CN105085839A - Preparation method of water soluble AM-AA-modified nanometer SiO2 functional monomer terpolymer oil displacement agent - Google Patents
Preparation method of water soluble AM-AA-modified nanometer SiO2 functional monomer terpolymer oil displacement agent Download PDFInfo
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- CN105085839A CN105085839A CN201410751157.8A CN201410751157A CN105085839A CN 105085839 A CN105085839 A CN 105085839A CN 201410751157 A CN201410751157 A CN 201410751157A CN 105085839 A CN105085839 A CN 105085839A
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Abstract
The invention relates to a preparation method of a water soluble AM-AA-modified nanometer SiO2 functional monomer terpolymer oil displacement agent. The preparation method comprises 1, mixing a modified nanometer SiO2 functional monomer, acrylamide and acrylic acid, adjusting pH to 7.3 by sodium hydroxide, and adding distilled water into the mixed solution to obtain an aqueous solution with a monomer total mass concentration of 22%, and 2, heating the aqueous solution to a temperature of 40 DEG C, adding an initiator into the aqueous solution, feeding nitrogen protective gas into the aqueous solution, carrying out a reaction process at a temperature of 40 DEG C for 6h, washing the reaction product by ethanol, and carrying out crushing and drying to obtain the terpolymer, wherein the raw materials comprise, by mass, 70-80% of acrylamide, 19.8-29.5% of acrylic acid and 0.2-0.5% of a modified nanometer SiO2 functional monomer. The oil displacement agent has performances of resisting a high temperature, salt and shearing and can satisfy real demand of high temperature high salt oil reservoir yield improvement.
Description
Technical field
The present invention relates to the technical field of oil production, more particularly, the present invention relates to a kind of water-soluble AM-AA-modified Nano SiO
2the preparation method of function monomer terpolymer oil-displacing agent.
Background technology
Oil, as Nonrenewable resources, has very important critical role in the fields such as industry, national defence.In order to improve mining term, the raising field output in oil field, employing polymer flooding is an important technology.Polymer flooding refers to and adds a small amount of polymkeric substance at injection water, relies on to increase aqueous viscosity and reduce reservoir permeability to play and improve sweep efficiency and improve the effect of recovery ratio.At present, polymer flooding enters industrialization phase in the Daqing oil field of China, Shengli Oil Field, Dagang Oilfield, Jilin Oil Field, Henan Oil Field, obtains good oil increasing effect.
At present, the widely used polymkeric substance of polymer flooding is polyacrylamide and derivative thereof.This base polymer desirable oil increasing effect can be obtained for when low temperature, low mineralization oil reservoir, but for during high temperature and high salinity oil reservoir, it improves recovery ratio effect and significantly reduces.In addition, because polymers soln can be subject to the shearing action of agitator, pipeline valve, injection pump, borehole and porous medium etc. in process of injection allocation, the viscosity of polymers soln will significantly reduce, and the effect of enhancing oil recovery in polymer flooding is had a strong impact on.Therefore, needing to develop heatproof, salt tolerant and shear resistant can better Polymer Used For Oil Displacement.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, the object of the present invention is to provide a kind of water-soluble AM-AA-modified Nano SiO
2the preparation method of function monomer terpolymer oil-displacing agent.The oil-displacing agent adopting preparation method of the present invention to prepare has high temperature resistant, anti-salt and shear-stable performance, can meet the current demand that high temperature and high salt oil deposit improves recovery ratio.
To achieve these goals, present invention employs following technical scheme:
A kind of water-soluble AM-AA-modified Nano SiO
2the preparation method of function monomer terpolymer oil-displacing agent, is characterized in that comprising the following steps: (1) is by modified Nano SiO
2function monomer, acrylamide and vinylformic acid mix, and with sodium hydroxide adjust ph to 7.0 ~ 7.5, add distilled water and be made into the aqueous solution that monomer total mass concentration is 20 ~ 25%; (2) when temperature is increased to 40 DEG C, add initiator, logical nitrogen protection, reacts 6 ~ 12h under temperature is 40 DEG C of conditions; Reaction product can obtain terpolymer oil-displacing agent through washing with alcohol, pulverizing, oven dry.
Wherein, described preparation method comprises the following steps: (1) is by modified Nano SiO
2function monomer, acrylamide and vinylformic acid mix, and by sodium hydroxide adjust ph to 7.3, add distilled water and be made into the aqueous solution that monomer total mass concentration is 22%; When temperature is increased to 40 DEG C, add initiator, logical nitrogen protection, reacts 6h under temperature is 40 DEG C of conditions; Reaction product can obtain terpolymer oil-displacing agent through washing with alcohol, pulverizing, oven dry.
