CN101220263B - Water-based fracturing fluid gelatinizer and producing method thereof - Google Patents
Water-based fracturing fluid gelatinizer and producing method thereof Download PDFInfo
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- CN101220263B CN101220263B CN2007101950336A CN200710195033A CN101220263B CN 101220263 B CN101220263 B CN 101220263B CN 2007101950336 A CN2007101950336 A CN 2007101950336A CN 200710195033 A CN200710195033 A CN 200710195033A CN 101220263 B CN101220263 B CN 101220263B
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Abstract
The invention provides a thickener used for water-base fracturing fluid, and is used for increasing yield and fracturing operation of oil field. The thickener comprises N, N to dialkyl acrylamide, dimethyl diallyl ammonium chloride, acrylonitrile, and methacryloyloxyethyl trimethyl ammonium chloride or acryloyloxyethyl trimethyl ammonium chloride. A method for producing the thickener is a water solution catalyst method is used for producing free radical, thus leading the monomer to polymerize. The thickener provided by the invention has the advantages of resisting high temperature 250 DEG C, resisting cutting, resisting salt, and no leftover, etc.
Description
Technical field
The present invention relates to a kind of viscosifying agent that is used for aqueous fracturing fluid, especially a kind of high temperature resistance reaches 250 ℃ of polymer thickening agents, and the production method of described viscosifying agent.
Background technology
Fracturing technique is conventional yield-increasing technology.Its objective is reservoir is extruded the crack, thus volume increase.Used fracturing liquid must have high viscosity, high shear resistant, high-strength take the characteristics such as the feature of environmental protection that sand and broken glue do not have residue during pressure break.High viscosity has only high viscosity just can make the crack reach the required width and the degree of depth so that it makes seam.Viscosifying agent is as the host of aqueous fracturing fluid, in order to improve of the fracturing fluid viscosity, reduces fracturing fluid leak, suspends and carries propping agent.
At present the viscosifying agent raw material that uses has vegetable jelly and derivative thereof, derivatived cellulose, biological poly-polysaccharide, synthetic polymer, and commonly used is melon glue, hydroxypropyl guar gum, fenugreek gum etc.General synthetic polymer has polyacrylamide, type methylene polyacrylamide etc., and these polymkeric substance are to change polymer property by the control synthesis condition, satisfy the construction needs, and resistance-reducing performance is good, but the problem that exists is that anti-shearing is poor; Salt tolerance is poor; Cull absorption is stopped up serious.Therefore above-mentioned two kinds of synthetic polymers do not obtain widely applying.In recent years, its performance of oligopolymer fracturing liquid that occurs has remedied the shortcoming of general polymerization thing, but the shortcoming that oligopolymer exists is can not superhigh temperature resistant, the bottom that generally can satisfy 90-120 ℃ uses down, and surpass 150 ℃ hot hole for some, these two kinds of products of oligopolymer and guanidine glue are just no longer suitable, they contain hydrolysable group, hydrolysis chain rupture under hot conditions, lose pressure break and be used for thickening, take sand, make the effect of seam, so research and develop the new scientific research task that has that the high temperature resistant novel viscosifying agent that has the oligopolymer performance simultaneously concurrently is domestic and international scientific research personnel.
Summary of the invention
The purpose of this invention is to provide a kind of high-temperature polymer viscosifying agent that is applied in the water-based fracturing, this viscosifying agent has high temperature resistant 250 ℃, has advantages such as anti-shearing, salt tolerant, noresidue simultaneously.
Another object of the present invention is to provide a kind of method of producing above-mentioned viscosifying agent.
Viscosifying agent of the present invention is by N, and N-dialkyl group acrylamide, dimethyl diallyl ammonium chloride (DADMAC), vinyl cyanide (AN), methylacryoyloxyethyl trimethyl ammonium chloride (DMC) or four kinds of monomer copolymerizations of acrylyl oxy-ethyl-trimethyl salmiac (DAC) form.Wherein, described alkyl can be methyl (being N,N-DMAA DMAA), ethyl (being N, N-diethyl acrylamide DEAA).
