CN100572494C - Microcapsule that retarding oil gas well working fluid additive discharges and preparation method thereof - Google Patents
Microcapsule that retarding oil gas well working fluid additive discharges and preparation method thereof Download PDFInfo
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- CN100572494C CN100572494C CNB2007101137590A CN200710113759A CN100572494C CN 100572494 C CN100572494 C CN 100572494C CN B2007101137590 A CNB2007101137590 A CN B2007101137590A CN 200710113759 A CN200710113759 A CN 200710113759A CN 100572494 C CN100572494 C CN 100572494C
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Abstract
The invention provides microcapsule of a kind of retarding oil gas well working fluid additive release and preparation method thereof, belong to the oilfield chemistry field.The microcapsule of being invented are made up of oil gas well working fluid additive 3.5～25%, silico-aluminate bead 70～94%, polymeric film 2～5%, wherein oil gas well working fluid additive is a kind of in oil well cement early strength coagulant, gel strength promotor, retardant or fracturing liquid linking agent, the gel breaker, and the silico-aluminate bead is particle diameter 10～250 μ m, pore volume 0.20～0.60cm
3The spent catalyst of/g, polymeric film are the non-soluble polymers of relative molecular mass 2～300,000.Prepared microcapsule delays that releasing effect is good, resistance to compression, heatproof, and is applied widely.The main raw material(s) silico-aluminate bead of preparation microcapsule belongs to refuse reclamation, not only economy but also environmental protection, and microcapsule preparation technology of the present invention in addition is simple, and production cost is low, helps suitability for industrialized production.
Description
Technical field
The present invention relates to microcapsule of a kind of retarding oil gas well working fluid additive release and preparation method thereof, relate in particular to microcapsule of a kind of energy retarding oil gas well well cementation early strength coagulant, gel strength promotor, retardant and aqueous fracturing fluid linking agent, gel breaker release and preparation method thereof, belong to the oilfield chemistry field.
Background technology
In the well cementation of oil gas well shallow-layer section, deep water cementing or cold district well cementation process, often need add a certain amount of early strength coagulant in order to shorten the grout curing time, but the adding of early strength coagulant makes the grout retrogradation undoubtedly, grout is just big, mobile very poor as denseness, even grout loses pumpability; At the well cementation that has water/has channeling stream, the normal gel strength promotor that adds the quiet gel strength development of promotion grout in the grout, with shorten cementitious grout intensity from 48Pa-240Pa " transit time " thus reach the anti-channeling purpose, but gel strength promotor equally also can make grout retrogradation, mobile variation; In long CEMENTING SECTION, because grout temperature up and down differs too big, for the normal retardant that adds of the thickening time that guarantees grout under the high temperature, yet retardant is but to producing time of coagulation of top water mud excessive delayed coagulation, occur that the bottom grout solidifies and top water mud still is " sposh " shape, seriously prolong oil gas well construction cycle.
Waterfrac treatment is a kind of effective well stimulation, and fracturing liquid is the important component part of waterfrac treatment technology, if fracturing liquid owner aqueous fracturing fluid commonly used as making the medium that stitches and carry propping agent.Aqueous fracturing fluid mainly adopts polymkeric substance (as hydroxypropyl guanidine glue etc.) to be cross-linked to form frozen glue with linking agents such as borax, boric acid to increase fracturing liquid viscosity with suspension high-strength ceramsite sand, but this directly crosslinked method makes fracturing liquid very big at pipeline mobile frictional resistance, cause the waterfrac treatment operation pressure very high, the dangerous energy consumption of also wasting; In addition, after pressure break is made seam and finished, often require fracturing liquid break glue fast, become low-viscosity (mobile) liquid and in time return and drain into ground,, need to add a certain amount of gel breaker for this reason with the pollution of the polymer residue in the minimizing fracturing liquid to hydrocarbon zone.Yet traditional gel breaker (as superoxide, enzyme etc.) is directly to join in the fracturing liquid with polymkeric substance, linking agent etc., and is very big to of the fracturing fluid performance impact.If excessive or constant adds, cross-linking properties may occur and reduce rapidly, break the glue phenomenon in advance, cause the sand plug of constructing; If the amount of owing adds, then frozen glue may break the bad even not broken glue of glue, causes the fracturing liquid row of returning in time, will cause serious injury reservoir.For slowly-releasing, the controlled-release function of realizing gel breaker, the gel breaker microcapsule of polymkeric substance parcel have been developed, though can play certain extended release effect to gel breaker, but it is this very little by gel breaker microcapsule self bearing capacity that polymkeric substance wrapped up merely, for the frac job of high pressure, microcapsule often break in advance, and its scope of application and effect are very limited.
