CN109837075A - High temperature thermal response bentonite and high temperature thermal response bentonite drilling fluid - Google Patents
High temperature thermal response bentonite and high temperature thermal response bentonite drilling fluid Download PDFInfo
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Abstract
The present invention provides a kind of high temperature thermal response bentonite and preparation method and high temperature thermal response bentonite drilling fluid.High temperature thermal response bentonite core is rigid bentonite clay particle, and outside is flexible high temperature thermal response molecular brush.Preparation method is, first by bentonite acid activation, to be then dried, then ATRP modified, rinses dry high temperature thermal response bentonite.Method of modifying is that activated bentonite and (3- aminopropyl) trimethoxy silane (ATMS) and methanol is miscible; magnetic agitation provides modified active site; methylene chloride (pyridine containing (v/v) arsenic) is added and 2- bromine isobutyl acylbromide carries out ATRP and is modified; it is added simultaneously and contains phenyl methacrylate and the paraxylene (N of the sum containing copper bromide; N, N', N "; N " pentamethyldivinyltriamine), nitrogen protection stirring.High temperature thermal response bentonite temperature sensitivity of the invention is strong, has high temperature self-healing capability, strengthens the high temperature seal-off effect of mud cake.Drilling fluid self-healing properties are good, and rheology is stablized, and have outstanding thermo-responsive and outstanding seal-off effect.
Description
Technical field
The present invention relates to a kind of high temperature thermal response bentonite and high temperature thermal response bentonite drilling fluids, belong to drilling technology neck
Domain.
Background technique
Bentonite is a kind of economic and environment-friendly essential industry raw material, and major clay minerals ingredient is montmorillonite, crystal knot
Structure is mainly made of oxygen-octahedron and alumina octahedral.Clay particle large specific surface area is rich in hydroxyl polarity adsorption group, right
Chemical treatments and hydrone have stronger adsorptivity.Therefore, in recent years, domestic and foreign scholars are using bentonite as primary raw material quilt
It is widely used in forming a film, plays the role of protection, antiseepage, antipollution.He Shichong is using natural sodium bentonite as main material structure
Build geomembrane, as refuse landfill impervious lining, have many advantages, such as infiltration coefficient it is low, it is anti-aging, can self-healing, effectively inhibit
The diafiltration of soot pollutant.For Bai et al. using bentonite as crosslinking agent, complex silicate aluminium closes object (LMSH) and N- isopropyl acyl
Amine monomers (NIPAM) are prepared for LMSH/NIPAM adsorbed film, have effectively removed the anionic pollutant in printing and dyeing material.Especially
Ground, during petroleum and natural drilling, drilling fluid is often prepared by primary raw material of bentonite in scene, using differential pressure in well
Eye surface constructs mud cake protective layer, avoids drilling fluid loss inside pit shaft from causing wellbore and the aquation avalanche of surrounding rock stratum, plays steady
Determine borehole wall effect.
But it with going deep into for drilling well, is influenced by stratum high-temperature hyperbaric environment, conventional bentonite base film technique cannot be effective
The leakage of drilling fluid is prevented, Microscopic is the increase of mud cake hole, filling blocking polymer degradation.Therefore, the present invention intends glutinous
Native surface constructs thermal response polymer molecule brush, and when formation temperature is higher than polymer phase transition temperature, polymer molecule brush can
Auto polymerization enhances the high temperature seal-off effect of mud cake.
Summary of the invention
The present invention is quasi- aiming at the problem that conventional bentonite base film technique not can effectively prevent the leakage of drilling fluid, in swelling
Native surface constructs thermal response polymer molecule brush, and when formation temperature is higher than polymer phase transition temperature, polymer molecule brush can
Auto polymerization enhances the high temperature seal-off effect of mud cake.
The present invention uses above-mentioned technical purpose, adopts the following technical scheme that.
