CN112852532B - High-temperature-resistant nano composite lubricant and preparation method and application of emulsion thereof - Google Patents

High-temperature-resistant nano composite lubricant and preparation method and application of emulsion thereof Download PDF

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CN112852532B
CN112852532B CN202110020946.4A CN202110020946A CN112852532B CN 112852532 B CN112852532 B CN 112852532B CN 202110020946 A CN202110020946 A CN 202110020946A CN 112852532 B CN112852532 B CN 112852532B
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CN112852532A (en
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柯扬船
付媛
潘雪超
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China University of Petroleum Beijing
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00—Lubricating compositions containing more than 10% water
    • 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
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    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/10—Nanoparticle-containing well treatment fluids
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    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/34—Lubricant additives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/084—Inorganic acids or salts thereof containing sulfur, selenium or tellurium
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10—Compounds containing silicon
    • C10M2201/102—Silicates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/04—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing aromatic monomers, e.g. styrene
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/18—Natural waxes, e.g. ceresin, ozocerite, bees wax, carnauba; Degras
    • C10M2205/183—Natural waxes, e.g. ceresin, ozocerite, bees wax, carnauba; Degras used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/40—Fatty vegetable or animal oils
    • C10M2207/401—Fatty vegetable or animal oils used as base material
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/18—Containing nitrogen-to-nitrogen bonds, e.g. hydrazine
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/02—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/028—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a nitrogen-containing hetero ring
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2221/00—Organic macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2221/02—Macromolecular compounds obtained by reactions of monomers involving only carbon-to-carbon unsaturated bonds

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Lubricants (AREA)

Abstract

The invention provides a high temperature resistant nano composite lubricant, a preparation method and application of emulsion thereof, which adopts a composition of high temperature resistant monomers, comonomers and a layered structure nano intermediate, and is prepared by the following steps: 1) mixing and stirring a high-temperature-resistant monomer, a comonomer, an inorganic layered structure nano intermediate, an emulsifier, a cross-linking agent and water for 30min under an inert atmosphere to obtain a mixed system; 2) heating the mixed system to 70 ℃, adding an initiator, maintaining the temperature, and continuously stirring for 7-10h to obtain a nano composite emulsion; 3) mixing the nano composite emulsion, oleic acid and industrial base oil, stirring for 10min at room temperature, and uniformly mixing to obtain the high-temperature-resistant nano composite lubricant, which is characterized by having extreme pressure wear resistance nano composite microsphere lubricant, nano high-efficiency nucleation property, high temperature resistance, easy dispersibility, good compatibility with drilling fluid and high-efficiency lubricity.

Description

High-temperature-resistant nano composite lubricant and preparation method and application of emulsion thereof
Technical Field
The invention relates to a high-temperature-resistant nano composite lubricant, a preparation method and a specific application thereof, belonging to the technical field of oil and gas field engineering.
Background
With the expansion and deepening of the field of petroleum and natural gas exploration and development, the drilling task amount is rapidly increased, accidents such as drilling tool abrasion, drilling tool jamming, failure and the like occur occasionally, particularly, the drilling fluid, the completion fluid, the fracturing fluid or other oil and gas engineering fluids used in deep wells and ultra-deep wells have very high temperature and pressure, and the drilling fluid, the completion fluid, the fracturing fluid or other oil and gas engineering fluids are required to have good high-temperature resistance and high-temperature lubrication and resistance reduction characteristics.
Lubricants are one treatment added to drilling, completion or fracturing fluids to improve the lubricating properties, primarily to reduce the torque, wear and abrasion of the tools of the drilling process and their rate of damage. Lubricants are classified into liquid type and solid type lubricants according to phase state. The liquid lubricant mainly comprises mineral oil, vegetable oil, alcohol ether, ester, nano-material lubricant and the like. The solid lubricant mainly comprises plastic pellets, glass pellets, graphite, carbon black lubricant and the like.
The deep well and ultra-deep well are in a high-temperature environment, the conventional liquid lubricant is easy to volatilize, degrade and crosslink under a high-temperature condition to lose activity and lose effectiveness, and the conventional lubricant for high-temperature resistant drilling fluid, completion fluid and fracturing fluid cannot effectively solve the problems of deactivation and effectiveness of the lubricant.
