CN1325598C - Microcapsule degelling agent and its preparation method - Google Patents

Microcapsule degelling agent and its preparation method Download PDF

Info

Publication number
CN1325598C
CN1325598C CNB200410097105XA CN200410097105A CN1325598C CN 1325598 C CN1325598 C CN 1325598C CN B200410097105X A CNB200410097105X A CN B200410097105XA CN 200410097105 A CN200410097105 A CN 200410097105A CN 1325598 C CN1325598 C CN 1325598C
Authority
CN
China
Prior art keywords
capsule
preparation
microcapsule degelling
agents according
microcapsule
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CNB200410097105XA
Other languages
Chinese (zh)
Other versions
CN1786101A (en
Inventor
刘德铸
刘建权
李军
刘伟
李超
张宁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Petroleum and Natural Gas Co Ltd
Original Assignee
China Petroleum and Natural Gas Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Petroleum and Natural Gas Co Ltd filed Critical China Petroleum and Natural Gas Co Ltd
Priority to CNB200410097105XA priority Critical patent/CN1325598C/en
Publication of CN1786101A publication Critical patent/CN1786101A/en
Application granted granted Critical
Publication of CN1325598C publication Critical patent/CN1325598C/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C09K8/706Encapsulated breakers

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Medicinal Preparation (AREA)

Abstract

The present invention discloses a microcapsule degelling agent and a preparation method thereof. The microcapsule degelling agent contains 85.5 to 91.2 wt% of capsule core material, 8 to 13 wt% of coating layer and 0.8 to 1.5 wt% of additive. The capsule core material contains persulphate, hypochlorite, hypobromite, potassium permanganate, potassium dichromate or combination of persulphate, hypochlorite, hypobromite, potassium permanganate and potassium dichromate. The preparation method comprises the following technical steps: raw materials are added into a side spray fluidized bed, binding agent solution is added, the side spray fluidized bed is turned on, etc., and the microcapsule degelling agent is prepared. The covered rate of a product can reach more than 99.8%, and the content of effective components can reach 90%. Simultaneously, within the range of 10 to 30 Mpa, the appropriate compressive strength for the product can be selected according to the closing pressure of different strata.

