CN106832145A - A kind of gas suspension proppant for slippery water pressure break and preparation method thereof and application method - Google Patents
A kind of gas suspension proppant for slippery water pressure break and preparation method thereof and application method Download PDFInfo
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- CN106832145A CN106832145A CN201611170927.5A CN201611170927A CN106832145A CN 106832145 A CN106832145 A CN 106832145A CN 201611170927 A CN201611170927 A CN 201611170927A CN 106832145 A CN106832145 A CN 106832145A
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- slippery water
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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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
- C08F220/10—Esters
- C08F220/22—Esters containing halogen
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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
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
- C09K8/805—Coated proppants
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/25—Methods for stimulating production
- E21B43/26—Methods for stimulating production by forming crevices or fractures
- E21B43/267—Methods for stimulating production by forming crevices or fractures reinforcing fractures by propping
Abstract
The invention provides a kind of gas suspension proppant for slippery water pressure break and preparation method thereof and application method, the gas suspension proppant includes particles of aggregates, hydrophobic close gas coating is solidified with outside the particles of aggregates, the hydrophobic close gas coating is obtained by hydrophobic close gas emulsions curing reaction；The hydrophobic close gas emulsions are obtained by fluoropolymer monomer, polymer binder, silane coupler, surfactant and deionized water polymerisation.Gas suspension proppant of the invention is in slippery water fracturing process with the nitrogen of note 10~20%, the micro-bubble that hydrophobic close gas coating energy absorption nitrogen is formed in slippery water, proppant is set to be still within suspended state under low viscosity conditions, reach the purpose that crosslinked fluid takes sand, therefore the viscosity of fracturing fluid need not be improved using substantial amounts of organic material, to stratum fanout free region, beneficial to the row of returning, volume increase is hidden to unconventionaloil pool significant.
Description
Technical field
The invention belongs to unconventionaloil pool development technique field, a kind of gas suspension for slippery water pressure break is specifically related to
Proppant and preparation method thereof and application method, slippery water fracturing technology is used in being mainly used in unconventionaloil pool exploitation.
Background technology
Unconventionaloil pool exploitation is current hot research field both domestic and external, and volume fracturing volume increase is opened as unconventionaloil pool
One of desirable route adopted.For unconventionaloil pool reservoir characteristics, the slippery water that main introduction North America domestic at present generally uses
Fracturing fluid technology, to reach the purpose of cost efficiency.Compared with crosslinked fluid, slippery water has low cost, it is more likely to form complicated
Fracture network, it is small to reservoir damage, the advantages of be easier to the row of returning；But the low characteristic of slippery water viscosity is unfavorable for taking sand, causes
Proppant sand setting is fast, and maximum sand concentration is low and the problems such as proppant skewness.Asking for sand difficulty is taken currently for slippery water
Topic, research worker is mainly from improvement fracturing fluid liquid properties and the aspect of proppant performance two.
Fracturing fluid is improved by optimizing liquid properties and takes sand concentration, typical practice be using mixing water fracturing technology, i.e., before
Put liquid and crack is produced using slippery water, the proppant for then carrying higher concentration using crosslinked fluid enters stratum.But for densification
Reservoir, one side polymer or natural plant gum residue can be damaged to proppant pack band, reduce pressure break flow conductivity, be unfavorable for
Liquid returns row；Another aspect high viscosity liquid can increase the difficulty of fracture height control.Another kind improves the method for taking sand concentration
It is to add to can dissolve fiber in slippery water, the network structure formed in slippery water by fiber helps take sand, but from now
Field applicable cases are seen, due to fiber agglomerate, disperse unequal reason, this technique to increased the risk of sand plug.Meanwhile, addition is fine
Dimension can influence the rheological property of fracturing fluid, uniform laying of the interference proppant in crack.
