CN108753267B - Superhigh temperature resistant anionic polymer fluid loss additive for drilling fluid and completion fluid and preparation method thereof - Google Patents
Superhigh temperature resistant anionic polymer fluid loss additive for drilling fluid and completion fluid and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an ultra-high temperature resistant anionic polymer fluid loss additive for a drilling fluid completion fluid and a preparation method thereof, the ultra-high temperature resistant salt resistant polymer fluid loss additive is a terpolymer generated by aqueous solution polymerization of alkenyl monomer acrylamide, strongly hydrophilic anionic alkenyl monomer 2-acrylamide-2-methylpropanesulfonic acid and alkenyl monomer dimethylaminoethyl methacrylate, wherein the molar ratio of anionic alkenyl monomer 2-acrylamide-2-methylpropanesulfonic acid contained in a molecular chain unit reaches 35-42.5%, the ultra-high temperature resistant salt resistant polymer fluid loss additive has extremely strong hydrophilicity and solubility, the molecular chain of the polymer contains 1,400-containing 2,000 structural units, the weight average molecular weight is 650,000-containing 850,000, and the number average molecular weight is 600,000-containing 700,000. The filtrate reducer has good solubility in ultra-high temperature water-based drilling fluid, the temperature resistance can reach 248 ℃, the filtrate reducer can obviously reduce the filtrate loss of the water-based drilling fluid completion fluid under the ultra-high temperature condition by adding a small amount of filtrate reducer, and the drilling fluid completion fluid can keep good colloidal stability under the ultra-high temperature condition.
Description
The technical field is as follows:
the invention relates to an ultra-high temperature resistant anionic polymer fluid loss additive and a preparation method thereof, belonging to the technical field of drilling fluid and completion fluid in petroleum and natural gas drilling engineering, exploration and development of earth deep resources and geothermal well drilling engineering.
Background art:
with the gradual expansion of oil and gas exploration and development in the world to deep oil and gas resources, the continuous promotion of deep resource exploration in China, continental scientific drilling engineering, earth deep exploration plans and other important deep projects, the exploration, development and utilization of geothermal resources, the ultrahigh-temperature water-based drilling fluid completion fluid technology has become one of the core technologies in the drilling engineering. At present, the ultra-high temperature water-based drilling fluid completion fluid system widely used all over the world mainly takes 'polysulfonate drilling fluid' as a main component, wherein polymer products are indispensable ultra-high temperature water-based drilling fluid completion fluid additives, have strong hydrophilicity and larger hydrodynamic volume after hydration, and can play a good role in protecting glue and reducing filtration loss on the drilling fluid completion fluid. However, the existing polymer fluid loss additive capable of resisting the drilling fluid and completion fluid with the temperature of above 220 ℃ is less in quantity, and has certain defects in the field practical application process, which mainly shows that the existing widely used polymer fluid loss additive has poor ultrahigh temperature (more than 220 ℃) resistance, insufficient complex salt resistance, unsatisfactory fluid loss resistance and gel protection performance under the ultrahigh temperature environment and the like.
In the past, when a high-temperature resistant polymer fluid loss additive is researched and developed, a temperature-resistant comonomer often selected needs to have more hydration groups and adsorption groups, so that a group of multipolymers with certain temperature resistance and salt resistance are developed, and the main reason is that a high-molecular polymer with more hydration groups and adsorption groups can effectively make up the reduction of the hydration performance of the high-molecular polymer and the reduction of the high-temperature adsorption characteristic caused by high-temperature dehydration of the polymer under the high-temperature condition. However, the multipolymer prepared from the comonomer containing more hydrated groups and adsorption groups still cannot meet the technical requirements of the ultrahigh-temperature water-based drilling fluid completion fluid on the polymer treating agent when the temperature exceeds 220 ℃, and the main reason is that the performance of the polymer treating agent at the temperature below 220 ℃ and the performance of the polymer treating agent in the ultrahigh-temperature environment when the temperature exceeds 220 ℃ cannot be coordinated and unified, especially the direct and indirect effects of the ultrahigh-temperature polymer treating agent on the change of the physicochemical property of water serving as a continuous phase in the water-based drilling fluid under the ultrahigh-temperature and high-pressure conditions are ignored in the past, so that the efficiency of the polymer treating agent under the ultrahigh-temperature environment is greatly reduced.