Wherein, the structural formula of described oil-displacing agent is as follows:
Wherein, the content of acrylamide is 70 ~ 80wt%, and acrylic acid content is 19.8 ~ 28.5wt%, modified Nano SiO
2the content of function monomer is 0.2 ~ 0.5wt%.
Wherein, described initiator is the mixture of ammonium persulphate and sodium bisulfite, and the mol ratio of the two is 1: 1.
Wherein, described modified Nano SiO
2function monomer adopts following methods to prepare: (1) is by Nano-meter SiO_2
2react in toluene solution with 3-aminopropyl triethoxysilane and prepare modified Nano SiO
2; (2) the modified Nano SiO will prepared
2react in DMF solution with maleic anhydride and prepare described modified Nano SiO
2function monomer.
Wherein, described modified Nano SiO
2function monomer adopts following methods to prepare: (1) is by Nano-meter SiO_2
2with 3-aminopropyl triethoxysilane in anhydrous toluene solution, at 80 DEG C, react more than 12h, reaction product absolute ethanol washing, then vacuum-drying obtains modified Nano SiO
2; (2) in DMF solution, add maleic anhydride, after stirring and dissolving is complete, add modified Nano SiO
2, more than stirring reaction 6h at 60 DEG C, reaction product distilled water wash, filtration, oven dry can obtain modified Nano SiO
2function monomer.
Wherein, described 3-aminopropyl triethoxysilane and Nano-meter SiO_2
2mass ratio 0.03 ~ 0.06: 1; Described maleic anhydride and modified Nano SiO
2mass ratio be 0.25 ~ 0.50: 1.
Compared with prior art, terpolymer oil-displacing agent of the present invention has following beneficial effect:
(1) contriver is by Nano-meter SiO_2
2be incorporated in oil-displacing agent, at Nano-meter SiO_2
2carbon-carbon double bond on surface grafting, make itself and vinylformic acid and acrylamide polymerization, the terpolymer synthesized has spacial framework.
(2) contriver finds modified Nano SiO
2the performance of content on multipolymer of surface carbon-carbon double bond has significant impact, and can control SiO by two step method of modifying
2the degree of the carbon-carbon double bond of surface grafting is in suitable content range.
(3) the terpolymer oil-displacing agent that the present invention obtains has higher viscosity at high shear rates, has stronger temperature resistance, anti-salt and anti-shear ability, can significantly improve oil recovery factor.
Accompanying drawing explanation
Fig. 1 is AM-AA-modified Nano SiO of the present invention
2the infrared spectrogram of function monomer terpolymer oil-displacing agent;
Fig. 2 is apparent viscosity and the shearing rate graph of a relation in time of terpolymer oil-displacing agent of the present invention;
Fig. 3 is apparent viscosity and the shearing rate graph of a relation in time of terpolymer oil-displacing agent of the present invention;
Fig. 4 is the apparent viscosity of terpolymer oil-displacing agent of the present invention and the graph of a relation of salt concn;
Fig. 5 is the injection rate of terpolymer oil-displacing agent of the present invention and the graph of a relation of recovery ratio.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is described in further detail.Should be appreciated that specific embodiment described herein only for setting forth technical scheme of the present invention, and be not used in the protection domain limiting invention.
Embodiment 1 modified Nano SiO
2the synthesis of function monomer
1.0g Nano-meter SiO_2 is added in 500ml round-bottomed flask
2, 0.05g3-aminopropyl triethoxysilane and 80mL dry toluene, at 80 DEG C, react 12h, reaction product absolute ethanol washing, then at 80 DEG C, vacuum-drying obtains modified Nano SiO
2.In 250ml Erlenmeyer flask, add DMF and the 0.5g maleic anhydride of 30.0ml, after stirring and dissolving is complete, in solution, add 2.0g modified Nano SiO
2, then stirring reaction 6h at 60 DEG C, reaction product distilled water wash, filtration, oven dry can obtain modified Nano SiO
2function monomer.
Embodiment 2AM-AA-modified Nano SiO
2the synthesis of function monomer terpolymer oil-displacing agent
First in 100ml there-necked flask, add 0.044g modified Nano SiO
2function monomer, 8.206gAM and 2.750gAA, by sodium hydroxide adjust ph to 7.3, add distilled water and be made into the aqueous solution that monomer total mass concentration is 22%; When temperature is elevated to 40 DEG C, add 0.022g initiator (mol ratio of ammonium persulphate and sodium bisulfite is 1: 1), logical nitrogen protection, reacts 6h under temperature is 40 DEG C of conditions; Reaction product can obtain terpolymer through washing with alcohol, pulverizing, oven dry.
