CN115947903B - High-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer and preparation method and application thereof - Google Patents
High-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer and preparation method and application thereof Download PDFInfo
- Publication number
- CN115947903B CN115947903B CN202211502848.5A CN202211502848A CN115947903B CN 115947903 B CN115947903 B CN 115947903B CN 202211502848 A CN202211502848 A CN 202211502848A CN 115947903 B CN115947903 B CN 115947903B
- Authority
- CN
- China
- Prior art keywords
- resistant
- temperature
- salt
- hyperbranched
- filtrate reducer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention provides a high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer, and a preparation method and application thereof. The hyperbranched organosilicon filtrate reducer is prepared by the free radical polymerization reaction of aqueous solution of hyperbranched organosilicon cross-linking agent, N-dimethylacrylamide, acrylic acid, sodium styrenesulfonate and diallyl dimethyl ammonium chloride monomer. The hyperbranched organosilicon cross-linking agent endows the polymer with a highly hyperbranched structure, so that the polymer has lower viscosity and temperature and salt resistance; the carboxyl group in the acrylic acid has stronger hydration capability, so that the filtrate reducer has excellent gel protecting capability; the introduction of the sulfonic acid anion monomer enhances the temperature resistance and salt hydration resistance of the polymer; the introduction of rigid cationic monomers significantly reduces fluid loss. The filtrate reducer prepared by the invention has excellent filtrate reducing performance after aging in a high-temperature (220 ℃) high-salt (saturated salt) environment.
Description
Technical Field
The invention belongs to the technical field of petroleum and natural gas, and particularly relates to a high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer, and a preparation method and application thereof.
Background
With the increasing consumption of global oil and gas resources and the gradual exhaustion of conventional middle-shallow oil and gas resources, the global oil and gas exploration and development gradually turns to deep and ultra-deep layers. The deep drilling process has complex formation, high bottom temperature, partial well temperature over 200 ℃, and large salt paste layer, and provides great challenges for the safety, economy and the like of the drilling process. The drilling fluid is called as drilling 'blood', and is a key factor for guaranteeing drilling safety, improving mechanical drilling speed and protecting an oil and gas reservoir. Oil-based drilling fluids offer advantages over water-based drilling fluids in terms of inhibition, high temperature resistance, salt and calcium resistance, lubrication, etc., but are limited in field applications due to their high cost and severe environmental pollution. The conventional water-based drilling fluid key treating agent is degraded or flocculated in a high-temperature and high-salt environment, so that a series of performances such as drilling fluid rheological property, fluid loss property, sedimentation stability and the like are deteriorated, and further the problems of differential pressure drilling sticking, drilling rate reduction, well wall instability, lost circulation, reservoir damage and the like are caused, and the safe and efficient exploration and development of deep and ultra-deep oil and gas resources are seriously restricted.
The filtrate reducer is one of core treatment agents consisting of water-based drilling fluid, and can reduce the filtrate loss of the drilling fluid in drilling operation by three modes of pore blocking, viscosity increasing and adhesive protecting adsorption. Currently, most filtrate reducers are artificially modified natural polymers or artificially synthesized high molecular polymers. The modified products such as cellulose, starch, humic acid, lignin and the like belong to modified natural polymer filtrate reducers and are widely applied to middle and shallow wells, but the natural polymers are limited to be applied to deep wells and ultra-deep wells due to poor temperature resistance. The synthetic polymer comprises nonionic polymer, anionic polymer and amphoteric polymer, and has excellent temperature resistance and salt resistance due to the advantages of multiple monomer types, adjustable composition and structure and the like. However, the current high temperature resistant (> 220 ℃) and high salt resistant (saturated) water-based slurry filtrate reducer is still a great technical problem, and needs to be solved.
In recent years, silicone polymer fluid loss additives have received attention for their excellent temperature resistance properties. For example, chinese patent document CN113896830a discloses a preparation method of a high temperature resistant filtrate reducer, and the introduced vinyltrimethoxysilane can avoid the defect that the amide group of the main chain of the filtrate reducer is easy to decompose at high temperature, so that the temperature resistance of the filtrate reducer can reach 220 ℃, but the salt resistance is not studied. Chinese patent document CN102174314A discloses an organosilicon filtrate reducer and a preparation method thereof, wherein gamma- (acrylamide) propyl triethoxysilane is used as a modifier to synthesize the organosilicon filtrate reducer, the temperature resistance of the filtrate reducer can reach 200 ℃, the two filtrate reducers are obtained by directly adding silane coupling agent monomers into aqueous phase reaction liquid and forming crosslinking through dehydration condensation reaction of the silane coupling agent, but the silane coupling agent monomers participate in less copolymerization of ethylene monomers, so that the crosslinking degree of polymers is low. Chinese patent document CN114773539A discloses a high temperature resistant high salt resistant micro-crosslinking hydrophobic association tackifying filtrate reducer for water-based drilling fluid, which is resistant to temperature up to 200 ℃ and 30% NaCl, wherein the filtrate reducer relates to a hyperbranched polysiloxane crosslinking agent which is prepared by hydrolysis polycondensation reaction of gamma-methacryloxypropyl trimethoxy silane and dimethoxy (methyl) phenylsilane in ethanol aqueous solution, but the molecular weight of the hyperbranched organosilicon crosslinking agent is lower, so that the hyperbranched crosslinking degree of a polymer is low, and the temperature resistance and salt resistance are required to be improved.
