CN107488247B - A kind of preparation method of polymer for drilling fluid shale control agent - Google Patents

A kind of preparation method of polymer for drilling fluid shale control agent Download PDF

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CN107488247B
CN107488247B CN201710739016.8A CN201710739016A CN107488247B CN 107488247 B CN107488247 B CN 107488247B CN 201710739016 A CN201710739016 A CN 201710739016A CN 107488247 B CN107488247 B CN 107488247B
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control agent
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CN107488247A (en
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邵亚
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DAQING BEIHUA CHEMICAL PLANT
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Jiangsu Normal University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers 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
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04—Acids; Metal salts or ammonium salts thereof
    • C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers 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
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52—Amides or imides
    • C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/56—Acrylamide; Methacrylamide
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/02—Well-drilling compositions
    • C09K8/03—Specific additives for general use in well-drilling compositions
    • C09K8/035—Organic additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/34—Lubricant additives

Abstract

The invention discloses a kind of preparation methods of polymer for drilling fluid shale control agent, with acrylamide, acrylic acid, potassium hydroxide, dimethyl diallyl ammonium chloride is raw material, polymer shale control agent is prepared by inverse emulsion polymerization method, it synthesizes optimum condition are as follows: acrylamide, acrylic acid, three kinds of monomer weight parts of dimethyl diallyl ammonium chloride are respectively 70 ~ 80 parts, 70 ~ 80 parts, 15 ~ 75 parts, three kinds of monomers are configured to the water phase that pH value is 10, 10 parts by weight Emulsifier Sp-80 are added, T-60, make its emulsion dispersion in the white oil of 100 parts by weight, stabilizer N is added, N’Bimonthly 1 ~ 3 part of osmanthus Ethylene Diamine diethyl sodium sulfonate, reaction temperature is 30 ~ 40 DEG C, reaction time 8h, oxidation/reduction ratio of initiator nPotassium peroxydisulfate: nSodium hydrogensulfite=1:1, initiator are 0.4 parts by weight.The product can be adsorbed on surface of clay and form a kind of semi-permeable membrane, and have stronger encapsulation action, can effectively wrap up landwaste and weaken it by aquation dispersion effect, while compression double electric layer avoids hydration and expansion of clay, inhibitory effect is prominent.

