CN106433599A - Weakly-acidic copolymer fracturing fluid system and preparation method therefor - Google Patents
Weakly-acidic copolymer fracturing fluid system and preparation method therefor Download PDFInfo
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- CN106433599A CN106433599A CN201610680221.7A CN201610680221A CN106433599A CN 106433599 A CN106433599 A CN 106433599A CN 201610680221 A CN201610680221 A CN 201610680221A CN 106433599 A CN106433599 A CN 106433599A
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- copolymer
- fracturing fluid
- fluid system
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- faintly acid
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
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- C—CHEMISTRY; METALLURGY
- 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
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
Abstract
The invention provides a weakly-acidic copolymer fracturing fluid system. The weakly-acidic copolymer fracturing fluid system is prepared from the following ingredients in parts by mass: 0.3-0.6 part of copolymer thickener, 0.4-0.8 part of complex type cross-linker and 98-99 parts of water. By the high-temperature resistant copolymer thickener and the complex type cross-linker which is used under weakly-acidic conditions, the weakly-acidic copolymer fracturing fluid system can form a weakly-acidic system and is a novel fracturing fluid system which has the advantages of adjustable gelatinization time, heat resistance, low residue, low fluid loss and easiness in flowback. The weakly-acidic copolymer fracturing fluid system can be applied to different environments of low seepage, alkali sensitiveness, deep zone, high temperature and the like.
Description
Technical field
The invention belongs to oil-gas reservoir fracturing technique field and be specifically related to a kind of copolymer faintly acid fracturing fluid system and system thereof
Preparation Method.
Background technology
Domestic many oil reservoirs are belonging to the conditions such as hypotonic, low pressure, high temperature, deep layer.And, deep with conventional block exploitation
Entering to carry out, it is more and more important that the exploration in these fields and exploitation have become.The thing followed is the transformation to these reservoirs so that it is
Effective production capacity can be formed.And the pressure break well stimulation that to be reservoir reconstruction maximally efficient and the most frequently used.Thickener is fracturing fluid
In one of most important composition, be mainly thickening, taken sand and reduce fluid loss effect, be to determine fracturing fluid property and pressure break
One of principal element of effect.Existing thickener mainly includes natural plant and synthetic polymer.But it is that typically in hypotonic, low
Under pressure, high temperature deep layer environment, there is the residue temperature difference many, resistance to, the easily weakness such as corruption in the natural plant being acted on；And synthesized polymer
If owner's polyacrylamide, its resistance to gentleness poor-performing of resistance to salinity.Meanwhile, natural plant gum used organic boron mostly is handed over
Connection agent, they are crosslinked under alkaline environment, and are suitable only for temperature 120 DEG C used below, it is impossible to meet more than 140 DEG C
The application of hot environment.Especially for the high stratum of clay content, it is easier to cause alkali quick and cause fine migration so that storage
Layer is by secondary injury.Having reports for work abroad develops the high temperature that fracturing fluid system can be used for 200 DEG C, but fracture flow conductivity and stratum
All can produce very big injury.
Content of the invention
For hypotonic at present, alkali is quick, the problem in the presence of pressure break such as deep layer, high temperature, the present invention provides a kind of copolymerization
Thing faintly acid fracturing fluid system, including thickening agent of copolymer and compound crosslinking agent.Copolymer as thickener is a kind of easy
Dissolve, pollution-free, fanout free region, take that husky performance is good, the good new copolymer of husky performance is taken in especially shearing, have just viscous little, rub
Hinder the features such as low, heatproof is high, gelling strength is big, rheological characteristic is good, residue is few, can serve as different blocks and different geology bars
The thickener of part fracturing liquid.Meanwhile, delay the compound crosslinking agent of release function by introducing to have, enter in acid condition
Row crosslinking, the network structure of strengthening fracturing fluid, thus improve the temperature tolerance of fracturing fluid.In constant temperature 140 DEG C and shear rate
170S-1Under the conditions of, more than continuous shear stress 120min, the viscosity of fracturing fluid is more than 120mPa S.Prove that this fracturing fluid system has
Good resistance to gentle anti-shear performance.And owing to system is that faintly acid has made it more for anti-swollen, the row of helping after fracturing liquid rubber-breaking
Effect, the first-selection of the oil reservoir fracturing reforms such as hypotonic, deep layer, high temperature will be become.
