CN104531104A - High-temperature-resistant and salt-bearing filtrate loss reducer and preparation method thereof - Google Patents

High-temperature-resistant and salt-bearing filtrate loss reducer and preparation method thereof Download PDF

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CN104531104A
CN104531104A CN201510024749.4A CN201510024749A CN104531104A CN 104531104 A CN104531104 A CN 104531104A CN 201510024749 A CN201510024749 A CN 201510024749A CN 104531104 A CN104531104 A CN 104531104A
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salt
resisting
temperature
fluid loss
mass parts
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王磊磊
王伟忠
徐浩然
张坤
冯超
王强
李文娟
李广环
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CNPC Bohai Drilling Engineering Co Ltd
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CNPC Bohai Drilling Engineering Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52Amides or imides
    • C08F220/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52Amides or imides
    • C08F220/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/58Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/02Well-drilling compositions
    • C09K8/03Specific additives for general use in well-drilling compositions
    • C09K8/035Organic additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52Amides or imides
    • C08F220/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/58Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
    • C08F220/585Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Engineering & Computer Science (AREA)
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  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention discloses a novel high-temperature-resistant and salt-bearing filtrate loss reducer and a preparation method thereof. The structural formula of the high-temperature-resistant and salt-bearing filtrate loss reducer is as shown in a formula I; the preparation method comprises the following steps: dissolving N-isopropyl acrylamide and other water-soluble acrylamide monomers in de-ionized water, then adding an initiator, carrying out a reaction under nitrogen atmosphere, and drying a product so as to obtain the high-temperature-resistant and salt-bearing filtrate loss reducer. The method has the characteristics of being simple in process and easy to realize industrial production; and the prepared filtrate loss reducer is resistant to high temperature at 200 DEG C and is salt-bearing to be saturated.

