CN102617794A - Temperature-resisting anti-salt type oil extraction chemical auxiliary agent and preparation method thereof - Google Patents
Temperature-resisting anti-salt type oil extraction chemical auxiliary agent and preparation method thereof Download PDFInfo
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- CN102617794A CN102617794A CN201210101300XA CN201210101300A CN102617794A CN 102617794 A CN102617794 A CN 102617794A CN 201210101300X A CN201210101300X A CN 201210101300XA CN 201210101300 A CN201210101300 A CN 201210101300A CN 102617794 A CN102617794 A CN 102617794A
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Abstract
The invention discloses a temperature-resisting anti-salt type oil extraction chemical auxiliary agent and a preparation method of the temperature-resisting anti-salt type oil extraction chemical auxiliary agent. The temperature-resisting anti-salt type oil extraction chemical auxiliary agent takes vinyl pyrrolidone and acrylamide as monomers and takes a mixed solvent of ethyl acetate/ethanol as a dispersing medium to obtain a bipolymer with better dispersion performance and heat stability by using a dispersion polymerization method in the presence of an initiator and a dispersant. The thermal decomposition temperature of the bipolymer is obviously improved compared with polyacrylamide. When the ratio of NVP (N Vinyl Pyrrolidinone) to AM (Acrylamide) is 1: 1 and 1: 4, and the volume ratio of the ethyl acetate to the ethanol is 8: 2, the viscosity retention rate of a polymer emulsion in a high-salinity salt solution is obviously improved and the temperature-resisting anti-salt performance is greatly improved. The temperature-resisting anti-salt type oil extraction chemical auxiliary agent and the preparation method of the temperature-resisting anti-salt type oil extraction chemical auxiliary agent, disclosed by the invention, have the advantages of simple process, easiness for controlling and high product yield.
Description
One, technical field
The present invention relates to a kind of oil recovery chemical assistant and preparation method thereof, specifically a kind of thermal resisting anti-salt type oil recovery chemical assistant and preparation method thereof.
Two, background technology
Oil has become one of contemporary most important energy and material.Because when partially hydrolyzed polyacrylamide (PHPA) conduct improves the chemical assistant of oil recovery; Its salt tolerance, temperature tolerance, anti-shear performance and antioxidant property are all not too satisfactory; Easy hydrolysis when high temperature, viscosity also can acutely descend when having salt to exist, in the presence of divalent-metal ion; It can produce the deposition and loses viscosity, and use temperature is the highest can not be above 75 ℃.Especially under the condition of high temperature and high salinity, use to have received very big restriction.
In order to overcome the above-mentioned weakness of SEPIGEL 305, people have worked out a lot of thermal resisting anti-salt type multipolymers.Lv Maosen etc. have studied binary temperature resistant antisalt multipolymer oil-displacing agent.Oil recovery chemical assistant NVP-AM copolymer has been synthesized in use solution polymerizations such as Song Linhua.Li Junzhong, Zhou Ni, Wang Guijiang etc. have studied the synthetic of ternary temperature resistant antisalt multipolymer, and Tang Hao etc. have then studied quaternary temperature resistant antisalt multipolymer.It is low or monomer conversion is not high that but above-mentioned synthetic multipolymer has plenty of the viscosity conservation rate, and what have then is the polymerization method more complicated, reacts bad control.
Three, summary of the invention
The present invention aims to provide a kind of thermal resisting anti-salt type oil recovery chemical assistant and preparation method thereof, and technical problem to be solved is to make the oil recovery chemical assistant when improving oil recovery, have higher thermostability and viscosity conservation rate.
Technical solution problem of the present invention adopts following technical scheme:
The raw material of thermal resisting anti-salt type oil recovery chemical assistant of the present invention is: monomer, dispersion agent, initiator and dispersion medium; Wherein the addition of dispersion agent is the 10-15% of monomer mass, and the addition of initiator is the 0.5-1.0% of monomer mass, and monomeric quality is the 10-25% of raw material total mass; Said monomer is vinyl pyrrolidone (NVP) and acrylic amide (AM), and the mass ratio of said vinyl pyrrolidone (NVP) and acrylic amide (AM) is 1: 1-4;
Said dispersion agent is selected from Vinylpyrrolidone polymer (PVP), Z 150PH (PVA) or polyoxyethylene glycol (PEG)
Said initiator is selected from Diisopropyl azodicarboxylate (AIBN), azo dicyano valeric acid (ACVA) or Potassium Persulphate (KPS);
Said dispersion medium is ETHYLE ACETATE and alcoholic acid mixing solutions, and ETHYLE ACETATE and alcoholic acid volume ratio are 8-6: 2-4.