The weight percent of each monomer of the present invention and water consists of:
(a) N of 25 to 35 weight %, N-dialkyl group acrylamide is N,N-DMAA (DMAA) for example;
(b) dimethyl diallyl ammonium chloride of 10 to 18 weight % (DADMAC);
(c) vinyl cyanide of 5 to 8 weight % (AN);
(d) the methylacryoyloxyethyl trimethyl ammonium chloride (DMC) of 10 to 15 weight % or acrylyl oxy-ethyl-trimethyl salmiac (DAC);
(e) surplus is a water.
More preferably be that the optimum weight per-cent of each monomer and water consists of:
N,N-DMAA (DMAA): 30%
Dimethyl diallyl ammonium chloride (DADMAC): 15%
Vinyl cyanide (AN): 6%
Methylacryoyloxyethyl trimethyl ammonium chloride (DMC) or acrylyl oxy-ethyl-trimethyl salmiac (DAC): 14%
Water: 35%
N, N-DMAA, dimethyl diallyl ammonium chloride, vinyl cyanide, methylacryoyloxyethyl trimethyl ammonium chloride or four kinds of monomer copolymerizations of acrylyl oxy-ethyl-trimethyl salmiac (DAC) can form straight chain and the non-hydrolysable polymkeric substance of ring texture is arranged, this polymkeric substance is completely different with the polymkeric substance that contained acrylamide, Acrylic Acid Monomer in the past, because acrylamide and vinylformic acid contain hydrolyzable amide group and hydroxy-acid group in polymkeric substance in the past.The existence of these hydrolysable group makes the heat resistance of main chain reduce greatly.
A kind of method of producing above-mentioned viscosifying agent, it comprises the steps:
(1) selected N,N-DMAA, dimethyl diallyl ammonium chloride, vinyl cyanide, methylacryoyloxyethyl trimethyl ammonium chloride or four kinds of monomers of acrylyl oxy-ethyl-trimethyl salmiac (DAC) carry out proportioning according to a certain percentage;
(2) said ratio is good monomer is put into the preparation that distilled water carries out solution;
(3) the pH value and the temperature of adjustment solution, the pH value that makes solution is 4.5 ± 0.5, and described temperature is 10 ± 1 ℃;
(4) produce free radical with aqueous solution catalyst method and make above-mentioned monomer generation polymerization.
Described aqueous solution catalyst method just refers in the building-up process of viscosifying agent, protects 15-20 minute to the monomer solution nitrogen blowing for preparing, and adds catalyzer then in solution, brings out 15-20 minute with the generation free radical, thereby makes monomer generation polymerization.Its building-up process can be envisioned for following two kinds of forms:
1. the molecular pattern when using the DMC monomer:
2. the molecular pattern when using the DAC monomer:
In with the process of aqueous solution polymerization, need solution nitrogen blowing 15-20 minute; to remove the dissolved oxygen in anhydrating; under protection of nitrogen gas, add catalyzer then; stop nitrogen blowing and polymeric kettle is airtight; brought out 15-20 minute, and observed whether temperature rise was arranged, 2 ℃ temperature rise is arranged in inductive phase; be considered as causing successfully, otherwise need add the catalyzer re-initiation again.Under the insulation air tight condition, finish, be incubated 3 hours until heating up.
Initiation starting temperature of the present invention is controlled within the 5-20 ℃ of scope.Preferred starting temperature is 10 ± 1 ℃.The pH value is controlled between the 3.5-5.5.PH alkalescence mediator agent mainly contains sodium hydroxide, salt of wormwood, ammoniacal liquor.The pH acid regulator mainly contains phosphoric acid, sulfuric acid, hydrochloric acid, acetate.Preferred pH value is controlled at 4.5 ± 0.5.
Be not particularly limited for described catalyzer.The oxygenant of polymerizing catalyst is persulphate or superoxide, for example ammonium persulphate, Potassium Persulphate, Sodium Persulfate, hydrogen peroxide, benzoyl peroxide or tert-butyl peroxide.Can use oxygenant to form redox system with reductive agent among the present invention, described reductive agent can be sulphite, hydrosulphite, protosalt, organic amine etc.