How to make the admixture of oil gas well working fluid can realize delaying release function, thereby make the oil gas well working fluid performance have adjustable controlled feature, this will be very meaningful research work.Realizing that by microencapsulation technology the time-delay of active ingredient in the microcapsule discharges or regularly discharges, is the focus and the difficult point of current oil gas well working fluid additive research.The research of this respect at present mainly contains patent CN1786101A (2006,6,4), and it is by high molecular polymer oxidant package such as persulphate, hypochlorite to be wrapped, and adopts the prepared gel breaker microcapsule of side jet flow bed process; Patent CN1944571A (2007,4,11) utilizes tensio-active agent to make the liquid film type microcapsule deep water blocking agent that coating obtains activators such as water glass, formaldehyde parcel.The above microcapsule to delay release action limited, preparation technology is complicated, and self bearing capacity is very little, can't satisfy pump pressure is higher, temperature is higher cementing well operation and waterfrac treatment operation etc.
Summary of the invention
The purpose of this invention is to provide microcapsule of a kind of retarding oil gas well working fluid additive release and preparation method thereof.Have excellent pressure-bearing, temperature resistant capability and delay release performance by the inventive method prepared microcapsule, it there is not influence substantially to the performance of oil gas well working fluid unwanted the time, can better realize the purpose controlled to the oil gas well working fluid performance.
The object of the present invention is achieved like this, the microcapsule that the retarding oil gas well working fluid additive that is proposed discharges are made up of oil gas well working fluid additive 3.5～25%, porous silicoaluminate bead 70～94%, polymeric film 2～5%, wherein oil gas well working fluid additive can be a kind of in oil well cement early strength coagulant, gel strength promotor, retardant or aqueous fracturing fluid linking agent, the gel breaker, and the porous silicoaluminate bead can particle diameter be that 10～250 μ m, pore volume are 0.20～0.60cm
3In the useless microspherodiale silica-alumina catalyst of/g, useless rare earth Y type zeolite catalyzer, useless carclazyte y-type zeolite catalyzer or the useless hydrogenation catalyst cracking catalyst one or several, polymeric film can be one or more in the non-soluble polymer.
Oil well cement early strength coagulant of the present invention can be CaCl
2, KCl, CaO, Na
2SO
4, Al
2(SO
4)
3, NaNO
2, Na
2CO
3, NH
4Among the Cl one or more.
Oil well cement gel strength promotor of the present invention can be Ca (AlO
2)
2, NaAlO
2, KAlO
2, Li
2CO
3, LiNO
3In one or more.
Oil well cement retarder of the present invention can be one or more in citric acid, sodium tartrate, borax, boric acid, sulfonated lignin, alkylphosphonic, Sunmorl N 60S, the sodium glucoheptonate.
Aqueous fracturing fluid linking agent of the present invention can be a kind of in borax, boric acid, the zirconium oxychloride.
Aqueous fracturing fluid gel breaker of the present invention can be a kind of in ammonium persulphate, Potassium Persulphate, clorox, the potassium permanganate.