Proppant predominantly quartz sand, haydite and its surface modified product used in current fracturing technique.From proppant
Performance is set out, and mainly reduces proppant relative density, such as low-density, super-low-density proppant, but this kind of proppant preparation side
Method is complicated, expensive, and compression strength is low, and percentage of damage is high.Another method is to carry out immersion coating in proppant surface, such as
A laminated resin is applied, this method can effectively improve the resistant to breakage ability and erosion resistance of proppant, but reduce branch
Support agent density is limited, it is impossible to make proppant Effective Suspension in slippery water.A kind of coating material newer at present is by water solubility
Macromolecular material is scattered in aggregate, proppant is met water and is expanded rapidly, and proppant proportion is reduced by the swollen volume that rises.But,
The face coat of this proppant can be damaged to stratum in the earth formation, reduce reservoir flow conductivity.
The content of the invention
It is an object of the invention in view of the shortcomings of the prior art, there is provided a kind of gas suspension for slippery water pressure break
Proppant and preparation method thereof and application method, the gas suspension proppant energy absorption nitrogen that the present invention is provided are formed in slippery water
Micro-bubble, proppant is still within suspended state under low viscosity conditions, the purpose that crosslinked fluid takes sand is reached, while right
Stratum fanout free region, beneficial to the row of returning, hides volume increase significant to unconventionaloil pool.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
The invention provides a kind of gas suspension proppant for slippery water pressure break, the gas suspension proppant includes aggregate
Particle, is solidified with hydrophobic close gas coating outside the particles of aggregates, and the hydrophobic close gas coating is anti-by hydrophobic close gas emulsions solidification
Should be obtained.
The particles of aggregates is quartz sand or haydite, and its particle size range is 0.125mm~2.0mm.
Preferably, the particles of aggregates is selected to pass through includes washing or pickling, and the pressure break of the processing procedure of classification is used
Quartz sand or pressure break haydite, its particle size range are 0.212mm~0.85mm.
The hydrophobic close gas emulsions are by fluoropolymer monomer, polymer binder, silane coupler, surfactant and go
Ionized water polymerisation is obtained；
The mass percent of each component is as follows in the reaction raw materials of the hydrophobic close gas emulsions：
Preferably, the mass percent of each component is as follows in the reaction raw materials of the hydrophobic close gas emulsions：
The fluoropolymer monomer be fluorinated acrylate, preferably hexafluorobutyl acrylate, Hexafluorobutyl mathacrylate,
The trifluoro monooctyl ester of methacrylic acid ten, dodecafluorhe-ptylacrylate, dodecafluoroheptyl methacrylate or methacrylic acid trifluoro second
Ester, most preferable dodecafluorhe-ptylacrylate；
The high score adhesive can be using usual polymer binder in the art, preferably methacrylic acid 12
In ester, octadecyl methacrylate, hydroxypropyl acrylate, hydroxy-ethyl acrylate, methacrylic acid -2- (dimethylamino) ethyl ester
The mixture of one or more arbitrary proportions；
The silane coupler is VTES, vinyltrimethoxy silane, (the 2- methoxies of vinyl three
Base oxethyl) silane, γ-aminopropyltrimethoxysilane, one or more any ratios in gamma-aminopropyl-triethoxy-silane
The mixture of example；
The surfactant can be using this area usual anion surfactant or nonionic surfactant；
Wherein anion surfactant is preferably neopelex or dodecyl sodium sulfate, most preferably detergent alkylate
Sodium sulfonate；Nonionic surfactant is preferably polyoxyethylene Zhong Xin phenolic ethers -10 or polyoxyethylene sorbitan monostearate,
Most preferably polyoxyethylene Zhong Xin phenolic ethers -10；
Present invention also offers a kind of preparation method of the gas suspension proppant for slippery water pressure break, specific steps are such as
Under：
Step 1, hydrophobic close gas emulsions deionized water is diluted to mass percentage concentration for 7~15%, obtains dilution breast
Liquid；
Step 2, by diluting emulsion and particles of aggregates by volume 1:2 mix, stirring 5~20 minutes, then staticaccelerator adsorption
0.5~2 hour；
Step 3, removal diluting emulsion, the particles of aggregates after absorption are put into baking oven and are dried；
Step 4, cooling, sieving obtain the gas suspension proppant for slippery water pressure break.
Mixing speed in the step 2 is 300~1000r/min, and whipping temp is room temperature.