A kind of copolymer faintly acid fracturing fluid system that this invention provides is made up of following component in parts by mass, copolymerization
Thing thickener 0.3-0.6 part, compound crosslinking agent 0.4-0.8 part, water 98-99 part；
Described thickening agent of copolymer is made up of following component in parts by mass：Acrylic monomers 0-2 part, 2-acryloyl
Amine-2-methyl propane sulfonic acid (AMPS) monomer 0-8 part, N, N dimethyl acrylamide monomer 0-2 part, sodium allylsulfonate monomer 0-8
Part, acrylamide monomer 0-25 part, water 50-75 part, described thickening agent of copolymer at least includes above-mentioned 3 kinds of monomers；
Described compound crosslinking agent is made up of following component in parts by mass：Transition metal salt 5-12 part, ligand 25-
45 parts, temperature accelerator 0-0.5 part, complexing agent 0-5 part and solvent 50-60 part, described transition metal salt is zirconates, aluminium salt, iron
One or more of salt, titanium salt and chromic salts, ligand is the organic compound containing lone pair electrons element.Solvent is water and alcohol
At least one, complexing agent is one or more of ethylenediamine tetra-acetic acid (EDTA), polyhydroxy sodium alkoxide and organic acid；Temperature accelerator
For rare earth metal salt.
Described thickening agent of copolymer is non-ionic polyalcohol, and mean molecule quantity is 200-300 ten thousand, have good water solubility,
The characteristics such as thickening capabilities is strong, saline-alkaline tolerance is strong, residue is few, safety and environmental protection.
Described polyhydroxy sodium alkoxide is to state one or more that strong oxidizer is Ammonium Persulfate 98.5, potassium peroxydisulfate and hydrogen peroxide.
Preferably described transition metal salt is at least one of zirconates and aluminium salt.Preferably described rare earth metal salt be cerous sulfate and
At least one of ceric sulfate.
The present invention also provides the synthetic method of a kind of copolymer faintly acid fracturing fluid system, comprises the steps：A. copolymerization
The synthesis of thing thickener：Described monomer is dissolved in water, the catalyst of the 0.05-0.1% adding quality to be monomer total amount, institute
Stating the mixture that catalyst is manganese dioxide and sodium acid carbonate or being strong oxidizer, control reaction temperature is at 30-50 DEG C, with instead
Answer the increase of fluid viscosity, be stepped up reaction temperature, reach 50 DEG C, react 4 hours, reactant is dried, pulverize, i.e. obtain this
The thickening agent of copolymer of invention.
B. the synthesis of compound crosslinking agent：Water and ethanol are mixed, adds transition metal salt, stir, add
Ligand, reacts 2 hours at 85 DEG C, adds complexing agent, temperature accelerator, reacts 4 hours, obtain compound at 80 DEG C
Crosslinking agent.
C. the synthesis of copolymer faintly acid fracturing fluid system：The thickening agent of copolymer that water and step A synthesize is stirred,
Place more than 30min, add the compound crosslinking agent of step B synthesis, stir, obtain copolymer faintly acid fracturing liquid.
Preferably described strong oxidizer is one or more of Ammonium Persulfate 98.5, potassium peroxydisulfate and hydrogen peroxide.
The invention has the beneficial effects as follows：The thickening agent of copolymer of the present invention is a kind of low-molecular-weight, soluble, pollution-free,
Fanout free region, take that husky performance is good, the good new copolymer of husky performance is taken in especially shearing, have that thickening capabilities is strong, saline-alkaline tolerance strong,
Residue is few, just glue the features such as little, frictional resistance is low, heatproof is high, gelling strength is big, rheological characteristic is good, and base fluid pH value is 5-6.
The copolymer of the present invention can select different monomers to be polymerized for different purposes.Height is required to intensity,
Acrylic monomers can be added；Require great thermotolerance, can be selected for acrylic acid and AMPS monomer；Require good salt tolerance, can be selected for AMPS mono-
Body.