The Chinese patent invention CN201510132577.2 in the prior art discloses a lubricant for high-temperature resistant drilling fluid, which comprises the main raw materials of synthetic lubricating grease, fatty acid, emulsifier, calcium petroleum sulfonate and sodium sulfite, wherein the lubricant has a reduction rate of lubricating coefficient of 80% after being aged for 16h at 200 ℃ and a reduction rate of 70% after being aged at 220 ℃, which indicates that the temperature resistance, the aging resistance and the lasting quality of the lubricant are all to be improved.
In the prior art (Zhang Wen, Du Yi and Kong Fa. preparation and performance evaluation of an emulsion type drilling fluid lubricant, 2016, 45 (04): 73-76 in the chemical industry of petroleum and natural gas) polyamine, cotton seed oil and low carbon acid are adopted to synthesize vegetable oil amide, and then the vegetable oil amide is modified to prepare the oil-in-water emulsion type drilling fluid lubricant, 0.5 percent of the product is added into the drilling fluid, and the reduction rate of the lubrication coefficient is 82.7 percent after the drilling fluid is aged at 170 ℃, but the lubrication effect at higher temperature is poor.
The Chinese invention patent CN201810407333.4 in the prior art discloses a high temperature resistant lubricant for drilling fluid and a preparation method thereof, wherein the lubricant mainly comprises biodiesel, white oil or diesel oil, zinc dialkyl dithiophosphate, boron nitride, an emulsifier and a dispersant. However, the preparation method needs calcination at the temperature of 280-300 ℃, the reaction conditions are harsh, and the energy consumption is large.
The defects of the prior art are that the prior lubricant is generally composed of organic matters, the high-temperature resistance stability of organic matter molecules is poor, and the organic matter molecular chains are obviously bent and rotated to be gradually broken under the impact of high temperature, so that the original characteristics are quickly lost. In order to solve the problem, the Chinese patent of invention CN201810390855.8 in the prior art discloses a method for preparing a lubricant by intercalation in-situ polymerization compounding of a lamellar compound, and a high polymer nano composite microsphere antiwear agent and a lubricant composition thereof are prepared by adopting a high polymer monomer and an inorganic lamellar compound.
Similarly, the existing high polymer nano composite lubricant technology has the well-known problems of nano agglomeration and the like, namely, the existing lubricant nano structure is unevenly distributed and is unevenly stressed under the action of an external force, so that the lubricating failure of machines and tools used under the complex working conditions of an underground deep ultra-deep layer or an oil and gas reservoir and the high-temperature complex working conditions of oil and gas engineering is caused, or the effects of persistent effect, efficient lubricating resistance reduction and torque reduction are difficult to generate, and therefore the problems of eccentric wear, diameter reduction or drilling blockage accidents and the like exist for a long time.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-temperature-resistant nano composite lubricant, and a preparation method and application of an emulsion thereof.
The technical scheme of the invention is as follows:
the high-temperature-resistant nano composite lubricant is characterized by comprising the following components in parts by mass:
Figure BDA0002886346690000021
the high-temperature resistant monomer is one or more of N-vinyl pyrrolidone, N-vinyl caprolactam, N-vinyl methyl diphenyl methoxysilane, sodium allyl sulfonate, sodium p-styrene sulfonate and sodium divinylbenzene sulfonate, and the high-temperature resistant monomer is a comonomer.
The preferable inorganic layered structure nano intermediate is a layered structure system of layered graphite, layered silicate and/or layered molybdenum disulfide, and the interlayer distance is enlarged to more than 1 time of the original interlayer distance through the intercalation of an intercalation agent.
Further preferably, the layered silicate is selected from one or more of montmorillonite, kaolin, hydrotalcite, sepiolite, wollastonite and chlorite.
Further preferably, the intercalation agent is selected from one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, hexadecyl trimethyl ammonium bromide and tributyl tetradecyl phosphorus chloride.
Preferably, the high-temperature resistant monomer is selected from one or more of N-vinyl pyrrolidone, N-vinyl caprolactam and sodium p-styrene sulfonate.
Preferably, the emulsifier is one or more selected from sodium dodecyl sulfate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate.
Preferably, the crosslinking agent is selected from one or more of divinylbenzene, N-methylene bisacrylamide and dicumyl peroxide.
Preferably, the initiator is one or more selected from potassium persulfate, ammonium persulfate, N-dimethylaniline and azobisisobutyronitrile.
Preferably, the base oil is one or more of industrial silicone oil, industrial paraffin oil, industrial white oil, industrial vegetable oil or industrial polyalphaolefin synthetic oil.