Description

A kind of high-temperature resisting and salt-resisting fluid loss agent and preparation method thereof
Technical field
The present invention relates to a kind of fluid loss agent, relate to a kind of high-temperature resisting and salt-resisting fluid loss agent and preparation method thereof particularly.
Background technology
Along with the development of petroleum industry and the continuous growth of petroleum demand, oil-gas exploration and development is gradually to deep formation and marine development, and the difficulty of drilling engineering is increasing, proposes requirements at the higher level to drilling fluid and additive for drilling fluid.Fluid loss agent, as one of the important process agent of water-base drilling fluid, plays an important role to the safe, fast, efficient drilling well of guarantee.Its consumption is maximum, and of a great variety, is mainly natural materials or natural materials modified product and synthetic polymer class.Natural materials or natural materials modified product comprise humic acid, Mierocrystalline cellulose, xylogen, starch based and derivative thereof; Synthetic polymer is mainly based on various vinyl monomer multiple copolymers and sulfomethylated resol etc.Under certain condition, some mineral compound such as calcium carbonate superfine powder, silicon ash also can be used as fluid loss agent.In recent years, in order to meet the needs of complex stratum condition safety drilling, the research of high temperature resistance, salt resistant drilling fluid loss agent is progressively paid attention to.And polymer class fluid loss agent enriches due to monomer whose classification, adjustability is strong, has broad application prospects in high temperature resistance, anti-salt, just progressively becomes the focus of research both at home and abroad.
Since twentieth century six the seventies, external just to fluid loss agent, particularly high-temperature resisting and salt-resisting fluid loss agent has been cooked a large amount of experimental studies, and also achieves good real world applications effect at the scene.As early stage SSMA (Zelan 338), VSVA (vinyl sulfonate and ethernamine multipolymer), the rare amide copolymer of methyl-prop of Soviet Union's development, the Hostadrill (ethernamine vinyl sulfonic acid salt copolymer) of West Germany's development and Resinex (valchovite) etc. produced in USA; The Driscal series product having U.S. Xue Fulong-Karen Phillips company to produce be widely used in the recent period.
China's additive for drilling fluid obtains in the 1970s and 1980s in 20th century and develops rapidly, and it is acrylamide, the acrylic-multipolymer class treatment agent of representative that period defines with PAC-141, has walked abreast into corresponding polymer drilling fluid system.There is the both sexes complex ionic additive for drilling fluid and the drilling fluid system that take FA-367 as representative in the nineties, polymer drilling fluid Technology is had again new development, compared with anionoid polymerization, amphoteric ion type polymkeric substance flocculation and anti-collapse in make moderate progress, but the restriction of the polymerization activity due to cationic monomer used, the introduction volume of cationic monomer is limited, there is no rapid progress improving in the over-all properties of polymkeric substance.Studies in China work in the last few years mainly concentrates on the multi-component copolymer objects system based on acrylamide, temperature resistance and the anti-salt property of product is improved by introducing sulfonation group and rigid chain segment on molecular chain, but in actual use, these products are all difficult to the high temperature bearing more than 200 DEG C, high-density weighting material is caused to precipitate, saline-alkaline tolerance declines, and cannot meet the requirement of deep & ultra-deep well.
Summary of the invention
The object of this invention is to provide a kind of novel high-temperature resisting and salt-resisting fluid loss agent material and preparation method thereof, to solve the poor problem of existing water-base drilling fluid fluid loss agent heat and salinity tolerance ability.NIPA (NIPAM) has stronger stability to hydrolysis and heat and salinity tolerance performance, simultaneously owing to having hydrophilic amide group and hydrophobic sec.-propyl in molecule, its homopolymer is made to have temperature sensitivity, at Kraft point (LCST) (40-65 DEG C) below, the uniform solution of the water-soluble formation of its homopolymer, when temperature rises to more than Kraft point, solution is separated.Given this characteristic, this monomer is introduced acrylic amide water-soluble polymers main chain, the multipolymer of preparation has responsive to temperature type equally, when temperature is lower than LCST, the interaction of macromolecular chain polar groups and surrounding water molecules is better than the interaction between hydrophobic grouping, macromolecular chain is water-soluble, and soltion viscosity is lower, is easy to situ configuration glue; When temperature is higher than LCST, the polar group extent of hydration of macromolecular chain reduces, hydrophobic segment in NIPAM is separated out from solution, produce in molecule and Interpolymer Association, increase hydrodynamic volume and make drilling fluid have good shear force with suspension high-density weighting material, and in salt-water drilling fluid, because solution polarity increases, heat resistance and salt tolerance is strengthened, obvious anti-salt property can be shown.Therefore, the introducing of NIPAM, can improve the heat and salinity tolerance effect of acrylic amide fluid loss agent.
High-temperature resisting and salt-resisting heat resisting fluid loss reducing agent of the present invention is obtained by NIPA (NIPAM) and other water soluble acrylamido's class monomer copolymerizations.
The structural formula of described high-temperature resisting and salt-resisting fluid loss agent is as follows:
In above-mentioned formula I, R can be selected from following any one or a few:
M and n be greater than 1 integer.
High-temperature resisting and salt-resisting fluid loss agent shown in above-mentioned formula I is made up of the feed composition comprising following mass parts:
NIPA 1-40
Other water soluble acrylamido's class monomers 1-40
Wherein, other described water soluble acrylamido's class monomers comprise: acrylamide (AM), NVP (NVP), 2-acrylamide-2-methyl propane sulfonic (AMPS), N, N-DMAA (DMAM), or its mixture two or more arbitrarily.
The mass parts of described NIPA is 15-35 further; The mass parts of other described water soluble acrylamido's class monomers is 5-25 further.
Preparation method comprises the steps:
(1) described water soluble acrylamido's class monomer is dissolved in deionized water, after stirring and dissolving, adds appropriate NaOH, regulate pH value of water solution to 9-11;
(2) add NIPA to the described aqueous solution, after dissolving completely, under nitrogen protection, slowly add initiator, 60-80 DEG C of reacting by heating 4-6 hour, obtains glue solution of sticky shape;
(3) described glue solution of sticky shape is placed in baking oven heat drying, then pulverizes, sieve, obtain described high-temperature resisting and salt-resisting heat resisting fluid loss reducing agent.
