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CN109679601A - Temporary plugging agent and preparation method and application thereof - Google Patents

Temporary plugging agent and preparation method and application thereof Download PDF

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Publication number
CN109679601A
CN109679601A CN201710976362.8A CN201710976362A CN109679601A CN 109679601 A CN109679601 A CN 109679601A CN 201710976362 A CN201710976362 A CN 201710976362A CN 109679601 A CN109679601 A CN 109679601A
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China
Prior art keywords
diverting agent
terpene resin
stearic acid
diverting
clay stabilizer
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CN201710976362.8A
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Inventor
刘建伟
张佩玉
舒福昌
刘海廷
邓强
廖天彬
袁玉梅
刘剑辉
何海波
陈文彬
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Petrochina Co Ltd
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Petrochina Co Ltd
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Priority to CN201710976362.8A priority Critical patent/CN109679601A/en
Publication of CN109679601A publication Critical patent/CN109679601A/en
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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
    • C09K8/50Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
    • C09K8/504Compositions based on water or polar solvents
    • C09K8/506Compositions based on water or polar solvents containing organic compounds
    • C09K8/508Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/5083Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • 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
    • C09K8/84Compositions based on water or polar solvents
    • C09K8/86Compositions based on water or polar solvents containing organic compounds
    • C09K8/88Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/882Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • EFIXED CONSTRUCTIONS
    • E21EARTH OR ROCK DRILLING; MINING
    • E21BEARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B33/00Sealing or packing boreholes or wells
    • E21B33/10Sealing or packing boreholes or wells in the borehole
    • E21B33/13Methods or devices for cementing, for plugging holes, crevices or the like

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geology (AREA)
  • Mining & Mineral Resources (AREA)
  • Physics & Mathematics (AREA)
  • Environmental & Geological Engineering (AREA)
  • Fluid Mechanics (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention provides a temporary plugging agent and a preparation method and application thereof, wherein the temporary plugging agent comprises the following components in percentage by weight: 34% of inorganic salt, 52-65% of terpene resin, 0-13% of stearic acid and 1% of clay stabilizer. The temporary plugging agent is suitable for medium and low temperature reservoirs, has good plugging effect, high permeability recovery rate, good solubility and small damage to the stratum, and is a diversion repeated fracturing temporary plugging agent with good effect.

Description

A kind of diverting agent and its preparation method and application
Technical field
The present invention relates to a kind of diverting agents and its preparation method and application, belong to petroleum industry chemicals technical field.
Background technique
The extensive successful application that hydraulic fracturing has worldwide been obtained as the well stimulation that low permeability reservoirs are transformed, But the crude oil in the draining area controlled with the development and production of fractured well (layer), the hydraulic fracture generated for the first time has produced journey Degree is very high, but a large amount of remaining oil producing degree outside draining area are lower.Therefore, if it is simple normal by primary fracture progress is extended Rule refracturing not necessarily has considerable fuel-displaced effect.
Turning to multiple fracturing technique is the new technique to grow up the nineties in last century, it overcomes conventional repetition to press Old crack can only be opened again by, which splitting, restores old seam flow conductivity with part.Artificial temporarily stall to multiple fracturing technique be in pressure break mistake Diverting agent is added in journey in real time, temporarily to block up old seam or sand has been added to stitch, fluid is made by the variation of fracture pressure, fracture propagation pressure It turns to, to produce new seam.It is this to be stitched by using diverting agent blocking primary fissure, make refracturing seam relative to primary fracture Orientation occurs to deviate, turn to, and the reservoir that development degree is low or even does not employ is transformed, refracturing oil increasing effect not only can be improved, Water drive direction can also be changed to a certain extent, improve injection water use efficiency.
But turn to refracturing diverting agent with claimed below: stronger temporarily stifled ability, resume permeability rate is high, to stratum It injures smaller.The turnaround fracture diverting agent of colleague's research and development early period both at home and abroad, the universal higher reservoir of Applicable temperature, but not Suitable for middle low temperature reservoir, reason is that the diverting agent suitable for temperature reservoirs is used to have crack to low temperature reservoir and blocks Afterwards, it is difficult to dissolve de-plugging, therefore recovery rate is extremely low.And existing diverting agent mostly uses the materials such as acrylamide, polyacrylamide, Oil-soluble is poor, big to formation damage.
