CN101397491B - Multi-element co-polymerization oil well cement fluid loss additive and preparation method thereof - Google Patents
Multi-element co-polymerization oil well cement fluid loss additive and preparation method thereof Download PDFInfo
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- CN101397491B CN101397491B CN2008100513384A CN200810051338A CN101397491B CN 101397491 B CN101397491 B CN 101397491B CN 2008100513384 A CN2008100513384 A CN 2008100513384A CN 200810051338 A CN200810051338 A CN 200810051338A CN 101397491 B CN101397491 B CN 101397491B
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Abstract
The invention relates to a multicomponent copolymerization oil well cement fluid loss additive and a preparation method thereof. The method comprises: 10-120 portions of 2-acrylamide-2-methyl-1-AMPSA, 1-5 portions of acrylic acid and 15-50 portions of deionized water are added, stirred and then added with sodium hydroxide aqueous solution with the mass fraction of 5-10 percent for neutralizing topH equal to 3-11; then 10 portions of acrylamide, 0.1-1 portion of complexing agent EDTA and 0.01-1 portion of chain transfer agent are added, the chain transfer agent is isopropyl alcohol or sodium benzoate, the temperature is controlled between 30 DEG C and 60 DEG C and N2 is introduced for 30 minutes; 2-10 portions of N-vinyl pyrrolidone and 0.01-0.5 portion of initiator are added, the initiator is potassium persulfate or ammonium persulfate, and the reaction is carried out for 4-12 hours. The solution keeps still for 5 hours at the temperature of 180 DEG C, and is cooled through flowing water after being taken out, without sedimentation or water separating; and the water loss is zero at the temperature of 180 DEG C according to the standards of drilling fluid, and the water loss is 48ml according to the standards of cement.
Description
Technical field
The present invention relates to multi-element co-polymerization oil well cement fluid loss additive and preparation method thereof, belong to the preparing technical field of macromolecular material.
Background technology
During cementing operation, diafiltration will take place when flowing through permeable strata under pressure in grout, cause the grout liquid phase stratum of bleeding, and this process is commonly referred to as " dehydration ".If do not control dehydration, the minimizing of liquid phase volume will make cement slurry density increase, and thickening time, rheological depart from original design requirement, and the cement slurry water loss amount is excessive, easily forms bridge blinding, cause being difficult to realize the grout turbulence replacement and might causing the resident fluid channelling; But a large amount of liquid flow into the stratum and grout are become be difficult to not even pumping of pumping, and in various degree injury is caused on the stratum, can make the well cementing operation failure when serious.Therefore, usually in grout, add water retaining, this is that a kind of liquid phase of controlling in the grout is to the permeable strata leak-off, thereby keep grout that suitable water cement ratio is arranged, can improve the rheological of grout and the dehydration of reduction grout after the adding, in the hope of safety, efficient well cementation, guarantee cementing quality.
Along with the development of petroleum exploration and development cause, the progress of drilling technique proposes higher requirement for well cementation.Can adopt, easily adopt at oil under the continuous situation about reducing of reserves, the oil field prospecting exploitation is to ocean, bad ground, deep-well, middle-deep well and the development of ultra deep well aspect.Along with the intensification of the oil gas well drilling degree of depth, formation temperature also constantly raises.High temperature not only can make the bad stability of drilling fluid, and drilling fluid is difficult in maintenance; And when well cementation, cement slurry thickening time is shortened, and fluid loss increases, and the cement strength decline causes conventional cement additive to lose efficacy, and is difficult to satisfy construction requirement.For satisfying High Temperature High Pressure well cementation requirement, the functional and stable heatproof water retaining that needs constantly research to make new advances.
High temperature resistant water retaining is different from general water retaining, except good falling the dehydration effect will be arranged, also requires water retaining that certain heat-resisting ability is arranged.At present, most of fluid loss agent product is water-soluble polymer and organic materials.Water-soluble polymer is based on polyacrylamide and multipolymer thereof.Yet polyacrylamide temperature resistant antisalt poor-performing not only is not suitable for high-temperature oil reservoir, is exactly under the low-temperature reservoir condition, because of its thickening capabilities descends, and can't normally use yet.Thereby the development of temperature resistance polymkeric substance becomes the heat subject of domestic and international water-soluble polymers development.
