CN108676129B - Comb-structured amphoteric ion polymer fluid loss agent and preparation method thereof - Google Patents
Comb-structured amphoteric ion polymer fluid loss agent and preparation method thereof Download PDFInfo
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- CN108676129B CN108676129B CN201810525580.4A CN201810525580A CN108676129B CN 108676129 B CN108676129 B CN 108676129B CN 201810525580 A CN201810525580 A CN 201810525580A CN 108676129 B CN108676129 B CN 108676129B
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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- 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
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
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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
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Abstract
The invention relates to a comb-structure amphoteric ion polymer fluid loss additive and a preparation method thereof. The fluid loss agent is prepared by copolymerizing the following monomers in parts by weight: 20-40 parts of 2-acrylamide-2-methylpropanesulfonic acid, 5-30 parts of polyethylene glycol monomethyl ether acrylate, 10-60 parts of N, N-dimethylacrylamide and 5-20 parts of dimethyl diallyl ammonium chloride. The filtrate reducer contains quaternary amino, amido, sulfonic acid and other molecular groups, wherein the sulfonic acid group has stronger hydration capability, and the amido and quaternary ammonium salt have strong adsorption capability to clay, so that the adsorption stability of the filtrate reducer under the high-temperature condition is improved; the product obtained by graft copolymerization of the macromolecular monomer polyethylene glycol monomethyl ether acrylate and other monomers is of a comb-shaped special structure, so that the shear resistance and the high-temperature stability can be further improved, the filtrate loss reduction performance is ensured, the temperature and salt resistance effect is good, and the polymer material can be effectively applied to drilling fluid in high-temperature complex stratum environments.
Description
Technical Field
The invention belongs to the field of additives for drilling fluids, and particularly relates to a comb-structure amphoteric ion polymer fluid loss additive and a preparation method thereof.
Background
With the development of the oil industry and the increasing demand for oil, the drilling depth is increased, and the high-temperature complex stratum and the underground complex conditions are met more and more. The drilling fluid is called 'blood' of a drilling process, is an important component of a drilling technology, and plays an increasingly important role in the drilling process. The filtrate reducer is one of the important agents of the drilling fluid, and has the function of forming a low-permeability, flexible, thin and compact filter cake on the well wall, so that the filtrate loss of the drilling fluid is reduced as much as possible, the stability of the well wall is maintained, and the downhole safety is ensured.
How to prepare a fluid loss additive with good temperature resistance and salt resistance is one of the key points of research of petroleum workers. The application publication No. CN101864030A discloses a preparation method of a high-temperature-resistant and salt-resistant filtrate reducer, which takes C6-C10 alkane as a continuous phase, three monomers of acrylamide, acrylic acid and styrene sodium sulfonate are dissolved in a water phase, and an emulsifier is added to obtain the high-temperature-resistant and salt-resistant amphoteric filtrate reducer by a reverse microemulsion polymerization method; in the preparation method, three initial monomers are strictly controlled in a certain proportion range, if the polymerization proportion of the reverse microemulsion is not proper, the system is difficult to form the microemulsion or the service performance of the polymer is reduced, and the stability of industrial large-scale production is difficult to guarantee.
The patent with the publication number of CN100595254C discloses a preparation method of a zwitterionic polymer fluid loss additive, the preparation method is to obtain a high-temperature-resistant and salt-resistant amphoteric fluid loss additive by an aqueous solution polymerization method, but the production process is complex, the production efficiency is low, and the conditions of large-scale production are difficult to meet. The patent with the publication number of CN104926986B discloses a preparation method of a zwitterionic polymer for drilling fluid, which is prepared by taking dimethylaminoethyl methacrylate, 1, 3-propane sultone and acrylamide as monomers through polymerization reaction.
Disclosure of Invention
The invention aims to provide a zwitterionic polymer fluid loss agent with a comb-shaped structure, so as to solve the problem that the existing fluid loss agent cannot have both excellent fluid loss performance and temperature and salt resistance.