Description

A kind of preparation method of polymer for drilling fluid shale control agent
Technical field
The present invention relates to polymer for drilling fluid shale control agent preparation fields, are a kind of preparation sides of ter-polymers Method.
Background technique
In drilling process, when boring chance strong retraction stratum, mud filtrate invasion mud shale layer will cause shale hydration expansion, Cause many underground problems.For inhibit hydration and expansion of clay, traditional method be in drilling fluid add potassium chloride, sodium chloride or Divalent salts, salt inhibit clay swelling significant effect, but the disadvantage is that can destroy drilling fluid thixotropy and increase filter loss, and Influence the application effect of other inorganic agents.
Amphoteric ion polyacrylamide emulsion is a kind of petroleum drilling and mining industry use that domestic fast development is got up in recent years Agent is managed, can be used as oilfield sewage treatment agent, oil field fracturing thickening agent, oil displacement agent used for tertiary oil recovery etc., molecular weight distribution Uniformly, solution rate is fast, quick in drilling well to form uniform glue, easy to use, but it is improving drilling fluid inhibition Property aspect be rarely reported at present, and mostly also in the desk research stage, the research for its anti-collapse Inhibitory Mechanism is even more It is fewer and fewer.If can will combine the advantages of ACPAM class inorganic agent with emulsion polymerization, it is equal to develop a kind of molecular weight distribution It is even, rate of dispersion is fast in drilling fluid and is capable of the amphoteric ion polyacrylamide emulsion inhibitor of salt-resisting high-temperature-resisting, to realize The fast development of strong rejection capability water-base drilling fluid provides new breakthrough mouth for easily dispersion clay stratum oil and gas development.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of emulsion-type polymer for drilling fluid shale control agent, the pages Rock inhibitor inhibition is good, can effectively wrap up landwaste and weaken it by aquation dispersion effect.
A kind of preparation method of polymer for drilling fluid shale control agent, it is characterised in that method includes the following steps:
1) after 70 ~ 90 parts of acrylic acid being mixed with the potassium hydroxide of equal parts with 70 ~ 90 parts of acrylamides, 15 ~ 75 parts Dimethyl diallyl ammonium chloride is configured to the mixing water phase that pH is 10, to 10 parts by weight Emulsifier Sp-80, T-60's of addition It is slowly added to mixing water phase in 100 parts by weight white oils and emulsion dispersion forms lotion in emulsification pretreatment blender；
2) lotion is transferred in reaction kettle, 5 ~ 9 parts by weight nanometer stabilizers is added while stirring, are then charged with nitrogen, risen Initiator (sodium peroxydisulfate, sodium hydrogensulfite) wiring solution-forming is slowly alternately added in reaction kettle, is slowly stirred, work as reaction by temperature Emulsion viscosity reaches 650cp or more in kettle, and discharging, cooling obtains polymer shale control agent.
Acrylic acid, acrylamide and dimethyl diallyl ammonium chloride mass ratio are 2:2:1 ~ 6:6:5
The utility model has the advantages that the present invention provides a kind of preparation method of emulsion-type polymer for drilling fluid shale control agent, the agent Production procedure is simple, and raw material relatively easily obtains, and joined a kind of nanometer of stabilizer during the preparation process, with good suction Attached performance, the stability for the enhancing water-in-oil emulsion that acts synergistically with emulsifier, is conducive to the growth of synthetic sample strand.With third The product that acrylamide, acrylic acid are synthesized with dimethyl diallyl ammonium chloride for principal monomer, inhibition is prominent, and has one Fixed thickening property, filtration reduction and lubricity, the dosage of low concentration can greatly improve drilling fluid and roll back in drilling fluid Yield.
Specific embodiment
Embodiment 1
It is stirred evenly after 75 parts of acrylic acid is mixed with the potassium hydroxide of equal parts, 75 parts of acrylamides and 25 is added Part dimethyl diallyl ammonium chloride is configured to the mixing water phase that pH is 10, to 10 parts by weight Emulsifier Sp-80, T-60's of addition Mixing water phase is slowly added in 100 parts by weight white oils and in emulsification pretreatment blender with 500r/min shear velocity stirring 1h cream Change dispersion and forms water-in-oil emulsion.Lotion is transferred in reaction kettle, 7 parts by weight nanometer stabilizers are added while stirring, then fill Enter nitrogen, heats up.By nSodium peroxydisulfate:nSodium hydrogensulfite=1:1 weighs 0.4 mass parts initiator wiring solution-forming, is slowly alternately added reaction kettle In, 5h is slowly stirred with 100r/min, when emulsion viscosity reaches 650cp or more in reaction kettle, discharging, cooling obtains polymer page Rock inhibitor.
Above stabilizer the preparation method is as follows:
Step 1, using sodium hydroxide as catalyst, by the 2- bromoethyl sulfonic acid of the ethylenediamine of 15 parts by weight and 105 parts by weight Sodium mixes after being separately added into a small amount of water dissolution, is evaporated under reduced pressure, recrystallizes after being stirred to react 6h at 50 DEG C, filters vacuum drying and obtains Ethylenediamine-N, N '-diethyl sodium sulfonate；
