CN101928556A - Five-membered copolymer fluid loss agent and preparation method thereof - Google Patents
Five-membered copolymer fluid loss agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a five-membered copolymer fluid loss agent and a preparation method thereof, which is used for drilling fluid and completion fluid in the drilling engineering of oil and gas fields. The five-membered copolymer fluid loss agent can improve the high-temperature resistant performance, performance for inhibiting shale expansion, salt tolerant performance and the like for fluid loss agent. The technical scheme is as follows: the raw materials for preparing the fluid loss agent comprise acrylamide A, acrylonitrile B, crylic acid C, 2-acrylamide-2-methylpropanesulfonic acid D and vinyl ammonium salt cation monomer E. Water is served as solvent, NaOH solution is pH value modifier, and (NH4)2S2O8 and NaHSO3 are served as initiators. C, D and E are dissolved in water according to the molar ratio of 13-15:10:8, and NaOH solution is used for regulating pH to 6-8; then, A and B are added at the molar ratio of 66-63:3-4; mixed liquor is heated to 40-55 DEG C; the initiators are added to be stirred for 10min; the obtained mixture stands and reacts at the constant temperature for 3-5h; finally, alcohol is adopted for purifying; and the product is cut, prilled and dried to obtain the five-membered copolymer fluid loss agent. The five-membered copolymer fluid loss agent has good temperature resistant performance and salt tolerant performance. The method has high yield and can be used for drilling fluid and completion fluid.
Description
Technical field
The present invention relates to a kind of five-membered copolymer fluid loss agent that is used for oilfield drilling engineering drilling fluid and well finishing liquid and preparation method thereof.
Background technology
Along with drilling strata is increasingly sophisticated, and countries in the world deep-well, exceptional well, ultra deep well and the increase of complicated well quantity, the drilling fluid Technology has been proposed more and more higher requirement.Practice shows, additive for drilling fluid is the key that guarantees the drilling fluid premium properties, for realize drilling operation safely and fast with higher comprehensive benefit, require drilling fluid to have the function of suitable leak-off building capacity, rheological, stabilizing borehole, high temperature resistance, salt tolerant, thereby fluid loss agent become one of volume of production and marketing maximum, the most active additive for drilling fluid of research and development.Fluid loss agent commonly used at present has latex, modified natural polymer fluid loss agents such as the Mierocrystalline cellulose of modification, xylogen, brown coal, tannin, non-ionic type, polyamine cation types such as polyvinyl alcohol, polyoxyethylene, PVP, anionic fluid loss agents such as hydrolysis polypropylene cyanogen, hydrolysed polyacrylic, polysulfonate, these fluid loss agents can not satisfy the requirement of present drilling fluid Technology fully.Therefore, the fluid loss agent of the high temperature resistance of the suitable present drilling well requirement of exploitation, salt tolerant, stabilizing borehole, inhibition shale expansion is the focus of studying at present.The direction of main research: (1) carries out modification to the natural polymer product, such as starch is carried out graft copolymerization, by the anionic group (SO of some high temperature resistances of grafting, salt tolerant
3 -) and the development shale expansion cation group (NH
3+).(2) by preferred existing ion monomer that cost is lower, raw material is easy to get or the extraordinary monomer of development of new, obtain amphoteric ion polymer fluid loss additive by polymerization.(3) exploitation environment-friendly type fluid loss agent, more abroad to this respect research and development, obtain polymer fluid loss agent or exploitation and natural product similar with the crosslinked lower molecular weight polymer of degradable crosslinker, the degradable synthetic macromolecule fluid loss agent of microorganism.
Summary of the invention
The objective of the invention is to for the high temperature resistance that improves fluid loss agent, suppress performances such as shale expansion, salt tolerant, make preparation method's mild condition, controlled, the spy provides a kind of five-membered copolymer fluid loss agent and preparation method thereof.
