CN105273707A - Viscous-elastic particle oil-displacing agent with fluorescence characteristic and preparation method therefor - Google Patents
Viscous-elastic particle oil-displacing agent with fluorescence characteristic and preparation method therefor Download PDFInfo
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- CN105273707A CN105273707A CN201410643131.1A CN201410643131A CN105273707A CN 105273707 A CN105273707 A CN 105273707A CN 201410643131 A CN201410643131 A CN 201410643131A CN 105273707 A CN105273707 A CN 105273707A
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Abstract
The invention discloses a viscous-elastic particle oil-displacing agent with a fluorescence characteristic and a preparation method therefor. The oil-displacing agent is a terpolymer composed of three structural units: acrylamide, N-vinyl carbazole and 2-(dimethylamino)ethyl methacrylate. The preparation method is as follows: 100 parts of acrylamide is dissolved in 250-290 parts of water to prepare a solution, 0.3-0.5 part of 2-(dimethylamino)ethyl methacrylate is dissolved in 40-60 parts of water to prepare a solution, 0.0004-0.025 part of N-vinyl carbazole is dissolved in 0.2-4 parts of ethanol to prepare a solution, the solutions are added in a three-necked bottle in order, and the three-necked bottle is placed in water-bath at a temperature of 15-25 DEG C; after nitrogen input is carried out for 20min, a solution prepared after 0.015-0.035 part of potassium peroxodisulfate is dissolved in 20-40 parts of water is added into the three-necked bottle; when the temperature rise of the reaction solution is more than 1 DEG C, nitrogen input is stopped, after the reaction is finished, the three-necked bottle is placed in a water bath kettle, thermal insulation is carried out for 3-5h, then gel is taken out, cut into pieces, dried, crushed and screened, and a powdery product can be obtained.
Description
Technical field
The present invention relates to technical field of tertiary oil recovery, particularly relate to and a kind ofly improve viscoelastic particle oil displacement agent with fluorescent characteristic of oil recovery factor and preparation method thereof.
Background technology
The characteristics of reservoirs in the most of oil field of China is heterogeneous body, and these oil fields have entered the development phase of High water cut or ultra-high water-containing at present, advance by leaps and bounds along most permeable zone or band after tradition oil-displacing agent partially hydrolyzed polyacrylamide injects oil reservoir, enter lacking of low permeability layer, oil-displacing agent swept volume is low, cause final oil-recovering rate not high, therefore have developed a kind of partial cross-linked and containing the polyacrylamide viscoelastic particle oil displacement agent (CN101775275B) of a large amount of branched structure.For this novel oil-displacing agent, its seepage flow characteristics in porous medium and oil-displacement mechanism not yet clear and definite, if introduce fluorophor on viscoelastic particle oil displacement agent polymer molecule, just in seepage flow, oil displacement experiment, real-time tracing can be carried out to it, specify its oil-displacement mechanism; And the concentration of viscoelastic particle oil displacement agent in recovery well Produced Liquid can be detected at the scene during application in time, exactly, therefore, develop the viscoelastic particle oil displacement agent with fluorescent characteristic, for raising oil recovery, there is extremely important theoretical investigation value and large-scale application prospect.
The fluorescent characteristic research of polymers soln can be divided into extrinsic fluorescent probe method and endogenous fluorescence probe method to carry out.Extrinsic fluorescent probe method refers to additional a kind of fluorescent chemicals and fluorescent probe in a polymer solution, then is studied this system by the change of the fluorescent characteristic measuring fluorescent probe.US Patent No. 5435969 adopt 2 ?naphthene sulfonic acid etc. add in water conditioner and directly mix with polymkeric substance, carry out monitoring polymer concentration, in this, as tracer agent by measuring fluorescence intensity; Yang Xueshan (application chemical industry, 2013,42,2,195 ?204) etc. people take pyrene as probe, research hydrophobic associated polymer Assembling Behavior in aqueous, although these class methods are simple, but additional fluorescent chemicals exists problem pockety, and in use fluorescent small molecule easily comes off, separates out, and makes the method there is certain restriction in use; Endogenous fluorescence probe method and polymkeric substance self contain fluorophor and have endogenous fluorescence.In endogenous fluorescence polymkeric substance, unit and fluorescence unit is connected on polymer by chemical bond-linking, difficult drop-off, and have good water tolerance and organic solvent resistance, and chromophoric group is evenly distributed, content is highly stable, and fluorescence property is excellent.The chemical preparation process of endogenous fluorescence polymkeric substance mainly contains two kinds, one is that the fluorescent small molecule with reactive behavior is realized high molecular by radical polymerization or polycondensation, and two is fluorescent small molecule be grafted on general polymer macromolecular chain by chemical reaction to prepare fluorescent polymer.Chinese patent CN102391848 adopts inverse emulsion polymerization to synthesize a kind of water miscible tracing polymer oil displacement agent, has fluorescence and good heat and salt resistance and shear resistant.But the monomer Xi Bing Ji adopted in this patent ?7 ?Qiang Ji ?4 ?the non-commercialization of methylcoumarin, not easily obtain, and polymerization technique relative complex, suitability for industrialized production difficulty is larger.