Description

A kind of microcapsule degelling agent and preparation method thereof
Technical field
The present invention relates to the oil field with broken glue technology, in particular for the microcapsule degelling agent technology in the fracturing liquid.
Background technology
Oil-field development is to the middle and later periods, and waterfrac treatment is one of the most effective well stimulation, and capsule breaker plays the effect that makes the crosslinked and broken glue ability of fracturing liquid united and coordinating in measure is implemented.
Present widely used conventional gel breaker in the construction, all be by with the fracturing liquid hybrid reaction, destroy crosslinked condition and the degradation polymer macromole reaches brokenly the glue viscosity reducing effect.Gel breaker directly is dissolved in the fracturing liquid, and release rate is fast, and to the liquid properties influence greatly: excessive or constant adds, and cross-linking properties may occur and reduce rapidly, breaks glue in advance, causes the sand plug of constructing; The amount of owing adds, and gelled fracturing fluid may break the bad even broken glue of glue, will cause serious secondary injury to reservoir, causes easily that also the stratum tells sand, influences construction effect greatly.Capsule breaker relies on its good slow release, controlled-release function well to solve this problem.
Capsule breaker have good slow release, a controlled release properties.In the construction process, the capsule breaker of excessive adding is because its slow releasing function makes fracturing liquid keep better performance; After construction finishes, crack closure, capsule clothing slowly-releasing reaches distortion under reservoir stress, breaks, and capsule heart effective constituent discharges in a large number, makes fracturing liquid rapidly, thoroughly break glue, has improved the of the fracturing fluid row of returning and has led, and reduces the secondary injury to the stratum.Capsule breaker had both increased the stability of construction, had improved the validity of construction again.
Existing capsule breaker product mostly is two-layered coating, and is impervious material substantially, and bed thickness then slow-release time is long, and layer is thin, and then encapsulation ratio is low, is difficult for grasping its performance; And capsule breaker of the present invention is three layers of dressing: slow release layer, impervious barrier, supporting layer.The slow release layer of product, impervious barrier provide the good slow release ability, and the hardness by supporting layer, fragility is the ultimate compression strength of may command product again, makes product have good controlled-release function.Preparation technology's main body that currently available products adopts mostly is coating pan or similar technology, the top whitewashing, this kind technology is subjected to the influence of pot body rotating speed and whitewashing mode, product degree of sphericity low (coating effect will be given a discount), the product skin that obtains is loose, encapsulation ratio is 95~98% only, and sustained release performance is wayward.Adopting process of the present invention is the granulation of side jet flow, end jet flow dressing, whitewashing and particle motion basically identical, and bed body employing frequency conversion control speed, and the particle degree of sphericity height that obtains, coating effect is good, the controllability height.
Technology contents
The purpose of this invention is to provide a kind of microcapsule degelling agent and preparation technology thereof, under the prerequisite of the prop-carrying capacity of not losing fracturing fluid gel, in the excessive adding fracturing liquid, make its broken glue more thorough, and the timely row of returning, reducing secondary injury to the stratum, the raising measure is efficient.
Microcapsule degelling agent of the present invention comprises capsule heartwood material, coating and additive, its weight ratio is 85.5~91.2%:8~13%:0.8~1.5%, and capsule heartwood material package is drawn together one-component or its combination of persulphate, hypochlorite, hypobromite, potassium permanganate, potassium bichromate.The particle diameter of capsule heartwood material is 0.2~0.45mm, and its size-grade distribution value is narrow, and granularity is thinner, be more evenly distributed, and helps the raising of encapsulation ratio and ultimate compression strength, the controllability of the product performance that improve from capsule heart selection aspect.
Its coating is divided into three parts, i.e. slow release layer, impervious barrier and supporting layer.Wherein, supporting layer is by the acrylonitritrile-styrene resin preparation, and slow release layer is by the acrylic resin preparation, and impervious barrier is by poly-asymmetric Ethylene Dichloride preparation.
Its additive comprises binding agent, antistatic agent, increases crisp dose, and total content is 0.8~1.5%, directly is mixed during use in coating liquid, improves the parcel quality.Binding agent is vegetable jelly (as a guar gum) or derivatives thereof, consumption 2~4 ‰, and its effect is to improve weighting material viscosity degree when preparation capsule bulbus cordis grain; Antistatic agent is white carbon black or talcum powder, consumption 3~6 ‰, and its effect is to reduce the poly-heap phenomenon that is produced by electrostatic interaction in the preparation process; Increase crisp dose and be cement, consumption 3~5 ‰, the releasing degree with regulating product can effectively break product under locking pressure, discharge capsule heart composition.
The preparation method of microcapsule degelling agent of the present invention is:
(1) getting some amount joins in the side spray fluidized-bed through the capsule heart particle of the 0.20-0.45mm of screen analysis;