Chinese patent 200710062680.X discloses and has been entitled as " nanometer composite heat resisting fluid loss reducing agent and preparation method thereof ".This method is in the presence of organo montmorillonite, adopts reversible-fracture chain transfer (RAFT) method to synthesize a kind of montmorillonite layer and is dispersed in the compound water retaining of Nano type in the Amphipathilic block polymer matrix with nano level.Though this method comparison novelty, preparation method's more complicated, the cost height is not suitable for large-scale practical application.Chinese patent 91103278.9 discloses and has been entitled as " a kind of preparation method of cement filter loss-reducing agent for oil well ".This method is that the certain proportion acrylamide is mixed mutually with acrylate solution, under certain temperature and nitrogen protection, adds initiator and has synthesized a kind of liquid product.This product has the ability of controlling leak-off preferably, good flowing properties, no thickening phenomenon.Since in the product acrylamide temperature during greater than 70 ℃ amide group hydrolysis easily takes place, carboxyl is very responsive to salt, therefore this product is unsuitable for high-temperature stratum.
Summary of the invention
The object of the invention provides multi-element co-polymerization oil well cement fluid loss additive and preparation method thereof.This method adopts industrial raw material acrylamide, 2-acrylamido-2-methyl-1-propanesulfonic acid, vinylformic acid and the copolymerization of N-vinyl pyrrolidone, obtains a kind of cement filter loss-reducing agent for oil well.
Because raw material that the present invention adopts is technical grade acrylamide, 2-acrylamido-2-methyl-1-propanesulfonic acid, vinylformic acid, N-vinyl pyrrolidone, before adding initiator, complexing agent EDTA (disodium ethylene diamine tetraacetate) must be added in advance, with purification reaction solution in solution system.Adding chain-transfer agent in solution is to prevent crosslinked generation.
The prescription of the composition weight part of multi-element co-polymerization oil well cement fluid loss additive provided by the invention is:
10 parts of acrylamides (AM)
10-120 parts of 2-acrylamidos-2-methyl-1-propanesulfonic acid (AMPS)
1-5 parts in vinylformic acid (AA)
2-10 parts of N-vinyl pyrrolidones (NVP)
0.1-1 part of complexing agent
0.01-1 part of chain-transfer agent
0.01-0.5 part of initiator
20-50 parts of aqueous sodium hydroxide solutions
15-50 parts of deionized waters
Described chain-transfer agent is Virahol or Sodium Benzoate; Complexing agent disodium ethylene diamine tetraacetate (EDTA)
Initiator is Potassium Persulphate or Ammonium Persulfate 98.5.
Preparation method's step and the condition that the invention provides multi-element co-polymerization oil well cement fluid loss additive is as follows:
In the reactor that has agitator and thermometer, by proportioning, earlier 2-acrylamido-2-methyl-1-propanesulfonic acid, vinylformic acid and deionized water are added and stir, add massfraction then and be 5%-10% aqueous sodium hydroxide solution and be neutralized to pH=3-11, add acrylamide, complexing agent disodium ethylene diamine tetraacetate and chain-transfer agent again, temperature is controlled at 30-60 ℃, logical N
230 minutes, add the N-vinyl pyrrolidone, add initiator, reacted 4-12 hours, obtain multi-element co-polymerization oil well cement fluid loss additive.
The present invention has following advantage: raw material of the present invention is industrial raw material all, need not carry out purification processes before the reaction.Preparation technology is simple.By the co-polypropylene acid mono, because the carboxylate radical (COO in the vinylformic acid
-) adsorptive power is very strong, can be adsorbed on the cement particle surface of positively charged, has hydration simultaneously concurrently, it mainly plays adsorption in water retaining.If but its ratio is too high, adsorptivity is strong excessively, will cause super delayed coagulation.The prepared multi-element co-polymerization oil well cement fluid loss additive of the present invention, be made into the high temperature resistance spacer pad 180 ℃ static 5 hours, take out back flowing water cooling, not deposition, no bleed, 180 ℃ is zero according to drilling fluid standard fluid loss, and 180 ℃ is 48ml according to the cement standard fluid loss.
