CN110218278A - A kind of oil well polyacrylamide and preparation method thereof - Google Patents
A kind of oil well polyacrylamide and preparation method thereof Download PDFInfo
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- CN110218278A CN110218278A CN201910554109.2A CN201910554109A CN110218278A CN 110218278 A CN110218278 A CN 110218278A CN 201910554109 A CN201910554109 A CN 201910554109A CN 110218278 A CN110218278 A CN 110218278A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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Abstract
The present invention relates to a kind of oil well polyacrylamide, the structural formulas of the polyacrylamide are as follows:Wherein, the polyacrylamide is alternate copolymer, x, y, z, w are monomer polymerization degree, and x:y:z:w=(60-70): (12-16): (6-8): (6-8), the molecular weight of the polyacrylamide are 11,000,000~14,000,000.The Molecular Weight for Polyacrylamide is big, has excellent heatproof, salt resistance and anti-shear performance；The substance is white solid, easily transports, is easy to maintain, being easy to oil well sample introduction.
Description
Technical field
The invention belongs to technical field of petroleum extraction, and in particular to a kind of oil well polyacrylamide and preparation method thereof.
Background technique
China is consumption of petroleum big country and oil-poor big country, enters the middle and later periods with recovering the oil, flushing makes water injection profile
Extremely uneven, some block injection water is along high permeability zone hasty breaching, so that stratum heterogeneity further expansion, causes oil well
A large amount of water outlets are asked so that a large amount of oil residual can not exploit in the earth formation therefore, it is necessary to carry out water-blocking operation to it and just can solve
Topic, blocks these high permeability zones, can keep stratum energy, the sweep efficiency of injection water is improved, to make the recovery ratio of crude oil
It is improved, to avoid the unnecessary wasting of resources.
The non-selective water-based cements of external early application are as water shutoff agent, later using crude oil, the oil-water emulsion of hydrophobic
The alternatively property blocking agent such as liquid, oil based cement.In the 1950s, the oil-water emulsion of field use crude oil, viscous oil, hydrophobic
Liquid, solid hydrocarbons solution and water dispenser cement etc. are used as water shutoff agent.Period, the former Soviet Union have also been attempted tert-butyl phenol, formaldehyde synthetic resin,
The chemical agents such as urea-formaldehyde resin can not finally meet industrial requirement although playing certain effect.From 70 years
Dai Qi, polyacrylamide high molecular polymer techniques of chemical water plugging open the new situation, and various blocking agent kinds increase sharply, place
Reason well increases, and economic benefit also significantly improves.Wherein the western countries based on the U.S. start development polymerization species water shutoff agent,
The research of chemical water shutoff in oilfield agent is set to enter a new stage.The eighties, the U.S. and the former Soviet Union are all proposed a batch
Novel chemical water shutoff agent.The U.S. selects based on polyacrylamide gel-type blocking agent, and the former Soviet Union is then with polyacrylonitrile-formaldehyde
For host agent, China's emphasis is furtherd investigate based on polyacrylamide and achieves progress.In recent decades, water-soluble polymer
Class blocking agent is widely used, and external many experts carry out the selection of the mechanism of water blockoff, the sealing characteristics of blocking agent and blocking agent
Research.After 2000, for the deep profile controlling of reservoir engineering, using the polyacrylamide (HPAM) of partial hydrolysis as chemical flooding
One kind of finish, two class oil reservoirs available reserves reduce rapidly, three classes high temperature and high salt oil deposit will be that domestic and international oil field will increase from now on
Store up the main making & breaking of volume increase.But HPAM is since salt tolerant cannot not because high temperature issues raw hydrolysis for the ester group on strand
Fully meet the requirement that recovery ratio is improved in high temperature and high salinity oil field.Therefore developing temperature-resistant anti-salt Polymer Used For Oil Displacement is mesh
The main direction of the high oil recovery factor of premise.
Summary of the invention
The purpose of the present invention is to provide a kind of oil well polyacrylamide, there is excellent heatproof, salt resistance and anti-shearing
Performance.
The object of the invention is also to provide a kind of preparation methods of oil well polyacrylamide.
To achieve the above object, the present invention provides a kind of oil well polyacrylamide, the structural formula of the polyacrylamide
Are as follows:
Wherein, the polyacrylamide be alternate copolymer, x, y, z, w be monomer polymerization degree, x:y:z:w=(60~
70): (12~16): (6~8): (6~8), the molecular weight of the polyacrylamide are 11,000,000~14,000,000.
To achieve the above object, the present invention also provides a kind of preparation methods of oil well polyacrylamide, including following step
It is rapid:
Acrylamide, 2- acrylamide-2-methyl propane sulfonic and talan are placed in polymeric kettle by S1, and distillation is added
Then water stirring and dissolving is added lye and adjusts pH value of solution to 8~10, hydroxyethyl methacrylate, ethylenediamine tetrem is then added
Acid, azo-bis-isobutyrate hydrochloride and urea, stir evenly；Wherein, acrylamide, 2- acrylamide-2-methyl propane sulfonic and
The mass ratio of talan is (6~7): (6~8): the solid-liquid ratio of (6~8), acrylamide and distilled water is (0.3~0.4) g:
(90~110) mL；The additional amount of hydroxyethyl methacrylate is acrylamide, 2- acrylamide-2-methyl propane sulfonic, hexichol second
The 0.6~0.8% of alkene and distilled water gross mass；The additional amount of EDTA and AIBA is acrylamide, 2- acrylamide -2- methyl
Propane sulfonic acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.01~0.02%；The additional amount of urea is third
Acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan, distilled water and hydroxyethyl methacrylate gross mass 0.01
~0.03%；
Redox initiator initiation reaction is added under nitrogen protection in S2, control system initial temperature；Redox
The mass ratio of Oxidizing and Reducing Agents and azo-bis-isobutyrate hydrochloride is (1~2): (2~3): (1~2) in initiator；And
S3, in confined conditions, 3~5h of isothermal reaction under initial temperature, the reaction was continued 3~5h after then heating up.
Further, the lye is the sodium hydroxide solution that mass fraction is 20~30%.
Further, system initial temperature is 20~30 DEG C in the S2.
Further, in the S2, before redox initiator is added, it is passed through 30~40min of nitrogen.
Further, in the S2, after redox initiator is added, it is passed through 10~20min. of nitrogen
Further, oxidant is ammonium persulfate in redox initiator, and reducing agent is sodium formaldehyde sulphoxylate.
Further, the S3 is 20~30 DEG C of 3~5h of isothermal reaction in confined conditions, then 35~50 DEG C of continuation
React 3~5h.
Beneficial effects of the present invention: the oil well Molecular Weight for Polyacrylamide is big, has excellent heatproof, salt resistance, shearing resistance
Cut performance and sealing characteristics；The substance is white solid, easily transports, is easy to maintain, being easy to oil well sample introduction.
Detailed description of the invention
Fig. 1 is the sealing characteristics schematic diagram at different temperatures of polyacrylamide prepared by the embodiment of the present invention 1.
Specific embodiment
In order to which technical problems, technical solutions and advantages to be solved are more clearly understood, tie below
Embodiment is closed, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to solve
The present invention is released, is not intended to limit the present invention.
A kind of oil well polyacrylamide, the structural formula of the polyacrylamide are as follows:
Wherein, the polyacrylamide be alternate copolymer, x, y, z, w be monomer polymerization degree, x:y:z:w=(60~
70): (12~16): (6~8): (6~8), the molecular weight of the polyacrylamide are 11,000,000~14,000,000.
The polymer not only has the characteristic feature of polyacrylamide, such as adsorbing metal ions, the impurity in the waste water that flocculates
Deng, and introducing sulfonic group, phenyl ring and ester group, molecular weight are big, and modified polyacrylamide is made to achieve the effect that qualitative modification,
Heatproof, salt resistance and the anti-shear performance for improving polyacrylamide, improve the application range of polyacrylamide.
A kind of preparation method of oil well polyacrylamide, comprising the following steps:
Acrylamide, 2- acrylamide-2-methyl propane sulfonic and talan are placed in polymeric kettle by S1, and distillation is added
Then water stirring and dissolving is added lye and adjusts pH value of solution to 8~10, hydroxyethyl methacrylate, ethylenediamine tetrem is then added
Acid, azo-bis-isobutyrate hydrochloride and urea, stir evenly；Wherein, acrylamide, 2- acrylamide-2-methyl propane sulfonic and
The mass ratio of talan is (6~7): (6~8): the solid-liquid ratio of (6~8), acrylamide and distilled water is (0.3~0.4) g:
(90~110) mL；The additional amount of hydroxyethyl methacrylate is acrylamide, 2- acrylamide-2-methyl propane sulfonic, hexichol second
The 0.6~0.8% of alkene and distilled water gross mass；The additional amount of EDTA and AIBA is acrylamide, 2- acrylamide -2- methyl
Propane sulfonic acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.01~0.02%；The additional amount of urea is third
Acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan, distilled water and hydroxyethyl methacrylate gross mass 0.01
~0.03%；
Redox initiator initiation reaction is added under nitrogen protection in S2, control system initial temperature；Redox
The mass ratio of Oxidizing and Reducing Agents and azo-bis-isobutyrate hydrochloride is (1~2): (2~3): (1~2) in initiator；And
S3, in confined conditions, 3~5h of isothermal reaction under initial temperature, the reaction was continued 3~5h after then heating up.
The lye is the sodium hydroxide solution that mass fraction is 20~30%.
System initial temperature is 20~30 DEG C in the S2.
In the S2, before redox initiator is added, it is passed through 30~40min of nitrogen.
In the S2, after redox initiator is added, it is passed through 10~20min. of nitrogen
Oxidant is ammonium persulfate in redox initiator, and reducing agent is sodium formaldehyde sulphoxylate.
The S3 is 20~30 DEG C of 3~5h of isothermal reaction in confined conditions, then 35~50 DEG C of the reaction was continued 3~5h.
The above method is with acrylamide (AM), sodium styrene sulfonate (AMPS), talan and hydroxyethyl methacrylate
It (HEMA) is monomer, using redox (ammonium persulfate-sodium formaldehyde sulphoxylate)+water-soluble azo (two NSC 18620 of azo
Hydrochloride, AIBA) composite initiation system, obtain Novel oil well polyacrylamide.
Embodiment 1
65:7:7 mixing acrylamide, AMPS and talan in mass ratio add distilled water, distilled water and acryloyl
Amine solid-liquid ratio is 0.3g:100mL, and stirring is sufficiently dissolved to acrylamide, AMPS and talan, obtains mixed solution A；Pass through
The sodium hydroxide solution that mass fraction is 20% adjusts the pH value of mixed solution A to 9, and hydroxyethyl methacrylate is then added
(HEMA), the additional amount of hydroxyethyl methacrylate be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan and
The 0.6% of distilled water gross mass, and stir evenly, obtain mixed solution B.A certain amount of EDTA, AIBA and urea are added to
In mixed solution B, the additional amount of EDTA, AIBA and urea is acrylamide, 2- acrylamide-2-methyl propane sulfonic, hexichol
The 0.01% of ethylene, distilled water and hydroxyethyl methacrylate gross mass；, obtain mixed solution C.Control mixed solution C temperature
At 20 DEG C, it is passed through nitrogen 30min, after ammonium persulfate and sodium formaldehyde sulphoxylate then is added in mixed solution, leads to nitrogen
The mass ratio of 10min, ammonium persulfate and sodium formaldehyde sulphoxylate and azo-initiator AIBA are 1.5:2.5:1.5, are obtained
Mixed solution D.40 DEG C will be risen to after the closed constant temperature 3h of mixed solution the reaction was continued 3h, obtains gum-like product E.Gum-like product E warp
Dry, crushing obtains white product, as Novel oil well polyacrylamide.
Embodiment 2
60:8:8 mixing acrylamide, AMPS and talan in mass ratio add distilled water, distilled water and acryloyl
Amine solid-liquid ratio is 0.3g:110mL, and stirring is sufficiently dissolved to acrylamide, AMPS and talan, obtains mixed solution A；Pass through
The sodium hydroxide solution that mass fraction is 30% adjusts the pH value of mixed solution A to 8, and hydroxyethyl methacrylate is then added
(HEMA), the additional amount of hydroxyethyl methacrylate be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan and
The 0.8% of distilled water gross mass, and stir evenly, obtain mixed solution B.A certain amount of EDTA, AIBA and urea are added to
In mixed solution B, the additional amount of EDTA and AIBA be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan,
The 0.01% of distilled water and hydroxyethyl methacrylate gross mass；The additional amount of urea is acrylamide, 2- acrylamide -2- first
Base propane sulfonic acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.03%, obtain mixed solution C.Control is mixed
Solution C temperature is closed at 30 DEG C, is passed through nitrogen 40min, ammonium persulfate is then added in mixed solution and formaldehyde closes bisulphite
After sodium, the mass ratio for leading to nitrogen 20min, ammonium persulfate and sodium formaldehyde sulphoxylate and azo-initiator AIBA is 1:1:1,
Obtain mixed solution D.40 DEG C will be risen to after the closed constant temperature 5h of mixed solution the reaction was continued 5h, obtains gum-like product E.Gum-like product
E obtains white product, as Novel oil well polyacrylamide through drying, crushing.
Embodiment 3
60:6:6 mixing acrylamide, AMPS and talan in mass ratio add distilled water, distilled water and acryloyl
Amine solid-liquid ratio is 0.3g:90mL, and stirring is sufficiently dissolved to acrylamide, AMPS and talan, obtains mixed solution A；Pass through
The sodium hydroxide solution that mass fraction is 25% adjusts the pH value of mixed solution A to 10, and hydroxyethyl methacrylate is then added
(HEMA), the additional amount of hydroxyethyl methacrylate be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan and
The 0.8% of distilled water gross mass, and stir evenly, obtain mixed solution B.A certain amount of EDTA, AIBA and urea are added to
In mixed solution B, the additional amount of EDTA and AIBA be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan,
The 0.02% of distilled water and hydroxyethyl methacrylate gross mass；The additional amount of urea is acrylamide, 2- acrylamide -2- first
Base propane sulfonic acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.03%, obtain mixed solution C.Control is mixed
Solution C temperature is closed at 30 DEG C, is passed through nitrogen 40min, ammonium persulfate is then added in mixed solution and formaldehyde closes bisulphite
After sodium, the mass ratio for leading to nitrogen 20min, ammonium persulfate and sodium formaldehyde sulphoxylate and azo-initiator AIBA is 2:3:2,
Obtain mixed solution D.50 DEG C will be risen to after the closed constant temperature 4h of mixed solution the reaction was continued 4h, obtains gum-like product E.Gum-like product
E obtains white product, as Novel oil well polyacrylamide through drying, crushing.
Embodiment 4
70:7.3:7.3 mixing acrylamide, AMPS and talan in mass ratio add distilled water, distilled water and third
Acrylamide solid-liquid ratio is 0.4g:95mL, and stirring is sufficiently dissolved to acrylamide, AMPS and talan, obtains mixed solution A；
The sodium hydroxide solution for being 27% by mass fraction adjusts the pH value of mixed solution A to 10, and hydroxyethyl methacrylate is then added
Ethyl ester (HEMA), the additional amount of hydroxyethyl methacrylate are acrylamide, 2- acrylamide-2-methyl propane sulfonic, hexichol second
The 0.77% of alkene and distilled water gross mass, and stir evenly, obtain mixed solution B.A certain amount of EDTA, AIBA and urea are added
Enter into mixed solution B, the additional amount of EDTA, AIBA and urea be acrylamide, 2- acrylamide-2-methyl propane sulfonic,
The 0.02% of talan, distilled water and hydroxyethyl methacrylate gross mass, obtains mixed solution C.Control mixed solution C temperature
Degree is passed through nitrogen 30min at 20 DEG C, after ammonium persulfate and sodium formaldehyde sulphoxylate then is added in mixed solution, leads to nitrogen
The mass ratio of gas 10min, ammonium persulfate and sodium formaldehyde sulphoxylate and azo-initiator AIBA are 1.2:3:1.2, are obtained
Mixed solution D.40 DEG C will be risen to after the closed constant temperature 4h of mixed solution the reaction was continued 4h, obtains gum-like product E.Gum-like product E warp
Dry, crushing obtains white product, as Novel oil well polyacrylamide.
Embodiment 5
65:6:6 mixing acrylamide, AMPS and talan in mass ratio add distilled water, distilled water and acryloyl
Amine solid-liquid ratio is 0.3g:110mL, and stirring is sufficiently dissolved to acrylamide, AMPS and talan, obtains mixed solution A；Pass through
The sodium hydroxide solution that mass fraction is 23% adjusts the pH value of mixed solution A to 8, and hydroxyethyl methacrylate is then added
(HEMA), the additional amount of hydroxyethyl methacrylate be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan and
The 0.7% of distilled water gross mass, and stir evenly, obtain mixed solution B.A certain amount of EDTA, AIBA and urea are added to
In mixed solution B, the additional amount of EDTA and AIBA be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan,
The 0.01% of distilled water and hydroxyethyl methacrylate gross mass；The additional amount of urea is acrylamide, 2- acrylamide -2- first
Base propane sulfonic acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.02%, obtain mixed solution C.Control is mixed
Solution C temperature is closed at 30 DEG C, is passed through nitrogen 40min, ammonium persulfate is then added in mixed solution and formaldehyde closes bisulphite
After sodium, the mass ratio for leading to nitrogen 20min, ammonium persulfate and sodium formaldehyde sulphoxylate and azo-initiator AIBA is 1:2.5:
1, obtain mixed solution D.48 DEG C will be risen to after the closed constant temperature 5h of mixed solution the reaction was continued 5h, obtains gum-like product E.Glue produces
Object E obtains white product, as Novel oil well polyacrylamide through drying, crushing.
Embodiment 6
70:8:8 mixing acrylamide, AMPS and talan in mass ratio add distilled water, distilled water and acryloyl
Amine solid-liquid ratio is 0.4g:110mL, and stirring is sufficiently dissolved to acrylamide, AMPS and talan, obtains mixed solution A；Pass through
The sodium hydroxide solution that mass fraction is 28% adjusts the pH value of mixed solution A to 9, and hydroxyethyl methacrylate is then added
(HEMA), the additional amount of hydroxyethyl methacrylate be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan and
The 0.7% of distilled water gross mass, and stir evenly, obtain mixed solution B.A certain amount of EDTA, AIBA and urea are added to
In mixed solution B, the additional amount of EDTA be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan, distilled water and
The 0.01% of hydroxyethyl methacrylate gross mass；The additional amount of AIBA and urea is acrylamide, 2- acrylamide -2- first
Base propane sulfonic acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.02%, obtain mixed solution C.Control is mixed
Solution C temperature is closed at 20 DEG C, is passed through nitrogen 30min, ammonium persulfate is then added in mixed solution and formaldehyde closes bisulphite
After sodium, the mass ratio for leading to nitrogen 10min, ammonium persulfate and sodium formaldehyde sulphoxylate and azo-initiator AIBA is 2:3:2,
Obtain mixed solution D.30 DEG C will be risen to after the closed constant temperature 3h of mixed solution the reaction was continued 3h, obtains gum-like product E.Gum-like product
E obtains white product, as Novel oil well polyacrylamide through drying, crushing.
Embodiment 7
60:7.2:7.2 mixing acrylamide, AMPS and talan in mass ratio add distilled water, distilled water and third
Acrylamide solid-liquid ratio is 0.3g:102mL, and stirring is sufficiently dissolved to acrylamide, AMPS and talan, obtains mixed solution A；
The sodium hydroxide solution for being 25% by mass fraction adjusts the pH value of mixed solution A to 10, and hydroxyethyl methacrylate is then added
Ethyl ester (HEMA), the additional amount of hydroxyethyl methacrylate are acrylamide, 2- acrylamide-2-methyl propane sulfonic, hexichol second
The 0.7% of alkene and distilled water gross mass, and stir evenly, obtain mixed solution B.A certain amount of EDTA, AIBA and urea are added
Enter into mixed solution B, the additional amount of EDTA and AIBA are acrylamide, 2- acrylamide-2-methyl propane sulfonic, hexichol second
The 0.02% of alkene, distilled water and hydroxyethyl methacrylate gross mass；The additional amount of urea is acrylamide, 2- acrylamide-
2- methyl propane sulfonic acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.03%, obtain mixed solution C.Control
Mixed solution C temperature processed is passed through nitrogen 40min at 30 DEG C, and ammonium persulfate is then added in mixed solution and formaldehyde closes time sulphur
After sour hydrogen sodium, lead to nitrogen 20min, the mass ratio of ammonium persulfate and sodium formaldehyde sulphoxylate and azo-initiator AIBA is
1.5:2:1.5 obtains mixed solution D.50 DEG C will be risen to after the closed constant temperature 5h of mixed solution the reaction was continued 5h, obtains gum-like product
E.Gum-like product E obtains white product, as Novel oil well polyacrylamide through drying, crushing.
Embodiment 8
70:6:6 mixing acrylamide, AMPS and talan in mass ratio add distilled water, distilled water and acryloyl
Amine solid-liquid ratio is 0.4g:90mL, and stirring is sufficiently dissolved to acrylamide, AMPS and talan, obtains mixed solution A；Pass through
The sodium hydroxide solution that mass fraction is 20% adjusts the pH value of mixed solution A to 8, and hydroxyethyl methacrylate is then added
(HEMA), the additional amount of hydroxyethyl methacrylate be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan and
The 0.6% of distilled water gross mass, and stir evenly, obtain mixed solution B.A certain amount of EDTA, AIBA and urea are added to
In mixed solution B, the additional amount of EDTA and AIBA be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan,
The 0.01% of distilled water and hydroxyethyl methacrylate gross mass；The additional amount of urea is acrylamide, 2- acrylamide -2- first
Base propane sulfonic acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.02%, obtain mixed solution C.Control is mixed
Solution C temperature is closed at 25 DEG C, is passed through nitrogen 35min, ammonium persulfate is then added in mixed solution and formaldehyde closes bisulphite
After sodium, the mass ratio for leading to nitrogen 15min, ammonium persulfate and sodium formaldehyde sulphoxylate and azo-initiator AIBA is 1:3:1,
Obtain mixed solution D.40 DEG C will be risen to after the closed constant temperature 4h of mixed solution the reaction was continued 4h, obtains gum-like product E.Gum-like product
E obtains white product, as Novel oil well polyacrylamide through drying, crushing.
Embodiment 9
70:7.8:7.8 mixing acrylamide, AMPS and talan in mass ratio add distilled water, distilled water and third
Acrylamide solid-liquid ratio is 0.4g:107mL, and stirring is sufficiently dissolved to acrylamide, AMPS and talan, obtains mixed solution A；
Hydroxyethyl methacrylate second is then added to 9 in the pH value for adjusting mixed solution A by the sodium hydroxide solution that mass fraction is 30%
Ester (HEMA), the additional amount of hydroxyethyl methacrylate are acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan
It with the 0.7% of distilled water gross mass, and stirs evenly, obtains mixed solution B.A certain amount of EDTA, AIBA and urea are added
Into mixed solution B, the additional amount of EDTA and AIBA are acrylamide, 2- acrylamide-2-methyl propane sulfonic, hexichol second
The 0.02% of alkene, distilled water and hydroxyethyl methacrylate gross mass；The additional amount of urea is acrylamide, 2- acrylamide-
2- methyl propane sulfonic acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.03%, obtain mixed solution C.Control
Mixed solution C temperature processed is passed through nitrogen 35min at 25 DEG C, and ammonium persulfate is then added in mixed solution and formaldehyde closes time sulphur
After sour hydrogen sodium, lead to nitrogen 15min, the mass ratio of ammonium persulfate and sodium formaldehyde sulphoxylate and azo-initiator AIBA is
1.8:3:1.8 obtains mixed solution D.30 DEG C will be risen to after the closed constant temperature 4h of mixed solution the reaction was continued 4h, obtains gum-like product
E.Gum-like product E obtains white product, as Novel oil well polyacrylamide through drying, crushing.
Embodiment 10
70:8:8 mixing acrylamide, AMPS and talan in mass ratio add distilled water, distilled water and acryloyl
Amine solid-liquid ratio is 0.4g:110mL, and stirring is sufficiently dissolved to acrylamide, AMPS and talan, obtains mixed solution A；Pass through
The sodium hydroxide solution that mass fraction is 25% adjusts the pH value of mixed solution A to 9, and hydroxyethyl methacrylate is then added
(HEMA), the additional amount of hydroxyethyl methacrylate be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan and
The 0.7% of distilled water gross mass, and stir evenly, obtain mixed solution B.A certain amount of EDTA, AIBA and urea are added to
In mixed solution B, the additional amount of EDTA and AIBA be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan,
The 0.02% of distilled water and hydroxyethyl methacrylate gross mass；The additional amount of urea is acrylamide, 2- acrylamide -2- first
Base propane sulfonic acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.03%, obtain mixed solution C.Control is mixed
Solution C temperature is closed at 22 DEG C, is passed through nitrogen 33min, ammonium persulfate is then added in mixed solution and formaldehyde closes bisulphite
After sodium, the mass ratio for leading to nitrogen 15min, ammonium persulfate and sodium formaldehyde sulphoxylate and azo-initiator AIBA is 2:3:2,
Obtain mixed solution D.50 DEG C will be risen to after the closed constant temperature 3h of mixed solution the reaction was continued 3h, obtains gum-like product E.Gum-like product
E obtains white product, as Novel oil well polyacrylamide through drying, crushing.
The heat and salt resistance and sealing ratiod of obtained polyacrylamide are evaluated.Evaluation method is as follows:
Temperature tolerance test: the gum-like product thermostatic curing at 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C and 100 DEG C respectively will be obtained
Then 48h tests its viscosity respectively.Each embodiment heat resistance is shown in Table 1.
Salt-resistance test: being respectively 1000mg/L, 2000mg/L, 4000mg/L, 10000mg/ with salinity at 70 DEG C
L, the salinity water of 20000mg/L, 30000mg/L, 40000mg/L dissolve gum-like product, then test its viscosity, salinity water
Mass ratio with gum-like product is 1:2.Each embodiment anti-salt property is shown in Table 2.
Sealing ratiod test: gum-like product, salinity water and gluey production are dissolved with the salinity water that salinity is 5000mg/L
The mass ratio of object is 5:1, is configured to solution, under 9.71MPa pressure, solution is injected rock core, thermostatic curing 48h at 70 DEG C.
Each embodiment sealing characteristics is shown in Table 3.
Table 1
Table 2
Table 3
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (8)
1. a kind of oil well polyacrylamide, which is characterized in that the structural formula of the polyacrylamide are as follows:
Wherein, the polyacrylamide be alternate copolymer, x, y, z, w be monomer polymerization degree, x:y:z:w=(60~70): (12
~16): (6~8): (6~8), the molecular weight of the polyacrylamide are 11,000,000~14,000,000.
2. the preparation method of oil well polyacrylamide described in claim 1, which comprises the following steps:
Acrylamide, 2- acrylamide-2-methyl propane sulfonic and talan are placed in polymeric kettle by S1, and distilled water is added and stirs
Dissolution is mixed, lye is then added and adjusts pH value of solution to 8~10, hydroxyethyl methacrylate, ethylenediamine tetra-acetic acid, idol is then added
Two NSC 18620 hydrochloride of nitrogen and urea, stir evenly；Wherein, acrylamide, 2- acrylamide-2-methyl propane sulfonic and hexichol second
The mass ratio of alkene is (6~7): (6~8): the solid-liquid ratio of (6~8), acrylamide and distilled water be (0.3~0.4) g:(90~
110)mL；The additional amount of hydroxyethyl methacrylate be acrylamide, 2- acrylamide-2-methyl propane sulfonic, talan and
The 0.6~0.8% of distilled water gross mass；The additional amount of EDTA and AIBA is acrylamide, 2- acrylamide -2- methyl-prop sulphur
Acid, talan, distilled water and hydroxyethyl methacrylate gross mass 0.01~0.02%；The additional amount of urea is acryloyl
Amine, 2- acrylamide-2-methyl propane sulfonic, talan, distilled water and hydroxyethyl methacrylate gross mass 0.01~
0.03%；
Redox initiator initiation reaction is added under nitrogen protection in S2, control system initial temperature；Redox Initiator
The mass ratio of Oxidizing and Reducing Agents and azo-bis-isobutyrate hydrochloride is (1:2): (2~3): (1~2) in agent；And
S3, in confined conditions, 3~5h of isothermal reaction under initial temperature, the reaction was continued 3~5h after then heating up.
3. the preparation method of oil well polyacrylamide according to claim 2, which is characterized in that the lye is quality
The sodium hydroxide solution that score is 20~30%.
4. the preparation method of oil well polyacrylamide according to claim 2, which is characterized in that in the S2 at the beginning of system
Beginning temperature is 20~30 DEG C.
5. the preparation method of oil well polyacrylamide according to claim 2, which is characterized in that in the S2, adding
Before entering redox initiator, it is passed through 30~40min of nitrogen.
6. the preparation method of oil well polyacrylamide according to claim 2, which is characterized in that in the S2, adding
After entering redox initiator, it is passed through 10~20min of nitrogen.
7. the preparation method of oil well polyacrylamide according to claim 2, which is characterized in that redox initiator
Middle oxidant is ammonium persulfate, and reducing agent is sodium formaldehyde sulphoxylate.
8. the preparation method of oil well polyacrylamide according to claim 2, which is characterized in that the S3 is closed
Under the conditions of, 20~30 DEG C of 3~5h of isothermal reaction, then 35~50 DEG C of the reaction was continued 3~5h.
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| CN110590993A (en) * | 2019-06-25 | 2019-12-20 | 河北科技大学 | Polyacrylamide for oil well and preparation method thereof |
| CN111892682A (en) * | 2020-07-22 | 2020-11-06 | 天津博弘化工有限责任公司 | Small-molecule salt-resistant polymer and preparation method thereof |
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| CN108530579A (en) * | 2018-03-05 | 2018-09-14 | 东北石油大学 | A kind of functional form polymer and preparation method thereof |
| CN110218278A (en) * | 2019-06-25 | 2019-09-10 | 河北科技大学 | A kind of oil well polyacrylamide and preparation method thereof |
| CN110283276A (en) * | 2019-06-28 | 2019-09-27 | 河北科技大学 | A kind of oil well polyacrylamide and preparation method thereof |
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| CN111892682A (en) * | 2020-07-22 | 2020-11-06 | 天津博弘化工有限责任公司 | Small-molecule salt-resistant polymer and preparation method thereof |
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