The second purpose of the invention is to provide a preparation method of the filtrate reducer.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a zwitterionic polymer filtrate reducer with a comb-type structure is prepared by copolymerizing the following monomers in parts by weight: 20-40 parts of 2-acrylamide-2-methylpropanesulfonic acid, 5-30 parts of polyethylene glycol monomethyl ether acrylate, 10-60 parts of N, N-dimethylacrylamide and 5-20 parts of dimethyl diallyl ammonium chloride.
The polyethylene glycol monomethyl ether acrylate has polyethylene glycol chain segments with excellent compatibility, and is widely applied to the surface modification of various medical biomaterials, the synthesis research of novel high-efficiency water reducing agents and other materials. The macromonomer is used as a branched chain of a comb polymer to enhance the rigidity of the whole molecular structure and ensure that the drilling fluid has better rheological property and high temperature resistance. The structural formula is as follows:
the amphoteric ion polymer fluid loss additive with the comb-type structure is a multi-component copolymer formed by graft copolymerization of 2-acrylamide-2-methylpropanesulfonic acid, polyethylene glycol monomethyl ether acrylate, N-dimethylacrylamide and dimethyl diallyl ammonium chloride in an aqueous solution, wherein the obtained copolymer contains molecular groups such as quaternary amino groups, amide groups and sulfonic groups, the sulfonic groups have strong hydration capacity (particularly high-temperature calcium and magnesium pollution resistance), and the amide groups and quaternary ammonium salts have strong adsorption capacity on clay, so that the adsorption stability of the fluid loss additive under a high-temperature condition is improved; the product is of a comb-shaped special structure, so that the shearing resistance and the high-temperature stability can be further improved, the filtrate loss reduction performance is ensured, the temperature resistance and salt resistance effects are good, and the drilling fluid can be effectively applied to the drilling fluid in the high-temperature complex stratum environment.
The preparation method of the amphoteric ion polymer filtrate reducer with the comb-shaped structure comprises the following steps:
1) dissolving 2-acrylamide-2-methylpropanesulfonic acid, polyethylene glycol monomethyl ether acrylate, N-dimethylacrylamide and dimethyl diallyl ammonium chloride in water to obtain a monomer solution;
2) and (3) adding an initiator to carry out copolymerization reaction under a protective atmosphere to obtain the catalyst.
In the step 1), 2-acrylamide-2-methylpropanesulfonic acid is dissolved by adding water, polyethylene glycol monomethyl ether acrylate is added and stirred uniformly, and N, N-dimethylacrylamide and dimethyl diallyl ammonium chloride are added in the mixture2And (3) uniformly stirring under protection of 35-50 ℃ to obtain the monomer solution.
In the step 1), a pH value regulator is added into the monomer solution to regulate the pH value of the system to be 6-8. The pH value regulator is one or a combination of sodium hydroxide, hydrogen oxidant and ammonia water.
In the step 1), the sum of the mass concentrations of the monomers in the monomer solution is 20-45%.
In the step 2), the initiator is a mixture of at least one of ammonium persulfate and potassium persulfate and sodium bisulfite. Preferably, the mass percentage of the sodium bisulfite in the initiator is 25 percent to 50 percent.
In the step 2), the concentration of the initiator in the polymerization system is 0.5-5%.
In the step 2), the copolymerization reaction is firstly carried out for 0.5-1.5 h at 35-50 ℃, and then for 2.5-3.5 h at 75-85 ℃.
And in the step 2), filtering after copolymerization, collecting a filtering product, washing and drying to obtain the filtrate reducer. The washing liquid used for washing is acetone; the drying is vacuum drying for 8-12 h at 100-110 ℃.
The preparation method of the amphoteric ion polymer filtrate reducer with the comb-shaped structure has the advantages of simple preparation process, low requirement on equipment, good production stability and low cost, and is easy to realize large-scale industrial production.
Detailed Description
The following examples are provided to further illustrate the practice of the invention. In the following examples, the number average molecular weight of polyethylene glycol monomethyl ether acrylate was 400-2000.