The present invention provides a kind of high temperature thermal response bentonite, is based on Transfer Radical Polymerization (ATRP), to swelling
The calibration activated sites point of soil carries out graft modification, constructs the response agent of star bentonite base, and core is rigid bentonite clay particle, outside
Portion is flexible high temperature thermal response molecular brush, and more specifically, the thermal response molecular brush is poly- (benzyl acrylic ester), point
Son amount Mn is 5000~60000, it is preferred that is 5000~25000.
High temperature thermal response preparation method for bentonite of the invention includes the following steps:
Step 1, bentonite acid activation, building activation site.
10~15wt% aqueous hydrochloric acid solution of 1~3g bentonite mixing 100mL is constructed into hydroxyl to dredge clay duct
Point is adsorbed, bentonite adsorption is improved.
Step 2 is dried bentonite.
In 120~150 DEG C of drying process bentonites, drying time is 10~for 24 hours, remove the hydrochloric acid and water in bentonite
Point.
Step 3, ATRP are modified.
Activated bentonite and 0.5~1mL (3- aminopropyl) trimethoxy silane (ATMS) and 10~40mL methanol is miscible,
12~16h of magnetic agitation under the conditions of 35~45 DEG C provides ATRP modified active site.
Then, be added the 2- bromine isobutyl acylbromide of 10~20mL methylene chloride (contain 3~5% (v/v) arsenic pyridines) and 5~10mL into
Row ATRP is modified.During ATRP is modified, be added containing 5~10g phenyl methacrylate and 5~10mL paraxylene (containing 0.5~
The N of 1g copper bromide and 0.3~0.5mL, N, N', N ", N "-pentamethyldivinyltriamine), under the conditions of 80~100 DEG C, nitrogen
Protection stirring 8~10 hours, it is modified to complete ATRP.
Step 4 rinses drying.
After modification, bentonite methylene chloride and ethyl alcohol rinse 3 times or more.Then, nitrogen protection is dry, and high temperature is made
Thermal response bentonite.
It adopts with the aforedescribed process, the height of preparation warms corresponding bentonite bentonite, poly- in the building thermal response of bentonite surface
Adduct molecule brush, when formation temperature be higher than polymer phase transition temperature when, polymer molecule brush can auto polymerization, enhance the height of mud cake
Warm seal-off effect, principle are as shown in Figure 1.Specifically, the thermal response molecular brush is poly- (benzyl acrylic ester), molecular weight
Mn is 5000~60000, it is preferred that is 5000~25000.
Based on self-healing ability excellent under thermal response bentonite hot environment, further prepared using thermal response bentonite high
Performance water-base drilling fluid, specifically, being used to prepare including the bentonitic high temperature thermal response bentonite drilling fluid of high temperature thermal response.
The high temperature thermal response bentonite drilling fluid includes:
Water 300mL；
8~12g of high temperature thermal response bentonite；
3~4.5g of sodium chloride；
Anionic carboxymethyl cellulose (Lv-PAC) 2~3g；
1~2g of amphoteric ion polymer FA367；
Calcium carbonate superfine powder powder (partial size is 2000 mesh) 10~15g；
Weighting material (blanc fixe, 200 mesh) is adjusted to required density.
The preparation method of high temperature thermal response bentonite drilling fluid, comprising the following steps:
Firstly, by high temperature thermal response bentonite prehydration.
8~12g high temperature thermal response bentonite and 300mL pure water are mixed, 4~5h is stirred at 30~50 DEG C, forms soil paste.
Then, 3~4.5g sodium chloride is added into soil paste, stirs 7~9h at 30~50 DEG C, enhances high temperature thermal response swelling
The aquation dispersion of soil.
Then, 2~3g anionic carboxymethyl cellulose (Lv-PAC) is added and 1~2g amphoteric ion polymer FA367 is micro-
Wave concussion 7~10h of stirring, enhances the stability and cliff performance of drilling fluid.
Common inertia plugging material calcium carbonate superfine powder powder (partial size is 2000 mesh) 10~15g is further added, it is sufficiently mixed
12~16h of stirring is closed, mixing speed is 500~700 revs/min.