(2) binder solution of adding 2 ‰ in liquid supply vehicle, the ratio in 1% adds capsule heartwood material;
(3) open side spray fluidized-bed sprays to the binding agent mixed solution on the capsule heart particle after the screen analysis by spray gun; This process continued to capsule bulbus cordis grain length to 0.7mm;
(4) preparation slow release layer dressing solution:, add antistatic agent with the dissolve with ethanol acrylic resin;
(5) open end spray fluidized-bed, slow release layer all is sprayed on the capsule bulbus cordis grain;
(6) preparation impervious barrier dressing solution:, add antistatic agent with the poly-asymmetric Ethylene Dichloride of pimelinketone dissolving;
(7) spraying impervious barrier coating liquid on capsule bulbus cordis grain;
(8) preparation supporting layer solution: acrylonitritrile-styrene resin is dissolved in the pimelinketone, adds antistatic agent, increase crisp dose;
(9) to capsule bulbus cordis grain spraying supporting layer.
Device parameter in the preparation process is as follows:
The A pelletization:
Side spray fluidized-bed rotating speed: 55~75rpm
Angle: level
Temperature: room temperature
Whitewashing flow: 20~30ml/min
Whiff pressure: 0.15~0.35Mpa
Air blast flux: 300~600l/min
B dressing process:
Air blast flux: 300~600l/min
Angle: vertical
Temperature: 38-50 ℃
Whitewashing flow: 35~70ml/min
Whiff pressure: 0.25~0.5Mpa
The present invention proposes the preparation technology of side spray fluidized bed granulation, end spray fluidized bed coating, film controlled release and framework controlled release association mechanism, four-layer structure: the capsule heart, slow release layer, impervious barrier and supporting layer are adopted in the release of product effective constituent.The product encapsulation ratio can reach more than 99.8%, and active constituent content can reach 90%, in 10~30Mpa scope, can select suitable product ultimate compression strength according to the Different Strata locking pressure simultaneously.
Embodiment
Embodiment 1
(1) getting the 2Kg particle diameter is that the ammonium persulphate particle of 0.20-0.45mm joins in the side spray fluidized-bed;
(2) preparation 4L binder solution (melon glue+4L water of 6g) adds 40g ammonium persulphate pulvis;
(3) open side spray fluidized-bed is regulated rotating speed 55rpm, and the whitewashing flow is 20ml/min, whiff pressure 0.20Mpa, and air blast flux: 400L/min sprays to binding agent on the ammonium persulphate particle; When binder solution was sprayed onto 3.6L, the raising rotating speed was 70rpm, whitewashing flow 25ml/min, whiff pressure 0.25Mpa;
(4) preparation slow release layer solution:, add 3g antistatic agent talcum powder with 5L dissolve with ethanol 90g acrylic resin;
(5) open end spray fluidized-bed, air blast flux: 450L/min, 40 ℃ of temperature, whitewashing flow 40ml/min, whiff pressure 0.25Mpa is sprayed into the slow release layer coating liquid on the capsule bulbus cordis grain;
(6) preparation impervious barrier solution:, add the 3g antistatic agent with the poly-asymmetric Ethylene Dichloride of 10L pimelinketone dissolving 60g;
(7) air blast flux: 450L/min, 45 ℃ of temperature, whitewashing flow 40ml/min, whiff pressure 0.25Mpa, spraying impervious barrier coating liquid on capsule bulbus cordis grain;
(8) preparation supporting layer solution: with 10L pimelinketone dissolving 50g acrylonitritrile-styrene resin, adding 5g antistatic agent talcum powder, 8g increase crisp dose;
(9) air blast flux: 520L/min, 45 ℃ of temperature, whitewashing flow 45ml/min, whiff pressure 0.3Mpa is to capsule bulbus cordis grain spraying supporting layer; When supporting layer solution was sprayed onto 9.8L, regulating the whitewashing flow was 60ml/min, whiff pressure 0.4Mpa.Dry fully until product.
Product encapsulation ratio 99.9%, ultimate compression strength 20Mpa can be used in the waterfrac treatment measure of middle hot hole section.
Embodiment 2
(1) getting Potassium Persulphate particle and the 1Kg Losantin powder that the 1Kg particle diameter is 0.20-0.45mm joins in the side spray fluidized-bed;
(2) preparation 4L binder solution (hydroxypropyl guar gum of 5g+4L water) adds 40g ammonium persulphate pulvis;
(3) open side spray fluidized-bed is regulated rotating speed 60rpm, and the whitewashing flow is 23ml/min, whiff pressure 0.22Mpa, and air blast flux: 400L/min sprays to binding agent on the Potassium Persulphate particle; When binder solution was sprayed onto 3.6L, the raising rotating speed was 70rpm, whitewashing flow 28ml/min, whiff pressure 0.25Mpa;
(4) preparation slow release layer solution:, add the 3g antistatic agent with 5L dissolve with ethanol 110g acrylic resin;
(5) open end spray fluidized-bed, air blast flux: 450L/min, 41 ℃ of temperature, whitewashing flow 38ml/min, whiff pressure 0.25Mpa is sprayed into the slow release layer coating liquid on the capsule bulbus cordis grain;
(6) preparation impervious barrier solution:, add the 3g antistatic agent with the poly-asymmetric Ethylene Dichloride of 10L pimelinketone dissolving 40g;
(7) air blast flux: 450L/min, 45 ℃ of temperature, whitewashing flow 42ml/min, whiff pressure 0.27Mpa, spraying impervious barrier coating liquid on capsule bulbus cordis grain;
(8) preparation supporting layer solution: with 10L pimelinketone dissolving 35g acrylonitritrile-styrene resin, adding 4g antistatic agent, 10g increase crisp dose;
(9) air blast flux: 520L/min, 45 ℃ of temperature, whitewashing flow 48ml/min, whiff pressure 0.35Mpa is to capsule bulbus cordis grain spraying supporting layer; When supporting layer solution was sprayed onto 9.8L, regulating the whitewashing flow was 65ml/min, whiff pressure 0.4Mpa.Dry fully until product.
Product encapsulation ratio 99.8%, ultimate compression strength 13Mpa can be used in the waterfrac treatment measure of low hot-well section.