In above-mentioned preparation process, the deionized water added, the mass parts of initiator are as follows:
Deionized water: 100
Initiator: 0.05-1
Described initiator comprises ammonium persulphate, Potassium Persulphate, benzoyl peroxide, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo diisobutyl amidine dihydrochloride, or its mixture two or more arbitrarily.
High-temperature resisting and salt-resisting fluid loss agent provided by the invention has the feature of heat and salinity tolerance, be different from classic water-soluble fluid loss agent, described fluid loss agent has temperature-sensing property, namely NIPAM segment is contained in molecular chain, when higher than Kraft point, hydrophobic segment in NIPAM is separated out from solution, the maintenance and good salt resistance of cutting is glued under can realizing high temperature by intermolecular hydrophobic association, overcome viscosity reduction under classic water-soluble fluid loss agent high temperature, cause the problems such as high-density weighting material sedimentation, in the middle of the water base drilling fluid system that can be used for deep & ultra-deep well, realize the exploratory development to deep bottom hydrocarbon resources.
The present invention has following advantage:
(1) the high-temperature resisting and salt-resisting fluid loss agent described in has certain Thermo-sensitive, water at normal temperature dissolubility is good, solution viscosity is lower, be easy to situ configuration glue, after entering well head, underground high temperature makes hydrophobic segment separate out from solution, produces in molecule and Interpolymer Association, can keep suspension and the saline-alkaline tolerance of drilling fluid;
(2) the high-temperature resisting and salt-resisting fluid loss agent temperature resistance 200 DEG C described in, anti-salt is to saturated;
(3) the high-temperature resisting and salt-resisting fluid loss agent preparation technology described in is simple, is easy to suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is ordinary method if no special instructions.In following each embodiment, described part is mass fraction.Described reactant all can obtain from open commercial sources if no special instructions.
Embodiment 1
1) in the four-hole bottle that mechanical stirrer is housed, add 5 parts of AM, 100 parts of deionized waters, stirring and dissolving, adds a small amount of NaOH, regulates pH to 11, obtains homogeneous phase aqueous solution;
2) add 35 parts of NIPAM to the described aqueous solution, and stirring and dissolving, then slowly add 0.05 part of ammonium persulphate under nitrogen protection, 60 ~ 80 DEG C of reacting by heating 4 hours, obtain glue solution of sticky shape;
3) described glue solution of sticky shape is placed in baking oven heat drying, then pulverizes, sieve, obtain described high-temperature resisting and salt-resisting heat resisting fluid loss reducing agent, specific performance is listed in table 1.
Embodiment 2
1) in the four-hole bottle that mechanical stirrer is housed, add 6 parts of AM, 6.9 parts of NVP, 100 parts of deionized waters, stirring and dissolving, adds NaOH, regulates pH to 11, obtains homogeneous phase aqueous solution;
2) add 30 parts of NIPAM to the described aqueous solution, and stirring and dissolving, then slowly add 0.05 part of Potassium Persulphate under nitrogen protection, 60 ~ 80 DEG C of reacting by heating 4 hours, obtain glue solution of sticky shape;
3) described glue solution of sticky shape is placed in baking oven heat drying, then pulverizes, sieve, obtain described high-temperature resisting and salt-resisting heat resisting fluid loss reducing agent, specific performance is listed in table 1.
Embodiment 3
1) in the four-hole bottle that mechanical stirrer is housed, add 13.3 parts of NVP, 100 parts of deionized waters, stirring and dissolving, adds a small amount of NaOH, regulates pH to 11, obtains homogeneous phase aqueous solution;
2) add 20 parts of NIPAM to the described aqueous solution, and stirring and dissolving, then slowly add 0.1 part of azo diisobutyl amidine dihydrochloride under nitrogen protection, 60 ~ 70 DEG C of reacting by heating 6 hours, obtain glue solution of sticky shape;
3) described glue solution of sticky shape is placed in baking oven heat drying, then pulverizes, sieve, obtain described high-temperature resisting and salt-resisting heat resisting fluid loss reducing agent, specific performance is listed in table 1.
Embodiment 4
1) in the four-hole bottle that mechanical stirrer is housed, add 15 parts of AMPS, 10 parts of DMAM, 100 parts of deionized waters, stirring and dissolving, adds NaOH, regulates pH to 11, obtains homogeneous phase aqueous solution;
2) add 15 parts of NIPAM to the described aqueous solution, and stirring and dissolving, then slowly add 0.1 part of Diisopropyl azodicarboxylate under nitrogen protection, 60 ~ 70 DEG C of reacting by heating 6 hours, obtain glue solution of sticky shape;
3) described glue solution of sticky shape is placed in baking oven heat drying, then pulverizes, sieve, obtain described high-temperature resisting and salt-resisting heat resisting fluid loss reducing agent, specific performance is listed in table 1.
Embodiment 5
1) in the four-hole bottle that mechanical stirrer is housed, add 6 parts of DMAM, 7.3 parts of NVP, 100 parts of deionized waters, stirring and dissolving, adds NaOH, regulates pH to 11, obtains homogeneous phase aqueous solution;
2) add 20 parts of NIPAM to the described aqueous solution, and stirring and dissolving, then slowly add 0.05 part of ammonium persulphate under nitrogen protection, 60 ~ 80 DEG C of reacting by heating 4 hours, obtain glue solution of sticky shape;
3) described glue solution of sticky shape is placed in baking oven heat drying, then pulverizes, sieve, obtain described high-temperature resisting and salt-resisting heat resisting fluid loss reducing agent, specific performance is listed in table 1.
In the water base slurry of saturated salt, performance evaluation is carried out to described high-temperature resisting and salt-resisting fluid loss agent, to investigate its temperature resistance and anti-salt property.
1) 350ml saturated brine is placed in height and stirs cup, add 1.00g NaHCO 3evaluate soil with 35.00g, stir 20min, centre at least stops to scrape wall twice.24 ± 3 DEG C of curing in airtight condition 24h, obtain the water base slurry of saturated salt; Stir 20min, measure its performance (see table 1).
2) to fill base slurry goblet in add 2% high-temperature resisting and salt-resisting fluid loss agent, high-speed stirring 20min, performance under mensuration room temperature, then pours 200 DEG C of aging 16h in digestion tank into by drilling fluid, high-speed stirring 5min after taking out, measures its performance (see table 1).
The performance evaluation of table 1. high-temperature resisting and salt-resisting fluid loss agent
Note: AV is apparent viscosity, and PV is plastic viscosity, and YP is yield value, FL aPIfor filter loss.
As can be seen from evaluation result, described high-temperature resisting and salt-resisting fluid loss agent, in saturated brine, still has good fluid loss agent performance after 200 DEG C of aging 16h, wherein optimum with embodiment 3 effect, the fluid loss agent heat and salinity tolerance excellent effect described in explanation.

