CN106167699A - A kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker and its preparation method and application - Google Patents

A kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker and its preparation method and application Download PDF

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Publication number
CN106167699A
CN106167699A CN201610581378.4A CN201610581378A CN106167699A CN 106167699 A CN106167699 A CN 106167699A CN 201610581378 A CN201610581378 A CN 201610581378A CN 106167699 A CN106167699 A CN 106167699A
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fracturing fluid
novel low
low carbon
aluminum crosslinker
crosslinker
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CN106167699B (en
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毛金成
王鼎立
杨小江
李勇明
赵金洲
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Southwest Petroleum University
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Southwest Petroleum University
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/62Compositions for forming crevices or fractures
    • C09K8/66Compositions based on water or polar solvents
    • C09K8/68Compositions based on water or polar solvents containing organic compounds
    • C09K8/685Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/62Compositions for forming crevices or fractures
    • C09K8/66Compositions based on water or polar solvents
    • C09K8/665Compositions based on water or polar solvents containing inorganic compounds

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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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Abstract

The present invention proposes a kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker and its preparation method and application, and wherein aluminum crosslinker is mainly made up of according to mass fraction following material: host 20 27 crosslinking accelerator 37 parts;45 60 parts of water.The preparation of cross-linking agent comprises the steps: to add the water of certain proportioning in reaction vessel;Add host to stir reaction;Finally add crosslinking accelerator stirring reaction 15 minutes.This novel aluminum crosslinker is fast with gellant crosslinking rate, plastic is stable, preparation process is simple and convenient, with low cost, and fracturing fluid system has stronger heatproof shear resistant, and unconventional temperature reservoirs fracturing work is had good effect.