Example 1
The amphoteric ionic polymer filtrate reducer with the comb-shaped structure is prepared by copolymerizing the following monomers in parts by weight: 40 parts of 2-acrylamide-2-methylpropanesulfonic acid, 20 parts of polyethylene glycol monomethyl ether acrylate, 30 parts of N, N-dimethylacrylamide and 10 parts of dimethyl diallyl ammonium chloride; the preparation process comprises the following steps:
1) adding 40 parts of 2-acrylamide-2-methylpropanesulfonic acid and 300 parts of distilled water into a reactor, and stirring until the materials are fully dissolved; then adding 20 parts of polyethylene glycol monomethyl ether acrylate, stirring uniformly, adding a sodium hydroxide solution with the mass concentration of 20%, and adjusting the pH value of the system to 6; then adding 30 parts of N, N-dimethylacrylamide and 10 parts of dimethyldiallylammonium chloride, and uniformly stirring at 40 ℃ to obtain a monomer solution with the sum of the mass concentrations of the monomers being 25%;
2) introducing nitrogen for protection for 30min, and then adding an initiator (the mass ratio of ammonium persulfate to sodium bisulfite is 2: 1, the concentration of an initiator in a system is 3 percent), polymerizing for 1h at 40 ℃, and then heating to 80 ℃ for polymerizing for 3h to obtain a reaction product;
3) washing the reaction product with acetone, filtering, collecting the filtered product, vacuum-drying at 105 deg.C for 10h, and pulverizing to obtain white powdery filtrate reducer.
Example 2
The amphoteric ionic polymer filtrate reducer with the comb-shaped structure is prepared by copolymerizing the following monomers in parts by weight: 30 parts of 2-acrylamide-2-methylpropanesulfonic acid, 10 parts of polyethylene glycol monomethyl ether acrylate, 50 parts of N, N-dimethylacrylamide and 10 parts of dimethyl diallyl ammonium chloride; the preparation process comprises the following steps:
1) adding 30 parts of 2-acrylamide-2-methylpropanesulfonic acid and 400 parts of distilled water into a reactor, and stirring until the materials are fully dissolved; then adding 10 parts of polyethylene glycol monomethyl ether acrylate, stirring uniformly, adding a sodium hydroxide solution with the mass concentration of 20%, and adjusting the pH value of the system to 7; then adding 50 parts of N, N-dimethylacrylamide and 10 parts of dimethyldiallylammonium chloride, and uniformly stirring at 35 ℃ to obtain a monomer solution with the sum of the mass concentrations of the monomers being 20%;
2) introducing nitrogen for protection for 30min, and then adding an initiator (the mass ratio of potassium persulfate to sodium bisulfite is 3: 2, the concentration of the initiator in the system is 1 percent), polymerizing for 1.5h at 35 ℃, and then heating to 75 ℃ for polymerizing for 3.5h to obtain a reaction product;
3) washing the reaction product with acetone, filtering, collecting the filtered product, vacuum drying at 100 deg.C for 11h, and pulverizing to obtain white powdery filtrate reducer.
Example 3
The amphoteric ionic polymer filtrate reducer with the comb-shaped structure is prepared by copolymerizing the following monomers in parts by weight: 30 parts of 2-acrylamide-2-methylpropanesulfonic acid, 5 parts of polyethylene glycol monomethyl ether acrylate, 60 parts of N, N-dimethylacrylamide and 5 parts of dimethyl diallyl ammonium chloride; the preparation process comprises the following steps:
1) adding 30 parts of 2-acrylamide-2-methylpropanesulfonic acid and 300 parts of distilled water into a reactor, and stirring until the materials are fully dissolved; then adding 5 parts of polyethylene glycol monomethyl ether acrylate, stirring uniformly, adding a sodium hydroxide solution with the mass concentration of 20%, and adjusting the pH value of the system to 8; then adding 60 parts of N, N-dimethylacrylamide and 5 parts of dimethyldiallylammonium chloride, and uniformly stirring at 50 ℃ to obtain a monomer solution with the sum of the mass concentrations of the monomers being 25%;
2) introducing nitrogen for protection for 30min, and then adding an initiator (the mass ratio of ammonium persulfate to sodium bisulfite is 1: 1, the concentration of an initiator in a system is 4 percent), polymerizing for 0.5h at 50 ℃, and then heating to 85 ℃ for polymerizing for 2.5h to obtain a reaction product;
3) washing the reaction product with acetone, filtering, collecting the filtered product, vacuum drying at 110 deg.c for 8 hr, and crushing to obtain white powdered filtrate reducer.