The mass ratio of said vinyl pyrrolidone (NVP) and acrylic amide (AM) preferred 1: 1 or 1: 4; ETHYLE ACETATE and alcoholic acid volume ratio are preferred 8: 2 in the dispersion medium.
The preparation method of thermal resisting anti-salt type oil recovery chemical assistant of the present invention be with monomer, dispersion agent and initiator blending dispersion in dispersion medium, under nitrogen protection in 60-80 ℃ of reaction 6-7 hour, after reaction finishes successively through centrifugal, washing and dry.
Main ingredient is monomer, dispersion agent, initiator and dispersion medium in the dispersion polymerization system.Reacting precursor system is homogeneous phase, and monomer, dispersion agent and initiator all are dissolved in the dispersion medium, and along with the carrying out of reaction, the polymkeric substance of generation is owing to the sterically hindered effect of dispersion agent separates out from medium.The dispersion copolymerization method production technique is simple and can prepare the polymer microballoon that particle diameter is little, molecular weight is big, can solve heat dissipation problem preferably, and the particle diameter of product generally is controlled between the 1-10 μ m.Compare and body or solution polymerization, diffuse-aggregate transformation efficiency and speed of reaction be than higher, and have the reaction mechanism and the speed of reaction of solution polymerization; Than letex polymerization, the particle of polymkeric substance is bigger, dispersed better.
The present invention adopts vinyl pyrrolidone (NVP) modification partially hydrolyzed polyacrylamide (PHPA); Because vinyl pyrrolidone (NVP) contains rigid structure; Can effectively suppress the hydrolysis of carboxamido-group; The PAM polymkeric substance of an amount of NVP of copolymerization its thermal stability under high temperature has had large increase than PAM, and compares other multipolymer, and the viscosity conservation rate is the highest.
[dependence test]
1, the test of AV
The present invention simulates the Zhongyuan Oil Field two factory's output water that recover the oil, with NaCl, CaCl
2And MgCl
2The preparation total mineralization is 1.6 * 10
5The normal saline solution solution of mg/L, wherein Ca
2+Concentration be 2630mg/L, Mg
2+Concentration be 612mg/L, Na
+Concentration be 59600mg/L.Use normal saline solution solution that multipolymer is mixed with the copolymer solution of concentration as 2500mg/L, use the LV-DV rotational viscosimeter to measure copolymer salt solution AV down at 25 ℃.
2, the test of heat decomposition temperature
The present invention uses TG209F3 type thermogravimetric analyzer to measure the heat decomposition temperature of multipolymer, and nitrogen atmosphere, temperature rise rate are 10 ℃/min, TR 0-800 ℃.
3, the test of viscosity conservation rate
The copolymer solution of getting preparation is packed in the bottle of deoxygenation in right amount, and sealing is placed on the senile experiment that schedules to last 30d in 90 ℃ the baking oven, regularly takes out, at 25 ℃ of conservation rates of its AV of mensuration down.Measure its thermostability with this.
4, salt resistance is measured
The total gram number that contains various salinities in 1 premium on currency is claimed salinity.According to Zhongyuan Oil Field recover the oil NaCl in two factory's output water, CaCl
2And MgCl
2Ratio; The preparation salinity is respectively 2000,4000,6000,8000,10000,12000, the salt brine solution of 14000mg/L; Salt brine solution with different salinities is the copolymer solution that the solvent compound concentration is 2500mg/L again, studies the influence of different salinities to the AV of aqueous copolymers solution.
Reach about 420 ℃ through the recover the oil heat decomposition temperature of chemical assistant of test shows the present invention, the temperature tolerance of comparing SEPIGEL 305 (heat decomposition temperature is about 350 ℃) is significantly improved; At NVP/AM=1: 1 and 1: 4, ETHYLE ACETATE and alcoholic acid volume ratio are 8: 2 o'clock, and copolymer emulsion reaches more than 69% at the salt solution medium viscosity conservation rate of high salinity, and temperature resistant antisalt property has obtained large increase.
Four, description of drawings
Fig. 1 is the size distribution figure of the multipolymer (chemical assistant promptly recovers the oil) for preparing of the present invention.As can beappreciated from fig. 1 the particle diameter ratio of multipolymer is more concentrated, and median size is about 1.72 μ m.
Fig. 2 is the thermogravimetric collection of illustrative plates of the multipolymer (chemical assistant promptly recovers the oil) that makes under the different monomer ratio.Can know that by Fig. 2 the quality of multipolymer before 150 ℃ lose 2.49% and 3.17% respectively; This is a spot of moisture; The remaining monomer and the volatilization of oligopolymer cause, and the rising multipolymer along with temperature constantly decomposes subsequently, in the time of 410-420 ℃; Multipolymer reaches maximum decomposition temperature, and 500 ℃ of later carbon yields almost remain unchanged.And the mass ratio at NVP/AM is 1: 4 o'clock, the remaining quality of multipolymer more the more, better heat stability.