The preparation method that retarding oil gas well working fluid additive of the present invention discharges microcapsule mainly comprised for three steps:
I, oil gas well working fluid additive is made into mass percentage concentration is 3～40% solution, then 1 part of solution and 1.0～2.0 parts of porous silicoaluminate beads is mixed under room temperature, treat fully absorption saturated after with its oven dry, obtain the core material material;
II, non-soluble polymer is joined in the organic solvent, be mixed with mass percentage concentration and be 1.8～3.5% shell material solution;
III, 1 part of core material material is dispersed in 1.0～2.0 parts of shell material solution, in 70～100 ℃ of air-flows, carries out spray drying treatment, the organic solvent of dissolving shell material is evaporated rapidly, thereby shell material is solidified and the core material micro encapsulation.
Non-soluble polymer shell material of the present invention can be one or more in methylcellulose gum, ethyl cellulose, Nitrocellulose, cellulose acetate, polyvinylacetal, polyvinyl butyral acetal, the hp-ldpe resin, and relative molecular weight is 2～300,000.
Organic solvent of the present invention can be one or more in ethanol, Virahol, ether, acetone, hexanaphthene, the tetracol phenixin.
The present invention has solved the existing deficiency of existing casing-head gas working fluid additive from following four aspects.(1) the microcapsule core material of the high intensity, porous silico-aluminate bead conduct of oil gas well working fluid additive has been adsorbed in utilization, has realized the release that delays of oil gas well working fluid additive as the Microencapsulation Method of shell material with non-soluble polymer; (2) prepared microcapsule of the present invention has excellent resistance to compression, heatproof and delays release performance, and is applied widely; (3) the present invention's main raw material(s) silico-aluminate bead of preparing microcapsule belongs to refuse reclamation, not only economy but also environmental protection; (4) microcapsule preparation technology of the present invention is simple, and production cost is low, helps suitability for industrialized production.
Embodiment
Embodiment 1, the preparation of early strength coagulant microcapsule and performance evaluation
Preparation 20%Al
2(SO
4)
31 part of solution adds 1.2 parts of porous silicoaluminate beads (useless microspherodiale silica-alumina catalyst, China Petroleum Univ. (East-China) wins magnificent refinery), after waiting to adsorb 20min, the porous silicoaluminate bead is dried; Take by weighing 2.2 parts of ethyl cellulose and 0.8 part of polyvinyl butyral acetal joins in the mixed organic solvents of 70 parts of acetone and 30 parts of cyclohexanes, make 3.0% shell material solution; Take by weighing 1 part and adsorbed Al
2(SO
4)
3The porous silicoaluminate bead joins in 1.5 part 3.0% the shell material solution, carries out spray drying treatment in 95 ℃ of air-flows, makes the early strength coagulant microcapsule, and code name is sample A.
The sample A that in winning Weihe River oil well G class g cement, adds certain mass percentage ratio (is benchmark with the cement quality), it by GB10238-88 standard fabrication water cement ratio 0.44 grout, by the influence of the oil and gas industry standard SY/T 5546-92 of the People's Republic of China (PRC) " oil well cement application performance test method " working sample A to oil well G class g cement thickening time, ultimate compression strength, experimental result is as shown in table 1 then.From table 1, can find out the early strength acceleration substance A l among the sample A
2(SO
4)
3Delaying time in grout discharges, and its grout initial stage consistency change is starkly lower than and directly adds equal in quality fractional Al
2(SO
4)
3Mortar architecture, and the adding of early strength coagulant microcapsule sample A does not have influence substantially to strength of cement.
Table 1
Embodiment 2, the preparation and the performance evaluation of gel strength setting accelerator microcapsule
Preparation 30%NaAlO
21 part of solution adds 1.2 parts of porous silicoaluminate beads (useless carclazyte y-type zeolite catalyzer, China Petroleum Univ. (East-China) wins magnificent refinery), after waiting to adsorb 20min, the porous silicoaluminate bead is dried; Take by weighing 1.8 parts of ethyl cellulose and 0.7 part of polyvinyl butyral acetal joins in the mixed organic solvents of 75 parts of acetone and 25 parts of hexanaphthenes, make 2.5% shell material solution; Take by weighing 1 part and adsorbed NaAlO
2The porous silicoaluminate bead joins in 1.5 part 2.5% the shell material solution, carries out spray drying treatment in 80 ℃ of air-flows, makes gel strength promotor microcapsule, and code name is sample B.