Azo-compound also is one of preferred catalyzer of the present invention, and the typical azo-compound that is suitable for is Diisopropyl azodicarboxylate (AZDN), 2,2'-Azobis(2,4-dimethylvaleronitrile) (V65), azo diisobutyl amidine hydrochloride (V50) etc.
Can use two or more above-mentioned catalyzer simultaneously, the amount of catalyzer is generally monomeric 0.001-3% weight.
Viscosifying agent of the present invention is applicable to the aqueous fracturing fluid in the oilfield stimulation, be a kind of high temperature resistant, easy dissolving, pollution-free, do not have injury, take good, the good novel high molecular polymer of resistance to elevated temperatures especially of husky performance, its principal feature is can anti-250 ℃ of high temperature, the pressure break that is fit to high-temperature stratum, has higher anti-shearing, to satisfy the pressing crack construction of high flow capacity, have high sand and the no residue taken, reservoir there are not characteristics such as nocuity.
Embodiment
To be described in detail viscosifying agent of the present invention and production process thereof according to specific embodiment below.
Embodiment 1
The weight percent of each monomer and water: DMAA: DADMAC: AN: DMC (DAC): H
2O=30: 15: 6: 14: 35.
The preparation of solution: in the 2000ml beaker, add distilled water 350g, add DMAA monomer 300g, DADMAC monomer 150g, add AN monomer 60g, add DMC (DAC) monomer 140g, stirring and dissolving 30 minutes slowly adds neutralizing agent (sodium hydroxide) to pH4.5 under agitation condition.Continue stirred solution slaking 30 minutes.
The adjustment of solution: regulate pH value to 4.5 ± 0.5 once more, 10 ± 1 ℃ of attemperation.
The polymerization of solution: nitrogen blowing deoxygenation 15-20 minute; under nitrogen protection, add catalyst V 650.5g/L successively; V50 0.05g/L, ammonium persulphate 0.03g/L, sodium formaldehyde sulphoxylate 0.03g/L; stop nitrogen blowing and polymeric kettle is airtight; brought out 15-20 minute, and observed whether temperature rise was arranged, 2 ℃ temperature rise is arranged in inductive phase; be considered as causing successfully, otherwise need add the catalyzer re-initiation again.Under the insulation air tight condition, finish, be incubated 3 hours until heating up.
The aftertreatment of product: the colloid that polymerization is good is carried out granulation, and oven dry is ground into 30 orders, is numbered T-1 and waits detection.
Embodiment 2
Each monomer is in the weight percent of water: DMAA: DADMAC: AN: DMC (DAC): H
2O=25: 15: 6: 14: 40.
The preparation of solution: in the 2000ml beaker, add distilled water 400g, add DMAA monomer 250g, DADMAC monomer 150g, add AN monomer 60g, add DMC (DAC) monomer 140g, stirring and dissolving 30 minutes slowly adds neutralizing agent (sodium hydroxide) to pH4.5 under agitation condition.Continue stirred solution slaking 30 minutes.
The adjustment of solution: regulate pH value to 4.5 ± 0.5 once more, 10 ± 1 ℃ of attemperation.
The polymerization of solution: nitrogen blowing deoxygenation 15-20 minute; under nitrogen protection, add catalyst V 650.5g/L successively; V50 0.04g/L, ammonium persulphate 0.03g/L, sodium formaldehyde sulphoxylate 0.03g/L; stop nitrogen blowing and polymeric kettle is airtight; brought out 15-20 minute, and observed whether temperature rise was arranged, 2 ℃ temperature rise is arranged in inductive phase; be considered as causing successfully, otherwise need add the catalyzer re-initiation again.Under the insulation air tight condition, finish, be incubated 3 hours until heating up.
The aftertreatment of product: the colloid that polymerization is good is carried out granulation, and oven dry is ground into 30 orders, is numbered T-2 and waits detection.
Embodiment 3
The weight percent of each monomer and water: DMAA: DADMAC: AN: DMC (DAC): H
2O=30: 15: 8: 14: 33.
