CN102372818B - Temperature and salt resistant copolymer for oil field and preparation method thereof - Google Patents
Temperature and salt resistant copolymer for oil field and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a temperature and salt resistant copolymer KWKY-PAD for oil field and a preparation method thereof, and mainly solves the problem that polyacrylamide is easy to hydrolyze at high temperature and high salinity in the prior art. The temperature and salt resistant copolymer KWKY-PAD as shown in formula (I) is obtained by the copolymerization of acrylamide and a N-alkyl substituted acrylamide derivative. The technical scheme provided by the invention greatly solves the problem. By the adoption of the preparation method, the hydrolytic stability of the copolymer is raised,and the copolymer has good viscosifying ability and hydrolytic stability at high temperature and high salinity as well as good temperature and salt resistance. The copolymer provided by the inventioncan be used in an oil displacement agent for oil extraction in oil field, and also can be used in oil field application fields of a thickening agent of fracturing fluids, a water plugging profile modification agent, a drilling fluid processing agent and the like. In addition, the preparation method requires less monomer, is simple and is suitable for industrialization.
Description
Technical field
The present invention relates to a kind of oil field heat-resistant salt-resistant multipolymer KWKY-PAD and preparation method thereof.
Background technology
Along with the development of petroleum exploration and development, tertiary oil recovery has begun to employ the oil reservoir of some high temperature and high salinities, and such as three class oil reservoirs of Shengli Oil Field, its salinity reaches more than the 30000mg/L, and temperature reaches 80~93 ℃.In this class oil reservoir, common partially hydrolyzed polyacrylamide is easy to hydrolysis, thereby causes tackifying ability greatly to reduce, and does not have the effect of good raising recovery ratio.Therefore, in the urgent need to a kind of under the high temperature and high salinity condition, the salt-tolerance product that stability to hydrolysis improves.At present, many investigators have launched a large amount of research, set about from the thinking of Molecular Structure Design, and the salt-tolerance products such as multipolymer of amphiphilic polymers, hydrophobic associated polymer, polynary combination multipolymer and novel molecular structure have been synthesized in design.
Patent CN 1814637A discloses a kind of preparation method of temperature-tolerant anti-salt polyacrylamide, introduce three kinds of heat-resistant salt-resistant monomers and acrylamide copolymerization, synthesized acrylamide/2-acrylamide-2-methylpro panesulfonic acid/methacrylic acid/dimethyl diallyl ammonium chloride tetrapolymer, acrylamide/2-acrylamide reaches-2-methyl propane sulfonic acid/methylene-succinic acid/heat-resistant salt-resistant multipolymers such as acrylyl oxy-ethyl-trimethyl salmiac tetrapolymer, the heat-resistant salt-resistant performance of the product that these polymkeric substance have improved really, but can only satisfy salinity and be lower than 10000mg/L, temperature is lower than under 65 ℃ the condition, can not satisfy the application demand under higher temperature and the salinity condition.
Patent CN 1876751A discloses a kind of braided comb-shaped thickener for salt-resistant polymer, this thickening material heat-resistant salt-resistant Performance Ratio comb shape heat-resistant salt-resistant thickening agent of copolymer will be got well, and molecular weight is lower, at grand celebration clear water (total mineralization 1000mg/L, calcium ions and magnesium ions 15mg/L wherein), grand celebration sewage (total mineralization 4000mg/L, calcium ions and magnesium ions 60mg/L wherein), huge port sewage (total mineralization 5024mg/L, calcium ions and magnesium ions 60mg/L wherein) Efficient Adhesive Promotion in is better than plain polypropylene acid amides product and comb shaped antisalt polymer industrial goods, the requirement of grand celebration two class oil reservoir tertiary oil recoveries can be adapted to, but still the more requirement of tertiary oil recovery in the high salinity reservoirs was of higher temperature can't be satisfied.
Polymkeric substance in the above document, or it is a lot of to introduce monomer, but the effect that plays is not very desirable, or by increasing the particular configuration of copolymer molecule chain, improve the temperature resistant antisalt performance of polymkeric substance, but still can not the hydrolysis of establishment amide group under the high temperature and high salinity condition.Therefore, when being used for high temperature and high salt oil deposit, especially during Shengli Oil Field three class oil reservoir, all there is the undesirable problem of Efficient Adhesive Promotion, still can not satisfies the application conditions of three class oil reservoirs of high temperature and high salinity.