For the deficiencies in the prior art, simultaneously in order to study the oil-displacement mechanism of granule type oil-displacing agent, this patent adopts simple aqueous solution polymerization, by fluorescent monomer N ?vinylcarbazole and acrylamide copolymerization, prepare the viscoelastic particle oil displacement agent with fluorescent characteristic, this oil-displacing agent has the two-fold advantage of linear polyacrylamide and cross-linked polyacrylamide concurrently, has excellent temperature resistant antisalt anti-shear performance, fluid diversion effect can be played in heterogeneous reservoir, increase substantially recovery ratio.Synthesize this oil-displacing agent desired raw material cheap and easy to get, polymerization cycle is short, and building-up process does not need to introduce a large amount of organic solvent, economic environmental protection, and product postprocessing is simple, is more suitable for suitability for industrialized production.
Summary of the invention
The object of this invention is to provide a kind of viscoelastic particle oil displacement agent with fluorescent characteristic and preparation method thereof.
One of to achieve these goals, the present invention adopts following technical scheme:
There is a partial cross-linked polyacrylamide viscoelastic particle oil displacement agent for fluorescent characteristic, be by acrylamide, N ?the terpolymer that forms of vinylcarbazole and dimethylaminoethyl acrylate methyl ammonia ethyl ester three kinds of structural units, each ingredients weight parts of this oil-displacing agent is:
To achieve these goals two, the present invention adopts following technical scheme:
There is a preparation method for the viscoelastic particle oil displacement agent of fluorescent characteristic, comprise the steps:
100 parts of acrylamides are dissolved in wiring solution-forming in 250 ~ 290 parts of water, 0.3 ~ 0.5 part of dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in wiring solution-forming in 40 ~ 60 parts of water, 0.0004 ~ 0.025 part of N-vinylcarbazole is dissolved in wiring solution-forming in 0.2 ~ 4 part of ethanol, add in three-necked bottle successively, and be placed in the water-bath of 15 ~ 25 DEG C; 0.015 ~ 0.035 part of Potassium Persulphate, after 20 minutes, is dissolved in the solution be made in 20 ~ 40 parts of water and adds three-necked bottle by logical nitrogen; Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 75 ~ 85 DEG C of water-baths insulations 3 ~ 5 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained after screening.
Fluorescence viscoelastic particle oil displacement agent of the present invention has the two-fold advantage of linear polyacrylamide and cross-linked polyacrylamide concurrently, has excellent temperature resistant antisalt anti-shear performance, can play fluid diversion effect in heterogeneous reservoir, improves recovery ratio Be very effective.The present invention adopts simple aqueous solution polymerization, by fluorescent monomer N ?vinylcarbazole and acrylamide copolymerization, prepare the viscoelastic particle oil displacement agent with fluorescent characteristic, synthesize this oil-displacing agent desired raw material cheap and easy to get, polymerization cycle is short, and building-up process does not need to introduce a large amount of organic solvent, economic environmental protection, product postprocessing is simple, is more suitable for suitability for industrialized production.
Accompanying drawing explanation
The infrared spectrum of Fig. 1 fluorescence viscoelastic particle oil displacement agent of the present invention;
The fluorescence emission spectrum of Fig. 2 fluorescence viscoelastic particle oil displacement agent of the present invention;
Fig. 3 fluorescence viscoelastic particle oil displacement agent of the present invention suspension suspension volume test schematic diagram;
The relation of Fig. 4 fluorescence viscoelastic particle oil displacement agent of the present invention suspension apparent viscosity and brine concentration;
The indoor oil displacement experiment curve of Fig. 5 fluorescence viscoelastic particle oil displacement agent of the present invention suspension.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but be not used for limiting the scope of the invention.