The preparation of solution: in the 2000ml beaker, add distilled water 330g, add DMAA monomer 300g, DADMAC monomer 150g, add AN monomer 80g, add DMC (DAC) monomer 140g, stirring and dissolving 30 minutes slowly adds neutralizing agent (sodium hydroxide) to pH4.5 under agitation condition.Continue stirred solution slaking 30 minutes.
The adjustment of solution: regulate pH value to 4.5 ± 0.5 once more, 10 ± 1 ℃ of attemperation.
The polymerization of liquid: nitrogen blowing deoxygenation 15-20 minute; under nitrogen protection, add catalyst V 650.8g/L successively; V50 0.08g/L, ammonium persulphate 0.04g/L, sodium formaldehyde sulphoxylate 0.04g/L; stop nitrogen blowing and polymeric kettle is airtight; brought out 15-20 minute, and observed whether temperature rise was arranged, 2 ℃ temperature rise is arranged in inductive phase; be considered as causing successfully, otherwise need add the catalyzer re-initiation again.Under the insulation air tight condition, finish, be incubated 3 hours until heating up.
The aftertreatment of product: the colloid that polymerization is good is carried out granulation, and oven dry is ground into 30 orders, is numbered T-3 and waits detection.
Embodiment 4
Each monomer is in the weight percent of water: DMAA: DADMAC: AN: DMC (DAC): H
2O=35: 15: 6: 14: 30.
The preparation of solution: in the 2000ml beaker, add distilled water 300g, add DMAA monomer 350g, DADMAC monomer 150g, add AN monomer 60g, add DMC (DAC) monomer 140g, stirring and dissolving 30 minutes slowly adds neutralizing agent (sodium hydroxide) to pH4.5 under agitation condition.Continue stirred solution slaking 30 minutes.
The adjustment of solution: regulate pH value to 4.5 ± 0.5 once more, 10 ± 1 ℃ of attemperation.
The polymerization of solution: nitrogen blowing deoxygenation 15-20 minute; under nitrogen protection, add catalyst V 650.8g/L successively; V50 0.08g/L, ammonium persulphate 0.05g/L, sodium formaldehyde sulphoxylate 0.05g/L; stop nitrogen blowing and polymeric kettle is airtight; brought out 15-20 minute, and observed whether temperature rise was arranged, 2 ℃ temperature rise is arranged in inductive phase; be considered as causing successfully, otherwise need add the catalyzer re-initiation again.Under the insulation air tight condition, finish, be incubated 3 hours until heating up.
The aftertreatment of product: the colloid that polymerization is good is carried out granulation, and oven dry is ground into 30 orders, is numbered T-4 and waits detection.
Embodiment 5
Each monomer is in the weight percent of water: DMAA: DADMAC: AN: DMC (DAC): H
2O=30: 10: 8: 15: 37.
The preparation of solution: in the 2000ml beaker, add distilled water 370g, add DMAA monomer 300g, DADMAC monomer 100g, add AN monomer 80g, add DMC (DAC) monomer 150g, stirring and dissolving 30 minutes slowly adds neutralizing agent (sodium hydroxide) to pH4.5 under agitation condition.Continue stirred solution slaking 30 minutes.
The adjustment of solution: regulate pH value to 4.5 ± 0.5 once more, 10 ± 1 ℃ of attemperation.
The polymerization of solution: nitrogen blowing deoxygenation 15-20 minute; under nitrogen protection, add catalyst V 650.5g/L successively; V50 0.04g/L, ammonium persulphate 0.02g/L, sodium formaldehyde sulphoxylate 0.02g/L; stop nitrogen blowing and polymeric kettle is airtight; brought out 15-20 minute, and observed whether temperature rise was arranged, 2 ℃ temperature rise is arranged in inductive phase; be considered as causing successfully, otherwise need add the catalyzer re-initiation again.Under the insulation air tight condition, finish, be incubated 3 hours until heating up.
The aftertreatment of product: the colloid that polymerization is good is carried out granulation, and oven dry is ground into 30 orders, is numbered T-5 and waits detection.