Summary of the invention
In view of the foregoing drawbacks, the present invention provides a kind of diverting agent and its preparation method and application, during which is suitable for Low temperature reservoir, plugging effect is good, and resume permeability rate is high, and dissolubility is good, small to formation damage, is a kind of with good result Steering refracturing diverting agent.
The present invention provides a kind of diverting agent, includes following component according to weight percentage: inorganic salts 34%, terpene resin 52-65%, stearic acid 0-13%, clay stabilizer 1%.
The above-mentioned each component of diverting agent of the present invention is common commercially available, wherein stearic acid and inorganic salts use industrial goods , the dosage of clay stabilizer is less compared to other components, is mainly used for good ground particle, prevents clay movement.
Stearic acid is also known as octadecanoid acid, molecular formula C18H36O2, structural formula is as shown in Equation 1:
Stearic acid is a kind of saturated fatty acid, and sterling is with the soft small pieces of glossiness white, and fusing point is 69.6 DEG C, boiling Point is 376.1 DEG C, and relative density is 0.9408 (20/4 DEG C), and refractive index is nD (80 DEG C) 1.4299.Stearic acid is to constitute dynamic, plant A kind of main component of object grease.Its poorly water-soluble only dissolves 0.00029g stearic acid at 20 DEG C in 100 milliliters of water, slightly molten In cold ethyl alcohol, it is dissolved in acetone, benzene, ether, chloroform, carbon tetrachloride, sulfur dioxide, chloroform, hot ethanol, toluene, acetic acid penta Ester etc..It can be used for the products such as pharmaceutical preparation, ointment, soap and suppository, also be used as the raw material and daily chemical product of auxiliary agent Raw material.
Diverting agent composition provided by the invention is simple, does not generate layering and precipitating, in stable condition.The density of the diverting agent is 1-1.13g/cm3, in preparing fracturing fluid, diverting agent particle is not floated in aqueous solution, is not precipitated, and can be dispersed in In water, it will not bond agglomerating.And the diverting agent is thermoplastic, itself has certain hardness and strength, but temporarily Blocking agent is after heated stress, it may occur that deformation, and have adhesion property, to be conducive to the closure in crack.
The diverting agent has preferable plugging effect to Reservoir Fracture not only to the temporary stifled rate of rock core 97.5% or more, And having good dissolubility again in oil, water mixed solution, after fracture blocks, under effect of splitting, oleic permeability restores Value easier can be dissolved or be discharged by oil stream, so that oleic permeability is gradually restored, reach and voluntarily solve up to 86.2% or more Stifled, protection oil-gas Layer purpose.
Further, the terpene resin is selected from terpene resin T-80 or terpene resin T-100.Terpene resin T-80 or terpene Olefine resin T-100 is specifically the difference of softening point, wherein the softening point of terpene resin T-80 is 80 ± 5 DEG C, terpene resin T100 Softening point be 100 ± 5 DEG C.
Specifically, the molecular formula of terpene resin T-80 is (C10H16) n, 8 > n > 4, structural formula is as shown in Equation 2:
Terpene resin T-80 is a kind of yellow transparent, and brittle solid thermoplastics, softening point is 80 ± 5 DEG C, average mark Son amount is 650-1000.It is a kind of excellent tackifier, and there is nontoxic, odorless, radiation hardness, Yao the performances such as to crystallize, to oxygen, Heat, light are more stable;There is good intermiscibility to various synthetics;Resistance to diluted acid, diluted alkaline;Tackifying is strong, and electrical insulating property is strong, readily soluble In organic solvents such as benzene, toluene, turpentine oil.Not soluble in water, methanol, ethyl alcohol etc..
The molecular formula of terpene resin T100 is (C10H16) n, 10 > n > 6, structural formula is as shown in Equation 3:
Structural formula:
Terpene resin T-100 is a kind of yellow transparent, brittle solid thermoplastics.Its softening point is 100 ± 5 DEG C, average Molecular weight is 850-1250.It is a kind of excellent tackifier, and there is nontoxic, odorless, radiation hardness, Yao the performances such as to crystallize, to oxygen, Heat, light are more stable;There is good intermiscibility to various synthetics;Resistance to diluted acid, diluted alkaline;Tackifying is strong, and electrical insulating property is strong, readily soluble In organic solvents such as benzene, toluene, turpentine oil.Not soluble in water, methanol, ethyl alcohol etc..
