CN107033869A - A kind of nanometer Delayed Release Breaker and preparation method thereof - Google Patents

A kind of nanometer Delayed Release Breaker and preparation method thereof Download PDF

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Publication number
CN107033869A
CN107033869A CN201710267831.9A CN201710267831A CN107033869A CN 107033869 A CN107033869 A CN 107033869A CN 201710267831 A CN201710267831 A CN 201710267831A CN 107033869 A CN107033869 A CN 107033869A
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CN
China
Prior art keywords
breaker
nanometer
delayed release
preparation
gel
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Pending
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CN201710267831.9A
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Chinese (zh)
Inventor
郑存川
黄志宇
鲁红升
全红平
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Southwest Petroleum University
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Southwest Petroleum University
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Priority to CN201710267831.9A priority Critical patent/CN107033869A/en
Publication of CN107033869A publication Critical patent/CN107033869A/en
Pending legal-status Critical Current

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    • 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
    • C09K8/70Compositions for forming crevices or fractures characterised by their form or by the form of their components, e.g. foams
    • 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
    • C09K8/92Compositions for stimulating production by acting on the underground formation characterised by their form or by the form of their components, e.g. encapsulated material
    • 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
    • C09K2208/00Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/26Gel breakers other than bacteria or enzymes

Abstract

The invention discloses a kind of for nanometer Delayed Release Breaker of oil field fracturing fluid and preparation method thereof.Nanometer Delayed Release Breaker is using mesoporous nano silicon dioxide as carrier, and gel breaker is loaded into formation nanometer Delayed Release Breaker in mesopore orbit, and gel breaker slow release from mesopore orbit reaches delayed breaking down.Its preparation method includes:(1) using trimethyl cetyl ammonium bromide as template, tetraethoxysilane is presoma, and mesoporous nano silicon dioxide is made in the basic conditions;(2) mesoporous silicon oxide is scattered in deionized water, adds gel breaker shading stirring 24h, gel breaker is loaded into the mesopore orbit of nano silicon, centrifugation, washing obtain a nanometer Delayed Release Breaker.This nanometer of Delayed Release Breaker has preferably machinery and chemical stability, prepares simply, carryover effects are good.Nanometer Delayed Release Breaker is a kind of totally new kind of Delayed Release Breaker based on porous material, is had broad application prospects in oil-gas field fracturing.