A kind of five-membered copolymer fluid loss agent, it is characterized in that: the amount of substance for preparing the raw materials used and component of this fluid loss agent is such as down, wherein the unit of amount of substance is a mole, mass unit is gram, raw material A is an acrylamide, and raw material B is a propylene cyanogen, and raw material C is a vinylformic acid, raw material D is 2-acrylamide-2-methyl propane sulfonic acid, and raw material E is vinyl ammonium salt cationic monomer, is with methylacryoyloxyethyl trimethyl ammonium chloride code name DMC or dimethyl diallyl ammonium chloride code name DMDAAC; Wherein the mol ratio of A: B: C: D: E is 66: 3: 13: 10: 8 or 63: 4: 15: 10: 8; PH regulator agent mass percentage concentration is 20% NaOH solution, and the pH value transfers to 6～8; The initiator redox system is that ammonium persulphate and sodium bisulfite, mol ratio are 1: 1, and initiator amount is 0.7%～1.6% of a monomer total mass; Solvent is a water, and the quality of water is 7: 3 with the ratio of monomer total mass; The purification solvent is a dehydrated alcohol.
To achieve these goals, technical scheme of the present invention is: a kind of preparation method of five-membered copolymer fluid loss agent is characterized in that following steps:
1) it is 13: 10: 8 or 15: 10: 8 with vinylformic acid and 2-acrylamide-2-methyl propane sulfonic acid and ethene ammonium salt cationic monomer mol ratio, soluble in water, the quality of water is 7: 3 with the ratio of monomer total mass, be the pH value that 20% sodium hydroxide solution is adjusted system with mass percentage concentration then, the pH value is 6～8, gets mixing solutions G;
2) in mixing solutions G, add acrylamide and propylene cyanogen, mol ratio is 66: 3 or 63: 4, and wherein the mol ratio of A: B: C: D: E is 66: 3: 13: 10: 8 or 63: 4: 15: 10: 8, get mixing solutions H, the mass percentage concentration of mixing solutions H is 30%;
3) mixing solutions H is heated to 40～55 ℃, add initiator ammonium persulfate and sodium bisulfite successively, mol ratio is 1: 1, initiator amount is 0.7%～1.6% of a monomer total mass, constantly stirs reaction 10min down, observe viscosity, standing and reacting 3～5h in water bath with thermostatic control;
4) top products therefrom is taken out, purify, obtain the oyster white colloidal solid,, promptly get the five-membered copolymer fluid loss agent product in 120 ℃ of oven dry down, pulverizing with the solid product shear granulation with dehydrated alcohol.
Described acrylamide (AM), vinylformic acid (AA), vinyl cyanide (AN), 2-acrylamide-2-methyl propane sulfonic acid (AMPS), vinyl ammonium salt cationic monomer (CM), ammonium persulphate, sodium bisulfite, sodium hydroxide is analytical pure, and the Long Huagongshijichang of Chengdu section produces.
Above-mentioned five-membered copolymer fluid loss agent product is used for fresh water, salt solution, saturated brine, compound brine mud, excellent filtration reduction energy is arranged.1.0% fluid loss agent makes the filter loss in the fresh water base slurry reach 7.2mL/30min, and the filter loss that 180 ℃ of heat are rolled behind the aging 16h is 10.6mL/30min.2.0% fluid loss agent makes the filter loss in the brine mud drop to 14.4mL from 78.6mL.Reach 120 ℃ of heat of fluid loss agent of 1.0% and roll the shale rate of recovery 73.4% behind the 16h.This fluid loss agent high temperature resistance of surface is strong, salt tolerant is better, shale inhibition is better.
The invention has the beneficial effects as follows:
1, the anionic group (SO in the five-membered copolymer fluid loss agent of the present invention
3 -), have good temperature resistance and anti-salt effect, thereby guarantee its filtration reduction under high temperature and high salt concentration; Anionic group (COO in this fluid loss agent
-), increased aquation group and adsorptive power greatly, improve the filtration reduction energy of polymkeric substance; Also has the cation group (NH in this fluid loss agent
3+) can strengthen the absorption of fluid loss agent at surface of clay, suppress hydration and expansion of clay ,-NH
3+Can snap in the mesh in the clay lattice, increase the probability that the fluid loss agent molecule stops up pore, improve filtration property.
