CN105647507B - A kind of moisture dissipates the preparation method of guanidine gum fracturing fluid crosslinking agent - Google Patents
A kind of moisture dissipates the preparation method of guanidine gum fracturing fluid crosslinking agent Download PDFInfo
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- CN105647507B CN105647507B CN201610065175.XA CN201610065175A CN105647507B CN 105647507 B CN105647507 B CN 105647507B CN 201610065175 A CN201610065175 A CN 201610065175A CN 105647507 B CN105647507 B CN 105647507B
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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
Abstract
The invention discloses the preparation method that a kind of moisture dissipates guanidine gum fracturing fluid crosslinking agent, comprise the following steps：It is 4 ~ 11 that Inorganic Boron containing borate is added into pH, and temperature is in 20 ~ 70 DEG C of reaction medium, and 150 ~ 300 revs/min of constant speed stir 0.5 ~ 1 hour；The organo-silicon compound containing reactable functional group are added, constant temperature stirs 1 ~ 8 hour in 20 ~ 120 DEG C, obtains cross-linked material；Cross-linked material produces the crosslinking agent of solid-state through filtering, dry, or cross-linked material is evaporated under reduced pressure, and produces the crosslinking agent of emulsion-type.The preparation technology that the present invention uses is simple, crosslinking agent can be quickly dispersed in water at normal temperatures and pressures, and can realize the regulation and control to crosslink density and crosslinking time, strive for controllable time for construction, the frictional resistance of fracturing fluid and transfer pipeline in work progress can be effectively reduced simultaneously, reduce energy consumption.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of moisture dissipates the preparation side of guanidine gum fracturing fluid crosslinking agent
Method.
Background technology
82% is hypotonic oil gas field in China's verified oil oil in place, and it is that hypotonic oil gas field raising is adopted that pressure break, which makes seam technology,
One of technical way of yield.Fracturing fluid is the important component and key link that pressure break makes seam technology, high-quality, low wound
Evil, low cost are the Main ways of fracturing fluid development.Thickener of the hydroxypropyl guar as aqueous fracturing fluid, there are thickening capabilities
By force, shear resistant is good, heat endurance is good, control filtration capacity it is strong the features such as and be widely used in Domestic Oil And Gas Fields pressure break
In.
Hydroxypropyl guar fracturing fluid system using Inorganic Boron as crosslinking agent, exist with liquid it is slow, dissolve insufficient, cross-linking efficiency
Low, the problems such as crosslinking rate is too fast；The problem of existing for borate crosslinker, existing frequently-used solution be it is carried out it is organic
Compounding or use transition metal, organo-metallic crosslinker, it integrates cross-linking properties and is better than boric acid, but is using as substitute
Also exist in various degree in journey and be crosslinked too fast, the performance problem not up to standard such as heatproof resistant to shearing, broken glue, residue content；And high temperature resistant
Organic borate cross-linker there is also chelating degree is low, concentration is high and the problems such as compound probability complexity, causes it to use limited.
The content of the invention
Based on the deficiencies in the prior art, the invention provides the preparation method that a kind of moisture dissipates guanidine gum fracturing fluid crosslinking agent,
Using the organo-silicon compound containing reactable functional group as carrier, the guanidine gum fracturing fluid that preparing surface modification has borate is crosslinked
Material, particle diameter is small, under normal temperature and pressure can in water system rapid dispersion.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of moisture dissipates the preparation method of guanidine gum fracturing fluid crosslinking agent, comprises the following steps：The inorganic of borate will be contained
It is 4 ~ 11 that boron, which adds pH, and temperature is in 20 ~ 70 DEG C of reaction medium, and 150 ~ 300 revs/min of constant speed stir 0.5 ~ 1 hour；Again plus
Enter the organo-silicon compound containing reactable functional group, constant temperature stirs 1 ~ 8 hour in 20 ~ 120 DEG C, obtains cross-linked material；Hand over
Connection material produces the crosslinking agent of solid-state through filtering, dry, or cross-linked material is evaporated under reduced pressure, and produces the crosslinking agent of emulsion-type；Its
In, the mass ratio of the Inorganic Boron containing borate, the organo-silicon compound containing reactable functional group and reaction medium for 1 ~
3：2~7：3~20.
Preferably, the Inorganic Boron containing borate is boric acid and/or borax.
Preferably, reaction medium is one or both of water, formamide, C1 ~ C5 alkylol and C1 ~ C5 alkyl acid
More than.
