CN101759838A - Preparation method of profile control and oil displacement system of polyacrylamide nanometer microsphere with low interfacial tension - Google Patents
Preparation method of profile control and oil displacement system of polyacrylamide nanometer microsphere with low interfacial tension Download PDFInfo
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Abstract
The invention relates to a preparation method of a profile control and oil displacement system of polyacrylamide nanometer microsphere with low interfacial tension, which comprises the steps of: inversely preparing microemulsion with oil phase, combined emulsifying agents and water phase containing crosslinking agents, initiating polyreaction with a redox initiation system used as initiating agents, neutralizing the obtained polyacrylamide nanometer microsphere with alkali, and preparing highly active sulphonate or carboxylate surfactants with the reaction of the alkali and the substance of organic acid in the combined emulsifying agents; the oil water interfacial tension can be greatly reduced by the surfactants. The profile control and oil displacement system is applied to enhancing enhanced recovery ratio, has good effect on enhancing oil cleaning efficiency, and is a novel profile control and oil displacement system with the dual functions of profile control and oil displacement.
Description
Technical field:
The present invention relates to a kind of preparation method of polyacrylamide nanometer microsphere with low transfer drive system.
Background technology:
Current most oil field all is in the high moisture mining phase of waterflooding, the nonuniformity of oil reservoir is serious, current advantage passage prosperity wherein, inject the invalid circulation of water, reservoir coverage is low, causes difficult problems such as the too low and later stage oil reservoir water logging of oil recovery factor, equipment corrosion, sewage disposal load be excessive.In addition, along with increasing day by day of crude oil consumption amount and remaining high of international oil price, the oil reservoir of severe condition such as numerous offshore oilfields, hypotonic, high salinity begins to drop into exploitation, and existing most of profile-controlling and plugging agent and relevant supporting technology are not suitable for this type of oil reservoir.
The polyacrylamide nano microballoon is to be dispersion system with the micro emulsion, is principal monomer with the acrylamide, is being added with the netted polyacrylamide particle for preparing under the condition of little amount of crosslinking agent.After these particles were annotated the stratum, because its water-swelling, volume increased, thereby can stop up the current advantage passage in the stratum, improves the sweep efficiency that injects water.Because just the polyacrylamide nano microspherulite diameter of preparation is little, solution viscosity is low, make the polyacrylamide nano microballoon enter earth formation deep easily and realize the deep transfer drive, therefore mean a great for the water and oil control of old oil reservoir and the waterflooding development effect of raising offshore oilfield, LOW PERMEABILITY RESERVOIR and high salinity oil reservoir.
Conversed phase micro emulsion copolymerization prepares polyacrylamide nanometer microsphere with low need use a large amount of emulsifying agents, generally accounts for more than 10% of system total mass, and a large amount of emulsifying agents of adding make cost significantly improve.Take a broad view of existing document and patent, the emulsifying agent that conversed phase micro emulsion copolymerization uses mostly is the composite emulsifier of lipophilic surfactant Span series and hydrophilic surfactant active Tween series, OP series, and the consumption of Span series accounts for the over half of emulsification system quality.Yet the lipophilicity of Span series of surfactants can make the active variation of water-oil interface, oil water interfacial tension is high, after the polyacrylamide nanometer microsphere with low system being made into aqueous solution injection oil reservoir, the Span series of surfactants can't play the effect that improves displacement efficiency, causes huge waste.
As everyone knows, the research of surfactant flooding in improving recovery ratio is with a long history, and it is remarkable to improve the recovery ratio effect, and wherein low interfacial tension is that the dominant mechanism of surfactant flooding raising recovery ratio also is the important indicator of screening displacing surfactant system.If can in the preparation process of polyacrylamide microsphere system, adopt suitable lipophilic surfactant, and then in the transfer drive application process by suitable processing, the hydrophilic surfactant active who this lipophilic surfactant is converted into can produce low interfacial tension is to bring into play the effect that it improves displacement efficiency, kill two birds with one stone beyond doubt, the synergistic effect of polyacrylamide nanometer microsphere with low and tensio-active agent is made something perfect even more perfect for improving recovery ratio especially in addition.
Summary of the invention:
The objective of the invention is to provide a kind of preparation method of low interfacial tension polyacrylamide nanometer microsphere with low transfer drive system, the particularly employed emulsifying agent that is converted into the low interfacial tension flooding system.