Step 2 is added 40 parts by weight lauric acid in dry three-necked flask, and keeps it complete in 60 DEG C of thermostat water baths It melts, then adjusts the temperature to 65 DEG C, be slowly dropped into 27 parts by weight phosphorus trichlorides with constant pressure funnel, stirring reacts it sufficiently Sealing and standing is stayed overnight afterwards, and supernatant is taken to be evaporated under reduced pressure to obtain lauroyl chloride；
Ethylenediamine-N, N '-diethyl sulfonic acid is added in step 3 in distilled water/acetone mixed solvent three-necked flask is housed Sodium is slowly added to lauroyl chloride after strong stirring, adjusts pH value of solution for 10, by solution after reaction 8h at 30 DEG C with potassium hydroxide 5h is stood, bottom sediment recrystallization 3 is taken to obtain a nanometer stabilizer inferior to 10h dry under nitrogen atmosphere.
Embodiment 2
It is stirred evenly after 70 parts of acrylic acid is mixed with the potassium hydroxide of equal parts, 70 parts of acrylamides and 35 is added Part dimethyl diallyl ammonium chloride is configured to the mixing water phase that pH is 10, to 10 parts by weight Emulsifier Sp-80, T-60's of addition Mixing water phase is slowly added in 100 parts by weight white oils and in emulsification pretreatment blender with 500r/min shear velocity stirring 1h cream Change dispersion and forms water-in-oil emulsion.Lotion is transferred in reaction kettle, 8 parts by weight stabilizers are added while stirring, are then charged with nitrogen Gas, heating.By nSodium peroxydisulfate:nSodium hydrogensulfite=1:1 weighs 0.4 mass parts initiator wiring solution-forming, is slowly alternately added in reaction kettle, with 100r/min is slowly stirred 5h, and when emulsion viscosity reaches 650cp or more in reaction kettle, discharging is cooling to obtain the suppression of polymer shale Preparation.
Embodiment 3
It is stirred evenly after 80 parts of acrylic acid is mixed with the potassium hydroxide of equal parts, 80 parts of acrylamides and 20 is added Part dimethyl diallyl ammonium chloride is configured to the mixing water phase that pH is 10, to 10 parts by weight Emulsifier Sp-80, T-60's of addition Mixing water phase is slowly added in 100 parts by weight white oils and in emulsification pretreatment blender with 500r/min shear velocity stirring 1h cream Change dispersion and forms water-in-oil emulsion.Lotion is transferred in reaction kettle, 9 parts by weight stabilizers are added while stirring, are then charged with nitrogen Gas, heating.By nSodium peroxydisulfate:nSodium hydrogensulfite=1:1 weighs 0.4 mass parts initiator wiring solution-forming, is slowly alternately added in reaction kettle, with 100r/min is slowly stirred 5h, and when emulsion viscosity reaches 650cp or more in reaction kettle, discharging is cooling to obtain the suppression of polymer shale Preparation.
Embodiment 4
It is stirred evenly after 85 parts of acrylic acid is mixed with the potassium hydroxide of equal parts, 85 parts of acrylamides and 17 is added Part dimethyl diallyl ammonium chloride is configured to the mixing water phase that pH is 10, to 10 parts by weight Emulsifier Sp-80, T-60's of addition Mixing water phase is slowly added in 100 parts by weight white oils and in emulsification pretreatment blender with 500r/min shear velocity stirring 1h cream Change dispersion and forms water-in-oil emulsion.Lotion is transferred in reaction kettle, 8 parts by weight stabilizers are added while stirring, are then charged with nitrogen Gas, heating.By nSodium peroxydisulfate:nSodium hydrogensulfite=1:1 weighs 0.4 mass parts initiator wiring solution-forming, is slowly alternately added in reaction kettle, with 100r/min is slowly stirred 5h, and when emulsion viscosity reaches 650cp or more in reaction kettle, discharging is cooling to obtain the suppression of polymer shale Preparation.
Embodiment 5
It is stirred evenly after 90 parts of acrylic acid is mixed with the potassium hydroxide of equal parts, 90 parts of acrylamides and 15 is added Part dimethyl diallyl ammonium chloride is configured to the mixing water phase that pH is 10, to 10 parts by weight Emulsifier Sp-80, T-60's of addition Mixing water phase is slowly added in 100 parts by weight white oils and in emulsification pretreatment blender with 500r/min shear velocity stirring 1h cream Change dispersion and forms water-in-oil emulsion.Lotion is transferred in reaction kettle, 7 parts by weight stabilizers are added while stirring, are then charged with nitrogen Gas, heating.By nSodium peroxydisulfate:nSodium hydrogensulfite=1:1 weighs 0.4 mass parts initiator wiring solution-forming, is slowly alternately added in reaction kettle, with 100r/min is slowly stirred 5h, and when emulsion viscosity reaches 650cp or more in reaction kettle, discharging is cooling to obtain the suppression of polymer shale Preparation.
Embodiment 6
Identical with embodiment 1, difference is: the parts by weight that dimethyl diallyl ammonium chloride is added are 50 parts.
Embodiment 7
Identical with embodiment 3, difference is: the parts by weight that dimethyl diallyl ammonium chloride is added are 60 parts.
Embodiment 8
Identical with embodiment 4, difference is: the parts by weight that dimethyl diallyl ammonium chloride is added are 68 parts.