Summary of the invention
One of technical problem to be solved by this invention is the problem that partially hydrolyzed polyacrylamide is easy to be hydrolyzed under the high temperature and high salinity in the prior art, and a kind of new multipolymer KWKY-PAD is provided, and this multipolymer has advantages of that stability to hydrolysis is good.Two of technical problem to be solved by this invention provides a kind of preparation method of the multipolymer corresponding with one of technical solution problem.
For one of solving the problems of the technologies described above, technical scheme of the present invention is as follows: a kind of oil field heat-resistant salt-resistant multipolymer KWKY-PAD has following logical formula I:
In the formula, R
1, R
2Be C
1~C
16Alkyl, x, y, m are respectively the structural unit mole numbers of acrylamide, hydrolysis acrylamide, N-AAM.
For solve the problems of the technologies described above two, technical scheme of the present invention is as follows: the preparation method of a kind of heat-resistant salt-resistant multipolymer KWKY-PAD may further comprise the steps:
A) the first monomer, the second monomer are made into the aqueous solution I that total mass concentration is 10~45w.t.%;
B) in the solution I, lead to nitrogen deoxidation 15~35 minutes, under 5~25 degree temperature, add the composite initiation system that accounts for monomer mass 0.001~3%, obtain the solution II; Wherein composite initiation system comprises following component by weight percentage: (A) 15~85% oxygenant; (B) 5~75% reductive agent; (C) 10~80% tertiary amines functional monomer.
C) in the solution II, lead to nitrogen deoxidation 15~35 minutes, under 5~25 degree temperature, caused 15~90 minutes, be warmed up to again 30~60 ℃, continue isothermal reaction 2~16 hours, the colloidal product I that obtains;
D) adding concentration in the colloidal product I is 1~30% alkali lye, is warming up to 75~95 ℃, is hydrolyzed 0.5~3 hour under this temperature, obtains colloidal product II;
E) colloidal product II is dry, pulverize, sieve after, make Powdered heat-resistant salt-resistant multipolymer KWKY-PAD.
In the technique scheme, the preferred acrylamide of the first monomer, the preferred N,N-DMAA of the second monomer, N, a kind of in the N-diethyl acrylamide; The total massfraction preferred 15~35% of the first monomer and the second monomer in the monomer solution; Composite initiation system concentration preferably accounts for monomer mass mark 0.003~1.5%; The preferred Potassium Persulphate of oxygenant and ammonium persulphate in the composite initiation system, the preferred sodium bisulfite of reductive agent, tertiary amines function monomer preferable methyl vinylformic acid N, N-dimethylaminoethyl; Preferred 5~15 ℃ of kick off temperature, preferred 30~60 minutes of initiation time; Preferred 30~50 ℃ of polymerization temperature, preferred 4~12 hours of polymerization reaction time; Alkali lye is preferably sodium hydroxide solution, and concentration is preferred 5~15%, preferred 80~90 ℃ of hydrolysis temperature, preferred 1~3 hour of hydrolysis time.
The angle of the present invention's amide group facile hydrolysis in high temperature and high salinity salt solution from suppress polymkeric substance; make the stability-enhanced monomer that maybe can suppress amide group hydrolysis in the polymkeric substance of amide group by in molecular chain, introducing; with the acrylamide copolymerization; the interaction of functional group and amide group by this type of monomer; such as hydrogen bond action etc.; amide group is formed protection; suppress the hydrolysis of amide group; thereby improve the stability to hydrolysis of polymkeric substance; and then the heat-resistant salt-resistant performance of raising polymkeric substance, a kind of new heat-resistant salt-resistant multipolymer KWKY-PAD and preparation method thereof is provided.This multipolymer is under high temperature and high salinity, and stability to hydrolysis improves, and has stronger Efficient Adhesive Promotion; This preparation method's technical process is comparatively easy, is conducive to suitability for industrialized production.
