CN113912770B - Star polymer for drilling fluid, preparation method and application thereof - Google Patents
Star polymer for drilling fluid, preparation method and application thereof Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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Abstract
The invention provides a star polymer for drilling fluid, a preparation method and application thereof, wherein the polymer is prepared from acrylamide monomers, 2-acrylamide-2-methylpropanesulfonic acid and branching agent through emulsion polymerization reaction; the branching agent structure comprises a plurality of alkyl hydroxyl groups; the star polymer for the drilling fluid has a branched structure and a nano polymer microsphere morphology. The molecular chain of the star polymer adopts a more extended conformation due to the mutual repulsive interaction between arms, so that the bridge has strong filtration reducing capability and better temperature resisting effect than that of a linear polymer. Experimental results show that the apparent viscosity of the 1.0% solution of the star polymer filtrate reducer is less than or equal to 35.0 mPa.s at room temperature; when the product addition amount is 3.0%, the API of the composite brine slurry is less than 5.0mL after 165 ℃/16h aging, and the API is less than 30mL after 180 ℃/16h aging.
Description
Technical Field
The invention belongs to the technical field of preparation methods of synthetic water-soluble polymer materials for oil fields, and particularly relates to a star-shaped polymer for drilling fluid, a preparation method and application thereof.
Background
Drilling fluid is an important fluid in drilling engineering, and the performance of the drilling fluid is directly related to the quality of drilling. The drilling fluid mainly comprises base slurry and various treating agents, wherein the treating agents comprise filtrate loss reducer, pH regulator and the like. Along with the continuous deep exploration and development, the requirements of high-temperature deep wells and special complex wells on the treatment agent for drilling fluid are higher and higher, and particularly, the high-temperature deep wells of the northwest and southward blocks are higher and higher in requirements on the temperature resistance of the treatment agent.
At present, a synthetic polymer treating agent such as a polyacrylamide filtrate reducer for site use is basically a linear polymer, the molecular chain length is long, the chain is easy to break after shearing at high temperature, the viscosity is greatly reduced, and the high-temperature stability of drilling fluid is reduced.
Therefore, research on polymers with special structures, changing the molecular conformation of the treating agent, improving the comprehensive effects of the existing polymer filtrate reducer such as high temperature resistance and the like, and becoming a main development trend.
Disclosure of Invention
Aiming at the problems existing in the prior art, the application provides a star-shaped polymer for drilling fluid, a preparation method and application thereof, and the polymer provided by the invention can be used as a filtrate reducer with temperature resistance and other functions, has outstanding filtrate reduction effect and can be widely used for drilling fluid.
The invention provides a star polymer for drilling fluid, which is prepared from acrylamide monomers, 2-acrylamide-2-methylpropanesulfonic acid and branching agent through emulsion polymerization reaction;
the branching agent structure comprises a plurality of alkyl hydroxyl groups;
the star polymer for the drilling fluid has a branched structure and a nano polymer microsphere morphology.
Preferably, the branching agent is pentaerythritol.
Preferably, the apparent viscosity of the star polymer for drilling fluid 1.0% solution is less than or equal to 35.0 mPa.s at room temperature.
The invention provides a preparation method of star polymer for drilling fluid, which comprises the following steps:
s1, adding a water phase material into an oil phase material for emulsification to obtain a monomer emulsion; the aqueous phase material comprises acrylamide monomers, 2-acrylamide-2-methylpropanesulfonic acid and a branching agent; the branching agent structure comprises a plurality of alkyl hydroxyl groups;
s2, carrying out polymerization reaction on the monomer emulsion under the existence of an initiator to obtain the star polymer of the nano polymer microsphere.
Preferably, the aqueous phase material comprises 390 to 420 parts by mass of water, 147.50 to 172.50 parts by mass of 2-acrylamido-2-methylpropanesulfonic acid, 152.00 to 177.50 parts by mass of acrylamide monomer, 0.15 to 0.175 part by mass of branching agent and 2.00 to 3.50 parts by mass of hydrophilic emulsifier.