Therefore, the development of a high-temperature (more than or equal to 220 ℃) resistant high-salt (saturated salt) resistant filtrate reducer for water-based drilling fluid with high crosslinking degree and without affecting the polymer dissolution performance is a requirement of the current high-temperature resistant drilling fluid technology development.
Disclosure of Invention
Aiming at the defects of the prior art, in particular to the technical problem that the existing filtrate reducer for water-based drilling fluid is easy to degrade and flocculate in a high-temperature and high-salt environment, the invention provides a high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer, and a preparation method and application thereof. The hyperbranched organosilicon fluid loss agent can resist high temperature (220 ℃) and high salt (saturated salt) and can effectively realize the fluid loss reducing effect.
The technical scheme of the invention is as follows:
the preparation method of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer comprises the following steps:
(1) Preparation of hyperbranched organosilicon crosslinker
Mixing gamma-methacryloxypropyl trimethoxysilane (KH 570) and 1, 4-Butanediol (BDO) to obtain a mixed solution; heating the mixed solution to a reaction temperature under a nitrogen atmosphere, and maintaining the temperature until distillation of the fraction is started; continuing the reaction until no fraction flows out, and finishing the reaction; dialyzing and removing the solvent to obtain the hyperbranched organosilicon cross-linking agent;
(2) Preparation of high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate loss reducer
Adding N, N-Dimethylacrylamide (DMAA), acrylic Acid (AA), anionic monomers and cationic monomers into water, and uniformly stirring the hyperbranched organosilicon crosslinking agent prepared in the step (1) and the surfactant to obtain a monomer solution; regulating the pH of the monomer solution, introducing nitrogen to remove oxygen, heating to the reaction temperature, adding an initiator, and thermally initiating free radical polymerization reaction; and after the reaction is finished, drying and crushing the obtained product to obtain the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer.
According to the invention, the molar ratio of gamma-methacryloxypropyl trimethoxysilane (KH 570) to 1, 4-Butanediol (BDO) in step (1) is preferably 1-1.5:1, more preferably 1-1.2:1.
According to the invention, the reaction temperature in step (1) is preferably from 100 to 180℃and more preferably from 120 to 160 ℃.
According to a preferred embodiment of the present invention, the dialysis step in step (1) is: dissolving the product obtained after the reaction is completed in absolute ethyl alcohol, then filling the absolute ethyl alcohol into a dialysis bag, dialyzing the absolute ethyl alcohol for 20 to 30 hours, and removing unreacted small molecules and hyperbranched cross-linking agents with lower molecular weight; the molecular weight cut-off of the dialysis bag is 2000Da.
According to a preferred embodiment of the invention, the mass ratio of N, N-Dimethylacrylamide (DMAA) to Acrylic Acid (AA) in step (2) is 1-2:1.
Preferably according to the invention, the anionic monomer in step (2) is one or more of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), sodium Styrene Sulfonate (SSS), sodium Vinyl Sulfonate (VS); the mass ratio of the anionic monomer to N, N-Dimethylacrylamide (DMAA) is 0.25-1:1.
Preferably according to the invention, the cationic monomer in step (2) is one or more of diallyldimethyl ammonium chloride (DMDAAC), methacryloxyethyl trimethyl ammonium chloride (DMC), acryloxyethyl trimethyl ammonium chloride (DAC); the mass ratio of the cationic monomer to N, N-Dimethylacrylamide (DMAA) is 0.25-1:1.
According to a preferred embodiment of the invention, the mass ratio of hyperbranched silicone crosslinker to N, N-Dimethylacrylamide (DMAA) in step (2) is from 0.05 to 0.07:1.
According to the invention, preferably, the surfactant in the step (2) is one or more of Sodium Dodecyl Sulfate (SDS), sodium Dodecyl Benzene Sulfonate (SDBS) and dodecylphenol polyoxyethylene ether (OP-10); the mass ratio of the surfactant to N, N-Dimethylacrylamide (DMAA) is 0.005-0.02:1.