Description

A kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker and its preparation method and application
Technical field
The present invention relates to technical field of petroleum extraction, especially relate to a kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker And its preparation method and application.
Background technology
Oil and natural gas is as the high-grade energy of national economy and social development, to ensureing that national economy and society hold Continuous fast development has very important significance.In recent years, along with the fast development of China's economy, oil gas imbalance between supply and demand is more drilled more Strong, crude oil import amount increases year by year.And conventional gas and oil resource is faced with production capacity and seriously reduces even exhausted problem, this allows for Shale gas, coal bed gas, the unconventional petroleum resources such as fine and close oil gas is increasingly paid attention to by whole world various countries.The unconventional oil of China Gas resource is the abundantest, and gross reserves is about the twice of conventional gas and oil resource, has the biggest exploration prospect.Unconventionaloil pool reservoir The core technology of exploitation is fracturing reform, and fracturing fluid is as one of important component part in pressing crack construction process, is described as pressure Split " blood ".Reservoir reconstruction effect after pressure break, while determining pressing crack construction success or not, also can be produced by the performance of fracturing fluid Raw strong influence.
Generally, fracturing fluid should have Heat stability is good, solid-carrying performance is good, frictional resistance is low, the row of returning leads height, residue is low, it is little to injure Etc. feature, but owing to Unconventional reservoir physical property is poor, porosity, permeability are relatively low, use the fracturing fluid of routine to easily cause Water trapping injures, and is unfavorable for fracturing yield increasing, and tradition fracturing fluid heatproof anti-shear performance is poor, perishable, needs to consume greatly Amount water resource, seldom returns and is discharged to ground and is safely handled, and the relevant environment pollution problem that pressure break causes increasingly is subject to Pay attention to people.For solving the problems referred to above, studying and prepare the anhydrous fracturing fluid of novel low-carbon alkanes has vital Effect.The anhydrous fracturing fluid of lower carbon number hydrocarbons is a kind of low-density of development, low-viscosity, low capillary pipe on the basis of conventional oil base fracturing fluid The fracturing fluid system of resistance, have good with Unconventional reservoir rock compatibility, pressure break efficiency high, little to formation damage, take sand The advantages such as performance is good, it is adaptable to the fracturing yield increasing that unconventionaloil pool is hidden.This technology is possible not only to solve a hydropenia difficult problem, moreover it is possible to reduce Oil and gas reservoir exploitation pollution on the environment, the exploitation to unconventionaloil pool reservoir has important directive significance.
Cross-linking agent is as a kind of important additive in the anhydrous fracturing fluid system of lower carbon number hydrocarbons, and its performance is to whole fracturing fluid The cross-linking process of system has important impact.Cross-linking agent is by host, phase transfer catalyst, chelating agent and crosslinking accelerator group Become.Host is generally ferric iron or the heavy metallic salt such as titanium, nickel, has an effect with gellant after addition, with the shape of colloidal particle Formula crosslinking is attached in alkyl gellant, makes base fluid thickening become frozen glue.Its space net structure can to greatest extent with stone Petroleum hydrocarbon molecule forms more stable supermolecule associated complex system, has specific viscosity and macroscopic property.Grind both at home and abroad at present The anhydrous fracturing liquid cross-linking agent of lower carbon number hydrocarbons studied carefully and apply is mainly with Fe3+Slaine is mainly used in oil base as host, trivalent aluminium salt In fracturing fluid, it is common that directly using trivalent iron salt to cross-link with dialkyl phosphate as cross-linking agent, cross-linking process is very Slowly, complex operation, dosing is complicated, wayward, and cross-linking agent dissolubility is slow, poor stability, and the requirement to pressing crack construction is special The highest.
Chinese patent CN104498017A discloses a kind of fracturing liquid cross-linking agent and preparation thereof and application, but this cross-linking agent Prepare fracturing fluid temperature tolerance and prop-carrying capacity be improved not yet, temperature tolerance only has 90 DEG C, it is impossible in adaptation high temperature oil field and Ultra-deep Holes of Complicated Wells.And, its crosslinker component is complicated, prepares loaded down with trivial details, uses alcohol and water to exist as mixed solvent, field operation Certain potential safety hazard.
Summary of the invention
The present invention proposes a kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker and its preparation method and application, this anhydrous Fracturing liquid cross-linking agent is fast with gellant crosslinking rate, plastic is stable, preparation process is simple and convenient, with low cost, and fracturing liquid It is that temperature resistance anti-shear ability is strong, ideal for temperature reservoirs fracturing effect.
A kind of technical scheme of the present invention is achieved in that a kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker, institute State fracturing liquid cross-linking agent to be made up of according to mass fraction following material:
Host 20-27 part;
Crosslinking accelerator 3-7 part;
Water 45-60 part.
As the preferred technical scheme of one, described host is in aluminum sulfate, aluminum chloride, aluminum nitrate and sodium metaaluminate Kind or several mixture.
As the preferred technical scheme of one, described crosslinking accelerator be ethanolamine, triethylene tetramine, diethylenetriamine, One or several mixture of N, N-dimethylated propyl diethylenetriamine and isopropanolamine.
The another kind of technical scheme of the present invention is achieved in that a kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker Preparation method, comprises the steps:
(1) in reaction vessel, add the water of certain proportioning;
(2) add a certain amount of host to stir reaction;
(3) crosslinking accelerator stirring reaction 15 minutes it is eventually adding.