Embodiment 3AM-AA-modified Nano SiO
2the sign of function monomer terpolymer oil-displacing agent
By the infrared spectrogram of the oil-displacing agent of the 2-in-1 one-tenth of embodiment as shown in Figure 1, N-H stretching vibration absorption peak is positioned at 3402.3cm
-1;-CH
2stretching vibration absorption peak is positioned at 2943.1cm
-1; C=O stretching vibration absorption peak is positioned at 1668.92cm
-1;-NH flexural vibration absorption peak (in face) absorption peak is positioned at 1558.9cm
-1; C-N stretching vibration absorption peak is positioned at 1396.4cm
-1;-NH flexural vibration absorption peak (outside face) absorption peak is positioned at 650.3cm
-1; SiO
2charateristic avsorption band be positioned at 1116.2cm
-1and 780.4cm
-1.
Embodiment 4AM-AA-modified Nano SiO
2the anti-shear performance of function monomer terpolymer oil-displacing agent
Above-mentioned obtained oil-displacing agent distilled water is mixed with the aqueous solution that mass concentration is 2000mg/L, by its viscosity under different shear rate of rheometer measurement at 70 DEG C.As shown in Figure 2, the oil-displacing agent solution of 2000mg/L is at 500s
-1viscosity retention ratio after down cut 5min is 84.9%.
Embodiment 5AM-AA-modified Nano SiO
2the heat resistance of function monomer terpolymer oil-displacing agent
Above-mentioned obtained oil-displacing agent distilled water is mixed with the aqueous solution that concentration is 2000mg/L, and with BrookfiledDV-III viscometer, (shearing rate is 7.34s
-1) measure oil-displacing agent aqueous solution viscosity at different temperatures.As shown in Figure 3, the viscosity of 2000mg/L oil-displacing agent solution reduces along with the rising of temperature, and at 95 DEG C, the viscosity of oil-displacing agent solution is 67.8mPa.s, and this oil-displacing agent has good heat resistance.
Embodiment 6AM-AA-modified Nano SiO
2the salt resistant character of function monomer terpolymer oil-displacing agent
Above-mentioned obtained oil-displacing agent distilled water is mixed with the copolymer solution that concentration is 2000mg/L, respectively to the NaCl adding different mass in the copolymer solution of 2000mg/L, be stirred to and dissolve completely, with BrookfiledDV-III viscometer, (shearing rate is 7.34s
-1) measure the viscosity of oil-displacing agent solution at 70 DEG C.As can be seen from Figure 4, along with NaCl dosage raises, the viscosity of oil-displacing agent solution reduces rapidly, substantially tends towards stability subsequently.When NaCl concentration is 20000mg/L, the viscosity of the oil-displacing agent aqueous solution is 67.8mPa.s, shows that this oil-displacing agent has stronger anti-salt property.
Embodiment 7AM-AA-modified Nano SiO
2the oil-displacement capacity of function monomer terpolymer oil-displacing agent
Preparation mass concentration is the oil-displacing agent aqueous solution (NaCl mass concentration is 5000mg/L) of 2000mg/L.Adopt the raising recovery ratio ability of the one dimension sand-packed model research oil-displacing agent aqueous solution, test and carry out at 70 DEG C.The internal diameter of one dimension sand-packed model is 2.5cm, and length is 50cm, middle filling quartz sand (rate of permeation: 573 × 10
-3μm
2, porosity: 24.7%).Experimental procedure is as follows: (1) saturation water: the NaCl salt solution injecting 5000mg/L with the speed of 0.6mL/min in one dimension sand-packed model; (2) saturated oil: make the saturated crude oil of one dimension sand-packed model (at 70 DEG C, viscosity is for 56.9mPa.s), until the outlet of one dimension sand-packed model only has crude oil to flow out with the speed of 0.2mL/min, 0.4mL/min and 0.6mL/min respectively; (3) water displacing oil: use the NaCl solution of 5000mg/L with the crude oil in the speed displacement one dimension sand-packed model of 0.6mL/min, until water ratio reaches 95%; (4) injection of polymer: the oil-displacing agent aqueous solution (using 5000mg/LNaCl saline) injecting 2000mg/L with the speed of 0.6mL/min to one dimension sand-packed model, until water ratio reaches 95% again.As can be seen from Figure 5, the recovery ratio in water displacing oil stage is that 32.2%, the 2000mg/L oil-displacing agent aqueous solution improves recovery ratio 23.1%, shows stronger oil-displacement capacity.