According to the invention, the total mass fraction of monomers in the monomer solution in step (2) is preferably from 10 to 30%; the total mass of the monomers refers to the sum of the mass of N, N-Dimethylacrylamide (DMAA), acrylic Acid (AA), anionic monomers and cationic monomers.
According to the invention, in the step (2), the pH of the system is regulated to 5-9 by using an alkali solution, wherein the alkali solution is a sodium hydroxide aqueous solution with the mass fraction of 20-40%.
Preferably, according to the invention, in the step (2), the initiator is one or more of potassium persulfate (KPS), ammonium Persulfate (APS), azodiisobutyronitrile (AIBN) and azodiisobutylamidine hydrochloride (V50); the ratio of the mass of the initiator to the total mass of N, N-Dimethylacrylamide (DMAA), acrylic Acid (AA), anionic monomer and cationic monomer is 0.01-0.05:1, and more preferably 0.02-0.03:1.
According to the invention, the reaction temperature in step (2) is preferably 30-80 ℃, more preferably 50-70 ℃; the polymerization time is 2 to 6 hours, more preferably 3 to 5 hours.
The high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer is prepared by adopting the preparation method.
According to the invention, the application of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer in water-based drilling fluid; preferably, the concentration of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer in the water-based drilling fluid is 5-10g/L.
The invention has the technical characteristics and beneficial effects that:
1. compared with the hydrolysis condensation reaction of directly adding the silane coupling agent into the reaction liquid, the hyperbranched organosilicon cross-linking agent has larger molecular weight and more reactive sites, has higher polymerization reaction efficiency with ethylene monomers and less consumption.
2. The organosilicon cross-linking agent capable of forming the highly branched structure is introduced into the filtrate reducer, so that the organosilicon cross-linking limits the movement of a polymer chain segment in a high-temperature environment, and the high-temperature resistance of the filtrate reducer is enhanced; the highly branched structure endows the polymer molecular chain with excellent anti-agglomeration performance, and enhances the salt tolerance of the polymer; compared with the traditional linear polymer, the hyperbranched polymer has smaller viscosity increasing effect, is more beneficial to the construction of a low-viscosity drilling fluid system, and further improves the mechanical drilling rate.
3. The anionic strong hydration group introduced into the filtrate reducer enhances the hydration capacity of the polymer, endows the polymer with excellent gel protection capacity, and maintains the particle size distribution of bentonite particles; the introduced cationic monomer strengthens the adsorption of the polymer on the surfaces of bentonite particles and enhances the gel protecting capability of the polymer on bentonite.
4. The hyperbranched filtrate reducer synthesized by the invention has excellent temperature resistance and salt resistance, has excellent filtrate reduction capability after aging in a saturated salt environment at a high temperature of 220 ℃, and has wide application prospect in the field of high-temperature resistance and high-salt water-based drilling fluid.
Drawings
FIG. 1 is a schematic structural diagram of the hyperbranched silicone crosslinker prepared in example 1.
Detailed Description
The invention is further illustrated, but not limited, by the following examples.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents, materials, and apparatus, unless otherwise specified, are all commercially available.
The mass fraction of concentrated hydrochloric acid used in the examples was 37%.
Example 1
The preparation method of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer comprises the following steps:
(1) Preparation of hyperbranched organosilicon crosslinker
29.7g of gamma-methacryloxypropyl trimethoxysilane (KH 570) and 9g of 1, 4-Butanediol (BDO) are put into a four-necked flask and stirred uniformly to obtain a mixed solution; the four openings of the flask are respectively connected with a thermometer and N 2 The gas inlet, overhead stirrer and distillation apparatus were connected and the mixed solution was heated to 130 ℃ and maintained at that temperature until distillation of the distillate began; then the reaction is continued for 5 hours, and no fraction flows out; dissolving the obtained product in absolute ethanol, packaging into dialysis bag (cut-off 2000 Da), dialyzing in absolute ethanol for 24 hr to removeRemoving unreacted small molecules and hyperbranched cross-linking agent with lower molecular weight, and then removing solvent by spin evaporation at room temperature to obtain the hyperbranched organosilicon cross-linking agent with the number average molecular weight (Mn) of 3600.
(2) Preparation of high-temperature-resistant high-salt-resistant hyperbranched filtrate reducer
5g of N, N-Dimethylacrylamide (DMAA), 5g of Acrylic Acid (AA), 4g of Sodium Styrene Sulfonate (SSS), 2g of diallyl dimethyl ammonium chloride (DMDAAC), 0.25g of hyperbranched organosilicon cross-linking agent, and 0.05g of Sodium Dodecyl Sulfate (SDS) are dissolved in 60g of water, and after sufficient stirring, a monomer solution is obtained; regulating the pH value of the monomer solution to 7 by using a NaOH aqueous solution with the mass fraction of 20% to obtain a mixed reaction solution; and (3) stirring and deoxidizing the mixed reaction liquid in a nitrogen atmosphere for 30min, placing the mixed reaction liquid in a water bath kettle at 60 ℃, adding 0.32g of Ammonium Persulfate (APS) initiator, carrying out polymerization reaction at 60 ℃ for 4h, drying the product in a blowing oven at 80 ℃ for 24h after the reaction is finished, and crushing to obtain the high-temperature-resistant high-salt-resistant hyperbranched filtrate reducer.
