CN1071591C - Tri-layer sphere type capsule breaker and preparing method thereof - Google Patents

Tri-layer sphere type capsule breaker and preparing method thereof Download PDF

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Publication number
CN1071591C
CN1071591C CN95107276A CN95107276A CN1071591C CN 1071591 C CN1071591 C CN 1071591C CN 95107276 A CN95107276 A CN 95107276A CN 95107276 A CN95107276 A CN 95107276A CN 1071591 C CN1071591 C CN 1071591C
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China
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capsule
breaker
tri
gel breaker
sphere type
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Expired - Fee Related
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CN95107276A
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CN1140101A (en
Inventor
谢建利
张惠蓉
宋运维
张玉田
艾孜木江
胡秀珍
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OIL-FIELD TECHNOLOGY INST XINJIANG PETROLEUM ADMINISTRATIVE BUREAU
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OIL-FIELD TECHNOLOGY INST XINJIANG PETROLEUM ADMINISTRATIVE BUREAU
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Priority to CN95107276A priority Critical patent/CN1071591C/en
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Abstract

The present invention provides a gel breaker for fracturing fluid, which is used for the fracturing construction operation of oil-gas fields, and a preparation method thereof. The gel breaker is used for bonding and wrapping a three-layer structure of a capsule core, a capsule screen and a capsule skin together by a physical method to form a three-layer spherical gel breaker for a capsule, wherein the main components of the capsule core and the capsule screen are gel breaker bodies, and the main component of the capsule skin is a water-proofing material with favorable mechanical and physical properties. The gel breaker has the functions of the delayed release and the high-concentration integral release of the gel breaker, can efficiently control the degrading time of gel fracturing fluid and can reduce the damage of the fracturing fluid to an oil layer.