Description

A kind of nanometer Delayed Release Breaker and preparation method thereof
Technical field
The present invention relates to nanometer Delayed Release Breaker of a kind of oil field compression fracture and preparation method thereof.
Background technology
Fracturing fluid is after pressing crack construction is finished, under crack closure stress, fracturing fluid leak formation filter cake so that split Polymer concentration is significantly increased in seam, is difficult thoroughly to break glue under the gel breaker of low concentration, the flow conductivity of fracture is produced sternly Grievous hurt.If adding excessive gel breaker, fracturing fluid can be caused to break glue in pressing crack construction again, cause pit shaft sand fallout.Broken glue Agent concentration is relatively low and glue can be caused brokenly not thorough, and it is relatively low that ability is flow backwards in crack.Therefore, fracturing fluid have to can and meanwhile have compared with Good solid-carrying performance and thorough broken colloidality energy.
In order to which fracturing fluid effectively takes sand when meeting pressing crack construction simultaneously and thoroughly broken glue returns row, Petroleum Engineer open It has issued capsule breaker.Capsule breaker is exactly that one layer of Paraffin wax coating is wrapped up outside conventional ammonium persulfate gel breaker, is prevented Only discharged in pressing crack construction.After pressing crack construction is finished, under the effect of formation closure pressure, brittle Paraffin wax coating rupture is released The gel breaker of parcel is released, so as to reach brokenly the purpose of glue.Because capsule breaker will not be released in advance in pressing crack construction process Put, to arrive after pressing crack construction finishes, can just be discharged under closure stress effect during crack closure, it is thereby achieved that prolonging The purpose of glue is broken late.The capsule breaker of higher concentration can be used in pressing crack construction, sand is taken when can meet pressing crack construction The requirement of performance, can meet pressure break and finish the requirement that thoroughly broken glue returns row again.
Although current capsule breaker has been carried out commercial Application, but still there are problems that.Capsule breaker exists Only part can rupture under fracture closure pressure.Fracturing fluid concentrates to form filter cake in crack closure, capsule breaker insertion In filter cake or in embedded rock, cyst wall can not effectively rupture, and gel breaker can not effectively discharge.The softgel shell of capsule breaker There are certain fracture pressure and fusing point, at high temperature under high pressure, the paraffin of cyst wall to melt or rupture in advance, therefore, It is subject to certain restrictions under HTHP.Further, since the imperfection of peel, causes gel breaker to discharge in advance.
Therefore, the present invention prepares a nanometer Delayed Release Breaker using mesoporous nano material.Mesoporous material is that a kind of duct is straight Footpath is more than 2nm and a kind of porous material less than 50nm, because mesoporous material has the skeleton structure enriched and duct knot Structure, with larger specific surface area, thus is widely applied to the fields such as catalysis, absorption, separation, insoluble drug release.The present invention Gel breaker is loaded into the mesopore orbit of mesoporous material, in pressing crack construction, gel breaker is from the mesopore orbit of nano material Slowly release, so as to realize the purpose for delaying brokenly glue.
The content of the invention
The purpose of the present invention:In order to realize the purpose of delayed breaking down in pressing crack construction, and overcome routine encapsulation delayed breaking down Agent discharges halfway problem, and the present invention is special to provide a kind of nanometer Delayed Release Breaker and its preparation side based on mesoporous material Method.
In order to achieve the above object, the present invention provides following technical scheme.
Nanometer Delayed Release Breaker, as carrier, gel breaker is loaded into mesopore orbit and made using mesoporous nano silicon dioxide It is standby to form.
The preparation of nanometer Delayed Release Breaker comprises the following steps:(1) 0.3g trimethyl cetyl ammonium bromides are added to In 80mL deionized waters, and add 0.175mL 2mol.L-1NaOH solution, stir and be warming up to 80 DEG C, then be added dropwise 1~ 1.2mL tetraethoxysilanes, are stirred for reacting 2h after dripping, and centrifuge and remove trimethyl ten with the ethanol solution of hydrochloric acid Six alkyl bromination ammoniums, that is, obtain mesoporous nano silicon dioxide;(2) 1g mesoporous nano silicon dioxides are scattered in 20mL deionized waters In, then add in 0.2~1g gel breakers shading stirring 24h, the mesopore orbit that gel breaker is loaded into nano silicon, centrifugation And washed with ethanol and obtain a nanometer Delayed Release Breaker.
Mesoporous nano silicon dioxide particle diameter is 10~300nm, a diameter of 2~4nm of mesopore orbit.
Gel breaker is loaded into the mesopore orbit of mesoporous silicon oxide, effective content be 5~10%, embedding rate be 85~ 95%.
During the gel breaker of loading can be ammonium persulfate, potassium peroxydisulfate, sodium hydrogensulfite, sodium sulfite, triethanolamine It is at least one;
Gel breaker slow dispersal events from the mesopore orbit of nano silicon, so as to realize delayed breaking down.
Compared with prior art, the invention has the advantages that:
(1) nanometer Delayed Release Breaker has preferably slow release performance, can realize delayed breaking down;
(2) nanometer Delayed Release Breaker has good mechanical stability and chemical stability;
(3) nanometer Delayed Release Breaker has nano-scale, can be more preferable in the microcrack that can enter pressure break formation Broken glue.
(4) nanometer Delayed Release Breaker is that slow dispersal events realize delayed breaking down in mesopore orbit by gel breaker, is broken Jelly release is more thorough.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
First, the preparation of nanometer Delayed Release Breaker
(1) 0.3g trimethyl cetyl ammonium bromides are added in 80mL deionized waters, and add 0.175mL 2mol.L-1NaOH solution, stir and be warming up to 80 DEG C, 1.2mL tetraethoxysilanes are then added dropwise, be stirred for after dripping anti- 2h is answered, centrifuges and removes trimethyl cetyl ammonium bromide with the ethanol solution of hydrochloric acid, that is, obtain mesoporous nano titanium dioxide Silicon;
(2) 1g mesoporous nano silicon dioxides are scattered in 20mL deionized waters, then add the stirring of 0.2g ammonium persulfates 24h, a nanometer delayed breaking down is obtained by the mesopore orbit of ammonium persulfate loading nano silicon, centrifuging and being washed with ethanol Agent.
2nd, the delayed breaking down ability of nanometer Delayed Release Breaker
Two parts of guanidine gum fracturing fluids are configured, original viscosity is 150mPa.s, the nanometer that 0.5% is added in wherein portion is prolonged It is directly added into slow gel breaker, another fracturing fluid under the conditions of ammonium persulfate gel breaker, 80 DEG C and carries out gel breaking test.Added after 1h The fracturing fluid viscosity retention rate of nanometer Delayed Release Breaker is still more than 60%, and is directly added into the fracturing fluid of the sour ammonium of persulfuric acid, thorough Glue is broken at bottom, and viscosity is less than 5mPa.s.
Embodiment 2
(1) 0.3g trimethyl cetyl ammonium bromides are added in 80mL deionized waters, and add 0.175mL NaOH Solution (2mol/L), stirs and is warming up to 80 DEG C, and 1.2mL tetraethoxysilanes are then added dropwise, and is stirred for reacting 2h after dripping, Centrifuge and use the ethanol solution of hydrochloric acid to remove trimethyl cetyl ammonium bromide, that is, obtain mesoporous nano silicon dioxide;
(2) 1g mesoporous nano silicon dioxides are scattered in 20mL deionized waters, then add 0.5g sodium hydrogensulfites and stir Mix 24h, will sodium hydrogensulfite be loaded into nano silicon mesopore orbit in, centrifuge and wash with ethanol obtain nanometer delay break Jelly.
2nd, the delayed breaking down ability of nanometer Delayed Release Breaker
Configure two parts of guanidine gum fracturing fluids, original viscosity be all add in 150mPa.s, two parts of fracturing fluids 0.1% over cure Sour ammonium.Added in portion 0.5% nanometer Delayed Release Breaker, be directly added into sodium hydrogensulfite gel breaker, 40 DEG C in another Under the conditions of carry out gel breaking test.The fracturing fluid viscosity retention rate that nanometer Delayed Release Breaker is added after 1h is still more than 80%, and straight The fracturing fluid for adding sodium hydrogensulfite is connect, viscosity retention ratio is only 20%.

