CN112011318A - Salt response type high temperature resistant amphoteric ion polymer fluid loss agent and preparation method and application thereof - Google Patents
Salt response type high temperature resistant amphoteric ion polymer fluid loss agent and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a salt response type high temperature resistant amphoteric ion polymer fluid loss agent, a preparation method and an application thereof, wherein the fluid loss agent is prepared from the following raw materials in parts by mass: 2-40 parts of N, N-dimethylacrylamide, 2-20 parts of methacryloxyethyltrimethyl ammonium chloride, 2-20 parts of 2-acrylamide-2-methylpropanesulfonic acid, 4-8 parts of nano-oxide, 1.0-1.5 parts of silane modifier and 0.3-0.4 part of initiator. The salt response type zwitterionic polymer has special polyelectrolyte resistance effect and positive response to salt, essentially realizes the conversion from salt resistance to salt response, and is essentially compatible with salt; the obtained filtrate reducer has excellent salt resistance, temperature resistance and filtrate reduction performance, and has shear thinning property.
Description
Technical Field
The invention relates to a salt response type high temperature resistant amphoteric ion polymer filtrate reducer, a preparation method and application thereof, belonging to the drilling fluid filtrate reducer technology in the field of petroleum exploration and development.
Background
Along with the gradual exhaustion of conventional oil and gas resources, unconventional oil and gas resources such as heavy oil, oil sand, shale oil, shale gas, coal bed gas and the like increasingly become hot spots for development. The deep oil gas resources in China have wide distribution range and large reserves, and become main backup energy for relieving the contradiction between energy supply and demand in China. The depth of deep reservoirs (Tarim, Sichuan, Bohai Bay and the like) in China generally exceeds 6000m, the deepest depth is 9000m, and the bottom temperature is 180-260 ℃. The ultra-deep well has the characteristics of high temperature and pressure, complex geological conditions (mostly salt-gypsum layers), multiple sets of pressure layer systems in the same open hole well section and the like, a target stratum in the drilling process mostly contains complex structures such as broken, cracks and karst caves, the very serious well leakage problem is often caused in the drilling operation process, the drilling construction progress can be seriously influenced, the operation cost is improved, multiple problems such as drilling fluid leakage, reservoir damage, well mouth collapse, drilling sticking, well blowout and the like are easily caused, and even the great influence is caused on the development of deep layer oil gas.
The water-base drilling fluid is a sol-suspension mixed system which takes water as a dispersing medium and takes clay (bentonite), a weighting agent and various chemical treatment agents as dispersing phases; the main components of the agent are water, clay, weighting agent and various chemical treatment agents. The development of water-based drilling fluids basically goes through five stages, namely, stages of natural drilling fluids, finely dispersed drilling fluids, coarsely dispersed drilling fluids, non-dispersed low solid phase drilling fluids, solid phase-free drilling fluids, polymer drilling fluids and the like. In the chemical treating agent for drilling fluid, the filtrate reducer has large dosage and various types, and mainly comprises natural materials, modified products thereof and synthetic polymers. Natural materials and their modified products include starch, cellulose, vegetable gums, xanthan gum and its derivatives; the synthetic polymer mainly takes reactants of phenolic resin and ethylene propylene monomer which are obtained by condensation polymerization of phenolic monomers and aldehyde monomers; under specific conditions, inorganic compounds such as superfine calcium carbonate, ceramic dust and the like can be compounded to be used as the fluid loss additive.
For the ultra-deep well, a high-temperature resistant and salt-resistant filtrate reducer is urgently needed to adapt to the exploitation of the ultra-deep well. The existing filtrate reducer polymer molecular chain is easy to be thermally degraded to lose efficacy under a high-temperature condition, so that the high-temperature resistance of the filtrate reducer polymer is poor. The traditional drilling fluid filtrate reducer has poor salt resistance, and the main reason is polyelectrolyte effect, namely polymer molecular chains extend in water and shrink in saline water, so that the solubility of the polymer molecular chains in the saline water is poor, and the filtrate reducer performance is lost. Reducing the polyelectrolyte effect is an effective way to improve the salt resistance of fluid loss additive polymers in water-based drilling fluids. Conventional additives used in drilling fluids maintain hydration and dispersion of brine drilling fluids by introducing strongly hydrophilic groups such as sulfonic acid groups (2-acrylamido-2-methylpropane sulfonic acid, sodium p-styrenesulfonate, etc.) and carboxylic acid groups; these additives can temporarily resist salt intrusion, but they are not at all compatible with salt; the salt-containing water-based drilling fluid has unstable thermodynamic properties, and is difficult to maintain the performances of stabilizing a well wall, balancing formation pressure, carrying rock debris and lubricating a drilling tool in a high-temperature and high-pressure environment.