Description

Tri-layer sphere type capsule breaker and preparation method thereof
The present invention relates to capsule breaker of the broken glue technical field of oil-gas field fracturing liquid and preparation method thereof.
At present, during the oil field compression fracture operation, the normal gel breaker that uses water miscible strong oxidizer persulfate as fracturing fluid gel, this exposed persulfate gel breaker is directly with after the mixing of water base (or emulsification) fracturing fluid gel contacts, cause fracturing fluid gel to lose viscosity too early, weaken prop-carrying capacity, make oil reservoir be subjected to external entry well fluid serious penetrate injury; Otherwise, if reduce the gel breaker consumption, then can cause a large amount of enrichments on the fracture guide bed of polymer fracturing fluid, thereby oil reservoir is caused fracturing fluid residue and is detained the body injury, oil well returns row's difficulty.In order fundamentally to solve the problem that the filtrate of causing owing to fracturing fluid penetrates and residual body injures oil reservoir, abroad all attempt development and use a kind of capsule breaker that can control the fracturing fluid depolymerization with domestic.Go up " the of the fracturing fluid capsule breaker of aqueous-based polymers " literary composition of publication as " Oil-Gas Field Development Engineering collected translation " (1991 the 10th phases), a kind of capsule breaker at the surface of persulfate parcel one deck waterproof foreskin is disclosed, this gel breaker product is divided into two-layer, the capsule heart is ammonium persulfate crystalline solid or discrete particles (referring to brief summary crystal adhesion group), the water proof covering is water base polyvinylidene chloride copolymer (PVCD-CP), is the preparation of fluid bed multichannel foreskin method by " wruster " method.In addition, disclosed patent application " double-layer microcapsule gum-breaking agent of water base polymer fracturing fluid " (number of patent application: 93117052.4) provide a kind of gel breaker, its product structure and above-mentioned gel breaker are similar, adopt the production technology preparation with two-phase dispersion and the whole rolling of particle and self rolling effect.This product capsule heart is ammonium persulfate crystalline solid (or discrete particles), and water barrier is slow release layer (vinyl chloride one vinylidene chloride copolymer PVDC-CO) and fixed point releasing layer (solid paraffin).Their weak point is: 1, the capsule core material particle surface of Shi Yonging is uneven, its outer surface is random multi-angular crystalline solid or is honeycomb particulate, be difficult to form the spheroid of certain sphericity behind the dressing, mostly be electuary formula substandard products, as if " slowly-releasing " effect of wanting to reach certain, water proof covering weight accounts for 30%-40% (referring to U.S. HALLIBURTON product) of capsule product weight, so covering liquid consumption is more, and cladding thickness is thicker.2,, place for a long time the very easily moisture absorption, adhesion, a group, so processing is granulated and the meeting of operation by stages of dressing influences coating quality because ammonium persulfate is the extremely strong strong oxidizer of respond.3, above-mentioned " double-layer microcapsule gel breaker " mainly relies on the slow release layer material to delay to discharge ammonium persulfate, finishes brokenly glue, and this method gel breaker rate of release is slower, and can not wholely discharge, and therefore broken glue is not thorough.
The purpose of this invention is to provide a kind of by water proofing property, temperature tolerance, slowly the oil-soluble material capsuleization and have that cementing strength is good, sphericity and surface flatness height, the tri-layer sphere type capsule breaker of release and preparation method thereof of fixing a point.
The invention provides a kind of like this gel breaker: the crystalline particle of gel breaker main body is examined as the capsule of this gel breaker, gel breaker main body powder and additive are bonded in capsule nuclear outer surface, form the capsule curtain, coating material and additive are wrapped in capsule curtain outer surface jointly and form the capsule skin, and the prescription of its weight % is:
Gel breaker main body 80%
Coating material 15-18%
Additive 2-5%
Wherein be respectively 0.20~0.80mm (containing 0.80mm) and 0.10-0.05mm as the capsule crystalline nucleation particle of gel breaker main body and the particle diameter of capsule curtain powder.Material is fracturing fluid gel breakers such as persulfate, biology cellulose enzyme, sodium carbonate, anhydrous sodium acetate;
Coating material is the inclined to one side copolymer emulsion of chloro-(adding 30-60g cement), ethyl cellulose solution or polyacrylic resin;
Additive is: binding agent, dispersant, increase crisp dose, temperature stability agent.Binding agent is the inclined to one side copolymer emulsion of chloro-or ethyl cellulose solution, poly-cloudy particle cellulose solution, polyacrylic resin, gelatin etc.Dispersant is dolomol or talcum powder.Increase crisp dose and be dolomol or cement.Temperature stability agent is a sodium thiosulfate.
Its step of preparation process is as follows:
(1), the gel breaker capsule nuclear through the 0.2-0.8mm that screen analysis forms of getting some is poured in the pot (3) of granulating;
(2), in granulation liquid reservoir (1), add a certain amount of binding agent;
(3), uniform rotation granulation pot (3), binding agent is sprayed continuously on capsule grain surface, and off-the-shelf gel breaker capsule curtain powder (0.1-0.05mm) through pulverizing is sprinkling upon capsule grain surface continuously uniformly, add temperature stability agent simultaneously, increase additives such as crisp dose, particle dispersants;
(4), dressing machine upper shell (20) is put in the granulation of the 0.45-0.9mm (or 0.9mm-1.25mm) that step (3) is drawn;