Preferably, the organo-silicon compound containing reactable functional group refer to the organosilicon with epoxy or amido
Compound.
Preferably, the pH of reaction medium by one or both of sodium hydroxide, potassium hydroxide, ammonium chloride and ammoniacal liquor with
Upper regulation.
Wherein, the Inorganic Boron containing borate and the organo-silicon compound containing reactable functional group are common
Commercially available prod.
Preparation technology of the present invention is simple, and guanidine glue point can be participated in using the reactable functional group on organo-silicon compound surface
The borate of son crosslinking is grafted to organo-silicon compound surface, and the autohemagglutination function having using organo-silicon compound itself, shape
Into the Organic-inorganic composite cross-linked material with three-dimensional-structure.The crosslinking agent that the present invention prepares at normal temperatures and pressures can be quick
It is dispersed in water, performance is substantially better than usually used organic or inorganic borate crosslinker.By to crosslinking agent particle size and table
The control of the load capacity of face borate can realize the regulation and control to crosslink density and crosslinking time, reach expected guanidine gum fracturing fluid and glue
Elasticity, and the frictional resistance of fracturing fluid and transfer pipeline in work progress can be effectively reduced, energy consumption is reduced, realizes effectively economic pressure
Split work progress.
Brief description of the drawings
Fig. 1 is size distribution of the crosslinking agent in laser particle size measurement analysis prepared by embodiment 1；
Fig. 2 is the cross-linking agents time prepared by embodiment 1 and the curve map of guanidine sol solution viscosity B coefficent；
Fig. 3 is comparison diagram of the crosslinking agent with borate cross-linking agent to guanidine gum fracturing fluid heat resistance prepared by embodiment 1.
Embodiment
Below by way of preferred embodiment, the present invention is described in more detail, but protection scope of the present invention is not limited to
This.
Embodiment 1
A kind of moisture dissipates the preparation method of guanidine gum fracturing fluid crosslinking agent, comprises the following steps：4g boric acid is added into 50mL third
In triol, it is 8 to add ammoniacal liquor regulation pH, is warming up to 40 DEG C, 300rpm constant speed stirring 0.5h, boric acid is completely dissolved；It is warming up to 60
DEG C, 14g γ-aminoethylaminopropyl trimethoxy silane is added, 200rpm constant speed stirring 4h, 90 DEG C is warming up to, continues to stir 1h,
Filter, drying obtains the guanidine gum fracturing fluid crosslinking agent of solid.
As shown in figure 1, the particle diameter of the above-mentioned guanidine gum fracturing fluid crosslinking agent being prepared is measured using laser particle tester
About 2 nanometers.The crosslinked fluid that mass fraction is 0.5%, 1%, 2% and 3% is respectively configured in the crosslinking agent of above-mentioned preparation, they
Light transmittance is respectively 91.5%, 92.7%, 77.7% and 65.8%, illustrates favorable dispersibility of the crosslinking agent in water.
The crosslinking agent of above-mentioned preparation is configured to the crosslinked fluid that mass fraction is 1%, and configuration quality fraction is 0.3% guanidine
Sol solution.The guanidine sol solution that 100 milliliters of mass fractions are 0.3% is taken, the crosslinked fluid that 2.5 milliliters of mass fractions are 1% is added, such as schemes
Shown in 2, with the delayed cross-linking section of 5 minutes when the nanometer cross-linking agent prepared by embodiment uses, entered after 9 minutes steady
Fixed crosslinking.Take 2 milliliters of crosslinked fluids to be added in the guanidine sol solution that 100 milliliters of mass fractions are 0.3% and stir, contrast guanidine peptization
Liquid is crosslinked initial stage and crosslinking later stage state, is hung after 5 ~ 6 minutes functional, it is seen that cross-linking effect is obvious.Take 100 milliliters of guanidine glue
Solution, the quasi- haydite of 20 ~ 40 targets is added, stirs, adds 3 milliliters of crosslinked fluids, stirred to not flowable, pour into 100 millis
Rising amount cylinder, the micro sedimentation of haydite after 2 hours, it is seen that cross-linking effect is preferable, hangs sand function admirable.100 milliliters of guanidine sol solutions are taken again,
The quasi- haydite of 20 ~ 40 targets is added, is stirred, 3 milliliters of mass fractions is added and is 1% crosslinked fluid, while adds gel breaker,
80 DEG C of constant temperature break glue haydite all sedimentations after 2 hours, and after tested, breaking glue solution viscosity is about 2.0mPa.s, it is seen that final broken glue
State is more satisfactory.
