CN104231168A - Polymer microsphere temporary plugging agent with ultralow interfacial tension and preparation method thereof - Google Patents
Polymer microsphere temporary plugging agent with ultralow interfacial tension and preparation method thereof Download PDFInfo
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- CN104231168A CN104231168A CN201410487961.XA CN201410487961A CN104231168A CN 104231168 A CN104231168 A CN 104231168A CN 201410487961 A CN201410487961 A CN 201410487961A CN 104231168 A CN104231168 A CN 104231168A
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Abstract
The invention discloses a polymer microsphere temporary plugging agent with ultralow interfacial tension and a preparation method thereof. The polymer microsphere temporary plugging agent is prepared from white oil, acrylamide monomer, acrylic acid, polyoxyethylene sorbitan fatty acid ester, N,N-methylene diacrylamide, ammonium persulphate, sodium hydrogen sulfite, hydrophilic group surfactant, water and other raw materials. According to the polymer microsphere temporary plugging agent and the preparation method thereof disclosed by the invention, polymer microspheres with the ultralow interfacial tension are synthesized by adopting an inverse emulsion copolymerization method; the interfacial tension of the polymer microspheres can reach 4.3*10<-3>mN/N and the salt tolerance can reach 50 thousand mineralization degrees, and the problems of low interfacial tension and low salt tolerance of existing polymer microspheres are improved.
Description
Technical field
The invention belongs to oilfield exploitation chemical technical field, be specifically related to a kind of polymer microballoon temporary plugging agent with ultra low interfacial tension and preparation method thereof.
Background technology
Polyacrylamide microsphere is the broad-spectrum absorbent resin of a class, is applied to oil field deep profile control and water plugging, the oil field deep profile control that, High water cut, macropore strong mainly for nonuniformity are grown, and is improving ecology development effectiveness and the new technology developed.
In prior art, Chinese patent CN1888374A discloses a kind of shutoff method of resisting high temperature, high salt, and adopt three slugs to inject shutoff method, the first slug adds temporary plugging agent, accounts for 10 ~ 20% of total injection; Temporary plugging agent injects closing well after 0.5 ~ 1.5 hour and waits solidifying, causes temporary plugging agent plastic first temporary stifled oil reservoir; Second slug of follow-up injection, the feature of this slug is low viscosity, and easily inject, can form high viscoelastic gel at the formation temperature, applicable temperature range is 90 ~ 280 DEG C, accounts for 70 ~ 80% of total injection; The 3rd slug be cement, as sealing compound, improve the intensity of shutoff principal piece plug, account for 10 ~ 20% of total injection, but it gel can occur in oil reservoir, can reduce the relative permeability of oil phase.
Polyacrylamide microsphere water shutoff agent prepared by Chinese patent CN103073679A, comprises raw materials weighing acrylamide, anti-salt monomer, N, N-methylene bisacrylamide acyl, sorbester p17, Potassium Persulphate, hexanaphthene and deionized water; Dispersion agent and hexanaphthene is uniformly mixed in polymerization single polymerization monomer; Cause and be polymerized and form plugging agent.What its external phase was selected is hexanaphthene, and cost is higher, and layering after leaving standstill, stability is bad, and its salt tolerance is only 30,000 salinities.
Existing pertinent literature and patent, do not find polymer microballoon temporary plugging agent with ultra low interfacial tension and preparation method thereof.
Summary of the invention
For solving defect of the prior art, the invention provides a kind of polymer microballoon temporary plugging agent with ultra low interfacial tension and preparation method thereof, the construction of this polymer microballoon temporary plugging agent is simple, good stability, has the salt tolerance of ultra low interfacial tension and Geng Gao.
For achieving the above object, the present invention is by the following technical solutions:
Have a polymer microballoon temporary plugging agent for ultra low interfacial tension, described polymer microballoon temporary plugging agent is prepared from by the raw material of following weight percent:
White oil 20 ~ 40wt%, acrylamide monomer 10 ~ 25wt%, vinylformic acid 5 ~ 15wt%, sorbitan fatty acid ester 5 ~ 15wt%, N,N methylene bis acrylamide 0.03 ~ 0.08wt%, ammonium persulphate 0.01 ~ 0.05wt%, sodium bisulfite 0.01 ~ 0.08wt%, hydrophilic group tensio-active agent 10 ~ 25wt%, water surplus.