Test examples
This test example tested the fluid loss performance and high temperature performance of the fluid loss additive of example 1 in a composite brine-based slurry and a brine-based slurry. Comparative example is a commercial acrylamide-based polymer fluid loss additive.
The preparation of the composite saline base slurry comprises the following steps: taking 1000mL of distilled water, 45.0g of sodium chloride, 7.0g of calcium chloride and 15g of magnesium chloride as composite brine, taking 350mL of composite brine, and adding 3.15g of sodium carbonate and 52.50g of calcium bentonite under stirring to obtain composite brine base slurry; the preparation of the saline base slurry comprises the following steps: 350mL of brine with different sodium chloride concentrations is taken, 35g of evaluation soil and 1g of sodium bicarbonate are added under stirring, after stirring is continued for 20min, brine base slurry is obtained, and the base slurry filtration loss is controlled to be 80-90 mL.
The performance evaluation results of the fluid loss additive in example 1 in the composite brine base slurry are shown in table 1, the mass fraction of the fluid loss additive is 0.7% when measuring the room-temperature fluid loss, and the amount of the fluid loss additive is 1.5% when measuring the high-temperature aged fluid loss, and the specific process is as follows:
(1) and (3) measuring the normal-temperature filtration loss: and taking the cured composite saline water-based slurry, adding 0.7% of filtrate reducer into the slurry at a certain rotating speed, stirring for 20min, and curing for 24h at room temperature. Stirring for 20min, and measuring the API filtration loss.
(2) High-temperature fluid loss measurement: and taking the cured composite saline water-based slurry, adding 1.5% of filtrate reducer into the slurry at a certain rotating speed, stirring for 20min, and curing for 6h at room temperature. Stirring for 20min, aging in stainless steel aging tank at 200 deg.C for 16 hr, cooling, stirring for 20min, and measuring API filtration loss.
Table 1 performance evaluation test data for fluid loss additive of example 1 in a composite brine-based slurry
| Serial number | Room temperature API filtrate loss/mL | API filtration loss/mL after 200 ℃ aging |
| Example 1 | 6.2 | 8.9 |
| Comparative example | 13.5 | 25.4 |
The performance evaluation results of the fluid loss additive of example 1 in saline-based slurry are shown in table 2, and 350mL of sodium chloride saline-based slurry with five different concentrations are taken and added with 2.45g and 5.25g of the fluid loss additive of example 1 respectively and stirred for 30 min; curing five of the materials at room temperature for 24h, curing the other five materials at room temperature for 6h, putting into a high-temperature tank, hot rolling at 200 ℃ for 16h, and cooling to room temperature; and (3) stirring the base slurry to be tested at a high speed (6000r/min) for 5min, and measuring the API filtration loss after aging at room temperature and 200 ℃.
Table 2 performance evaluation test data for fluid loss additive of example 1 in brine-based slurry
As can be seen from the performance evaluation results in tables 1 and 2, the fluid loss additive of example 1 performed well at a high temperature of 200 ℃ in the composite brine-based slurry and the brine-based slurry, and had excellent temperature resistance, salt resistance, and fluid loss properties.
Claims (7)
1. The amphoteric ionic polymer filtrate reducer with the comb-type structure is characterized by being prepared by dissolving the following monomers in parts by weight in water to obtain a monomer solution, and adding an initiator for copolymerization: 20-40 parts of 2-acrylamide-2-methylpropanesulfonic acid, 5-30 parts of polyethylene glycol monomethyl ether acrylate, wherein the number average molecular weight of the polyethylene glycol monomethyl ether acrylate is 400-2000, 10-60 parts of N, N-dimethylacrylamide and 5-20 parts of dimethyldiallylammonium chloride, the sum of the mass concentrations of the monomers in the monomer solution is 20-25%, and the concentration of an initiator in a polymerization system is 1-4%.
2. A method of making the comb-structured zwitterionic polymer fluid loss additive of claim 1, comprising the steps of:
1) dissolving 2-acrylamide-2-methylpropanesulfonic acid, polyethylene glycol monomethyl ether acrylate, N-dimethylacrylamide and dimethyl diallyl ammonium chloride in water to obtain a monomer solution;
2) and (3) adding an initiator to carry out copolymerization reaction under a protective atmosphere to obtain the catalyst.
3. The preparation method of the comb-structure zwitterionic polymer fluid loss agent according to claim 2, wherein in the step 1), the monomer solution is obtained by dissolving 2-acrylamide-2-methylpropanesulfonic acid in water, adding polyethylene glycol monomethyl ether acrylate, stirring uniformly, adding N, N-dimethylacrylamide and dimethyldiallylammonium chloride, and stirring uniformly at 35-50 ℃.
4. The preparation method of the comb-structure zwitterionic polymer fluid loss additive as defined in claim 2, wherein in the step 1), a pH value regulator is added into the monomer solution to regulate the pH value of the system to 6-8.
5. The method for preparing the comb-structured zwitterionic polymer fluid loss additive of claim 2, wherein in step 2), the initiator is a mixture of at least one of ammonium persulfate and potassium persulfate and sodium bisulfite.
6. The method for preparing the comb-structured zwitterionic polymer fluid loss additive according to claim 5, wherein the mass percentage of the sodium bisulfite in the initiator is 25-50%.
7. The method for preparing the comb-structured zwitterionic polymer fluid loss additive according to claim 2, wherein in the step 2), the copolymerization is performed at 35-50 ℃ for 0.5-1.5 h and then at 75-85 ℃ for 2.5-3.5 h.
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| CN113563510B (en) * | 2021-08-09 | 2022-09-06 | 建平天正矿业有限公司 | Temperature-resistant salt-resistant comb polymer fluid loss additive for drilling mud bentonite |
| CN115672261B (en) * | 2022-10-31 | 2024-02-20 | 江苏海洋大学 | Sulfhydryl Schiff base side group-containing polymer modified attapulgite and preparation method thereof |
| CN117645869B (en) * | 2024-01-29 | 2024-04-12 | 广饶县盛泉化工厂 | Emulsion polymer composite fracturing fluid and preparation method thereof |
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| CN101967369A (en) * | 2010-08-16 | 2011-02-09 | 山东大学 | Comb-like polymer fluid loss additive for drilling fluid and preparation method thereof |
| CN105542090A (en) * | 2015-12-08 | 2016-05-04 | 江苏苏博特新材料股份有限公司 | Rheology modifier for concrete and preparation method thereof |
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| CA2760734C (en) * | 2009-05-20 | 2017-05-16 | Basf Se | Hydrophobically associating copolymers |
| US8362180B2 (en) * | 2009-05-20 | 2013-01-29 | Basf Se | Hydrophobically associating copolymers |
| CN106146722B (en) * | 2015-03-31 | 2018-07-06 | 大庆市新万通科技开发有限公司 | Amphoteric ion complex microsphere and its preparation method and application |
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| CN101967369A (en) * | 2010-08-16 | 2011-02-09 | 山东大学 | Comb-like polymer fluid loss additive for drilling fluid and preparation method thereof |
| CN105542090A (en) * | 2015-12-08 | 2016-05-04 | 江苏苏博特新材料股份有限公司 | Rheology modifier for concrete and preparation method thereof |
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