Drying temperature in the step 3 is 110 DEG C, and drying time is 20~30 minutes.
The preparation method of the hydrophobic close gas emulsions is as follows：
1) fluoropolymer monomer, polymer binder, silane coupler are mixed in proportion, obtains raw material mixing
Thing；
2) surfactant and deionized water are proportionally added into a kettle.；
3) reactor is heated to 65~85 DEG C under nitrogen protection, is then mixed to dropwise addition raw material in reactor
Thing；
4) the follow-up continuous insulation reaction of completion of dropping 3~6 hours, it is 6~7 that reaction terminates rear regulation system pH value；
5) discharge, product is filtered, that is, obtain hydrophobic close gas emulsions.
Present invention also offers a kind of application method of the gas suspension proppant for slippery water pressure break, in slippery water pressure break
During with nitrogen injection, to produce the nitrogen foam that can be adsorbed by gas suspension proppant, make gas suspension proppant in slippery water
It is middle freely to suspend, wherein being the 10~20% of the smooth water volume injected with the nitrogen volume of note.
Relative to prior art, the invention has the advantages that：
Provided by the present invention for the gas suspension proppant of slippery water pressure break, it focuses on being formed on particles of aggregates surface
One layer of hydrophobic close gas coating.With nitrogen injection in slippery water fracturing process when using, hydrophobic close gas coating energy absorption nitrogen exists
In slippery water formed micro-bubble (nitrogen foam), enable gas suspension proppant low viscosity (<Under the conditions of 3mPas) still
So freely suspended in slippery water.Therefore, there is no need to be improved using substantial amounts of organic material the viscosity of fracturing fluid, it is right to reduce
The injury on stratum；Compared with conventional slippery water pressure break, can be increased substantially with gas suspension proppant slippery water pressure break of the invention
Proppant maximum sand ratio, and proppant is effectively distributed on crack, increase flow conductivity of the proppant in frac-pack layer；Often
Rule slippery water is to take sand by forming turbulent flow under huge discharge, and gas suspension proppant slippery water pressure break of the invention is due to support
Agent can suspend in water, on the one hand reduce the consumption of water, on the other hand reduce pump truck output, reduce pump truck and use load；
Sand fallout, sand plug risk can be reduced, coiled tubing washing and cleaning operation and cost is reduced.
Provided by the present invention for the preparation method of the gas suspension proppant of slippery water pressure break, it focuses on using hydrophobic
Close gas emulsions carry out hydrophobic close gas to particles of aggregates surface and are modified, and one layer of hydrophobic close gas coating is formd on particles of aggregates surface.
Hydrophobic close gas emulsions in the present invention have very strong adsorption capacity to proppant particles of aggregates so that the preparation of gas suspension proppant
Process is easy and effective, and gas suspension proppant can be continuously produced under the conditions of technique for fixing, with production efficiency is high, product quality is steady
Fixed advantage.In use, by nitrogen micro-bubble and the synergy of gas suspension proppant, gas suspension proppant is made
Can in slippery water Effective Suspension, reach the purpose that crosslinked fluid takes sand, can effectively solve the problem that slippery water takes that sand is difficult, limitation branch
The support agent dense scope of most STOL, influence proppant is effectively uniformly distributed, and reduces many problems such as reservoir flow conductivity, and without residue,
Stratum will not be damaged, be additionally favorable for the row of returning, it is significant to hide volume increase to unconventionaloil pool.
Application method provided by the present invention for the gas suspension proppant of slippery water pressure break is very convenient, in smooth hydraulic pressure
With nitrogen injection during splitting, gas suspension proppant just can freely be suspended by absorption nitrogen foam in slippery water, be reached
Crosslinked fluid takes the effect of sand.
Specific embodiment
The present invention is described in further details with reference to embodiment and comparative example.