Claims (7)

1. a high-temperature resisting and salt-resisting fluid loss agent, its structural formula is such as formula shown in I:
In formula I, R can be selected from any one or a few mixture following:
M and n be greater than 1 integer.
2. prepare a method for high-temperature resisting and salt-resisting fluid loss agent according to claim 1, it is characterized in that: described high-temperature resisting and salt-resisting fluid loss agent is made up of the raw material comprising following mass parts:
NIPA 1-40;
Other water soluble acrylamido's class monomers 1-40;
Wherein, other water soluble acrylamido's class monomers described comprise: acrylamide (AM), NVP (NVP), 2-acrylamide-2-methyl propane sulfonic (AMPS), N, N-DMAA (DMAM), or above-mentioned two or more arbitrarily.
3. method according to claim 2, the mass parts of described NIPA is 15-35; The mass parts of other water soluble acrylamido's class monomers described is 5-25.
4. method according to claim 2, comprises the steps:
(1) described water soluble acrylamido's class monomer is dissolved in deionized water, after stirring and dissolving, adds appropriate NaOH, regulate pH value of water solution to 9-11;
(2) add NIPA to the described aqueous solution, after dissolving completely, under nitrogen protection, slowly add initiator, 60 ~ 80 DEG C of reacting by heating 4-6 hour, obtain glue solution of sticky shape;
(3) described glue solution of sticky shape is placed in baking oven heat drying, then pulverizes, sieve, obtain described high-temperature resisting and salt-resisting heat resisting fluid loss reducing agent.
5. method according to claim 4, in described method, the deionized water added and the mass parts of initiator as follows, and identical in quality representated by every part of mass parts of described deionized water and initiator and every part of mass parts of described raw material:
Deionized water: 100
Initiator: 0.05-1.
6. method according to claim 5, described initiator is selected from following any one or two or more mixtures: ammonium persulphate, Potassium Persulphate, benzoyl peroxide, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo diisobutyl amidine dihydrochloride.
7. an application method for high-temperature resisting and salt-resisting fluid loss agent, adds the high-temperature resisting and salt-resisting fluid loss agent according to claim 1 of 1-5% in base slurry.
CN201510024749.4A 2015-01-19 2015-01-19 High-temperature-resistant and salt-bearing filtrate loss reducer and preparation method thereof Pending CN104531104A (en)