Example 2
The preparation method of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer is as described in example 1, except that: the amount of Acrylic Acid (AA) monomer added in step (2) was 2.5g.
Example 3
The preparation method of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer is as described in example 1, except that: the Sodium Styrene Sulfonate (SSS) monomer in step (2) was added in an amount of 2g.
Example 4
The preparation method of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer is as described in example 1, except that: the amount of diallyldimethylammonium chloride (DMDAAC) monomer added in step (2) was 4g.
Example 5
The preparation method of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer is as described in example 1, except that: the pH of the monomer solution in step (2) was adjusted to 5.
Example 6
The preparation method of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer is as described in example 1, except that: the pH of the monomer solution in step (2) was adjusted to 9.
Example 7
The preparation method of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer is as described in example 1, except that: the reaction temperature of the mixture in step (2) was set to 50 ℃.
Example 8
The preparation method of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer is as described in example 1, except that: the reaction temperature of the mixture in the step (2) was set to 70 ℃.
Comparative example 1
A fluid loss additive was prepared as described in example 1, except that: the addition amount of the hyperbranched organosilicon cross-linking agent in the step (2) is 0.5g.
Comparative example 2
A fluid loss additive was prepared as described in example 1, except that: the addition amount of the hyperbranched organosilicon cross-linking agent in the step (2) is 0g.
Comparative example 3
A fluid loss additive was prepared as described in example 1, except that: the hyperbranched organosilicon cross-linking agent in the step (2) is added in an amount of 0g, and 0.25g of N, N-methylene bisacrylamide is additionally added.
Comparative example 4
A fluid loss additive was prepared as described in example 1, except that: the hyperbranched organosilicon cross-linking agent in the step (2) is added in an amount of 0g, and 0.25g of triallylamine is additionally added.
Comparative example 5
A fluid loss additive was prepared as described in example 1, except that: in step (2), 5g of Acrylic Acid (AA) was not added.
Comparative example 6
A fluid loss additive was prepared as described in example 1, except that: in step (2) 4g Sodium Styrene Sulfonate (SSS) was not added.
Comparative example 7
A fluid loss additive was prepared as described in example 1, except that: 2g of diallyldimethylammonium chloride (DMDAAC) was not added in step (2).
Comparative example 8
A fluid loss additive was prepared as described in example 1, except that: the hyperbranched organosilicon cross-linking agent in the step (1) is prepared according to the preparation example 1 of the Chinese patent document CN 114773539A.
Comparative example 9
A fluid loss additive was prepared as described in example 1, except that: in the preparation process of the hyperbranched organosilicon cross-linking agent in the step (1), gamma-methacryloxypropyl trimethoxysilane (KH 570) is replaced by vinyl trimethoxysilane (A171).
Comparative example 10
A fluid loss additive was prepared as described in example 1, step (2), except that: gamma-methacryloxypropyl trimethoxysilane (KH 570) was used instead of hyperbranched silicone crosslinker.
Test examples
Rheological and fluid loss performance evaluation was performed on the fluid loss additives prepared in examples and comparative examples:
(1) Preparation of 4% bentonite-based slurry: adding 16g of bentonite and 0.56g of anhydrous sodium carbonate into 400mL of water, stirring for 20 minutes at a rotating speed of 8000r/min, sealing, standing and hydrating for 24 hours at room temperature;
(2) Drilling fluid sample configuration: taking 400mL of 4% bentonite slurry, respectively adding 8g (2%) of the filtrate reducer prepared in the examples and the comparative examples, and stirring for 20min at 8000 r/min;
(3) Sample configuration of saturated brine drilling fluid: taking 400mL of 4% bentonite slurry, respectively adding 8g (2%) of the filtrate reducer prepared in the examples and the comparative examples, and stirring for 20min at 8000 r/min; subsequently, 144g (36%) of sodium chloride were added and stirred at 8000r/min for 20min;
(4) Aging treatment of drilling fluid samples: and placing the drilling fluid sample into a roller heating furnace, and setting the aging temperature to 220 ℃ and the aging time to 16 hours.
