CN105367710A - Preparation method for modified polyacrylamide filtrate reducer for drilling fluid - Google Patents

Preparation method for modified polyacrylamide filtrate reducer for drilling fluid Download PDF

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CN105367710A
CN105367710A CN201510988818.3A CN201510988818A CN105367710A CN 105367710 A CN105367710 A CN 105367710A CN 201510988818 A CN201510988818 A CN 201510988818A CN 105367710 A CN105367710 A CN 105367710A
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modified polyacrylamide
preparation
drilling fluid
fluid loss
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宋介珍
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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
    • C08F220/56Acrylamide; Methacrylamide
    • 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

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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)
  • Materials Engineering (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention relates to a preparation method for a modified polyacrylamide filtrate reducer for drilling fluid, and belongs to the technical field of petroleum drilling oilfield chemistry high-molecular polymers. The preparation method comprises the following steps: adding acrylamide monomer, 1,3-butylene glycol diacrylate, ethylene thiourea, hydroxy-propyl acrylate, cardanol, trimethylol propyl triacrylate, maleic anhydride, polyvinyl butyral, a chain extender, water, a crosslinking agent, a surfactant and a catalyst into a reactor, uniformly mixing, adding the mixture into a phosphoric acid adjusting system to adjust the pH value to 4-6, feeding inert gas to remove dissolved oxygen in the reaction system; cooling the reaction system, adding an initiating agent, and warming up for polymerization reaction; taking out the obtained jelly reactant, and conducting granulation, stoving and smashing so as to obtain the modified polyacrylamide filtrate reducer. The provided modified polyacrylamide filtrate reducer has the advantages of being good in high-temperature resistance and small in filtrate reduction loss.