Claims (11)

1 one kinds of microcapsule degelling agents, comprise capsule heartwood material, coating and additive, its weight ratio is a capsule heartwood material: coating: additive is 85.5%~91.2%:8%~13%:0.8%~1.5%, and capsule heartwood material package is drawn together the one-component of the combination of persulphate, hypochlorite, hypobromite, potassium permanganate, potassium bichromate or oxymuriate, hypobromite, potassium permanganate, potassium bichromate.
The 2 described microcapsule degelling agents according to claim 1, the granularity of its capsule heartwood material is 0.2~0.45mm.
3 microcapsule degelling agents according to claim 1, described coating are three layers, i.e. supporting layer, slow release layer and impervious barrier.
4 microcapsule degelling agents according to claim 3, described supporting layer is prepared by acrylonitritrile-styrene resin.
5 microcapsule degelling agents according to claim 3, described slow release layer is by poly-asymmetric Ethylene Dichloride preparation.
6 microcapsule degelling agents according to claim 3, described impervious barrier is prepared by acrylic resin.
7 microcapsule degelling agents according to claim 1, described additive comprise binding agent, antistatic agent, increase crisp dose, and total content is 0.8%~1.5%.
8 microcapsule degelling agents according to claim 7, binding agent wherein are the vegetable jelly or derivatives thereof, and consumption is 2 ‰~4 ‰.
9 microcapsule degelling agents according to claim 7, antistatic agent wherein are talcum powder, consumption 3 ‰~6 ‰.
10 microcapsule degelling agents according to claim 7, wherein increase crisp dose for cement or white carbon black, consumption 3 ‰~5 ‰.
The preparation method of 11 1 kinds of microcapsule degelling agents as claimed in claim 1:
(1) getting some amount joins in the side spray fluidized-bed through the capsule heart particle of the 0.20-0.45mm of screen analysis;
(2) in reservoir, add a certain proportion of binder solution, add capsule heartwood material more by a certain percentage;
(3) open side spray fluidized-bed sprays to the binding agent mixed solution on the capsule heart particle after the screen analysis by spray gun; This process continued to capsule bulbus cordis grain length to 0.7mm;
(4) preparation slow release layer dressing solution:, add antistatic agent with the dissolve with ethanol acrylic resin;
(5) open end spray fluidized-bed, slow release layer all is sprayed on the capsule bulbus cordis grain;
(6) preparation impervious barrier dressing solution:, add antistatic agent with the poly-asymmetric Ethylene Dichloride of pimelinketone dissolving;
(7) spraying impervious barrier coating liquid on capsule bulbus cordis grain;
(8) preparation supporting layer solution: acrylonitritrile-styrene resin is dissolved in the pimelinketone, adds antistatic agent, increase crisp dose;
(9) to capsule bulbus cordis grain spraying supporting layer.
CNB200410097105XA 2004-12-09 2004-12-09 Microcapsule degelling agent and its preparation method Expired - Fee Related CN1325598C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB200410097105XA CN1325598C (en) 2004-12-09 2004-12-09 Microcapsule degelling agent and its preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB200410097105XA CN1325598C (en) 2004-12-09 2004-12-09 Microcapsule degelling agent and its preparation method

Publications (2)

Publication Number Publication Date
CN1786101A CN1786101A (en) 2006-06-14
CN1325598C true CN1325598C (en) 2007-07-11

Family

ID=36783715

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB200410097105XA Expired - Fee Related CN1325598C (en) 2004-12-09 2004-12-09 Microcapsule degelling agent and its preparation method

Country Status (1)