Above two terpene resin is all widely used in adhesive, solid, double faced adhesive tape, solvent type glue, books dress Order version, color dress, adhesive plaster, alkene adhesive plaster, brown paper stuck glue cloth, tapes labels, carpenter's glue, pressure sensitive adhesive, thermosol, sealant, oil Paint and ink and other polymer modification agents etc..
Diverting agent of the invention is suitable for middle low temperature environment, and signified middle low temperature environment specifically refers to 45-80 DEG C herein, is Further enhance the temporary stifled ability of the diverting agent, the present invention is in this in low temperature range, for different specific stratum temperature T is spent, also there is preferred diverting agent composition, for example, above-mentioned temperature range is mainly divided into three sections, section 1 are as follows: 45 DEG C≤ T≤60℃;Section 2 are as follows: 60 DEG C≤T≤70 DEG C;Section 3 are as follows: 70 DEG C≤T≤80 DEG C, when specific formation temperature it is above-mentioned certain In one interval range, temporarily stifled operation can be implemented using more targeted diverting agent.Specific each temperature range range Corresponding diverting agent is as follows:
When processing temperature is in section 1, i.e. when 45 DEG C≤T≤60 DEG C, diverting agent includes as follows according to weight percentage Component: inorganic salts 34%, terpene resin T-80 52-57%, stearic acid 8-13%, clay stabilizer 1%.
When processing temperature is in section 2, i.e. when 60 DEG C≤T≤70 DEG C, diverting agent includes as follows according to weight percentage Component: inorganic salts 34%, terpene resin T-100 52-57%, stearic acid 8-13%, clay stabilizer 1%.
When processing temperature is in section 3, i.e. when 70 DEG C≤T≤80 DEG C, diverting agent includes as follows according to weight percentage Component: inorganic salts 34%, terpene resin T-100 57-65%, stearic acid 0-8%, clay stabilizer 1%.
Above three forms the difference for being mainly concerned with terpene resin type, the difference of content and stearic acid content.? Within the scope of Applicable temperature, when Applicable temperature increases, the amount of terpene resin is increase accordingly in using concentration range, and stearic Amount is corresponding to be reduced;Conversely, the amount of terpene resin is accordingly reduced in using concentration range, and stearic acid when Applicable temperature reduces Amount increase accordingly.Wherein, terpene resin T-80 is more suitable for lower formation temperature compared to terpene resin T-100;And terpene Olefine resin is more suitable for higher formation temperature compared to stearic acid, i.e., when formation temperature is lower, terpene resin selection is lower Percentage composition, stearic acid selects higher percentage composition, and when formation temperature is higher, terpene resin selects higher percentage composition, Stearic acid selects lower percentage composition.
For example, being applicable in, formation temperature is lower when being 45 DEG C, and terpene resin (TX80) percentage is 52%, stearic percentage Than being 13%, be applicable in formation temperature it is 60 DEG C more a height of when, terpene resin (TX80) percentage is 57%, and stearic percentage is 8%.Specifically terpene resin and the adjustment of stearic ratio in certain temperature range, can select according to temperature.
Further, above-mentioned inorganic salts are sodium chloride.
Further, above-mentioned clay stabilizer is a kind of inorganic salts soluble easily in water.
The present invention also provides a kind of preparation methods of any of the above-described diverting agent, include the following steps:
1) inorganic salts, terpene resin, stearic acid and clay stabilizer are mixed, mixture is generated;
2) mixture is heated to 110-120 DEG C, after stirring lower reaction 1-2h, is granulated, it is dry, it generates described temporarily stifled Agent.
In step 1), according to above-mentioned composition by inorganic salts, terpene resin, stearic acid and clay stabilizer in a kettle Mixing generates mixture.Preparation method provided by the present invention, inorganic salts, terpene resin, stearic acid and clay stabilizer Addition sequence can be it is any, each addition sequence does not have significant adverse influence to temporarily stifled effect obtained.