Finally, being slowly added to weighting material (blanc fixe, 200 mesh) into the base fluid of above-mentioned preparation, while adding strength
Mechanical stirring, mixing speed is 500~800 revs/min, until drilling fluid density reaches 2.1g/cm3Until.Obtain high warm
Respond bentonite drilling fluid.
The present invention by adopting the above technical scheme, obtains following technical effect.
1, high temperature thermal response bentonite of the invention, temperature sensitivity is strong, polymer molecule brush block filling performance it is strong and
Stablize.
2, high temperature thermal response bentonite of the invention has high temperature self-healing capability, strengthens the high temperature seal-off effect of mud cake.
3, high temperature thermal response bentonite drilling fluid of the invention, self-healing properties are good, and rheology is stablized, and have outstanding thermal response
Property and outstanding seal-off effect.
Detailed description of the invention
Fig. 1 is that the bentonitic high temperature of high temperature thermal response blocks mechanism figure；
Fig. 2 is the influence diagram that temperature is percolated high temperature thermal response bentonite slurry；
Fig. 3 is that seal-off effect and Shale Hydration expand variation diagram to high temperature thermal response bentonite in a high temperauture environment；
Fig. 4 is that common bentonite drilling fluid and high temperature thermal response bentonite drilling fluid apparent viscosity change under different temperatures
Figure；
Fig. 5 is the high temperature seal-off effect comparison diagram of common bentonite drilling fluid and high temperature thermal response bentonite drilling fluid.
Specific embodiment
With reference to embodiment, technical solution of the present invention is further described, makes the skill of this field
Art personnel can better understand the present invention and can be practiced.
Embodiment 1 to embodiment 4 is high temperature thermal response preparation method for bentonite
Embodiment 1
A kind of high temperature thermal response bentonite, preparation method the following steps are included:
Step 1, bentonite acid activation, building activation site.
By the 7wt% aqueous hydrochloric acid solution of 3g bentonite mixing 100mL, to dredge clay duct, building hydroxyl adsorbs point,
Improve bentonite adsorption.
Step 2 is dried bentonite.
In 120~150 DEG C of drying process bentonites, drying time is 10~for 24 hours, remove the hydrochloric acid and water in bentonite
Point.
Step 3, ATRP are modified.
Miscible, 42 DEG C of items by activated bentonite and 0.5mL (3- aminopropyl) trimethoxy silane (ATMS) and 10mL methanol
12~16h of magnetic agitation under part provides ATRP modified active site.
Then, 10mL methylene chloride (containing 2% (v/v) arsenic pyridine) is added and the 2- bromine isobutyl acylbromide progress ATRP of 5mL is modified.
During ATRP is modified, be added phenyl methacrylate containing 5g and 5mL paraxylene (N, the N of bromination containing 5mL ketone and 0.14mL,
N', N ", N "-pentamethyldivinyltriamine), under the conditions of 90 DEG C, nitrogen protection is stirred 6 hours, and it is modified to complete ATRP.
Step 4 rinses drying.
After polymerization, bentonite methylene chloride and ethyl alcohol rinse 3 times or more.Then, nitrogen protection is dry, and high temperature is made
Thermal response bentonite.Its core is rigid bentonite clay particle, and outside is the poly- (benzyl third that molecular weight Mn is 5000~10000
Olefin(e) acid ester) flexible high temperature thermal response molecular brush.
Embodiment 2
A kind of high temperature thermal response bentonite, preparation method the following steps are included:
Step 1, bentonite acid activation, building activation site.
By the 10wt% aqueous hydrochloric acid solution of 1g bentonite mixing 100mL, to dredge clay duct, building hydroxyl adsorbs point
Bentonite adsorption is improved in position.
Step 2 is dried bentonite.
In 120~150 DEG C of drying process bentonites, drying time is 10~for 24 hours, remove the hydrochloric acid and water in bentonite
Point.
Step 3, ATRP are modified.
Miscible, 35 DEG C of items by activated bentonite and 0.5mL (3- aminopropyl) trimethoxy silane (ATMS) and 10mL methanol
Magnetic agitation 12h under part provides ATRP modified active site.