Claims (6)

1. a kind of nanometer Delayed Release Breaker and preparation method thereof, it is characterised in that:Nanometer Delayed Release Breaker uses mesoporous nano two Gel breaker is loaded into mesopore orbit and is prepared from as carrier by silica.
2. a kind of nanometer Delayed Release Breaker as claimed in claim 1 and preparation method thereof, comprises the following steps:(1) by 0.3g tri- Methyl cetyl ammonium bromide is added in 80mL deionized waters, and adds 0.175mL 2mol/L NaOH solution, and stirring is simultaneously 80 DEG C are warming up to, 1~1.2mL tetraethoxysilanes are then added dropwise, is stirred for reacting 2h after dripping, centrifuges and use hydrochloric acid Ethanol solution remove trimethyl cetyl ammonium bromide, that is, obtain mesoporous nano silicon dioxide;(2) by 1g mesoporous nano dioxies SiClx is scattered in 20mL deionized waters, then adds 0.2~1g gel breakers stirring 24h, gel breaker is loaded into nanometer titanium dioxide In the mesopore orbit of silicon, centrifuge and washed with ethanol and obtain a nanometer Delayed Release Breaker.
3. a kind of nanometer Delayed Release Breaker as claimed in claim 1 and preparation method thereof, it is characterised in that:Mesoporous nano titanium dioxide Silicon grain footpath is 10~300nm, a diameter of 2~4nm of mesopore orbit.
4. a kind of nanometer Delayed Release Breaker as claimed in claim 1 and preparation method thereof, it is characterised in that:Gel breaker is loaded into Jie In the mesopore orbit of hole silica, effective content is 5~10%, and embedding rate is 85~95%.
5. a kind of nanometer Delayed Release Breaker as claimed in claim 1 and preparation method thereof, it is characterised in that:The gel breaker of loading can To be at least one of ammonium persulfate, potassium peroxydisulfate, sodium hydrogensulfite, sodium sulfite, triethanolamine.
6. a kind of nanometer Delayed Release Breaker as claimed in claim 1 and preparation method thereof, it is characterised in that:Gel breaker is from nanometer two Dissolve, be desorbed in the mesopore orbit of silica and slow dispersal events, so as to reach the effect of delayed breaking down.
CN201710267831.9A 2017-04-22 2017-04-22 A kind of nanometer Delayed Release Breaker and preparation method thereof Pending CN107033869A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109439071A (en) * 2018-11-26 2019-03-08 西南石油大学 A kind of preparation method of the smart coat of carbon dioxide stimuli responsive
CN112940703A (en) * 2021-02-03 2021-06-11 中国石油化工股份有限公司 Low-temperature gel breaker for fracturing fluid and preparation method of low-temperature gel breaker
CN115612477A (en) * 2022-10-31 2023-01-17 陕西科技大学 Silica aerogel loaded gel breaker and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103641122A (en) * 2013-11-15 2014-03-19 华东师范大学 Preparation method for multilevel mesoporous silica nanoparticles
CN104263335A (en) * 2014-08-29 2015-01-07 中国石油集团渤海钻探工程有限公司 Low-density early-strength micro-expanding cement mortar and preparation method thereof
CN105419773A (en) * 2015-12-25 2016-03-23 中国石油天然气股份有限公司 High temperature resistant delayed gel breaking agent and preparation method thereof
CN106190084A (en) * 2016-07-12 2016-12-07 山东大学 The preparation of a kind of nano material height wax heavy crude thinner and performance test

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103641122A (en) * 2013-11-15 2014-03-19 华东师范大学 Preparation method for multilevel mesoporous silica nanoparticles
CN104263335A (en) * 2014-08-29 2015-01-07 中国石油集团渤海钻探工程有限公司 Low-density early-strength micro-expanding cement mortar and preparation method thereof
CN105419773A (en) * 2015-12-25 2016-03-23 中国石油天然气股份有限公司 High temperature resistant delayed gel breaking agent and preparation method thereof
CN106190084A (en) * 2016-07-12 2016-12-07 山东大学 The preparation of a kind of nano material height wax heavy crude thinner and performance test

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109439071A (en) * 2018-11-26 2019-03-08 西南石油大学 A kind of preparation method of the smart coat of carbon dioxide stimuli responsive
CN112940703A (en) * 2021-02-03 2021-06-11 中国石油化工股份有限公司 Low-temperature gel breaker for fracturing fluid and preparation method of low-temperature gel breaker
CN115612477A (en) * 2022-10-31 2023-01-17 陕西科技大学 Silica aerogel loaded gel breaker and preparation method and application thereof

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