As a further improvement on the present invention, described hydrophilic group tensio-active agent is one or more the mixture in tween 80, TX-10, OP-10 and SAS60.
As a further improvement on the present invention, described sorbitan fatty acid ester is one or more the mixture in span 40, sorbester p18 and sorbester p17.
As a further improvement on the present invention, described water is tap water or deionized water.
As a further improvement on the present invention, described white oil is technical grade.
As a further improvement on the present invention, described polymer microballoon temporary plugging agent is prepared from by the raw material of following weight percent: white oil is 30wt%, and acrylamide monomer is 18wt%, vinylformic acid is 5%, sorbester p18 is 4%, and sorbester p17 is 3wt%, N, N-methylene-bisacrylamide is 0.04wt%, ammonium persulphate is 0.05wt%, and sodium bisulfite is 0.03wt%, OP-10 is 9wt%, SAS60 is 3wt%, and tap water is surplus.
There is a preparation method for the polymer microballoon temporary plugging agent of ultra low interfacial tension, comprise the following steps:
1) raw material for standby is taken by weight;
2), under room temperature under condition, in the container that agitator, thermometer, reflux condensate device are housed, add white oil, sorbitan fatty acid ester, hydrophilic group tensio-active agent, stir, make solution A;
3) acrylamide monomer taken, vinylformic acid, N,N methylene bis acrylamide are added to the water, stir after making it dissolve completely, add alkali lye neutralization, then add sodium bisulfite, stir and make it dissolve completely, make solution B; The mass ratio of solution A and solution B is (1 ~ 4): 1;
4) add in solution A by solution B, after fully emulsified, be warming up to 60 ~ 70 DEG C, unlatching condensing reflux, is added dropwise to ammonium persulphate, continues to be stirred to react completely after being added dropwise to complete, and be then cooled to room temperature, namely discharging after cooling obtains polymer microballoon temporary plugging agent.
As a further improvement on the present invention, step 3) in alkali lye in and adopt aqueous sodium hydroxide solution neutralization, degree of neutralization is 50 ~ 80%.
As a further improvement on the present invention, step 4) in ammonium persulfate initiator be that the aqueous solution being 10% with mass concentration drips in batches, time for adding 45 ~ 60min.
As a further improvement on the present invention, step 4) in emulsification condition be, stirring velocity 500 ~ 600r/min, time 20 ~ 30min.
As a further improvement on the present invention, step 4) in ammonium persulphate to be added dropwise to complete rear continuation mixing speed be 200 ~ 300r/min, the time of continuing reaction is 6 ~ 7h.
As a further improvement on the present invention, step 2) medium speed is 200 ~ 300r/min.
Relative to prior art, the present invention has the following advantages:
A kind of polymer microballoon temporary plugging agent with ultra low interfacial tension disclosed by the invention, with acrylamide and vinylformic acid for comonomer, N, N-methylene-bisacrylamide is linking agent, ammonium persulphate and sodium bisulfite are redox initiator, white oil is external phase, with sorbitan fatty acid ester and hydrophilic group tensio-active agent for compound emulsifying agent, reversed emulsion polymerization is adopted to synthesize the polymer microballoon of ultra low interfacial tension, analyze and show that this temporary plugging agent is a kind of polymer microspheres with ultra low interfacial tension, its interfacial tension can reach 4.3 × 10
-3mN/N, salt tolerance can reach 50,000 salinities, improves the problem that existing polymer microballoon interfacial tension is low, salt tolerance is less.
Further, polymer microballoon plugging agent construction prepared by the present invention is simple, and good stability, has ultra low interfacial tension, and salt tolerance is higher, can reach the effect of shutoff and the displacement of reservoir oil simultaneously.
Further, in the present invention's formula with sorbitan fatty acid ester and hydrophilic group tensio-active agent for compound emulsifying agent, add emulsifying effectiveness, improve speed, improve emulsion intercalation method.
Further, the water used in the present invention's formula is tap water or deionized water, and all can ensure reaction effect and productive rate, especially the use of tap water, effectively simulates actual production situation, improves the applicability of polymer microballoon temporary plugging agent of the present invention.