Country Link
CN (1) CN1325598C (en)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101781552B (en) * 2009-12-21 2012-11-07 陕西延长石油(集团)有限责任公司研究院 Bio-enzyme gel breaker and technique for water-based guargum fracturing gel breaking with the same
CN102533244B (en) * 2010-12-27 2013-10-16 中国石油天然气股份有限公司 Encapsulated sustained-release acid for oil-water well reconstruction and preparation method thereof
CN103114833B (en) * 2011-11-17 2015-06-24 中国石油化工股份有限公司 Microbe oil extraction method for activating oil deposit deep portion function flora
CN102536178B (en) * 2011-12-27 2014-12-24 中国石油天然气股份有限公司 Method for prolonging augmented injection measure period of water injection well scaling easily
CN102627959B (en) * 2012-03-26 2013-10-09 中国石油化工股份有限公司 Gel breaker microcapsule controlled to release concentratedly in 2-3 h and preparation method thereof
CN102627958B (en) * 2012-03-26 2013-10-09 中国石油化工股份有限公司 Efficient microcapsule gel breaker and preparation method thereof
US10000681B2 (en) 2012-12-21 2018-06-19 Halliburton Energy Services, Inc. Hollow hydrogel capsules and methods of using the same
CN105860952B (en) * 2016-03-26 2018-10-23 北京化工大学 A kind of processing method of gel breaker
CN106223923B (en) * 2016-10-17 2019-03-19 平安煤炭开采工程技术研究院有限责任公司 Coal bed fracturing method
CN106566517A (en) * 2016-10-21 2017-04-19 长江大学 Low temperature gel breaking viscosity reducer of crosslinked guar gum backflow fracturing fluid, and preparation method thereof
CN106351607A (en) * 2016-11-17 2017-01-25 烟台智本知识产权运营管理有限公司 Water shut-off and profile control method for oil-water well
CN106522880A (en) * 2016-11-17 2017-03-22 烟台智本知识产权运营管理有限公司 Controllable temporary plugging method applied during water plugging and profile control conducted through gel plugging agent
CN108822816A (en) * 2018-06-25 2018-11-16 中国石油集团渤海钻探工程有限公司 A kind of molten GEL USED FOR PLUGGING WELL LOST CIRCULATION of loose sand theobromine and preparation method thereof
CN109319913B (en) * 2018-10-11 2022-07-01 仲恺农业工程学院 Slow-release potassium hydrogen persulfate preparation and preparation method thereof
CN116426262A (en) * 2022-01-04 2023-07-14 中国石油天然气股份有限公司 Delayed gel breaker with double-shell structure and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1303463A (en) * 1998-05-29 2001-07-11 3M创新有限公司 Encapsulated breaker slurry compositions and methods of use

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1303463A (en) * 1998-05-29 2001-07-11 3M创新有限公司 Encapsulated breaker slurry compositions and methods of use

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
石油钻采工艺 刘建权,55页1.2节,中温胶囊过破胶技术 2004 *

Also Published As

Publication number Publication date
CN1786101A (en) 2006-06-14

Similar Documents

Publication Publication Date Title
CN1325598C (en) Microcapsule degelling agent and its preparation method
US20200115609A1 (en) Controlled break enzyme formulations
CN102690645B (en) Sustained-release gel-breaking type fracturing propping agent and preparation method thereof
US8273426B1 (en) Encapsulated compositions
CN104003807B (en) A kind of double wrapped water-retaining type sustained release pesticide granules preparation and preparation method
CN102108293A (en) Preparation method of slow-release rubber breaking agent for chemical temporary-plugging rubber plug
GB2199872A (en) Method for treating subterranean formations
EA006323B1 (en) Method of obtaining capsules with a bulk-powder substance for treating subterranean formation
WO2008001591A1 (en) Nucleus particle for layering and method for producing the same
CN102423299B (en) Preparation method for drug-loaded chitosan nano-microspheres
CN101712578A (en) Method for releasing actual effect of fertilizer, actual effect releasing type controlled release fertilizer and preparation method
CN107573920A (en) A kind of biology enzyme capsule breaker and preparation method thereof
CN106431069A (en) Slowly released type anti-rust microcapsules applied to steel reinforced concrete and preparation method thereof
CN105484697B (en) A kind of profile control envelope of super-heavy oil deposit alters method
CN109575906B (en) Resin film coated polymer composite proppant particles and preparation method and application thereof
CN110540228A (en) modification method of nano zinc oxide
CN1071591C (en) Tri-layer sphere type capsule breaker and preparing method thereof
CN111019396A (en) Preparation method of modified heavy calcium carbonate for PVC foamed sheet hard plastic product and modified heavy calcium carbonate
CN103160270A (en) Encapsulated gel breaker for hydraulic fracturing of coalbed methane well, as well as preparation and using methods thereof
CN112191199B (en) Microcapsule for embedding liquid grease and preparation method thereof
Chang et al. Application and prospect of self-healing microcapsules in surface coating of wood
JP2629013B2 (en) Granulation method for powder etc.
CN105623281A (en) Preparation method for asphalt composition particles with high softening points
CN112980416B (en) Composite nano-coated oil displacement agent particles and preparation method thereof
CN115948155B (en) Preparation process and application of viscosity-reducing oil displacement agent for petroleum exploitation

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20070711