Fig. 3 is multipolymer (chemical assistant promptly recovers the oil) AV of solution and the graph of a relation of salinity with the preparation of normal saline solution solution.As can beappreciated from fig. 3, along with the increase of salinity, the viscosity of polymers soln reduces, and surpasses 6 * 10 but work as salinity
4During mg/L, the soltion viscosity kept stable shows that multipolymer has certain salt resistance.
Five, embodiment
Embodiment 1:
Raw material and proportioning:
Monomer vinyl pyrrolidone and acrylic amide, dispersion agent PVP-K30, initiator A IBN and dispersion medium ETHYLE ACETATE and alcoholic acid mixing solutions; Wherein the addition of dispersion agent is 10% of a monomer mass, and the addition of initiator is 1.0% of a monomer mass, and monomeric quality is 20% of a raw material total mass;
The mass ratio of therein ethylene base pyrrolidone and acrylic amide is 1: 1;
ETHYLE ACETATE and alcoholic acid volume ratio are 8: 2 in the dispersion medium.
The preparation method:
In the 250mL there-necked flask, add ETHYLE ACETATE and alcoholic acid mixing solutions, add dispersion agent PVP-K30 subsequently, start stirring; After dissolving fully Deng dispersion agent; Add monomer A M and NVP, add initiator A IBN at last, 70 ℃ of water bath with thermostatic control stirring and dissolving; The water bath with thermostatic control reaction is 6-7 hour under the nitrogen atmosphere, obtains milky emulsion.Be placed in the supercentrifuge milky emulsion centrifugal; In the centrifugal process with the white solid product 4-5 of solvent cleaning lower floor time; Get centrifuge tube lower floor white product after the end, product is placed in the vacuum drying oven dry 12 hours, obtain the white powder solid and be product.
The decomposition temperature that records product is 420 ℃, and AV is 18.3mpa.s, and the viscosity conservation rate is 69.8%.
Embodiment 2:
The preparation method of present embodiment is with embodiment 1, and the mass ratio of different is vinyl pyrrolidone and acrylic amide is 1: 2.
The decomposition temperature that records product is 412 ℃, and AV is 17.2mpa.s, and the viscosity conservation rate is 66.9%.
Embodiment 3:
The preparation method of present embodiment is with embodiment 1, and the mass ratio of different is vinyl pyrrolidone and acrylic amide is 1: 4.
The decomposition temperature that records product is 405 ℃, and AV is 17.8mpa.s, and the viscosity conservation rate is 69.5%.
Embodiment 4:
The preparation method of present embodiment is with embodiment 1, and the mass ratio of different is vinyl pyrrolidone and acrylic amide is 1: 1, and the consumption of initiator is 0.5% of a monomer mass.
The decomposition temperature that records product is 407 ℃, and AV is 17.8mpa.s, and the viscosity conservation rate is 68.8%.
Embodiment 5:
The preparation method of present embodiment is with embodiment 1, and the mass ratio of different is vinyl pyrrolidone and acrylic amide is 1: 2, and the consumption of initiator is 0.5% of a monomer mass.
The decomposition temperature that records product is 402 ℃, and AV is 17.3mpa.s, and the viscosity conservation rate is 67.2%.
Embodiment 6:
The preparation method of present embodiment is with embodiment 1, and the mass ratio of different is vinyl pyrrolidone and acrylic amide is 1: 4, and the consumption of initiator is 0.5% of a monomer mass.
The decomposition temperature that records product is 411 ℃, and AV is 17.6mpa.s, and the viscosity conservation rate is 68.9%.
Embodiment 7:
The preparation method of present embodiment is with embodiment 1, and the mass ratio of different is vinyl pyrrolidone and acrylic amide is 1: 1, and the consumption of initiator is 0.5% of a monomer mass, and the consumption of dispersion agent is 15% of a monomer mass.
The decomposition temperature that records product is 417 ℃, and AV is 17.9mpa.s, and the viscosity conservation rate is 69.7%.
Embodiment 8:
The preparation method of present embodiment is with embodiment 1, and the mass ratio of different is vinyl pyrrolidone and acrylic amide is 1: 2, and the consumption of initiator is 0.5% of a monomer mass, and the consumption of dispersion agent is 15% of a monomer mass.
The decomposition temperature that records product is 423 ℃, and AV is 17.5mpa.s, and the viscosity conservation rate is 66.2%.
Embodiment 9:
The preparation method of present embodiment is with embodiment 1, and the mass ratio of different is vinyl pyrrolidone and acrylic amide is 1: 4, and the consumption of initiator is 0.5% of a monomer mass, and the consumption of dispersion agent is 15% of a monomer mass.