The crosslinking agent of above-mentioned preparation is configured to the crosslinked fluid that mass fraction is 3%, while configuration quality fraction is 3% boron
Acid solution, 1mL is respectively taken to be added separately in the guanidine sol solution that two 100mL mass fractions are 0.3%, as shown in figure 3, with temperature
The rise of degree, the viscosity of two guanidine sol solutions are gradually reduced, but the cross-linking properties and heatproof of the crosslinking agent prepared by the present embodiment
Performance is substantially better than boric acid.
Embodiment 2
A kind of moisture dissipates the preparation method of guanidine gum fracturing fluid crosslinking agent, comprises the following steps：5g boraxs are added into 50mL first
In acid amides, it is 7 to add sodium hydroxide solution regulation pH, is warming up to 40 DEG C, 300rpm constant speed stirring 0.5h to borax is completely dissolved；
60 DEG C are warming up to, 10g γ-aminoethylaminopropyl trimethoxy silane is slowly added dropwise, 150rpm constant speed stirring 4h, is evaporated under reduced pressure to
To the guanidine gum fracturing fluid crosslinking agent of emulsion form.
The particle diameter that the above-mentioned guanidine gum fracturing fluid crosslinking agent being prepared is measured using laser particle tester is about 2 nanometers.
The crosslinking agent of above-mentioned preparation is configured to the crosslinked fluid that mass fraction is 1%, and configuration quality fraction is 0.3% guanidine sol solution.
Take 2 milliliters of crosslinked fluids to be added in the guanidine sol solution that 100 milliliters of mass fractions are 0.3% and stir, the crosslinking of contrast guanidine sol solution is just
Phase and crosslinking later stage state, hang functional, it is seen that cross-linking effect is obvious after 5 ~ 6 minutes.100 milliliters of guanidine sol solutions are taken, are added
Enter the quasi- haydite of 20-40 targets, stir, add 3 milliliters of crosslinked fluids, stir to not flowable, pour into 100 milliliters of graduated cylinders, 2
The micro sedimentation of haydite after hour, it is seen that cross-linking effect is preferable, hangs sand function admirable.100 milliliters of guanidine sol solutions are taken again, add 20-
The quasi- haydite of 40 targets, stirs, and adds 3 milliliters of mass fractions and is 1% crosslinked fluid, while adds gel breaker, 80 DEG C of constant temperature
The haydite all sedimentations after 2 hours of broken glue, after tested, breaking glue solution viscosity is about 2.0mPa.s, it is seen that finally broken glue epidemic situation comparison reason
Think.
Embodiment 3
A kind of moisture dissipates the preparation method of guanidine gum fracturing fluid crosslinking agent, comprises the following steps：4g boric acid is added into 20mL second
In alcohol, it is 8 to add ammoniacal liquor regulation pH, is warming up to 40 DEG C, 300rpm constant speed stirring 1h to boric acid is completely dissolved；60 DEG C are warming up to,
4g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added, 200rpm constant speed stirring 4h, 90 DEG C is warming up to, continues to stir
1h is mixed, is filtered, drying obtains the guanidine gum fracturing fluid crosslinking agent of solid.
The particle diameter that the above-mentioned guanidine gum fracturing fluid crosslinking agent being prepared is measured using laser particle tester is about 2 nanometers.
The nanometer cross-linking agent of above-mentioned preparation is configured to the crosslinked fluid that mass fraction is 1%, and configuration quality fraction is 0.3% guanidine peptization
Liquid.Take 2 milliliters of crosslinked fluids to be added in the guanidine sol solution that 100 milliliters of mass fractions are 0.3% and stir, contrast guanidine sol solution is handed over
Connection initial stage and crosslinking later stage state, hang functional, it is seen that cross-linking effect is obvious after 5 ~ 6 minutes.Take 100 milliliters of guanidine peptizations
Liquid, the quasi- haydite of 20-40 targets is added, stirs, adds 3 milliliters of crosslinked fluids, stirred to not flowable, pour into 100 milliliters
Graduated cylinder, the micro sedimentation of haydite after 2 hours, it is seen that cross-linking effect is preferable, hangs sand function admirable.100 milliliters of guanidine sol solutions are taken again, are added
Enter the quasi- haydite of 20-40 targets, stir, add 3 milliliters of mass fractions and be 1% crosslinked fluid, while add gel breaker, 80
DEG C constant temperature break glue after 2 hours haydite all settle, after tested, breaking glue solution viscosity is about 2.0mPa.s, it is seen that finally breaks gluey state
It is more satisfactory.