Embodiment
Embodiment 1: get the 2-acrylamido-2-methyl-1-propanesulfonic acid of 10 weight parts, the deionized water that 1 parts by weight of acrylic adds 15 weight parts, add weight fraction then and be 5% aqueous sodium hydroxide solution and be neutralized to PH=3, the acrylamide that adds 10 weight parts again, 0.1 the complexing agent EDTA of weight part, the chain-transfer agent Virahol of 0.01 weight part stir, lead to N down 30 ℃ of temperature
2Add the N-vinyl pyrrolidone of 2 weight parts after 30 minutes, the Potassium Persulphate of 0.01 weight part reacted 12 hours.
Embodiment 2: get the 2-acrylamido-2-methyl-1-propanesulfonic acid of 50 weight parts, the deionized water that 3 parts by weight of acrylic add 30 weight parts, add weight fraction then and be 8% aqueous sodium hydroxide solution and be neutralized to PH=7, the acrylamide that adds 10 weight parts again, 0.5 the complexing agent EDTA of weight part, the chain-transfer agent Virahol of 0.1 weight part stir, lead to N down 45 ℃ of temperature
2Add the N-vinyl pyrrolidone of 5 weight parts after 30 minutes, the Ammonium Persulfate 98.5 of 0.1 weight part reacted 8 hours.
Embodiment 3: get the 2-acrylamido-2-methyl-1-propanesulfonic acid of 120 weight parts, the deionized water that 5 parts by weight of acrylic add 50 weight parts, add weight fraction then and be 10% aqueous sodium hydroxide solution and be neutralized to PH=11, the acrylamide that adds 10 weight parts again, the complexing agent EDTA of 1 weight part, the chain-transfer agent Sodium Benzoate of 1 weight part stir, lead to N down 60 ℃ of temperature
2Add the N-vinyl pyrrolidone of 10 weight parts after 30 minutes, the Ammonium Persulfate 98.5 of 1 weight part reacted 4 hours.
Embodiment 4: get the 2-acrylamido-2-methyl-1-propanesulfonic acid of 80 weight parts, the deionized water that 3 parts by weight of acrylic add 45 weight parts, add weight fraction then and be 9% aqueous sodium hydroxide solution and be neutralized to PH=9, the acrylamide that adds 10 weight parts again, 0.8 the complexing agent EDTA of weight part, the chain-transfer agent Virahol of 0.5 weight part stir, lead to N down 50 ℃ of temperature
2Add the N-vinyl pyrrolidone of 8 weight parts after 30 minutes, the Potassium Persulphate of 0.5 weight part reacted 5 hours.
Claims (1)
1. multi-element co-polymerization oil well cement fluid loss additive is characterized in that, the composition of this fluid loss agents and the prescription of weight part are:
10 parts of acrylamides
2-acrylamido-2-methyl isophthalic acid-propanesulfonic acid 10-120 part
Vinylformic acid 1-5 part
N-vinyl pyrrolidone 2-10 part
Complexing agent 0.1-1 part
Chain-transfer agent 0.01-1 part
Initiator 0.01-0.5 part
Aqueous sodium hydroxide solution 20-50 part
Deionized water 15-50 part;
Described chain-transfer agent is Virahol or Sodium Benzoate; Complexing agent is a disodium ethylene diamine tetraacetate, and initiator is Potassium Persulphate or Ammonium Persulfate 98.5;
Described multi-element co-polymerization oil well cement fluid loss additive is prepared by following method: in the reactor that has agitator and thermometer, by proportioning, earlier 2-acrylamido-2-methyl isophthalic acid-propanesulfonic acid, vinylformic acid and deionized water are added and stir, the aqueous sodium hydroxide solution that adds massfraction then and be 5%-10% is neutralized to pH=3-11, add acrylamide, complexing agent disodium ethylene diamine tetraacetate and chain-transfer agent again, temperature is controlled at 30-60 ℃, logical N
230 minutes, add the N-vinyl pyrrolidone, add initiator, reacted 4-12 hour, obtain multi-element co-polymerization oil well cement fluid loss additive.