This compound crosslinking agent of invention is a kind of novel fire resistant, have and delay release function.It can make system
Carry out crosslinking under mildly acidic conditions；It includes Determination of multiple metal elements and can form ligand complex with these metallic elements
The gas chromatography of body.As：The organic compound of hydroxyl, carbonyl and carboxyl.And owing to its design feature can strengthen pressure break
The network structure of liquid, thus improve the temperature tolerance of fracturing fluid.Meanwhile, it is a kind of temperature sensitive material, can be at 20-
45 DEG C and 60-120 DEG C discharge cross-linking ion.Therefore, it can also according to the requirement of different crosslinking times and temperature,
Fracturing fluid base fluid is made to form colloid, to carry out taking sand and pressure break under conditions of certain.
The crosslinking agent that this invention is comprised, as the main component of copolymer faintly acid fracturing fluid system, can make base fluid exist
Formed under the conditions of weakly acidic heatproof, anti-shearing, solid-carrying performance good, fragile glue, can the fracturing fluid of at high temperature secondary cross-linking
System.
By using the compound crosslinking agent using under the high temperature resistant thickening agent of copolymer invented and solutions of weak acidity, make
Copolymer faintly acid fracturing fluid system can form faintly acid system, gelation time is adjustable, heatproof, low residue, low filtration loss, easily
The New Fracturing Fluid system of the row of returning.It can apply to the different environment such as hypotonic, alkali is quick, deep layer, high temperature.
Brief description
Fig. 1 be the viscous temperature of copolymer faintly acid fracturing fluid system 140 DEG C, viscous when curve.
Fig. 2 be the viscous temperature of copolymer faintly acid fracturing fluid system 180 DEG C, viscous when curve.
Detailed description of the invention
The synthesis of thickening agent of copolymer
Embodiment 1
In parts by mass, taking 0.2 part of N, N dimethyl acrylamide, joining in 50 parts of water, heating is dissolved, then adds
Enter 8 parts of AMPS monomers, add 3 parts of acrylic monomers, add 20 parts of acrylamide monomers, by its whole dissolvings, in stirring
Being slowly added to monomer gross mass 0.5% temperature accelerator cerous sulfate under state, question response temperature reaches more than 30 DEG C, and reaction 2 is little
When.It with the increase of reactant liquor viscosity, is stepped up reaction temperature, after reaching 50 DEG C, then reacts 2 hours, reactant is dried,
Pulverize, i.e. obtain the copolymer of the present invention.Mass percent be 0.5% copolymer base fluid pH value be 5-6.
Embodiment 2
Based on quality is divided, taking 2 parts of N, N dimethyl acrylamide, joining in 50 parts of water, heating is dissolved, and adds 8
Part AMPS monomer, stirring and dissolving.Add 25 parts of acrylamide monomers, by its whole dissolvings.It is slowly added under stirring
Monomer total amount 0.5% temperature accelerator cerous sulfate, question response temperature reaches more than 30 DEG C, reacts 2 hours.Add 15 parts of water,
Stirring, continues reaction.It with the increase of reactant liquor viscosity, is stepped up reaction temperature, after reaching 50 degree, then react 2 hours, will
Reactant is dried, and pulverizes, i.e. obtains the copolymer of the present invention.Mass percent be 0.5% copolymer base fluid pH value be 5-6, viscous
Degree is more than 80mPa s, and copolymer is soluble in water, and by the same sex electrostatic repulsion of carboxylic acid ion, strand is stretched by helical form
For bar-shaped, thus improve the viscosity of aqueous phase.By formation network structure of building bridge each other, add the viscosity of system.
The synthesis of compound crosslinking agent
Embodiment 3
Based on quality is divided, take 45 parts of water, 15 parts of ethanol, mix, add 10 parts of zirconium oxychlorides, stir, add
22 parts of sodium gluconates, react 2 hours at 85 DEG C, add the acetic acid of 8 parts, the cerous sulfate of 0.5 part, react 4 at 80 DEG C
Hour, obtain brown uniform liquid.
Embodiment 4
Based on quality is divided, take 45 parts of water, 15 parts of ethanol, mix, add 8 parts of zirconium oxychlorides, stir, add
The cerous sulfate of 0.5 part, reacts 1 hour under normal temperature.Add 30 parts of polyhydroxyketones and 8 parts of acetic acid, react 4 hours at 85 DEG C,
Add 1 part of EDTA, continue reaction 1 hour, obtain brown uniform liquid.