The another kind of technical scheme of the present invention is achieved in that a kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker Application, the anhydrous fracturing liquid cross-linking agent of described lower carbon number hydrocarbons can be cross-linked to form fracturing fluid with phosphate ester gellant and lower carbon number hydrocarbons alkane and freeze Glue.
As the preferred technical scheme of one, comprise the steps:
(1) phosphate ester gellant is joined fully dissolve in the middle of lower carbon number hydrocarbons alkane;
(2) fracturing liquid cross-linking agent joined in the middle of the mixing base fluid described in step (1) and stir two with mechanical agitator Minute can be prepared by the anhydrous fracturing fluid gel of novel low carbon hydrocarbon.
As the preferred technical scheme of one, described fracturing liquid cross-linking agent is 1 with the mass ratio of described phosphate ester gellant: 1.1-1:1.4;Described phosphate ester gellant weight/mass percentage composition in lower carbon number hydrocarbons is 3%-7%.
As the preferred technical scheme of one, described lower carbon number hydrocarbons be carbon number be the alkane of 4-8.
As the preferred technical scheme of one, described lower carbon number hydrocarbons is pentane or hexane.
Have employed technique scheme, the invention have the benefit that
(1) crosslinking accelerator in this cross-linking agent can be accelerated the formation of metal cation complex and appoint without adding What alcohols double solvents, reduces running cost, it is easier to reach the purpose of industrialized production.
(2) this cross-linking agent preparation technology is simple, and raw material is cheap, and preparation time is short, can matching while using at any time, and permissible It is greatly shortened crosslinking time within two minutes.
(3) this fracturing fluid gel is at 150 DEG C, and more than 2MPa high pressure fracturing fluid viscosity still can reach 50mPa s, complete Full up sufficient pressing crack construction standard, fracturing fluid system has stronger temperature resistance shear resistant and takes husky performance, to on-the-spot pressing crack construction There is important practical significance.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing In having technology to describe, the required accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only this Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, also may be used To obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the pressure break utilizing the cross-linking agent prepared in embodiment 1 to prepare with phosphate ester gellant plastic in pentane Liquid system is viscosity time dependent heatproof curve when 120 DEG C;
Fig. 2 is the pressure break utilizing the cross-linking agent prepared in embodiment 2 to prepare with phosphate ester gellant plastic in normal hexane Liquid system is viscosity time dependent resistant to shearing curve when 150 DEG C.
Fig. 3 is the pressure break utilizing the cross-linking agent prepared in embodiment 1 to prepare with phosphate ester gellant plastic in pentane The gel structure figure that lyogel is observed under scanning electron microscope.
Wherein:
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments wholely.Based on Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under not making creative work premise Embodiment, broadly falls into the scope of protection of the invention.
Embodiment 1:
Take in the beaker that 45 parts of water join 250mL, and be positioned on magnetic stirring apparatus, add 20 parts of aluminum sulfate stirrings anti- Answer 10 minutes, be eventually adding 3 parts of isopropanolamines and stir reaction within 15 minutes, can be prepared by novel crosslinker.
Embodiment 2:
Take in the beaker that 52 parts of water join 250mL, and be positioned on magnetic stirring apparatus, add 25 parts of aluminum chloride stirrings React 10 minutes, be eventually adding 6 parts of ethanolamine and stir reaction within 15 minutes, can be prepared by novel crosslinker.
Embodiment 3:
Take in the beaker that 60 parts of water join 250mL, and be positioned on magnetic stirring apparatus, add 27 parts of aluminum nitrate stirrings React 10 minutes, be eventually adding 7 parts of triethylene tetramines and stir reaction within 15 minutes, can be prepared by novel crosslinker.
Embodiment 4:
The cross-linking agent dosage 4% prepared according to embodiment 1 and the phosphate ester gellant of dosage 5% join in pentane to be handed over Connection (seeing patent of invention US4877894, US7328744, US5614010 etc., the preparation method of the anhydrous fracturing fluid of lower carbon number hydrocarbons), hands over After connection, fracturing fluid gel has good viscoelasticity and apparent viscosity.Subsequently in Mars III type High Temperature High Pressure rotational rheometer, Test the heatproof endurance of cutting of fracturing fluid gel.Result shows at 120 DEG C of constant temperature, 170s-1Under rotating speed, persistently shear 2h (i.e. 120min), viscosity can be maintained at more than 100mPa s;At 170s-1Under rotating speed, in 50min, it is gradually heating to 150 DEG C, investigates Its resistant to shearing performance, along with the rising of temperature, the viscosity of fracturing fluid gel is gradually reduced;When temperature is increased to 150 DEG C, pressure break The viscosity of lyogel can also reach 50mPa s, and (seeing Fig. 1, Fig. 2) meets industry standard.Additionally, the knot to fracturing fluid gel Structure is investigated, and is placed under Quanta 450 type environmental scanning electron microscope observing, and (seeing Fig. 3) finds, The tridimensional network of complexity it has been internally formed so that gel molecular becomes a kind of stable supermolecule and associates at fracturing fluid gel Thing, and there is specific viscosity and macroscopic property, meet expection imagination.Show fracturing fluid gel to have well and take husky effect Really, fracturing work requirement can be fully met.
Embodiment 5:
Respectively according to embodiment 2, the phosphate ester gellant of the cross-linking agent dosage 4% and 6% prepared by 3 also adds normal hexane Fracturing fluid gel (with embodiment 4) is prepared in crosslinking, and after crosslinking, fracturing fluid gel has good viscoelasticity and apparent viscosity.Subsequently Investigate the heatproof endurance of cutting of fracturing fluid gel rubber system.In Mars III type High Temperature High Pressure rotational rheometer, carry out that heatproof is resistance to cuts Cutting property is tested.Result shows at 90 DEG C of constant temperature, 170s-1Persistently shear 2h (i.e. 120min) viscosity afterwards under rotating speed can be kept at 460mPa s and more than 520mPa s, when temperature is increased to 150 DEG C, the viscosity of two kinds of fracturing fluid gels still can maintain More than 70mPa s.Show this fracturing fluid gel to have well and take husky effect, fracturing work requirement can be fully met.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention Within god and principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.

