CN101805423A - Method for preparing polyacrylamide nano microsphere system - Google Patents
Method for preparing polyacrylamide nano microsphere system Download PDFInfo
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- CN101805423A CN101805423A CN200910256125A CN200910256125A CN101805423A CN 101805423 A CN101805423 A CN 101805423A CN 200910256125 A CN200910256125 A CN 200910256125A CN 200910256125 A CN200910256125 A CN 200910256125A CN 101805423 A CN101805423 A CN 101805423A
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Abstract
The invention provides a method for preparing low-cost polyacrylamide nano microspheres by two times of microemulsion polymerization. The prepared polyacrylamide nano microspheres are used for improving an oil recovery factor. The method comprises: firstly, preparing a dispersion of polyacrylamide nano microspheres by microemulsion polymerization; secondly, adding a monomer and aqueous solution of an initiator into the product of the primary polymerization serving as a dispersion medium to form microemulsion by using an emulsifier in the dispersion medium; and finally, initiating polymerization again to obtain high-content polyacrylamide nano microspheres. As no oil soluble solvent and emulsifier are added for the secondary polymerization, the synthesis cost of the polyacrylamide nano microspheres can be reduced considerably. The prepared polyacrylamide nano microsphere system can be directly diluted by water to form polymer microsphere aqueous solution at required concentration and can be used alone or in combination with other oil-field chemicals in fields of profile control, water plugging, fuel scavenge and the like for improving recovery operation.
Description
Technical field:
The present invention relates to a kind of preparation method who is used to improve the low-cost polyacrylamide nano microsphere system of recovery ratio.
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 in the space 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.
Present polyacrylamide nano microballoon adopts micro emulsion polymeric technology once to synthesize usually and obtains, in this process owing to used a large amount of expensive emulsifying agent and oil-dissolving solvent, make that polyacrylamide nano microballoon cost is higher, limited applying of this material.If can improve the effective content of polyacrylamide nano microballoon, reduce the content of emulsifying agent and oil-dissolving solvent, then can reduce the cost of polyacrylamide nano microballoon greatly.
Summary of the invention:
The objective of the invention is to provide a kind of method for preparing low-cost polyacrylamide nano microsphere system.
Purpose of the present invention realizes in two steps: the first step, and oil-dissolving solvent and emulsifier mix is even, add the water that contains acrylamide monomers and linking agent and oxygenant, fully stir, lead to N
2After the deoxygenation, add the reductive agent initiation reaction again in above-mentioned system, peak heat release continues reaction half an hour to two hour later, obtains being dispersed with the transparent or semitransparent system of polyacrylamide nano microballoon; Second step, continue in this system, to add the water that contains acrylamide monomers and linking agent and oxygenant, its dosage be in the first step water consumption 50%～100%, fully stir the logical N in back
2Deoxygenation adds the reductive agent initiation reaction again in system, peak heat release continues reaction 0.5～2 hour later, obtains transparent or semitransparent polyacrylamide nano microsphere system, and microspherulite diameter is less than 150nm.Owing to no longer add oil-dissolving solvent and emulsifying agent in the second step building-up process, therefore can reduce the consumption of oil-dissolving solvent and emulsifying agent significantly.
Oil-dissolving solvent used in the said process is oily liquids such as gasoline, kerosene, diesel oil, white oil, paraffin, vegetables oil, toluene, hexanaphthene or octane-iso, and oil-dissolving solvent accounts for 28%～45% of dispersion system total mass.Emulsifying agent is by lipophilic surfactant Span class and composite the forming of hydrophilic surfactant active Tween class, and the quality of Span class and Tween class is 1: 4～4: 1 than scope, and total consumption accounts for 12～16% of system total mass.Water is that massfraction is 50%～70% acrylamide solution, and the water quality accounts for 40%～58% of system total mass.Linking agent is one or more of methylene-bisacrylamide, Vinylstyrene and polyethyleneglycol diacrylate, consumption accounts for 0.01%～0.20% of water quality, oxygenant is Potassium Persulphate, ammonium persulphate or benzoyl peroxide, and consumption accounts for 0.02%～0.10% of water quality.It can be initiator initiation, thermal initiation, light-initiated and radiation initiation etc. that polyreaction causes mode, preferably select for use initiator to cause mode, preferentially select oxidation-reduction trigger system for use, wherein oxygenant can be selected Potassium Persulphate, ammonium persulphate or benzoyl peroxide for use, and consumption accounts for 0.02%～0.10% of water quality; The optional iron protochloride of reductive agent, S-WAT, Sulfothiorine and sodium bisulfite etc., consumption accounts for 0.02%～0.04% of water quality; The mass ratio of Oxidizing and Reducing Agents is 1: 2～5: 1, optional 25 ℃～35 ℃ of range of reaction temperature.