After generating mixture, the temperature of reaction kettle is risen to 110-120 DEG C and starts to be stirred to react, during the reaction, mixed Fusing can be gradually uniformly mixed and occur, deaerate by closing object, and after 1-2h, reaction terminates.Preparation method of the invention is by using suitable Suitable heating temperature, mixing speed and mixing time not only contributes to form stable diverting agent system, temporary in addition there are being conducive to Mobility of the blocking agent in fracturing fluid, thus it is more convenient to use, particularly suitable for temporary envelope crannied in reservoir It is stifled.Wherein, the revolving speed of stirring needs to control in 5-15r/min.In addition, range can be used in order to accurately control reaction temperature Temperature monitoring is carried out for 30-200 DEG C of thermometer.
Specifically when being granulated, it can be granulated using SE series Screw Extrusion, by the reactant wet feed after reaction in 80-115 It under conditions of DEG C, conveys to screw extruder pelletizer, under screw extruder pelletizer squeezing action, is squeezed out from head aperture template Molding materials.Prilling temperature specifically needs to be determined according to the type of terpene resin in diverting agent, when using terpene resin T-80, Prilling temperature is greater than 5-10 DEG C of softening point of terpene resin T-80;When using terpene resin T-100, prilling temperature is greater than terpene 5-10 DEG C of softening point of olefine resin T-100.
The molding materials of extrusion are using the finished granule for obtaining diverting agent after wind cold drying.The specifically particle of diverting agent The shape of finished product be it is cylindric, the diameter of columned cross section can have template open pore size regulation and control.
Have crack the present invention also provides a kind of pair of reservoir and carry out temporarily stifled method, by any of the above-described diverting agent with Fracturing fluid injects in the reservoir, wherein the diverting agent and the crannied mass volume ratio be (1:1)~(1: 1.2)。
Wherein, crannied volume is calculated according to formula 1:
V=h*a*b formula 1
V: crannied volume;
H: crannied height;
A: crannied slit width;
B: diverting agent simulates depth of invasion.
Diverting agent usability methods of the invention are also more simple, when needing fracture to carry out turnaround fracture, it is only necessary to will Diverting agent of the invention is added into fracturing fluid, and control diverting agent quality and crevice volume to be blocked be 1:1~1:1.2 ?.After the completion of configuration, the fracturing fluid containing diverting agent of the present invention is injected into reservoir by oil pipe.One times of tubing string is replaced to hold Long-pending fracturing fluid is observed temporarily stifled effect, is completed to crannied closure work.
Implementation of the invention, at least has the advantage that
1, diverting agent density of the invention is 1-1.13g/cm3, therefore in preparing fracturing fluid, diverting agent particle is water-soluble In liquid not float, do not precipitate, and can it is evenly dispersed in water, will not bond agglomerating;
2, diverting agent of the invention is thermoplastic, itself has certain hardness and strength, meanwhile, which exists It can deform after heated, after stress, and there is stronger adhesion property, be conducive to the closure in crack;
3, diverting agent of the invention there is preferable block to imitate Reservoir Fracture to the temporary stifled rate of rock core 96.9% or more Fruit;
4, diverting agent of the invention has good dissolubility in oil, water mixed solution, temporarily after stifled pressure break, with pressure break The row of returning of liquid and the exploitation of oil well, diverting agent can easier be dissolved by oil stream and can return to the greatest extent discharge stratum, make oil Phase permeability is gradually restored, and oleic permeability recovery value reaches the mesh of voluntarily de-plugging, protection oil-gas Layer up to 86.2% or more 's;
5, the diverting agent of the invention low temperature environment suitable for 45~80 DEG C, and can to above range section not It is synthermal that there is specific aim, 45~60 DEG C of temperature, 60~70 DEG C, 70~80 DEG C of reservoir can be respectively suitable for;
6, the preparation method of diverting agent of the invention is easy to operate, easily controllable, not only contributes to be formed stable temporary Blocking agent system, in addition there are be conducive to mobility of the diverting agent in fracturing fluid to be convenient in subsequent use process to crannied envelope It is stifled;
7, the temporary stifled effect of diverting agent of the invention when for temporarily blocking up to crack existing in reservoir is good, temporarily blocks up required equipment Simply, it not will cause secondary pollution, additionally conveyance conduit and equipment will not be caused to damage, to extend pipeline and equipment Service life.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this Technical solution in inventive embodiments is clearly and completely described, it is clear that described embodiment is that a part of the invention is real Example is applied, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creation Property labour under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
Raw material sources in the embodiment of the present invention are as described below:
Terpene resin T-80: Shandong Shouguang Hongyuan Chemical Co., Ltd.