Claims (9)

1. a novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker, it is characterised in that: described fracturing liquid cross-linking agent is by following material Form according to mass fraction:
Host 20-27 part;
Crosslinking accelerator 3-7 part;
Water 45-60 part.
A kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker the most according to claim 1, it is characterised in that: described host For one or several the mixture in aluminum sulfate, aluminum chloride, aluminum nitrate and sodium metaaluminate.
A kind of novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker the most according to claim 1, it is characterised in that: described crosslinking Accelerator is ethanolamine, triethylene tetramine, diethylenetriamine, N, one or several of N-dimethylated propyl diethylenetriamine and isopropanolamine Mixture.
4. the preparation method of a novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker, it is characterised in that: comprise the steps:
(1) in reaction vessel, add the water of certain proportioning;
(2) add a certain amount of host to stir reaction;
(3) crosslinking accelerator stirring reaction 15 minutes it is eventually adding.
5. the application of a novel low carbon hydrocarbon anhydrous fracturing fluid aluminum crosslinker, it is characterised in that: the anhydrous fracturing fluid of described lower carbon number hydrocarbons Cross-linking agent can be cross-linked to form fracturing fluid gel with phosphate ester gellant and lower carbon number hydrocarbons alkane.
The application of a kind of novel low carbon hydrocarbon the most according to claim 5 anhydrous fracturing fluid aluminum crosslinker, it is characterised in that bag Include following steps:
(1) phosphate ester gellant is joined fully dissolve in the middle of lower carbon number hydrocarbons alkane;
(2) fracturing liquid cross-linking agent joined in the middle of the mixing base fluid described in step (1) and stir two minutes with mechanical agitator Can be prepared by the anhydrous fracturing fluid gel of novel low carbon hydrocarbon.
The application of a kind of novel low carbon hydrocarbon the most according to claim 6 anhydrous fracturing fluid aluminum crosslinker, it is characterised in that institute The mass ratio stating fracturing liquid cross-linking agent and described phosphate ester gellant is 1:1.1-1:1.4;Described phosphate ester gellant is at low-carbon (LC) In hydrocarbon, weight/mass percentage composition is 3%-7%.
The application of a kind of novel low carbon hydrocarbon the most according to claim 7 anhydrous fracturing fluid aluminum crosslinker, it is characterised in that institute State lower carbon number hydrocarbons be carbon number be the alkane of 4-8.
The application of a kind of novel low carbon hydrocarbon the most according to claim 8 anhydrous fracturing fluid aluminum crosslinker, it is characterised in that institute Stating lower carbon number hydrocarbons is pentane or hexane.
CN201610581378.4A 2016-07-21 2016-07-21 A kind of anhydrous fracturing fluid aluminum crosslinker of novel low carbon hydrocarbon and its preparation method and application Expired - Fee Related CN106167699B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106905360A (en) * 2017-04-07 2017-06-30 西南石油大学 One-step synthesis phosphate gelling agent and the method for preparing the anhydrous fracturing fluid of lower carbon number hydrocarbons
CN108300449A (en) * 2018-03-16 2018-07-20 中国石油大学(华东) A kind of ethers fracturing fluid
CN113755151A (en) * 2021-10-25 2021-12-07 郑州市新郑梅久实业有限公司 Novel high-temperature-resistant nano composite zirconium cross-linking agent and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060096756A1 (en) * 2004-11-09 2006-05-11 Halliburton Energy Services, Inc. Difunctional phosphorus-based gelling agents and gelled nonaqueous treatment fluids and associated methods
CN104004506A (en) * 2014-06-18 2014-08-27 西安石油大学 Anhydrous fracturing fluid suitable for unconventional reservoir fracturing and preparing method of anhydrous fracturing fluid
CN104498017A (en) * 2014-12-22 2015-04-08 中国石油天然气股份有限公司 Fracturing fluid cross-linking agent and preparation and application thereof
CN105062458A (en) * 2015-09-02 2015-11-18 西南石油大学 Preparation and application of low-hydrocarbon anhydrous fracturing fluid crosslinking agent for unconventional reservoirs

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060096756A1 (en) * 2004-11-09 2006-05-11 Halliburton Energy Services, Inc. Difunctional phosphorus-based gelling agents and gelled nonaqueous treatment fluids and associated methods
CN104004506A (en) * 2014-06-18 2014-08-27 西安石油大学 Anhydrous fracturing fluid suitable for unconventional reservoir fracturing and preparing method of anhydrous fracturing fluid
CN104498017A (en) * 2014-12-22 2015-04-08 中国石油天然气股份有限公司 Fracturing fluid cross-linking agent and preparation and application thereof
CN105062458A (en) * 2015-09-02 2015-11-18 西南石油大学 Preparation and application of low-hydrocarbon anhydrous fracturing fluid crosslinking agent for unconventional reservoirs

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106905360A (en) * 2017-04-07 2017-06-30 西南石油大学 One-step synthesis phosphate gelling agent and the method for preparing the anhydrous fracturing fluid of lower carbon number hydrocarbons
CN108300449A (en) * 2018-03-16 2018-07-20 中国石油大学(华东) A kind of ethers fracturing fluid
CN113755151A (en) * 2021-10-25 2021-12-07 郑州市新郑梅久实业有限公司 Novel high-temperature-resistant nano composite zirconium cross-linking agent and preparation method and application thereof

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