Embodiment 1
(1) hydrophobic close gas emulsions are prepared：
Raw material：Dodecafluoroheptyl methacrylate 40.0g (fluoropolymer monomer 40wt%)；
Lauryl methacrylate 5.0g, hydroxypropyl acrylate 5.0g, methacrylic acid -2- (dimethylamino) ethyl esters 5.0g
It is (high
Molecular adhesion agent 15wt%)
VTES 7.0g (silane coupler 7wt%)
The 3.0g (surfactant 3wt%) of polyoxyethylene Zhong Xin phenolic ethers -10
Deionized water 35.0g (35wt%)
1) fluoropolymer monomer, polymer binder, silane coupler are mixed in proportion, obtains raw material mixing
Thing；
2) surfactant and deionized water, mixing speed 600r/min are proportionally added into a kettle.；
3) 75 DEG C are heated under nitrogen protection, then to raw mixture is added dropwise in reactor；
4) the follow-up continuous insulation reaction of completion of dropping 4 hours, reaction terminates rear regulation system pH value and is about 6.5；
5) discharge, filtered with 200 mesh gauzes, obtain hydrophobic close gas emulsions.
(2) gas suspension proppant is prepared：
1) it is 10% hydrophobic close gas emulsions to be diluted into mass percentage concentration with deionized water, obtains diluting emulsion
1000mL。
2) haydite aggregate (the grain density 3.15g/cm of 2000mL 0.425~0.85mm particle diameters is added in agitator tank3,
Bulk density 1.68g/cm3) and 1000mL diluting emulsions；Stirred 20 minutes with the speed of 500r/min；Then staticaccelerator adsorption 1 is small
When.
3) diluting emulsion is removed, the particles of aggregates after absorption is put into 110 DEG C of baking ovens, constant temperature drying 20 minutes；
4) cool down, sieving obtains the gas suspension proppant for slippery water pressure break.
Embodiment 2
(1) hydrophobic close gas emulsions are prepared：
Raw material：Dodecafluorhe-ptylacrylate 40.0g (fluoropolymer monomer 40wt%)；
Octadecyl methacrylate 5.0g, hydroxypropyl acrylate 5.0g, methacrylic acid -2- (dimethylamino) ethyl esters 5.0g
(polymer binder 15wt%)
Vinyltrimethoxy silane 7.0g (silane coupler 7wt%)
Neopelex 3.0g (surfactant 3wt%)
Deionized water 35.0g (35wt%)
1) fluoropolymer monomer, polymer binder, silane coupler are mixed in proportion, obtains raw material mixing
Thing；
2) surfactant and deionized water, mixing speed 600r/min are proportionally added into a kettle.；
3) 75 DEG C are heated under nitrogen protection, then to raw mixture is added dropwise in reactor；
4) the follow-up continuous insulation reaction of completion of dropping 4 hours, reaction terminates rear regulation system pH value and is about 6.5；
5) discharge, filtered with 200 mesh gauzes, obtain hydrophobic close gas emulsions.
(2) gas suspension proppant is prepared：
1) it is 10% hydrophobic close gas emulsions to be diluted into mass percentage concentration with deionized water, obtains diluting emulsion
1000mL。
2) haydite aggregate (the grain density 3.15g/ of 2000mL 0.212~0.425mm particle diameters is added in agitator tank
cm3, bulk density 1.70g/cm3) and 1000mL diluting emulsions；Stirred 20 minutes with the speed of 500r/min；Then staticaccelerator adsorption
1 hour.
3) diluting emulsion is removed, the particles of aggregates after absorption is put into 110 DEG C of baking ovens, constant temperature drying 20 minutes；
4) cool down, sieving obtains the gas suspension proppant for slippery water pressure break.
Embodiment 3
(1) hydrophobic close gas emulsions are prepared：
Raw material：The trifluoro monooctyl ester 40.0g (fluoropolymer monomer 40wt%) of methacrylic acid ten；
Lauryl methacrylate 5.0g, hydroxy-ethyl acrylate 5.0g, methacrylic acid -2- (dimethylamino) ethyl esters 5.0g
(polymer binder 15wt%)
γ-aminopropyltrimethoxysilane 7.0g (silane coupler 7wt%)
Polyoxyethylene sorbitan monostearate 3.0g (surfactant 3wt%)
Deionized water 35.0g (35wt%)
1) fluoropolymer monomer, polymer binder, silane coupler are mixed in proportion, obtains raw material mixing
Thing；
2) surfactant and deionized water, mixing speed 600r/min are proportionally added into a kettle.；
3) 75 DEG C are heated under nitrogen protection, then to raw mixture is added dropwise in reactor；
4) the follow-up continuous insulation reaction of completion of dropping 4 hours, reaction terminates rear regulation system pH value and is about 6.5；
5) discharge, filtered with 200 mesh gauzes, obtain hydrophobic close gas emulsions.