Embodiment 5
Based on quality is divided, take 35 parts of water, 15 parts of ethanol, mix, add 12 parts of zirconium oxychlorides, stir, add
The cerous sulfate of 0.5 part, reacts 1 hour under normal temperature.Add 25 parts of polyhydroxyketones and 8 parts of acetic acid, react 4 hours at 85 DEG C,
Add 5 parts of sodium gluconates, continue reaction 1 hour, obtain brown uniform liquid.
The synthesis of copolymer faintly acid fracturing fluid system
Embodiment 6
Based on quality is divided, take 99 parts of water, add the thickener of 0.5 part of embodiment 1 gained, stir, place 30min with
On, add the crosslinking agent of 0.5 part of embodiment 3 gained, stir, i.e. obtain the copolymer fracturing liquid of the present invention.
Embodiment 7
Based on quality is divided, take 99 parts of water, add the thickener of 0.6 part of embodiment 2 gained, stir, place 30min with
On, add the crosslinking agent of 0.4 part of embodiment 4 gained, stir, i.e. obtain the copolymer fracturing liquid of the present invention.
Embodiment 8
Based on quality is divided, take 98 parts of water, add the thickener of 0.3 part of embodiment 2 gained, stir, place 30min with
On, add the crosslinking agent of 0.8 part of embodiment 5 gained, stir, i.e. obtain the copolymer fracturing liquid of the present invention.
Copolymer faintly acid fracturing fluid system performance test described in embodiment 6-8：1. temperature tolerance：
At 140 DEG C, 170s-1Under the conditions of shearing different time after fracturing fluid viscosity with shear time change as it is shown in figure 1,
After shearing 1h, the viscosity of fracturing fluid is at more than 100mpa s；At 180 DEG C, 170s-1Under the conditions of fracturing fluid after shearing different time
Viscosity has well resistance to shear time change as in figure 2 it is shown, the viscosity of fracturing fluid is still above 50mPa s after shearing 2h
Temperature, anti-shear performance, be entirely capable of meeting high temperature, the pressing crack construction of deep layer requires.
2 surface tension：26.6mN/m (guanidine glue 33.82mN/m).
3 interfacial tensions：<1.2mN/m (guanidine glue 1.25mN/m).
4 residues：About 50mg/L, is the 1/18 of conventional guar gum.
5 leakoff coefficents：2.3×10-4
6 Low Damage
7 rotten denaturation：15-20d can be deposited for 20-35 DEG C；
8 fracturing fluid break times：2.5-3h, gel breaker dosage 0.1-0.3%
9 under normal circumstances the row of returning lead up to：More than 75%.The reality constructed at the scene is up to 90%；
10 solid-carrying performance：Form high intensity crosslinked, there is extraordinary solid-carrying performance.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every utilize this
Equivalent structure or equivalence flow process that bright specification and accompanying drawing content are made convert, or are directly or indirectly used in other related skills
Art field, all in like manner includes in the scope of patent protection of the present invention.
Claims (6)
1. a copolymer faintly acid fracturing fluid system, it is characterised in that：Being made up of following component in parts by mass, copolymer increases
Thick dose of 0.3-0.6 part, compound crosslinking agent 0.4-0.8 part, water 98-99 part；Described thickening agent of copolymer is by parts by mass
Following component forms：Acrylic monomers 0-2 part, 2-acrylamide-2-methyl propane sulfonic (AMPS) monomer 0-8 part, N, N dimethyl
Acrylamide monomer 0-2 part, sodium allylsulfonate monomer 0-8 part, acrylamide monomer 0-25 part, water 50-75 part, described copolymer
Thickener at least includes above-mentioned 3 kinds of monomers；Described compound crosslinking agent is made up of following component in parts by mass：Transition metal
Salt 5-12 part, ligand 25-45 part, temperature accelerator 0-0.5 part, complexing agent 0-5 part and solvent 50-60 part, described transition gold
Belonging to one or more that salt is zirconates, aluminium salt, molysite, titanium salt and chromic salts, ligand is organising containing lone pair electrons element
Compound, solvent is the mixture of water and alcohol, and complexing agent is the one of ethylenediamine tetra-acetic acid (EDTA), polyhydroxy sodium alkoxide and organic acid
Or several, temperature accelerator is rare earth metal salt.
