CN106047333A - High-temperature-resistant gelling agent in acid liquid and method for preparing high-temperature-resistant gelling agent - Google Patents
High-temperature-resistant gelling agent in acid liquid and method for preparing high-temperature-resistant gelling agent Download PDFInfo
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/72—Eroding chemicals, e.g. acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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Abstract
The invention discloses a high-temperature-resistant gelling agent in acid liquid and a method for preparing the high-temperature-resistant gelling agent. Acrylamide monomers, acryloyloxyethyl trimethyl ammonium chloride monomers and third monomers are polymerized to obtain the high-temperature-resistant gelling agent. The method includes adding azo initiators, chain transfer agents, oxidation and reduction initiators and iron ion complexing agents during polymerization reaction to obtain reaction products; granulating and drying the reaction products to obtain the high-temperature-resistant gelling agent. The high-temperature-resistant gelling agent in the acid liquid and the method have the advantages that the high-temperature-resistant gelling agent is easy to synthesize, gelling acid liquid systems are stable in performance, easy to prepare and convenient to construct, can be applied to high-temperature carbonate rock acidizing construction, are high-temperature-resistant and salt-resistant and are excellent in retardance, filtration reduction, fracture forming and resistance decrease performance, secondary damage can be alleviated, the flow guide capacity of acid erosion fracture can be effectively improved, penetration distances of acid can be effectively extended, and the deep acidizing purpose can be achieved.
Description
Technical field
The present invention relates to oilfield reservoir renovation technique field, particularly relate to a kind of high temperature resistant acid liquor gellant and preparation side thereof
Method.
Background technology
Progressively turn to superhigh temperature reservoir along with In Oil Field Exploration And Development, the most conventional gelled acid system uses temperature to be respectively less than
150 DEG C, it is difficult to meet the needs of on-the-spot reservoir acidfracturing treatment.Middle oil Tarim Basin, the temperature of middle petrochemical industry northwest office major part well
Average all between 160-180 DEG C, small part well has reached 190 DEG C, and the North China Oilfield hill reservoir well temperature at middle part reaches especially
201 DEG C (cattle Dong1Jing), NW Hebei hill reservoir well temperature the most all at about 160-180 DEG C, current superelevation hot-well acidfracturing treatment
In the Major Difficulties that faces be well temperature superelevation, conventional acid liquid performance index is extremely difficult to requirement, and existing way be use clear
Water or the cooling of fracturing fluid pit shaft, re-use conventional acid liquid system and transform, thus considerably increase the risk of reservoir damage,
Too increase the complexity of construction simultaneously.The domestic reservoir acid liquid for acid fracturing system substantially dependence on import more than 160 DEG C, significantly
Add production cost.
The SGA-HT high temperature gelled acid system of Halliburton Company of the U.S., this Type of Collective in external high temperature resistance gelled acid system
Thing stability in high concentrated acid is preferable, and maximum operation (service) temperature has reached 204 DEG C.Domestic aspect, Southwest Oil branch company grinds
Study carefully and define a set of high temperature gelled acid system being suitable for 140 DEG C-160 DEG C.Oil Exploration in China developmental research alure mill branch
Developing a kind of VY-101 gellant uses temperature at 120 DEG C-130 DEG C.Therefore 180 DEG C of gel acid acid fluid system of heatproof are carried out
Develop the most necessary.
Present Domestic acid liquor gellant majority is modified propylene amide copolymer, and the gel acid acid system formed is only capable of
Meet less than 150 DEG C stratum constructions, at a higher temperature almost without viscosity, it is impossible to play good retarded acting, only have few
Number offshore company has 180 DEG C of gel acid acid systems of heatproof.The domestic reservoir acid liquid for acid fracturing system more than 160 DEG C substantially depends on
Rely import, considerably increase production cost.
Summary of the invention
In view of this, it is contemplated that propose a kind of high temperature resistant acid liquor gellant and preparation method thereof, to solve existing skill
In art, reservoir acid liquid for acid fracturing system resistance to elevated temperatures is poor, the problem that cost is high.