Use technique scheme, the heat-resistant salt-resistant multipolymer KWKY-PAD that obtains, molecular weight>10
7Reaching (wherein calcium ions and magnesium ions concentration is greater than 500mg/L), temperature about 20000mg/L in salinity reaches in the salt solution under the high temperature and high salinity condition more than 65 ℃, have good solubility, tackifying, and stability to hydrolysis improves, apparent viscosity 〉=21mPas, the viscosity retention ratio behind the high temperature ageing more than 65 ℃ is more than 70%.
Adopt the heat-resistant salt-resistant multipolymer KWKY-PAD of the present invention's preparation, take consumption as 0.1~0.3wt% and the aliphatic acid polyethenoxy ether sulphonic acids tensio-active agent of 0.1~0.4wt% form displacement of reservoir oil composition, under the alkali-free condition, the in-place oil and the water that can be used for the oil field block of comparatively high temps and salinity, measure this oil-displacing agent and won solution apparent viscosity under 65 ℃ of the Tuo Er district Simulated Water greater than 21mPas at Shengli Oil Field, and Shengli Oil Field wins the dynamic interface tension value between the Tuo Er district crude oil, can reach 10
-3~10
-4The ultra low interfacial tension of mN/m, can on the water drive basis, can reach 17.8% by (water drive improves oil recovery factor and reaches 40.6%) raising oil recovery factor through physical simulation displacement test Lab-evaluation at this oil-displacing agent on high temperature, the high salinity reservoir, obtain preferably technique effect.
Description of drawings
After purification of products, use U.S. Nicolet-380FT-IR spectrograph, utilize the KBr pressed disc method to carry out infrared analysis (sweep limit 4000~400cm
-1), Fig. 1 is the infrared spectra of multipolymer among the embodiment 1, has figure can find out 3452.9cm
-1Be NH
2Characteristic peak, 1633.8cm
-1Be the absorption peak of C=O on the acid amides, 1403.1cm
-1Be the absorption peak of the C-N of acid amides, 1454.4 is the flexural vibration absorption peak of methyl, and the characteristic peak of acrylamide, two kinds of monomers of N,N-DMAA has embodiment, proves that products therefrom is the multipolymer of acrylamide, N,N-DMAA really; 1048cm among the figure
-1Near the charateristic avsorption band of C-O-C has appearred, functions monomer methacrylic acid-2-(dimethylamino) ethyl ester has participated in polymerization, gives multipolymer with the special construction characteristics.
The present invention is further elaborated below by embodiment.
Embodiment
[embodiment 1]
The N,N-DMAA of 69.3 parts acrylamides and 5.7 parts is dissolved in 422 parts of water, and making the total massfraction of two kinds of monomers of acrylamide and N,N-DMAA is 15%; Reconcile pH value to 8~10 with 2 parts of sodium hydroxide solutions, pour monomer solution into reaction vessel, making bath temperature is 5 ℃, logical nitrogen deoxygenation 30 minutes; Then add 0.003% composite initiation system: 0.23 part of 0.15% potassium persulfate solution, 0.09% 0.13 part of sodium sulfite solution, 0.6% methacrylic acid N, 0.3 part of N-dimethylaminoethyl; React after 30 minutes, be warmed up to 30 ℃, continue the constant temperature polyreaction after 4 hours, stopped reaction, with the colloidal product that obtains, adding concentration is 5% sodium hydroxide solution 157.6g, under 80 ℃, is hydrolyzed 1 hour, then vacuum-drying, pulverize, namely obtain heat-resistant salt-resistant multipolymer KWKY-PAD, molecular weight 1.2 * 10
7, reaching the viscosity retention ratio that (wherein calcium ions and magnesium ions concentration is greater than 500mg/L), temperature about 20000mg/L reach after aging in the salt solution under the high temperature and high salinity condition more than 65 ℃ in salinity is 71.2%.