(5) Apparent viscosity of formulated drilling fluids was tested against the American Petroleum Institute (API) standard (API RP 13B-1,2009)(AV), plastic Viscosity (PV), dynamic shear force (YP) and normal temperature and pressure Fluid Loss (FL) API )。
Results of Performance test
TABLE 1 rheological properties and fluid loss data sheets for drilling fluids obtained by adding the fluid loss additives prepared in the examples
As can be seen from the test results in Table 1, compared with the base slurry, the high temperature and high salt resistant hyperbranched filtrate reducer prepared in examples 1-8 is added, the Apparent Viscosity (AV), the Plastic Viscosity (PV) and the dynamic shear force (YP) of drilling fluid are all obviously improved, and the hyperbranched filtrate reducer still has excellent filtrate reducing performance after being aged at 220 ℃ for 16 hours, thus indicating that the hyperbranched filtrate reducer has excellent high temperature resistant performance. The dosage of key monomers is reduced in the examples 2 and 3, the hydration groups in the filtrate reducer are reduced, and the effect of the filtrate reducer is slightly reduced. In example 4, the amount of cationic monomer is increased, and the excessive amount of macrocyclic cationic monomer can prevent the polymerization reaction from proceeding and reduce the polymerization degree, so that the filtration performance of the product is slightly reduced. Examples 5 and 6 are pH-adjusted reaction solutions, and in acidic and alkaline environments, respectively, it can be seen that the hyperbranched filtrate reducer prepared in a neutral environment has optimal performance. Examples 7 and 8 are, respectively, lowering and increasing the reaction temperature, too low a reaction temperature would decrease the reactivity of the polymerized monomer, too high a reaction temperature would exacerbate the explosive polymerization of the reactive monomer, and 60 ℃ would be seen to be the optimum temperature for the fluid loss additive synthesis.
Table 2 rheological properties and fluid loss properties data table for drilling fluids obtained by adding the fluid loss additive prepared in comparative example
From table 2 it can be seen that: in the comparative example 1, the consumption of the hyperbranched organosilicon cross-linking agent is increased, and excessive consumption of the cross-linking agent can reduce the regularity of a polymer grid structure, so that the filtrate loss reducing performance of the filtrate loss reducer is weakened; in comparative example 2, no hyperbranched organosilicon cross-linking agent is added, the linear polymer has larger molecular weight, poor stability in high-temperature environment and poor protection on the colloid stability of bentonite in high-temperature environment; comparative examples 3 and 4 are N, N-methylenebisacrylamide with two functional groups and triallylamine with three functional groups, and compared with a hyperbranched organosilicon cross-linking agent with multiple functional groups, hyperbranched polymers cannot be formed, and the high-temperature stability is poor, so that the filtration reducing effect is poor; comparative example 5 has less hydrated groups in the polymer and greater fluid loss due to the absence of AA monomer; comparative example 6 has poor temperature resistance and insufficient hydration capacity because it does not contain an anionic monomer, and thus the fluid loss is increased; comparative example 7, which does not contain cationic monomer, cannot form strong interaction with bentonite after the filtrate reducer is added, has weak gel protection capability, and results in maximum filtrate loss; the organosilicon cross-linking agent used in comparative example 8 has small molecular weight and low hyperbranched degree of the filtrate reducer, and reduces the temperature resistance thereof; comparative example 9 preparation of hyperbranched crosslinker using vinyltrimethoxysilane (a 171), the high temperature resistance and fluid loss performance of the fluid loss additive was reduced compared to crosslinker prepared with gamma-methacryloxypropyl trimethoxysilane (KH 570); comparative example 10 gamma-methacryloxypropyl trimethoxysilane (KH 570) was used instead of hyperbranched silicone crosslinker, the crosslink density was reduced and the fluid loss performance was reduced.
TABLE 3 rheological properties and fluid loss data sheets for saturated salt drilling fluids obtained by adding the fluid loss additives prepared in the examples
As can be seen from the test results of table 3, when salt intrudes into the drilling fluid, positively charged sodium ions enter between bentonite, and the electrostatic repulsive force between bentonite is broken, so that dispersibility of bentonite is deteriorated, particles are aggregated, particle size becomes large, thin and dense mud cake cannot be formed, and thus fluid loss is drastically increased. After the filtrate reducer prepared in the examples 1-8 is added into the base slurry, the filtrate reducer of the drilling fluid sample can still maintain even after aging in a saturated salt environment at a high temperature of 220 ℃, so that the filtrate reducer prepared in the examples has excellent high-temperature and high-salt resistance, and further the filtrate loss is reduced. Wherein, the drilling fluid sample added with the filtrate reducer of the example 1 has minimum filtrate loss, the pressure filtration loss is 7mL at normal temperature before aging, and the pressure filtration loss is 12mL at normal temperature after aging, thus the filtrate reducer has excellent filtrate loss performance.