For reaching above-mentioned purpose, the technical scheme is that and be achieved in that: a kind of high temperature resistant acid liquor gellant, its system
Standby raw material includes acrylamide monomer, acrylyl oxy-ethyl-trimethyl salmiac monomer, Third monomer, also includes accounting for above-mentioned three kinds
The azo-initiator of monomer gross mass 0.6-0.8 ‰, account for the chain-transferring agent of above-mentioned three kinds of monomer gross masses 0.2-0.3 ‰, account for
The oxidizing initiators of above-mentioned three kinds of monomer gross masses 0.4-0.6 ‰, the reduction accounting for above-mentioned three kinds of monomer gross masses 0.4-0.6 ‰ are drawn
Send out agent, account for the iron ion chelating agent of above-mentioned three kinds of monomer gross masses 0.1-0.2 ‰, described acrylamide monomer, acryloyl-oxy second
Mass ratio between base trimethyl ammonium chloride monomer, Third monomer three is 38～55:35～50:1～10, described Third monomer
For any one in acrylic acid, itaconic acid, three kinds of compounds of 1,2,3-tricarboxylic acids butylene.
Preferably, acrylyl oxy-ethyl-trimethyl salmiac monomer is alkene acyloxyethyl trimethyl ammonium chloride 80% aqueous solution list
Body.
Preferably, azo-initiator is azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo-bis-isobutyrate hydrochloride, azo
Any one in two isobutyl imidazoline hydrochloride four kinds compounds.
Preferably, chain-transferring agent is sodium formate.
Preferably, oxidizing initiators is potassium peroxydisulfate, and reduction initiator is sodium sulfite.
Preferably, iron ion chelating agent is b diammonium edta or triethylene tetramine pentaacetic acid five sodium.
The preparation method of a kind of high temperature resistant acid liquor gellant, comprises the following steps successively:
(1) preparation reaction mother liquor: by acrylamide monomer, acrylyl oxy-ethyl-trimethyl salmiac monomer, Third monomer
Dissolve in deionized water, stir, it is thus achieved that above-mentioned three kinds of monomer total mass fraction are the aqueous solution of 30%-35%, then add
Enter Na2CO3Regulation solution ph, to 11-12, stirs, it is thus achieved that reaction mother liquor, is inserted in polyplant by mother solution；
(2) when the temperature of mother solution is 8 DEG C, in mother solution, high-purity N it is passed through2；
(3) polyreaction: be sequentially added into azo-initiator, chain-transferring agent, oxidoreduction in the mother solution in step (2)
Initiator, iron ion chelating agent, fully reaction 1 hour, then insulation 3 hours；
(4) polymer obtained after polyreaction in step (3) is taken out pelletize, dries 4-5 hour, pulverize and make gelling
Agent.
Preferably, drying temperature in step (4) is 60 DEG C.
Relative to prior art, one of the present invention is high temperature resistant acid liquor gellant and preparation method thereof, have following
Advantage:
(1) the high temperature resistant acid liquor gellant of one of the present invention, can apply in high temperature carbonate rock acidizing treatment,
High temperature resistance, anti-salt, have good slow, filtrate reducing, make seam and the performance of fall resistance, can effectively alleviate secondary injury, effectively
Improve flow conductivity and the penetration range of acid of acid-etched fracture, reach the purpose of deep acidizing.
(2) preparation method of a kind of high temperature resistant acid liquor gellant of the present invention, gellant synthesis is simple, gel acid acid
Liquid system stable performance, preparation is simple, easy construction, can be efficiently applied to high temperature carbonate rock acidifying rebuilding construction.
Accompanying drawing explanation
Fig. 1 be the gel acid for preparing of the high temperature resistant acid liquor gellant prepared by embodiment 1 at 180 DEG C, 170s-1
Curve chart during viscous under shear rate.
Detailed description of the invention
Below in conjunction with specific embodiment, present disclosure is further illustrated.