Description

A kind of preparation method of the modified polyacrylamide fluid loss agent for drilling fluid
Technical field
The present invention relates to a kind of preparation method of the modified polyacrylamide fluid loss agent for drilling fluid, belong to petroleum drilling oilfield chemistry technical field of high-molecular polymer.
Background technology
In oil and gas well drilling construction process, for reaching the object of wellbore stability and reservoir protec-tion, adding fluid loss agent and reduce drilling fluid filtration, is the measure that must take.Fluid loss agent mostly is water-soluble high-molecular compound, and conventional fluid loss agent has carboxymethyl cellulose, resene, acrylic amide and treated starch etc.But these fluid loss agents often cause drilling fluid viscosity significantly to increase, make drilling fluid mobility be deteriorated, this increased frequency that will punching made to put drilling fluid, cause the waste of drilling fluid while reducing filter loss.
The action principle of fluid loss agent has: the first, protective colloid effect.In order to form the low mud cake of rate of permeation, require that in drilling fluid, clay particle particle diameter has suitable size distribution, requires more fine particle simultaneously.The protective colloid effect of fluid loss agent is that (1) is adsorbed on surface of clay and forms adsorption layer, and flocculating to stop clay particle becomes large; (2) fine particle of breaking under circulation of drilling fluid stirring can be settled out by absorption, be no longer bonded to macrobead.Which increase fine grain ratio, be conducive to forming fine and close mud cake.The second, improve filtrate viscosity and can reduce filter loss.0.5 power of filter loss and drilling fluid filtrate viscosity is inversely proportional to.Organic fluid loss agent improves filtrate viscosity after adding drilling fluid, and filter loss is reduced.In 3rd increase drilling fluid, the extent of hydration of clay particle, can reduce filter loss.Fluid loss agent is adsorbed on the clay particle in drilling fluid, and the hydration shell making its extent of hydration increase particle thickens, and the filter cake of formation is under high pressure yielding, the permeability reduction of filter cake.Four, the plug-hole effect of fluid loss agent molecule itself.The molecular dimension of organic polymer fluid loss agent is within the scope of colloidal solid, and after adding these outer reason agent, they are in the gap of long-chain wedging filter cake of molecule on the one hand, long chain molecule is curled into spherical on the other hand, blocking filter cake microporosity, makes filter cake thin and fine and close, thus reduces filter loss.
CN104531101A discloses a kind of fluid loss additive for boring fluid and preparation method thereof and application, wherein said preparation method comprises the steps: white dextrin, yellow starch gum, caustic soda, 95% ethanol, water and the epoxy chloropropane weight ratio according to 30 ~ 50:30 ~ 50:7 ~ 15:10 ~ 20:5 ~ 10:9 ~ 18 to react 2.5 ~ 3 hours at 70 ~ 90 DEG C, after cooling, discharging, dry, pulverize, obtain product fluid loss additive for boring fluid.CN102746834A discloses a kind of polymer filtrate reducer and preparation method thereof, specifically acid monomer is first neutralized with sodium hydroxide, then non-ionic monomer acrylamide is added, N-caprolactam, control the pH value of polymerization system 6.0 ~ 11.0, using oxidation-reduction trigger system as initiator, under molecular weight regulator exists, carry out aqueous solution polymerization form, the starting temperature of reaction is 10 ~ 80 DEG C, polyreaction completed within 5 ~ 60 minutes, the porous elastomers obtained is easy to dry, pulverizing obtains ultrahigh-temperature polymer filtrate reducer, its 1% aqueous solution apparent viscosity is at 8 ~ 15mPa.s.But above-mentioned fluid loss agent also exist high temperature resistant property not high, the large problem of filter loss is fallen when reality uses.
Summary of the invention
The object of the invention is: provide a kind of and have the modified polyacrylamide fluid loss agent that high temperature resistant property is good, fall the little advantage of filter loss, technical scheme is:
For a preparation method for the modified polyacrylamide fluid loss agent of drilling fluid, comprise the steps:
1st step, by weight, add acrylamide monomer 50 ~ 60 parts in the reactor, 1, 3-butylene glycol diacrylate 5 ~ 10 parts, ethylene thiourea 3 ~ 7 parts, Propylene glycol monoacrylate 3 ~ 6 parts, cardanol 4 ~ 7 parts, Viscoat 295 5 ~ 8 parts, MALEIC ANHYDRIDE 3 ~ 4 parts, polyvinyl butyral acetal 2 ~ 8 parts, chainextender 5 ~ 10 parts, 400 ~ 700 parts, water, linking agent 2 ~ 8 parts, 5 ~ 8 parts, tensio-active agent, catalyzer 5 ~ 8 parts, mix, add phosphoric acid regulation system pH value to 4 ~ 6, pass into rare gas element to remove the dissolved oxygen in reaction system,
2nd step, the reaction system of the 1st step gained is cooled to 5 ~ 15 DEG C, then add initiator 5 ~ 8 parts, heat up and carry out polyreaction;
3rd step, the jelly obtained by the reactant that the 2nd step obtains take out, and after granulation, oven dry, pulverizing, obtain modified polyacrylamide fluid loss agent.
In the 1st described step, tensio-active agent refers to sorbitan ester class tensio-active agent.
In the 1st described step, chainextender is the mixture of one or more in l, 4-butyleneglycol, neopentyl glycol, ethylene glycol, glycol ether, glycerine, MALEIC ANHYDRIDE, TriMethylolPropane(TMP), quadrol, diethylenetriamine, triethylene tetramine or dimethylol propionic acid.
In the 1st described step, described linking agent is one or more in vinylbenzene, methacrylic acid, methyl methacrylate, vinylformic acid, Phthalic acid, diallyl ester, Ethylene glycol dimethacrylate, vinyl cyanide.
In the 1st described step, rare gas element is selected from hydrogen, helium or nitrogen.
In the 1st described step, catalyzer is Hypophosporous Acid, 50 or dibutyl tin laurate.
Described sorbitan ester class tensio-active agent is selected from span 40 or dehydrated sorbitol mono-fatty acid ester.
In the 2nd described step, initiator is selected from azo-bis-isobutyrate hydrochloride, 2,2-azos (2-amidine propane) hydrochloride or 2,2-azo [2-(2-tetrahydroglyoxaline-2-base) propane] dihydrochloride.
In the 2nd described step, the temperature of polyreaction is 50 ~ 60 DEG C.
Beneficial effect
Modified polyacrylamide fluid loss agent provided by the invention have high temperature resistant property good, the little advantage of filter loss is fallen.
Embodiment
Embodiment 1
1st step, add acrylamide monomer 50g, 1 in the reactor, 3-butylene glycol diacrylate 5g, ethylene thiourea 3g, Propylene glycol monoacrylate 3g, cardanol 4g, Viscoat 295 5g, MALEIC ANHYDRIDE 3g, polyvinyl butyral acetal 2g, chainextender l, 4-butyleneglycol 5g, water 400g, linking agent vinyl cyanide 2g, span 40 5g, catalyst dibutyltin dilaurylate 5g, mix, add phosphoric acid regulation system pH value to 4 ~ 6, pass into helium to remove the dissolved oxygen in reaction system;
2nd step, the reaction system of the 1st step gained is cooled to 5 DEG C, then add initiator azo-bis-isobutyrate hydrochloride 5g, heat up 50 DEG C and carry out polyreaction;
3rd step, the jelly obtained by the reactant that the 2nd step obtains take out, and after granulation, oven dry, pulverizing, obtain modified polyacrylamide fluid loss agent.
Embodiment 2
1st step, add acrylamide monomer 60g, 1 in the reactor, 3-butylene glycol diacrylate 10g, ethylene thiourea 7g, Propylene glycol monoacrylate 6g, cardanol 7g, Viscoat 295 8g, MALEIC ANHYDRIDE 4g, polyvinyl butyral acetal 8g, chainextender l, 4-butyleneglycol 10g, water 700g, linking agent vinyl cyanide 8g, span 40 8g, catalyst dibutyltin dilaurylate 8g, mix, add phosphoric acid regulation system pH value to 4 ~ 6, pass into helium to remove the dissolved oxygen in reaction system;
2nd step, the reaction system of the 1st step gained is cooled to 15 DEG C, then add initiator azo-bis-isobutyrate hydrochloride 8g, heat up 60 DEG C and carry out polyreaction;
3rd step, the jelly obtained by the reactant that the 2nd step obtains take out, and after granulation, oven dry, pulverizing, obtain modified polyacrylamide fluid loss agent.
Embodiment 3
1st step, add acrylamide monomer 55g, 1 in the reactor, 3-butylene glycol diacrylate 7g, ethylene thiourea 5g, Propylene glycol monoacrylate 5g, cardanol 5g, Viscoat 295 6g, MALEIC ANHYDRIDE 3g, polyvinyl butyral acetal 5g, chainextender l, 4-butyleneglycol 7g, water 600g, linking agent vinyl cyanide 5g, span 40 6g, catalyst dibutyltin dilaurylate 6g, mix, add phosphoric acid regulation system pH value to 4 ~ 6, pass into helium to remove the dissolved oxygen in reaction system;
2nd step, the reaction system of the 1st step gained is cooled to 8 DEG C, then add initiator azo-bis-isobutyrate hydrochloride 6g, heat up 55 DEG C and carry out polyreaction;
3rd step, the jelly obtained by the reactant that the 2nd step obtains take out, and after granulation, oven dry, pulverizing, obtain modified polyacrylamide fluid loss agent.
Reference examples 1
Be with the difference of embodiment 3: in the 1st step, do not add monomer cardanol.