The sample B that in winning Weihe River oil well G class g cement, adds certain mass percentage ratio (is benchmark with the cement quality), it by GB10238-88 standard fabrication water cement ratio 0.44 grout, press the oil and gas industry standard SY/T 5546-92 of the People's Republic of China (PRC) " oil well cement application performance test method " working sample B then to the oil well G influence of class g cement thickening time, utilize the quiet gel strength of the happy industrial instrumentation of the U.S.'s thousand morals 5265U of company type/ultrasonic wave compressive strength determination instrument come assess sample B to the quiet gel strength of grout from the 48Pa-240Pa influence of " transit time ", experimental result is as shown in table 2.Can find out that from table 2 gel strength among the sample B promotes material NaAlO
2In grout, can realize the purpose that time-delay discharges, thereby effectively reduce the favourable infusion of initial consistency of grout, simultaneously to cementitious grout intensity " transit time " without any disadvantageous effect, make gel strength " transit time " that shortening is arranged approximately on the contrary.
Table 2
Embodiment 3, the preparation of retardant microcapsule and performance evaluation
Prepare 1 part of 20% citric acid solution, add 1.2 parts of porous silicoaluminate beads (useless rare earth Y type zeolite catalyzer, China Petroleum Univ. (East-China) wins magnificent refinery), after waiting to adsorb 20min, the porous silicoaluminate bead is dried; Take by weighing 1.5 parts of ethyl cellulose and 1.5 parts of polyvinyl butyral acetals join in the mixed organic solvents of 60 parts of acetone and 40 parts of hexanaphthenes, make 3.0% shell material solution; Take by weighing 1 part and adsorbed in the shell material solution that citric acid porous silicoaluminate bead joins 1.5 part 3.0%, carry out spray drying treatment in 95 ℃ of air-flows, make the retardant microcapsule, code name is sample C.
The sample C that in winning Weihe River oil well G class g cement, adds certain mass percentage ratio (is benchmark with the cement quality), it by GB10238-88 standard fabrication water cement ratio 0.44 grout, by the influence of the oil and gas industry standard SY/T 5546-92 of the People's Republic of China (PRC) " oil well cement application performance test method " working sample C to oil well G class g cement thickening time, ultimate compression strength, experimental result is as shown in table 3 then.From table 3, can find out, the citric acid that is wrapped up among the sample C shows in grout and is subjected to the temperature controlled release phenomenon that delays, its citric acid at high temperature discharges fast and slow in the next release of lower temperature, can effectively control the thickening time of grout under condition of different temperatures, guarantee that grout all has more approaching thickening time and high compression strength in than large-temperature range, avoided the slow deficiency of serious slow setting of direct adding citric acid low temperature that retardant shows or ultimate compression strength development.
Table 3
| Retardant | Citric acid | Sample C |
| Dosage (%) | 0.2 | 1.5 |
| Citric acid effective content (%) in the cement | 0.2 | 0.2 |
| 50 ℃, 20MPa thickening time (h:min) | 10:57 | 5:10 |
| 70 ℃, 35MPa thickening time (h:min) | 5:62 | 3:28 |
| 90 ℃, 50MPa thickening time (h:min) | 2:55 | 3:43 |
| 50 ℃, 24h ultimate compression strength (MPa) | 1.37 | 13.20 |
| 70 ℃, 24h ultimate compression strength (MPa) | 10.19 | 17.57 |
| 90 ℃, 24h ultimate compression strength (MPa) | 19.62 | 18.90 |
Embodiment 4, the preparation of linking agent microcapsule and performance evaluation
Prepare 1 part of 5.0% borax soln, add 1.2 parts of porous silicoaluminate beads (useless hydrogenation catalyst cracking catalyst, Daqing petrochemical factory), after waiting to adsorb 20min, the porous silicoaluminate bead is dried; Take by weighing 2.0 parts of Nitrocelluloses and join in 80 parts of acetone and the 20 parts of alcoholic acid mixed organic solvents, make 2.0% shell material solution; Take by weighing 1 part of porous silicoaluminate bead that has adsorbed borax and join in 1.3 part 2.0% the shell material solution, carry out spray drying treatment in 80 ℃ of air-flows, make the linking agent microcapsule, code name is sample D.