Then, 10mL methylene chloride (containing 3% (v/v) arsenic pyridine) is added and the 2- bromine isobutyl acylbromide progress ATRP of 5mL is modified.
During ATRP is modified, be added phenyl methacrylate containing 5g and 5~10mL paraxylene (copper bromide containing 0.5g and 0.3mL's
N, N, N', N ", N "-pentamethyldivinyltriamine), under the conditions of 80 DEG C, nitrogen protection is stirred 8 hours, and it is modified to complete ATRP.
Step 4 rinses drying.
After modification, bentonite methylene chloride and ethyl alcohol rinse 3 times or more.Then, nitrogen protection is dry, and high temperature is made
Thermal response bentonite.Its core is rigid bentonite clay particle, and outside is the poly- (benzyl third that molecular weight Mn is 10000~15000
Olefin(e) acid ester) flexible high temperature thermal response molecular brush.
Embodiment 3
A kind of high temperature thermal response bentonite, preparation method the following steps are included:
Step 1, bentonite acid activation, building activation site.
By the 15wt% aqueous hydrochloric acid solution of 3g bentonite mixing 100mL, to dredge clay duct, building hydroxyl adsorbs point
Bentonite adsorption is improved in position.
Step 2 is dried bentonite.
In 120~150 DEG C of drying process bentonites, drying time is 10~for 24 hours, remove the hydrochloric acid and water in bentonite
Point.
Step 3, ATRP are modified.
Miscible, 45 DEG C of conditions by activated bentonite and 1mL (3- aminopropyl) trimethoxy silane (ATMS) and 40mL methanol
Lower magnetic agitation 16h provides ATRP modified active site.
Then, the 2- bromine isobutyl acylbromide progress ATRP that 20mL methylene chloride (containing 5% (v/v) arsenic pyridine) and 10mL is added changes
Property.During ATRP is modified, be added phenyl methacrylate containing 10g and 10mL paraxylene (N of copper bromide containing 1g and 0.5mL,
N, N', N ", N "-pentamethyldivinyltriamine), under the conditions of 90 DEG C, nitrogen protection is stirred 10 hours, and it is modified to complete ATRP.
Step 4 rinses drying.
After modification, bentonite methylene chloride and ethyl alcohol rinse 3 times or more.Then, nitrogen protection is dry, and high temperature is made
Thermal response bentonite.Its core is rigid bentonite clay particle, and outside is the poly- (benzyl third that molecular weight Mn is 20000~25000
Olefin(e) acid ester) flexible high temperature thermal response molecular brush.
Embodiment 4
A kind of high temperature thermal response bentonite, preparation method the following steps are included:
Step 1, bentonite acid activation, building activation site.
By the 12wt% aqueous hydrochloric acid solution of 2g bentonite mixing 100mL, to dredge clay duct, building hydroxyl adsorbs point
Bentonite adsorption is improved in position.
Step 2 is dried bentonite.
In 120~150 DEG C of drying process bentonites, drying time is 10~for 24 hours, remove the hydrochloric acid and water in bentonite
Point.
Step 3, ATRP are modified.
Miscible, 40 DEG C of items by activated bentonite and 0.7mL (3- aminopropyl) trimethoxy silane (ATMS) and 25mL methanol
Magnetic agitation 14h under part provides ATRP modified active site.
Then, 15mL methylene chloride (containing 4% (v/v) arsenic pyridine) is added and the 2- bromine isobutyl acylbromide progress ATRP of 7mL is modified.
During ATRP is modified, be added phenyl methacrylate containing 7g and 8mL paraxylene (N, the N of copper bromide containing 0.7g and 0.4mL,
N', N ", N "-pentamethyldivinyltriamine), under the conditions of 100 DEG C, nitrogen protection is stirred 9 hours, and it is modified to complete ATRP.
Step 4 rinses drying.