Embodiment 1:
100g acrylamide is dissolved in wiring solution-forming in 260g water, and 0.45g dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in wiring solution-forming in 50g water, and 0.0005gN ?vinylcarbazole is dissolved in wiring solution-forming in 1g ethanol, adds in three-necked bottle successively, and is placed in the water-bath of 20 DEG C; 0.02g Potassium Persulphate, after 20 minutes, is dissolved in the solution be made in 40g water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 75 DEG C of water-baths insulations 5 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained after screening.
Embodiment 2:
100g acrylamide is dissolved in wiring solution-forming in 290g water, and 0.5g dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in wiring solution-forming in 60g water, and 0.0004gN ?vinylcarbazole is dissolved in wiring solution-forming in 0.2g ethanol, adds in three-necked bottle successively, and is placed in the water-bath of 15 DEG C; 0.035g Potassium Persulphate, after 20 minutes, is dissolved in the solution be made in 40g water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 80 DEG C of water-baths insulations 4 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained after screening.
Embodiment 3:
100g acrylamide is dissolved in wiring solution-forming in 250g water, and 0.3g dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in wiring solution-forming in 40g water, and 0.025gN ?vinylcarbazole is dissolved in wiring solution-forming in 4g ethanol, adds in three-necked bottle successively, and is placed in the water-bath of 25 DEG C; 0.015g Potassium Persulphate, after 20 minutes, is dissolved in the solution be made in 20g water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 85 DEG C of water-baths insulations 3 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained after screening.
Embodiment 4: the infrared spectrum of fluorescence viscoelastic particle oil displacement agent
The fluorescence viscoelastic particle oil displacement agent of embodiment 1 is cleaned 3 times in ethanol, removes unreacted monomer.Fluorescence viscoelastic particle oil displacement agent after purifying is carried out examination of infrared spectrum, and result as shown in Figure 1.Can learn from spectrogram, 1658cm
?1, 1602cm
?1, 1454cm
?1, 1405cm
?1for Ben Huan ?C=C skeletal vibration absorption peak; At 634cm
?1absorption peak be on phenyl ring C ?the out-of-plane deformation vibration peak of H key; At 3186cm
?1and 2931cm
?1absorption peak be on phenyl ring C ?H stretching vibration peak, it can thus be appreciated that, N ?vinylcarbazole success copolymerization.Embodiment 5: fluorescence viscoelastic particle oil displacement agent fluorescent characteristic is investigated
The suspension using deionized water to become concentration to be 5000mg/L the product configuration of the embodiment 1 after purifying, carries out fluorescence spectrum test.Fixing Hitachi F4600 fluorescence spectrophotometer slit width 10nm, during test, excitation wavelength is 260nm, records emmission spectrum as shown in Figure 2.Can learn from collection of illustrative plates, the maximum emission wavelength of fluorescence viscoelastic particle oil displacement agent is 354nm, and has very strong fluorescence intensity.
Embodiment 6: fluorescence viscoelastic particle oil displacement agent suspension property is investigated
Take 1g particle diameter be 100 ?the polymkeric substance of 150 object embodiments 1, slowly add in 80mL distilled water under magnetic stirring, stirring velocity is set to 500r/min, and churning time is 15min.Then the suspension configured to be poured in the graduated cylinder of 100mL and to add water to 100 scales.After placing for some time, can find that solid-liquid interface appears in this suspension, as shown in Figure 3, place and read interfacial scale value in 2 hours, be the suspension volume of fluorescence viscoelastic particle oil displacement agent.Test result shows, the suspension property of fluorescence viscoelastic particle oil displacement agent is excellent, and suspension volume is 85%.
Embodiment 7: fluorescence viscoelastic particle oil displacement agent anti-salt property is investigated
Adopt salinity to be the reservoir simulation salt solution of 6666mg/L, 30000mg/L and 50000mg/L respectively, the fluorescence viscoelastic particle oil displacement agent in embodiment 1 is mixed with the suspension that concentration is 5000mg/L, is 25 DEG C in temperature, shearing rate be 0.01 ?100s
?1under, the apparent viscosity of test suspension liquid, test result is as shown in Figure 4, as seen from the figure, along with the increase of salinity, the apparent viscosity change of fluorescence viscoelastic particle oil displacement agent suspension is little, sticky cut curve and almost overlap, show that embodiment 1 polymkeric substance has excellent salt-resistant type energy.