2, the inventive method, productive rate is higher, favorable reproducibility, mild condition is controlled, acrylamide and vinylformic acid and 2-acrylamide-2-methyl propane sulfonic acid wide material sources, cost is low.
Embodiment
Embodiment 1:
A kind of five-membered copolymer fluid loss agent and preparation method thereof, it comprises the steps:
1) with vinylformic acid 0.041mol, 2-acrylamide-2-methyl propane sulfonic acid 0.032mol, methylacryoyloxyethyl trimethyl ammonium chloride 0.025mol, be dissolved in the 70mL water, be the pH value that 20% sodium hydroxide solution is adjusted system with mass percentage concentration then, the pH value is 7, must mixing solutions G;
2) in mixing solutions G, add acrylamide 0.208mol, propylene cyanogen 0.010mol, get mixing solutions H, the mass percentage concentration of mixing solutions H is 30%;
3) mixing solutions H is heated to 50 ℃, add initiator ammonium persulfate and sodium bisulfite successively, mol ratio is 1: 1, initiator amount is 1.6% of a monomer total mass, constantly stirs reaction 10min down, observe viscosity, standing and reacting 3h in water bath with thermostatic control;
4) top products therefrom is taken out, purify, obtain the oyster white colloidal solid,, promptly get the five-membered copolymer fluid loss agent product in 120 ℃ of oven dry down, pulverizing with the solid product shear granulation with dehydrated alcohol.
Described acrylamide (AM), vinylformic acid (AA), vinyl cyanide (AN), 2-acrylamide-2-methyl propane sulfonic acid (AMPS), methylacryoyloxyethyl trimethyl ammonium chloride (DMC), ammonium persulphate, sodium bisulfite, sodium hydroxide is analytical pure, and the Long Huagongshijichang of Chengdu section produces.
Embodiment 2:
A kind of five-membered copolymer fluid loss agent and preparation method thereof, it comprises the steps:
1) with vinylformic acid 0.047mol, 2-acrylamide-2-methyl propane sulfonic acid 0.032mol, dimethyl diallyl ammonium chloride 0.025mol, be dissolved in the 70mL water, be the pH value that 20% sodium hydroxide solution is adjusted system with mass percentage concentration then, the pH value is 7, must mixing solutions G;
2) in mixing solutions G, add acrylamide 0.199mol, propylene cyanogen 0.012mol, get mixing solutions H, the mass percentage concentration of mixing solutions H is 30%;
3) mixing solutions H is heated to 50 ℃, add initiator ammonium persulfate and sodium bisulfite successively, mol ratio is 1: 1, initiator amount is 1.6% of a monomer total mass, constantly stirs reaction 10min down, observe viscosity, standing and reacting 3h in water bath with thermostatic control;
4) top products therefrom is taken out, purify, obtain the oyster white colloidal solid,, promptly get the five-membered copolymer fluid loss agent product in 120 ℃ of oven dry down, pulverizing with the solid product shear granulation with dehydrated alcohol.
Described acrylamide (AM), vinylformic acid (AA), vinyl cyanide (AN), 2-acrylamide-2-methyl propane sulfonic acid (AMPS), dimethyl diallyl ammonium chloride (DMDAAC), ammonium persulphate, sodium bisulfite, sodium hydroxide is analytical pure, and the Long Huagongshijichang of Chengdu section produces.
Embodiment 3:
A kind of five-membered copolymer fluid loss agent and preparation method thereof, it comprises the steps:
1) with vinylformic acid 0.043mol, 2-acrylamide-2-methyl propane sulfonic acid 0.033mol, methylacryoyloxyethyl trimethyl ammonium chloride 0.026mol, be dissolved in the 70mL water, be the pH value that 20% sodium hydroxide solution is adjusted system with mass percentage concentration then, the pH value is 8, must mixing solutions G;
2) in mixing solutions G, add acrylamide 0.217mol, propylene cyanogen 0.010mol, get mixing solutions H, the mass percentage concentration of mixing solutions H is 30%;
3) mixing solutions H is heated to 45 ℃, add initiator ammonium persulfate and sodium bisulfite successively, mol ratio is 1: 1, initiator amount is 1.0% of a monomer total mass, constantly stirs reaction 10min down, observe viscosity, standing and reacting 5h in water bath with thermostatic control;
4) top products therefrom is taken out, purify, obtain the oyster white colloidal solid,, promptly get the five-membered copolymer fluid loss agent product in 120 ℃ of oven dry down, pulverizing with the solid product shear granulation with dehydrated alcohol.