The preparation method of the high-temperature-resistant nano composite lubricant is characterized by comprising the following steps of:
(1) mixing and stirring the styrene monomer, the high-temperature resistant monomer, the inorganic layered structure nano intermediate, the emulsifier, the cross-linking agent and water for 20-40min under inert atmosphere;
(2) heating the mixed system to 65-75 ℃, adding an initiator, continuously stirring for 7-10h, and carrying out emulsion polymerization, suspension polymerization or dispersion polymerization reaction to obtain a nano composite emulsion;
(3) and mixing the base oil, the nano-composite emulsion and the oleic acid, and uniformly stirring at room temperature to obtain the high-temperature-resistant nano-composite lubricant.
Preferably, the step (1) is carried out under the protection of inert atmosphere, nitrogen is firstly introduced into the reaction kettle for 20-30min to remove oxygen in the reaction kettle, the purity of the nitrogen is not less than 99.999 percent, the pressure is 0.5-0.55MPa, and the flow is 40-50m3/h。
Preferably, the styrene monomer in the step (1) is pretreated, washed with 7-9% by mass of aqueous sodium hydroxide solution, adjusted to pH 7-8, dried over anhydrous magnesium sulfate and stored at low temperature.
The preferable inorganic layered structure nano intermediate is prepared by the following steps:
1) mixing 1.0-10.0 parts by mass of layered silicate and 100-200 parts by mass of water, heating to 70-80 ℃, and stirring for 30 min;
2) adding 1.0-5.0 parts by mass of an intercalating agent, and stirring at constant temperature for 10-12h to obtain an intercalation system;
3) and filtering, washing, drying and grinding the intercalation system to obtain the inorganic layered structure nano intermediate.
The drilling fluid is characterized by comprising the high-temperature-resistant nano-composite lubricant, wherein the mass fraction of the high-temperature-resistant nano-composite lubricant in the drilling fluid is 0.1-5%.
The invention has the following technical effects:
the invention adopts high temperature resistant monomer, comonomer and nano material, and in-situ copolymerization reaction is carried out to form a copolymerization chain winding structure and a nanometer controllable and uniformly dispersed copolymerization nanometer composite microsphere system, and the system has inorganic nanometer phase-organic phase interface bonding, loaded lubricating component and extreme pressure antiwear lubricating property. High temperature resistant monomers, containing heteroatoms, especially N heteroatoms, are converted to positive nitrogen ions (-N) by reaction under acidic conditions+) The quaternary amination structural monomer is N-vinyl caprolactam, N-vinyl pyrrolidone and N-vinyl methyl diphenyl methoxylsilane, the structure of the quaternary amination structural monomer can increase the volume of a side group of a macromolecular chain to increase the steric hindrance of a main chain, inhibit the high-temperature rotation and the bending property of the macromolecular chain, and form a multipolymer molecular chain with a multi-heterocyclic structure, and the multipolymer molecular chain has higher rigidity and temperature resistance. Positive nitrogen ion (-N)+) Quaternizing the structural monomer, and carrying out in-situ intercalation copolymerization reaction with the layered structure nano intermediate to peel the layered structure intermediate in situ to form an inorganic lamella-organic copolymerization chain composite structure system, wherein the composite structure has strong interface adsorption, bonding and high-temperature stability. The nanometer intermediate with layered structure and the high temperature resistant monomer have copolymerization reaction and crosslinking reactionTo form a 0.35-1.0nm lamella or 0.35-1.0nm lamella multiple dispersed composite system, to generate high temperature resistant interface stability, compatibility, uniform dispersibility and pressure bearing lubricity, to form high temperature resistant, extreme pressure resistant and wear resistant lubricant copolymerized nano composite microspheres and a composition system thereof.
The high-temperature-resistant nano composite lubricant is prepared by in-situ copolymerization intercalation reaction of a high molecular monomer and a nano intermediate with a layered structure, stripping and dispersing to generate a large surface area and a strong-adsorption high-activity 1nm lamella, and a copolymerization chain nano composite microsphere system is formed in situ, has the characteristics of blocking and isolating external high-temperature thermal shock and aging effect or high-temperature resistance, has viscoelasticity, and generates strong-adsorption viscoelasticity, extreme pressure wear-resistant lubrication migration and protection effect on a metal surface, a metal drilling tool surface or a rock surface; in the process of migration and friction on the metal surface, the surface of a metal drilling tool or the rock surface, a nano composite lubricating film is formed to generate the protection characteristics of friction hot melting or sintering state, strong adsorption, high toughness, high tensile strength and high breaking strength.