Embodiment 9
Identical with embodiment 5, difference is: the parts by weight that dimethyl diallyl ammonium chloride is added are 75 parts.
Comparative example 1
Identical with embodiment 1, difference is: being only added without a nanometer stabilizer.
Comparative example 2
Identical with embodiment 1, difference is: the stabilizer being only added is not nanometer stabilizer but hexadecanol.
Comparative example 3
Identical with embodiment 1, difference is: by 20 parts by weight ethylenediamines and 140 weight when only preparing stabilizer Part 2- bromoethyl sodium sulfonate mixing.
Comparative example 4
Identical with embodiment 1, difference is: by 12 parts by weight ethylenediamines and 106 weight when only preparing stabilizer Part 2- bromoethyl sodium sulfonate mixing.
Comparative example 5
Identical with embodiment 1, difference is: lauric acid being replaced with nutmeg when only preparing nanometer stabilizer Acid.
Comparative example 6
Identical with embodiment 1, difference is: dimethyl diallyl ammonium chloride only being replaced with N- vinylpyridine Pyrrolidone.
Performance comparison is carried out with regard to reagent of the present invention and scene common shale control agent NH-1, FCC201 below, it is specific to walk It is rapid as follows:
1, rolling rate of recovery test experiments
Rejection is evaluated using 1500 0032-2013 inhibiting and anti-sloughing agent for drilling fluid evaluation method of Q/SH.
Solution is prepared: measuring 350ml distilled water, 3.50g sample to be tested is added, stirring dissolves it sufficiently.
Xinjiang south Haiti edge An Ji layer core particle 50.0g is weighed, is fitted into the aging tank for filling 350ml sample to be tested, It covers tightly.The aging tank for installing sample is put into roller furnace (pressurize 0.7MPa in aging tank), rolls 16h at 100 DEG C.It takes out old Change tank, is cooled to room temperature, pot liquid and rock sample are all poured on the sub-sieve of a length of 0.425mm of eyelet trim, tap water is used Sieve and wash 1min.Rock sample will be tailed over and be put into 105 DEG C of insulating box dry 4h, taken out cooling, stand in drier and claimed for 24 hours Amount, is calculated as follows its rolling rate of recovery.
In formula, R is the mud shale rate of recovery, %；M 1For the landwaste quality before rolling, g；M 2For landwaste quality after rolling, g.
Table 1 is inhibition evaluation result
Infusing 1:NH-1 is Research Institute of Nanjing Chemical Industry Group and the united polyamines inhibitor of Sinopec Group.
Infuse the shale control agent that 2:FCC201 is the production of U.S. Nalco company.
As shown in Table 1, rolling rate of recovery is increased compared with water after containing landwaste heat rolling in different sample aqueous solutions The rolling rate of recovery of height, clear water generally rises to 65-83% from 25.94%, and embodiment 1 reaches surprising 95.7%,
It can be seen that the proportion of raw material has an immense impact on for the rejection of entire product, the raw material in embodiment 1 is matched Than reaching optimal combination, unexpected benefit is obtained,
In addition, its performance of synthesized inhibitor is better than scene commonly NH-1, FCC201 reagent, but comparison in embodiment 1 Synthesized inhibitor performance decreases compared to embodiment 1 in example 1 ~ 3, it is seen that nanometer stabilizer achieves expectation in embodiment 1 Except technical effect.Comparative example 1-3 explanation, the addition of nanometer stabilizer and the selection of monomer have emphatically inhibitor performance The influence wanted.
2, inhibitor is to drilling fluid rheology, lubricity and filtration reduction comparative evaluation's result
Using GB/T 16783.1-2006 industrial gas oil drilling fluid on-the-spot test part 1 water-base drilling fluid come Evaluate its traditional performance.
Base slurry is prepared: being stirred addition 350ml distilled water in cup, the Huaian 35g soil and 1g sodium bicarbonate, height in height and is stirred 20min, room Temperature maintenance is spare for 24 hours.
Experiment slurry is prepared and test: it is separately added into the sample prepared in 1 part of NH-1, FCC201 and embodiment 1 in base slurry, Its rheological property, middle pressure fluid loss and lubricity are surveyed after heat rolling 16h at 120 DEG C after high-speed stirred 20min.
Table 2 is rheological characteristic, lubricity and filtration reduction comparative evaluation's result
Infusing 1:NH-1 is Research Institute of Nanjing Chemical Industry Group and the united polyamines inhibitor of Sinopec Group.
Infuse the shale control agent that 2:FCC201 is the production of U.S. Nalco company.
As shown in Table 2, NH-1, FCC201 are little to base slurry rheology impact, and polymer shale control agent in the present invention Certain thickening property is shown in base slurry；Three kinds of reagents show stronger filtration reduction, wherein polymer in the present invention Shale control agent filtration reduction is best；Compared with NH-1, FCC201, polymer shale control agent lubricity in base slurry is preferable, Lubricating coefficient reduced rate reaches 50% or more.Therefore, in the present invention polymer for drilling fluid shale control agent except having compared with strong rejection capability Outside, there are also certain thickening property, filtration reduction and lubricities.