Described acrylamide (AM), vinylformic acid (AA), vinyl cyanide (AN), 2-acrylamide-2-methyl propane sulfonic acid (AMPS), methylacryoyloxyethyl trimethyl ammonium chloride (DMC), ammonium persulphate, sodium bisulfite, sodium hydroxide is analytical pure, and the Long Huagongshijichang of Chengdu section produces.
Embodiment 4:
A kind of five-membered copolymer fluid loss agent and preparation method thereof, it comprises the steps:
1) with vinylformic acid 0.049mol, 2-acrylamide-2-methyl propane sulfonic acid 0.033mol, dimethyl diallyl ammonium chloride 0.026mol, be dissolved in the 70mL water, be the pH value that 20% sodium hydroxide solution is adjusted system with mass percentage concentration then, the pH value is 8, must mixing solutions G;
2) in mixing solutions G, add acrylamide 0.207mol, propylene cyanogen 0.013mol, get mixing solutions H, the mass percentage concentration of mixing solutions H is 30%;
3) mixing solutions H is heated to 45 ℃, add initiator ammonium persulfate and sodium bisulfite successively, mol ratio is 1: 1, initiator amount is 1.0% of a monomer total mass, constantly stirs reaction 10min down, observe viscosity, standing and reacting 5h in water bath with thermostatic control;
4) top products therefrom is taken out, purify, obtain the oyster white colloidal solid,, promptly get the five-membered copolymer fluid loss agent product in 120 ℃ of oven dry down, pulverizing with the solid product shear granulation with dehydrated alcohol.
Described acrylamide (AM), vinylformic acid (AA), vinyl cyanide (AN), 2-acrylamide-2-methyl propane sulfonic acid (AMPS), dimethyl diallyl ammonium chloride (DMDAAC), ammonium persulphate, sodium bisulfite, sodium hydroxide is analytical pure, and the Long Huagongshijichang of Chengdu section produces.
Embodiment 5:
A kind of performance analysis of five-membered copolymer fluid loss agent, the five-membered copolymer fluid loss agent that embodiment 1 is prepared carries out performance evaluation, and evaluation result is as follows:
1. high temperature resistance and rheological evaluation
In order to estimate the temperature resistance of synthetic copolymer, fresh-water drilling fluid, salt-water drilling fluid (NaCl of adding 4% in the 1L 6% sodium bentonite base slurry), saturated salt-water drilling fluid (NaCl of adding 36% in the sodium bentonite base slurry of 1L 6%) and the composite salt aqueous drilling fluid that will contain fluid loss agent (add 45g NaCl in the 1L distilled water, the 5g Calcium Chloride Powder Anhydrous, 13gMgCl
26H
2O, 150g calcium bentonite and 9g anhydrous sodium carbonate) high temperature filtrate-loss control energy and the rheological property of the aging front and back of aging 16h evaluation property of drilling fluid to fluid loss agent rolls under 180 ℃ of high temperature.Experimental data is as shown in table 1:
Table 1 is through the dissimilar mud of polymer treatment
180 ℃ of heat are rolled the performance before and after the aging 16h
As shown in Table 1, fresh water base slurry under the room temperature, brine mud adds the be improved effect of apparent viscosity and plastic viscosity of drilling fluid of fluid loss agent in water base slurry of saturated salt and the compound brine mud, and increase rate is bigger in fresh water base slurry.Obviously reduce carrying out 16 hours 180 ℃ of aging back filter losses, compare with filter loss under the room temperature change little.As seen, the heat-resisting property of this fluid loss agent is fine.