In the prior art, reports on improving the temperature and salt resistance of a fluid loss additive have been reported, for example, chinese patent document CN110564381A discloses a composite fluid loss additive for drilling fluid and a preparation method thereof, the composite fluid loss additive comprises: 15-35 parts of modified microcrystalline cellulose, 10-50 parts of acrylamide, 10-40 parts of acrylic acid, 10-30 parts of 2-acrylamide-2-methylpropanesulfonic acid, 10-20 parts of maleic anhydride grafted lignin, 5-20 parts of N-vinyl pyrrolidone and 5-10 parts of nano silicon dioxide. The invention can effectively improve the temperature resistance and salt resistance of the filtrate reducer; however, the drilling fluid system treating agent related by the invention is complex in type, and the later maintenance cost of the drilling fluid is high; the filtration loss is large (more than 12mL) in a high-temperature and high-salt environment, and the molecular structure is essentially incompatible with salt, so that the performance of the drilling fluid is easily deteriorated (viscosity is reduced, the drilling fluid is flocculated), the filtration loss is increased, and the drilling risk is increased. For another example, chinese patent document CN110591667A discloses a high temperature resistant fluid loss additive for drilling fluid and a preparation method thereof, the fluid loss additive includes: 30-60 parts of humic acid resin, 10-50 parts of acrylamide, 10-40 parts of acrylic acid, 10-30 parts of 2-acrylamido-2-methylpropanesulfonic acid, 10-20 parts of maleic anhydride, 5-20 parts of N-vinyl pyrrolidone and 5-10 parts of nano material. The filtrate reducer can effectively improve the temperature resistance and salt resistance of the filtrate reducer, but the drilling fluid system treating agent related by the invention has the advantages of various types, high solid phase content and high later maintenance cost of the drilling fluid; the viscosity of the drilling fluid is reduced in a high-temperature and high-salinity environment, and the filtration loss is large (more than 13 mL); and the molecular structure is essentially incompatible with salt, so that the performance of the drilling fluid is easily deteriorated (viscosity is reduced, the drilling fluid is flocculated), the rock carrying capacity of the drilling fluid is reduced, and the filtration loss is increased, so that the drilling risk is increased.
Disclosure of Invention
Aiming at the defects of the existing filtrate reducer: (1) the traditional filtrate reducer has poor salt resistance, and the drilling fluid is difficult to maintain the performances of stabilizing the well wall, balancing the formation pressure, carrying rock debris and lubricating a drilling tool; (2) the molecular chain of the fluid loss additive is thermally degraded and loses efficacy under the high-temperature condition. The invention aims to provide a salt-response type high-temperature-resistant amphoteric polymer fluid loss agent which has the characteristics of salt responsiveness, salt resistance, high temperature resistance and fluid loss reduction.
The invention also provides a preparation method of the salt response type high temperature resistant zwitterionic polymer fluid loss agent.
The invention also provides application of the salt response type high-temperature resistant zwitterionic polymer fluid loss agent.
The technical scheme of the invention is as follows:
the salt response type high-temperature resistant zwitterionic polymer filtrate reducer is prepared from the following raw materials in parts by mass:
2-40 parts of N, N-dimethylacrylamide, 2-20 parts of methacryloxyethyltrimethyl ammonium chloride, 2-20 parts of 2-acrylamide-2-methylpropanesulfonic acid, 4-8 parts of nano-oxide, 1.0-1.5 parts of silane modifier and 0.3-0.4 part of initiator.
According to the preferable selection of the invention, the salt response type high temperature resistant zwitterionic polymer fluid loss agent is prepared from the following raw materials in parts by mass: 2-30 parts of N, N-dimethylacrylamide, 2-15 parts of methacryloxyethyltrimethyl ammonium chloride, 2-15 parts of 2-acrylamide-2-methylpropanesulfonic acid, 5-7 parts of nano-oxide, 1.0-1.3 parts of silane modifier and 0.3-0.4 part of initiator.
Preferably, the salt-response type high-temperature resistant zwitterionic polymer filtrate reducer is prepared from the following raw materials in parts by mass: 6-20 parts of N, N-dimethylacrylamide, 4-10 parts of methacryloxyethyltrimethyl ammonium chloride, 4-10 parts of 2-acrylamide-2-methylpropanesulfonic acid, 6 parts of nano-oxide, 1.2 parts of silane modifier and 0.375 part of initiator.
According to the invention, the molar ratio of the N, N-dimethylacrylamide, the methacryloxyethyltrimethylammonium chloride and the 2-acrylamido-2-methylpropanesulfonic acid is preferably 7-9:1: 1.
According to the invention, the nano oxide is preferably nano silicon dioxide, nano aluminum oxide, nano titanium dioxide, nano iron oxide, nano zinc oxide or nano zirconium oxide; preferably nano-silica.
Preferably, according to the present invention, the nano-oxide has an average particle size of 10 to 20 nm.
Preferably, according to the invention, the silane modifier is one or a combination of methylchlorosilane, phenylchlorosilane, methylvinylchlorosilane, ethyltrichlorosilane, propyltrichlorosilane, vinyltrichlorosilane or gamma-methacryloxypropyltrimethoxysilane.
According to the invention, the initiator is preferably one or the combination of more than two of ammonium persulfate/sodium bisulfite, potassium persulfate/sodium bisulfite, ammonium persulfate/ferrous sulfate, hydrogen peroxide/ferrous sulfate, benzoyl peroxide/N, N-diethylaniline, potassium persulfate/silver nitrate or persulfate/mercaptan.
The preparation method of the salt response type high temperature resistant amphoteric ion polymer filtrate reducer can adopt the prior art; as a preferable scheme, the preparation method of the salt-response type high-temperature resistant zwitterionic polymer fluid loss agent comprises the following steps:
(1) fully dispersing the nano oxide in ethanol, and adjusting the pH value to 3-5; adding a silane coupling agent, reacting for 1-3h at 60-80 ℃, and performing centrifugal separation and drying to obtain a modified nano oxide;
(2) fully dispersing N, N-dimethylacrylamide, methacryloxyethyltrimethyl ammonium chloride and 2-acrylamide-2-methylpropanesulfonic acid in deionized water, and adjusting the pH value to be neutral to obtain a solution A; fully dispersing the modified nano oxide in ethanol to obtain a solution B; and fully mixing the solution A and the solution B, then adding an aqueous solution of an initiator at the temperature of 50-60 ℃ under an anaerobic condition, stirring for reaction for 4-6 hours, washing with acetone, filtering, and drying to obtain the salt response type high temperature resistant amphoteric ion polymer filtrate reducer.