Further, adopt the mass ratio of solution A and solution B for (1 ~ 4) in preparation method of the present invention: 1 ensure that inverse emulsion polymerization react in water in oil requirement.
Further, ammonium persulfate initiator is that the aqueous solution being 10% with concentration adds in batches and prevents reaction too violent, and ensure sufficient reacting, productive rate is high.
Accompanying drawing illustrates:
The interfacial tension figure of the polymer microballoon of Fig. 1 embodiment 1;
The interfacial tension figure of the polymer microballoon of Fig. 2 embodiment 2;
The interfacial tension figure of the polymer microballoon of Fig. 3 embodiment 3;
The interfacial tension figure of the polymer microballoon of Fig. 4 embodiment 4;
The interfacial tension figure of the polymer microballoon of Fig. 5 embodiment 5;
The Salt Tolerance Analysis figure of the polymer microballoon of Fig. 5 a embodiment 5;
The polymer microballoon of Fig. 5 b embodiment 5 places the stability analysis figure of 15 days;
The TEM figure of the polymer microballoon of Fig. 5 c embodiment 5.
Embodiment
There is a polymer microballoon temporary plugging agent for ultra low interfacial tension, be prepared from by the raw material of following weight percent:
White oil 20 ~ 40wt%, acrylamide monomer 10 ~ 25wt%, vinylformic acid 5 ~ 15wt%, sorbitan fatty acid ester 5 ~ 15wt%, N,N methylene bis acrylamide 0.03 ~ 0.08wt%, ammonium persulphate 0.01 ~ 0.05wt%, sodium bisulfite 0.01 ~ 0.08wt%, hydrophilic group tensio-active agent 10 ~ 25wt%, water surplus.
Wherein, optional one or more in tween 80, TX-10, OP-10 and SAS60 of hydrophilic group tensio-active agent; Sorbitan fatty acid ester can be selected from span 40, sorbester p18 and sorbester p17 one or more; Water is tap water or deionized water; White oil is technical grade.
There is a preparation method for the polymer microballoon temporary plugging agent of ultra low interfacial tension, it is characterized in that: comprise the following steps:
1) raw material for standby is taken by weight;
2), under room temperature under condition, in the container that agitator, thermometer, reflux condensate device are housed, add white oil, sorbitan fatty acid ester, hydrophilic group tensio-active agent, stir, stirring velocity 200 ~ 300r/min makes solution A;
3) acrylamide monomer taken, vinylformic acid, N,N methylene bis acrylamide are added to the water, stir after making it dissolve completely, add aqueous sodium hydroxide solution neutralization, degree of neutralization is 50 ~ 80%.Then add sodium bisulfite, stir and make it dissolve completely, make solution B; The mass ratio of solution A and solution B is (1 ~ 4): 1;
4) solution B is added in solution A, emulsification stirring speed is 500 ~ 600r/min, time 20 ~ 30min, and then be warming up to 60 ~ 70 DEG C, open condensing reflux, dropping mass concentration is the ammonium persulfate aqueous solution of 10% in batches, time for adding 45 ~ 60min, time for adding 45 ~ 60min; Be added dropwise to complete rear continuation to stir, mixing speed is 200 ~ 300r/min is 6 ~ 7h to the time of reacting completely.Then be cooled to room temperature, namely discharging after cooling obtains polymer microballoon temporary plugging agent.
Wherein, about the calculating of degree of neutralization, y=(M × 71)/(40 × m × c), wherein, y is degree of neutralization, and M is the quality of sodium hydroxide, 40 is the relative molecular mass of sodium hydroxide, m is acrylic acid quality, and c is acrylic acid concentration, and 71 is acrylic acid relative molecular mass.