By the oil and gas industry standard SY/T 5107-2005 of the People's Republic of China (PRC) " aqueous fracturing fluid method of evaluating performance " preparation 0.5% hydroxypropyl guanidine glue (HPG) water-based fracturing base fluid, the sample D that in base fluid, adds certain mass percentage ratio then, estimate the crosslinking time of linking agent microcapsule, experimental result is as shown in table 4.Can find out that from table 4 the cross-linked material borax among the sample D can realize delaying to discharge purpose in the water-based fracturing base fluid, suitably postponed the of the fracturing fluid one-tenth frozen glue time, help reducing the frictional resistance of fracturing liquid in pipeline flows.
Table 4
| Linking agent | Dosage | Borax effective content in the solution | Crosslinking time |
| Borax | 0.05％ | 0.05％ | 25 seconds |
| Sample D | 1.3％ | 0.05％ | 10 minutes 37 seconds |
Embodiment 5, the preparation of gel breaker microcapsule and performance evaluation
Prepare 1 part of 20% potassium persulfate solution, add 1.2 parts of porous silicoaluminate beads (useless hydrogenation catalyst cracking catalyst, Daqing petrochemical factory), after waiting to adsorb 20min, the porous silicoaluminate bead is dried; Take by weighing 1.8 parts of ethyl cellulose and 1.2 parts of polyvinyl butyral acetals join in the mixed organic solvents of 70 parts of acetone and 30 parts of hexanaphthenes, make 3.0% shell material solution; Take by weighing 1 part of porous silicoaluminate bead that has adsorbed Potassium Persulphate and join in 1.5 part 3.0% the shell material solution, carry out spray drying treatment in 90 ℃ of air-flows, make the gel breaker microcapsule, code name is sample E.
The sample E that in the fracturing base fluid of 0.5% hydroxypropyl guanidine glue (HPG)+0.05% borax linking agent, adds certain mass percentage ratio, by the oil and gas industry standard SY/T 6380-1998 of the People's Republic of China (PRC) " pressure break gel breaker method for testing performance " standard, adopt RV20 rotary viscosity design determining fracturing base fluid at 70 ℃, 170s
-1Viscosity number under the shearing rate changes the broken glue ability of coming assess sample E in time, and experimental result is as shown in table 5.From table 5, can find out, less at experiment initial stage sample E to fracturing liquid apparent viscosity decline influence, help pressing crack construction stage fracturing liquid suspended prop; Along with time lengthening, the Potassium Persulphate that wraps up in the microcapsule discharges gradually fully, and it is very low that the fracturing liquid apparent viscosity is dropped to, the row of returning after helping pressure break and finishing.The prepared gel breaker microcapsule of experimental result explanation the present invention have the good releasability that delays.
Table 5
Claims (8)
1. the microcapsule that discharge of a retarding oil gas well working fluid additive, it is characterized in that it is made up of oil gas well working fluid additive 3.5～25%, porous silicoaluminate bead 70～94%, polymeric film 2～5%, wherein oil gas well working fluid additive is a kind of in oil well cement early strength coagulant, gel strength promotor, retardant or aqueous fracturing fluid linking agent, the gel breaker, and the porous silicoaluminate bead is that particle diameter is that 10～250 μ m, pore volume are 0.20～0.60cm
3In the useless microspherodiale silica-alumina catalyst of/g, useless rare earth Y type zeolite catalyzer, useless carclazyte y-type zeolite catalyzer or the useless hydrogenation catalyst cracking catalyst one or several, polymeric film is one or more in methylcellulose gum, ethyl cellulose, Nitrocellulose, cellulose acetate, polyvinylacetal, polyvinyl butyral acetal, the hp-ldpe resin, and the relative molecular weight of described polymkeric substance is 2～300,000.