Terpene resin T-100: Shandong Shouguang Hongyuan Chemical Co., Ltd.
Stearic acid (industrial goods): Guangzhou Guo Kaikai industrial chemicals Co., Ltd
Inorganic salts: (sodium chloride, industrial goods): Xi'an weber Li Yang chemical company
Clay stabilizer (003-A): TulufanHami oil field chemical company
Embodiment 1
Diverting agent in the present embodiment is suitable for the reservoir that temperature is 50 DEG C, includes such as the following group according to weight percentage Point:
1, inorganic salts (NaCl): 34%;
2, terpene resin T-80:53%;
3, stearic acid (octadecanoid acid): 12%;
4, clay stabilizer (003-A) 1%;
The sum of weight percentage of each component is 100%.
Method preparation can be prepared as follows in the diverting agent:
1) under stirring, above-mentioned raw materials are added according to aforementioned proportion in a kettle, produce mixture;
2) heating mixture after stirring lower reaction 1-2h, stops reaction to 110 DEG C (being measured with 30~200 DEG C of thermometers);
3) SE series screw extruder pelletizer is used, 2) reactant wet stock obtained in is being higher than terpene resin T-80 Under the conditions of the temperature that 5~10 DEG C of softening point, conveyed to screw extruder pelletizer, under screw extruder pelletizer squeezing action, from Head aperture template extrusion molding material.Using obtaining graininess diverting agent finished product after wind cold drying.
Temporarily stifled test is carried out using the embodiment diverting agent, wherein uses the multi-functional rock core flowing test of HAQT-2HKY type Instrument, test method are following (test temperature is 50 DEG C):
1, rock core is chosen: choosing two three oil field Tang Hu horses, 56 block P2T oil reservoir has intrinsic fracture, diameter 2.5cm The rock core of long 3cm, number 1#, 2#;
2, sieve after diverting agent crushes is prepared in this implementation takes the particle of 50~70 mesh spare (due to laboratory experiment equipment The diverting agent of condition bulky grain can not pass through the experiment manifold of minor diameter);
3, it is K that i.e. 1# core forward direction, which is passed through water flooding and measures water phase permeability,W1, 2# core forward direction is passed through aviation kerosine and measures Oleic permeability KO1
4, inverse injection contains the fracturing fluid for estimating 1.2 times of quality diverting agents of crevice volume, injection rate to 1#, 2# core respectively For 1PV, the water flooding for reversely replacing 1 times of experiment manifold volume of injection is then proceeded to;
5, after 1# core continues inverse injection water flooding until pressure flow is steady, temporarily stifled rear water phase permeability K is measuredW2, Temporarily stifled rate H is calculated according to formula 2:
H=(1-KW2)÷KW1× 100% formula 2
6, after 2# core forward direction injection aviation kerosine is until pressure flow is steady, temporarily stifled rear oleic permeability K is measuredO2, press Illuminated 3 calculates infiltration recovery rate G:
G=KO2÷KO1× 100% formula 3
Following testing result is obtained according to above-mentioned steps:
The core experiment of low temperature oil-soluble temporary plugging agent temporarily blocks up rate up to 97.7% in the present embodiment turnaround fracture use.Oil mutually returns Row, infiltration recovery rate are 87.4%.
Embodiment 2:
Diverting agent in the present embodiment is suitable for the reservoir that temperature is 60 DEG C, includes such as the following group according to weight percentage Point:
1, inorganic salts (NaCl): 34%;
2, terpene resin (T-80): 57%;
3, stearic acid (octadecanoid acid): 8%;
4, clay stabilizer (003-A) 1%;
The sum of weight percentage of each component is 100%.
Method preparation can be prepared as follows in the diverting agent:
1) under stirring, above-mentioned raw materials are added according to aforementioned proportion in a kettle, produce mixture;
2) heating mixture after stirring lower reaction 1-2h, stops reaction to 115 DEG C (being measured with 30~200 DEG C of thermometers);
3) SE series screw extruder pelletizer is used, 2) reactant wet stock obtained in is being higher than terpene resin T-80 Under the conditions of the temperature that 5~10 DEG C of softening point, conveyed to screw extruder pelletizer, under screw extruder pelletizer squeezing action, from Head aperture template extrusion molding material.Using obtaining graininess diverting agent finished product after wind cold drying.