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| CN102212351A (en) * | 2010-04-02 | 2011-10-12 | 卫辉市化工有限公司 | Water retaining agent for liquid well cementing cement |
| CN102372819B (en) * | 2010-08-26 | 2014-02-05 | 中国石油化工股份有限公司 | Long branched chain polymer used for oil displacement and synthesis method thereof |
| CN102372820B (en) * | 2010-08-26 | 2013-07-03 | 中国石油化工股份有限公司 | Long branched chain polymer used for tertiary oil recovery and synthesis method thereof |
| CN102464975B (en) * | 2010-11-17 | 2013-08-21 | 中国石油化工股份有限公司 | Composition for increasing recovery ratio of high-temperature and high-salt oil reservoir and preparation method thereof |
| 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 |
| 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 |
| CN103788292B (en) * | 2012-10-29 | 2016-06-29 | 中国石油化工股份有限公司 | A kind of acrylamide based copolymer and its preparation method and application |
| CN103113875B (en) * | 2013-02-28 | 2015-05-20 | 中国科学院长春应用化学研究所 | Water-based fracturing fluid thickener and method for preparing same |
| CN104179466B (en) * | 2013-05-21 | 2016-08-24 | 金川集团股份有限公司 | The method reducing fluid loss in probing |
| CN103382237A (en) * | 2013-08-09 | 2013-11-06 | 卫辉市化工有限公司 | Preparation method for dispersed oil well cement fluid loss additives |
| CN103555296B (en) * | 2013-11-05 | 2016-03-16 | 库尔勒同益工贸有限责任公司 | Water retaining of the anti-composite salt polymkeric substance of drilling fluid high temperature resistance and preparation method thereof |
| CN103710008B (en) * | 2013-12-29 | 2016-09-07 | 哈尔滨工业大学 | A kind of high temperature resistant drilling fluids fluid loss additive and preparation method thereof |
| CN105017478B (en) * | 2015-08-19 | 2017-07-28 | 中国海洋石油总公司 | A kind of high temperature resistance, anti-high salt concentration flow pattern regulator and preparation method thereof |
| CN105349127B (en) * | 2015-12-16 | 2018-07-31 | 中国石油大学(华东) | A kind of pre- chelating aluminate-base cement water reducer and preparation method and the cement mortar comprising it |
| CN105778921A (en) * | 2016-04-08 | 2016-07-20 | 北京市首发天人生态景观有限公司 | Soil ball fixing agent and preparation method and use method thereof |
| CN106632917B (en) * | 2016-12-23 | 2019-12-06 | 卫辉市化工有限公司 | Preparation method of polymer fluid loss agent for sulphoaluminate cement |
| CN107365403A (en) * | 2017-08-19 | 2017-11-21 | 新沂市中诺新材料科技有限公司 | A kind of preparation method of drilling fluid heat resisting fluid loss reducing agent |
| CN108033533A (en) * | 2017-12-27 | 2018-05-15 | 山东诺尔生物科技有限公司 | A kind of thin tailing flucculation process of oil-sand |
| CN115404061A (en) * | 2021-12-31 | 2022-11-29 | 南京绿界新材料研究院有限公司 | Preparation method of high-temperature-resistant salt-tolerant fluid loss additive composition |
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Owner name: CHANGZHOU INSTITUTE OF ENERGY STORAGE MATERIALS + Free format text: FORMER OWNER: CHANGCHUN INST. OF APPLIED CHEMISTRY, CHINESE ACADEMY OF SCIENCES Effective date: 20130916 |
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Effective date of registration: 20130916 Address after: Changzhou City, Jiangsu province Hehai road 213000 No. 9 Patentee after: Changzhou Institute of Energy Storage Materials & Devices Address before: 130022 Changchun people's street, Jilin, No. 5625 Patentee before: Changchun Institue of Applied Chemistry, Chinese Academy of Sciences |