After modification, bentonite methylene chloride and ethyl alcohol rinse 3 times or more.Then, nitrogen protection is dry, and high temperature is made
Thermal response bentonite.Its core is rigid bentonite clay particle, and outside is the poly- (benzyl third that molecular weight Mn is 15000~20000
Olefin(e) acid ester) flexible high temperature thermal response molecular brush.
Embodiment 5 to embodiment 8 is the preparation of high temperature thermal response bentonite drilling fluid
Embodiment 5
A kind of high temperature thermal response bentonite drilling fluid, preparation method the following steps are included:
First by high temperature thermal response bentonite prehydration, 12g high temperature thermal response bentonite and 300mL pure water are mixed, 30~
4~5h is stirred at 50 DEG C, forms soil paste.
Then, 4.5g sodium chloride particle is added into soil paste, 7~9h is stirred at 30~50 DEG C, enhancing high temperature thermal response is swollen
The aquation dispersion of profit soil.
Then, 3g anionic carboxymethyl cellulose (Lv-PAC) is added and 1.5g amphoteric ion polymer FA367 microwave shakes
7~10h of stirring is swung, the stability and cliff performance of drilling fluid are enhanced.The common ultra-fine carbon of inertia plugging material is further added
Sour calcium powder (partial size is 2000 mesh) 10g, is sufficiently mixed 12~16h of stirring, mixing speed is 500~700 revs/min.
Finally, being gradually added into weighting material (blanc fixe, 200 mesh) into the base fluid of above-mentioned preparation, while adding strength
Mechanical stirring, mixing speed is 500~800 revs/min, until drilling fluid density reaches 2.1g/cm3Until.Obtain high warm
Respond bentonite drilling fluid.
Embodiment 6
A kind of high temperature thermal response bentonite drilling fluid, preparation method the following steps are included:
Firstly, by high temperature thermal response bentonite prehydration, mixing 8g high temperature thermal response bentonite and 300mL pure water, 30~
4~5h is stirred at 50 DEG C, forms soil paste.
Then, 3g sodium chloride is added into soil paste, 7~9h is stirred at 30~50 DEG C, enhancing high temperature thermal response is bentonitic
Aquation dispersion.
Then, 2g anionic carboxymethyl cellulose (Lv-PAC) is added and 1g amphoteric ion polymer FA367 microwave shakes
7~10h is stirred, the stability and cliff performance of drilling fluid are enhanced.
Common inertia plugging material calcium carbonate superfine powder powder (partial size is 2000 mesh) 10g is further added, is sufficiently mixed and stirs
12~16h is mixed, mixing speed is 500~700 revs/min.
Finally, being slowly added to weighting material (blanc fixe, 200 mesh) into the base fluid of above-mentioned preparation, while adding strength
Mechanical stirring, mixing speed is 500~800 revs/min, until drilling fluid density reaches 2.1g/cm3Until.Obtain high warm
Respond bentonite drilling fluid.
Embodiment 7
A kind of high temperature thermal response bentonite drilling fluid, preparation method the following steps are included:
Firstly, by high temperature thermal response bentonite prehydration.
12g high temperature thermal response bentonite and 300mL pure water are mixed, 4~5h is stirred at 30~50 DEG C, forms soil paste.
Then, 4.5g sodium chloride is added into soil paste, stirs 7~9h at 30~50 DEG C, enhances high temperature thermal response bentonite
Aquation dispersion.
Then, 3g anionic carboxymethyl cellulose (Lv-PAC) is added and 2g amphoteric ion polymer FA367 microwave shakes
7~10h is stirred, the stability and cliff performance of drilling fluid are enhanced.
Common inertia plugging material calcium carbonate superfine powder powder (partial size is 2000 mesh) 5g is further added, is sufficiently mixed stirring
12~16h, mixing speed are 500~700 revs/min.
Finally, being slowly added to weighting material (blanc fixe, 200 mesh) into the base fluid of above-mentioned preparation, while adding strength
Mechanical stirring, mixing speed is 500~800 revs/min, until drilling fluid density reaches 2.1g/cm3Until.Obtain high warm
Respond bentonite drilling fluid.