1st step, add acrylamide monomer 55g, 1 in the reactor, 3-butylene glycol diacrylate 7g, ethylene thiourea 5g, Propylene glycol monoacrylate 5g, Viscoat 295 6g, MALEIC ANHYDRIDE 3g, polyvinyl butyral acetal 5g, chainextender l, 4-butyleneglycol 7g, water 600g, linking agent vinyl cyanide 5g, span 40 6g, catalyst dibutyltin dilaurylate 6g, mix, add phosphoric acid regulation system pH value to 4 ~ 6, pass into helium to remove the dissolved oxygen in reaction system;
2nd step, the reaction system of the 1st step gained is cooled to 8 DEG C, then add initiator azo-bis-isobutyrate hydrochloride 6g, heat up 55 DEG C and carry out polyreaction;
3rd step, the jelly obtained by the reactant that the 2nd step obtains take out, and after granulation, oven dry, pulverizing, obtain modified polyacrylamide fluid loss agent.
Reference examples 2
Be with the difference of embodiment 3: in the 1st step, do not add monomer MALEIC ANHYDRIDE.
1st step, add acrylamide monomer 55g, 1 in the reactor, 3-butylene glycol diacrylate 7g, ethylene thiourea 5g, Propylene glycol monoacrylate 5g, cardanol 5g, Viscoat 295 6g, polyvinyl butyral acetal 5g, chainextender l, 4-butyleneglycol 7g, water 600g, linking agent vinyl cyanide 5g, span 40 6g, catalyst dibutyltin dilaurylate 6g, mix, add phosphoric acid regulation system pH value to 4 ~ 6, pass into helium to remove the dissolved oxygen in reaction system;
2nd step, the reaction system of the 1st step gained is cooled to 8 DEG C, then add initiator azo-bis-isobutyrate hydrochloride 6g, heat up 55 DEG C and carry out polyreaction;
3rd step, the jelly obtained by the reactant that the 2nd step obtains take out, and after granulation, oven dry, pulverizing, obtain modified polyacrylamide fluid loss agent.
Reference examples 3
Be with the difference of embodiment 3: in the 1st step, do not add monomer Viscoat 295.
1st step, add acrylamide monomer 55g, 1 in the reactor, 3-butylene glycol diacrylate 7g, ethylene thiourea 5g, Propylene glycol monoacrylate 5g, cardanol 5g, MALEIC ANHYDRIDE 3g, polyvinyl butyral acetal 5g, chainextender l, 4-butyleneglycol 7g, water 600g, linking agent vinyl cyanide 5g, span 40 6g, catalyst dibutyltin dilaurylate 6g, mix, add phosphoric acid regulation system pH value to 4 ~ 6, pass into helium to remove the dissolved oxygen in reaction system;
2nd step, the reaction system of the 1st step gained is cooled to 8 DEG C, then add initiator azo-bis-isobutyrate hydrochloride 6g, heat up 55 DEG C and carry out polyreaction;
3rd step, the jelly obtained by the reactant that the 2nd step obtains take out, and after granulation, oven dry, pulverizing, obtain modified polyacrylamide fluid loss agent.
To temperature resistance and the filtrate reducing effect assessment of product of the present invention, result is as follows:
Performance evaluation in fresh water-based slurry
4% fresh water-based slurry configuration: add 400mL water in high-speed stirring cup, add 0.48g sodium carbonate, 16g test sodium bentonite under stirring, height stirs 20min, and 24h is placed in sealing.
Experiment slurry preparation: the fluid loss agent prepared in embodiment and reference examples is joined in 4% fresh water-based slurry, preparation concentration is the experiment slurry of 0.01g/mL, cooling after aging 16h of rolling at 270 DEG C is taken out, its rheological property and middle press filtration vector FLAPI is measured by GB/T16783.1, wherein rheological property comprises apparent viscosity AV, moulding viscosity PV and yield value YP, and its test result is in table 1.
Table 1
AV /mPa·s PV / mPa·s YP /Pa FL /mL
Base is starched 8.0 5.0 3.0 46.0
The experiment slurry of embodiment 1 4.0 2.6 0.7 11.5
The experiment slurry of embodiment 2 4.5 2.8 0.8 10.5
The experiment slurry of embodiment 3 3.5 2.5 0.5 10.8
The experiment slurry of reference examples 1 5.6 3.5 1.2 16.4
The experiment slurry of reference examples 2 5.4 3.6 1.3 15.8
The experiment slurry of reference examples 3 5.4 3.4 1.2 16.8
Add product of the present invention in 4% base slurry after, fluid loss agent of the present invention is effective, is shown by table 1 result, add product of the present invention in 4% base slurry after, aging through 270 DEG C/16h, filter loss is down to about 11.0mL by 46.0mL, illustrates that this fluid loss agent has good high temperature resistance filtrate reducing effect.In addition, embodiment 3, relative to reference examples 1, significantly can reduce the adding of monomer cardanol the apparent viscosity of base slurry; Embodiment 3 is relative to reference examples 2, and adding of monomer MALEIC ANHYDRIDE can reduce moulding viscosity and yield value; Embodiment 3 relative to reference examples 3, press filtration vector in can reducing the adding of monomer Viscoat 295.