The invention has the beneficial effects as follows: obtain polyacrylamide nano microballoon dispersion by twice micro emulsion polymerization, made full use of keep after the polymerization for the first time the polyacrylamide microsphere dispersion system stable unwanted unnecessary emulsifying agent, only need to add the monomeric aqueous solution, contain monomeric water and carry out the micro emulsion polymerization once more with its further emulsification, no longer add oil-dissolving solvent and emulsifying agent, therefore can reduce the consumption of oil-dissolving solvent and emulsifying agent significantly, reduce the production cost of polyacrylamide microsphere system significantly, and each used component wide material sources.Show that through transmission electron microscope observing twice synthetic polyacrylamide microsphere particle diameter and disposable synthetic difference that obtains is not obvious, all less than 150nm.The polyacrylamide nano microsphere system that makes can directly be diluted with water to the polymer microballoon aqueous solution of desired concn, is applied to profile control, water blockoff, the displacement of reservoir oil etc. and improves the recovery ratio operations separately or with other oil field chemicals are composite.
Embodiment:
Further specify the present invention below by embodiment.
Embodiment 1:
At first take by weighing 86.50g diesel oil, add the emulsifying agent that is re-dubbed by 26.10g Span20 and 8.70g Tween80 again, mix with magnetic stirrer, to add wherein by the water of 48.70g acrylamide (AM), 0.01g methylene-bisacrylamide (MBA), 0.03g ammonium persulphate (APS), the preparation of 29.82g water then, after treating 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 at last mass concentration and is 20% the acrylamide triggered Raolical polymerizable of S-WAT (SS) aqueous solution 0.20 gram in flask when stirring.
After the exothermic heat of reaction peak, continue reaction 30 minutes, obtain polymerisate for the first time.
70.0 identical gram waters (promptly contain 26.571g H in weighing proportion of composing and the polyreaction for the first time again
2O, 43.394g AM, 0.009g MBA and 0.027g APS), it is joined 200.06g for the first time in the polymerisate, mix to system and become transparent or semitransparent shape, logical N
2Deoxygenation 10 minutes adds mass concentration and is 20% sodium sulfite aqueous solution 0.18 gram re-initiation reaction then.
Peak heat release continues reaction 30 minutes later, promptly gets transparent or semitransparent polyacrylamide nano microballoon dispersion system.
Calculating twice reacted product of contrast forms as can be known, twice synthesis method has been reduced to 44.89% with expensive emulsifying agent in the microsphere system and oil phase massfraction from 60.63%, the polyacrylamide that plays a major role in improving recovery ratio has brought up to 34.08% from 24.34%, successfully realize the reduction of invalid component concentration in the unit mass microsphere system and the lifting of useful component content, reached the purpose that reduces polyacrylamide microsphere system cost.Transmission electron microscope photo shows that the particle diameter of twice synthetic microballoon that obtains is less than 150nm and a synthetic microspherulite diameter size no significant difference.
Embodiment 2:
At first take by weighing the 40.00g white oil, add the emulsifying agent that is re-dubbed by 4.00g Span20 and 16.00g Tween85 again, mix with magnetic stirrer, to add wherein by the water of 20.00g acrylamide (AM), 0.01g polyethyleneglycol diacrylate (PEGD), 0.01g Potassium Persulphate (KPS), the preparation of 19.93g water then, after treating 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 at last mass concentration and is 20% the acrylamide triggered Raolical polymerizable of sodium bisulfite (SHS) aqueous solution 0.05 gram in flask when stirring.
After the exothermic heat of reaction peak, continue reaction 30 minutes, obtain polymerisate for the first time.
Identical 39.95g water (promptly contains 19.93g H in weighing proportion of composing and the polyreaction for the first time again
2O, 20.00gAM, 0.01g PEGD and 0.01g KPS), it is joined 100g for the first time in the polymerisate, mix to system and become transparent or semitransparent shape, logical N
2Deoxygenation 10 minutes adds mass concentration and is 20% aqueous solution of sodium bisulfite 0.05 gram re-initiation reaction then.
Peak heat release continues reaction 30 minutes later, promptly gets transparent or semitransparent polyacrylamide nano microballoon dispersion system.
Calculating twice reacted product of contrast forms as can be known, twice synthesis method has been reduced to 42.86% with expensive emulsifying agent in the microsphere system and oil phase massfraction from 60.00%, the polyacrylamide amine content that plays a major role in improving recovery ratio has brought up to 28.57% from 20.00%, successfully realize the reduction of invalid component concentration in the unit mass microsphere system and the lifting of useful component content, reached the purpose that reduces polyacrylamide microsphere system cost.
The transmission electron microscope photo shows the particle diameter of synthetic polyacrylamide microsphere less than 150nm, and twice synthetic microballoon and synthetic microspherulite diameter difference that obtains is not obvious.