In a mixed solution of a plurality of polymers, under a certain constant temperature and pressure, the thermodynamic equilibrium condition of a multi-component polymer solution system is that the change delta G of free enthalpy before and after each polymer solution is mixed is less than or equal to 0. Since the entropy of mixing between high-molecular polymers is small, complete compatibility can be achieved only when there is a strong interaction between the polymers or the repulsive force between segments of the components themselves is greater than that between the components. Most polymers are thermodynamically incompatible or only partially compatible with each other. Generally, the larger the relative molecular mass of the polymer participating in the multi-component polymer solution, the more difficult the thermodynamic equilibrium condition of the multi-component polymer solution system is to be met, and the new knowledge proves why the solubility of the high molecular polymer filtrate reducer in water is changed from soluble to insoluble along with the increase of the relative molecular mass, and simultaneously can also verify that the water-soluble treating agent of the drilling fluid completion fluid in a high-temperature or ultra-high-temperature environment forms a super-large molecular or three-dimensional cross-linked high molecular compound due to the cross-linking effect or free radical polymerization reaction caused by high temperature, finally leads to the deterioration of the solubility, loses the efficacy of the water-soluble drilling fluid treating agent, and even acts on the drilling fluid completion fluid reversely. In addition, the interaction between the molecular chains of different high molecular polymers is an important influence factor for influencing the thermodynamic compatibility of the multi-component polymer solution, and the larger the interaction between the macromolecular chains of the high molecular polymers is, the better the compatibility is if hydrogen bonds, strong dipole effects, ionic effects and the like are formed. The compatibility of the multi-component high molecular polymer solution can be promoted by hydrogen bond action, ion interaction, pi-pi electron conjugation action, intermolecular charge transfer action generated when high molecules with electron-rich groups and electron-deficient groups are blended, and the like.
Chinese patent document CN105733524A (application number: 201610150092.0) discloses a high-temperature-resistant and salt-resistant filtrate reducer and a preparation method thereof. The fluid loss agent comprises, by weight, 3-10 parts of acrylamide, 15-25 parts of 2-acrylamide-2-methylpropanesulfonic acid, 20-40 parts of sodium styrene sulfonate, 3-8 parts of maleic anhydride, 27-52 parts of a sodium hydroxide aqueous solution, 3-6 parts of an ammonium persulfate aqueous solution and 220 parts of purified water. The preparation method of the filtrate reducer comprises the following steps: adding purified water, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, sodium styrene sulfonate and maleic anhydride into a container, dissolving, adding a sodium hydroxide aqueous solution and an ammonium persulfate aqueous solution, and reacting at constant temperature to obtain the fluid loss additive. The filtrate reducer can effectively reduce the filtrate loss of a high-temperature saturated brine water-based drilling fluid system, but when persulfate is used as an initiator, two reaction monomers of sodium styrene sulfonate and maleic anhydride and two monomer tools of acrylamide and 2-acrylamide-2-methylpropanesulfonic acid are used, the product performance change is large along with the change of the reaction process due to the obvious difference of reactivity ratios of the reaction monomers, and meanwhile, similar comonomers such as maleic anhydride and sodium styrene sulfonate are not high in activity, so that the conversion rate of the reaction monomers is not high, the product performance is influenced, and the field application temperature of the product in the drilling fluid completion fluid is generally lower than 220 ℃.
Chinese patent document CN104388061A (application number: 201410513354.6) discloses a high-temperature-resistant salt-resistant polymer filtrate reducer for water-based drilling fluid and a preparation method thereof, wherein the filtrate reducer comprises 8-39 parts by weight of N-vinyl caprolactam, 20-100 parts by weight of 2-acrylamido-2-methylpropanesulfonic acid, 20-50 parts by weight of acrylic acid, 10-45 parts by weight of N, N-2 methacrylamide and 100-200 parts by weight of water; the preparation method specifically comprises the steps of neutralizing an acidic monomer with sodium hydroxide, controlling the pH value of a system to be 7.0-11.0, adding a nonionic monomer, stirring until the nonionic monomer is dissolved, taking an oxidation-reduction initiation system as an initiator, carrying out aqueous solution polymerization in the presence of a molecular weight regulator to obtain the polymer filtrate reducer, wherein the reaction temperature is 25-60 ℃, the reaction time is 4-6 hours, and drying and crushing the obtained colloidal product to obtain the polymer filtrate reducer. The filtrate reducer can effectively improve the problems of temperature resistance, salt resistance, viscosity retention rate after high-temperature aging and the like of drilling fluid in deep wells and ultra-deep wells. However, the catalyst used in this patent document is still a conventional oxidation-reduction initiation system, which has low initiation efficiency, high initiation temperature, and is not favorable for effectively controlling the relative molecular mass of the product during the reaction process, and is prone to "implosion" for an alkenyl reaction monomer which is prone to polymerization, and at the same time, the reaction time is relatively long or very short; in addition, the product synthesized by the initiation system can only reduce the filtration loss of the drilling fluid by 50-80% under the influence of the subcritical water property change in a high-temperature and high-pressure environment.