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
Raw material weight compares: white oil is 40wt%, and acrylamide monomer is 20wt%, and vinylformic acid is 5wt%, and sorbester p18 is 5wt%, N,N methylene bis acrylamide is 0.03wt%, and ammonium persulphate is 0.01wt%, sodium bisulfite is 0.015wt%, and tween 80 is 10wt%, and distilled water is surplus.By white oil, sorbester p18, tween 80 puts into the there-necked flask that agitator, reflux exchanger and thermometer are housed, and 200r/min rotating speed stirs and makes solution A, with beaker, monomeric acrylamide is dissolved in water, then vinylformic acid is added, N, N-methylene-bisacrylamide, be placed on magnetic stirring apparatus and stir, add aqueous sodium hydroxide solution neutralization until completely dissolved, degree of neutralization is 50%, add sodium bisulfite to dissolving solution B processed completely, then solution B is slowly added in A, and with rotating speed 500r/min, time 20min, carry out emulsification stirring, 60 DEG C are warming up to after emulsification completes, ammonium persulphate is made into the aqueous solution of 10wt%, slowly add in batches, be added dropwise to complete in 1h, initiator drips off rear continuation and continues stirring reaction 6h with 200r/min rotating speed, cooling discharging.Resulting polymers microballoon is placed and is not occurred layering in 7 days, and its interfacial tension figure shows in FIG, and in 30,000 salinities, when microballoon concentration is 0.5%, its interfacial tension is 8.6 × 10
-1mN/M.
Embodiment 2
Raw material weight compares: white oil is 20wt%, and acrylamide monomer is 25wt%, and vinylformic acid is 10wt%, and span 40 is 10wt%, N, N methylene-bisacrylamide is 0.08wt%, and ammonium persulphate is 0.05wt%, sodium bisulfite is 0.08wt%, OP-10 is 25wt%, and tap water is surplus.By white oil, span 40, OP-10 puts into the there-necked flask that agitator, reflux exchanger and thermometer are housed, and 300r/min rotating speed stirs and makes solution A, with beaker, monomeric acrylamide is dissolved in water, then vinylformic acid is added, N, N-methylene-bisacrylamide, be placed on magnetic stirring apparatus and stir, add aqueous sodium hydroxide solution neutralization until completely dissolved, degree of neutralization is 60%, add sodium bisulfite to dissolving completely, solution B processed, then solution B is slowly added in A, and with rotating speed 600r/min, time 25min, carry out emulsification stirring, 65 DEG C are warming up to after emulsification completes, ammonium persulphate is made into the aqueous solution of 10wt%, slowly add in batches, initiator drips off rear continuation and continues stirring reaction 6h with 300r/min rotating speed, cooling discharging.Resulting polymers microballoon is placed 24h and is not occurred layering, and its interfacial tension figure shows in fig. 2, and in 30,000 salinities, when microballoon concentration is 0.5%, its interfacial tension is 7.2 × 10
-1mN/M.
Embodiment 3
Raw material weight compares: white oil is 38wt%, and acrylamide monomer is 15wt%, vinylformic acid 15wt%, and sorbester p17 is 8wt%, N, N methylene-bisacrylamide is 0.04wt%, and ammonium persulphate is 0.02wt%, sodium bisulfite is 0.05wt%, TX-10 is 12wt%, and tap water is surplus.By white oil, sorbester p17, TX-10, puts into the there-necked flask that agitator, reflux exchanger and thermometer are housed, and 200r/min rotating speed stirs and makes solution A, with beaker, monomeric acrylamide is dissolved in water, then vinylformic acid is added, N, N-methylene-bisacrylamide, be placed on magnetic stirring apparatus and stir, add aqueous sodium hydroxide solution neutralization until completely dissolved, degree of neutralization is 65%, add sodium bisulfite to dissolving solution B processed completely, then solution B is slowly added in A, and with rotating speed 500r/min, time 30min carries out emulsification, after emulsification completes, be warming up to 65 DEG C, ammonium persulphate is made into the aqueous solution of 10wt%, slowly add in batches, be added dropwise to complete in 45min, stirring reaction 7h is continued with 200r/min rotating speed after initiator drips off, cooling discharging.Resulting polymers microballoon is placed and is not occurred layering in 30 days, and its interfacial tension figure shows in figure 3, and in 30,000 salinities, when microballoon concentration is 0.5%, its interfacial tension is 8.1 × 10
-2mN/M.