Embodiment 8
A kind of high temperature thermal response bentonite drilling fluid, preparation method the following steps are included:
Firstly, by high temperature thermal response bentonite prehydration.
10g high temperature thermal response bentonite and 300mL pure water are mixed, 4~5h is stirred at 30~50 DEG C, forms soil paste.
Then, 4g sodium chloride is added into soil paste, 7~9h is stirred at 30~50 DEG C, enhancing high temperature thermal response is bentonitic
Aquation dispersion.
Then, 2.5g anionic carboxymethyl cellulose (Lv-PAC) and 1.5g amphoteric ion polymer FA367 microwave is added
Concussion 7~10h of stirring, enhances the stability and cliff performance of drilling fluid.
Common inertia plugging material calcium carbonate superfine powder powder (partial size is 2000 mesh) 12g is further added, is sufficiently mixed and stirs
12~16h is mixed, mixing speed is 500~700 revs/min.
Finally, being slowly added to weighting material (blanc fixe, 200 mesh) into the base fluid of above-mentioned preparation, while adding strength
Mechanical stirring, mixing speed is 500~800 revs/min, until drilling fluid density reaches 2.1g/cm3Until.Obtain high warm
Respond bentonite drilling fluid.
Comparative example 1
First by common bentonite prehydration, the common bentonite of 12g and 300mL pure water are mixed, stirring 4 at 30~50 DEG C~
5h forms soil paste.
Then, 4.5g sodium chloride particle is added into soil paste, 7~9h is stirred at 30~50 DEG C, enhancing is common bentonitic
Aquation dispersion.
Then, 3g anionic carboxymethyl cellulose (Lv-PAC) is added and 1.5g amphoteric ion polymer FA367 microwave shakes
7~10h of stirring is swung, the stability and cliff performance of drilling fluid are enhanced.
Common inertia plugging material calcium carbonate superfine powder powder (partial size is 2000 mesh) 9g is further added, is sufficiently mixed stirring
12~16h, mixing speed are 500~700 revs/min.
Finally, being gradually added into weighting material (blanc fixe, 200 mesh) into the base fluid of above-mentioned preparation, while adding strength
Mechanical stirring, mixing speed is 500~800 revs/min, until drilling fluid density reaches 2.1g/cm3Until.It obtains common swollen
Moisten earth boring auger well liquid.
The raw material of embodiment and comparative example are from sodium bentonite, and purchase is in Nan DEG C of or company, mud cake film forming master
Raw material is wanted, granular size is 200 mesh, and cation exchange capacity (CEC) is 145meq/100g, mineralogical composition 13.22%
Al2O3, 71.30%SiO2, 7.10%MgO, 4.79%Na2O and 3.59%Fe2O3；Hydrochloric acid, (3- aminopropyl) trimethoxy silane
(ATMS) and methanol activated bentonite, the two are that chemical analysis is pure, are purchased from Shanghai Aladdin Reagent Company；Methylene chloride and 2-
Bromine isobutyl acylbromide is modified (ATRP) for bentonite surface atom transition free radical aggregation, and the two is that chemical analysis is pure, is purchased from
Shanghai Aladdin Reagent Company.Phenyl methacrylate, paraxylene (p-xylene), bromination ketone (CuBr) and N, N, N', N ",
N "-pentamethyldivinyltriamine (PMDETA) is that chemical analysis is pure, modified for bentonite Thermo-sensitive, be purchased from Shanghai Ah
Latin reagent；Anionic carboxymethyl cellulose (Lv-PAC), amphoteric ion polymer (FA367), calcium carbonate superfine powder powder and weight are brilliant
Mountain flour is purchased from Chengdu Ke Long chemical reagent factory for drilling fluid preparation.