Temporarily stifled test is carried out using the embodiment diverting agent, wherein uses the multi-functional rock core flowing test of HAQT-2HKY type Instrument, test method are following (test temperature is 60 DEG C):
1, rock core is chosen: choosing two three oil field Tang Hu horses, 56 block P2T oil reservoir has intrinsic fracture, diameter 2.5cm The rock core of long 3cm, number 1#, 2#;
2, sieve after diverting agent crushes is prepared in this implementation takes the particle of 50~70 mesh spare (due to laboratory experiment equipment The diverting agent of condition bulky grain can not pass through the experiment manifold of minor diameter);
3, it is K that i.e. 1# core forward direction, which is passed through water flooding and measures water phase permeability,W1, 2# core forward direction is passed through aviation kerosine and measures Oleic permeability KO1
4, inverse injection contains the fracturing fluid for estimating 1.2 times of quality diverting agents of crevice volume, injection rate to 1#, 2# core respectively For 1PV, the water flooding for reversely replacing 1 times of experiment manifold volume of injection is then proceeded to;
5, after 1# core continues inverse injection water flooding until pressure flow is steady, temporarily stifled rear water phase permeability K is measuredW2, Temporarily stifled rate H is calculated according to formula 2:
H=(1-KW2)÷KW1× 100% formula 2
6, after 2# core forward direction injection aviation kerosine is until pressure flow is steady, temporarily stifled rear oleic permeability K is measuredO2, press Illuminated 3 calculates infiltration recovery rate G:
G=KO2÷KO1× 100% formula 3
Following testing result is obtained according to above-mentioned steps:
The core experiment of low temperature oil-soluble temporary plugging agent temporarily blocks up rate up to 99.1% in the present embodiment turnaround fracture use.Oil mutually returns Row, infiltration recovery rate are 89.6%.
Embodiment 3:
Diverting agent in the present embodiment is suitable for the reservoir that temperature is 70 DEG C, includes such as the following group according to weight percentage Point:
1, inorganic salts (NaCl): 34%;
2, terpene resin T-100:57%;
3, stearic acid (octadecanoid acid): 8%;
4, clay stabilizer (003-A) 1%
The sum of weight percentage of each component is 100%.
Method preparation can be prepared as follows in the diverting agent:
1) under stirring, above-mentioned raw materials are added according to aforementioned proportion in a kettle, produce mixture;
2) heating mixture after stirring lower reaction 1-2h, stops reaction to 120 DEG C (being measured with 30~200 DEG C of thermometers);
3) SE series screw extruder pelletizer is used, 2) reactant wet stock obtained in is being higher than terpene resin T- Under the conditions of the temperature of 100 5~10 DEG C of softening points, conveyed to screw extruder pelletizer, under screw extruder pelletizer squeezing action, From head aperture template extrusion molding material.Using obtaining graininess diverting agent finished product after wind cold drying.
Temporarily stifled test is carried out using the embodiment diverting agent, wherein uses the multi-functional rock core flowing test of HAQT-2HKY type Instrument, test method are following (test temperature is 70 DEG C):
1, rock core is chosen: choosing two three oil field Tang Hu horses, 56 block P2T oil reservoir has intrinsic fracture, diameter 2.5cm The rock core of long 3cm, number 1#, 2#;
2, sieve after diverting agent crushes is prepared in this implementation takes the particle of 50~70 mesh spare (due to laboratory experiment equipment The diverting agent of condition bulky grain can not pass through the experiment manifold of minor diameter);
3, it is K that i.e. 1# core forward direction, which is passed through water flooding and measures water phase permeability,W1, 2# core forward direction is passed through aviation kerosine and measures Oleic permeability KO1
4, inverse injection contains the fracturing fluid for estimating 1.2 times of quality diverting agents of crevice volume, injection rate to 1#, 2# core respectively For 1PV, the water flooding for reversely replacing 1 times of experiment manifold volume of injection is then proceeded to;
5, after 1# core continues inverse injection water flooding until pressure flow is steady, temporarily stifled rear water phase permeability K is measuredW2, Temporarily stifled rate H is calculated according to formula 2:
H=(1-KW2)÷KW1× 100% formula 2
6, after 2# core forward direction injection aviation kerosine is until pressure flow is steady, temporarily stifled rear oleic permeability K is measuredO2, press Illuminated 3 calculates infiltration recovery rate G:
G=KO2÷KO1× 100% formula 3
Following testing result is obtained according to above-mentioned steps:
The core experiment of low temperature oil-soluble temporary plugging agent temporarily blocks up rate up to 97.5% in the present embodiment turnaround fracture use.Oil mutually returns Row, infiltration recovery rate are 90.4%.