[embodiment 2]
With the N of 95 parts acrylamides and 80 parts, N-diethyl acrylamide is dissolved in 293 parts of water, makes acrylamide and N, and the total massfraction of two kinds of monomers of N-diethyl acrylamide is 35%; Reconcile pH value to 8~10 with 2 parts of sodium hydroxide solutions, pour monomer solution into reaction vessel, making bath temperature is 15 ℃, logical nitrogen deoxygenation 30 minutes; Then add 1.5% composite initiation system: 12.5 parts of 3.15% potassium persulfate solutions, 15.75% 12.5 parts of sodium sulfite solution, 5.25% methacrylic acid N, 5 parts of N-dimethylaminoethyls; React after 60 minutes, be warmed up to 50 ℃, continue the constant temperature polyreaction after 12 hours, stopped reaction, with the colloidal product that obtains, adding concentration is 15% sodium hydroxide solution 71.3g, under 90 ℃, is hydrolyzed 3 hours, then vacuum-drying, pulverize, namely obtain heat-resistant salt-resistant multipolymer KWKY-PAD, molecular weight 1.1 * 10
7, reaching the viscosity retention ratio that (wherein calcium ions and magnesium ions concentration is greater than 500mg/L), temperature about 20000mg/L reach after aging in the salt solution under the high temperature and high salinity condition more than 65 ℃ in salinity is 71.8%.
[embodiment 3]
The N,N-DMAA of 138.6 parts acrylamides and 11.4 parts is dissolved in 340 parts of water, and making the total massfraction of two kinds of monomers of acrylamide and N,N-DMAA is 30%; Reconcile pH value to 8~10 with 2 parts of sodium hydroxide solutions, pour monomer solution into reaction vessel, making bath temperature is 5 ℃, logical nitrogen deoxygenation 30 minutes; Then add 0.03% composite initiation system: 5 parts of 0.76% potassium persulfate solutions, 0.23% 1 part of sodium sulfite solution, 0.45% methacrylic acid N, 1 part of N-dimethylaminoethyl; React after 60 minutes, be warmed up to 30 ℃, continue the constant temperature polyreaction after 12 hours, stopped reaction, with the colloidal product that obtains, adding concentration is 10% sodium hydroxide solution 157.6g, under 90 ℃, is hydrolyzed 2 hours, then vacuum-drying, pulverize, namely obtain heat-resistant salt-resistant multipolymer KWKY-PAD, molecular weight 1.8 * 10
7, reaching the viscosity retention ratio that (wherein calcium ions and magnesium ions concentration is greater than 500mg/L), temperature about 20000mg/L reach after aging in the salt solution under the high temperature and high salinity condition more than 65 ℃ in salinity is 72.7%.
[embodiment 4]
With the N of 40.7 parts acrylamides and 34.3 parts, N-diethyl acrylamide is dissolved in 420 parts of water, makes acrylamide and N, and the total massfraction of two kinds of monomers of N-diethyl acrylamide is 15%; Reconcile pH value to 8~10 with 2 parts of sodium hydroxide solutions, pour monomer solution into reaction vessel, making bath temperature is 5 ℃, logical nitrogen deoxygenation 30 minutes; Then add 0.15% composite initiation system: 1 part of 0.45% potassium persulfate solution, 0.15% 1.5 parts of sodium sulfite solution, 0.45% methacrylic acid N, 1 part of N-dimethylaminoethyl; React after 30 minutes, be warmed up to 50 ℃, continue the constant temperature polyreaction after 4 hours, stopped reaction, with the colloidal product that obtains, adding concentration is 7.5% sodium hydroxide solution 45.8g, under 85 ℃, is hydrolyzed 1 hour, then vacuum-drying, pulverize, namely obtain heat-resistant salt-resistant multipolymer KWKY-PAD, molecular weight 1.3 * 10
7, reaching the viscosity retention ratio that (wherein calcium ions and magnesium ions concentration is greater than 500mg/L), temperature about 20000mg/L reach after aging in the salt solution under the high temperature and high salinity condition more than 65 ℃ in salinity is 70.6%.