Purpose of the present invention realizes according to the following steps:
1. oil phase and emulsifying agent are stirred evenly with the magnetic stirrer mixing, the oil phase quality accounts for 30%～55% of microemulsion quality, and the emulsifying agent quality accounts for 15%～25% of microemulsion quality, and microemulsion is the homogeneous mixture of oil phase, emulsifying agent and water;
2. in the mixture of above-mentioned oil phase and emulsifying agent, add the water that contains linking agent and oxygenant, water is that monomer mass concentration is the aqueous solution that 40%～70% acrylamide monomers adds linking agent and oxygenant, the water quality accounts for 30%～55% of microemulsion quality, the contained linking agent of aqueous phase is a Vinylstyrene, methylene-bisacrylamide, one or more of Viscoat 295 and polyethyleneglycol diacrylate etc., its content is 0.01%～1.00% of water quality, the contained oxygenant of aqueous phase is a Potassium Persulphate, ammonium persulphate or benzoyl peroxide etc., its content is 0.03%～0.10% of water quality, the reverse micro emulsion that fully stirs transparent or semitransparently;
3. logical N
2After the deoxygenation 10 minutes, in reverse micro emulsion, add the acrylamide triggered class polymerization reaction take place of reductive agent, treat after the peak heat release, continue to react half an hour, obtain the transparent or semitransparent thermodynamically stable transfer drive system that is dispersed with the polyacrylamide nano microballoon, the transmission electron microscope photo shows that microspherulite diameter is less than 150nm.
The employed oil phase of above-mentioned steps is one or more of gasoline, kerosene, diesel oil, white oil, vegetables oil, toluene, hexanaphthene and octane-iso etc.; Emulsifying agent is lipophilic surfactant and hydrophilic surfactant active's a binary, ternary or multicomponent mixture, lipophilic surfactant comprises organic acid substance and other lipophilic surfactants, organic acid substance is wherein selected lauric acid, linolenic acid, mountain Yu acid, oleic acid, stearic acid, naphthenic acid, the oil carboxylic acid, alkylsulphonic acid, alkyl benzene sulphonate (ABS), one or more of carboxylic acids such as mahogany acid and sulfonic acid, other lipophilic surfactants can be from Span series, the Stearinsaeure propylene diester, distearyl acid second diester, select one or more in single oleic acid two sweet esters etc.The hydrophilic surfactant active selects one or more of Tween series and OP series for use; Organic acid composition accounts for 30%～55% of emulsifying agent total mass in the emulsifying agent, and other lipophilic surfactants account for 25%～45% of emulsifying agent total mass, and Tween series or OP series account for 20%～40% of emulsifying agent total mass.Acrylamide monomers can be selected non-ionic type, one or more of cationic, anionic and ampholytic monomer, and wherein nonionic monomers can be selected acrylamide etc. for use; Cationic monomer can be selected dimethyl diallyl ammonium chloride or methylacryoyloxyethyl trimethyl ammonium chloride etc. for use; The anionic monomer can be selected vinylformic acid, methacrylic acid or 2-acrylamido-2 methyl propane sulfonic acid salt etc.; Ampholytic monomer can be selected dimethylaminoethyl acrylate etc. for use.Used linking agent is selected from one or more of Vinylstyrene, methylene-bisacrylamide, Viscoat 295, polyethyleneglycol diacrylate etc., and consumption is 0.01%～1.00% of a water quality.It can be thermal initiation, light-initiated and radiation initiation etc. that polyreaction causes mode, preferably select for use oxidation-reduction trigger system to cause, wherein oxygenant can be selected Potassium Persulphate, ammonium persulphate, benzoyl peroxide etc. for use, and consumption is 0.03%～0.10% of a water quality; The optional iron protochloride of reductive agent, S-WAT, Sulfothiorine, sodium bisulfite, sulfurous gas, sodium formaldehyde sulphoxylate etc., consumption is 0.02%～0.06% of a water quality; The mass ratio of Oxidizing and Reducing Agents is 1: 2～5: 1.Temperature of reaction is 25 ℃～45 ℃.
In prepared polyacrylamide nanometer microsphere with low system and the alkali and after could obtain low interfacial tension or even ultra low interfacial tension (＜10
-3MN/m) characteristic.Employed alkali can be NaOH, Na
2CO
3, NaHCO
3, KOH etc. one or more.
The directly dilute with water dispersion of polyacrylamide nanometer microsphere with low system that the present invention is prepared, then according to the content of organic acid substance in the emulsifying agent, according to the metering of organic bronsted lowry acids and bases bronsted lowry generation neutralization reaction than the quality that calculates required alkali, alkali and microballoon aqueous solution is even, after neutralization reaction is complete, promptly can be applicable to improve the recovery ratio operation.Microspheres prepared system of the present invention is a kind of novel transfer drive system that has profile control and displacement of reservoir oil dual function concurrently.