Embodiment 3:
At first take by weighing 90.00g peanut oil, add the emulsifying agent that is re-dubbed by 20.00g Span80 and 20.00g Tween60 again, mix with magnetic stirrer, to add wherein by the water of 47.00g acrylamide (AM), 0.01g methylene-bisacrylamide (MBA), 0.02g polyethyleneglycol diacrylate (PEGD), 0.04g ammonium persulphate (APS), the preparation of 22.83g water then, after treating 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 at last mass concentration and is 20% the acrylamide triggered Raolical polymerizable of Sulfothiorine (STS) aqueous solution 0.10 gram in flask when stirring.
After the exothermic heat of reaction peak, continue reaction 30 minutes, obtain polymerisate for the first time.
Identical 62.91g water (promptly contains 20.547g H in weighing proportion of composing and the polyreaction for the first time again
2O, 42.300g AM, 0.009g MBA, 0.018g PEGD and 0.036g APS), it is joined 200g for the first time in the polymerisate, mix to system and become transparent or semitransparent shape, logical N
2Deoxygenation 10 minutes adds mass concentration and is 20% sodium thiosulfate solution 0.09 gram re-initiation reaction then.
Peak heat release continues reaction 30 minutes later, promptly gets transparent or semitransparent polyacrylamide nano microballoon dispersion system.
Calculating twice reacted product of contrast forms as can be known, twice synthesis method has been reduced to 49.43% with expensive emulsifying agent in the microsphere system and oil phase massfraction from 65.00%, the polyacrylamide amine content that plays a major role in improving recovery ratio has brought up to 33.95% from 23.50%, successfully realize the reduction of invalid component concentration in the unit mass microsphere system and the lifting of useful component content, reached the purpose that reduces polyacrylamide microsphere system cost.
The transmission electron microscope photo shows the particle diameter of synthetic polyacrylamide microsphere less than 150nm, and twice synthetic microballoon and synthetic microspherulite diameter difference that obtains is not obvious.
Claims (2)
1. the preparation method of a polyacrylamide nano microsphere system is characterized in that being finished by two steps:
The first step, oil-dissolving solvent and emulsifier mix is even, add the water that contains acrylamide monomers and linking agent and oxygenant, fully stir, lead to N
2After the deoxygenation, add the reductive agent initiation reaction again in above-mentioned mixed system, peak heat release continues reaction 0.5～2 hour later, obtains being dispersed with the transparent or semitransparent system of polyacrylamide nano microballoon;
Second step, continue in this system, to add the water that contains acrylamide monomers and linking agent and oxygenant, its dosage be in the first step water consumption 50%～100%, fully stir the logical N in back
2Deoxygenation adds the reductive agent initiation reaction again in system, after the peak heat release, obtain transparent or semitransparent polyacrylamide nano microsphere system, and microspherulite diameter is less than 150nm;
The used oil-dissolving solvent of above-mentioned steps is gasoline, kerosene, diesel oil, white oil, paraffin, vegetables oil, toluene, hexanaphthene or octane-iso, and consumption accounts for 28%～45% of oil-dissolving solvent, emulsifying agent and water three mixed system total mass; Emulsifying agent is by lipophilic surfactant Span class and composite the forming of hydrophilic surfactant active Tween class, and the mass ratio of Span class and Tween class is 1: 4～4: 1, and total consumption of emulsifying agent accounts for 12%～16% of three's mixed system total mass; Water is that massfraction is the aqueous solution that 50%～70% acrylamide adds linking agent and oxygenant, and the water quality accounts for 40%～58% of three's mixed system total mass; Linking agent is one or more of methylene-bisacrylamide, Vinylstyrene and polyethyleneglycol diacrylate, and its consumption accounts for 0.01%～0.20% of water quality; Oxygenant is Potassium Persulphate, ammonium persulphate or benzoyl peroxide, and consumption accounts for 0.02%～0.10% of water quality; Polyreaction initiation mode is that initiator initiation, thermal initiation, light-initiated, radiation initiation or oxidation-reduction initiator cause.
2. the preparation method of polyacrylamide nano microsphere system according to claim 1, it is characterized in that polyreaction initiation mode is that oxidation-reduction initiator causes, wherein oxygenant is selected Potassium Persulphate, ammonium persulphate or benzoyl peroxide for use, and its consumption is 0.02%～0.10% of a water quality; Reductive agent selects iron protochloride, S-WAT, Sulfothiorine or sodium bisulfite, and its consumption is 0.02%～0.04% of a water quality; The mass ratio of Oxidizing and Reducing Agents is 1: 2～5: 1, and redox system causes and polymeric reaction temperature is set in 25 ℃～35 ℃.
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