The invention content is as follows:
aiming at the defects of the prior art, the invention provides the polymer fluid loss additive which can resist ultra-high temperature (higher than 248 ℃), has strong salt resistance, has strong glue protection capability to a water-based drilling fluid completion fluid under the environment of ultra-high temperature and high pressure, has good fluid loss reduction effect, has good compatibility with other treating agents, and simultaneously has the function of inhibiting hydration and dispersion of deep complex shale.
The technical scheme of the invention is as follows:
an ultra-high temperature resistant anionic polymer fluid loss additive for a drilling and completion fluid, having the structure of formula (I):
the filtrate reducer is a terpolymer generated by the aqueous solution polymerization reaction of an alkenyl reaction monomer acrylamide, a strongly hydrophilic anionic alkenyl monomer 2-acrylamide-2-methylpropanesulfonic acid and an alkenyl monomer dimethylaminoethyl methacrylate;
in the formula (I), x, y and z represent the mole numbers of acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and dimethylaminoethyl methacrylate, respectively, and the mole ratio x: y: z is (4.75-5.25): 3.5-4.25): 1.0-3.0.
According to the invention, preferably, the anionic alkenyl monomer 2-acrylamide-2-methylpropanesulfonic acid contained in the filtrate reducer molecular chain unit accounts for 35-42.5 mol%, and has extremely strong hydrophilicity and solubility;
preferably, the molecular chain of the fluid loss agent contains 1,400-2,000 structural units, the weight-average molecular weight is 650,000-850,000, and the number-average molecular weight is 600,000-700,000.
According to the invention, the filtrate reducer preferably comprises 1,600-1,700 structural units in the molecular chain, and the molar ratio x/y/z is (4.95-5.05): 3.75-4.05): 1.0-1.5); the weight average molecular weight is 690,000-740,000, and the number average molecular weight is 620,000-650,000.
According to the invention, the preparation method of the ultrahigh-temperature resistant anionic polymer fluid loss additive for the drilling fluid and completion fluid comprises the following steps:
dissolving reactants of acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and dimethylaminoethyl methacrylate in a solvent, putting the mixture into a reaction kettle, adjusting the concentration of the mixed solution of the reactants by the solvent, adjusting the pH value by alkali, adding a catalyst, heating the mixed solution in the reaction kettle, maintaining the reaction time, terminating the reaction, drying, crushing and sieving to obtain the superhigh temperature resistant anionic polymer filtrate reducer.
According to the present invention, preferably, the solvent is water;
preferably, the catalyst is one or two of azodiisobutyamidine oxazoline hydrochloride, azodiisobutyamidine hydrochloride, azodicyan valeric acid or azodiisopropyl imidazoline;
preferably, the alkali is sodium hydroxide or potassium hydroxide;
preferably, the pH is adjusted to 5 to 9, more preferably 6.5 to 7.5.
According to the present invention, the total weight of the reactant monomers is preferably 8 to 20wt%, more preferably 12 to 16wt%, of the total weight of the solution formed by the reactants and the solvent;
preferably, the weight of the required catalyst is 0.05 to 0.5wt%, more preferably 0.15 to 0.30wt% of the total weight of the reactants;
preferably, the reaction temperature is 35 to 80 ℃, and more preferably 40 to 60 ℃;
preferably, the reaction time is 2 hours to 8 hours, and more preferably 3.5 hours to 4.5 hours;
preferably, the drying temperature is 105-;
preferably, the granularity of the fine granular product after crushing and sieving is 10-40 meshes, and more preferably 20-40 meshes; the particle size of the fine particle product is 0.9mm, and the balance of the sieve is less than 15%; the dry content of the fine-particle product is > 90%.
In order to improve the solubility and compatibility of the polymer fluid loss additive in an ultrahigh-temperature environment, the invention creatively optimizes and selects the alkenyl reaction monomer acrylamide, the alkenyl reaction monomer 2-acrylamide-2-methylpropanesulfonic acid with excellent salt resistance and the novel alkenyl polymerization monomer dimethylaminoethyl methacrylate with a plurality of methyl groups, methylene groups and ester groups through the molecular structure optimization design. Meanwhile, in the polymerization catalysis method, a novel water-soluble azo initiator is optimally selected as a catalyst for reaction, so that the novel ultrahigh-temperature-resistant salt-resistant polymer filtrate reducer for the drilling fluid completion fluid is obtained, the polymer filtrate reducer can form an association structure through ionic or intermolecular interaction force and the like between molecular chains under the ultrahigh-temperature environment by depending on a part of hydrophobic groups, the solubility of a high-molecular polymer under the ultrahigh-temperature and high-pressure environment is obviously improved, the action effect of the polymer filtrate reducer under the ultrahigh-temperature environment is enhanced, and the gel protection effect and the filtrate reduction effect of the polymer filtrate reducer for the drilling fluid completion fluid under the ultrahigh-temperature and high-pressure environment are better than those of the conventional polymer filtrate reducer for the drilling fluid completion fluid.