Preferably, in step (1), the ratio of the mass of the nano-oxide to the volume of the ethanol is 0.01 to 0.02 g/mL.
Preferably, according to the invention, in step (1), the pH is adjusted with an aqueous solution of acetic acid or hydrochloric acid having a mass concentration of 10 to 30%.
According to the present invention, in the step (2), the mass ratio of the total mass of the N, N-dimethylacrylamide, the methacryloxyethyltrimethylammonium chloride and the 2-acrylamido-2-methylpropanesulfonic acid to the deionized water is 1: 2-4.
According to the invention, in the step (2), NaOH water solution with the mass concentration of 15-25% is used for adjusting the pH; preferably, the pH is adjusted with a 20% NaOH aqueous solution.
According to the invention, the mass ratio of the volume of ethanol in the step (2) to the nano oxide in the step (1) is 1-2: 1 mL/g.
According to the invention, in step (2), the mass concentration of the initiator in the aqueous solution of the initiator is preferably 0.02 to 0.05 g/mL.
Preferably, in step (2), the stirring speed in the stirring reaction is 300-500 rpm.
Preferably, according to the invention, the drying in step (2) is carried out under vacuum at 45-55 ℃ for 6-8 hours.
According to the invention, in step (2), the amount of acetone used for washing is determined as required, and the stirring is continued until the precipitate is completely precipitated.
The salt response type high-temperature resistant zwitterionic polymer fluid loss agent is applied to drilling fluid as a fluid loss agent. The specific application method is as follows.
The invention has the technical characteristics that:
under a high-salt environment, the net charge of the conventional fluid loss additive is not 0, when salt ions invade, charged groups on a molecular chain and the salt ions attract each other to form electrostatic attraction, a polyelectrolyte effect is easily generated, the molecular chain is curled, the hydrodynamic volume is rapidly reduced, the viscosity is reduced, the solubility is poor or even insoluble, the viscosity of the drilling fluid is further rapidly reduced, the rheological property is poor, and the fluid loss is increased; the present invention overcomes the above problems. The salt response type zwitterionic polymer fluid loss agent has special polyelectrolyte resisting effect and positive response to salt, 0 net charge zwitterionic polymer is designed from the molecular structure, the conversion from salt resistance to salt response is realized essentially, and the polymer is compatible with the salt essentially. In the molecular structure of the polymer fluid loss additive, positive charges and negative charges on a cationic group and an anionic group are mutually attracted to form an ion interaction network structure among molecular chains; when salt ions invade, the salt ions destroy an ion interaction network, electrostatic interaction on molecular chains of the zwitterionic polymer is shielded, and the molecular structure is changed from a collapsed sphere into a more open spiral shape; under the stimulation of salt ions, the polymer chain is converted from a curling state to a stretching state, so that the solubility and the stability of the salt response type zwitterionic polymer in a high-salt environment are improved, the zwitterionic polymer has higher viscosity in the high-salt environment, and the fluid loss performance of the fluid loss additive under the high-salt environment is further ensured. The molecular chain of the polymer in the fluid loss additive is gradually extended along with the increase of the salt ion strength in the drilling fluid, the hydrodynamic volume is gradually increased, the solubility is gradually increased, and the viscosity is gradually increased, so that the viscosity of the drilling fluid is increased, the fluid loss of the drilling fluid is reduced, and the fluid loss performance is improved. Meanwhile, the filtrate reducer still keeps high-temperature stability at 287 ℃, and polymer molecular chains are difficult to be degraded thermally, so that the filtrate reducer has better high-temperature resistance.
In a high-salt environment, the bentonite drilling fluid is easy to flocculate, so that the viscosity of the drilling fluid is reduced, the rheological property is poor, and the performance of the drilling fluid cannot be normally maintained; the present invention overcomes the above problems. Due to the existence of cation and anion groups in the filtrate reducer, the salt response type zwitterionic polymer has strong hydrophilicity and surface properties and has positive and negative charges; when the salt-responsive zwitterionic polymer is mixed in the drilling fluid, the cationic group, the anionic group and the amide group on the molecular chain of the salt-responsive zwitterionic polymer are respectively connected with the negative charge at the edge of bentonite and Al+Form ionic bonds and hydrogen bonds with Al-OH; therefore, the salt response type zwitterionic polymer can be strongly adsorbed in a clay layer to form a stable space network structure, the bentonite can be effectively dispersed, the bentonite can form a compact mud cake under the action of stratum pressure difference, and the water permeation is reduced, so that the filtration loss is reduced, and the problems of reduced viscosity of drilling fluid, poor rheological property, increased filtration loss and the like caused by flocculation and aggregation of bentonite particles are solved. And most negative charges of the bentonite layer and ammonium salt groups of the salt response type amphoteric ion polymer form ionic bonds, so that ion exchange adsorption between a large amount of sodium ions and the bentonite layer can be effectively prevented, and the problems of viscosity reduction, poor rheological property, filtration loss increase and the like of the drilling fluid caused by flocculation and aggregation of bentonite particles are further avoided.