Table 4 rheological properties and fluid loss properties data table for drilling fluids obtained by adding the fluid loss additive prepared in comparative example
As can be seen from table 4: in the comparative example 1, the dosage of the hyperbranched organosilicon cross-linking agent is increased, and excessive dosage of the cross-linking agent can weaken the regularity of a polymer grid structure, weaken the temperature resistance and salt resistance, and further weaken the fluid loss reducing capacity of the fluid loss agent; in comparative example 2, hyperbranched organosilicon cross-linking agent is not added, the linear polymer has larger molecular weight, the polymer chain is easy to curl and degrade in a high-temperature and high-salt environment, the protective capability of bentonite is lost, and the filtration loss is increased; comparative examples 3 and 4 are N, N-methylenebisacrylamide with two functional groups and triallylamine with three functional groups, and compared with a hyperbranched organosilicon cross-linking agent with multiple functional groups, hyperbranched polymers cannot be formed, and the high-temperature stability and the salt tolerance are poor, so that the filtration reducing effect is poor; comparative example 5 has less hydrated groups in the polymer and greater fluid loss due to the absence of AA monomer; comparative example 6 has poor temperature resistance and salt resistance, and poor filtrate reduction performance because of no anionic monomer; comparative example 7 has poor temperature resistance of the fluid loss additive because of no cationic monomer, and the polymer has insufficient adsorption groups, so that the gel protection capability in a saline water environment is weakened, and the fluid loss is increased; comparative example 8 preparation of organosilicon crosslinker, the obtained crosslinker has small molecular weight, low hyperbranched degree of filtrate reducer, reduced anti-curling capability in saline environment, and reduced filtrate reducer performance in saline environment; comparative example 9 preparation of hyperbranched crosslinker using vinyltrimethoxysilane (a 171), the filtrate reducer had reduced filtrate reduction performance in high temperature, high salt environment compared to crosslinker prepared from γ -methacryloxypropyl trimethoxysilane (KH 570); comparative example 10 uses gamma-methacryloxypropyl trimethoxysilane (KH 570) instead of hyperbranched silicone crosslinker, the crosslink density is reduced, the hyperbranched conformation is absent, the temperature resistance and salt tolerance of the filtrate reducer are reduced, and the filtrate reducer has reduced filtrate reducer failure.
In conclusion, the high-temperature-resistant high-salt-resistant hyperbranched filtrate reducer has the remarkable advantages that: firstly, the addition of the hyperbranched organosilicon cross-linking agent can effectively improve the temperature resistance and the salt hydrolysis resistance of the polymer, and has lower tackifying effect compared with the conventional linear polymer; secondly, the addition of the acrylic acid and the anionic monomer can lead the polymer to contain a large amount of anti-salt hydration groups, thereby being beneficial to protecting the dispersibility of bentonite and further forming compact mud cakes; finally, the addition of the cationic monomer can enhance the adsorption of the polymer on the surfaces of the bentonite particles, and further enhance the gel protecting capability of the polymer. The hyperbranched fluid loss additive prepared by the invention has excellent fluid loss performance after aging in a high-temperature (220 ℃) high-salt (saturated salt) environment, and can enrich the development of the high-temperature-resistant saturated salt water-based drilling fluid technology.
Claims (9)
1. The preparation method of the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer comprises the following steps:
(1) Preparation of hyperbranched organosilicon crosslinker
Mixing gamma-methacryloxypropyl trimethoxysilane and 1, 4-butanediol to obtain a mixed solution; heating the mixed solution to a reaction temperature under a nitrogen atmosphere, and maintaining the temperature until distillation of the fraction is started; continuing the reaction until no fraction flows out, and finishing the reaction; dialyzing and removing the solvent to obtain the hyperbranched organosilicon cross-linking agent; the molar ratio of the gamma-methacryloxypropyl trimethoxy silane to the 1, 4-butanediol is 1-1.5:1; the reaction temperature is 100-180 ℃;
(2) Preparation of high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate loss reducer
Adding N, N-dimethylacrylamide, acrylic acid, an anionic monomer and a cationic monomer into water, and uniformly stirring the hyperbranched organosilicon crosslinking agent and the surfactant prepared in the step (1) to obtain a monomer solution; regulating the pH of the monomer solution, introducing nitrogen to remove oxygen, heating to the reaction temperature, adding an initiator, and thermally initiating free radical polymerization reaction; after the reaction is finished, the obtained product is dried and crushed to obtain the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer;
the mass ratio of the N, N-dimethylacrylamide to the acrylic acid is 1-2:1;
the anionic monomer is one or more of 2-acrylamide-2-methylpropanesulfonic acid, sodium styrene sulfonate and sodium vinyl sulfonate; the mass ratio of the anionic monomer to the N, N-dimethylacrylamide is 0.25-1:1;
the cationic monomer is one or more of diallyl dimethyl ammonium chloride, methacryloxyethyl trimethyl ammonium chloride and acryloxyethyl trimethyl ammonium chloride; the mass ratio of the cationic monomer to the N, N-dimethylacrylamide is 0.25-1:1;
the mass ratio of the hyperbranched organosilicon cross-linking agent to the N, N-dimethylacrylamide is 0.05-0.07:1;
the reaction temperature is 30-80 ℃.