Claims (9)

1., for a preparation method for the modified polyacrylamide fluid loss agent of drilling fluid, it is characterized in that, comprise the steps:
1st step, by weight, add acrylamide monomer 50 ~ 60 parts in the reactor, 1, 3-butylene glycol diacrylate 5 ~ 10 parts, ethylene thiourea 3 ~ 7 parts, Propylene glycol monoacrylate 3 ~ 6 parts, cardanol 4 ~ 7 parts, Viscoat 295 5 ~ 8 parts, MALEIC ANHYDRIDE 3 ~ 4 parts, polyvinyl butyral acetal 2 ~ 8 parts, chainextender 5 ~ 10 parts, 400 ~ 700 parts, water, linking agent 2 ~ 8 parts, 5 ~ 8 parts, tensio-active agent, catalyzer 5 ~ 8 parts, mix, add phosphoric acid regulation system pH value to 4 ~ 6, pass into rare gas element to remove the dissolved oxygen in reaction system,
2nd step, the reaction system of the 1st step gained is cooled to 5 ~ 15 DEG C, then add initiator 5 ~ 8 parts, heat up and carry out polyreaction;
3rd step, the jelly obtained by the reactant that the 2nd step obtains take out, and after granulation, oven dry, pulverizing, obtain modified polyacrylamide fluid loss agent.
2. the preparation method of the modified polyacrylamide fluid loss agent for drilling fluid according to claim 1, is characterized in that: in the 1st described step, tensio-active agent refers to sorbitan ester class tensio-active agent.
3. the preparation method of the modified polyacrylamide fluid loss agent for drilling fluid according to claim 1, it is characterized in that: in the 1st described step, chainextender is the mixture of one or more in l, 4-butyleneglycol, neopentyl glycol, ethylene glycol, glycol ether, glycerine, MALEIC ANHYDRIDE, TriMethylolPropane(TMP), quadrol, diethylenetriamine, triethylene tetramine or dimethylol propionic acid.
4. the preparation method of the modified polyacrylamide fluid loss agent for drilling fluid according to claim 1, it is characterized in that: in the 1st described step, described linking agent is one or more in vinylbenzene, methacrylic acid, methyl methacrylate, vinylformic acid, Phthalic acid, diallyl ester, Ethylene glycol dimethacrylate, vinyl cyanide.
5. the preparation method of the modified polyacrylamide fluid loss agent for drilling fluid according to claim 1, is characterized in that: in the 1st described step, rare gas element is selected from hydrogen, helium or nitrogen.
6. the preparation method of the modified polyacrylamide fluid loss agent for drilling fluid according to claim 1, is characterized in that: in the 1st described step, catalyzer is Hypophosporous Acid, 50 or dibutyl tin laurate.
7. the preparation method of the modified polyacrylamide fluid loss agent for drilling fluid according to claim 1, is characterized in that: described sorbitan ester class tensio-active agent is selected from span 40 or dehydrated sorbitol mono-fatty acid ester.
8. the preparation method of the modified polyacrylamide fluid loss agent for drilling fluid according to claim 1, it is characterized in that: in the 2nd described step, initiator is selected from azo-bis-isobutyrate hydrochloride, 2,2-azo (2-amidine propane) hydrochloride or 2,2-azo [2-(2-tetrahydroglyoxaline-2-base) propane] dihydrochloride.
9. the preparation method of the modified polyacrylamide fluid loss agent for drilling fluid according to claim 1, is characterized in that: in the 2nd described step, and the temperature of polyreaction is 50 ~ 60 DEG C.
CN201510988818.3A 2015-12-26 2015-12-26 Preparation method for modified polyacrylamide filtrate reducer for drilling fluid Pending CN105367710A (en)