Claims (7)

1. a kind of preparation method of polymer for drilling fluid shale control agent, it is characterised in that method includes the following steps:
1) after 70 ~ 90 parts of acrylic acid being mixed with the potassium hydroxide of equal parts with 70 ~ 90 parts of acrylamides, 15 ~ 75 parts of diformazans Base diallyl ammonium chloride is configured to the mixing water phase that pH is 10, to 100 weights that 10 parts by weight Emulsifier Sp-80, T-60 are added It is slowly added to mixing water phase in amount part white oil and emulsion dispersion forms lotion in emulsification pretreatment blender；
2) lotion is transferred in reaction kettle, 5 ~ 9 parts by weight nanometer stabilizers is added while stirring, are then charged with nitrogen, heated up, it will Sodium peroxydisulfate and sodium hydrogensulfite are made into initiator solution, ratio of initiator n sodium peroxydisulfate: n sodium hydrogensulfite=1:1, initiator Parts by weight are 0.4 part, are slowly alternately added in reaction kettle, are slowly stirred, when emulsion viscosity reaches 650cp or more in reaction kettle, Discharging, cooling obtain polymer shale control agent；The nanometer stabiliser materials the preparation method is as follows:
Step 1, using sodium hydroxide as catalyst, by the ethylenediamine of 15 parts by weight and the 2- bromoethyl sodium sulfonate of 105 parts by weight point It is mixed after a small amount of water dissolution is not added, is evaporated under reduced pressure, recrystallizes after being stirred to react 6h at 50 DEG C, filtered vacuum drying and obtain second two Amine-N, N '-diethyl sodium sulfonate；
Step 2 is added 40 parts by weight lauric acid in dry three-necked flask, and keeps it completely molten in 60 DEG C of thermostat water baths Solution, then 65 DEG C are adjusted the temperature to, 27 parts by weight phosphorus trichlorides are slowly dropped into constant pressure funnel, after stirring reacts it sufficiently Sealing and standing is stayed overnight, and supernatant is taken to be evaporated under reduced pressure to obtain lauroyl chloride；
Step 3, the addition ethylenediamine-N in distilled water/acetone mixed solvent three-necked flask is housed, N '-diethyl sodium sulfonate, It is slowly added to lauroyl chloride after strong stirring, it is after reaction 8h that solution is quiet at 30 DEG C with potassium hydroxide adjusting pH value of solution for 10 5h is set, bottom sediment recrystallization 3 is taken to obtain a nanometer stabilizer inferior to 10h dry under nitrogen atmosphere.
2. a kind of preparation method of polymer for drilling fluid shale control agent according to claim 1, it is characterised in that step 1) acrylic acid, acrylamide and dimethyl diallyl ammonium chloride mass ratio are 2:2:1 ~ 6:6:5 in.
3. a kind of preparation method of polymer for drilling fluid shale control agent according to claim 1, it is characterised in that step 1) white oil is one of 10# white oil, 15# white oil or a variety of in, and kinematic viscosity is 9.0 ~ 15.0mm2/s.
4. a kind of preparation method of polymer for drilling fluid shale control agent according to claim 1, it is characterised in that step 2) reaction kettle is ceramic electric heating reaction kettle in.
5. a kind of preparation method of polymer for drilling fluid shale control agent according to claim 1, it is characterised in that step 1) emulsification shear velocity is 500r/min in, and mixing speed is 100r/min in step 2.
6. a kind of preparation method of polymer for drilling fluid shale control agent according to claim 1, it is characterised in that step 1) emulsification shear time is 1h in, and the reaction time is 5h in step 2.
7. a kind of preparation method of polymer for drilling fluid shale control agent according to claim 1, it is characterised in that described Polymer inhibitor weight average molecular weight is 140 ~ 1,800,000.
CN201710739016.8A 2017-08-25 2017-08-25 A kind of preparation method of polymer for drilling fluid shale control agent Active CN107488247B (en)

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CN108329901B (en) * 2018-01-08 2020-10-30 中国石油天然气集团公司 Emulsion type thickening agent for fracturing fluid and preparation method and application thereof
CN110452326B (en) * 2018-12-25 2021-04-23 北京石大博诚科技有限公司 Coating agent for water-based drilling fluid and preparation method thereof
CN111978934A (en) * 2019-05-21 2020-11-24 中石化南京化工研究院有限公司 Strong coating inhibitor for drilling fluid and preparation method thereof
CN113105874B (en) * 2021-04-08 2022-10-28 山东达维石油技术有限公司 Double-inorganic-acid-salt clay stabilizer for shale fracturing and preparation method thereof

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CN102863584A (en) * 2012-09-27 2013-01-09 北京奥凯立科技发展股份有限公司 Preparation method for macromolecule emulsion coating agent for drilling fluid
CN106279520A (en) * 2016-08-31 2017-01-04 成都西油华巍科技有限公司 A kind of drilling fluid amide polymer shale control agent and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102863584A (en) * 2012-09-27 2013-01-09 北京奥凯立科技发展股份有限公司 Preparation method for macromolecule emulsion coating agent for drilling fluid
CN106279520A (en) * 2016-08-31 2017-01-04 成都西油华巍科技有限公司 A kind of drilling fluid amide polymer shale control agent and preparation method thereof

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