Embodiment 4
Raw material weight compares: white oil is 30wt%, acrylamide monomer is 10wt%, vinylformic acid is 12%, and sorbester p18 is 15wt%, N, N methylene-bisacrylamide is 0.04wt%, ammonium persulphate is 0.015wt%, and sodium bisulfite is 0.03wt%, TX-10 is 9wt%, tween 80 is 3%, and tap water is surplus.By white oil, sorbester p18, TX-10, tween 80 puts into the there-necked flask that agitator, reflux exchanger and thermometer are housed, and 200r/min rotating speed stirs and makes solution A, with beaker, monomeric acrylamide is dissolved in water, then vinylformic acid is added, N, N-methylene-bisacrylamide, be placed on magnetic stirring apparatus and stir, add aqueous sodium hydroxide solution neutralization until completely dissolved, degree of neutralization is 70%, add sodium bisulfite to dissolving solution B processed completely, then solution B is slowly added in A, and with rotating speed 600r/min, time 30min carries out emulsification, after emulsification completes, be warming up to 70 DEG C, ammonium persulphate is made into the aqueous solution of 10wt%, slowly add in batches, initiator drips off rear continuation and continues stirring reaction 7h with 300r/min rotating speed, cooling discharging.Resulting polymers microballoon is placed and is not occurred layering in 30 days, and its interfacial tension figure shows in the diagram, and in 30,000 salinities, when microballoon concentration is 0.5%, its interfacial tension is 2.9 × 10
-2mN/M.
Embodiment 5
Raw material weight compares: white oil is 30wt%, acrylamide monomer is 18wt%, and vinylformic acid is 5%, and sorbester p18 is 4%, sorbester p17 is 3wt%, N, N methylene-bisacrylamide is 0.04wt%, and ammonium persulphate is 0.05wt%, sodium bisulfite is 0.03wt%, OP-10 is 9wt%, SAS60 is 3wt%, and tap water is surplus.By white oil, sorbester p18, sorbester p17, OP-10, SAS60 put into the there-necked flask that agitator, reflux exchanger and thermometer are housed, and 300r/min rotating speed stirs and makes solution A, with beaker, monomeric acrylamide is dissolved in water, then vinylformic acid is added, N, N-methylene-bisacrylamide, be placed on magnetic stirring apparatus and stir, add aqueous sodium hydroxide solution neutralization until completely dissolved, degree of neutralization is 75%, add sodium bisulfite to dissolving solution B processed completely, then solution B is slowly added in A, and with rotating speed 600r/min, time 30min carries out emulsification, after emulsification completes, be warming up to 70 DEG C, ammonium persulphate is made into the aqueous solution of 10wt%, slowly add in batches, be added dropwise to complete in 1h, initiator drips off rear continuation reaction 6h, cooling discharging.
This embodiment resulting polymers microballoon is placed and is not occurred layering in 30 days, and its interfacial tension figure shows in Figure 5, and in 30,000 salinities, when microballoon concentration is 0.5%, its interfacial tension is 4.3 × 10
-3mN/M.Can find out that it still has ultralow interfacial tension when salinity is 50,000 by Fig. 5 a, illustrate that it has good salt tolerance; Fig. 5 b is the stability test figure that this polymer microballoon is placed 15 days, by observing its scattering of light rate, can find out, comparatively Article 1 baseline is compared, remaining curve overlaps with Article 1 baseline substantially, and along with the prolongation of test duration, the microballoon that particle diameter is large sinks gradually, therefore increase in bottle bottom 1mm place's scattering of light rate, resistance to overturning is fine; Can find out that microballoon emulsion particle shape is the globosity of rule and size distribution is comparatively even by the transmission electron microscope picture of Fig. 5 c polymer microballoon.
Compared with prior art, polymer microballoon of the present invention has shutoff and the double effect of the displacement of reservoir oil, and its sealing ratiod can reach more than 75%, and its oil displacement efficiency can reach more than 90%, and interfacial tension is minimum is 4.3 × 10
-3mN/M, salt tolerance is up to 50,000 salinities, and common polymer microballoon salt tolerance can only reach 30,000 salinities, and does not possess oil displacement efficiency.
Although done detailed description and explanation to specific examples of the present invention above, what should indicate has been that we can make various changes and modifications above embodiment, but these do not depart from the scope of the claim appended by the present invention.
Claims (10)
1. there is a polymer microballoon temporary plugging agent for ultra low interfacial tension, it is characterized in that: described polymer microballoon temporary plugging agent is prepared from by the raw material of following weight percent:
White oil 20 ~ 40wt%, acrylamide monomer 10 ~ 25wt%, vinylformic acid 5 ~ 15wt%, sorbitan fatty acid ester 5 ~ 15wt%, N,N methylene bis acrylamide 0.03 ~ 0.08wt%, ammonium persulphate 0.01 ~ 0.05wt%, sodium bisulfite 0.01 ~ 0.08wt%, hydrophilic group tensio-active agent 10 ~ 25wt%, water surplus.