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Cited By (6)

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CN108018032A (en) * 2017-12-29 2018-05-11 中国石油集团长城钻探工程有限公司钻井液公司 A kind of fluid loss additive for oil base drilling fluid and preparation method thereof
CN111778004A (en) * 2020-08-12 2020-10-16 中国石油大学(北京) Amphiphilic block polymer ultra-low permeability agent and intelligent temporary plugging type water-based drilling fluid
CN111961160A (en) * 2020-08-04 2020-11-20 中国石油大学(华东) Active polymer for high-molecular gel plugging agent, and preparation method and application thereof
CN114957556A (en) * 2022-06-14 2022-08-30 天津渤海中联石油科技有限公司 Fluid loss additive, preparation method and application thereof, and oil-based drilling fluid
CN116023667A (en) * 2022-12-28 2023-04-28 荆州市东泽化工科技有限公司 Demulsifier and preparation method and application thereof
CN117430748A (en) * 2023-12-20 2024-01-23 东营江源化工有限公司 Emulsion type hydrophobically associating polyacrylamide thickener and preparation process thereof

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108018032A (en) * 2017-12-29 2018-05-11 中国石油集团长城钻探工程有限公司钻井液公司 A kind of fluid loss additive for oil base drilling fluid and preparation method thereof
CN108018032B (en) * 2017-12-29 2020-10-09 中国石油集团长城钻探工程有限公司钻井液公司 Filtrate reducer for oil-based drilling fluid and preparation method thereof
CN111961160A (en) * 2020-08-04 2020-11-20 中国石油大学(华东) Active polymer for high-molecular gel plugging agent, and preparation method and application thereof
CN111961160B (en) * 2020-08-04 2021-06-29 中国石油大学(华东) Active polymer for high-molecular gel plugging agent, and preparation method and application thereof
CN111778004A (en) * 2020-08-12 2020-10-16 中国石油大学(北京) Amphiphilic block polymer ultra-low permeability agent and intelligent temporary plugging type water-based drilling fluid
US11578251B2 (en) 2020-08-12 2023-02-14 China University Of Petroleum (Beijing) Amphiphilic block polymer ultralow-permeability agent and intelligent temporary plugging type water-based drilling fluid
CN114957556A (en) * 2022-06-14 2022-08-30 天津渤海中联石油科技有限公司 Fluid loss additive, preparation method and application thereof, and oil-based drilling fluid
CN114957556B (en) * 2022-06-14 2024-04-05 天津渤海中联石油科技有限公司 Fluid loss additive, preparation method and application thereof, and oil-based drilling fluid
CN116023667A (en) * 2022-12-28 2023-04-28 荆州市东泽化工科技有限公司 Demulsifier and preparation method and application thereof
CN116023667B (en) * 2022-12-28 2024-02-20 荆州市东泽化工科技有限公司 Demulsifier and preparation method and application thereof
CN117430748A (en) * 2023-12-20 2024-01-23 东营江源化工有限公司 Emulsion type hydrophobically associating polyacrylamide thickener and preparation process thereof
CN117430748B (en) * 2023-12-20 2024-03-08 东营江源化工有限公司 Emulsion type hydrophobically associating polyacrylamide thickener and preparation process thereof

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Application publication date: 20160302