2. a kind of copolymer faintly acid fracturing fluid system as claimed in claim 1, it is characterised in that：Described thickening agent of copolymer
For non-ionic polyalcohol, mean molecule quantity is 200-300 ten thousand.
3. a kind of copolymer faintly acid fracturing fluid system as claimed in claim 1, it is characterised in that：Described transition metal salt is
Zirconates and at least one of aluminium salt.
4. a kind of copolymer faintly acid fracturing fluid system as claimed in claim 1, it is characterised in that：Described temperature accelerator is
Cerous sulfate and at least one of ceric sulfate.
5. the synthetic method of the copolymer faintly acid fracturing fluid system described in a claim 1, it is characterised in that：Including it is as follows
Step：
A. the synthesis of polymers thickener：Described monomer is dissolved in water, the 0.05-0.1% adding quality to be monomer total amount
Catalyst, described catalyst is the mixture of manganese dioxide and sodium acid carbonate or is strong oxidizer, and control reaction temperature is at 30-50
DEG C, it with the increase of reactant liquor viscosity, is stepped up reaction temperature to 50 DEG C, reacts 4 hours, reactant is dried, pulverize, i.e.
Obtain the copolymer copolymer of the present invention；
B. the synthesis of compound crosslinking agent：Water and ethanol are mixed, adds transition metal salt, stir, add coordination
Body, reacts 2 hours at 85 DEG C, adds complexing agent, temperature accelerator, reacts 4 hours, obtain compound crosslinking at 80 DEG C
Agent；
C. the synthesis of copolymer faintly acid fracturing fluid system：The thickening agent of copolymer that water and step A synthesize is stirred, places
More than 30min, adds the compound crosslinking agent of step B synthesis, stirs, obtain copolymer faintly acid fracturing liquid.
6. the synthetic method of a kind of copolymer faintly acid fracturing fluid system as claimed in claim 5, it is characterised in that：Described by force
Oxidant is one or more of Ammonium Persulfate 98.5, potassium peroxydisulfate and hydrogen peroxide.
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| CN201610680221.7A CN106433599A (en) | 2016-08-17 | 2016-08-17 | Weakly-acidic copolymer fracturing fluid system and preparation method therefor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110259427A (en) * | 2019-07-10 | 2019-09-20 | 河南理工大学 | Hydrofrac fluid, gas drainage system and gas pumping method |
| CN114426835A (en) * | 2021-12-21 | 2022-05-03 | 中国石油化工股份有限公司 | Preparation method and application of degradable fracturing fluid thickening agent |
| CN114456782A (en) * | 2020-10-22 | 2022-05-10 | 中国石油化工股份有限公司 | High-viscosity system for regulating and controlling oil deposit fluidity in strongly water flooded zone and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103396780A (en) * | 2013-08-07 | 2013-11-20 | 北京博德世达石油技术股份有限公司 | High temperature resistant delayed organic boron crosslinking agent and its preparation method |
| CN105295885A (en) * | 2015-11-06 | 2016-02-03 | 中国石油化工股份有限公司 | Acid polymer weighted fracture fluid and preparation method thereof |
-
2016
- 2016-08-17 CN CN201610680221.7A patent/CN106433599A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103396780A (en) * | 2013-08-07 | 2013-11-20 | 北京博德世达石油技术股份有限公司 | High temperature resistant delayed organic boron crosslinking agent and its preparation method |
| CN105295885A (en) * | 2015-11-06 | 2016-02-03 | 中国石油化工股份有限公司 | Acid polymer weighted fracture fluid and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110259427A (en) * | 2019-07-10 | 2019-09-20 | 河南理工大学 | Hydrofrac fluid, gas drainage system and gas pumping method |
| CN114456782A (en) * | 2020-10-22 | 2022-05-10 | 中国石油化工股份有限公司 | High-viscosity system for regulating and controlling oil deposit fluidity in strongly water flooded zone and preparation method and application thereof |
| CN114426835A (en) * | 2021-12-21 | 2022-05-03 | 中国石油化工股份有限公司 | Preparation method and application of degradable fracturing fluid thickening agent |
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Application publication date: 20170222 |