The invention has the beneficial effects as follows: in prepared polyacrylamide nanometer microsphere with low system and the alkali and after can obtain low interfacial tension or even ultra low interfacial tension characteristic.Organic acid substance in the transfer drive system preparation process in the used emulsifying agent can generate highly active sulfonate or carboxylate surfactant with alkali reaction, it is brought into play deep profile controlling at polyacrylamide nanometer microsphere with low, enlarges on the basis of sweep efficiency effect, can reduce oil water interfacial tension significantly, improve displacement efficiency, finally improve oil recovery factor.Simultaneously, organic acid substance has substituted a large amount of lipophilic surfactants such as Span series, and these tensio-active agents have been avoided waste to improving almost not contribution of displacement efficiency.
Embodiment:
Further specify the present invention below by embodiment.
Embodiment 1:
At first take by weighing the 49.00g white oil and also use the magnetic stirrer mixing by the emulsifying agent that 8.50g lauric acid (LA), 5.10g Span80 and 3.40g Tween80 are re-dubbed, then will be by 13.50g deionized water (H
2O), the aqueous solution of 18.56g acrylamide (AM), 2.28g 2-acrylamido-2 methyl propane sulfonic acid sodium (NaAMPS), 0.01g linking agent polyethyleneglycol diacrylate (PEGDA) and 0.03g oxygenant ammonium persulphate (APS) composition adds wherein, stir be transparent or semitransparent shape to whole system after, it is transferred to the four-hole boiling flask that has stirring rod that places 30 ℃ of waters bath with thermostatic control in advance, logical N
2Deoxygenation 10 minutes adds mass concentration and is 10% S-WAT (SS) aqueous solution 0.20 gram initiated polymerization subsequently when stirring.After the exothermic heat of reaction peak, continued stoichiometric number ten minutes, promptly get the copolymerization nano microsphere system of transparent or semitransparent polyacrylamide and 2-acrylamido-2 methyl propane sulfonic acid sodium, the transmission electron microscope photo shows that microspherulite diameter is less than 150nm.The composition of system sees Table 1.
The composition of table 1 system
| System is formed | White oil | ??LA | ??Span80 | ??Tween80 | ??H 2O | ??AM | ??NaAMPS | ??PEGDA | ??APS | ??SS |
| Quality/g | ??49.00 | ??8.50 | ??5.10 | ??3.40 | ??13.68 | ??18.56 | ??2.28 | ??0.01 | ??0.03 | ??0.02 |
| Massfraction/% | ??48.72 | ??8.45 | ??5.07 | ??3.38 | ??13.60 | ??18.45 | ??2.27 | ??0.01 | ??0.03 | ??0.02 |
The polyacrylamide nanometer microsphere with low system of getting preparation directly is 1.0% microballoon aqueous solution 500g with deionized water dilution preparation polyacrylamide massfraction, adds 0.86 gram NaHCO
3Fully mixing makes wherein LA and NaHCO
3Neutralization reaction is complete, obtains low interfacial tension transfer drive system.
The dynamic interface tension force between interfacial tensimeter mensuration crude oil and the transfer drive system is dripped in the TX-550A type rotation that the present invention adopts Bowing Industry Corp to produce.Crude oil is taken from Shengli Oil Field stake west oil recovery factory's stake 106 wells, and (50 ℃ of viscosity are 1450mPas, ρ=0.93g/cm
-3, the gum asphalt massfraction is 20.54%).Measurement result under 70 ℃ shows that the transfer drive system can be reduced to 10 with the oil water interfacial tension of the western crude oil of stake
-3The order of magnitude.Compare with the oil water interfacial tension (being about 30mN/m) of the western crude oil of stake with the Span80/Tween80 composite emulsifier aqueous solution of equal conditions, it is remarkable that transfer drive system of the present invention reduces the interfacial tension effect, be applied to improve in the recovery ratio operation, will play good raising displacement efficiency and the final effect that improves recovery ratio.
Embodiment 2: at first takes by weighing 84.00g diesel oil and also uses the magnetic stirrer mixing by the emulsifying agent that 14.76g oleic acid (OA), 11.16g Span20 and 10.08gOP10 are re-dubbed, and then will be by 43.87g deionized water (H
2O), the aqueous solution of 36.00g acrylamide (AM), 0.01g methylene-bisacrylamide (MBA), 0.04g linking agent polyethyleneglycol diacrylate (PEGDA) and 0.08g oxygenant ammonium persulphate (APS) composition adds wherein, after stirring treats that whole system mixes and is transparent or semitransparent shape, it is transferred to the four-hole boiling flask that has stirring rod that places 40 ℃ of waters bath with thermostatic control in advance, logical N
2Deoxygenation 10 minutes adds mass concentration and is 10% the acrylamide triggered Raolical polymerizable of sodium formaldehyde sulphoxylate (FS) aqueous solution 0.30 gram subsequently when stirring.After the exothermic heat of reaction peak, continue reaction 30 minutes, promptly get transparent or semitransparent polyacrylamide nano microsphere system, microspherulite diameter is less than 150nm.The system composition sees Table 2.
The composition of table 2 system
| The system moiety | Diesel oil | ??OA | ??Span20 | ??OP10 | ??H 2O | ??AM | ??MBA | ??PEGDA | ??APS | ??FS |
| Quality/g | ??84.00 | ??14.76 | ??11.16 | ??10.08 | ??44.14 | ??36.00 | ??0.01 | ??0.04 | ??0.08 | ??0.03 |
| Massfraction/% | ??41.94 | ??7.37 | ??5.57 | ??5.03 | ??22.04 | ??17.97 | ??0.00 | ??0.02 | ??0.04 | ??0.02 |
The polyacrylamide nanometer microsphere with low system of getting preparation directly is 0.10% microballoon aqueous solution 500g with deionized water dilution preparation polyacrylamide massfraction, add the abundant mixing of 0.03 gram NaOH and make wherein OA and NaOH neutralization reaction complete, obtain low interfacial tension transfer drive system.
The dynamic interface tension force between interfacial tensimeter mensuration crude oil and the transfer drive system is dripped in the TX-550A type rotation that the present invention adopts Bowing Industry Corp to produce.Crude oil is taken from Shengli Oil Field stake west oil recovery factory's stake 106 wells, and (50 ℃ of viscosity are 1450mPas, ρ=0.93g/cm
-3, the gum asphalt massfraction is 20.54%).Measurement result under 70 ℃ shows that the transfer drive system can reduce to 10 with the interfacial tension of the western crude oil of stake
-2The order of magnitude.Compare with the oil water interfacial tension (being about 0.1mN/m) of the western crude oil of stake with the Span80/OP10 composite emulsifier aqueous solution of equal conditions, it is obvious that transfer drive system of the present invention reduces the interfacial tension effect, be applied to improve in the recovery ratio operation, will play good raising displacement efficiency and the final effect that improves recovery ratio.
Embodiment 3: at first take by weighing 24.00g kerosene, 72.00g diesel oil, 10.24g Witco 1298 Soft Acid (DBSA, purity 90%), 12.80g Span80 and 8.96g Tween60 magnetic stirrer mixing, then will be by the 29.90g deionized water, 31.50g acrylamide (AM), 10.50g methylacryoyloxyethyl trimethyl ammonium chloride (DMC), 0.04g the aqueous solution that linking agent polyethyleneglycol diacrylate (PEGDA) and 0.06g oxygenant Potassium Persulphate (KPS) are formed adds wherein, after stirring treats that whole system mixes and is transparent or semitransparent shape, it is transferred to the four-hole boiling flask that has stirring rod that places 30 ℃ of waters bath with thermostatic control in advance, logical N
2Deoxygenation 10 minutes adds mass concentration and is the polyreaction of the acrylamide triggered and methylacryoyloxyethyl trimethyl ammonium chloride of 10% sodium bisulfite (SHS) aqueous solution 0.40 gram subsequently when stirring.After the exothermic heat of reaction peak, continue reaction 30 minutes, promptly get transparent or semitransparent polyacrylamide nano microsphere system, microspherulite diameter is less than 150nm.The system composition sees Table 3.
The composition of table 3 system
| System is formed | Kerosene | Diesel oil | ??DBSA | ??Sp80 | ??Tw60 | ??H 2O | ??AM | ??DMC | ??PEGDA | ??KPS | ??SHS |
| Quality/g | ??24.00 | ??72.00 | ??10.24 | ??12.80 | ??8.96 | ??30.26 | ??31.50 | ??10.50 | ??0.04 | ??0.06 | ??0.04 |
| Massfraction/% | ??11.98 | ??35.93 | ??5.11 | ??6.39 | ??4.47 | ??15.10 | ??15.72 | ??5.24 | ??0.02 | ??0.03 | ??0.02 |
The polyacrylamide nanometer microsphere with low system of getting preparation directly is 1.0% microballoon aqueous solution 500g with deionized water dilution preparation polyacrylamide massfraction, add the abundant mixing of 0.18 gram NaOH and make wherein DBSA and NaOH neutralization reaction complete, obtain low interfacial tension transfer drive system.