(2) gas suspension proppant is prepared：
1) it is 10% hydrophobic close gas emulsions to be diluted into mass percentage concentration with deionized water, obtains diluting emulsion
1000mL。
2) quartz sand aggregate (the grain density 2.63g/ of 2000mL 0.425~0.85mm particle diameters is added in agitator tank
cm3, bulk density 1.54g/cm3) and 1000mL diluting emulsions；Stirred 20 minutes with the speed of 500r/min；Then staticaccelerator adsorption
1 hour.
3) diluting emulsion is removed, the particles of aggregates after absorption is put into 110 DEG C of baking ovens, constant temperature drying 20 minutes；
4) cool down, sieving obtains the gas suspension proppant for slippery water pressure break.
Embodiment 4
(1) hydrophobic close gas emulsions are prepared：
Raw material：Hexafluorobutyl mathacrylate 40.0g (fluoropolymer monomer 40wt%)；
Octadecyl methacrylate 5.0g, hydroxypropyl acrylate 5.0g, methacrylic acid -2- (dimethylamino) ethyl esters 5.0g
(polymer binder 15wt%)
VTES 7.0g (silane coupler 7wt%)
Neopelex 3.0g (surfactant 3wt%)
Deionized water 35.0g (35wt%)
1) fluoropolymer monomer, polymer binder, silane coupler are mixed in proportion, obtains raw material mixing
Thing；
2) surfactant and deionized water, mixing speed 600r/min are proportionally added into a kettle.；
3) 75 DEG C are heated under nitrogen protection, then to raw mixture is added dropwise in reactor；
4) the follow-up continuous insulation reaction of completion of dropping 4 hours, reaction terminates rear regulation system pH value and is about 6.5；
5) discharge, filtered with 200 mesh gauzes, obtain hydrophobic close gas emulsions.
(2) gas suspension proppant is prepared：
1) it is 10% hydrophobic close gas emulsions to be diluted into mass percentage concentration with deionized water, obtains diluting emulsion
1000mL。
2) haydite aggregate (the grain density 2.63g/ of 2000mL 0.212~0.425mm particle diameters is added in agitator tank
cm3, bulk density 1.46g/cm3) and 1000mL diluting emulsions；Stirred 20 minutes with the speed of 500r/min；Then staticaccelerator adsorption
1 hour.
3) diluting emulsion is removed, the particles of aggregates after absorption is put into 110 DEG C of baking ovens, constant temperature drying 20 minutes；
4) cool down, sieving obtains the gas suspension proppant for slippery water pressure break.
Embodiment 5
(1) hydrophobic close gas emulsions are prepared：
Raw material：Dodecafluoroheptyl methacrylate 20.0g (fluoropolymer monomer 20wt%)；
Methacrylic acid -2- (dimethylamino) ethyl ester 5.0g (polymer binder 5wt%)
Vinyl three (2- methoxy ethoxies) silane 8.0g (silane coupler 8wt%)
The 7.0g (surfactant 7wt%) of polyoxyethylene Zhong Xin phenolic ethers -10
Deionized water 60.0g (60wt%)
1) fluoropolymer monomer, polymer binder, silane coupler are mixed in proportion, obtains raw material mixing
Thing；
2) surfactant and deionized water, mixing speed 550r/min are proportionally added into a kettle.；
3) 65 DEG C are heated under nitrogen protection, then to raw mixture is added dropwise in reactor；
4) the follow-up continuous insulation reaction of completion of dropping 5 hours, reaction terminates rear regulation system pH value and is about 6；
5) discharge, filtered with 200 mesh gauzes, obtain hydrophobic close gas emulsions.