Preferably, the oil phase material comprises 208 to 224 parts by mass of base oil and 18.50 to 30.50 parts by mass of lipophilic emulsifier; the kinematic viscosity of the base oil at 40 ℃ is preferably 1.5mm 2 /s～3.0mm 2 /s。
Preferably, the hydrophilic emulsifier is selected from the tween series; the lipophilic emulsifier is selected from span series.
Preferably, the initiator is one or more of a cerium salt initiator and a persulfate initiator.
Preferably, the monomer emulsion is placed in a water bath with the temperature of 30-65 ℃, inert gas is preferably introduced, an initiator is added, and the polymerization reaction is carried out for 3-5 hours under low-speed stirring, so as to obtain the star polymer.
The invention also provides application of the star polymer for drilling fluid as the filtrate reducer in the drilling fluid.
Compared with the prior art, the invention provides the star polymer with the branched structure, which can be used as a filtrate reducer in drilling fluid, and is mainly prepared from acrylamide monomers, 2-acrylamide-2-methylpropanesulfonic acid and a branching agent containing a plurality of alkyl hydroxyl groups through emulsion polymerization, and is a nano polymer microsphere. In the invention, the molecular chain of the star polymer adopts a more extended conformation due to the mutual repulsive interaction between arms, has strong bridging and filtration reducing capability, and has better temperature resistance effect than that of a linear polymer. Experimental results show that the apparent viscosity of the 1.0% solution of the star polymer filtrate reducer is less than or equal to 35.0 mPa.s at room temperature; when the product addition amount is 3.0%, the API of the composite brine slurry is less than 5.0mL after 165 ℃/16h aging, and the API is less than 30mL after 180 ℃/16h aging (the linear polymer filtrate reducer with the same ratio of groups and group proportion, the filtrate reduction rate is more than 50%).
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other examples of modifications and alterations will be apparent to those skilled in the art based on the examples herein, and are intended to be within the scope of the invention.
The invention provides a star polymer for drilling fluid, which is prepared from acrylamide monomers, 2-acrylamide-2-methylpropanesulfonic acid and a branching agent through emulsion polymerization;
the branching agent structure comprises a plurality of alkyl hydroxyl groups;
the star polymer for the drilling fluid has a branched structure and a nano polymer microsphere morphology.
The polymer provided by the invention can be used as a filtrate reducer with the functions of temperature resistance, salt resistance and the like, is convenient to use, has low addition, has outstanding filtrate reduction effect, and can be widely used for drilling fluid.
The polymer provided by the invention is a star polymer prepared by emulsion polymerization of an acrylamide monomer, a 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) monomer and a branching agent containing a plurality of alkyl hydroxyl groups, and has a branched structure (also called as a star structure). Among them, the acrylamide monomer such as acrylamide and methacrylamide is preferably Acrylamide (AM).
The star-structured polymer has a three-dimensional structure, the molecular chains are in a more extended conformation due to the mutual repulsive interaction among arms, the group density in the molecular structure is increased, the performances of reducing filtration capacity, lifting cutting and the like in drilling fluid are improved, and the suspension stability of the drilling fluid can be greatly improved. Meanwhile, the star-shaped three-dimensional structure can increase the intermolecular steric hindrance effect, is beneficial to improving the temperature resistance and salt resistance of the drilling fluid, has better action effect than a linear polymer, and has certain advantages in improving the long-term stability, shearing dilutability and suspension stability of the drilling fluid at high temperature.
In addition, pentaerythritol is preferably used as a branching agent, so that the four-arm star-shaped polymer for drilling fluid can be obtained; the molecular structure of pentaerythritol contains four-CH which is easy to undergo oxidation-reduction reaction 2 OH groups are spatially four-oriented and symmetrical in structure, and are suitable for forming branched structures, so that the molecular conformation of the existing polymer is changed, and the comprehensive effect of the existing polymer is improved.
The embodiment of the invention can form polymer emulsion by adopting an inverse emulsion polymerization mode, wherein the star polymer is in the shape of nano polymer microspheres, which is beneficial to the stability of drilling fluid, the application simplicity and the like. In an embodiment of the invention, the apparent viscosity of the 1.0% solution of the star polymer for drilling fluid is less than or equal to 35.0 mPa.s at room temperature.
Correspondingly, the embodiment of the invention provides a preparation method of a star polymer for drilling fluid, which comprises the following steps:
s1, adding a water phase material into an oil phase material for emulsification to obtain a monomer emulsion; the aqueous phase material comprises acrylamide monomers, 2-acrylamide-2-methylpropanesulfonic acid and a branching agent; the branching agent structure comprises a plurality of alkyl hydroxyl groups;
s2, carrying out polymerization reaction on the monomer emulsion under the existence of an initiator to obtain the star polymer of the nano polymer microsphere.
The embodiment of the invention adopts an inverse emulsion polymerization mode to form the nano polymer microsphere treating agent, which is applied to drilling fluid, has outstanding filtration-reducing and failure effects, good temperature resistance and salt resistance and convenient use.
Inverse emulsion polymerization refers to a process in which water-soluble monomers are made into an aqueous solution, and reacted with an organic phase to form a water-in-oil emulsion under the action of an oil-soluble surfactant, and then polymerized by initiator initiation to form a water-in-oil (water/oil) polymer latex.
In the reaction kettle, pure water, acrylamide monomer, 2-acrylamide-2-methylpropanesulfonic acid and branching agent are firstly added, preferably hydrophilic emulsifier is added, and then the pH value of the system can be adjusted to be alkaline (for example, the pH value is 9-10) to obtain a water phase.
Specifically, the aqueous phase material comprises 390 to 420 parts by mass of water, 147.50 to 172.50 parts by mass of 2-acrylamido-2-methylpropanesulfonic acid, 152.00 to 177.50 parts by mass of acrylamide monomer, 0.15 to 0.175 part by mass of branching agent and 2.00 to 3.50 parts by mass of hydrophilic emulsifier.
Wherein, the acrylamide monomer is preferably acrylamide or N, N-dimethylacrylamide; the branching agent is preferably pentaerythritol. The hydrophilic emulsifier may be selected from the tween series, preferably tween 80 or tween 60. Ethoxylated fatty acid glycidyl esters are of the Tween series (Tween series). The glycidyl esters of different fatty acids are known as Span series, generally oil-soluble; span80 is sorbitan monooleate, is oily at room temperature, and has an HLB value of 4.3. The HLB value range of span series and tween series products is 1.8-16.7, and can be used in a compounding way.
In addition, the base oil and the lipophilic emulsifier are added into the reaction kettle, and the mixture is stirred until the mixture is completely dissolved, so that an oil phase is obtained. Specifically, the oil phase material comprises 208-224 parts by mass of base oil and 18.50-30.50 parts by mass of lipophilic emulsifier. The kinematic viscosity of the base oil at 40 ℃ is preferably 1.5mm 2 /s～3.0mm 2 And/s. For example, white oil # 2 or # 3. The lipophilic emulsifier may be selected from the span series, preferably commercially available span80 or span 60.
In the invention, the water-phase material preferably comprises 390 to 420 parts by mass of water, 147.86 to 172.50 parts by mass of 2-acrylamido-2-methylpropanesulfonic acid, 152.14 to 177.50 parts by mass of acrylamide monomer, 2.08 to 3.36 parts by mass of tween 80 emulsifier or tween 60 and 0.15 to 0.175 part by mass of branching agent. The oil phase material preferably comprises 208-224 parts by mass of white oil and 18.72-30.24 parts by mass of span-80 or span-60 emulsifying agent.
The invention preferably adds the water phase into the oil phase slowly under the condition of stirring, and can emulsify for 20min at high speed to obtain the monomer emulsion. In the embodiment of the invention, the monomer emulsion is placed in a water bath with the temperature of 30-65 ℃, inert gas is preferably introduced, 1-1.5 parts by mass of initiator can be added, and the polymerization is carried out for 3-5 hours by stirring at a low speed, so that the star polymer for drilling fluid is obtained.
In the present invention, the initiator is preferably one or more of a cerium salt initiator and a persulfate initiator. The cerium salt initiator is preferably ceric ammonium nitrate; the persulfate initiator is preferably ammonium persulfate or potassium persulfate. In the embodiment of the invention, 1.006-1.173 parts by mass of cerium salt or a cerium salt and persulfate composite initiation system is preferably adopted to polymerize to form the star polymer under the protection of high-purity nitrogen.
In the preparation process of the star polymer filtrate reducer emulsion, the embodiment of the invention takes pentaerythritol as branching agent (the molecular structure of pentaerythritol contains four-CH which is easy to generate oxidation-reduction reaction) 2 OH groups, spatially four-oriented and structurally symmetrical, suitable for forming branched structures); one or two of sodium hydroxide and potassium hydroxide are adopted to compositely adjust the pH value of the system, balance the heat dissipation capacity of the system, and avoid potential safety hazards of the process flow caused by overlarge heat at a certain stage; controlling the pH value of the system, balancing the reactivity ratio among monomers, adjusting the reaction time of different initiation stages, balancing the monomer conversion rate of each stage, balancing the heat dissipation capacity of each stage system, and ensuring the stable reaction. The invention is preferably initiated by adopting low temperature of 30-45 ℃ water bath, the whole reaction process is heated at a constant speed, when the system temperature reaches 40 ℃, the monomer conversion rate can reach 50%, and the highest temperature of the system in the whole polymerization process is not more than 60 ℃.
The star polymer prepared by the method has the advantages that the molecular chain can adopt a more extended conformation due to the mutual repulsive interaction among arms, the bridging filtrate reducer has strong capability, and the effect is better than that of a linear polymer. The preparation method is simple and convenient, and the obtained product has better temperature resistance and salt resistance, can be used for high-temperature and high-salt stratum, and reduces the filtration loss of drilling fluid.
The invention also provides application of the star polymer for drilling fluid as the filtrate reducer in the drilling fluid. The invention is not particularly limited to components such as base slurry in the drilling fluid; the addition amount of the star polymer filtrate reducer product can be 1.0-3.0%.
Experiments show that when the addition amount of the product is 3.0%, the API of the composite brine slurry is less than 5.0mL after 165 ℃/16h aging, and the API of the composite brine slurry is less than 30mL after 180 ℃/16h aging (the filtration loss rate of the same type of linear polymer filtrate loss reducer is more than 50%). The star polymer filtrate reducer has higher comprehensive effects of high temperature resistance and the like, and has important significance for solving the problem of controlling the liquid of high-salt and high-temperature deep well drilling fluid in the northbound direction and promoting the technical progress of the drilling fluid.
For a further understanding of the present invention, the star polymers for drilling fluids provided herein, methods of making and using the same, are described in detail below in connection with the examples. It is to be understood that these examples are provided for the purpose of illustrating the details of the invention and the particular process and are not intended to limit the scope of the invention, which is defined solely by the claims, but not by the way of limitation.
In the following examples: the white oil is 2# or 3# white oil with the kinematic viscosity of 2.0-3.0 mm 2 /s。
Example 1:
420g of water is added into a reaction kettle, 152g of 2-acrylamide-2-methylpropanesulfonic acid, 156g of acrylamide, 0.15g of pentaerythritol and 2.8g of tween-80 emulsifier are added by stirring, and then the pH of the system is regulated to 9.0 by 30% potassium hydroxide, so as to obtain a water phase;
224g of No. 2 white oil and 25.2g of span-80 emulsifying agent are added into a reaction kettle, and stirred until all the materials are dissolved, so as to obtain an oil phase;
slowly adding the water phase into the oil phase under stirring, stirring for 20min, and emulsifying at high speed for 20min to obtain monomer emulsion; and (3) placing the monomer emulsion in a constant-temperature water bath at 35 ℃, introducing nitrogen for 30min, adding 1.006g of ammonium cerium nitrate, and reacting for 5h under low-speed stirring to obtain the target polymer emulsion.
Example 2:
390g of water is added into a reaction kettle, 172.5g of 2-acrylamide-2-methylpropanesulfonic acid, 177.5g of acrylamide, 0.175g of pentaerythritol and 2.6g of tween-80 emulsifier are added with stirring, and then the pH value of the system is regulated to 10.0 by 30% sodium hydroxide, so as to obtain a water phase;
adding 208g of No. 2 white oil and 23.4g of span-80 emulsifier into a reaction kettle, and stirring until the materials are completely dissolved to obtain an oil phase;
slowly adding the water phase into the oil phase under stirring, fully stirring, and emulsifying at high speed for 20min to obtain monomer emulsion; placing the monomer emulsion in a constant-temperature water bath at 40 ℃, introducing nitrogen for 30min, adding 1.173g of ammonium persulfate, and reacting for 3h under low-speed stirring to obtain a target product.
Example 3:
408g of water is added into a reaction kettle, 158g of 2-acrylamide-2-methylpropanesulfonic acid, 162g of N, N-methacrylamide, 0.16g of pentaerythritol, 1.125g of ceric ammonium nitrate and 3.264g of Tween-80 emulsifier are added by stirring, and then the pH value of the system is regulated to 9.0 by 30% potassium hydroxide, so as to obtain a water phase;
adding 217g of No. 2 white oil and 29.38g of span-80 emulsifier into a reaction kettle, and stirring until the mixture is completely dissolved to obtain an oil phase;
slowly adding the water phase into the oil phase under stirring, stirring for 20min, and emulsifying at high speed for 20min to obtain monomer emulsion; and (3) placing the monomer emulsion in a constant-temperature water bath at 35 ℃, introducing nitrogen for 30min, adding 0.833g of ammonium cerium nitrate and 0.173g of ammonium persulfate, and reacting for 5h under low-speed stirring to obtain the target product.
Example 4:
390g of water is added into a reaction kettle, 172.5g of 2-acrylamide-2-methylpropanesulfonic acid, 177.5g of acrylamide, 0.175g of pentaerythritol and 2.6g of tween-80 emulsifier are added by stirring, and then the pH value of the system is regulated to 10.0 by 30% sodium hydroxide, so as to obtain a water phase;
adding 208g of 3# white oil and 23.4g of span-80 emulsifier into a reaction kettle, and stirring until the materials are completely dissolved to obtain an oil phase;
slowly adding the water phase into the oil phase under stirring, fully stirring, and emulsifying at high speed for 20min to obtain monomer emulsion; and (3) placing the monomer emulsion in a constant-temperature water bath at 40 ℃, introducing nitrogen for 30min, adding 0.971g of ammonium cerium nitrate and 0.202g of ammonium persulfate, and reacting for 3h under low-speed stirring to obtain the target product.
Example 5:
420g of water is added into a reaction kettle, 152g of 2-acrylamide-2-methylpropanesulfonic acid, 156g of N, N-methacrylamide, 0.175g of pentaerythritol, 1.173g of ceric ammonium nitrate and 2.8g of tween-80 emulsifier are added by stirring, then 30% of potassium hydroxide and sodium hydroxide are mixed according to the mass ratio of 2:1, and the pH value of the system is regulated to 10, so as to obtain a water phase;
224g of No. 3 white oil and 25.2g of span-80 emulsifier are added into a reaction kettle, and stirred until all the components are dissolved, so as to obtain an oil phase;
slowly adding the water phase into the oil phase under stirring, stirring for 20min, and emulsifying at high speed for 20min to obtain monomer emulsion; and (3) placing the monomer emulsion in a constant-temperature water bath at 35 ℃, introducing nitrogen for 30min, adding 1.006g ammonium persulfate initiator, and reacting for 5h under low-speed stirring to obtain a target product.
The products obtained in examples 1-5 above were subjected to evaluation of drilling fluid properties: the medium pressure fluid loss of the drilling fluid is measured by adopting a composite brine-based slurry and polymer emulsion with the concentration of +3.0% through rolling aging for 16 hours at 165 ℃ and 180 ℃, and then according to the specification of 7.2 in GB/T16783.1-2006, the temperature is 24 ℃ +/-3 ℃, and the pressure is 690KPa. The results are shown in Table 1.
Wherein, the composite brine-based slurry: 350mL of distilled water+4.5% of sodium chloride+0.5% of calcium chloride+1.3% of magnesium chloride+0.9% of anhydrous sodium carbonate+15% of calcium bentonite.
TABLE 1 Performance index of the products prepared in examples 1 to 5
As is clear from Table 1, when the apparent viscosity of the 1.0% emulsion is less than 35.0 mPas and the addition amount of the emulsion in the composite brine slurry is 3.0%, the API filtrate loss is less than 5.0mL after 165 ℃/16h high temperature aging, the API filtrate loss is less than 30.0mL after 180 ℃/16h high temperature aging, the apparent viscosity is reduced, and the API filtrate loss is less than 50% after high temperature aging. Therefore, the star-shaped polymer product has better temperature resistance and salt resistance, can be used for high-temperature and high-salt stratum, and reduces the filtration loss of drilling fluid.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications to these embodiments can be made by those skilled in the art without departing from the technical principles of the present invention, and these modifications should also be considered as the scope of the present invention.
Claims (10)
1. The star polymer for the drilling fluid is characterized by being prepared from acrylamide monomers, 2-acrylamide-2-methylpropanesulfonic acid and a branching agent through emulsion polymerization;
the branching agent is pentaerythritol;
the star polymer for the drilling fluid has a branched structure and a nano polymer microsphere morphology.
2. The star polymer for a drilling fluid according to claim 1, wherein the apparent viscosity of a 1.0% solution of the star polymer for a drilling fluid is not more than 35.0 mpa.s at room temperature.
3. A preparation method of star polymer for drilling fluid comprises the following steps:
s1, adding a water phase material into an oil phase material for emulsification to obtain a monomer emulsion; the aqueous phase material comprises acrylamide monomers, 2-acrylamide-2-methylpropanesulfonic acid and a branching agent; the branching agent is pentaerythritol;
s2, carrying out polymerization reaction on the monomer emulsion under the existence of an initiator to obtain the star polymer of the nano polymer microsphere.
4. The preparation method according to claim 3, wherein the aqueous phase material comprises 390 to 420 parts by mass of water, 147.50 to 172.50 parts by mass of 2-acrylamido-2-methylpropanesulfonic acid, 152.00 to 177.50 parts by mass of acrylamide-type monomers, 0.15 to 0.175 parts by mass of branching agent, and 2.00 to 3.50 parts by mass of hydrophilic emulsifier.
5. The preparation method according to claim 4, wherein the oil phase material comprises 208 to 224 parts by mass of base oil and 18.50 to 30.50 parts by mass of lipophilic emulsifier.
6. The process of claim 5, wherein the base oil has a kinematic viscosity of 1.5mm at 40 ℃ 2 /s～3.0mm 2 /s。
7. The method of claim 5, wherein the hydrophilic emulsifier is selected from the tween series; the lipophilic emulsifier is selected from span series.
8. The method of claim 3, wherein the initiator is one or more of a cerium salt initiator and a persulfate initiator.
9. The preparation method of claim 8, wherein the monomer emulsion is placed in a water bath at 30-65 ℃, inert gas is introduced, an initiator is added, and the polymerization is carried out for 3-5 hours under low-speed stirring, so as to obtain the star polymer.
10. Use of a star polymer for drilling fluids according to any of claims 1-2 as a fluid loss additive in drilling fluids.
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| EP2789670A1 (en) * | 2013-04-08 | 2014-10-15 | S.P.C.M. Sa | Polymers for enhanced hydrocarbon recovery |
| CN104497220B (en) * | 2015-01-04 | 2017-02-22 | 西南石油大学 | Starlike anti-shearing polyacrylamide for fracturing fluid and preparation method of starlike anti-shearing polyacrylamide |
| CN107586360B (en) * | 2017-10-23 | 2018-07-03 | 中国地质大学（北京） | A kind of Star Polyacrylamide copolymer and preparation method thereof and drilling fluid |
| CN111205395B (en) * | 2020-01-16 | 2020-11-24 | 中国地质大学（北京） | Star-shaped copolymer, preparation method and application thereof, constant-current modified water-based drilling fluid, and preparation method and application thereof |
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2020
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