The reaction process of the invention is as follows:
the ultrahigh-temperature resistant anionic polymer fluid loss additive has the following action mechanism and beneficial effects:
(1) according to the viscosity increasing mechanism, after a small amount of the polymer fluid loss additive is added, the viscosity of the water-based drilling fluid completion fluid is obviously increased, and the viscosity retention rate of the drilling fluid completion fluid after high-temperature aging is relatively high, so that the filtrate viscosity of the drilling fluid completion fluid is increased, and a compact mud cake can be formed, so that the fluid loss is reduced.
(2) In a high-temperature environment, sulfonic groups in the molecular chain of the polymer fluid loss additive can be adsorbed on the surface of clay particles to form a thicker hydration film, so that the content of free water is reduced, and the thermal stability of the drilling fluid is enhanced.
(3) Polymer fluid loss additives with higher relative molecular mass can effectively coat drill cuttings, thereby reducing the hydration dispersion capacity of the drill cuttings.
(4) The high-compatibility high-temperature and high-pressure environment can be realized by the aid of more methyl and methylene contained in dimethylaminoethyl methacrylate chain links in polymer molecular chains.
(5) The filtrate reducer of the invention has good solubility in ultra-high temperature water-based drilling fluid, good compatibility with other water-based drilling fluid completion fluid treating agents, temperature resistance up to 248 ℃, and can significantly reduce the filtrate loss of the water-based drilling fluid completion fluid under the ultra-high temperature condition, and simultaneously can maintain good gel protection performance under the ultra-high temperature condition.
Description of the drawings:
FIG. 1 is an infrared spectrum characteristic diagram of the ultra-high temperature resistant anionic polymer fluid loss additive for the drilling fluid and completion fluid prepared in example 1 of the invention.
The specific implementation mode is as follows:
the present invention is further illustrated by, but is not limited to, the following specific examples.
In the examples, the starting materials used are all conventional commercial products unless otherwise specified.
The polymeric fluid loss additives of the examples have the structure described by formula (I):
the filtrate reducer is a terpolymer generated by the aqueous solution polymerization reaction of an alkenyl reaction monomer acrylamide, a strongly hydrophilic anionic alkenyl monomer 2-acrylamide-2-methylpropanesulfonic acid and an alkenyl monomer dimethylaminoethyl methacrylate;
in formula (I), x, y and z represent the mole numbers of acrylamide, 2-acrylamide-2-methyl-propanesulfonic acid and dimethylaminoethyl methacrylate, respectively.
Example 1:
respectively weighing 64.8 g of acrylamide and 43.0 g of dimethylaminoethyl methacrylate in a 2.5L reaction kettle provided with a stirrer, a reflux condenser, a nitrogen protection device, a temperature sensor and a heating device, pouring the weighed materials into the reaction kettle, adding 500 ml of tap water, and stirring at a high speed to fully dissolve the materials; weighing 132.2 g of 2-acrylamide-2-methylpropanesulfonic acid, dissolving in 300 ml of tap water, adjusting the pH to 7 by using 10-14 mol/L NaOH solution, and pouring into a reaction kettle; the reactant mixture in the reaction kettle is fully stirred. Weighing 0.72 g of azodiisobutyl amidine hydrochloride, dissolving the azodiisobutyl amidine hydrochloride in 100 ml of tap water, stirring the mixture to be completely dissolved, and placing the mixture into a reaction kettle; the reaction kettle is supplemented with tap water to 1600 ml, the total concentration of reactants is controlled to be 15%, and the solution in the reaction kettle is rapidly stirred for 5 minutes. Stirring at high speed for 30 minutes under the protection of nitrogen, heating to 55 ℃, reacting for 4 hours, cooling to room temperature, taking out the jelly in the reaction kettle, drying in a vacuum oven at 105 ℃ for 8 hours, crushing, and sieving with a 20-mesh sieve to obtain the ultrahigh-temperature resistant anionic polymer filtrate reducer.
The molar ratio of reacted monomers in the polymer, x: y: z, was 5.0: 3.5: 1.5, the polymer had a weight average molecular weight of about 73.4 ten thousand, a number average molecular weight of about 64.6 ten thousand and a number of structural units of about 1680.