(2) gas suspension proppant is prepared：
1) it is 15% hydrophobic close gas emulsions to be diluted into mass percentage concentration with deionized water, obtains diluting emulsion
1000mL。
2) haydite aggregate (the grain density 3.15g/cm of 2000mL 0.125~212mm particle diameters is added in agitator tank3)
With 1000mL diluting emulsions；Stirred 10 minutes with the speed of 600r/min；Then staticaccelerator adsorption 2 hours.
3) diluting emulsion is removed, the particles of aggregates after absorption is put into 110 DEG C of baking ovens, constant temperature drying 30 minutes；
4) cool down, sieving obtains the gas suspension proppant for slippery water pressure break.
Embodiment 6
(1) hydrophobic close gas emulsions are prepared：
Raw material：Hexafluorobutyl acrylate 35.0g (fluoropolymer monomer 35wt%)；
Hydroxy-ethyl acrylate 10.0g, methacrylic acid -2- (dimethylamino) ethyl ester 10.0g (polymer binders
20wt%)
γ-aminopropyltrimethoxysilane 5.0g, gamma-aminopropyl-triethoxy-silane 5.0g (silane coupler 10wt%)
Dodecyl sodium sulfate 2.0g (surfactant 2wt%)
Deionized water 33.0g (33wt%)
1) fluoropolymer monomer, polymer binder, silane coupler are mixed in proportion, obtains raw material mixing
Thing；
2) surfactant and deionized water, mixing speed 650r/min are proportionally added into a kettle.；
3) 70 DEG C are heated under nitrogen protection, then to raw mixture is added dropwise in reactor；
4) the follow-up continuous insulation reaction of completion of dropping 3 hours, reaction terminates rear regulation system pH value and is about 7；
5) discharge, filtered with 200 mesh gauzes, obtain hydrophobic close gas emulsions.
(2) gas suspension proppant is prepared：
1) it is 12% hydrophobic close gas emulsions to be diluted into mass percentage concentration with deionized water, obtains diluting emulsion
1000mL。
2) haydite aggregate (the grain density 3.15g/cm of 2000mL 0.85~2.0mm particle diameters is added in agitator tank3) and
1000mL diluting emulsions；Stirred 15 minutes with the speed of 300r/min；Then staticaccelerator adsorption 1.5 hours.
3) diluting emulsion is removed, the particles of aggregates after absorption is put into 110 DEG C of baking ovens, constant temperature drying 25 minutes；
4) cool down, sieving obtains the gas suspension proppant for slippery water pressure break.
Embodiment 7
(1) hydrophobic close gas emulsions are prepared：
Raw material：Trifluoroethyl methacrylate 50.0g (fluoropolymer monomer 50wt%)；
Lauryl methacrylate 6.0g, hydroxy-ethyl acrylate 6.0g (polymer binder 12wt%)
VTES 1.0g, vinyltrimethoxy silane 1.0g (silane coupler 2wt%)
Polyoxyethylene sorbitan monostearate 10.0g (surfactant 10wt%)
Deionized water 26.0g (26wt%)
1) fluoropolymer monomer, polymer binder, silane coupler are mixed in proportion, obtains raw material mixing
Thing；
2) surfactant and deionized water, mixing speed 700r/min are proportionally added into a kettle.；
3) 80 DEG C are heated under nitrogen protection, then to raw mixture is added dropwise in reactor；
4) the follow-up continuous insulation reaction of completion of dropping 6 hours, reaction terminates rear regulation system pH value and is about 6.2；
5) discharge, filtered with 200 mesh gauzes, obtain hydrophobic close gas emulsions.
(2) gas suspension proppant is prepared：
1) it is 8% hydrophobic close gas emulsions to be diluted into mass percentage concentration with deionized water, obtains diluting emulsion 1000mL.
2) quartz sand aggregate (the grain density 2.63g/ of 2000mL 0.125~0.212mm particle diameters is added in agitator tank
cm3) and 1000mL diluting emulsions；Stirred 5 minutes with the speed of 1000r/min；Then staticaccelerator adsorption 0.5 hour.