Drawings
FIG. 1 is a scanning electron microscope photograph of nanocomposite particles prepared in example 1 of the present invention;
FIG. 2 is a transmission electron microscope photograph of the nanocomposite particles prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to examples of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The formula of the embodiment is as follows by mass:
20 parts of styrene monomer, 5 parts of high-temperature resistant monomer N-vinyl pyrrolidone, 3 parts of layered structure nano intermediate layered silicate, 3 parts of emulsifier sodium dodecyl sulfate, 5 parts of cross-linking agent divinylbenzene, 3 parts of initiator potassium persulfate, 100 parts of water, 30 parts of base oil industrial silicone oil and 30 parts of oleic acid.
The inorganic layered structure nano intermediate is prepared by the following steps:
1) mixing 3 parts by mass of phyllosilicate and 100 parts by mass of water, heating to 70-80 ℃, and stirring for 30 min;
2) adding 3 parts by mass of sodium dodecyl sulfate serving as an intercalation agent, and stirring at a constant temperature for 10 hours to obtain an intercalation system;
3) and filtering, washing, drying and grinding the intercalation system to obtain the inorganic layered structure nano intermediate.
The preparation method of the high-temperature-resistant nano-composite lubricant of the embodiment is as follows: firstly, washing a styrene monomer by using 8% sodium hydroxide aqueous solution, adjusting the pH to 7-8, drying a pretreated product by using anhydrous magnesium sulfate, and carrying out reduced pressure distillation to obtain the styrene monomer with polymerization purity; mixing and stirring a styrene monomer, a high-temperature-resistant monomer, a layered nano intermediate, an emulsifier, a cross-linking agent and water for 30min under an inert atmosphere; adding an initiator, heating the mixed system to 70 ℃, and keeping the temperature for continuously stirring for 7-10h to obtain a nano composite emulsion; mixing the base oil, the oleic acid and the nano-composite emulsion, and uniformly stirring at room temperature to obtain the high-temperature-resistant nano-composite lubricant.
And (3) performing post-treatment on part of the obtained nano composite emulsion in the step (2), performing emulsion breaking, filtering, drying and grinding by using ethanol to obtain nano composite particles, and using the nano composite particles as test characteristics. As shown in the scanning electron microscope image of fig. 1, it is illustrated that the synthetic particles are spherical in shape, and microscopically change sliding friction into rolling friction, reduce friction coefficient, reduce abrasion, and can function like a "ball bearing"; as shown in the transmission electron micrograph of fig. 2, an intercalated structure was demonstrated.
Example 2
The formula of the embodiment is as follows by mass:
10 parts of styrene monomer, 3 parts of high-temperature resistant monomer N-vinyl pyrrolidone, 0.1 part of layered structure nano intermediate layered silicate, 0.1 part of emulsifier sodium dodecyl sulfate, 0.1 part of cross-linking agent divinylbenzene, 0.01 part of initiator potassium persulfate, 50 parts of water, 20 parts of base oil industrial silicone oil and 20 parts of oleic acid.
Example 3
The formula of the embodiment is as follows by mass:
30 parts of styrene monomer, 10 parts of high-temperature resistant monomer N-vinyl pyrrolidone, 5 parts of layered structure nano intermediate layered silicate, 5 parts of emulsifier sodium dodecyl sulfate, 10 parts of cross-linking agent divinylbenzene, 5 parts of initiator potassium persulfate, 200 parts of water, 50 parts of base oil industrial silicone oil and 50 parts of oleic acid.
Example 4
The formula of the embodiment is as follows by mass:
20 parts of styrene monomer, 5 parts of high-temperature resistant monomer N-vinyl caprolactam, 3 parts of layered structure nano intermediate layered silicate, 3 parts of emulsifier lauryl sodium sulfate, 5 parts of cross-linking agent N, N-methylene bisacrylamide, 3 parts of initiator ammonium persulfate, 100 parts of water, 30 parts of base oil industrial paraffin oil and 30 parts of oleic acid.
Example 5
20 parts of styrene monomer, 5 parts of high-temperature resistant monomer sodium styrene sulfonate, 3 parts of layered structure nano intermediate layered silicate, 3 parts of emulsifier sodium dodecyl benzene sulfonate, 5 parts of cross-linking agent dicumyl peroxide, 3 parts of initiator N, N-dimethylaniline, 100 parts of water, 30 parts of base oil industrial white oil and 30 parts of oleic acid.