The decomposition temperature that records product is 404 ℃, and AV is 18.2mpa.s, and the viscosity conservation rate is 68.5%.
Claims (3)
1. a thermal resisting anti-salt type oil recovery chemical assistant is characterized in that its raw material is: monomer, dispersion agent, initiator and dispersion medium; Wherein the addition of dispersion agent is the 10-15% of monomer mass, and the addition of initiator is the 0.5-1.0% of monomer mass, and monomeric quality is the 10-25% of raw material total mass;
Said monomer is vinyl pyrrolidone and acrylic amide, and the mass ratio of said vinyl pyrrolidone and acrylic amide is 1: 1-4;
Said dispersion agent is selected from Vinylpyrrolidone polymer, Z 150PH or polyoxyethylene glycol;
Said initiator is selected from Diisopropyl azodicarboxylate, azo dicyano valeric acid or Potassium Persulphate;
Said dispersion medium is ETHYLE ACETATE and alcoholic acid mixing solutions, and ETHYLE ACETATE and alcoholic acid volume ratio are 8-6: 2-4.
2. thermal resisting anti-salt type oil recovery chemical assistant according to claim 1 is characterized in that: the mass ratio of said vinyl pyrrolidone and acrylic amide is 1: 1 or 1: 4; ETHYLE ACETATE and alcoholic acid volume ratio are 8: 2 in the dispersion medium.
3. the preparation method of claim 1 or 2 described thermal resisting anti-salt type oil recovery chemical assistants is characterized in that:
With monomer, dispersion agent and initiator blending dispersion in dispersion medium, under nitrogen protection in 60-80 ℃ of reaction 6-7 hour, after reaction finishes successively through centrifugal, washing and dry.
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| CN104448129A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | High-temperature-resistant hydrolyzed copolymer for oilfields, and preparation method and application thereof |
| CN108559475A (en) * | 2018-03-27 | 2018-09-21 | 中国石油大学(华东) | A kind of heat-resistant salt-resistant polyvinyl acetate ester microsphere and its preparation and application |
| CN110041462A (en) * | 2019-05-22 | 2019-07-23 | 北京安德兴石油技术有限公司 | A kind of heat-resistant salt-resistant type amphiphilic macromolecule heavy crude thinner and preparation method thereof |
| CN114853954A (en) * | 2022-07-06 | 2022-08-05 | 山东诺尔生物科技有限公司 | Preparation method of carbomer resin and carbomer resin |
| CN115261005A (en) * | 2021-04-30 | 2022-11-01 | 中国石油天然气股份有限公司 | Modifying and flooding agent and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104448129A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | High-temperature-resistant hydrolyzed copolymer for oilfields, and preparation method and application thereof |
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| CN104193868A (en) * | 2014-09-02 | 2014-12-10 | 湖南理工学院 | Method and process for preparing polyacrylamide polymers with controllable grain sizes, molecular weights and molecular amount distribution |
| CN108559475A (en) * | 2018-03-27 | 2018-09-21 | 中国石油大学(华东) | A kind of heat-resistant salt-resistant polyvinyl acetate ester microsphere and its preparation and application |
| CN108559475B (en) * | 2018-03-27 | 2020-12-25 | 中国石油大学(华东) | Temperature-resistant salt-resistant polyvinyl acetate microsphere and preparation and application thereof |
| CN110041462A (en) * | 2019-05-22 | 2019-07-23 | 北京安德兴石油技术有限公司 | A kind of heat-resistant salt-resistant type amphiphilic macromolecule heavy crude thinner and preparation method thereof |
| CN110041462B (en) * | 2019-05-22 | 2020-12-08 | 北京安德兴石油技术有限公司 | Temperature-resistant salt-tolerant amphiphilic high-molecular viscosity reducer for thickened oil and preparation method thereof |
| CN115261005A (en) * | 2021-04-30 | 2022-11-01 | 中国石油天然气股份有限公司 | Modifying and flooding agent and preparation method thereof |
| CN114853954A (en) * | 2022-07-06 | 2022-08-05 | 山东诺尔生物科技有限公司 | Preparation method of carbomer resin and carbomer resin |
| CN116217796A (en) * | 2023-03-15 | 2023-06-06 | 上海宇昂水性新材料科技股份有限公司 | Multi-copolymer based on N-vinyl pyrrolidone and preparation method and application thereof |
| CN116217796B (en) * | 2023-03-15 | 2023-10-03 | 上海宇昂水性新材料科技股份有限公司 | Multi-copolymer based on N-vinyl pyrrolidone and preparation method and application thereof |
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Application publication date: 20120801 |