Embodiment 1
(1) preparation reaction mother liquor: by 66g acrylamide monomer, 75g acrylyl oxy-ethyl-trimethyl salmiac monomer
(80% aqueous solution), 2g acrylic acid, dissolve in the deionized water of 300g, stir, be subsequently adding Na2CO3Regulation pH value of solution
Value, is 11 to pH value, stirs, it is thus achieved that reaction mother liquor, inserted in polyplant by mother solution；
(2) when the temperature of mother solution is 8 DEG C, in mother solution, high-purity N it is passed through2；
(3) polyreaction: the mother solution in step (2) is sequentially added into 0.11g azo two isobutyl imidazoline hydrochloride,
0.03g sodium formate, 0.06g potassium peroxydisulfate, 0.06g sodium sulfite, 0.03g triethylene tetramine pentaacetic acid five sodium, fully react 1
Hour, then insulation 3 hours；
(4) polymer that obtains after polyreaction in step (3) taking out pelletize, is dried 5 hours at 60 DEG C, pulverizing is made
Gellant.
Embodiment 2
(1) preparation reaction mother liquor: by 50g acrylamide monomer, 56.7g acrylyl oxy-ethyl-trimethyl salmiac monomer
(80% aqueous solution), 5g itaconic acid, dissolve in the deionized water of 186.5g, stir, be subsequently adding Na2CO3Regulation pH value of solution
Value, is 12 to pH value, stirs, it is thus achieved that reaction mother liquor, inserted in polyplant by mother solution；
(2) when the temperature of mother solution is 8 DEG C, in mother solution, high-purity N it is passed through2；
(3) polyreaction: the mother solution in step (2) is sequentially added into 0.07g azodiisobutyronitrile, 0.03g sodium formate,
0.07g potassium peroxydisulfate, 0.07g sodium sulfite, 0.01g b diammonium edta, fully reaction 1 hour, then insulation 3 hours；
(4) polymer that obtains after polyreaction in step (3) taking out pelletize, is dried 5 hours at 60 DEG C, pulverizing is made
Gellant.
Embodiment 3
(1) preparation reaction mother liquor: by 38.5g acrylamide monomer, 43.7g acrylyl oxy-ethyl-trimethyl salmiac monomer
(80% aqueous solution), 10g acrylic acid, dissolve in the deionized water of 155g, stir, be subsequently adding Na2CO3Regulation pH value of solution
Value, is 12 to pH value, stirs, it is thus achieved that reaction mother liquor, inserted in polyplant by mother solution；
(2) when the temperature of mother solution is 8 DEG C, in mother solution, high-purity N it is passed through2；
(3) polyreaction: the mother solution in step (2) is sequentially added into 0.06g azo two isobutyl imidazoline hydrochloride,
0.02g sodium formate, 0.04g potassium peroxydisulfate, 0.04g sodium sulfite, 0.01g b diammonium edta, fully reaction 1 hour, so
Rear insulation 3 hours；
(4) polymer that obtains after polyreaction in step (3) taking out pelletize, is dried 5 hours at 60 DEG C, pulverizing is made
Gellant.
Embodiment 4
(1) preparation reaction mother liquor: by 66g acrylamide monomer, 75g acrylyl oxy-ethyl-trimethyl salmiac monomer
(80% aqueous solution), 2g acrylic acid, dissolve in the deionized water of 310g, stir, be subsequently adding Na2CO3Regulation pH value of solution
Value, is 11 to pH value, stirs, it is thus achieved that reaction mother liquor, inserted in polyplant by mother solution；
(2) when the temperature of mother solution is 8 DEG C, in mother solution, high-purity N it is passed through2；
(3) polyreaction: the mother solution in step (2) is sequentially added into 0.11g azo two isobutyl imidazoline hydrochloride,
0.03g sodium formate, 0.06g potassium peroxydisulfate, 0.06g sodium sulfite, 0.03g triethylene tetramine pentaacetic acid five sodium, fully react 1
Hour, then insulation 3 hours；
(4) polymer that obtains after polyreaction in step (3) taking out pelletize, is dried 5 hours at 60 DEG C, pulverizing is made
Gellant.