3) diluting emulsion is removed, the particles of aggregates after absorption is put into 110 DEG C of baking ovens, constant temperature drying 22 minutes；
4) cool down, sieving obtains the gas suspension proppant for slippery water pressure break.
Embodiment 8
(1) hydrophobic close gas emulsions are prepared：
Raw material：Dodecafluoroheptyl methacrylate 60.0g (fluoropolymer monomer 60wt%)；
Octadecyl methacrylate 10.0g (polymer binder 10wt%)
γ-aminopropyltrimethoxysilane 5.0g (silane coupler 5wt%)
Neopelex 5.0g (surfactant 5wt%)
Deionized water 20.0g (20wt%)
1) fluoropolymer monomer, polymer binder, silane coupler are mixed in proportion, obtains raw material mixing
Thing；
2) surfactant and deionized water, mixing speed 500r/min are proportionally added into a kettle.；
3) 85 DEG C are heated under nitrogen protection, then to raw mixture is added dropwise in reactor；
4) the follow-up continuous insulation reaction of completion of dropping 4.5 hours, reaction terminates rear regulation system pH value and is about 6.8；
5) discharge, filtered with 200 mesh gauzes, obtain hydrophobic close gas emulsions.
(2) gas suspension proppant is prepared：
1) it is 7% hydrophobic close gas emulsions to be diluted into mass percentage concentration with deionized water, obtains diluting emulsion 1000mL.
2) haydite aggregate (the grain density 2.63g/cm of 2000mL 0.85~2.0mm particle diameters is added in agitator tank3) and
1000mL diluting emulsions；Stirred 18 minutes with the speed of 800r/min；Then staticaccelerator adsorption 1.2 hours.
3) diluting emulsion is removed, the particles of aggregates after absorption is put into 110 DEG C of baking ovens, constant temperature drying 28 minutes；
4) cool down, sieving obtains the gas suspension proppant for slippery water pressure break.
Comparative example 1
Proppant：Haydite, 0.425~0.85mm of granularity, grain density 3.15g/cm3, bulk density 1.68g/cm3。
Comparative example 2
Proppant：Haydite, 0.212~0.425mm of granularity, grain density 3.15g/cm3, bulk density 1.70g/cm3。
Comparative example 3
Proppant：Quartz sand, 0.425~0.85mm of granularity, grain density 2.63g/cm3, bulk density 1.54g/cm3。
Comparative example 4
Proppant：Quartz sand, 0.212~0.425mm of granularity, grain density 2.63g/cm3, bulk density 1.46g/cm3。
Experiment and result：
In order to verify the suspension effect of gas suspension proppant of the invention, proppant sedimentation experiment is done in slippery water, tied
Fruit is as shown in table 1.
Slippery water：The friction reducer of deionized water+0.05%.
Because gas suspension proppant of the present invention needs and bubble synergy, can just suspend in water；Therefore sedimentation is done real
Slippery water and proppant are stirred 1 minute under 2000r/min rotating speeds using waring agitators first before testing, to form small gas
Bubble.
Embodiment 1-4, the sinking speed of comparative example 1-4 proppants in the slippery water of table 1
With reference to People's Republic of China's oil and gas industry standard, the short-term flow conductivity evaluation of fracturing propping agents filling bed
Method, i.e. APIRP61 test permeability, the mechanical property of different proppant packed layers.The results are shown in Table 2, table 3.
Slippery water：The friction reducer of deionized water+0.05%.
Each test group permeability result of table 2
The mechanical strength test of table 3
| Detection | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 |
| Single particle strength (N) | 37 | 16 | 22 | 12 | 22 | 14 |
| Clossing pressure (MPa) | 69 | 69 | 35 | 35 | 69 | 69 |
| Percentage of damage (%)/(69MPa) | 2.8 | 2.1 | 6.2 | 4.8 | 3.6 | 2.4 |
Gas suspension proppant of the invention can well hang in low viscous slippery water as can be seen from Table 1
It is floating, and general aggregate then can be settled substantially.From table 2 and table 3 as can be seen that under identical sanding concentration, gas of the invention hangs
The flow conductivity of floating proppant is suitable with the flow conductivity of non-overlay film conventional proppants, but percentage of damage is lower, and mechanical strength is more
It is high.