(5), be in the ratio adding dressing reservoir (30) of 45ml/100g in capsule skin amount/granulation amount with capsule skin liquid;
(6), at the uniform velocity rotate the dressing machine, the hot-air pre-heating coated granule, the while with the granulation surface of capsule skin liquid spraying in upper shell (20), adds a certain amount of dispersant by spray gun (18) before taking the dish out of the pot, promptly get the tri-layer sphere capsule breaker.
Wherein the bleed pressure scope of using in the step (3) is 0.35-0.7MPa; The pot rotating speed of granulating is controlled at 48-54 rev/min, and the pot axis and the horizontal plane elevation angle are 15 °-45 °; The whitewashing flow-control was at 30-80ml/min when binding agent sprayed, and whiff pressure is in the 0.08-0.12MPa scope;
Dressing machine rotational speed regulation is in 120-160 rev/min scope in the step (6); Hot blast temperature is controlled at 50 ℃-65 ℃, and air blast flux is 400l/min, and the coated granule temperature is 30 ℃-40 ℃.The capsule skin sprays flow at 25-40ml/min, and whiff pressure is controlled at 0.1-0.2MPa, and jet flow is 15-20l/min.
Advantage of the present invention is: 1, at capsule nuclear outer wrapping one deck superfines layer capsule curtain, can reach by changing capsule curtain THICKNESS CONTROL capsule size size, original random capsule crystalline nucleation body (or discrete particles) multi-angular and shape such as cellular surface is wrapped up in circle and fill and lead up, form sphericity height, ganoid spheric granules, thereby simplified art for coating, reduce cladding thickness, improved broken colloidality energy; 2, the outer capsule cortex of capsule curtain has: water-resisting property, temperature tolerance and slow oil-soluble characteristics, in addition this layer have also that filming performance is good, strong adhesion, with by bag thing generation chemical reaction, moisture-resistant, heat resistanceheat resistant (being applicable to 40 ℃ of-80 ℃ of reservoir temperatures), acid and alkali-resistance character such as (pH=2-3), the capsule machinery function admirable behind the parcel; 3, this gel breaker relies on crack closure stress to trigger capsule covering distortion or broken, has to delay to discharge and the whole releasing effect of high concentration, can effectively control aqueous-based polymers fracturing fluid degradation time, alleviates formation damage; 4, two or more gel breaker main body mixing granulations can be had " two-in-one or multiple unification " function.5, the binding agent and the capsule leather material of the present invention's employing can be dissolved by oil in 4-8 hour voluntarily fully, can not cause the secondary injury to the stratum.
Accompanying drawing is preparation method's process chart of the present invention.
Embodiment:
(1), the 0.2-0.45mm ammonium persulfate capsule nuclear that 10Kg is become through screen analysis is poured in the pot (3) of granulating;
(2), in granulation liquid reservoir (1), add the 2022ml binding agent;
(3), prepare the ultra-fine ammonium persulfate powder of the 0.05-0.1mm 16Kg crush capsule curtain charges as rolling capsule nuclear surface;
(4), connect air compressor (9), bleed pressure table (8) is controlled between the 0.4-0.7MPa;
(5), start the pot motor (11) of granulating, the pot rotating speed of granulating is adjusted at 50 rev/mins, 30 ° at the pot axis and the horizontal plane elevation angle;
(6), open the gas control switch of spray gun (2), jet switch, whitewashing switch, regulate whiff pressure table (4) indication 0.09MPa with pressure-reducing valve (5), the whitewashing flow-control is at about 75ml/ branch by the correspondence position of six-way valve (6);
(7), capsule nuclear does the vortex gyration in the pot of granulating, by spray gun (2) binding agent is sprayed on capsule nuclear surface, sprays ultra-fine ammonium persulfate powder simultaneously continuously equably, has the spherolite of capsule nuclear, capsule curtain double-layer structure until formation;
(8), the spherolite of making is carried out polishing, add particle dispersants (or temperature stability agent) 0.28Kg then, prevent inter-adhesive group between particle;
(9), the granulation 2.5Kg that gets above-mentioned 0.45-0.90mm (or 0.90-1.25mm) puts in the dressing machine upper shell (20);
(10), connect dressing machine motor (29), driving main frame rotating disk (21) rotates, its rotational speed regulation is at 160 rev/mins, utilize dust, moisture in dust catcher (19) the absorption dressing machine upper shell, blow rate required control valve (25) control flowmeter (24) indication of air blast (26) is at 400l/min, make the temperature of air blast preheating reach 59 ℃ through electric heater (31), material dressing temperature is 36 ℃;
(11), press the granulate proportioning of product adding 450ml capsule skin liquid measure of 1Kg ammonium persulfate then and in dressing liquid reservoir (30), add capsule skin liquid measure 1125ml;
(12), connect spray pump (23), jet magnetic valve (14) and whitewashing magnetic valve (10) in order successively, regulate pressure-reducing valve (16) and make whiff pressure table (15) indication 0.1MPa, adjust choke valve (13) and make jet flowmeter (12) indication at 20ml/min, the whitewashing flow is 30ml/min;
(13), spray gun (18) ejects atomizing shape coating solution and makes particle surface parcel one deck capsule leather material;
(14), need to add 60g dolomol dispersant (or temperature stability agent) before taking the dish out of the pot, carry out the polishing of 4min then;
(15), the coated granule after will taking the dish out of the pot dries, and selects the 0.45-0.90mm particle, can obtain meeting the tri-layer sphere type capsule breaker product that fracturing fluid is used.
Can carry out similar processing with gel breaker to fracturing fluids such as potassium peroxydisulfate, biology cellulose enzyme, sodium carbonate, anhydrous sodium acetates according to said method.