Embodiment 4:
Diverting agent in the present embodiment is suitable for the reservoir that temperature is 80 DEG C, includes such as the following group according to weight percentage Point:
1, inorganic salts (NaCl): 34%;
2, terpene resin T-100:65%;
3, stearic acid (octadecanoid acid): 0%;
4, clay stabilizer (003-A) 1%
The sum of weight percentage of each component is 100%.
Method preparation can be prepared as follows in the diverting agent:
1) under stirring, above-mentioned raw materials are added according to aforementioned proportion in a kettle, produce mixture;
2) heating mixture after stirring lower reaction 1-2h, stops reaction to 110 DEG C (being measured with 30~200 DEG C of thermometers);
3) SE series screw extruder pelletizer is used, 2) reactant wet stock obtained in is being higher than terpene resin T- Under the conditions of the temperature of 100 5~10 DEG C of softening points, conveyed to screw extruder pelletizer, under screw extruder pelletizer squeezing action, From head aperture template extrusion molding material.Using obtaining graininess diverting agent finished product after wind cold drying.
Temporarily stifled test is carried out using the embodiment diverting agent, wherein uses the multi-functional rock core flowing test of HAQT-2HKY type Instrument, test method are following (test temperature is 80 DEG C):
1, rock core is chosen: choosing two three oil field Tang Hu horses, 56 block P2T oil reservoir has intrinsic fracture, diameter 2.5cm The rock core of long 3cm, number 1#, 2#;
2, sieve after diverting agent crushes is prepared in this implementation takes the particle of 50~70 mesh spare (due to laboratory experiment equipment The diverting agent of condition bulky grain can not pass through the experiment manifold of minor diameter);
3, it is K that i.e. 1# core forward direction, which is passed through water flooding and measures water phase permeability,W1, 2# core forward direction is passed through aviation kerosine and measures Oleic permeability KO1
4, inverse injection contains the fracturing fluid for estimating 1.2 times of quality diverting agents of crevice volume, injection rate to 1#, 2# core respectively For 1PV, the water flooding for reversely replacing 1 times of experiment manifold volume of injection is then proceeded to;
5, after 1# core continues inverse injection water flooding until pressure flow is steady, temporarily stifled rear water phase permeability K is measuredW2, Temporarily stifled rate H is calculated according to formula 2:
H=(1-KW2)÷KW1× 100% formula 2
6, after 2# core forward direction injection aviation kerosine is until pressure flow is steady, temporarily stifled rear oleic permeability K is measuredO2, press Illuminated 3 calculates infiltration recovery rate G:
G=KO2÷KO1× 100% formula 3
Following testing result is obtained according to above-mentioned steps:
The core experiment of low temperature oil-soluble temporary plugging agent temporarily blocks up rate up to 96.9% in the present embodiment turnaround fracture use.Oil mutually returns Row, infiltration recovery rate are 87.6%.
Embodiment 5:
Diverting agent in the present embodiment is suitable for the reservoir that temperature is 45 DEG C, includes such as the following group according to weight percentage Point:
1, inorganic salts (NaCl): 34%;
2, terpene resin T-80:52%;
3, stearic acid (octadecanoid acid): 13%;
4, clay stabilizer (003-A) 1%
The sum of weight percentage of each component is 100%.
Method preparation can be prepared as follows in the diverting agent:
1) under stirring, above-mentioned raw materials are added according to aforementioned proportion in a kettle, produce mixture;
2) heating mixture after stirring lower reaction 1-2h, stops reaction to 110 DEG C (being measured with 30~200 DEG C of thermometers);
3) SE series screw extruder pelletizer is used, 2) reactant wet stock obtained in is being higher than terpene resin T-80 Under the conditions of the temperature that 5~10 DEG C of softening point, conveyed to screw extruder pelletizer, under screw extruder pelletizer squeezing action, from Head aperture template extrusion molding material.Using obtaining graininess diverting agent finished product after wind cold drying.