The dynamic interface tension force between interfacial tensimeter mensuration crude oil and the transfer drive system is dripped in the TX-550A type rotation that the present invention adopts Bowing Industry Corp to produce.Crude oil is taken from Shengli Oil Field stake west oil recovery factory's stake 106 wells, and (50 ℃ of viscosity are 1450mPas, ρ=0.93g/cm
-3, the gum asphalt massfraction is 20.54%).Measurement result under 70 ℃ shows that the transfer drive system can be reduced to 10 with the oil water interfacial tension of the western crude oil of stake
-3The order of magnitude.Compare with the oil water interfacial tension (being about 20mN/m) of the western crude oil of stake with the Span80/Tween60 composite emulsifier aqueous solution of equal conditions, it is remarkable that transfer drive system of the present invention reduces the interfacial tension effect, be applied to improve in the recovery ratio operation, will play good raising displacement efficiency and the final effect that improves recovery ratio.
Claims (1)
1. the preparation method of a low interfacial tension polyacrylamide nanometer microsphere with low transfer drive system is characterized in that realizing according to the following steps:
1. oil phase and emulsifying agent are stirred evenly with the magnetic stirrer mixing, oil phase is one or more of gasoline, kerosene, diesel oil, white oil, vegetables oil, toluene, hexanaphthene and octane-iso, and oil phase accounts for 30%～55% of microemulsion quality; The consumption of emulsifying agent accounts for 15%～25% of microemulsion quality, emulsifying agent is lipophilic surfactant and hydrophilic surfactant active's a binary, ternary or multicomponent mixture, lipophilic surfactant comprises organic acid substance and other lipophilic surfactants, organic acid substance is wherein selected lauric acid, linolenic acid, mountain Yu acid, oleic acid, stearic acid, naphthenic acid, the oil carboxylic acid, alkylsulphonic acid, alkyl benzene sulphonate (ABS), one or more of carboxylic acids such as mahogany acid and sulfonic acid, other lipophilic surfactants are from Span series, the Stearinsaeure propylene diester, distearyl acid second diester, select one or more in single oleic acid two sweet esters; The hydrophilic surfactant active selects one or more of Tween series and OP series for use; Organic acid composition accounts for 30%～55% of emulsifying agent total mass in the emulsifying agent, and other lipophilic surfactants account for 25%～45% of emulsifying agent total mass, and Tween series or OP series account for 20%～40% of emulsifying agent total mass; Microemulsion is the homogeneous mixture of oil phase, emulsifying agent and water;
2. in the mixture of above-mentioned oil phase and emulsifying agent, add the water that contains linking agent and oxygenant, water is that monomer mass concentration is the aqueous solution that 40%～70% acrylamide monomers adds linking agent and oxygenant, the water quality accounts for 30%～55% of microemulsion quality, the contained linking agent of aqueous phase is a Vinylstyrene, methylene-bisacrylamide, one or more of Viscoat 295 and polyethyleneglycol diacrylate, its content is 0.01%～1.00% of water quality, the contained oxygenant of aqueous phase is a Potassium Persulphate, ammonium persulphate or benzoyl peroxide, its content is 0.03%～0.10% of water quality, the reverse micro emulsion that fully stirs transparent or semitransparently;
3. logical N
2After the deoxygenation 10 minutes, in reverse micro emulsion, add the acrylamide triggered class polymerization reaction take place of reductive agent, treat after the peak heat release, continue to react half an hour, obtain the transparent or semitransparent thermodynamically stable transfer drive system that is dispersed with the polyacrylamide nano microballoon, microspherulite diameter is less than 150nm;
Above-mentioned steps 2. in said acrylamide monomers be one or more of non-ionic type, cationic, anionic and ampholytic monomer, wherein, nonionic monomers is selected acrylamide for use, cationic monomer is selected dimethyl diallyl ammonium chloride or methylacryoyloxyethyl trimethyl ammonium chloride for use, the anionic monomer is selected vinylformic acid, methacrylic acid or 2-acrylamido-2 methyl propane sulfonic acid salt, and ampholytic monomer is selected dimethylaminoethyl acrylate for use; The reductive agent of step in 3. selects iron protochloride, S-WAT, Sulfothiorine, sodium bisulfite, sulfurous gas, and consumption is 0.02%～0.06% of a water quality; The mass ratio of Oxidizing and Reducing Agents is 1: 2～5: 1; Temperature of reaction is 25 ℃～45 ℃.
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