Example 2:
adding 1000 kg of tap water into a stainless steel corrosion-resistant reaction kettle which is provided with a stirrer, a reflux condenser, a nitrogen protection device, a thermometer and a heating device and has the capacity of 3-3.5 tons, starting the stirrer, adding 211.8kg of 2-acrylamide-2-methyl-propanesulfonic acid at the speed of 25 kg/min, stirring for 10 minutes, adding 5 kg/min of sodium hydroxide solid, adjusting the pH value to 7-7.5, adding 1500 kg of tap water into the reaction kettle, and controlling the temperature to be lower than 40 ℃; adding 96.3 kg of acrylamide at the speed of 25 kg/min, adding 500 kg of tap water, and stirring for 10 min; then 53.2 kg of dimethylaminoethyl methacrylate is added, and the mixture is stirred for 5 minutes; 1.038 kg of azobisisobutylamidine hydrochloride was weighed, dissolved in 25 kg of tap water and poured into the reactor. Continuously adding tap water into a reaction kettle until the total weight of the tap water is 2400kg, introducing nitrogen, stirring for 30 minutes, heating to 55-58 ℃, reacting for 4 hours, cooling to room temperature, taking out jelly in the reaction kettle, drying by a drying device (spray drying method), and then crushing and screening by a 20-mesh sieve to obtain the ultrahigh-temperature resistant anionic polymer filtrate reducer.
The molar ratio of reacted monomers in this polymer, x: y: z, was 5.0: 3.75: 1.25, the weight average molecular weight of the polymer was about 72.4 ten thousand, the number average molecular weight was about 62.6 ten thousand, and the number of structural units was about 1640.
Comparative example 1:
the amide group in acrylamide has a strong adsorption effect on clay minerals, so that the amide group is usually used as one of key functional monomers for synthesizing the polymer fluid loss agent, while the amide group is easy to generate hydrolysis reaction under a high temperature condition to generate carboxyl, so that the fluid loss effect of the fluid loss agent is influenced, and the temperature resistance of the traditional polymer fluid loss agent containing acrylamide chain units in a polymer molecular chain is generally less than 180 ℃. However, when acrylamide is copolymerized with dimethylaminoethyl methacrylate and other anionic alkenyl reaction monomers, the indoor test result of the obtained product shows that the temperature resistance of the polymer containing the acrylamide monomer in the molecular chain is obviously improved. For this purpose, in the synthesis of the fluid loss agent, x/y was set to 5.0/3.75, and by changing the molar ratio of dimethylaminoethyl methacrylate in the polymer under constant conditions for other variables, comparative example 1-1 (containing no molecular chain units of dimethylaminoethyl methacrylate), comparative example 1-2 (containing 0.5 molar ratio of dimethylaminoethyl methacrylate), comparative example 1-3 (containing 0.75 molar ratio of dimethylaminoethyl methacrylate), comparative example 1-4 (containing 1.0 molar ratio of dimethylaminoethyl methacrylate), and comparative example 1-5 (containing 1.25 molar ratio of dimethylaminoethyl methacrylate) were synthesized.
And (3) preparing saturated saline base slurry, namely adding 400m L of tap water into a high-stirring cup, sequentially adding 0.8g of anhydrous sodium carbonate and 16g of second-grade bentonite for the drilling fluid at the stirring speed of 8000 rpm, stirring for 2 hours, sealing and standing for 24 hours, adding NaCl to reach a saturated concentration, and uniformly stirring to obtain the saturated saline base slurry.
Preparation and testing of test slurries: 1.5% of the comparative example was added to the saturated saline base slurry, and the slurry was stirred at a high speed of 8000 rpm to be uniform, and the rheology and fluid loss of each test slurry were measured. The test slurries were loaded into a high temperature aging tank, heat roll aged at 180 ℃ for 16 hours, and the rheology and fluid loss of each test slurry were measured in the same manner, with the results shown in Table 1.
Table 1 test results in saturated brine-based slurries
Comparative example 2:
in the invention, the proportion of acrylamide and anionic monomer 2-acrylamide-2-methyl-propanesulfonic acid has obvious influence on the high temperature and salt resistance of the polymer fluid loss additive. When the molar ratio of the acrylamide to the 2-acrylamide-2-methyl-propanesulfonic acid is too large, the temperature resistance, the salt resistance and the filtrate loss reduction performance of the obtained product are not ideal; when the molar ratio of acrylamide to 2-acrylamido-2-methyl-propanesulfonic acid is too small, the temperature resistance, salt resistance and fluid loss resistance of the resulting product are also not satisfactory. For this purpose, the molar ratio of dimethylaminoethyl methacrylate was set to 1.25 during the synthesis of the filtrate reducer, and comparative examples 2-1 (x/y: 5.0: 3.75 in the product), 2-2 (x/y: 6.0: 3.75 in the product), 2-3 (x/y: 7.0: 3.75 in the product), 2-4 (x/y: 5.0: 4.75 in the product), and 2-5 (x/y: 5.0: 5.75 in the product) were synthesized by changing the ratio of acrylamide to anionic monomer 2-acrylamido-2-methylpropanesulfonic acid under constant conditions with other variables.