The main polymerization catalyzed agent prescription of above-mentioned real embodiment gathers (as table 1).
Table 1
| Numbering | T-1 | T-2 | T-3 | T-4 | T-5 | |
| g/L | V65 | 0.5 | 0.5 | 0.8 | 0.8 | 0.5 |
| V50 | 0.05 | 0.04 | 0.08 | 0.08 | 0.04 | |
| AO1 | 0.03 | 0.03 | 0.04 | 0.05 | 0.02 | |
| NFS | 0.03 | 0.03 | 0.04 | 0.05 | 0.02 |
Wherein, AO1 is an ammonium persulphate, and NFS is a sodium formaldehyde sulphoxylate
The foregoing description product is carried out fundamental property detect (result such as table 2).
Table 2
| Project | T-1 | T-2 | T-3 | T-4 | T-5 | |
| Outward appearance | White powder | White powder | White powder | White powder | White powder | |
| Solid content, % | 89.0 | 90.1 | 90.0 | 89.9 | 90.6 | |
| Granularity, % | ≤ 30 orders | The all-pass mistake | The all-pass mistake | The all-pass mistake | The all-pass mistake | The all-pass mistake |
| UL viscosity, cps | 3.5 | 4.0 | 3.2 | 3.8 | 2.5 | |
| Viscosity at ambient temperature, mpa.s | 16 | 21 | 13 | 19 | 10 |
The said products is carried out the detection (result such as table 3) of use properties aspect
Table 3
| Project | T-1 | T-2 | T-3 | T-4 | T-5 |
| Viscosity at ambient temperature, mpa.s | 16 | 21 | 13 | 19 | 10 |
| Cold cross-linking under 0.3% consumption | Crosslinked adjustable extension | Crosslinked hanging | A little less than crosslinked, partly hang | A little less than crosslinked, partly hang | Crosslinked hanging |
| Normal temperature is taken sand | Can take | Can take | Can take | Can take | Can take |
| High speed shear was taken sand after 1 minute | Evenly take sand | More evenly take sand | Evenly take sand | Evenly take sand | More evenly take sand |
| Shear the viscosity of temperature variation (mps.s) in time in the RV20 rheometer | |||||
| 0.36min，20.8℃ | 410.65 | 542.3 | 326.1 | 297.0 | 531.2 |
| 2.08min，37.1℃ | 582.43 | 509.4 | 385.5 | 308.69 | 502.0 |
| 6.12min，58.8℃ | 511.41 | 466.59 | 310.09 | 271.4 | 347.52 |
| 10.19min，96.7℃ | 408.6 | 393.8 | 265.87 | 265.3 | 299.6 |
| 19.86min，132.1℃ | 631.5 | 308.06 | 192.50 | 210.54 | 206.5 |
| 30.75min，186.8℃ | 311.3 | 265.5 | 152.30 | 173.5 | 135.6 |
| 60.0min，248.1℃ | 128.89 | 97.47 | 92.89 | 99.5 | 88.5 |
| 90.0min，250.1℃ | 99.32 | 72.30 | 80.14 | 74.05 | 76.3 |
| 120.0min，251.2℃ | 79.16 | 53.4 | 68.45 | 57.64 | 65.0 |
From top detected result, the T-1 product is to carry out the product that polymerization obtains according to viscosifying agent prescription of the present invention, and its heat-resisting property can reach 250 ℃, and have high anti-shearing, to characteristic such as storage no nocuity etc.
Claims (7)
1. viscosifying agent that is used for aqueous fracturing fluid, it is characterized in that: described viscosifying agent is by N, N-dialkyl group acrylamide, dimethyl diallyl ammonium chloride, vinyl cyanide, methylacryoyloxyethyl trimethyl ammonium chloride or four kinds of monomer copolymerizations of acrylyl oxy-ethyl-trimethyl salmiac form; The weight proportion of each monomer and water is specially in polymerization process:
(a) N of 25 to 35 weight %, N-dialkyl group acrylamide;
(b) dimethyl diallyl ammonium chloride of 10 to 18 weight % (DADMAC);
(c) vinyl cyanide of 5 to 8 weight % (AN);
(d) the methylacryoyloxyethyl trimethyl ammonium chloride (DMC) of 10 to 15 weight % or acrylyl oxy-ethyl-trimethyl salmiac (DAC);
(e) surplus is a water.