2. inhibition evaluation
Well behaved additive for drilling fluid not only has the good filtration capacity that falls, and also should have to suppress ability preferably.For this reason, carried out shale rolling recovery test, five-membered copolymer fluid loss agent has been added in the clear water under 120 ℃, behind the rolling 16h, reclaimed, weighed after the oven dry with 40 mesh standard sieves.Experimental result is shown in Table 2:
Table 2 shale rolling recovery test result
Can find out from table 2, in the blank clear water of shale, five yuan of polymkeric substance heat of dosage 0.5%, dosage 1% primary recovery after rolling is respectively 14.2%, 51.0%, 73.4%.Then, the 40 order shale that reclaim oven dry are joined respectively in the clear water, roll 16h in 120 ℃ of following heat equally, reclaim with 40 mesh standard sieves, weigh after the oven dry, try to achieve the secondary recovery rate, five yuan of polymkeric substance of dosage 0.5%, dosage 1% are respectively 40.8%, 67.0%.The rate of recovery only 14.2% shows that shale is easy to aquation and disperses in clear water, and reaches 73.4% in five yuan of polymer recovery of dosage 1.0%, and its secondary recovery rate also reaches 67.0%, shows that this fluid loss agent has good inhibition effect.Show that institute's synthetic five-membered copolymer has the good adsorption ability on the shale surface, have good inhibition, can effectively control shale hydration and disperse, help protection hydrocarbon zone.
Claims (2)
1. five-membered copolymer fluid loss agent, it is characterized in that: the amount of substance for preparing raw materials used and each component of this fluid loss agent is such as down, wherein the unit of amount of substance is a mole, mass unit is gram, raw material A is an acrylamide, and raw material B is a propylene cyanogen, and raw material C is a vinylformic acid, raw material D is 2-acrylamide-2-methyl propane sulfonic acid, and raw material E is vinyl ammonium salt cationic monomer, is with methylacryoyloxyethyl trimethyl ammonium chloride code name DMC or dimethyl diallyl ammonium chloride code name DMDAAC; Wherein the mol ratio of A: B: C: D: E is 66: 3: 13: 10: 8 or 63: 4: 15: 10: 8; PH regulator agent mass percentage concentration is 20% NaOH solution, and the pH value transfers to 6～8; The initiator redox system is that ammonium persulphate and sodium bisulfite, mol ratio are 1: 1, and initiator amount is 0.7%～1.6% of a monomer total mass; Solvent is a water, and the quality of water is 7: 3 with the ratio of monomer total mass; The purification solvent is a dehydrated alcohol.
2. preparation method of fluid loss agent according to claim 1, it is characterized in that: earlier that vinylformic acid and 2-acrylamide-2-methyl propane sulfonic acid and vinyl ammonium salt cationic monomer is soluble in water, the mol ratio of its C: D: E is 13: 10: 8 or 15: 10: 8, and the quality of water is 7: 3 with the ratio of monomer total mass; Use pH to 6～8 of 20% NaOH solution regulation system then, mixing solutions G; Secondly in mixing solutions G, add acrylamide and propylene cyanogen, the mol ratio of its A: B is 66: 3 or 63: 4, gets mixing solutions H, and the mass percentage concentration of mixing solutions H is 30%; Again mixing solutions H is heated to 40～55 ℃, add initiator ammonium persulfate and sodium bisulfite successively, initiator amount is 0.7%～1.6% of a monomer total mass, constantly stirs reaction 10min down, observe viscosity, standing and reacting 3～5h in water bath with thermostatic control; At last top products therefrom is taken out, purify, obtain the oyster white colloidal solids,,, make product five-membered copolymer fluid loss agent of the present invention in 120 ℃ of oven dry, pulverizing again with solid product shearing, granulation with dehydrated alcohol.