The saturated brine-based slurry formulation, test slurry formulation and test method were identical to those described in comparative example 1, with the results shown in table 2.
Table 2 test results in saturated brine-based slurries
The temperature resistance, salt resistance and fluid loss reduction performance of the polymer fluid loss additive of the present invention are evaluated by the following test examples.
The test method in the test example is ① GB/T32198-2015 general rules of infrared spectrum quantitative analysis technology, and ② adopts GB/T16738-1997 water-based drilling fluid field test program.
Test example 1: infrared spectroscopic analysis of the ultra high temperature resistant anionic polymer fluid loss additive of example 1 of the present invention.
An infrared spectrum characteristic spectrum of the superhigh temperature resistant anionic polymer fluid loss additive is measured by a potassium bromide tabletting method by adopting a Fourier transform infrared spectrometer, and is shown in figure 1.
Test example 2: the fluid loss additive of the superhigh temperature resistant anionic polymer described in example 1 was tested for relative molecular mass.
The relative molecular mass of the superhigh temperature resistant anionic polymer fluid loss additive is obtained by analysis by adopting a gel permeation chromatograph, and is shown in table 3.
Table 3 relative molecular mass analysis of example 1 samples
Test example 3: test for inhibiting hydration and dispersion performance of shale
An aqueous solution of the sample of example 2 with a concentration of 0.5%, a 0.5% aqueous solution of a polymer high-temperature-resistant and salt-resistant fluid loss additive drisca D for an inlet drilling fluid, a 0.5% aqueous solution of polyacrylamide potassium salt KPAM for a drilling fluid, and a 0.5% aqueous solution of a zwitterionic polymer tackifier 80a51 for a drilling fluid were prepared, respectively, and a shale rolling dispersion experiment was performed on a shale sample of a deep complex formation, and the results are shown in table 4.
TABLE 4 inhibition of shale hydration dispersion test results
| Name (R) | Percent recovery% |
| Tap water | 47.3 |
| 0.5% of example 2 sample | 81.7 |
| 0.5％Driscal D | 70.1 |
| 0.5％KPAM | 56.8 |
| 0.5％80A51 | 66.0 |
Test example 4: testing in fresh water-based slurries
And (3) preparing base slurry, namely adding 400m L of tap water into a high-stirring cup, sequentially adding 0.8g of anhydrous sodium carbonate and 16g of second-grade bentonite for the drilling fluid at the stirring speed of 8000 rpm, stirring for 2 hours, and sealing and standing for 24 hours to obtain the pre-hydrated fresh water base slurry.
Preparation and testing of test slurries: separately, 0.3% of an evaluation sample (sample of example 2, Driscal D) was added to the pre-hydrated fresh water-based slurry, stirred at a high speed of 8000 rpm, and the apparent viscosities of the respective test slurries at different temperatures were measured using a Brookfield DV-2 rheometer; the test slurries were loaded into a high temperature aging tank, heat roll aged at 180 ℃ for 16 hours, and each test slurry was tested for fluid loss at 20 ℃ with the results shown in table 5.
Table 5 test results in fresh water based slurries
Test example 5: testing in a brine-based slurry
And (3) preparing the saline base slurry, namely adding 400m L of tap water into a high-stirring cup, sequentially adding 0.8g of anhydrous sodium carbonate and 16g of second-grade bentonite for the drilling fluid at the stirring speed of 8000 rpm, stirring for 2 hours, hermetically standing for 24 hours, adding 4% NaCl, and stirring for 20 minutes to obtain the saline base slurry.
Preparation and testing of test slurries: 1.5% of each evaluation sample (sample of example 2, Driscal D) was added to the saline-based slurry, and the slurry was stirred at a high speed at 8000 rpm to obtain a homogeneous mixture, and the rheology and fluid loss of each test slurry were measured. The test slurries were charged into a high temperature aging tank, heat roll aged at 180 ℃ for 16 hours, and the rheology and fluid loss of each test slurry were measured in the same manner, with the results shown in Table 6.
Table 6 test results in brine-based slurries
Test example 6: testing in saturated brine-based slurries
The saturated brine-based slurry was prepared as described in comparative example 1.
Preparation and testing of test slurries: each of the test slurries was measured for rheology and fluid loss by adding 1.5% of the evaluation sample (sample of example 2, DriscalD) to a saturated saline base slurry, stirring at high speed at 8000 rpm, and stirring uniformly. The test slurries were charged into a high temperature aging tank, heat roll aged at 180 ℃ for 16 hours, and the rheology and fluid loss of each test slurry were measured in the same manner, with the results shown in Table 7.