Temporarily stifled test is carried out using the embodiment diverting agent, wherein uses the multi-functional rock core flowing test of HAQT-2HKY type Instrument, test method are following (test temperature is 45 DEG C):
1, rock core is chosen: choosing two three oil field Tang Hu horses, 56 block P2T oil reservoir has intrinsic fracture, diameter 2.5cm The rock core of long 3cm, number 1#, 2#;
2, sieve after diverting agent crushes is prepared in this implementation takes the particle of 50~70 mesh spare (due to laboratory experiment equipment The diverting agent of condition bulky grain can not pass through the experiment manifold of minor diameter);
3, it is K that i.e. 1# core forward direction, which is passed through water flooding and measures water phase permeability,W1, 2# core forward direction is passed through aviation kerosine and measures Oleic permeability KO1
4, inverse injection contains the fracturing fluid for estimating 1.2 times of quality diverting agents of crevice volume, injection rate to 1#, 2# core respectively For 1PV, the water flooding for reversely replacing 1 times of experiment manifold volume of injection is then proceeded to;
5, after 1# core continues inverse injection water flooding until pressure flow is steady, temporarily stifled rear water phase permeability K is measuredW2, Temporarily stifled rate H is calculated according to formula 2:
H=(1-KW2)÷KW1× 100% formula 2
6, after 2# core forward direction injection aviation kerosine is until pressure flow is steady, temporarily stifled rear oleic permeability K is measuredO2, press Illuminated 3 calculates infiltration recovery rate G:
G=KO2÷KO1× 100% formula 3
Following testing result is obtained according to above-mentioned steps:
The core experiment of low temperature oil-soluble temporary plugging agent temporarily blocks up rate up to 99.2% in the present embodiment turnaround fracture use.Oil mutually returns Row, infiltration recovery rate are 86.2%.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into Row equivalent replacement;And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution The range of scheme.

Claims (10)

1. a kind of diverting agent, which is characterized in that according to weight percentage include following component: inorganic salts 34%, terpene resin 52-65%, stearic acid 0-13%, clay stabilizer 1%.
2. diverting agent according to claim 1, which is characterized in that the terpene resin is selected from terpene resin T-80 or terpenes Resin T-100.
3. diverting agent according to claim 2, which is characterized in that according to weight percentage include following component: inorganic Salt 34%, terpene resin T-80 52-57%, stearic acid 8-13%, clay stabilizer 1%.
4. diverting agent according to claim 2, which is characterized in that according to weight percentage include following component: inorganic Salt 34%, terpene resin T-100 52-57%, stearic acid 8-13%, clay stabilizer 1%.
5. diverting agent according to claim 2, which is characterized in that according to weight percentage include following component: inorganic Salt 34%, terpene resin T-100 57-65%, stearic acid 0-8%, clay stabilizer 1%.
6. -5 any diverting agent according to claim 1, which is characterized in that the inorganic salts are sodium chloride.
7. the preparation method of any diverting agent of claim 1-6, which comprises the steps of:
1) inorganic salts, terpene resin, stearic acid and clay stabilizer are mixed, mixture is generated;
2) mixture is heated to 110-120 DEG C, after stirring lower reaction 1-2h, is granulated, it is dry, generate the diverting agent.
8. the preparation method of diverting agent according to claim 7, which is characterized in that the revolving speed of the stirring is 5-15r/ min。
9. the preparation method of diverting agent according to claim 8, which is characterized in that the temperature for controlling the granulation is 80- 115℃。
10. a kind of pair of reservoir, which has crack, carries out temporarily stifled method, which is characterized in that claim 1-6 is any described temporary Blocking agent is injected in the reservoir with fracturing fluid, wherein the diverting agent and the crannied mass volume ratio be (1:1)~ (1:1.2)。
CN201710976362.8A 2017-10-19 2017-10-19 Temporary plugging agent and preparation method and application thereof Pending CN109679601A (en)

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CN111793485A (en) * 2020-08-13 2020-10-20 陕西安诺瑞特石油科技有限公司 Water plugging agent and preparation method and application thereof
CN116064011A (en) * 2023-01-09 2023-05-05 西安石油大油气科技有限公司 Oil-water-miscible temporary plugging agent for oilfield fracturing and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN111793485A (en) * 2020-08-13 2020-10-20 陕西安诺瑞特石油科技有限公司 Water plugging agent and preparation method and application thereof
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Application publication date: 20190426