Example 6
20 parts of styrene monomer, 5 parts of high-temperature resistant monomer N-vinyl pyrrolidone, 3 parts of layered structure nano intermediate layered silicate, 3 parts of emulsifying agent hexadecyl trimethyl ammonium bromide, 5 parts of cross-linking agent divinylbenzene, 3 parts of initiator azobisisobutyronitrile, 100 parts of water, 30 parts of base oil industrial vegetable oil and 30 parts of oleic acid.
Preparing base slurry of drilling fluid: adding 20.0g of montmorillonite and 0.8g of anhydrous sodium carbonate into 400mL of deionized water, stirring for 20min at a high speed of 5000rpm on a high-speed stirrer, and sealing and maintaining for 24h at room temperature to obtain the drilling fluid base slurry with the soil content of 6%.
The nano-composite lubricant of example 1 was added to the prepared base slurry of the drilling fluid at room temperature, and stirred at a high speed of 5000rpm for 20min on a high speed stirrer to obtain the drilling fluid of this example. Wherein the mass fractions of the lubricant composition in the drilling fluid are 0.2%, 0.5%, 0.8%, and 1.0%, and examples 1-1 to 1-4 are constituted.
The obtained drilling fluid is subjected to performance test, and the specific test method refers to SY/T1088-2012.
Lubrication Performance test
The drilling fluid was taken and the lubrication coefficient was measured with an extreme pressure lubricator, the results of which are shown in table 1.
The lubrication coefficient reduction rate was calculated as follows (formula is not given):
R＝(K0-K1)/K0×100％
wherein R represents a lubrication coefficient decrease rate; k0Represents the extreme pressure lubrication coefficient of the base slurry; k1Representing the extreme pressure lubrication coefficient of the drilling fluid.
The test characterization results are shown in table 1.
TABLE 1
Examples Lubrication factor reduction rate R (%)
1-1 63.5
1-2 76.4
1-3 85.8
1-4 89.6
As can be seen from Table 1, with the increase of the amount of the lubricant, the lubricating property of the drilling fluid is obviously improved, and the reduction rate of the lubricating coefficient is gradually increased, which shows that the lubricating property of the drilling fluid can be obviously improved by adding the nano composite lubricant, the friction coefficient is effectively reduced, and the lubricating and drag reducing effects are achieved.
Rheological Property test
And (3) respectively taking the base drilling fluid slurry and the drilling fluid of the embodiments 1-4, and pouring the base drilling fluid slurry and the drilling fluid of the embodiments 1-4 into a measuring cup of a six-speed rotary viscometer to enable the liquid level to be equal to the scale mark of an outer cylinder of the viscometer. The viscometer's speed was measured from high to low set at 600, 300, 200, 100, 6 and 3rpm, respectively, and after stabilization, the readings were taken and recorded as θ600、θ300、θ200、θ100、θ6、θ3. After the test is finished, the rotating speed is set to 600rpm, the drilling fluid in the measuring cup is stirred for 1 minute, after the measuring cup is kept still for 10 seconds, the rotating speed is set to 3rpm, the maximum value of the dial is read, and the maximum value is recorded as theta3-1. Stir again for 1 minute, rest for 10 minutes, set the speed to 3rpm, read the maximum dial value, and record as θ3-2. The test results are shown in Table 2.
Apparent viscosity: AV ═ θ600×0.5
Plastic viscosity: PV ═ theta600－θ300
Dynamic shear force: YP is 0.511 × (θ)300－PV)
Static shearing force: g ″, 0.511 × θ3-1，G'＝0.511×θ3-2
The test characterization results are shown in table 2.
TABLE 2
Figure BDA0002886346690000071
As can be seen from Table 2, with the addition of the lubricant, the changes of the values of the apparent viscosity, the plastic viscosity, the dynamic shear force and the static shear force are small, which indicates that the lubricant has good compatibility with the drilling fluid, has little influence on the rheological property of the drilling fluid, and indicates that the system has good rheological stability.
Heat resistance test
The drilling fluids of examples 1-4 were taken and tested for changes in their properties after hot rolling in roller furnaces at 160 deg.C, 200 deg.C and 240 deg.C, respectively, for 16 h.