Claims (9)

1. tri-layer sphere type capsule breaker, it is characterized in that the capsule nuclear of the crystalline particle of gel breaker main body as this gel breaker, gel breaker main body powder and additive are bonded in capsule nuclear outside, form the capsule curtain, coating material and additive are wrapped in capsule curtain outer surface jointly and form the capsule skin, and the prescription of its weight % is:
Gel breaker main body 80%;
Coating material 15-18%;
Additive 2-5%;
Gel breaker main body crystallization grain diameter is 0.20-0.80mm, and gel breaker main body powder diameter is 0.1-0.05mm.
2. tri-layer sphere type capsule breaker as claimed in claim 1 is characterized in that described gel breaker main body is persulfate, biology cellulose enzyme, sodium carbonate or anhydrous sodium acetate.
3. tri-layer sphere type capsule breaker as claimed in claim 1 is characterized in that described coating material is for adding the inclined to one side copolymer emulsion of chloro-, ethyl cellulose filtrate or the polyacrylic resin of 30-60g cement.
4. tri-layer sphere type capsule breaker as claimed in claim 1 is characterized in that described additive is binding agent, dispersant, increases crisp dose, temperature stability agent.
5. tri-layer sphere type capsule breaker as claimed in claim 4 is characterized in that described binding agent is the inclined to one side copolymer emulsion of chloro-, ethyl cellulose filtrate, poly-cloudy particle cellulose solution, polyacrylic resin or gelatin.
6. tri-layer sphere type capsule breaker as claimed in claim 4 is characterized in that described dispersant is dolomol or talcum powder.
7. tri-layer sphere type capsule breaker as claimed in claim 4 is characterized in that describedly increasing crisp dose for dolomol or cement.
8. tri-layer sphere type capsule breaker as claimed in claim 4 is characterized in that described temperature stability agent is a sodium thiosulfate.
9. the preparation method of tri-layer sphere type capsule breaker, its feature comprises the steps: successively
(1), the gel breaker capsule nuclear through the 0.20-0.80mm that screen analysis forms of getting some is poured in the pot of granulating;
(2), in granulation liquid reservoir (1), add a certain amount of binding agent;
(3), uniform rotation granulation pot (3), binding agent is sprayed continuously on capsule grain surface, and with off-the-shelf be that the gel breaker powder of 0.10-0.05mm is sprinkling upon capsule grain surface continuously uniformly through powder particle diameter, add temperature stability agent simultaneously, increase crisp dose, these additives of particle dispersants;
(4) dressing machine upper shell (20) is put in the granulation of 0.45-0.90mm that step (3) is drawn or 0.90-1.25mm;
(5), be in the ratio adding dressing reservoir (30) of 45ml/100g in capsule skin amount/granulation amount with capsule skin liquid;
(6), at the uniform velocity rotate the dressing machine, the hot-air pre-heating coated granule, the while with the granulation surface of capsule skin liquid spraying in upper shell (20), adds a certain amount of dispersant by spray gun (18) before taking the dish out of the pot, promptly get tri-layer sphere type capsule breaker;
Wherein, the bleed pressure scope of using in the step (3) is 0.35-0.7Mpa; The pot rotating speed of granulating is controlled at 48-54 rev/min, and the pot axis and the horizontal plane elevation angle are 15-45 °; The whitewashing flow-control was at 30-80ml/min when binding agent sprayed, and whiff pressure is in the 0.08-0.12Mpa scope;
Dressing machine rotational speed regulation is in 120-160 rev/min scope in the step (6); Hot blast temperature is controlled at 50-65 ℃, and air blast flux is 400l/min, and the coated granule temperature is 30-40 ℃; The capsule skin sprays flow at 25-40ml/min, and whiff pressure is controlled at 0.1-0.2Mpa, and jet flow is 15-20l/min.
CN95107276A 1995-07-12 1995-07-12 Tri-layer sphere type capsule breaker and preparing method thereof Expired - Fee Related CN1071591C (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
CN95107276A CN1071591C (en) 1995-07-12 1995-07-12 Tri-layer sphere type capsule breaker and preparing method thereof

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CN1071591C true CN1071591C (en) 2001-09-26

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Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6840318B2 (en) * 2002-06-20 2005-01-11 Schlumberger Technology Corporation Method for treating subterranean formation
CN105647504A (en) * 2016-01-25 2016-06-08 西南石油大学 Microcapsule gel breaker and preparation method thereof
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
CN107573920A (en) * 2017-10-18 2018-01-12 中国石油化工股份有限公司 A kind of biology enzyme capsule breaker and preparation method thereof
CN108102622B (en) * 2017-11-23 2020-10-23 中国石油大学(华东) Shielding temporary plugging protective agent 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
CN110776879A (en) * 2019-11-04 2020-02-11 新疆大德广源石油技术服务有限公司 Strong-inhibition bunching environment-friendly drilling and completion fluid

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN88100379A (en) * 1987-01-16 1988-11-02 陶氏化学公司 Handle the method on stratum
EP0379236A1 (en) * 1989-01-17 1990-07-25 Sofitech N.V. Method for treating subterranean formations
CN1099786A (en) * 1993-09-01 1995-03-08 朱海峰 Double-layer microcapsule gum-breaking agent of water base polymer fracturing fluid

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN88100379A (en) * 1987-01-16 1988-11-02 陶氏化学公司 Handle the method on stratum
EP0379236A1 (en) * 1989-01-17 1990-07-25 Sofitech N.V. Method for treating subterranean formations
CN1099786A (en) * 1993-09-01 1995-03-08 朱海峰 Double-layer microcapsule gum-breaking agent of water base polymer fracturing fluid

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