Claims (3)
1. a kind of moisture dissipates the preparation method of guanidine gum fracturing fluid crosslinking agent, it is characterised in that comprises the following steps：Boric acid will be contained
It is 4 ~ 11 that the Inorganic Boron of root, which adds pH, and temperature is 150 ~ 300 revs/min of constant speed stirrings 0.5 ~ 1 in 20 ~ 70 DEG C of reaction medium
Hour；The organo-silicon compound containing reactable functional group are added, constant temperature stirs 1 ~ 8 hour in 20 ~ 120 DEG C, is handed over
Join material；Cross-linked material produces the crosslinking agent of solid-state through filtering, dry, or cross-linked material is evaporated under reduced pressure, and produces emulsion-type
Crosslinking agent；Wherein, the matter of the Inorganic Boron containing borate, the organo-silicon compound containing reactable functional group and reaction medium
Amount is than being 1 ~ 3：2~7：3~20；
Reaction medium is more than one or both of water, formamide, C1 ~ C5 alkylol and C1 ~ C5 alkyl acid；
The organo-silicon compound containing reactable functional group refer to the organo-silicon compound with epoxy or amido.
2. moisture according to claim 1 dissipates the preparation method of guanidine gum fracturing fluid crosslinking agent, it is characterised in that：Contain boric acid
The Inorganic Boron of root is boric acid and/or borax.
3. moisture according to claim 1 dissipates the preparation method of guanidine gum fracturing fluid crosslinking agent, it is characterised in that：Reaction medium
PH pass through one or both of sodium hydroxide, potassium hydroxide, ammonium chloride and ammoniacal liquor more than adjust.
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| CN106544001B (en) * | 2016-10-21 | 2019-12-31 | 河南大学 | Guanidine gum fracturing fluid nano cross-linking agent with good temperature resistance and preparation method thereof |
| CN106566516B (en) * | 2016-10-21 | 2020-02-11 | 河南大学 | Preparation method of structure-controllable guanidine gum fracturing fluid nano cross-linking agent |
| CN107722959B (en) * | 2017-09-28 | 2020-07-21 | 河南大学 | Guanidine gum fracturing fluid organic titanium crosslinking agent and preparation method thereof |
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| US6475329B1 (en) * | 1999-10-04 | 2002-11-05 | Tyco Electronics Corporation | Primer for silicone compositions |
| CN101531892A (en) * | 2009-04-16 | 2009-09-16 | 大庆油田有限责任公司 | Ultra low temperature super guanidine gum fracturing fluid |
| CN103965860A (en) * | 2014-04-23 | 2014-08-06 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | Cleanup vegetable gum fracturing fluid and preparation method thereof |
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2016
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Patent Citations (4)
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|---|---|---|---|---|
| US5364920A (en) * | 1993-01-08 | 1994-11-15 | Dow Corning Corporation | Method of crosslinking polysilazane polymers |
| US6475329B1 (en) * | 1999-10-04 | 2002-11-05 | Tyco Electronics Corporation | Primer for silicone compositions |
| CN101531892A (en) * | 2009-04-16 | 2009-09-16 | 大庆油田有限责任公司 | Ultra low temperature super guanidine gum fracturing fluid |
| CN103965860A (en) * | 2014-04-23 | 2014-08-06 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | Cleanup vegetable gum fracturing fluid and preparation method thereof |
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| 耐高温有机硅树脂的研制;吴松浩 等;《沈阳理工大学学报》;20111015;第30卷(第5期);第91-94页 * |
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Address after: Room 217, Comprehensive Building, Engineering Research Center for Nanomaterials, Jiyuan Hi-tech Industrial Development Zone, Henan Province, 454650 Patentee after: Jiyuan Haibori New Material Technology Co., Ltd. Address before: Room 217, Comprehensive Building of Henan Wangwu Nanotechnology Co., Ltd., Jiyuan Hi-tech Industrial Development Zone, Henan Province Patentee before: Jiyuan sea bri new and materials Co. Ltd. |
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