Table 7 test results in saturated brine-based slurries
Test example 7: testing in ultra high temperature water-based drilling fluid completion fluids
The preparation of the completion fluid base slurry of the ultra-high temperature water-based drilling fluid comprises the steps of measuring 400m L fresh water base slurry, stirring the fresh water base slurry for 20 minutes at a high speed in a high-speed stirrer with 8000 rpm, then sequentially adding 0.3-0.5 part of sodium hydroxide, 0.3-1 part of amphoteric ion hydrophobic association polymer filtrate reducer resisting ultra-high temperature complex salt, 3-5 parts of sulfomethyl phenolic resin II type, 3-5 parts of sulfonated lignite resin, 2-4 parts of sulfonated asphalt powder, 1-2 parts of modified graphite, 1-2 parts of polyalcohol, 3-5 parts of high temperature resistant plugging agent and 20-50 g of barite, stirring the mixture for 20 minutes at a high speed after adding each treating agent, and preparing the completion fluid base slurry of the ultra-high temperature water-based drilling fluid, wherein the density of the completion fluid base slurry of the ultra-high temperature water-based drilling fluid is 1.10-1.30g/cm3。
The testing method comprises the steps of taking 400m L of the base slurry of the ultrahigh-temperature water-based drilling fluid completion fluid, uniformly stirring at a high speed of 8000 rpm, adding 0.5-1 part of the sample of example 2, stirring at a high speed for 20 minutes to obtain a system of the ultrahigh-temperature water-based drilling fluid completion fluid, testing the rheological property and the filtration loss of the test slurry, loading the test slurry into a high-temperature aging tank, carrying out hot-roll aging in a high-temperature roller furnace at 248 ℃ for 16 hours, and testing the rheological property and the filtration loss of the test slurry by the same method, wherein the results are shown in Table 8.
TABLE 8 test results in ultra high temperature water-based drilling fluid completion fluids
Note: the formula 1 is an ultrahigh-temperature water-based drilling fluid completion fluid system added with the sample of the embodiment, the formula 2 is ultrahigh-temperature water-based drilling fluid completion fluid base slurry not added with the sample of the embodiment, and the HTHP fluid loss test condition is 180 ℃/3.5 MPa.
Test example 8: testing in ultra-high temperature ultra-high density water-based drilling fluid completion fluids
And (3) preparing the low solid phase fresh water base slurry, namely adding 400m L tap water into a high stirring cup, sequentially adding 0.3-0.5g of anhydrous sodium carbonate and 6-10g of second-stage bentonite for the drilling fluid at the stirring speed of 8000 rpm, stirring for 2 hours, and sealing and standing for 24 hours to obtain the pre-hydrated low solid phase fresh water base slurry.
The preparation method of the completion fluid base slurry of the ultrahigh-temperature and ultrahigh-density water-based drilling fluid comprises the steps of measuring 400m L low-solid-phase fresh water base slurry, stirring the low-solid-phase fresh water base slurry for 20 minutes on a high-speed stirrer at 8000 rpm, then sequentially adding 0.1 to 0.5 part of an ultrahigh-temperature resistant complex salt resistant zwitterionic hydrophobic association polymer filtrate reducer, 2 to 4 parts of sulfomethyl phenolic resin type I, 3 to 8 parts of sulfonated lignite resin, 2 to 9 parts of sulfonated asphalt powder, 3 to 7 parts of potassium chloride and 900-3。
The testing method comprises the steps of taking 400m L of the base slurry of the ultrahigh-temperature ultrahigh-density water-based drilling fluid completion fluid, uniformly stirring at a high speed of 8000 rpm, adding 0.1-0.3 part of the sample of example 2, stirring at a high speed for 30 minutes to obtain the ultrahigh-temperature ultrahigh-density water-based drilling fluid completion fluid system, testing the rheological property and the filtration loss of the test slurry, loading the test slurry into a high-temperature aging tank, carrying out hot-roll aging in a high-temperature roller furnace at 240 ℃ for 16 hours, and testing the rheological property and the filtration loss of the test slurry by the same method, wherein the results are shown in Table 9.
TABLE 9 test results in ultra high temperature ultra high density water-based drilling fluid completion fluids
Note: the formula 1 is an ultrahigh-temperature and ultrahigh-density water-based drilling fluid completion fluid system added with the sample in the example 2, the formula 2 is ultrahigh-temperature and ultrahigh-density water-based drilling fluid completion fluid base slurry without the sample in the example 2, and the HTHP fluid loss test condition is 180 ℃/3.5 MPa.