2. The method for preparing the high temperature resistant and high salt resistant hyperbranched organosilicon fluid loss additive according to claim 1, wherein the molar ratio of the gamma-methacryloxypropyl trimethoxysilane to the 1, 4-butanediol in the step (1) is 1-1.2:1.
3. The method for preparing the high temperature resistant and high salt resistant hyperbranched organosilicon filtrate reducer, according to claim 1, wherein the reaction temperature in the step (1) is 120-160 ℃;
the reaction dialysis steps are as follows: dissolving the product obtained after the reaction in absolute ethyl alcohol, then filling the absolute ethyl alcohol into a dialysis bag, and dialyzing the absolute ethyl alcohol for 20-30h; the molecular weight cut-off of the dialysis bag is 2000Da.
4. The method for preparing the high-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer, which is characterized in that the surfactant in the step (2) is one or a combination of more than two of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and dodecylphenol polyoxyethylene ether; the mass ratio of the surfactant to the N, N-dimethylacrylamide is 0.005-0.02:1; the total mass fraction of the monomers in the monomer solution is 10-30%.
5. The preparation method of the high temperature resistant high salt resistant hyperbranched organosilicon filtrate reducer, as claimed in claim 1, is characterized in that in the step (2), an alkali solution is used for adjusting the pH of the system to 5-9, and the alkali solution is a sodium hydroxide aqueous solution with the mass fraction of 20-40%.
6. The preparation method of the high temperature resistant and high salt resistant hyperbranched organosilicon filtrate reducer, as claimed in claim 1, characterized in that the initiator in the step (2) is one or more of potassium persulfate, ammonium persulfate, azobisisobutyronitrile and azobisisobutyronitrile hydrochloride; the ratio of the mass of the initiator to the total mass of N, N-dimethylacrylamide, acrylic acid, anionic monomers and cationic monomers is 0.01-0.05:1;
the reaction temperature is 50-70 ℃; the polymerization reaction time is 2-6h.
7. The method for preparing the high temperature resistant and high salt resistant hyperbranched organosilicon filtrate reducer, according to claim 1, wherein the ratio of the mass of the initiator to the total mass of N, N-dimethylacrylamide, acrylic acid, anionic monomers and cationic monomers in the step (2) is 0.02-0.03:1;
the polymerization reaction time is 3-5h.
8. A high temperature resistant and high salt resistant hyperbranched organosilicon fluid loss additive, characterized in that the agent is prepared by the preparation method of any one of claims 1-7.
9. The application of the high temperature-resistant high-salt-resistant hyperbranched organosilicon fluid loss additive in water-based drilling fluid, which is characterized in that the concentration of the high temperature-resistant high-salt-resistant hyperbranched organosilicon fluid loss additive in the water-based drilling fluid is 5-10g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211502848.5A CN115947903B (en) | 2022-11-28 | 2022-11-28 | High-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211502848.5A CN115947903B (en) | 2022-11-28 | 2022-11-28 | High-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115947903A CN115947903A (en) | 2023-04-11 |
| CN115947903B true CN115947903B (en) | 2023-08-11 |
Family
ID=87288170
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211502848.5A Active CN115947903B (en) | 2022-11-28 | 2022-11-28 | High-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115947903B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102174314A (en) * | 2011-03-09 | 2011-09-07 | 西南石油大学 | Organic silicon fluid loss additive and preparation method thereof |
| CN105017475A (en) * | 2015-06-29 | 2015-11-04 | 山东得顺源石油科技有限公司 | Tackifying and filtrate reducing agent for low soil phase and high density drilling fluid, and preparation method thereof |
| CN107033280A (en) * | 2017-03-06 | 2017-08-11 | 山东诺尔生物科技有限公司 | Drilling fluid both sexes heat and salinity tolerance fluid loss additive and preparation method |
| CN108774507A (en) * | 2018-05-31 | 2018-11-09 | 钦州学院 | A kind of mixing fluid loss additive and preparation method thereof |
| CN112011318A (en) * | 2020-08-11 | 2020-12-01 | 中国石油大学(华东) | Salt response type high temperature resistant amphoteric ion polymer fluid loss agent and preparation method and application thereof |
| CN112457454A (en) * | 2020-12-01 | 2021-03-09 | 西南石油大学 | High-temperature-resistant organic/inorganic hybrid polymer filtrate reducer and preparation method thereof |
-
2022