[embodiment 5]
The N,N-DMAA of 78.4 parts acrylamides and 21.6 parts is dissolved in 395 parts of water, and making the total massfraction of two kinds of monomers of acrylamide and N,N-DMAA is 20%; Reconcile pH value to 8~10 with 2 parts of sodium hydroxide solutions, pour monomer solution into reaction vessel, making bath temperature is 10 ℃, logical nitrogen deoxygenation 30 minutes; Then add 0.009% composite initiation system: 1 part of 0.27% potassium persulfate solution, 0.54% 1 part of sodium sulfite solution, 0.27% methacrylic acid N, 1 part of N-dimethylaminoethyl; React after 45 minutes, be warmed up to 35 ℃, continue the constant temperature polyreaction after 8 hours, stopped reaction, with the colloidal product that obtains, adding concentration is 7% sodium hydroxide solution 156.0g, under 85 ℃, is hydrolyzed 1.5 hours, then vacuum-drying, pulverize, namely obtain heat-resistant salt-resistant multipolymer KWKY-PAD, molecular weight 1.9 * 10
7, reaching the viscosity retention ratio that (wherein calcium ions and magnesium ions concentration is greater than 500mg/L), temperature about 20000mg/L reach after aging in the salt solution under the high temperature and high salinity condition more than 65 ℃ in salinity is 73.2%.
[comparative example 1]
The commonly used partially hydrolyzed polyacrylamide stability to hydrolysis in oil field was poor in the past, under identical examination condition, (viscosity retention ratio is higher with viscosity retention ratio, illustrate that stability to hydrolysis is better) be evaluation index, compare the stability to hydrolysis of commercially available partially hydrolyzed polyacrylamide, self-control partially hydrolyzed polyacrylamide, temperature resistant antisalt multipolymer KWKY-PAD, the results are shown in Table 1.As seen, the viscosity retention ratio of temperature resistant antisalt multipolymer KWKY-PAD is the highest, illustrates that temperature resistant antisalt multipolymer KWKY-PAD stability to hydrolysis of the present invention improves greatly.
Table 1
Sample | Molecular weight *(ten thousand) | Viscosity retention ratio **(%) |
Commercially available HPAM | 2800 | 26.7 |
Self- |
2500 | 50.2 |
KWKY-PAD | 1900 | 73.2 |
*: press the GBT12005.10-92 Molecular Weight for Polyacrylamide and measure (viscosimetry) mensuration intrinsic viscosity, and by [η]=3.73 * 10
-4Mw
0.66Calculate molecular weight
*: in total mineralization be 19334mg/L, wherein the total amount of calcium ion and magnesium ion is in the aqueous solution of 514mg/L, and 1500mg/L polymer concentration solution is at 65 ℃ of apparent viscosity retention rates after aging 7 days.
Claims (1)
1. an oil field is with the preparation method of heat-resistant salt-resistant multipolymer KWKY-PAD, N with 78.4 parts acrylamides and 21.6 parts, the N-DMAA is dissolved in 395 parts of water, and making the total massfraction of two kinds of monomers of acrylamide and N,N-DMAA is 20%; Reconcile pH value to 8~10 with 2 parts of sodium hydroxide solutions, pour monomer solution into reaction vessel, making bath temperature is 10 ℃, logical nitrogen deoxygenation 30 minutes; Then add and account for monomer mass mark 0.009% composite initiation system: 1 part of 0.27% potassium persulfate solution, 0.54% 1 part of sodium sulfite solution, 0.27% methacrylic acid N, 1 part of N-dimethylaminoethyl; React after 45 minutes, be warmed up to 35 ℃, continue the constant temperature polyreaction after 8 hours, stopped reaction, with the colloidal product that obtains, adding concentration is 7% sodium hydroxide solution 156.0g, under 85 ℃, is hydrolyzed 1.5 hours, then vacuum-drying, pulverize, namely obtain heat-resistant salt-resistant multipolymer KWKY-PAD, molecular weight 1.9 * 10
7, reach 20000mg/L in salinity, wherein calcium ions and magnesium ions concentration is 73.2% greater than the viscosity retention ratio that 500mg/L, temperature reach after aging in the salt solution under the high temperature and high salinity condition more than 65 ℃.
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CN107365402B (en) * | 2017-05-02 | 2020-05-12 | 中国石油化工股份有限公司 | Preparation method of micro-branched micro-crosslinked polyacrylamide |
CN113185630B (en) * | 2021-04-22 | 2022-11-01 | 四川川庆井下科技有限公司 | Biodegradable salt-tolerant thickening system and preparation method and application thereof |
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