2. the microcapsule that retarding oil gas well working fluid additive according to claim 1 discharges is characterized in that described oil well cement early strength coagulant can be CaCl
2, KCl, CaO, Na
2SO
4, Al
2(SO
4)
3, NaNO
2, Na
2CO
3, NH
4Among the Cl one or more.
3. the microcapsule that retarding oil gas well working fluid additive according to claim 1 discharges is characterized in that described oil well cement gel strength promotor can be Ca (AlO
2)
2, NaAlO
2, KAlO
2, Li
2CO
3, LiNO
3In one or more.
4. the microcapsule that retarding oil gas well working fluid additive according to claim 1 discharges is characterized in that described oil well cement retarder can be one or more in citric acid, sodium tartrate, borax, boric acid, sulfonated lignin, alkylphosphonic, Sunmorl N 60S, the sodium glucoheptonate.
5. the microcapsule that retarding oil gas well working fluid additive according to claim 1 discharges is characterized in that described aqueous fracturing fluid linking agent can be a kind of in borax, boric acid, the zirconium oxychloride.
6. the microcapsule that retarding oil gas well working fluid additive according to claim 1 discharges is characterized in that described aqueous fracturing fluid gel breaker can be a kind of in ammonium persulphate, Potassium Persulphate, clorox, the potassium permanganate.
7. the preparation method of the microcapsule that discharge of a retarding oil gas well working fluid additive is characterized in that mainly comprising three steps:
I, oil gas well working fluid additive is made into mass percentage concentration is 3～40% solution, then 1 mass parts solution and 1.0～2.0 mass parts porous silicoaluminate beads are mixed under room temperature, treat fully absorption saturated after with its oven dry, obtain the core material material;
II, be 2～300,000 polymkeric substance with relative molecular weight: one or more in methylcellulose gum, ethyl cellulose, Nitrocellulose, cellulose acetate, polyvinylacetal, polyvinyl butyral acetal, the hp-ldpe resin join in the organic solvent, are mixed with mass percentage concentration and are 1.8～3.5% shell material solution;
III, 1 mass parts core material material is dispersed in 1.0～2.0 mass parts shell material solution, in 70～100 ℃ of air-flows, carries out spray drying treatment, the organic solvent of dissolving shell material is evaporated rapidly, thereby shell material is solidified and the core material micro encapsulation.
8. the preparation method of the microcapsule that retarding oil gas well working fluid additive according to claim 7 discharges is characterized in that described organic solvent is one or more in ethanol, Virahol, ether, acetone, hexanaphthene, the tetracol phenixin.
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| US4741401A (en) * | 1987-01-16 | 1988-05-03 | The Dow Chemical Company | Method for treating subterranean formations |
-
2007
- 2007-09-06 CN CNB2007101137590A patent/CN100572494C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4202795A (en) * | 1978-09-28 | 1980-05-13 | Halliburton Company | Methods and additives for delaying the release of chemicals in aqueous fluids |
| US4741401A (en) * | 1987-01-16 | 1988-05-03 | The Dow Chemical Company | Method for treating subterranean formations |
Non-Patent Citations (4)
| Title |
|---|
| 微胶囊包裹化学生热压裂液破胶技术. 吴金桥等.石油钻采工艺，第27卷第3期. 2005 |
| 微胶囊包裹化学生热压裂液破胶技术. 吴金桥等.石油钻采工艺，第27卷第3期. 2005 * |
| 胶囊破胶剂优选方法探讨. 柴巧玲等.内蒙古石油化工，第2006年第7期卷. 2006 |
| 胶囊破胶剂优选方法探讨. 柴巧玲等.内蒙古石油化工，第2006年第7期卷. 2006 * |
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|---|---|
| CN101144011A (en) | 2008-03-19 |
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