Embodiment 5
(1) preparation reaction mother liquor: by 50g acrylamide monomer, 45g acrylyl oxy-ethyl-trimethyl salmiac monomer
(80% aqueous solution), 5g itaconic acid, dissolve in the deionized water of 217g, stir, be subsequently adding Na2CO3Regulation pH value of solution
Value, is 12 to pH value, stirs, it is thus achieved that reaction mother liquor, inserted in polyplant by mother solution；
(2) when the temperature of mother solution is 8 DEG C, in mother solution, high-purity N it is passed through2；
(3) polyreaction: the mother solution in step (2) is sequentially added into 0.08g azodiisobutyronitrile, 0.02g sodium formate,
0.03g potassium peroxydisulfate, 0.03g sodium sulfite, 0.02g b diammonium edta, fully reaction 1 hour, then insulation 3 hours；
(4) polymer that obtains after polyreaction in step (3) taking out pelletize, is dried 5 hours at 60 DEG C, pulverizing is made
Gellant.
Embodiment 6
(1) preparation reaction mother liquor: by 38g acrylamide monomer, 35g acrylyl oxy-ethyl-trimethyl salmiac monomer
(80% aqueous solution), 1g1,2,3-tricarboxylic acids butylene, dissolve in the deionized water of 172g, stir, be subsequently adding Na2CO3Adjust
Joint solution ph, is 11.5 to pH value, stirs, it is thus achieved that reaction mother liquor, inserted in polyplant by mother solution；
(2) when the temperature of mother solution is 8 DEG C, in mother solution, high-purity N it is passed through2；
(3) polyreaction: the mother solution in step (2) is sequentially added into 0.05g 2,2'-Azobis(2,4-dimethylvaleronitrile), 0.02g sodium formate,
0.02g Ammonium persulfate., 0.03g sodium sulfite, 0.01g triethylene tetramine pentaacetic acid five sodium, fully reaction 1 hour, then protects
Temperature 3 hours；
(4) polymer that obtains after polyreaction in step (3) taking out pelletize, is dried 4 hours at 60 DEG C, pulverizing is made
Gellant.
Embodiment 7
(1) preparation reaction mother liquor: by 55g acrylamide monomer, 50g acrylyl oxy-ethyl-trimethyl salmiac monomer
(80% aqueous solution), 10g1,2,3-tricarboxylic acids butylene, dissolve in the deionized water of 250g, stir, be subsequently adding Na2CO3
Regulation solution ph, is 11 to pH value, stirs, it is thus achieved that reaction mother liquor, inserted in polyplant by mother solution；
(2) when the temperature of mother solution is 8 DEG C, in mother solution, high-purity N it is passed through2；
(3) polyreaction: be sequentially added into 0.08g azo-bis-isobutyrate hydrochloride, 0.03g in the mother solution in step (2)
Sodium formate, 0.06g potassium peroxydisulfate, 0.06g sodium sulfite, 0.02g b diammonium edta, fully reaction 1 hour, is then incubated
3 hours；
(4) polymer that obtains after polyreaction in step (3) is taken out pelletize, is dried 4.5 hours at 60 DEG C, pulverize system
Become gellant.
In order to prove the technique effect of the present invention further, the high temperature resistant acid solution gelling that embodiment 1 is prepared by we
The gel acid that agent prepares under the conditions of 180 DEG C, 170s-1Rheological property under shear rate is tested, and test result is such as
Shown in Fig. 1.
By Fig. 1 it will be seen that gel acid acid fluid system viscosity at ambient temperature 60mpa s, under the conditions of 180 DEG C, 170s-1
Acid liquid viscosity 30mpa s after down cut 60min, demonstrates good temperature and shearing sustainability.
The foregoing is only the preferred embodiment of the invention, not in order to limit the invention, all at this
Within the spirit of innovation and creation and principle, any modification, equivalent substitution and improvement etc. made, should be included in the invention
Protection domain within.