The indoor displacement of reservoir oil of embodiment 8 fluorescence viscoelastic particle oil displacement agent is investigated
Fluorescence viscoelastic particle oil displacement agent in embodiment 1 is mixed with the suspension that concentration is 2000mg/L, salt water salinity is 30000mg/L, fill out sand tube rate of permeation is 1500 millidarcies, laboratory simulation flooding result as shown in Figure 5, can find out, after injecting fluorescence viscoelastic particle oil displacement agent suspension, pressure obviously increases, water content declines, recovery ratio increases, and calculation result shows, and ultimate recovery factor reaches 76.22%, after water drive, recovery ratio improves 14.43%, illustrates that this fluorescence viscoelastic particle oil displacement agent has the effect of higher raising recovery ratio.
Claims (2)
1. have a viscoelastic particle oil displacement agent for fluorescent characteristic, it is characterized in that, this oil-displacing agent is the terpolymer be made up of acrylamide, N-vinylcarbazole and dimethylaminoethyl acrylate methyl ammonia ethyl ester three kinds of structural units, and wherein each ingredients weight parts is:
2. prepare a method for the viscoelastic particle oil displacement agent as claimed in claim 1 with fluorescent characteristic, it is characterized in that, preparation method is as follows:
100 parts of acrylamides are dissolved in wiring solution-forming in 250 ~ 290 parts of water, 0.3 ~ 0.5 part of dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in wiring solution-forming in 40 ~ 60 parts of water, 0.0004 ~ 0.025 part of N-vinylcarbazole is dissolved in wiring solution-forming in 0.2 ~ 4 part of ethanol, add in three-necked bottle successively, and be placed in the water-bath of 15 ~ 25 DEG C; 0.015 ~ 0.035 part of Potassium Persulphate, after 20 minutes, is dissolved in the solution be made in 20 ~ 40 parts of water and adds three-necked bottle by logical nitrogen; Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 75 ~ 85 DEG C of water-baths insulations 3 ~ 5 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained after screening.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107298973A (en) * | 2016-04-14 | 2017-10-27 | 中国石油化工股份有限公司 | A kind of seriation fluorescence viscoelastic particle oil displacement agent and preparation method thereof |
| CN110054728A (en) * | 2019-04-25 | 2019-07-26 | 河北华北石油天成实业集团有限公司 | A kind of preparation method of embedded tracer polymer microballoon |
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| US20050009999A1 (en) * | 2000-02-16 | 2005-01-13 | Lai John Ta-Yuan | Hydroxyl-terminated thiocarbonate containing compounds, polymers, and copolymers, and polyurethanes and urethane acrylics made therefrom |
| CN101605829A (en) * | 2006-12-12 | 2009-12-16 | 联合利华公司 | Polymkeric substance |
| US20100130641A1 (en) * | 2006-12-12 | 2010-05-27 | Unilever Plc | Polymers |
| WO2013029837A1 (en) * | 2011-08-26 | 2013-03-07 | Evonik Rohmax Additives Gmbh | Method for reducing the halogen content of a polymer |
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2014
- 2014-11-07 CN CN201410643131.1A patent/CN105273707A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050009999A1 (en) * | 2000-02-16 | 2005-01-13 | Lai John Ta-Yuan | Hydroxyl-terminated thiocarbonate containing compounds, polymers, and copolymers, and polyurethanes and urethane acrylics made therefrom |
| CN101605829A (en) * | 2006-12-12 | 2009-12-16 | 联合利华公司 | Polymkeric substance |
| US20100130641A1 (en) * | 2006-12-12 | 2010-05-27 | Unilever Plc | Polymers |
| WO2013029837A1 (en) * | 2011-08-26 | 2013-03-07 | Evonik Rohmax Additives Gmbh | Method for reducing the halogen content of a polymer |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107298973A (en) * | 2016-04-14 | 2017-10-27 | 中国石油化工股份有限公司 | A kind of seriation fluorescence viscoelastic particle oil displacement agent and preparation method thereof |
| CN110054728A (en) * | 2019-04-25 | 2019-07-26 | 河北华北石油天成实业集团有限公司 | A kind of preparation method of embedded tracer polymer microballoon |
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