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| CN102181009A (en) * | 2011-04-14 | 2011-09-14 | 孙安顺 | Method for preparing temperature-resistant and salt-resistant polymer for drilling fluid |
| CN102181010A (en) * | 2011-04-14 | 2011-09-14 | 孙安顺 | Preparation method of high-temperature-resistant high-salt polymer oil-replacement agent |
| CN102432751A (en) * | 2011-09-05 | 2012-05-02 | 中国石油大学(华东) | High-temperature colloid protecting anticaving fluid loss additive for drilling fluid and preparation method thereof |
| CN102643632A (en) * | 2012-04-06 | 2012-08-22 | 茂名市三元化工有限公司 | High-temperature salt-resistant fluid loss agent and production method thereof |
| CN103409118A (en) * | 2013-08-27 | 2013-11-27 | 赵贤正 | Synthetic method of water-base drilling fluid ultra-temperature stabilizing agent |
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| CN102181010A (en) * | 2011-04-14 | 2011-09-14 | 孙安顺 | Preparation method of high-temperature-resistant high-salt polymer oil-replacement agent |
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| CN102432751B (en) * | 2011-09-05 | 2013-11-27 | 中国石油大学(华东) | High-temperature colloid protecting anticaving fluid loss additive for drilling fluid and preparation method thereof |
| CN102432751A (en) * | 2011-09-05 | 2012-05-02 | 中国石油大学(华东) | High-temperature colloid protecting anticaving fluid loss additive for drilling fluid and preparation method thereof |
| CN102643632A (en) * | 2012-04-06 | 2012-08-22 | 茂名市三元化工有限公司 | High-temperature salt-resistant fluid loss agent and production method thereof |
| CN103509535A (en) * | 2012-06-29 | 2014-01-15 | 中国石油化工股份有限公司 | Filtrate loss reduction method for water-based drilling fluid, and preparation method for filtrate loss reducer |
| CN103509535B (en) * | 2012-06-29 | 2016-12-21 | 中国石油化工股份有限公司 | The filtrate reducing method of water-base drilling fluid and the preparation method of fluid loss additive |
| CN103409118A (en) * | 2013-08-27 | 2013-11-27 | 赵贤正 | Synthetic method of water-base drilling fluid ultra-temperature stabilizing agent |
| CN104151490A (en) * | 2014-06-10 | 2014-11-19 | 翟常忠 | High-temperature-resistant salt-resistant fluid loss additive for drilling fluids and preparation method thereof |
| CN104151490B (en) * | 2014-06-10 | 2016-04-27 | 翟常忠 | A kind of loss additive for drilling fluid loss agent and preparation method thereof |
| CN105646793B (en) * | 2014-12-02 | 2018-09-04 | 中国石油天然气集团公司 | A kind of oil gas well cementing operation low hydration heat high-early (strength) cement fluid loss agent and preparation method |
| CN105646793A (en) * | 2014-12-02 | 2016-06-08 | 中国石油天然气集团公司 | Low hydration heat early strength cement fluid loss reducer for oil-gas well cementing and preparation method |
| CN104531103B (en) * | 2015-01-19 | 2017-07-11 | 中国石油集团渤海钻探工程有限公司 | A kind of drilling fluid sealing agent and preparation method thereof |
| CN104531103A (en) * | 2015-01-19 | 2015-04-22 | 中国石油集团渤海钻探工程有限公司 | Blocking agent for drilling liquid and preparation method thereof |
| CN104962250A (en) * | 2015-06-17 | 2015-10-07 | 成都高普石油工程技术有限公司 | Treating agent used for high-performance copolymer drilling fluid |
| CN105566559A (en) * | 2015-12-29 | 2016-05-11 | 北京希涛技术开发有限公司 | Temperature-control sticky-becoming acid liquid thickening agent and synthetic method thereof |
| CN109652029A (en) * | 2018-12-07 | 2019-04-19 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | A kind of sea water base drilling fluid salt-resisting high-temperature-resisting fluid loss additive and preparation method thereof |
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| CN114989348B (en) * | 2022-07-21 | 2024-01-19 | 中国石油大学(华东) | High-temperature-resistant salt-resistant organosilicon fluid loss additive and preparation method and application thereof |
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Application publication date: 20101229 |