Claims (8)
1. a water-soluble AM-AA-modified Nano SiO
2the preparation method of function monomer terpolymer oil-displacing agent, is characterized in that comprising the following steps: (1) is by modified Nano SiO
2function monomer, acrylamide and vinylformic acid mix, and with sodium hydroxide adjust ph to 7.0 ~ 7.5, add distilled water and be made into the aqueous solution that monomer total mass concentration is 20 ~ 25%; (2) when temperature is increased to 40 DEG C, add initiator, logical nitrogen protection, reacts 6 ~ 12h under temperature is 40 DEG C of conditions; Reaction product can obtain terpolymer oil-displacing agent through washing with alcohol, pulverizing, oven dry.
2. preparation method according to claim 1, is characterized in that comprising the following steps: (1) is by modified Nano SiO
2function monomer, acrylamide and vinylformic acid mix, and by sodium hydroxide adjust ph to 7.3, add distilled water and be made into the aqueous solution that monomer total mass concentration is 22%; When temperature is increased to 40 DEG C, add initiator, logical nitrogen protection, reacts 6h under temperature is 40 DEG C of conditions; Reaction product can obtain terpolymer oil-displacing agent through washing with alcohol, pulverizing, oven dry.
3. preparation method according to claim 1 and 2, is characterized in that the structural formula of described oil-displacing agent is as follows:
4. preparation method according to claim 3, is characterized in that: the content of acrylamide is 70 ~ 80wt%, and acrylic acid content is 19.8 ~ 28.5wt%, modified Nano SiO
2the content of function monomer is 0.2 ~ 0.5wt%.
5. preparation method according to claim 1 and 2, is characterized in that: described initiator is the mixture of ammonium persulphate and sodium bisulfite, and the mol ratio of the two is 1: 1.
6. preparation method according to claim 1 and 2, is characterized in that: described modified Nano SiO
2function monomer adopts following methods to prepare: (1) is by Nano-meter SiO_2
2react in toluene solution with 3-aminopropyl triethoxysilane and prepare modified Nano SiO
2; (2) the modified Nano SiO will prepared
2react in DMF solution with maleic anhydride and prepare described modified Nano SiO
2function monomer.
7. preparation method according to claim 6, is characterized in that: described modified Nano SiO
2function monomer adopts following methods to prepare: (1) is by Nano-meter SiO_2
2with 3-aminopropyl triethoxysilane in anhydrous toluene solution, at 80 DEG C, react more than 12h, reaction product absolute ethanol washing, then vacuum-drying obtains modified Nano SiO
2; (2) in DMF solution, add maleic anhydride, after stirring and dissolving is complete, add modified Nano SiO
2, more than stirring reaction 6h at 60 DEG C, reaction product distilled water wash, filtration, oven dry can obtain modified Nano SiO
2function monomer.
8. preparation method according to claim 7, is characterized in that: described 3-aminopropyl triethoxysilane and Nano-meter SiO_2
2mass ratio 0.03 ~ 0.06: 1; Described maleic anhydride and modified Nano SiO
2mass ratio be 0.25 ~ 0.50: 1.
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CN115404067A (en) * | 2021-05-26 | 2022-11-29 | 大庆油田有限责任公司 | Salt-tolerant polymer and oil displacement agent system and preparation method thereof |
CN117106430A (en) * | 2023-10-18 | 2023-11-24 | 西南石油大学 | Profile control and flooding system suitable for strong heterogeneous oil reservoir and application |
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CN115404067A (en) * | 2021-05-26 | 2022-11-29 | 大庆油田有限责任公司 | Salt-tolerant polymer and oil displacement agent system and preparation method thereof |
CN115404067B (en) * | 2021-05-26 | 2023-10-03 | 大庆油田有限责任公司 | Salt-tolerant polymer and oil displacement agent system and preparation method thereof |
CN113278118A (en) * | 2021-07-22 | 2021-08-20 | 山东聚星石油科技有限公司 | Temperature-resistant and salt-resistant nano polymer emulsion and synthesis method and application thereof |
CN113278118B (en) * | 2021-07-22 | 2021-09-24 | 山东聚星石油科技有限公司 | Temperature-resistant and salt-resistant nano polymer emulsion and synthesis method and application thereof |
CN117106430A (en) * | 2023-10-18 | 2023-11-24 | 西南石油大学 | Profile control and flooding system suitable for strong heterogeneous oil reservoir and application |
CN117106430B (en) * | 2023-10-18 | 2024-01-23 | 西南石油大学 | Profile control and flooding system suitable for strong heterogeneous oil reservoir and application |
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