And (4) analyzing results:
the test results of the test examples 1 to 2 show that the superhigh temperature resistant anionic polymer fluid loss additive is prepared by the polymerization reaction of three alkenyl monomers, namely acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and an alkenyl monomer, namely dimethylaminoethyl methacrylate, and has the weight average molecular weight of about 73 ten thousand and the number average molecular weight of about 64 ten thousand.
The test result of the test example 3 shows that the superhigh temperature resistant anionic polymer fluid loss additive has good performance of inhibiting hydration and dispersion of shale.
The test results of the test examples 4 to 6 show that the tackifying performance of the superhigh temperature resistant anionic polymer fluid loss additive in the drilling fluid completion fluid is slightly less than that of a comparative product Driscal D, and the superhigh temperature resistant anionic polymer fluid loss additive has good high temperature resistance and salt resistance in fresh water base slurry, salt water base slurry and saturated salt water base slurry.
Test results of test examples 7 to 8 show that the rheological property and the filtration loss property of the drilling fluid completion fluid are stable after the ultra-high temperature anionic polymer fluid loss additive is added into an ultra-high temperature water-based drilling fluid system and an ultra-high temperature ultra-high density water-based drilling fluid system, so that the temperature resistance of the drilling fluid completion fluid system can be improved to at least 248 ℃, meanwhile, the medium pressure filtration loss of the ultra-high temperature water-based drilling fluid completion fluid and the ultra-high temperature ultra-high density water-based drilling fluid completion fluid can be controlled within 5m L, and the high temperature and high pressure filtration loss is controlled within 20m L.
The test results of the comprehensive test examples 1 to 8 show that the superhigh temperature resistant anionic polymer fluid loss additive has good temperature resistance, the temperature resistance in a drilling fluid and completion fluid system reaches 248 ℃, and meanwhile, the superhigh temperature resistant anionic polymer fluid loss additive also has good salt resistance and fluid loss resistance.
Claims (12)
1. The ultra-high temperature resistant anionic polymer fluid loss additive for the drilling fluid and completion fluid is characterized in that the fluid loss additive is a terpolymer generated by the aqueous solution polymerization reaction of an alkenyl reaction monomer acrylamide, a strongly hydrophilic anionic alkenyl monomer 2-acrylamide-2-methyl-propanesulfonic acid and an alkenyl monomer dimethylaminoethyl methacrylate;
(iii) acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, and dimethylaminoethyl methacrylate at a molar ratio = 5.0: 3.75: 1.25; the molecular chain of the fluid loss agent contains 1,600-1,700 structural units, the weight average molecular weight is 690,000-740,000, and the number average molecular weight is 620,000-650,000.
2. The preparation method of the superhigh temperature resistant anionic polymer fluid loss additive for the drilling and completion fluid as described in claim 1, which comprises the following steps:
dissolving reactants of acrylamide, 2-acrylamide-2-methyl-propanesulfonic acid and dimethylaminoethyl methacrylate in a solvent, putting the mixture into a reaction kettle, adjusting the concentration of the mixed solution of the reactants by the solvent, adjusting the pH value by alkali, adding a catalyst, heating the mixed solution in the reaction kettle, maintaining the reaction time, terminating the reaction, drying, crushing and sieving to obtain the superhigh temperature resistant anionic polymer filtrate reducer.
3. The method of claim 2, wherein the solvent is water;
the catalyst is one or two of azodiisobutyamidine oxazoline hydrochloride, azodiisobutyamidine hydrochloride, azodicyano valeric acid or azodiisopropyl imidazoline;
the alkali is sodium hydroxide or potassium hydroxide.
4. The method according to claim 2, wherein the pH is adjusted to 5 to 9.
5. The method according to claim 2, wherein the pH is adjusted to 6.5 to 7.5.
6. The method of claim 2, wherein the total weight of the reactant monomers is 8-20wt% of the total weight of the solution of the reactants and the solvent.
7. The method of claim 2, wherein the total weight of the reactant monomers is 12-16wt% of the total weight of the solution of the reactants and the solvent.
8. The method of claim 2, wherein the weight of the catalyst is 0.05 to 0.5wt% based on the total weight of the reactants.
9. The method of claim 2, wherein the weight of the catalyst is 0.15-0.30wt% based on the total weight of the reactants.
10. The method according to claim 2, wherein the reaction temperature is 35 to 80 ℃ and the reaction time is 2 to 8 hours.
11. The method according to claim 2, wherein the reaction temperature is 40 to 60 ℃ and the reaction time is 3.5 to 4.5 hours.
12. The method as claimed in claim 2, wherein the drying temperature is 105-135 ℃;
after crushing and sieving, the granularity of the fine granular product is 10-40 meshes; the particle size of the fine particle product is 0.9mm, and the balance of the sieve is less than 15%; the dry content of the fine-particle product is > 90%.
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