Meanwhile, the salt response type zwitterionic polymer viscosity reducer disclosed by the invention shows low apparent viscosity at a high shear rate, shows high apparent viscosity at a low shear rate, has better viscoelasticity and shear dilutability, is beneficial to suspending and carrying rock debris, cleans a well hole and enhances the stability of the well wall.
In addition, the nano oxide has large specific surface energy and small particle size, so that the nano oxide can be effectively adsorbed on the surface of clay to physically block micro-nano pores on a well wall. The invention grafts the polymer of specific category on the surface of the nano oxide, realizes the effects of physically blocking cracks, chemically adsorbing bentonite and preventing bentonite particles from flocculating and aggregating, ensures that the temperature resistance of the filtrate reducer can reach 200 ℃, resists salt to saturation, can effectively block nano pores and micro cracks, and reduces the filtrate loss.
The invention has the beneficial effects that:
1. the salt response type zwitterionic polymer has special polyelectrolyte resistance effect and positive response to salt, essentially realizes the conversion from salt resistance to salt response, and is essentially compatible with salt; the filtrate reducer has excellent salt resistance and temperature resistance, and can be suitable for high-temperature deep well strata; experiments prove that the salt-response type zwitterionic polymer filtrate reducer disclosed by the invention can resist the temperature of 200 ℃ and resist the salt to saturation.
2. The salt response type zwitterionic polymer filtrate reducer can effectively block nano pores and microcracks in a stratum under a high-temperature and high-salt environment, so that the filtrate reducer reduces the filtrate loss, and has better filtrate reduction performance when applied to a deep well.
3. The salt response type amphoteric ion polymer fluid loss agent shows low apparent viscosity at a high shear rate, shows high apparent viscosity at a low shear rate, has better viscoelasticity and shear dilutability, is beneficial to suspending and carrying rock debris, cleans a well hole and enhances the stability of the well wall.
Drawings
FIG. 1 is a thermogram of a salt-responsive high temperature resistant zwitterionic polymer fluid loss additive prepared in example 1;
FIG. 2 is an infrared spectrum of a salt-responsive high temperature resistant zwitterionic polymer fluid loss additive prepared in example 1;
figure 3 is a plot of viscosity as a function of shear rate for brine drilling fluids containing fluid loss additives prepared in example 1(a), comparative example 1(b), comparative example 2(c) and comparative example 3 (d).
Detailed Description
The present invention will be further described with reference to the following examples, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified. Unless otherwise specified,% in examples are mass percentages.
Example 1
The salt response type high-temperature resistant zwitterionic polymer filtrate reducer is prepared from the following raw materials in parts by mass:
16.4g of N, N-dimethylacrylamide, 4.3g of methacryloxyethyltrimethyl ammonium chloride, 4.3g of 2-acrylamide-2-methylpropanesulfonic acid, 6g of nano-silica (average particle size of 15nm), 1.2g of a silane modifier (vinyltrichlorosilane), and 0.375g of initiator ammonium persulfate/sodium bisulfite (mass ratio of ammonium persulfate to sodium bisulfite is 1: 1).
The preparation method of the salt response type high temperature resistant zwitterionic polymer fluid loss agent comprises the following steps:
(1) fully dispersing 6g of nano silicon dioxide in 500mL of ethanol, and adjusting the pH to 4 by using an acetic acid water solution with the mass concentration of 20%; after 30min of ultrasonic treatment, 1.2g of silane coupling agent is added, and the mixture is condensed and refluxed for 2h at the water bath temperature of 70 ℃; then centrifugally separating for 10min at the rotating speed of 10000r/min, taking the lower-layer solid, and drying at 50 ℃ to obtain modified nano silicon dioxide;
(2) fully dispersing 16.4g N, N-dimethylacrylamide, 4.3g of methacryloxyethyltrimethyl ammonium chloride and 4.3g of 2-acrylamide-2-methylpropanesulfonic acid in 75mL of deionized water, and adjusting the pH value to 7 by using a sodium hydroxide aqueous solution with the mass concentration of 20% to obtain a solution A; fully dispersing the modified nano oxide obtained in the step (1) in 10mL of ethanol to obtain a solution B; fully mixing the solution A and the solution B, and stirring to prepare a suspension; under the condition of condensing and refluxing in a constant-temperature water bath at 50 ℃, after nitrogen purging for 30min, adding an aqueous solution of an initiator with the mass concentration of 0.02g/mL, mixing and stirring uniformly, and reacting for 4h under stirring at 50 ℃ (400 rpm); and finally, repeatedly washing the synthesized product by using acetone, carrying out suction filtration and vacuum drying at 50 ℃ for 7 hours to obtain the salt response type high-temperature resistant amphoteric ion polymer filtrate reducer.
Thermogravimetric analysis:
in a TA Instruments SDT-Q600 thermogravimetric analyzer/differential scanning calorimeter, an aluminum crucible was used with a purge flow of 50mL min-1Thermogravimetric analysis (TGA) and derivative thermogravimetric analysis (DTG) were performed on the zwitterionic polymer fluid loss additive obtained in this example. The initial temperature was 40 ℃ and the final temperature was 800 ℃.
The TGA profile is shown in fig. 1, and considering that the hydrophilic group (sulfonic group) in the polymer molecule adsorbs moisture in the air, the slow loss of mass from 40 ℃ to 155 ℃ in the TGA profile corresponds to slow evaporation of bound water and free water, resulting in a 4.83% mass loss of the salt-responsive zwitterionic polymer fluid loss additive. In the temperature range of 155-352 ℃, the TGA curve also slowly decreases, which is caused by the thermal degradation of amide groups in the molecular chain of the salt response type zwitterionic polymer fluid loss agent. In the range of 352-432 ℃, the TGA curve is sharply reduced, and the mass loss of the salt response type zwitterionic polymer filtrate reducer is 71.22% corresponding to the thermal degradation of side chain groups such as sulfonic groups in a molecular chain. The TGA curve is smooth after 432 ℃, which shows that the main chain of the salt response type zwitterionic polymer fluid loss agent is broken, and the thermal degradation is basically completed. Overall, the salt-responsive zwitterionic polymer fluid loss additive of the present invention has good thermal stability.
Infrared spectrum determination:
the salt response type amphoteric ion polymer fluid loss agent prepared in the embodiment is uniformly mixed with potassium bromide according to a certain proportion, and then the mixture is pressed for 5 to 10 minutes under the pressure of 2mpa to prepare a thin sheet, and an IRTRacer-100 infrared series spectrophotometer is utilized to carry out the preparation at 400-4000cm-1Absorption spectra in the infrared region are obtained in the wavenumber range.
The infrared spectrum is shown in FIG. 2 and is at 2942cm-1The peak at the wavelength is caused by tensile vibration of methylene in the molecular main chain. At a wavelength of 1645cm-1And 1805cm-1The peak value is respectively absorbed by amido C ═ O bond and C-N bond in the molecular chain of N, N-dimethylacrylamideContraction vibration and contraction vibration. Wavelength of 1421cm-1And 951cm-1The peak values correspond to the absorption vibration peak of a C-N bond and the absorption peak of an N-Cl ionic bond in a molecular chain of the methacryloxyethyltrimethyl ammonium chloride respectively. At 1217cm-1And 1040cm-1The peak at (a) corresponds to the absorption vibration peak of the sulfonic acid group in 2-acrylamido-2-methylpropanesulfonic acid. Wavelength of 478cm-1The peak at (a) corresponds to the peak of the bending vibration of the Si-O-Si bond. In conclusion, the target product is prepared in the example.
Example 2
The salt response type high-temperature resistant zwitterionic polymer filtrate reducer is prepared from the following raw materials in parts by mass:
10.44g of N, N-dimethylacrylamide, 7.28g of methacryloxyethyltrimethyl ammonium chloride, 7.28g of 2-acrylamide-2-methylpropanesulfonic acid, 6g of nano-silica (average particle size of 15nm), 1.2g of a silane modifier (vinyl trichlorosilane), and 0.375g of initiator ammonium persulfate/sodium bisulfite (mass ratio of ammonium persulfate to sodium bisulfite is 1: 1).
The preparation method of the salt response type high temperature resistant zwitterionic polymer fluid loss agent comprises the following steps:
(1) fully dispersing 6g of nano silicon dioxide in 500mL of ethanol, and adjusting the pH to 4 by using an acetic acid water solution with the mass concentration of 20%; after 30min of ultrasonic treatment, 1.2g of silane coupling agent is added, and the mixture is condensed and refluxed for 2h at the water bath temperature of 70 ℃; then centrifugally separating for 10min at the rotating speed of 10000r/min, taking the lower-layer solid, and drying at 50 ℃ to obtain modified nano silicon dioxide;
(2) fully dispersing 10.44g N, N-dimethylacrylamide, 7.28g of methacryloxyethyltrimethyl ammonium chloride and 7.28g of 2-acrylamide-2-methylpropanesulfonic acid in 75mL of deionized water, and adjusting the pH value to 7 by using a sodium hydroxide aqueous solution with the mass concentration of 20% to obtain a solution A; fully dispersing the modified nano oxide obtained in the step (1) in 10mL of ethanol to obtain a solution B; fully mixing the solution A and the solution B, and stirring to prepare a suspension; under the condition of condensing and refluxing in a constant-temperature water bath at 50 ℃, after nitrogen purging for 30min, adding an aqueous solution of an initiator with the mass concentration of 0.02g/mL, mixing and stirring uniformly, and reacting for 4h under stirring at 50 ℃ (400 rpm); and finally, repeatedly washing the synthesized product by using acetone, carrying out suction filtration and vacuum drying at 50 ℃ for 7 hours to obtain the salt response type high-temperature resistant amphoteric ion polymer filtrate reducer.
Example 3
The salt response type high-temperature resistant zwitterionic polymer filtrate reducer is prepared from the following raw materials in parts by mass:
6.06g of N, N-dimethylacrylamide, 9.47g of methacryloxyethyltrimethyl ammonium chloride, 9.47g of 2-acrylamide-2-methylpropanesulfonic acid, 6g of nano-silica (average particle size of 15nm), 1.2g of a silane modifier (vinyltrichlorosilane), and 0.375g of initiator ammonium persulfate/sodium bisulfite (mass ratio of ammonium persulfate to sodium bisulfite is 1: 1).
The preparation method of the salt response type high temperature resistant zwitterionic polymer fluid loss agent comprises the following steps:
(1) fully dispersing 6g of nano silicon dioxide in 500mL of ethanol, and adjusting the pH to 4 by using an acetic acid water solution with the mass concentration of 20%; after 30min of ultrasonic treatment, 1.2g of silane coupling agent is added, and the mixture is condensed and refluxed for 2h at the water bath temperature of 70 ℃; then centrifugally separating for 10min at the rotating speed of 10000r/min, taking the lower-layer solid, and drying at 50 ℃ to obtain modified nano silicon dioxide;
(2) fully dispersing 6.06g N, N-dimethylacrylamide, 9.47g of methacryloxyethyltrimethyl ammonium chloride and 9.47g of 2-acrylamide-2-methylpropanesulfonic acid in 75mL of deionized water, and adjusting the pH value to 7 by using a sodium hydroxide aqueous solution with the mass concentration of 20% to obtain a solution A; fully dispersing the modified nano oxide obtained in the step (1) in 10mL of ethanol to obtain a solution B; fully mixing the solution A and the solution B, and stirring to prepare a suspension; condensing and refluxing the obtained suspension in a constant-temperature water bath at 50 ℃, purging with nitrogen for 30min, adding an aqueous solution of an initiator with the mass concentration of 0.02g/mL, uniformly mixing and stirring, and reacting for 4h at 50 ℃ with stirring (400 rpm); and finally, repeatedly washing the synthesized product by using acetone, carrying out suction filtration and vacuum drying at 50 ℃ for 7 hours to obtain the salt response type high-temperature resistant amphoteric ion polymer filtrate reducer.
Comparative example 1
A preparation method of a filtrate reducer comprises the following steps:
(1) weighing 5g of modified nano-silica (the modified nano-silica prepared by the method in example 1) and placing the modified nano-silica in a conical flask, adding 100mL of deionized water to prepare a suspension with a certain concentration, and magnetically stirring the suspension for 24 hours at normal temperature to obtain an inorganic modified nano-silica suspension.
(2) Adding 50g of acrylic acid and 25g of DMDAAC (dimethyldiallylammonium chloride) into the suspension, uniformly mixing, adjusting the pH to 7-8 by using an aqueous NaOH solution, heating to 50 ℃, stirring, and introducing nitrogen for 30 min. Stopping stirring, adding an initiator ammonium persulfate and sodium bisulfite into the system, wherein the adding amount of the ammonium persulfate and the sodium bisulfite is the same, the total adding amount of the ammonium persulfate and the sodium bisulfite is 0.4 percent of the total mass of the monomers, reacting for 5 hours at 50 ℃, and drying to obtain the target product fluid loss additive.
Comparative example 2
The filtrate reducer is prepared from the following raw materials in parts by mass:
16.4g of N, N-dimethylacrylamide, 4.3g of methacryloxyethyltrimethyl ammonium chloride, 6g of nano-silica (average particle size of 15nm), 1.2g of a silane modifier (vinyl trichlorosilane), and 0.375g of initiator ammonium persulfate/sodium bisulfite (mass ratio of ammonium persulfate to sodium bisulfite is 1: 1).
The preparation method of the filtrate reducer comprises the following steps:
(1) fully dispersing 6g of nano silicon dioxide in 500mL of ethanol, and adjusting the pH to 4 by using an acetic acid water solution with the mass concentration of 20%; after 30min of ultrasonic treatment, 1.2g of silane coupling agent (vinyl trichlorosilane) is added, and the mixture is condensed and refluxed for 2h at the water bath temperature of 70 ℃; then centrifugally separating for 10min at the rotating speed of 10000r/min, taking the lower-layer solid, and drying at 50 ℃ to obtain modified nano silicon dioxide;
(2) fully dispersing 16.4g N, N-dimethylacrylamide and 4.3g of methacryloxyethyltrimethyl ammonium chloride in 75mL of deionized water to obtain a solution A; fully dispersing the modified nano oxide obtained in the step (1) in 10mL of ethanol to obtain a solution B; fully mixing the solution A and the solution B, and stirring to prepare a suspension; under the condition of condensing and refluxing in a constant-temperature water bath at 50 ℃, after nitrogen purging for 30min, adding an initiator aqueous solution with the mass concentration of 0.02g/mL, mixing and stirring uniformly, and reacting for 4h under stirring at 50 ℃ (400 rpm); and finally, repeatedly washing the synthesized product by using acetone, carrying out suction filtration, and carrying out vacuum drying at 50 ℃ for 7h to obtain the filtrate reducer.
Comparative example 3
The filtrate reducer is prepared from the following raw materials in parts by mass:
16.4g of N, N-dimethylacrylamide, 4.3g of 2-acrylamide-2-methylpropanesulfonic acid, 6g of nano-silica (average particle size of 15nm), 1.2g of a silane modifier (vinyl trichlorosilane), and 0.375g of initiator ammonium persulfate/sodium bisulfite (the mass ratio of ammonium persulfate to sodium bisulfite is 1: 1).
The preparation method of the filtrate reducer comprises the following steps:
(1) fully dispersing 6g of nano silicon dioxide in 500mL of ethanol, and adjusting the pH to 4 by using an acetic acid water solution with the mass concentration of 20%; after 30min of ultrasonic treatment, 1.2g of silane coupling agent (vinyl trichlorosilane) is added, and the mixture is condensed and refluxed for 2h at the water bath temperature of 70 ℃; then centrifugally separating for 10min at the rotating speed of 10000r/min, taking the lower-layer solid, and drying at 50 ℃ to obtain modified nano silicon dioxide;
(2) fully dispersing 16.4g N, N-dimethylacrylamide and 4.3g of 2-acrylamide-2-methylpropanesulfonic acid in 75mL of deionized water, and adjusting the pH value to 7 by using a sodium hydroxide aqueous solution with the mass concentration of 20% to obtain a solution A; fully dispersing the modified nano oxide obtained in the step (1) in 10mL of ethanol to obtain a solution B; fully mixing the solution A and the solution B, and stirring to prepare a suspension; under the condition of condensing and refluxing in a constant-temperature water bath at 50 ℃, after nitrogen purging for 30min, adding an initiator aqueous solution with the mass concentration of 0.02g/mL, mixing and stirring uniformly, and reacting for 4h under stirring at 50 ℃ (400 rpm); and finally, repeatedly washing the synthesized product by using acetone, carrying out suction filtration, and carrying out vacuum drying at 50 ℃ for 7h to obtain the filtrate reducer.
Test example 1
Rheological Property test
Preparing a brine drilling fluid: NaCl with different amounts is respectively added into 400mL drilling fluid base slurry with the bentonite content of 4 wt%, and the mixture is uniformly stirred to obtain the brine drilling fluid. The mass concentrations of NaCl in the brine drilling fluid are 0.5%, 10%, 20% and saturated, respectively.
The fluid loss additives prepared in example 1 and comparative examples 1-3 were each added to a brine drilling fluid at a mass fraction of 1%, and the rheological measurements were performed in a Haake Mars rheometer with a shear rate in the range of 10s-1To 200s-1。
The results of the rheological experiment are shown in fig. 3, and it can be seen that the fluid loss additive prepared by the invention shows shear thinning behavior, and the viscosity gradually decreases along with the increase of the shear rate; maintaining high viscosity at low shear rates allows cuttings to be suspended in the wellbore, while at high shear rates, low viscosity allows for rapid injection into the bottom of the wellbore. Furthermore, the viscosity of the drilling fluid increases significantly due to the increased amount of sodium chloride, a phenomenon that intuitively explains the salt response characteristics of the fluid loss additive of the present invention. Compared with the filtrate reducer disclosed by the invention, the filtrate reducer related to the comparative example shows a typical polyelectrolyte effect, the viscosity of the filtrate reducer solution is gradually reduced along with the increase of the content of sodium chloride, so that the viscosity of the drilling fluid in a high-salt environment is rapidly reduced, clay particles cannot be effectively adsorbed and are easy to aggregate and flocculate, the rheological property of the drilling fluid cannot be normally maintained, and the drilling problems such as rock debris accumulation, well diameter expansion, well wall instability and the like are further caused; in addition, pores with larger cracks are easily formed under the action of pressure difference, and the filtration loss is increased.
Test example 2
Fluid loss performance test
Preparing saturated brine drilling fluid: 144g of NaCl is added into 400mL of drilling fluid base slurry with 4 wt% of bentonite, and the mixture is uniformly stirred to obtain the saturated brine drilling fluid.
API low temperature low pressure fluid loss experiment: the fluid loss additives prepared in example 1, example 2, example 3 and comparative examples 1-3 were added to the above-described saturated brine drilling fluid at a mass fraction of 2% each and then aged at aging temperatures of 25 ℃, 120 ℃, 150 ℃, 180 ℃ and 200 ℃ for 30 minutes, respectively, and the API low temperature low pressure fluid loss test was conducted at a constant pressure of 100psi at ambient temperature (25 ℃) in accordance with the GB/T16783-.
HTHP high temperature high pressure fluid loss experiment: the fluid loss additives prepared in example 1, example 2, example 3 and comparative examples 1-3 were each added to the above-described saturated brine drilling fluid at a mass fraction of 2% and tested according to the GB/T16783-.
The results of the experiment are shown in table 1 below:
TABLE 1 fluid loss at different temperatures
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| FLAPI(25℃) | 4.2 | 4.4 | 4.8 | 10.5 | 12.4 | 11.8 |
| FLAPI(120℃) | 4.4 | 4.6 | 5 | 12.6 | 18.6 | 17.2 |
| FLAPI(150℃) | 4.6 | 5.2 | 5.5 | 13 | 25 | 24.2 |
| FLAPI(180℃) | 5.2 | 5.8 | 6.6 | 13.6 | 36.7 | 34 |
| FLAPI(200℃) | 6.8 | 7.8 | 8.4 | 16.8 | 68.4 | 61.2 |
| FLHTHP(120℃) | 14.6 | 15.8 | 16.4 | 26.8 | 56.4 | 52.4 |
| FLHTHP(150℃) | 15.8 | 16.2 | 17.9 | 33.4 | 79.2 | 68.8 |
| FLHTHP(180℃) | 17.2 | 18.6 | 19.6 | 34.6 | 94.6 | 85.7 |
| FLHTHP(200℃) | 25.8 | 26.3 | 31.8 | 39.5 | 142.8 | 168.3 |
As can be seen from table 1 above, the fluid loss additive of example 1 is most effective in reducing fluid loss in brine drilling fluids. The molecular chain of the fluid loss additive is stretched in saturated saline water, so that the fluid loss additive has high viscosity and high solubility, and can effectively adsorb bentonite particles; in addition, the amide group and the sulfonate group respectively form stable hydrogen bonds and ionic bonds with the bentonite, so that the amide group and the sulfonate group are effectively adsorbed on the surface of the bentonite, and simultaneously, ion exchange adsorption between a large amount of sodium ions and a bentonite layer can be effectively prevented, so that the bentonite keeps certain dispersibility, and the flocculation and aggregation of bentonite particles are avoided; so that the bentonite with better dispersion forms compact mud cakes under the action of pressure difference, the water permeation is reduced, and the filtration loss is reduced. In the comparative example, the viscosity of the filtrate reducer is reduced in saturated saline water, the solubility is reduced, clay particles cannot be effectively adsorbed, the clay particles are aggregated and flocculated, and a mud cake formed under the action of pressure difference has large cracks and pores, which results in higher filtrate loss.
Claims (9)
1. The salt response type high-temperature resistant zwitterionic polymer filtrate reducer is prepared from the following raw materials in parts by mass: 2-40 parts of N, N-dimethylacrylamide, 2-20 parts of methacryloxyethyltrimethyl ammonium chloride, 2-20 parts of 2-acrylamide-2-methylpropanesulfonic acid, 4-8 parts of nano-oxide, 1.0-1.5 parts of silane modifier and 0.3-0.4 part of initiator.
2. The salt-responsive high-temperature resistant zwitterionic polymer fluid loss agent as claimed in claim 1, which is prepared from the following raw materials in parts by mass: 2-30 parts of N, N-dimethylacrylamide, 2-15 parts of methacryloxyethyltrimethyl ammonium chloride, 2-15 parts of 2-acrylamide-2-methylpropanesulfonic acid, 5-7 parts of nano-oxide, 1.0-1.3 parts of silane modifier and 0.3-0.4 part of initiator.
3. The salt-responsive high-temperature resistant zwitterionic polymer fluid loss agent as claimed in claim 2, wherein the salt-responsive high-temperature resistant zwitterionic polymer fluid loss agent is prepared from the following raw materials in parts by mass: 6-20 parts of N, N-dimethylacrylamide, 4-10 parts of methacryloxyethyltrimethyl ammonium chloride, 4-10 parts of 2-acrylamide-2-methylpropanesulfonic acid, 6 parts of nano-oxide, 1.2 parts of silane modifier and 0.375 part of initiator.
4. The salt-responsive high temperature resistant zwitterionic polymer fluid loss additive of claim 1, wherein the molar ratio of N, N-dimethylacrylamide, methacryloxyethyltrimethylammonium chloride, and 2-acrylamido-2-methylpropanesulfonic acid is 7-9:1: 1.
5. The salt-responsive high temperature resistant zwitterionic polymer fluid loss additive of claim 1, characterized by one or more of the following conditions:
a. the nano oxide is nano silicon dioxide, nano aluminum oxide, nano titanium dioxide, nano iron oxide, nano zinc oxide or nano zirconium oxide; preferably nano silicon dioxide;
b. the average grain diameter of the nano oxide is 10-20 nm;
c. the silane modifier is one or a combination of methyl chlorosilane, phenyl chlorosilane, methyl vinyl chlorosilane, ethyl trichlorosilane, propyl trichlorosilane, vinyl trichlorosilane or gamma-methacryloxypropyl trimethoxysilane;
d. the initiator is one or the combination of more than two of ammonium persulfate/sodium bisulfite, potassium persulfate/sodium bisulfite, ammonium persulfate/ferrous sulfate, hydrogen peroxide/ferrous sulfate, benzoyl peroxide/N, N-diethylaniline, potassium persulfate/silver nitrate or persulfate/mercaptan.
6. A method of preparing a salt-responsive high temperature resistant zwitterionic polymer fluid loss additive as described in any one of claims 1-5, comprising the steps of:
(1) fully dispersing the nano oxide in ethanol, and adjusting the pH value to 3-5; adding a silane coupling agent, reacting for 1-3h at 60-80 ℃, and performing centrifugal separation and drying to obtain a modified nano oxide;
(2) fully dispersing N, N-dimethylacrylamide, methacryloxyethyltrimethyl ammonium chloride and 2-acrylamide-2-methylpropanesulfonic acid in deionized water, and adjusting the pH value to be neutral to obtain a solution A; fully dispersing the modified nano oxide in ethanol to obtain a solution B; and fully mixing the solution A and the solution B, then adding an aqueous solution of an initiator at the temperature of 50-60 ℃ under an anaerobic condition, stirring for reaction for 4-6 hours, washing with acetone, filtering, and drying to obtain the salt response type high temperature resistant amphoteric ion polymer filtrate reducer.
7. The method for preparing the salt-responsive high temperature resistant zwitterionic polymer fluid loss additive of claim 6, wherein step (1) comprises one or more of the following conditions:
a. the volume ratio of the mass of the nano oxide to the volume of the ethanol is 0.01-0.02 g/mL;
b. adjusting pH with 10-30% acetic acid or hydrochloric acid aqueous solution.
8. The method for preparing the salt-responsive high temperature resistant zwitterionic polymer fluid loss additive of claim 6, wherein step (2) comprises one or more of the following conditions:
a. the mass ratio of the total mass of the N, N-dimethylacrylamide, the methacryloxyethyltrimethyl ammonium chloride and the 2-acrylamide-2-methylpropanesulfonic acid to the deionized water is 1: 2-4;
b. adjusting the pH value by using a NaOH aqueous solution with the mass concentration of 15-25%;
c. the volume of the ethanol and the mass ratio of the nano oxides in the step (1) are 1-2: 1 mL/g;
d. the mass concentration of the initiator in the initiator aqueous solution is 0.02-0.05 g/mL.
9. Use of the salt-responsive high temperature resistant zwitterionic polymer fluid loss additive as defined in any one of claims 1 to 5 as a fluid loss additive in drilling fluids.
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