The above, is only presently preferred embodiments of the present invention, and not the present invention is imposed any restrictions, every according to the present invention
Any simple modification, change and equivalent structure transformation that technical spirit is made to above example, still fall within skill of the present invention
In the protection domain of art scheme.
Claims (10)
1. a kind of gas suspension proppant for slippery water pressure break, it is characterised in that：The gas suspension proppant includes aggregate
Grain, is solidified with hydrophobic close gas coating outside the particles of aggregates, and the hydrophobic close gas coating is by hydrophobic close gas emulsions curing reaction
It is obtained.
2. the gas suspension proppant for slippery water pressure break according to claim 1, it is characterised in that：The particles of aggregates
It is quartz sand or haydite, its particle size range is 0.125mm~2.0mm.
3. the gas suspension proppant for slippery water pressure break according to claim 1, it is characterised in that：The hydrophobic close gas
Emulsion is obtained by fluoropolymer monomer, polymer binder, silane coupler, surfactant and deionized water polymerisation；
The mass percent of each component is as follows in the reaction raw materials of the hydrophobic close gas emulsions：
4. the gas suspension proppant for slippery water pressure break according to claim 3：Characterized in that, the fluoropolymer
Monomer is fluorinated acrylate.
5. the gas suspension proppant for slippery water pressure break according to claim 3, it is characterised in that the macromolecule glues
Mixture be lauryl methacrylate, octadecyl methacrylate, hydroxypropyl acrylate, hydroxy-ethyl acrylate, methacrylic acid-
The mixture of one or more arbitrary proportions in 2- (dimethylamino) ethyl ester.
6. the gas suspension proppant for slippery water pressure break according to claim 3, it is characterised in that described silane coupled
Agent is VTES, vinyltrimethoxy silane, vinyl three (2- methoxy ethoxies) silane, γ-ammonia
The mixture of one or more arbitrary proportions in propyl trimethoxy silicane, gamma-aminopropyl-triethoxy-silane.
7. the gas suspension proppant for slippery water pressure break according to claim 3, it is characterised in that the surface-active
Agent is anion surfactant or nonionic surfactant.
8. the preparation method of the gas suspension proppant for slippery water pressure break in claim 1~7 described in any one, it is special
Levy and be, comprise the following steps that：
Step 1, hydrophobic close gas emulsions deionized water is diluted to mass percentage concentration for 7~15%, obtains diluting emulsion；
Step 2, by diluting emulsion and particles of aggregates by volume 1:2 mixing, stir 5~20 minutes, then staticaccelerator adsorption 0.5~
2 hours；
Step 3, removal diluting emulsion, the particles of aggregates after absorption are put into baking oven and are dried；
Step 4, cooling, sieving obtain the gas suspension proppant for slippery water pressure break.
9. the preparation method of the gas suspension proppant for slippery water pressure break according to claim 8, it is characterised in that institute
The preparation method for stating hydrophobic close gas emulsions is as follows：
1) fluoropolymer monomer, polymer binder, silane coupler are mixed in proportion, obtains raw mixture；
2) surfactant and deionized water are proportionally added into a kettle.；
3) reactor is heated to 65~85 DEG C under nitrogen protection, then to raw mixture is added dropwise in reactor；
4) the follow-up continuous insulation reaction of completion of dropping 3~6 hours, it is 6~7 that reaction terminates rear regulation system pH value；
5) discharge, product is filtered, that is, obtain hydrophobic close gas emulsions.
10. the application method of the gas suspension proppant for slippery water pressure break in claim 1~7 described in any one, its
It is characterised by：With nitrogen injection in slippery water fracturing process, to produce the nitrogen foam that can be adsorbed by gas suspension proppant, make
Gas suspension proppant freely suspends in slippery water, wherein with note nitrogen volume be injection smooth water volume 10~
20%.
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| CN108165253A (en) * | 2017-12-29 | 2018-06-15 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | A kind of pressure break extremely-low density water-control oil-increasing proppant |
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