- 2022-11-28 CN CN202211502848.5A patent/CN115947903B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102174314A (en) * | 2011-03-09 | 2011-09-07 | 西南石油大学 | Organic silicon fluid loss additive and preparation method thereof |
| CN105017475A (en) * | 2015-06-29 | 2015-11-04 | 山东得顺源石油科技有限公司 | Tackifying and filtrate reducing agent for low soil phase and high density drilling fluid, and preparation method thereof |
| CN107033280A (en) * | 2017-03-06 | 2017-08-11 | 山东诺尔生物科技有限公司 | Drilling fluid both sexes heat and salinity tolerance fluid loss additive and preparation method |
| CN108774507A (en) * | 2018-05-31 | 2018-11-09 | 钦州学院 | A kind of mixing fluid loss additive and preparation method thereof |
| CN112011318A (en) * | 2020-08-11 | 2020-12-01 | 中国石油大学(华东) | Salt response type high temperature resistant amphoteric ion polymer fluid loss agent and preparation method and application thereof |
| CN112457454A (en) * | 2020-12-01 | 2021-03-09 | 西南石油大学 | High-temperature-resistant organic/inorganic hybrid polymer filtrate reducer and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 抗温耐盐有机硅降滤失剂制备与性能研究;罗霄等;《化工新型材料》;第第45卷卷(第第8期期);138-143页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115947903A (en) | 2023-04-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111875758B (en) | Preparation method of environment-friendly ultra-high temperature resistant filtrate reducer for water-based drilling fluid | |
| CN106866881B (en) | hydrophobic association acrylamide polymer emulsion and preparation method thereof | |
| CN106867496B (en) | Online injection type oil displacement agent containing hydrophobically associating polymer emulsion and preparation method thereof | |
| WO2013138156A1 (en) | Synthesis and application of high pressure high temperature fluid loss additive and rheology stabilizer | |
| CN112898488B (en) | Polysaccharide modified salt-resistant resistance-reducing agent for shale gas fracturing fluid and preparation method thereof | |
| CN114989348B (en) | High-temperature-resistant salt-resistant organosilicon fluid loss additive and preparation method and application thereof | |
| CN115572347A (en) | High-temperature-resistant high-salt-resistant tackifying and shearing-improving agent for water-based drilling fluid and preparation method and application thereof | |
| CN114181682A (en) | High-temperature-resistant salt-resistant cross-linked polymer filtrate reducer and preparation method and application thereof | |
| CN115947903B (en) | High-temperature-resistant high-salt-resistant hyperbranched organosilicon filtrate reducer and preparation method and application thereof | |
| CN115975112A (en) | High-temperature-resistant organic silicon crosslinked starch fluid loss agent and preparation method and application thereof | |
| CN111592616A (en) | Preparation method of nanoscale hyperbranched hydrophobically associating polyacrylamide | |
| CN112126017B (en) | Acrylamide functional polymer, and preparation method and application thereof | |
| CN115181212B (en) | Temperature-resistant salt-resistant zwitter-ion filtrate reducer and preparation method thereof | |
| CN114874391B (en) | Multifunctional treating agent for sea natural gas hydrate drilling fluid and preparation method and application thereof | |
| CN113563510B (en) | Temperature-resistant salt-resistant comb polymer fluid loss additive for drilling mud bentonite | |
| CN115678518A (en) | Environment-friendly high-temperature-resistant saturated saline water high-density polymer drilling fluid system and preparation method and application thereof | |
| CN111925479B (en) | Modified polyacrylamide, preparation method thereof and polymer slurry | |
| CN116284570B (en) | High-temperature-resistant high-salt-resistant filtrate reducer for water-based drilling fluid and preparation method and application thereof | |
| CN115677925B (en) | Constant-rheological stabilizer, drilling fluid and preparation method thereof | |
| CN113943399A (en) | Self-aggregation self-suspension proppant and preparation method and application thereof | |
| CN117820565A (en) | High-temperature-resistant and composite-salt-resistant polymer filtrate reducer and preparation method thereof | |
| CN115785922B (en) | Super-large displacement well high-temperature water-based drilling fluid | |
| CN115785293B (en) | Environment-friendly high-temperature-resistant starch nanoparticle plugging agent for drilling fluid and preparation method and application thereof | |
| CN115677923B (en) | Pre-crosslinked gel particle plugging agent and preparation method and application thereof | |
| CN115960304B (en) | High-resistance Wen Jianji bionic wall fixing agent for water-based drilling fluid and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |