CN108752505A - A kind of hydrophobically modified dissaving polymer and preparation method thereof - Google Patents
A kind of hydrophobically modified dissaving polymer and preparation method thereof Download PDFInfo
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- CN108752505A CN108752505A CN201810645142.1A CN201810645142A CN108752505A CN 108752505 A CN108752505 A CN 108752505A CN 201810645142 A CN201810645142 A CN 201810645142A CN 108752505 A CN108752505 A CN 108752505A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
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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
- C08F220/56—Acrylamide; Methacrylamide
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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
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
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Abstract
The invention belongs to technical field of polymer, a kind of hydrophobically modified dissaving polymer and preparation method thereof is disclosed, is prepared using the method for Light lnduced Free Radicals micellar copolymerization:In the aqueous solution containing water-soluble monomers such as acrylamide, acrylic acid, 2- acrylamide-2-methyl propane sulfonics, hyperbranched modified monomers, Surfactant SDS and N- benzyl-N- alkyl (methyl) acrylamide is added, using surfactant by hydrophobic monomer solubilising its formation micella in, by light-initiated mode, hydrophobic monomer and water-soluble monomer are copolymerized.The product that the present invention is prepared has good dissolubility, stronger increasing stick ability, good temperature-resistant anti-salt performance and preferable anti-shear performance, intends the oil displacement agent or acid fracturing thickener that are used as improving oil recovery factor, has broad application prospects.
Description
Technical field
The invention belongs to technical field of polymer more particularly to a kind of hydrophobically modified dissaving polymer and its preparation sides
Method.
Background technology
After decades of development, polymer be widely used to a series of oil wells probings for adapting to different reservoir conditions,
In the effective technology of water and oil control and acid fracturing.However in oil field practice application, there are serious degradations to ask for polymer
Topic, including mechanical degradation, thermal degradation, chemical degradation and microbial degradation etc..
Currently, the main path for improving the performance of polymer has:
(1) it uses acrylamide and carries temperature-resistant anti-salt performance structure (such as sulfonic group, rigid radical, quaternary ammonium salt cationic
Deng) function monomer copolymerization, prepare Heat Resistant and Salt Tolerant Polymer.The reports such as Chen Shilan use reversed emulsion polymerization, with acryloyl
Amine, 2- acrylamide-2-methyl propane sulfonics, n-vinyl-2-pyrrolidone are monomer, and kerosene is oil phase, Span-80 and are spat
Temperature -60 is emulsifier, and potassium peroxydisulfate and sodium hydrogensulfite are that initiator prepares copolymer, and polymer solution shows stronger resistance to
Warm saline-alkaline tolerance (Chen Shilan etc., reversed emulsion polymerization prepare temperature-resistant anti-salt acrylamide polymer [J], using chemical industry, 2017
(8)), but synthetic method is complicated and n-vinyl-2-pyrrolidone reactivity ratio is relatively low, it is difficult to acrylamide and 2- acryloyls
Amine -2- methyl propane sulfonic acids etc. are copolymerized.
(2) a small amount of hydrophobic grouping is carried on polymer hydrophilicity macromolecular chain, prepares hydrophobic associated polymer.Patent
CN106397694 reports a kind of high salt tolerance combed block hydrophobic associated polymer, hydrogen bond and hydrophobic association between macromolecular etc.
Intermolecular force makes polymer solution have supramolecular structure, improves temperature-resistant anti-salt, the anti-shear ability of polymer, but
Still there is a problem of that hydrolytic resistance and anti-aging property are poor to a certain extent.
(3) bi-vinyl or double propenyl monomer are added in polymerization, copolymer macromolecular is made micro- cross-linked structure, system occur
Standby micro-crosslinked polymer.Patent CN102408518 reports a kind of micro- crosslinking Polymer Used For Oil Displacement, draws in acrylamide copolymer
Enter bi-vinyl monomer, to improve the temperature-resistant anti-salt performance of polyacrylamide.However bi-vinyl or double propenyl monomer add
Amount is not easy to control, crosses low polymer increasing stick effect unobvious, and it is difficult to cross high polymer dissolving.
(4) hyperbranched polymerize is prepared using the dissaving polymer of end modified ethylene linkage as parent nucleus with copolymerization such as acrylamides
Object.Patent CN103865008 reports a kind of polyamide-amide hybridized nanometer silica dissaving polymer, by functional poly
Amide-amine hybridized nanometer silica monomer and acrylamide, acrylic acid, heat and salt resistance monomer, with redox initiator
Or two NSC 18620 initiator of azo causes polymerization, which shows excellent anti-shear performance, heat resistance, but
The increasing stick and anti-salt property of polymer are still undesirable.
In conclusion problem of the existing technology is:There are synthetic methods for the method for the existing performance for improving polymer
Complicated and n-vinyl-2-pyrrolidone reactivity ratio is relatively low, it is difficult to acrylamide and 2- acrylamide-2-methyl propane sulfonics etc.
It is copolymerized;There is a problem of that hydrolytic resistance and anti-aging property are poor;Bi-vinyl or double propenyl monomer dosage are not
It is easy to control, low polymer increasing stick effect unobvious are crossed, it is difficult to cross high polymer dissolving;The increasing stick and anti-salt property of polymer are still not
It is ideal.
Invention content
In view of the problems of the existing technology, the present invention provides a kind of hydrophobically modified dissaving polymer and its preparation sides
Method.
The invention is realized in this way a kind of hydrophobically modified dissaving polymer, the hydrophobically modified dissaving polymer
Molecular formula be:
In formula, x, y, z, m are structural unit percentage, and it be 10~20%, z is that 0~5%, m is that x, which is 75~85%, y,
0.05~0.2%, x+y+z+m=1;A is structural unit number, a 7,9,11,13 or 15;R is CH3Or H;Polymer is viscous to be divided equally
Son amount is 100~9,000,000.
Another object of the present invention is to provide a kind of preparation method of the hydrophobically modified dissaving polymer, the systems
Preparation Method includes the following steps:
Acrylamide, acrylic acid, 2- acrylamide-2-methyl propane sulfonics and over-expense is added in step 1 in deionized water
Change modified monomer, stir evenly, it is 7 to adjust pH value with sodium hydroxide, adds hydrophobic monomer N- benzyl-N- alkyl (methyl) third
Acrylamide and Surfactant SDS, magnetic agitation to solution clear;
Step 2, logical inert gas remove the dissolved oxygen in water 15 minutes;
Step 3 is added photoinitiator, reaction system is placed under light-initiated device and is reacted 3~5 hours, reaction temperature is
10~30 DEG C, obtain white colloidal, as hydrophobically modified dissaving polymer.
Further, the photoinitiator is azo-bis-isobutyrate hydrochloride (v50) or 2- hydroxyls -4'- (2- hydroxy ethoxies) -
2- methyl phenyl ketones (Irgacure2959).
The hydrophobically modified dissaving polymer of the present invention, preparation process are light-initiated water phase micellar free radical copolymerization, condition
Mildly, easy to operate, the product being prepared has good dissolubility, stronger increasing stick ability, good heat and salt resistance
Energy and preferable anti-shear performance intend the oil displacement agent or acid fracturing thickener that are used as improving oil recovery factor, have wide
Application prospect.The preparation method principle of the present invention is true and reliable, easy to operate, the hydrophobically modified dissaving polymer table of preparation
Reveal excellent increasing stick, Polymer Solution Viscosity reaches 253.4mPa.s when 1000mg/L, and when 2000mg/L reaches
682.4mPa.s;Under the conditions of 90 DEG C, viscosity retention rate may remain in 60% or more, show good heat resistance;With
The raising of NaCl, the apparent viscosity of polymer show the trend for first reducing and increasing reduce again afterwards, and the region of salt thickening is wider, and
And 20 × 104Viscosity retention rate still may remain in 10% or more saline-alkaline tolerance under the conditions of mg/LNaCl, show good;?
90 DEG C, 170s-1Under the conditions of, viscosity retention rate still 10% or more, shows good anti-shear performance.
Description of the drawings
Fig. 1 is viscosity-concentration relationship curve synoptic diagram of polymer provided in an embodiment of the present invention.
Fig. 2 is viscosity-temperature curve schematic diagram of polymer provided in an embodiment of the present invention.
Fig. 3 is viscosity-NaCl concentration relation curve schematic diagram of polymer provided in an embodiment of the present invention.
Fig. 4 is conjunction object viscosity-shear rate relation curve schematic diagram provided in an embodiment of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
The molecular formula of hydrophobically modified dissaving polymer provided in an embodiment of the present invention is:
In formula, x, y, z, m are structural unit percentage, and it be 10~20%, z is that 0~5%, m is that x, which is 75~85%, y,
0.05~0.2%, x+y+z+m=1;A is structural unit number, a 7,9,11,13 or 15;R is CH3Or H;Polymer is viscous to be divided equally
Son amount is 100~9,000,000.
As shown in Figure 1, the preparation method of hydrophobically modified dissaving polymer provided in an embodiment of the present invention includes following step
Suddenly:
S101:Acrylamide, acrylic acid, 2- acrylamide-2-methyl propane sulfonics and hyperbranched are added in deionized water
Modified monomer stirs evenly, and it is 7 to adjust pH value with sodium hydroxide, adds hydrophobic monomer N- benzyl-N- alkyl (methyl) propylene
Amide and Surfactant SDS, magnetic agitation to solution clear;
S102:Logical inert gas removes the dissolved oxygen in water 15 minutes;
S103:Photoinitiator 2- hydroxyls -4'- (2- hydroxy ethoxies) -2- methyl phenyl ketones are added, reaction system is placed in light
It is reacted 3~5 hours under initiating device, reaction temperature is 10~30 DEG C, obtains white colloidal, the as hyperbranched polymerization of hydrophobically modified
Object.
In a preferred embodiment of the invention:Photoinitiator is azo-bis-isobutyrate hydrochloride (v50) or 2- hydroxyls -4'-
(2- hydroxy ethoxies) -2- methyl phenyl ketones (Irgacure2959).
The application principle of the present invention is further described with reference to specific embodiment.
One, the preparation of hydrophobically modified dissaving polymer
Embodiment one:
10g acrylamides, 2.5g acrylic acid, the hyperbranched modified monomers of 0.01g are weighed, distilled water is added to stir evenly, is adjusted
PH value is 7;Add 0.2gN- benzyl-N- dodecyl methacrylamides and 0.7g lauryl sodium sulfate, then adds a certain amount of steaming
Distilled water makes solution quality reach 50g, stirring to solution clear;Logical nitrogen 15min, removes the dissolved oxygen in water;Addition is drawn
Agent Irgacure2959 (0.016wt% of monomer gross mass) is sent out, is placed under light-initiated device, 4h is reacted.
Embodiment two:
It is hyperbranched to weigh 9.9g acrylamides, 1.6g acrylic acid, 1.0g 2- acrylamide-2-methyl propane sulfonics, 0.01g
Modified monomer adds distilled water to stir evenly, and it is 7 to adjust pH value;Add 0.2gN- benzyl-N- dodecyl methacrylamides and
0.7g lauryl sodium sulfate, then add a certain amount of distilled water, so that solution quality is reached 50g, stirring to solution clear;Logical nitrogen
Gas 15min removes the dissolved oxygen in water;Initiator Irgacure2959 (0.016wt% of monomer gross mass) is added, is placed in light
Under initiating device, 4h is reacted.
Embodiment three:
10g acrylamides, 2.5g acrylic acid, the hyperbranched modified monomers of 0.01g are weighed, distilled water is added to stir evenly, is adjusted
PH value is 7;Add 0.2gN- benzyl-N- dodecyl methacrylamides and 0.7g lauryl sodium sulfate, then adds a certain amount of steaming
Distilled water makes solution quality reach 50g, stirring to solution clear;Logical nitrogen 15min, removes the dissolved oxygen in water;Light is added
Initiator V50 (0.1wt% of monomer gross mass), is placed under light-initiated device, reacts 4h.
Example IV:
It is hyperbranched to weigh 9.9g acrylamides, 1.6g acrylic acid, 1.0g 2- acrylamide-2-methyl propane sulfonics, 0.01g
Modified monomer adds distilled water to stir evenly, and it is 7 to adjust pH value;Add 0.2gN- benzyl-N- dodecyl methacrylamides and
0.7g lauryl sodium sulfate, then add a certain amount of distilled water, so that solution quality is reached 50g, stirring to solution clear;Logical nitrogen
Gas 15min removes the dissolved oxygen in water;Photoinitiator v50 (0.1wt% of monomer gross mass) is added, is placed in light-initiated device
Under, react 4h.
Two, the increasing stick performance of hydrophobically modified dissaving polymer
By the polymer of embodiment one, it is configured to the polymer solution of various concentration.In 30 DEG C, shear velocity 7.34s-1
Under conditions of, measure viscosity-concentration relationship curve (as shown in Figure 1) of polymer.From figure 1 it appears that polymer hydrophobic
Association is strong, and increasing stick is with obvious effects, and Polymer Solution Viscosity reaches 253.4mPa.s when 1000mg/L, and when 2000mg/L polymerize
Object solution viscosity reaches 682.4mPa.s.
Three, the heat resistance of hydrophobically modified dissaving polymer
Heat resistance research is carried out to the polymer of embodiment one.By polymer formulation at the solution of 1000mg/L, 30
DEG C, shear velocity 7.34s-1Under conditions of, the apparent viscosity variation with temperature relationship of polymer solution is measured (such as Fig. 2 institutes
Show).From figure 2 it can be seen that with the raising of temperature, the apparent viscosity of polymer continuously decreases, even if under the conditions of 90 DEG C,
The viscosity retention rate of polymer solution still may remain in 60% or more, show good heat resistance.
Four, the anti-salt property of hydrophobically modified dissaving polymer
Anti-salt property research is carried out to the polymer of embodiment one.Polymer is configured under different NaCl concentrations
The solution of 1000mg/L.In 30 DEG C, shear velocity 7.34s-1Under conditions of, the apparent viscosity of polymer solution is measured with NaCl
The variation relation (as shown in Figure 3) of concentration.From figure 3, it can be seen that with the raising of NaCl, the apparent viscosity of polymer shows
The trend for increasing reduce again afterwards is first reduced, the region of salt thickening is wider, and in high salinity (20 × 104Mg/LNaCl it is sticked under)
Degree retention rate still may remain in 10% or more, show good anti-salt property.
Five, the anti-shear performance of hydrophobically modified dissaving polymer
Anti-shear performance research is carried out to the polymer of embodiment one.By polymer formulation at the solution of 1000mg/L.?
Different temperatures, different shear velocity down cut 120s, measure the apparent viscosity of polymer solution with the variation of temperature, shear rate
Relationship (as shown in Figure 4).Figure 4, it is seen that with the increase of temperature, shear rate, the viscosity of polymer solution is continuous
It reduces, but at 90 DEG C, 170s-1Under the conditions of, viscosity retention rate still 10% or more, shows good anti-shear performance.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (3)
1. a kind of hydrophobically modified dissaving polymer, which is characterized in that the molecular formula of the hydrophobically modified dissaving polymer is:
In formula, x, y, z, m are structural unit percentage, x be 75~85%, y be 10~20%, z be 0~5%, m be 0.05~
0.2%, x+y+z+m=1;A is structural unit number, a 7,9,11,13 or 15;R is CH3Or H;Polymer viscosity average molecular weigh is
100~9,000,000.
2. a kind of preparation method of hydrophobically modified dissaving polymer as described in claim 1, which is characterized in that the preparation side
Method includes the following steps:
(1) acrylamide, acrylic acid, 2- acrylamide-2-methyl propane sulfonics and hyperbranched modified list are added in deionized water
Body stirs evenly, and it is 7 to adjust pH value with sodium hydroxide, adds thin N- benzyls-N- alkyl (methyl) acrylamide and surface is lived
Property agent lauryl sodium sulfate, magnetic agitation to solution clear;
(2) logical inert gas removes the dissolved oxygen in water 15 minutes;
(3) photoinitiator is added, reaction system is placed under light-initiated device and is reacted 3~5 hours, reaction temperature is 10~30
DEG C, obtain white colloidal, as hydrophobically modified dissaving polymer.
3. preparation method as claimed in claim 2, which is characterized in that the photoinitiator is azo-bis-isobutyrate hydrochloride
(v50) or 2- hydroxyls -4'- (2- hydroxy ethoxies) -2- methyl phenyl ketones (Irgacure2959).
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Cited By (5)
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CN110437817A (en) * | 2019-08-16 | 2019-11-12 | 中石化石油工程技术服务有限公司 | A kind of multi-functional emulsion-type salt tolerant fracturing fluid and preparation method thereof |
CN110483701A (en) * | 2019-08-27 | 2019-11-22 | 西南石油大学 | A kind of water-soluble ultrabranching reducing thick oil viscosity oil displacement agent and preparation method thereof |
CN110591012A (en) * | 2019-09-09 | 2019-12-20 | 中海石油(中国)有限公司 | Water-soluble hyperbranched polymer thickened oil viscosity reducer and preparation method thereof |
CN110669492A (en) * | 2019-10-14 | 2020-01-10 | 西南石油大学 | Anti-shearing hyperbranched polymer oil-displacing agent and preparation method and application thereof |
CN115386047A (en) * | 2022-07-15 | 2022-11-25 | 北京伸恒能源科技有限公司 | Polymer for high-temperature-resistant saline-water-based fracturing fluid thickening agent of oil-gas well |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110437817A (en) * | 2019-08-16 | 2019-11-12 | 中石化石油工程技术服务有限公司 | A kind of multi-functional emulsion-type salt tolerant fracturing fluid and preparation method thereof |
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CN110483701B (en) * | 2019-08-27 | 2022-04-15 | 西南石油大学 | Water-soluble hyperbranched viscosity-reducing oil displacement agent for heavy oil and preparation method thereof |
CN110591012A (en) * | 2019-09-09 | 2019-12-20 | 中海石油(中国)有限公司 | Water-soluble hyperbranched polymer thickened oil viscosity reducer and preparation method thereof |
CN110591012B (en) * | 2019-09-09 | 2021-09-21 | 中海石油(中国)有限公司 | Water-soluble hyperbranched polymer thickened oil viscosity reducer and preparation method thereof |
CN110669492A (en) * | 2019-10-14 | 2020-01-10 | 西南石油大学 | Anti-shearing hyperbranched polymer oil-displacing agent and preparation method and application thereof |
CN115386047A (en) * | 2022-07-15 | 2022-11-25 | 北京伸恒能源科技有限公司 | Polymer for high-temperature-resistant saline-water-based fracturing fluid thickening agent of oil-gas well |
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