penetrability reservoir.
Above-mentioned hydrophobic monomer refers to vinylbenzene or alpha-methyl styrene or a kind of to styryl phenyl; Above-mentioned hydrophilic monomer has comprised anionic monomer, nonionic monomers and cationic monomer.Its anionic monomer vinylformic acid, sodium acrylate, potassium acrylate, ammonium acrylate, 2-acrylamide-2-methyl propane sulfonic sodium etc.; Nonionic monomers is a kind of with acrylamide or N-Methacrylamide or N-basic alkene acid amides; Cationic hydrophilic monomer dimethyl diallyl ammonium chloride or 2-MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride; These unsaturated monomers are to mix with a kind of monomer or two kinds of monomers to use, if use two kinds of its nonionic monomers of monomer and the ratio of anionic monomer or cationic monomer to be 15.0:5.0～19.5:0. 5.
The migration rule of polymer microballoon in the stratum: because heat and salinity tolerance core-shell polymer microdilatancy ball can be migrated in the reservoir rock hole, the stacking energy macropore plugging of the microdilatancy of microballoon (2～10 times) energy shutoff low permeability layer and a plurality of microballoons streams water, pressure difference of blocking is elevated to a certain degree simultaneously, require microballoon generation recoverable deformation, continue to the oil reservoir deep migration by venturi, it is a kind of novel step by step deep profile controlling oil-displacing agent.Polymer microballoon heatproof, anti-salinity are very competent, plugging strength is high, and microspherulite diameter is little, with water for carrying medium, do not need special injection device, do not need waterflood-transmission line is transformed, be applicable to high water cut oil field, block oilfield, offshore oilfield, can improve oil recovery rate more than 10%.
Experiment shows that this polymer microballoon adopts double crosslinker to improve temperature resistance, and the introducing of phenyl ring has improved temperature resistance and salt resistance, can make temperature resistance reach 130 ℃, and substantially is not subjected to the impact of salinity.Nuclear phase contains phenyl ring rigidity hydrophobic grouping, does not absorb water, and is in vitreous state under normal temperature or low temperature, but at high temperature be to be in elastomeric state under the reservoir temperature, and shell contains hydrophilic radical mutually, is in the microdilatancy state after the suction, and the comprehensive action of the two is so that microballoon has good elastic deformability.
Compared with prior art, the present invention has following beneficial effect: (1) the present invention adopts emulsifier-free emulsion polymerization to prepare the polymer microballoon adjusting driving agnet, and the impact that chemical reaction has been avoided reservoir condition does not occur under reservoir condition; (2) this polymer microballoon adjusting driving agnet injection is good, can migrate at earth formation deep, can be used for the transfer drive of high temperature and high salt oil deposit, and use temperature can reach 130 ℃, uses salinity unrestricted.(3) in this technology implementation process, adjust microdilatancy ball intensity and size distribution by the construction monitoring process, can avoid because of the unclear drawback of bringing of stratum macropore understanding.(4) adjusting driving agnet that the invention solves present field use becomes the defective of the difficult control of adhesive tape part, narrow application range, complicated construction technique, and the relative ordinary gel particle of injection is good, LOW PERMEABILITY RESERVOIR in being fit to.If unite use with conventional gel particle, also be fit to high permeability reservoir.
Embodiment
The invention will be further described below in conjunction with specific examples, but the present invention is not limited to this.
Example one: in the three-necked bottle that the 78g deionized water is housed, add linking agent 1 N; N ＇-methylene-bisacrylamide 0.00010g and acrylamide 2g; after having dissolved, add again linking agent 2 Vinylstyrene 0.00005g and vinylbenzene 20g, be warmed up to 70 ℃; logical nitrogen protection; add initiator ammonium persulfate 0.5g, stir speed (S.S.) is controlled at 350rpm, reaction 7h; get core-shell emulsion type product, adopting laser particle analyzer to record particle diameter is 347nm.Polymer emulsion is by centrifugal break milk separation, absolute ethanol washing is purified three times, after the vacuum-drying product, infrared analysis can get that the strength ratio of acrylamide unit and styrene units is 0.62 in the copolymerization microsphere, and the ratio of the quantity of Unit two in the copolymerization microsphere can be described qualitatively.Be 110 ℃ in temperature, salinity is 10 * 10
4Mg/L NaCl+5 * 10
3Measuring rate of expansion in the mg/L CaCl2 situation is 2.6g/g.
Example two: in the three-necked bottle that the 76g deionized water is housed, add linking agent 1 N; N ＇-methylene-bisacrylamide 0.00010g and acrylamide 5g; after having dissolved, add again linking agent 2 Vinylstyrene 0.00005g and vinylbenzene 19g, be warmed up to 70 ℃; one straight-through nitrogen protection; add initiator ammonium persulfate 0.2g, stir speed (S.S.) is controlled at 350rpm, reaction 7h; get core-shell emulsion type product, adopting laser particle analyzer to record particle diameter is 330nm.Polymer emulsion is by centrifugal break milk separation, absolute ethanol washing is purified three times, after the vacuum-drying product, infrared analysis can get sodium acrylate unit in the copolymerization microsphere and be 0.79 to the strength ratio of styryl phenyl unit, and the ratio of the quantity of Unit two in the copolymerization microsphere can be described qualitatively.Be 130 ℃ in temperature, salinity is 10 * 10
4Mg/LNaCl+5 * 10
3Mg/LCaCl
2Measuring rate of expansion in the situation is 4.5g/g.
Example three: in the three-necked bottle that the 78g deionized water is housed, add linking agent 1 N; N ＇-methylene-bisacrylamide 0.00005g and 2-acrylamide-2-methyl propane sulfonic sodium 4g; after having dissolved, add again linking agent 2 Vinylstyrene 0.00005g and vinylbenzene 18g, be warmed up to 70 ℃; one straight-through nitrogen protection; add initiator ammonium persulfate 0.1g, stir speed (S.S.) is controlled at 350rpm, reaction 7h; get core-shell emulsion type product, adopting laser particle analyzer to record particle diameter is 315nm.Polymer emulsion is by centrifugal break milk separation, absolute ethanol washing is purified three times, get product after the vacuum-drying, infrared analysis can get that the strength ratio of 2-acrylamide-2-methyl propane sulfonic sodium unit and propyl benzene ethylene unit is 0.71 in the copolymerization microsphere, and the ratio of the quantity of Unit two in the copolymerization microsphere can be described qualitatively.Be 130 ℃ in temperature, salinity is 10 * 10
4Mg/L NaCl+5 * 10
3Mg/L CaCl
2Measure rate of expansion 8.6g/g in the situation.
Example four: in the three-necked bottle that the 75g deionized water is housed, add linking agent 1 N; N ＇-methylene-bisacrylamide 0.00005g and N methacrylamide 10g; after the dissolving, add linking agent 2 Vinylstyrene 0.00005g and alpha-methyl styrene 15g fully, be warmed up to 70 ℃; logical nitrogen protection; add initiator ammonium persulfate 0.5g, stir speed (S.S.) is controlled at 300rpm, reaction 7h; get core-shell emulsion type product, adopting laser particle analyzer to record particle diameter is 806nm.Polymer emulsion is by centrifugal break milk separation, absolute ethanol washing is purified three times, get product after the vacuum-drying, infrared analysis can get that the strength ratio of N methacrylamide unit and alpha-methyl styrene unit is 0.88 in the copolymerization microsphere, and the ratio of the quantity of Unit two in the copolymerization microsphere can be described qualitatively.Be 90 ℃ in temperature, salinity is 10 * 10
4Mg/L NaCl+5 * 10
3Mg/L CaCl
2Measuring rate of expansion in the situation is 4.3g/g.
Example five: in the three-necked bottle that the 70g deionized water is housed, add linking agent 1 N; N ＇-methylene-bisacrylamide 0.00005g and sodium acrylate 10g; after the dissolving, add again linking agent 2 Vinylstyrene 0.00005g and vinylbenzene 20g fully, be warmed up to 70 ℃; one straight-through nitrogen protection; add initiator ammonium persulfate 0.5g, stir speed (S.S.) is controlled at 350rpm, reaction 7h; get core-shell emulsion type product, adopting laser particle analyzer to record particle diameter is 626nm.Polymer emulsion is by centrifugal break milk separation, and absolute ethanol washing is purified three times, after the vacuum-drying product, infraredly record that the strength ratio of sodium acrylate unit and styrene units is 0.84 in the copolymerization microsphere, the ratio of quantity can be described qualitatively.Be 130 ℃ in temperature, salinity is 10 * 10
4Mg/L NaCl+5 * 10
3Mg/L CaCl
2Measuring rate of expansion in the situation is 7.5g/g.
Example six: in the three-necked bottle that the 83g deionized water is housed, add linking agent 1 N; the dimethyl diallyl ammonium chloride 0.2g of N ＇-methylene-bisacrylamide 0.00005 and acrylamide 1.8g; after the dissolving, the vinylbenzene 15g of linking agent 2 Vinylstyrene 0.00005g is warmed up to 30 ℃ fully; logical nitrogen protection; add respectively initiator ammonium persulfate and sodium bisulfite 0.01g, stir speed (S.S.) is controlled at 300rpm, reaction 7h; get core-shell emulsion type product, adopting laser particle analyzer to record particle diameter is 305nm.Polymer emulsion is by centrifugal break milk separation, absolute ethanol washing is purified three times, after the vacuum-drying product, infraredly record that the strength ratio of acrylamide and dimethyl diallyl ammonium chloride Unit two and styrene units is 0.65 in the copolymerization microsphere, the ratio of its quantity is described qualitatively.Be 130 ℃ in temperature, salinity is 10 * 10
4Mg/L NaCl+5 * 10
3Mg/L CaCl
2Measuring rate of expansion in the situation is 2.3g/g.
Claims (2)
1. hud typed polymer microballoon adjusting driving agnet, it is characterized in that: this adjusting driving agnet content raw materials used and each component is, the unit of its quality is gram or kilogram, hydrophobic monomer 15～20th, vinylbenzene or alpha-methyl styrene or a kind of in styryl phenyl or the acrylate; Hydrophilic monomer is 2～10th, with one or both monomers mixing of acrylamide or vinylformic acid or acrylate or 2-acrylamide-2-methyl propane sulfonic salt or dimethyl diallyl ammonium chloride; Deionized water 60～85; Shell phase linking agent is that linking agent 1 is 0.00005～0.00015th, uses N, N '-methylene-bisacrylamide; The nuclear phase linking agent is that linking agent 2 is 0.00005～0.00015th, uses Vinylstyrene; Initiator 0.01～1st is used a kind of of ammonium persulphate or Potassium Persulphate or hydrogen peroxide-ferrous sulfate or Potassium Persulphate-sodium bisulfite.
2. preparation method of polymer microballoon adjusting driving agnet as claimed in claim 1, it is characterized in that: first in the three-necked bottle that 60～85g deionized water is housed, add 0.00005～0.00015g linking agent 1N, N '-methylene-bisacrylamide and 2～10g acrylamide or vinylformic acid or acrylate or 2-acrylamide-2-methyl propane sulfonic salt, or one or both monomers of dimethyl diallyl ammonium chloride mix, fully after the dissolving, add again 0.00005～0.00015g linking agent, 2 Vinylstyrenes and 15～20g vinylbenzene or alpha-methyl styrene, or to styryl phenyl, or a kind of in the acrylate, be warmed up to 30～75 ℃, logical nitrogen protection, add initiator 0.01～1g, stirring velocity is controlled at 300～400rpm, reaction 6～8h, make hud typed polymer emulsion, obtain the polymer microballoon adjusting driving agnet solution of median size 300～800nm; This polymer emulsion does not need to separate, and being diluted to needs to be directly used in transfer drive under the concentration.
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