CN111675787A - Preparation method of post-hydrolyzed ultra-high molecular weight comb-shaped polyacrylamide - Google Patents
Preparation method of post-hydrolyzed ultra-high molecular weight comb-shaped polyacrylamide Download PDFInfo
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Abstract
The invention discloses a preparation method of post-hydrolyzed ultra-high molecular weight comb polyacrylamide, which comprises the following steps: s1: dissolving 20-25% of acrylamide in 70-77.5% of distilled water by mass percent, adding 2.5-5% of a functional side group mixed monomer consisting of N-triethyl- (4-vinyl benzyl) ammonium chloride, sodium styrene sulfonate, N-methyl maleimide and 4-hydroxybutyl vinyl polyoxyethylene ether, and performing ultrasonic dispersion to obtain a mixed solution; s2: cooling the mixed solution to 0-5 ℃, adding a complexing agent, stirring for 0.5-1 h, introducing nitrogen to drive out oxygen, adding a chain transfer agent, adding an initiator to initiate polymerization reaction under the condition of continuously introducing nitrogen, and sealing for reaction for 3-8 h; s3: post-hydrolysis; s4: oven drying, pulverizing, and sieving. The polyacrylamide prepared by the method is in a rigid comb-shaped structure, and the molecular side chains repel each other, so that the high-temperature resistance, salt resistance and shear resistance of the polyacrylamide are effectively improved, and the polyacrylamide can be used as an ideal oil displacement agent for high-salt high-temperature stratums of oil fields.
Description
Technical Field
The invention belongs to the field of functional polymers, and particularly relates to a preparation method of post-hydrolyzed ultrahigh molecular weight high temperature resistant comb-shaped polyacrylamide, wherein hydrophilic oleophilic rigid side groups are introduced, so that the tackifying performance of polyacrylic acid under the conditions of high salinity and high temperature can be effectively improved.
Background
At present, the ultrahigh molecular weight partially hydrolyzed polyacrylamide is a polymer which is most widely applied in the process of improving the recovery ratio of crude oil, and is mainly prepared by hydrolyzing polyacrylamide in an alkaline environment or copolymerizing acrylamide and sodium acrylate. The molecular weight of the polyacrylamide with the ultrahigh relative molecular mass reaches more than 2500 ten thousand, and the polyacrylamide has larger molecular hydrodynamic volume, so that the solution has higher initial viscosity and residual viscosity, but because the polyacrylamide with the ultrahigh relative molecular mass is generally in a straight-chain structure, the molecular chain structure of the polyacrylamide is unstable and is easy to break or intertwine under the high shear condition, the viscosity and viscoelasticity are reduced rapidly, the water-oil flow rate ratio is reduced, the polymer flooding effect is influenced finally, in addition, the problem of difficult dissolution is caused along with the increase of the molecular weight, and the high-temperature and high-salt resistance of the polyacrylamide with the ultrahigh relative molecular mass still needs to be further improved.
Based on the above, the hydrophobic association rigid comb-shaped polyacrylamide is formed by polymerizing the rigid monomer containing the hydrophilic and lipophilic groups and acrylamide, so that the rigidity and structural stability of a molecular main chain are effectively improved, the shear resistance, high temperature resistance and salt tolerance of the polyacrylamide are improved, the solubility of the polyacrylamide is improved by introducing a branched chain, the molecular weight of the polyacrylamide is further improved by a post-hydrolysis process, the solubility is adjusted, and the shear resistance, the high temperature resistance and the salt tolerance of the polyacrylamide are further improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of post-hydrolyzed ultra-high molecular weight comb polyacrylamide.
The technical scheme of the invention is summarized as follows:
the invention relates to a preparation method of post-hydrolyzed comb-shaped polyacrylamide with ultrahigh molecular weight more than or equal to 3031 ten thousand, the filtration ratio is less than or equal to 0.98, insoluble substances are less than or equal to 0.17%, the apparent viscosity is more than or equal to 19.4 mPa.s, and the content of residual monomers is less than or equal to 0.036%. The method specifically comprises the following steps:
s1: dissolving 20-25% of acrylamide in 70-77.5% of distilled water by mass percent, adding 2.5-5% of a functional side group mixed monomer, and performing ultrasonic dispersion to obtain a mixed solution;
the functional side group mixed monomer is prepared from N-triethyl- (4-vinyl benzyl) ammonium chloride, sodium styrene sulfonate, N-methyl maleimide and 4-hydroxybutyl vinyl polyoxyethylene ether according to the weight ratio of 1: (0.6-1.2): (0.2-0.4): (0.6-1.2) by mass;
s2: transferring the mixed solution into a reaction container, cooling to 0-5 ℃, adding a complexing agent, stirring for 0.5-1 h, introducing nitrogen to drive out oxygen, adding a chain transfer agent, adding an initiator to initiate polymerization reaction under the condition of continuously introducing nitrogen, and sealing for 3-8 h;
s3: taking out the rubber block prepared by the reaction of S2, shearing, dripping a hydrolytic agent solution, uniformly mixing, and performing sealed hydrolysis for 1-2 h at 75-85 ℃;
s4: and (3) drying, crushing and sieving the hydrolyzed S3 gel block to obtain the ultrahigh molecular weight comb-shaped polyacrylamide.
Preferably, the amount of the complexing agent is 0.001-0.01% of the mass of the acrylamide monomer, and the complexing agent is selected from one or more of ethylenediamine tetraacetic acid, disodium ethylenediamine tetraacetic acid and tetrasodium ethylenediamine tetraacetic acid.
Preferably, the amount of the chain transfer agent is 0.008-0.02% of the mass of the acrylamide monomer, and the chain transfer agent is selected from one or more of sodium formate, isopropanol and dodecyl mercaptan.
Preferably, the amount of the initiator is 0.12-0.2% of the mass of the acrylamide monomer, and the ratio of the oxidant to the reducing agent is 1: (2.5-5) in mass ratio for standby.
Preferably, the oxidant is selected from one or more of ammonium persulfate, sodium persulfate, hydrogen peroxide and ferric chloride.
Preferably, the reducing agent is selected from one or more of sodium bisulfite, sodium metabisulfite and ferrous chloride.
Preferably, the dosage of the hydrolytic agent solution is 16-20% of the mass of the acrylamide monomer, and the hydrolytic agent solution is one selected from 30 wt% sodium hydroxide solution, 30 wt% potassium hydroxide solution and 30 wt% sodium carbonate solution.
The invention has the beneficial effects that:
1. according to the invention, N-triethyl- (4-vinylbenzyl) ammonium chloride, sodium styrene sulfonate, N-methyl maleimide, 4-hydroxybutyl vinyl polyoxyethylene ether and other hydrophilic lipophilic group-containing monomers are copolymerized with acrylamide, and due to mutual repulsion of hydrophilic groups and lipophilic groups in molecular side chains, intramolecular and intermolecular curling and entanglement are avoided, so that a comb-shaped structure with mutually independent molecular side chains is formed, the molecular weight of polyacrylamide is increased, the rigidity and structural stability of the molecular main chains are improved, and the solubility of ultrahigh molecular weight polyacrylamide is ensured, so that the polyacrylamide can be used as an ideal oil displacement agent for high-salt high-temperature strata of oil fields; in addition, N-triethyl- (4-vinylbenzyl) ammonium chloride is a cationic rigid hydrophobic monomer containing a benzene ring, sodium styrene sulfonate is a rigid monomer containing a sulfonated group and a benzene ring (sulfonate ions can react with metal ions to improve salt resistance), N-methyl maleimide is a rigid monomer containing a pyrrole five-membered ring, and is subjected to addition polymerization with acrylamide to form hydrophobically-associated comb-shaped polyacrylamide containing a rigid side group, the three components synergistically improve the rigidity of a polyacrylamide molecular chain, effectively degrade an acrylamide group, further improve the high temperature resistance, salt resistance and shear resistance of the polyacrylamide, and effectively maintain the viscosity of the polyacrylamide.
2. The comb-shaped polyacrylamide is further subjected to post-hydrolysis process treatment, so that the solubility of the polyacrylamide with side chains is effectively improved, the molecular weight and viscosity are increased, and the degree of breakage of the side chains during shearing is reduced.
3. The comb-shaped polyacrylamide prepared by the method has the advantages of high molecular weight, easy dissolution, high viscosity, high temperature resistance, salt resistance and excellent anti-shearing performance.
Drawings
FIG. 1 is a flow chart of the method for preparing post-hydrolyzed ultra-high molecular weight comb polyacrylamide of the present invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
Example one
A preparation method of post-hydrolyzed ultra-high molecular weight comb polyacrylamide comprises the following steps:
s1: preparing a functional side group mixed monomer: according to the following steps of 1: 0.6: 0.2: uniformly mixing N-triethyl- (4-vinylbenzyl) ammonium chloride, sodium styrene sulfonate, N-methylmaleimide and 4-hydroxybutyl vinyl polyoxyethylene ether in a mass ratio of 0.6 to obtain a functional side group mixed monomer;
s2: preparing a redox system initiator: according to the following steps of 1: 2.5, respectively preparing an oxidant ammonium persulfate and a reducing agent sodium bisulfite for later use.
S3: dissolving 125g of acrylamide in 362.5g of distilled water, adding 12.5g of functional side group mixed monomer, and performing ultrasonic dispersion to obtain a mixed solution;
s4: transferring the mixed solution into a reaction container, cooling to 1 ℃, adding 0.003g of complexing agent ethylenediaminetetraacetic acid disodium salt, stirring for 0.5h, introducing high-purity nitrogen (the purity of the nitrogen is more than or equal to 99.99%) to expel oxygen in the system, adding 0.0125g of chain transfer agent sodium formate when the oxygen content of the system is less than 0.01%, continuing introducing the nitrogen, adding 0.043g of ammonium persulfate and 0.107g of sodium bisulfite, initiating a polymerization reaction, and reacting for 6 h;
s5: taking out the rubber block prepared by the reaction, shearing, dripping 20mL of 30% sodium hydroxide solution, mixing uniformly, and sealing and hydrolyzing for 2h at 85 ℃;
s6: and drying the hydrolyzed gel block in an oven, crushing the gel block by a crusher, and sieving the gel block to obtain the ultrahigh molecular weight comb-shaped polyacrylamide.
The polyacrylamide prepared by detecting the polyacrylamide for oil displacement according to the Q/SH 10201572-2017 & ltenterprise standard of China petrochemical group Shengli Petroleum administration-polyacrylamide for oil displacement', and the detection result of the product is as follows:
example two
A preparation method of post-hydrolyzed ultra-high molecular weight comb polyacrylamide comprises the following steps:
s1: preparing a functional side group mixed monomer: according to the following steps of 1: 0.8: 0.3: uniformly mixing N-triethyl- (4-vinylbenzyl) ammonium chloride, sodium styrene sulfonate, N-methylmaleimide and 4-hydroxybutyl vinyl polyoxyethylene ether in a mass ratio of 0.8 to obtain a functional side group mixed monomer;
s2: preparing a redox system initiator: according to the following steps of 1: 2.5, uniformly mixing the oxidant sodium persulfate and the reducing agent sodium metabisulfite to obtain an initiator;
s3: dissolving 115g of acrylamide in 370g of distilled water, adding 15g of functional side group mixed monomer, and performing ultrasonic dispersion to obtain a mixed solution;
s4: transferring the mixed solution into a reaction container, cooling to 1 ℃, adding 0.005g of complexing agent ethylene diamine tetraacetic acid tetrasodium salt, stirring for 0.5h, introducing high-purity nitrogen (the purity of the nitrogen is more than or equal to 99.99%) to expel oxygen in the system, adding 0.015g of dodecanethiol when the oxygen content of the system is less than 0.01%, continuing introducing the nitrogen, adding 0.057g of sodium persulfate and 0.143g of sodium metabisulfite, initiating a polymerization reaction, and reacting for 6 h;
s5: taking out the rubber block prepared by the reaction, shearing, dripping 20mL of 30% potassium hydroxide solution, mixing uniformly, and sealing and hydrolyzing for 2h at 85 ℃;
s6: and drying the hydrolyzed gel block in an oven, crushing the gel block by a crusher, and sieving the gel block to obtain the ultrahigh molecular weight comb-shaped polyacrylamide.
The polyacrylamide prepared by detecting the polyacrylamide for oil displacement according to the Q/SH 10201572-2017 & ltenterprise standard of China petrochemical group Shengli Petroleum administration-polyacrylamide for oil displacement', and the detection result of the product is as follows:
| item | Index (I) | Results |
| Molecular weight (ten thousand) | ≥2400 | 3031 |
| Degree of hydrolysis (%) | 20-30 | 28.61 |
| Apparent viscosity (mPa. s) | ≥12.5 | 20.3 |
| Filtration ratio | ≤2 | 0.98 |
| Insoluble matter (%) | ≤0.2 | 0.14 |
| AM residual amount (%) | ≤0.1 | 0.036 |
EXAMPLE III
A preparation method of post-hydrolyzed ultra-high molecular weight comb polyacrylamide comprises the following steps:
s1: preparing a functional side group mixed monomer: according to the following steps of 1: 1.0: 0.3: 1.0 mass ratio, evenly mixing N-triethyl- (4-vinyl benzyl) ammonium chloride, sodium styrene sulfonate, N-methyl maleimide and 4-hydroxybutyl vinyl polyoxyethylene ether to obtain a functional side group mixed monomer;
s2: preparing a redox system initiator: according to the following steps of 1: 3, uniformly mixing the oxidant ammonium persulfate and the reducing agent sodium metabisulfite in a mass ratio to obtain an initiator;
s3: dissolving 105g of acrylamide in 382.5g of distilled water, adding 12.5g of functional side group mixed monomer, and performing ultrasonic dispersion to obtain a mixed solution;
s4: transferring the mixed solution into a reaction container, cooling to 1 ℃, adding 0.005g of complexing agent ethylene diamine tetraacetic acid disodium salt, stirring for 1h, introducing high-purity nitrogen (the purity of the nitrogen is more than or equal to 99.99%) to expel oxygen in the system, adding 0.015g of chain transfer agent isopropanol when the oxygen content of the system is less than 0.01%, continuing introducing the nitrogen, adding 0.05g of ammonium persulfate and 0.15g of sodium metabisulfite, initiating a polymerization reaction, and reacting for 6 h;
s5: taking out the rubber block prepared by the reaction, shearing, dripping 20mL of 30% potassium hydroxide solution, mixing uniformly, and sealing and hydrolyzing for 2h at 85 ℃;
s6: and drying the hydrolyzed gel block in an oven, crushing the gel block by a crusher, and sieving the gel block to obtain the ultrahigh molecular weight comb-shaped polyacrylamide.
The polyacrylamide prepared by detecting the polyacrylamide for oil displacement according to the Q/SH 10201572-2017 & ltenterprise standard of China petrochemical group Shengli Petroleum administration-polyacrylamide for oil displacement', and the detection result of the product is as follows:
| item | Index (I) | Results |
| Molecular weight (ten thousand) | ≥2400 | 3212.5 |
| Degree of hydrolysis (%) | 20-30 | 29.12 |
| Apparent viscosity (mPa. s) | ≥12.5 | 19.4 |
| Filtration ratio | ≤2 | 0.68 |
| Insoluble matter (%) | ≤0.2 | 0.17 |
| AM residual amount (%) | ≤0.1 | 0.029 |
Example four
A preparation method of post-hydrolyzed ultra-high molecular weight comb polyacrylamide comprises the following steps:
s1: preparing a functional side group mixed monomer: according to the following steps of 1: 1.0: 0.2: uniformly mixing N-triethyl- (4-vinylbenzyl) ammonium chloride, sodium styrene sulfonate, N-methylmaleimide and 4-hydroxybutyl vinyl polyoxyethylene ether in a mass ratio of 0.8 to obtain a functional side group mixed monomer;
s2: preparing a redox system initiator: according to the following steps of 1: 3, uniformly mixing the oxidant and the reducing agent according to the mass ratio to obtain an initiator;
s3: dissolving 115g of acrylamide in 365g of distilled water, adding 20g of functional side group mixed monomer, and performing ultrasonic dispersion to obtain a mixed solution;
s4: transferring the mixed solution into a reaction container, cooling to 1 ℃, adding 0.01g of complexing agent ethylene diamine tetraacetic acid disodium salt, stirring for 1h, introducing high-purity nitrogen (the purity of the nitrogen is more than or equal to 99.99%) to expel oxygen in the system, adding 0.02g of chain transfer agent sodium formate when the oxygen content of the system is less than 0.01%, continuing introducing the nitrogen, adding 0.05g of ammonium persulfate and 0.15g of sodium metabisulfite, initiating a polymerization reaction, and reacting for 6 h;
s5: taking out the rubber block prepared by the reaction, shearing, dripping 20mL of 30% hydrolytic agent solution, mixing uniformly, and sealing and hydrolyzing for 2h at 85 ℃;
s6: and drying the hydrolyzed gel block in an oven, crushing the gel block by a crusher, and sieving the gel block to obtain the ultrahigh molecular weight comb-shaped polyacrylamide.
The polyacrylamide prepared by detecting the polyacrylamide for oil displacement according to the Q/SH 10201572-2017 & ltenterprise standard of China petrochemical group Shengli Petroleum administration-polyacrylamide for oil displacement', and the detection result of the product is as follows:
| item | Index (I) | Results |
| Molecular weight (ten thousand) | ≥2400 | 3318 |
| Degree of hydrolysis (%) | 20-30 | 27.52 |
| Apparent viscosity (mPa. s) | ≥12.5 | 21.6 |
| Filtration ratio | ≤2 | 0.88 |
| Insoluble matter (%) | ≤0.2 | 0.16 |
| AM residual amount (%) | ≤0.1 | 0.033 |
Comparative example one: the difference is the same as the first embodiment: the functional side group mixed monomer does not contain N-triethyl- (4-vinyl benzyl) ammonium chloride.
Comparative example two: the difference is the same as the first embodiment: the functional side group mixed monomer does not contain 4-hydroxybutyl vinyl polyoxyethylene ether.
Comparative example three: the difference is the same as the first embodiment: the functional side group mixed monomer does not contain sodium styrene sulfonate.
Comparative example four: the difference is the same as the first embodiment: no functional side group mixed monomer is added in the process of preparing polyacrylamide.
The polyacrylamide prepared according to the first to fourth comparative examples is detected according to Q/SH 10201572-2017 polyacrylamide for oil displacement used in China petrochemical group Shengli Petroleum administration Enterprise Standard, and the detection results of the product are as follows:
and (3) testing the shearing resistance: the polyacrylamides prepared in comparative examples one-fourth and one-fifth were mixed to 100mg/L aqueous polymer solution, and the apparent viscosity W was measured at 25 ℃ using a Brookfield viscometer1Stirring for 1h by a high-speed stirrer at 1000r/min, and measuring the apparent viscosity W before and after shearing2And according to the formula 100% × W2/W1The viscosity retention was calculated.
High temperature resistance test: the polyacrylamides prepared in examples one-four and comparative examples one-four were mixed to prepare 100mg/L aqueous polymer solution, and the apparent viscosity W was measured at 25 ℃ using a Brookfield viscometer3Heating in 80 deg.C water bath for 1 hr, and measuring apparent viscosity W after heating4And according to the formula 100% × W4/W3The viscosity retention was calculated.
The test results are shown in the following table:
as can be seen from the above table, compared with the comparative example, the invention utilizes the copolymerization and post-hydrolysis processes of monomers containing hydrophilic and lipophilic groups, such as N-triethyl- (4-vinylbenzyl) ammonium chloride, sodium styrene sulfonate, 4-hydroxybutyl vinyl polyoxyethylene ether and the like, and acrylamide to obviously improve the solubility, high temperature resistance and shear resistance of polyacrylamide, and improve the molecular weight of the polyacrylamide.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (8)
1. A preparation method of post-hydrolyzed ultra-high molecular weight comb polyacrylamide is characterized by comprising the following steps:
s1: dissolving 20-25% of acrylamide in 70-77.5% of distilled water by mass percent, adding 2.5-5% of a functional side group mixed monomer, and performing ultrasonic dispersion to obtain a mixed solution;
the functional side group mixed monomer is prepared from N-triethyl- (4-vinyl benzyl) ammonium chloride, sodium styrene sulfonate, N-methyl maleimide and 4-hydroxybutyl vinyl polyoxyethylene ether according to the weight ratio of 1: (0.6-1.2): (0.2-0.4): (0.6-1.2) by mass;
s2: transferring the mixed solution into a reaction container, cooling to 0-5 ℃, adding a complexing agent, stirring for 0.5-1 h, introducing nitrogen to drive out oxygen, adding a chain transfer agent, adding an initiator to initiate polymerization reaction under the condition of continuously introducing nitrogen, and sealing for 3-8 h;
s3: taking out the rubber block prepared by the reaction of S2, shearing, dripping a hydrolytic agent solution, uniformly mixing, and performing sealed hydrolysis for 1-2 h at 75-85 ℃;
s4: and (3) drying, crushing and sieving the hydrolyzed S3 gel block to obtain the ultrahigh molecular weight comb-shaped polyacrylamide.
2. The method of claim 1 wherein said post-hydrolyzed ultra-high molecular weight comb polyacrylamide is prepared by: the amount of the complexing agent is 0.001-0.01% of the mass of the acrylamide monomer, and the complexing agent is selected from one or more of ethylenediamine tetraacetic acid, disodium ethylenediamine tetraacetic acid and tetrasodium ethylenediamine tetraacetic acid.
3. The method of claim 1 wherein said post-hydrolyzed ultra-high molecular weight comb polyacrylamide is prepared by: the dosage of the chain transfer agent is 0.008-0.02% of the mass of the acrylamide monomer, and the chain transfer agent is selected from one or more of sodium formate, isopropanol and dodecyl mercaptan.
4. The method of claim 1 wherein said post-hydrolyzed ultra-high molecular weight comb polyacrylamide is prepared by: the dosage of the initiator is 0.12-0.2% of the mass of the acrylamide monomer, and the ratio of the oxidant to the reducing agent is 1: (2.5-5) in mass ratio for standby.
5. The method of claim 4 wherein said post-hydrolyzed ultra-high molecular weight comb polyacrylamide is prepared by: the oxidant is selected from one or more of ammonium persulfate, sodium persulfate, hydrogen peroxide and ferric chloride.
6. The method of claim 4 wherein said post-hydrolyzed ultra-high molecular weight comb polyacrylamide is prepared by: the reducing agent is selected from one or more of sodium bisulfite, sodium metabisulfite and ferrous chloride.
7. The method of claim 1 wherein said post-hydrolyzed ultra-high molecular weight comb polyacrylamide is prepared by: the dosage of the hydrolytic agent solution is 16-20% of the mass of the acrylamide monomer, and the hydrolytic agent solution is one selected from 30 wt% of sodium hydroxide solution, 30 wt% of potassium hydroxide solution and 30 wt% of sodium carbonate solution.
8. The method for preparing post-hydrolyzed ultra-high molecular weight comb polyacrylamide according to any one of claims 1-7, wherein the method comprises the following steps: the molecular weight of the ultra-high molecular weight comb-shaped polyacrylamide prepared by the method is more than or equal to 3031 ten thousand, the filtration ratio is less than or equal to 0.98, the insoluble substance is less than or equal to 0.17%, the apparent viscosity is more than or equal to 19.4 mPa.s, and the content of the residual monomer is less than or equal to 0.036%.
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|---|---|---|---|---|
| CN113583177A (en) * | 2021-08-17 | 2021-11-02 | 安徽天润化学工业股份有限公司 | Preparation method and application of temperature-resistant and salt-resistant six-arm star polyacrylamide |
| CN116804073A (en) * | 2023-06-28 | 2023-09-26 | 河南正佳能源环保股份有限公司 | Polyacrylamide suitable for oil extraction with extremely high mineralization degree and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031101A (en) * | 2009-09-25 | 2011-04-27 | 中国石油化工股份有限公司 | Heat-resistant and salt-resistant polymer thickening agent and preparation method thereof |
| US20180346804A1 (en) * | 2015-11-20 | 2018-12-06 | Hercules Llc | Crosslinked polymers derived from monomers having acryloyl and lactam moieties and sulfonic acid/sulfonate comonomers, compositions thereof, and applications thereof |
| CN111234097A (en) * | 2020-01-15 | 2020-06-05 | 西南石油大学 | Salt-tolerant quinary hydrophobic association polymer and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102031101A (en) * | 2009-09-25 | 2011-04-27 | 中国石油化工股份有限公司 | Heat-resistant and salt-resistant polymer thickening agent and preparation method thereof |
| US20180346804A1 (en) * | 2015-11-20 | 2018-12-06 | Hercules Llc | Crosslinked polymers derived from monomers having acryloyl and lactam moieties and sulfonic acid/sulfonate comonomers, compositions thereof, and applications thereof |
| CN111234097A (en) * | 2020-01-15 | 2020-06-05 | 西南石油大学 | Salt-tolerant quinary hydrophobic association polymer and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113583177A (en) * | 2021-08-17 | 2021-11-02 | 安徽天润化学工业股份有限公司 | Preparation method and application of temperature-resistant and salt-resistant six-arm star polyacrylamide |
| CN116804073A (en) * | 2023-06-28 | 2023-09-26 | 河南正佳能源环保股份有限公司 | Polyacrylamide suitable for oil extraction with extremely high mineralization degree and preparation method thereof |
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