Claims (8)
1. a high temperature resistant acid liquor gellant, it is characterised in that prepare raw material and include acrylamide monomer, acrylyl oxy-ethyl three
Ammonio methacrylate monomer, Third monomer, also include accounting for the azo-initiator of above-mentioned three kinds of monomer gross masses 0.6-0.8 ‰, accounting for
The chain-transferring agent of above-mentioned three kinds of monomer gross masses 0.2-0.3 ‰, the oxidation accounting for above-mentioned three kinds of monomer gross masses 0.4-0.6 ‰ cause
Agent, account for above-mentioned three kinds of monomer gross masses 0.4-0.6 ‰ reduction initiator, account for above-mentioned three kinds of monomer gross masses 0.1-0.2 ‰
Iron ion chelating agent, between described acrylamide monomer, acrylyl oxy-ethyl-trimethyl salmiac monomer, Third monomer three
Mass ratio is 38～55:35～50:1～10, and described Third monomer is acrylic acid, itaconic acid, 1,2,3-tricarboxylic acids butylene three kinds
Any one in compound.
One the most according to claim 1 is high temperature resistant acid liquor gellant, it is characterised in that described acrylyl oxy-ethyl front three
Ammonium chloride monomer is alkene acyloxyethyl trimethyl ammonium chloride 80% aqueous solution monomer.
One the most according to claim 1 is high temperature resistant acid liquor gellant, it is characterised in that described azo-initiator is even
In nitrogen bis-isobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo-bis-isobutyrate hydrochloride, four kinds of compounds of azo two isobutyl imidazoline hydrochloride
Any one.
One the most according to claim 1 is high temperature resistant acid liquor gellant, it is characterised in that described chain-transferring agent is sodium formate.
One the most according to claim 1 is high temperature resistant acid liquor gellant, it is characterised in that described oxidizing initiators is over cure
Acid potassium, described reduction initiator is sodium sulfite.
One the most according to claim 1 is high temperature resistant acid liquor gellant, it is characterised in that described iron ion chelating agent is second
Diammonium tetraacethyl or triethylene tetramine pentaacetic acid five sodium.
7. a preparation method for high temperature resistant acid liquor gellant, comprises the following steps successively:
(1) preparation reaction mother liquor: acrylamide monomer, acrylyl oxy-ethyl-trimethyl salmiac monomer, Third monomer are dissolved in
In deionized water, stir, it is thus achieved that above-mentioned three kinds of monomer total mass fraction are the aqueous solution of 30%-35%, are subsequently adding
Na2CO3Regulation solution ph, to 11-12, stirs, it is thus achieved that reaction mother liquor, is inserted in polyplant by mother solution；
(2) when the temperature of mother solution is 8 DEG C, in mother solution, high-purity N it is passed through2；
(3) polyreaction: be sequentially added into azo-initiator, chain-transferring agent, redox initiation in the mother solution in step (2)
Agent, iron ion chelating agent, fully reaction 1 hour, then insulation 3 hours；
(4) polymer obtained after polyreaction in step (3) is taken out pelletize, dries 4-5 hour, pulverize and make gellant.
The preparation method of a kind of high temperature resistant acid liquor gellant the most according to claim 7, it is characterised in that in step (4)
Drying temperature is 60 DEG C.
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| CN108204231A (en) * | 2016-12-20 | 2018-06-26 | 中国石油天然气股份有限公司 | A kind of evaluation method of carbonate reservoir volume acid fracturing flow conductivity |
| CN114106240A (en) * | 2021-12-16 | 2022-03-01 | 中国石油化工股份有限公司 | Gelling agent for degradable gelled acid system and preparation method thereof |
| CN116731250A (en) * | 2023-06-16 | 2023-09-12 | 广汉市华星新技术开发研究所（普通合伙） | Preparation method of high-temperature-resistant acid liquid gelatinizing agent |
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| CN116731250A (en) * | 2023-06-16 | 2023-09-12 | 广汉市华星新技术开发研究所（普通合伙） | Preparation method of high-temperature-resistant acid liquid gelatinizing agent |
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