2. a kind of polymer microballoon temporary plugging agent with ultra low interfacial tension according to claim 1, is characterized in that: described hydrophilic group tensio-active agent is one or more the mixture in tween 80, TX-10, OP-10 and SAS60.
3. a kind of polymer microballoon temporary plugging agent with ultra low interfacial tension according to claim 1, is characterized in that: described sorbitan fatty acid ester is one or more the mixture in span 40, sorbester p18 and sorbester p17.
4. a kind of polymer microballoon temporary plugging agent with ultra low interfacial tension according to claim 1, is characterized in that: described water is tap water or deionized water.
5. a kind of preparation method with the polymer microballoon temporary plugging agent of ultra low interfacial tension in Claims 1-4 described in any one, is characterized in that: comprise the following steps:
1) raw material for standby is taken by weight;
2), under room temperature condition, in the container that agitator, thermometer, reflux condensate device are housed, add white oil, sorbitan fatty acid ester, hydrophilic group tensio-active agent, stir, make solution A;
3) acrylamide monomer taken, vinylformic acid, N,N methylene bis acrylamide are added to the water, stir after making it dissolve completely, add alkali lye neutralization, then add sodium bisulfite, stir and make it dissolve completely, make solution B; The mass ratio of solution A and solution B is (1 ~ 4): 1;
4) add in solution A by solution B, after fully emulsified, be warming up to 60 ~ 70 DEG C, unlatching condensing reflux, is added dropwise to ammonium persulphate, continues to be stirred to react completely after being added dropwise to complete, and be then cooled to room temperature, namely discharging after cooling obtains polymer microballoon temporary plugging agent.
6. a kind of preparation method with the polymer microballoon temporary plugging agent of ultra low interfacial tension according to claim 5, is characterized in that: step 3) in alkali lye in and adopt aqueous sodium hydroxide solution neutralization, degree of neutralization is 50 ~ 80%.
7. a kind of preparation method with the polymer microballoon temporary plugging agent of ultra low interfacial tension according to claim 5, it is characterized in that: step 4) in ammonium persulfate initiator be that the aqueous solution being 10% with mass concentration drips in batches, time for adding 45 ~ 60min.
8. a kind of preparation method with the polymer microballoon temporary plugging agent of ultra low interfacial tension according to claim 5, is characterized in that: step 4) in emulsification condition be, stirring velocity 500 ~ 600r/min, time 20 ~ 30min.
9. a kind of preparation method with the polymer microballoon temporary plugging agent of ultra low interfacial tension according to claim 5, it is characterized in that: step 4) in ammonium persulphate to be added dropwise to complete rear continuation mixing speed be 200 ~ 300r/min, the time of continuing reaction is 6 ~ 7h.
10. a kind of preparation method with the polymer microballoon temporary plugging agent of ultra low interfacial tension according to claim 5, is characterized in that: step 2) medium speed is 200 ~ 300r/min.
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| CN109652042A (en) * | 2018-11-15 | 2019-04-19 | 陕西丰登石化有限公司 | Agent and preparation method thereof is adopted in a kind of increasing of intelligent nano microballoon transfer drive |
| CN110698589A (en) * | 2019-10-30 | 2020-01-17 | 海塔石油科技有限公司 | High-molecular profile control and plugging agent, and preparation method and application thereof |
| CN112851856A (en) * | 2021-01-29 | 2021-05-28 | 陕西科技大学 | Salt-tolerant polymer microsphere plugging agent and preparation method thereof |
| US20230050157A1 (en) * | 2021-08-12 | 2023-02-16 | Shaanxi University Of Science & Technology | Salt-tolerant polymer microsphere plugging agent and preparation method thereof |
| US11629282B2 (en) * | 2021-08-12 | 2023-04-18 | Shaanxi University Of Science & Technology | Salt-tolerant polymer microsphere plugging agent and preparation method thereof |
| CN116178619A (en) * | 2022-12-14 | 2023-05-30 | 汉中聚智达远环能科技有限公司 | Polymer nano microsphere plugging agent and preparation method thereof |
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