2. viscosifying agent as claimed in claim 1 is characterized in that: described N, N-dialkyl group acrylamide are N,N-DMAA (DMAA).
3. method of producing the described viscosifying agent of claim 1, it comprises the steps:
(1) selected N,N-DMAA, dimethyl diallyl ammonium chloride, vinyl cyanide, methylacryoyloxyethyl trimethyl ammonium chloride or four kinds of monomers of acrylyl oxy-ethyl-trimethyl salmiac carry out proportioning according to the ratio described in the claim 1;
(2) said ratio is good monomer is put into the preparation that distilled water carries out solution;
(3) the pH value and the temperature of adjustment solution make the pH value 4.5 ± 0.5, and described temperature is 10 ± 1 ℃;
(4) monomer solution for preparing is added in the reaction vessel, protect 15-20 minute, in solution, add catalyzer then, bring out 15-20 minute with the generation free radical, thereby make monomer generation polymerization to the monomer solution nitrogen blowing for preparing.
4. method as claimed in claim 3 is characterized in that: the weight ratio of described four kinds of monomers and water is:
N,N-DMAA (DMAA): 30%
Dimethyl diallyl ammonium chloride (DADMAC): 15%
Vinyl cyanide (AN): 6%
Methylacryoyloxyethyl trimethyl ammonium chloride (DMC) or acrylyl oxy-ethyl-trimethyl salmiac (DAC): 14%
Water: 35%.
5. method as claimed in claim 3 is characterized in that: described catalyzer is persulphate or superoxide; Perhaps form redox system with reductive agent for persulphate or superoxide; It perhaps is azo-compound; Described catalyzer or form by two or more catalyzer in the above-mentioned catalyst type.
6. method as claimed in claim 5 is characterized in that: described persulphate is one or more in ammonium persulphate, Potassium Persulphate, the Sodium Persulfate; Described superoxide is one or more in hydrogen peroxide, benzoyl peroxide and the tert-butyl peroxide; Described reductive agent is one or more in sulphite, hydrosulphite, the organic amine; Described azo-compound is one or more in Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), the azo diisobutyl amidine hydrochloride.
7. method as claimed in claim 3 is characterized in that: the amount of catalyzer is the 0.001-3% of monomer weight.
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| CN101481608B (en) * | 2009-01-19 | 2011-08-10 | 中国石油大学(华东) | Clean fracturing fluid and use thereof |
| CN101857658B (en) * | 2009-04-09 | 2012-07-04 | 北京佛瑞克技术发展有限公司 | Copolymer for acid fracturing retarded gel acid and preparation method thereof |
| CN106883835A (en) * | 2017-03-14 | 2017-06-23 | 中国石油集团渤海钻探工程有限公司 | Self-association fracturing fluid system with control water function and preparation method thereof |
| CN110093148A (en) * | 2019-04-10 | 2019-08-06 | 南通科益化工有限公司 | A kind of hydrochlorate reaction reduction of speed agent and preparation method thereof |
| CN110423602A (en) * | 2019-07-09 | 2019-11-08 | 华东理工大学 | A kind of superhigh temperature resistant polymer fracturing fluid system |
| CN114790385A (en) * | 2021-01-25 | 2022-07-26 | 中国石油天然气股份有限公司 | Calcium chloride-weighted high-density slickwater as well as preparation method and application thereof |
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Effective date of registration: 20190507 Address after: 226400 North Road of Yangkou Port Lingang Industrial Park, Changsha Town, Rudong County, Nantong City, Jiangsu Province Patentee after: Nantong Keyi Chemical Co., Ltd. Address before: 101309 South Yangmu Road, Qianwanggezhuang Village, Mulin Town, Shunyi District, Beijing Patentee before: Beijing Xitao Polymer Research Center |
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