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CN105017475A (en) * 2015-06-29 2015-11-04 山东得顺源石油科技有限公司 Tackifying and filtrate reducing agent for low soil phase and high density drilling fluid, and preparation method thereof
CN108441178A (en) * 2018-05-14 2018-08-24 中国石油集团西部钻探工程有限公司 A kind of drilling fluid sealing agent NVP-DMAM copolymers and preparation method thereof
CN109054782A (en) * 2018-08-03 2018-12-21 长江大学 Temperature sensitive polymer rheology control agent and constant current are denaturalized water-base drilling fluid
CN109748990A (en) * 2017-11-03 2019-05-14 中国石油化工股份有限公司 Polymer and its preparation method and application with selective water plugging function
CN112194755A (en) * 2020-10-09 2021-01-08 中国石油大学(华东) Preparation method of temperature-sensitive flow type regulator for deepwater water-based drilling fluid
CN112979883A (en) * 2021-03-17 2021-06-18 江苏富淼科技股份有限公司 High-temperature-resistant salt-resistant polymer, and preparation method and application thereof
CN113583182A (en) * 2021-07-27 2021-11-02 中国石油大学(华东) Filtrate reducer with core-shell structure, preparation method and application thereof, and water-based drilling fluid
CN114891489A (en) * 2022-03-24 2022-08-12 长江大学 Non-sulfonated high-temperature-resistant water-based drilling fluid
CN115417950A (en) * 2022-11-04 2022-12-02 中石化西南石油工程有限公司 Temperature-sensitive fluid loss agent for well cementation cement slurry and preparation method thereof

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CN105017475A (en) * 2015-06-29 2015-11-04 山东得顺源石油科技有限公司 Tackifying and filtrate reducing agent for low soil phase and high density drilling fluid, and preparation method thereof
CN109748990A (en) * 2017-11-03 2019-05-14 中国石油化工股份有限公司 Polymer and its preparation method and application with selective water plugging function
CN108441178A (en) * 2018-05-14 2018-08-24 中国石油集团西部钻探工程有限公司 A kind of drilling fluid sealing agent NVP-DMAM copolymers and preparation method thereof
CN109054782A (en) * 2018-08-03 2018-12-21 长江大学 Temperature sensitive polymer rheology control agent and constant current are denaturalized water-base drilling fluid
CN112194755A (en) * 2020-10-09 2021-01-08 中国石油大学(华东) Preparation method of temperature-sensitive flow type regulator for deepwater water-based drilling fluid
CN112979883A (en) * 2021-03-17 2021-06-18 江苏富淼科技股份有限公司 High-temperature-resistant salt-resistant polymer, and preparation method and application thereof
CN112979883B (en) * 2021-03-17 2022-03-25 江苏富淼科技股份有限公司 High-temperature-resistant salt-resistant polymer, and preparation method and application thereof
CN113583182A (en) * 2021-07-27 2021-11-02 中国石油大学(华东) Filtrate reducer with core-shell structure, preparation method and application thereof, and water-based drilling fluid
CN114891489A (en) * 2022-03-24 2022-08-12 长江大学 Non-sulfonated high-temperature-resistant water-based drilling fluid
CN114891489B (en) * 2022-03-24 2023-10-10 长江大学 Non-sulfonated high-temperature-resistant water-based drilling fluid
CN115417950A (en) * 2022-11-04 2022-12-02 中石化西南石油工程有限公司 Temperature-sensitive fluid loss agent for well cementation cement slurry and preparation method thereof

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Application publication date: 20150422