The test results are shown in Table 3
TABLE 3
Figure BDA0002886346690000081
As can be seen from Table 3, with the temperature rise, the apparent viscosity, the plastic viscosity and the dynamic shear force of the drilling fluid are slightly changed, the reduction rate of the lubricating coefficient is gradually reduced, and the drilling fluid still has good lubricating property after being hot rolled for 16 hours at 240 ℃, which indicates that the lubricating drilling fluid can resist the temperature of 240 ℃. Similar effects can be obtained by carrying out the above experiments using examples 2 to 6.

Claims (14)

1. The high-temperature-resistant nano composite lubricant is characterized by comprising the following components in parts by mass:
Figure FDA0003540563620000011
the high-temperature resistant monomer is one or more of N-vinyl pyrrolidone, N-vinyl caprolactam, N-vinyl methyl diphenyl methoxysilane, sodium allyl sulfonate, sodium p-styrene sulfonate and sodium divinylbenzene sulfonate, and a copolymerization chain winding structure and a nanometer controllable and uniformly dispersed copolymerization nanometer composite microsphere system are formed through in-situ copolymerization.
2. The composite lubricant according to claim 1, characterized in that the inorganic layered structured nano-intermediate is a layered structure system of layered graphite, layered silicate and/or layered molybdenum disulfide, and the interlayer spacing is enlarged to more than 1 time of its original interlayer spacing by intercalation of an intercalating agent.
3. The composite lubricant according to claim 2, characterized in that the layered silicate is selected from one or more of montmorillonite, kaolin, hydrotalcite, sepiolite, wollastonite and chlorite.
4. The composite lubricant according to claim 2, wherein the intercalating agent is selected from one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, cetyl trimethyl ammonium bromide, and tributyl tetradecyl phosphonium chloride.
5. The composite lubricant according to claim 1, wherein the high temperature resistant monomer is selected from one or more of N-vinyl pyrrolidone, N-vinyl caprolactam, and sodium p-styrene sulfonate.
6. The composite lubricant according to claim 1, wherein the emulsifier is one or more selected from sodium dodecyl sulfate, and sodium dodecyl benzene sulfonate.
7. The composite lubricant according to claim 1, wherein the cross-linking agent is selected from one or more of divinylbenzene, N-methylenebisacrylamide, and dicumyl peroxide.
8. The composite lubricant according to claim 1, wherein the initiator is selected from one or more of potassium persulfate, ammonium persulfate, N-dimethylaniline and azobisisobutyronitrile.
9. The composite lubricant according to claim 1, wherein the base oil is one or more of industrial silicone oil, industrial paraffin oil, industrial white oil, industrial vegetable oil, or industrial polyalphaolefin synthetic oil.
10. The method for preparing the emulsion of the high temperature resistant nanocomposite lubricant according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) mixing and stirring the styrene monomer, the high-temperature resistant monomer, the inorganic layered structure nano intermediate, the emulsifier, the cross-linking agent and water for 20-40min under inert atmosphere;
(2) heating the mixed system to 65-75 ℃, adding an initiator, continuously stirring for 7-10h, and carrying out emulsion polymerization, suspension polymerization or dispersion polymerization reaction to obtain a nano composite emulsion;
(3) and mixing the base oil, the nano-composite emulsion and the oleic acid, and uniformly stirring at room temperature to obtain the high-temperature-resistant nano-composite lubricant.
11. The method of claim 10, wherein step (1) is carried out under an inert atmosphere by introducing nitrogen into the reactor at a purity of not less than 99.999% at a pressure of 0.5-0.55MPa and a flow rate of 40-50m for 20-30min to remove oxygen therein3/h。
12. The method according to claim 10, wherein the styrene monomer in the step (1) is subjected to pretreatment, washed with a 7-9% by mass aqueous solution of sodium hydroxide, adjusted to pH 7-8, dried over anhydrous magnesium sulfate and stored at low temperature.
13. The method according to claim 10, wherein the inorganic layered nano-intermediate is prepared by the steps of:
1) mixing 1.0-10.0 parts by mass of layered silicate and 100-200 parts by mass of water, heating to 70-80 ℃, and stirring for 30 min;
2) adding 1.0-5.0 parts by mass of an intercalating agent, and stirring at constant temperature for 10-12h to obtain an intercalation system;
3) and filtering, washing, drying and grinding the intercalation system to obtain the inorganic layered structure nano intermediate.
14. Use of a high temperature resistant nanocomposite lubricant according to any of claims 1 to 9 in a drilling fluid wherein the high temperature resistant nanocomposite lubricant is present in the drilling fluid at a weight fraction of 0.1 to 5%.
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