Experimental example
1 high temperature and pressure diafiltration experiments of experimental example
For simulated formation high temperature and high pressure environment, using high pressure high temperature filter tester test different hot environments (120 DEG C, 140
DEG C, 150 DEG C, 160 DEG C, 170 DEG C) under influence of the high temperature thermal response bentonite to kettle internal water seepage flow.By 12g embodiment 1
Thermal response bentonite mixing 300mL deionized water, 400~600r/min mechanical stirring 30min prepare high temperature thermal response bentonite
Slurries (abbreviation soil paste).Then, soil paste will be prepared and pour into high-temperature and high-pressure filter press, and with nitrogen injection pressure 3.5MPa, set simultaneously
Meter experiment diafiltration temperature.When temperature in the kettle reaches experimental temperature, seepage channel valve is opened, is recorded in different time, in kettle
The filter loss of fluid is shown below with calculating soil paste percolation flow velocity.
vHTHPFor under soil paste high temperature and high pressure environment, average infiltration rate in the t time, cm3/min；
QHTHPFor under soil paste high temperature and high pressure environment, infiltration capacity in the t time, cm3；
T is diafiltration time, min.
The infiltration rate of high temperature thermal response bentonite base slurry changes as shown in Fig. 2, figure temperature is to high temperature thermal response bentonite
The influence of slurries diafiltration.As seen from the figure, experimental temperature (120 DEG C) is not up to modified alta-mud response temperature, and soil paste is instantaneous
Infiltration rate (in 1min average infiltration rate) is greater than 6mL/min, and API infiltration rate (30min be averaged infiltration rate) is greater than
3mL/min.However, the instantaneous infiltration rate of soil paste significantly reduces when experimental temperature is 140 DEG C, it is 2.1mL/min, API diafiltration
Speed is 1.2mL/min, same to significantly reduce, show that temperature reaches the phase transition temperature of polymer molecule brush, starts filling simultaneously
Block mud cake hole.As temperature increases, soil paste infiltration rate is further decreased, it is shown that the self-healing row of modified alta-mud
For.And when temperature reaches 160 DEG C, it is seen that soil paste infiltration rate changes over time rule and tends to straight line, and soil paste instantaneously seeps
Filtering velocity degree shows that modified alta-mud temperature sensitivity is strong, and polymer molecule brush blocks filling performance close to API infiltration rate
It is strong and stable.
2 high temperature and pressure shale linear expansion of experimental example experiment
Currently, borehole well instability mostly occurs on water-sensitive shale stratum.Therefore, herein with Longma small stream group water-sensitive shale be grind
Study carefully object, further tests seal-off effect and its influence to Shale Hydration in a high temperauture environment of high temperature thermal response bentonite.It is real
It tests shale used and is derived from Sichuan Province Yibin City Longma small stream group stratum.Firstly, chisel take part shale and using solid disintegrating machine by its
It smashes to powder (partial size is 200 mesh).Then, 5g slate flour is taken to be placed in rock core pressure setting, compacting 10min preparation experiment rock
The heart, experimental pressure 10MPa.Then rock core will be tested and be placed in high-temperature high pressure dilatometer (purchased from Qingdao with spring petroleum instrument plant)
In rock core cup, and the 10mL soil paste of injection experiments example 1, it sets under record different temperatures (experimental pressure 3.5MPa), rock core 16
The variation of linear expansion rate, linear expansion rate calculation formula are shown below in hour.
ω=(Rt-R0)/H × 100%
ω is rock core linear expansion rate, %；
RtFor the altitude reading of rock core t time, mm；
RoFor rock core elemental height reading, mm；
H is the initial length of rock core, mm.
Experimental result is as shown in figure 3, as seen from the figure, shale linear expansion rate increases with temperature and reduced.Temperature is
At 140 DEG C, shale linear expansion rate is substantially reduced, and expansion amplitude obviously reduces in 16 hours, with soil paste diafiltration experiments result phase
Unanimously, the high-temperature healing ability of the bentonitic polymer molecule brush of thermal response is embodied.When test temperature be greater than 150 DEG C, experiment
The result shows that the seal-off effect of mud cake tends towards stability, shale expansion rate is small, and amplitude of variation is little.This is because thermal response bentonite
High temperature self-healing capability, strengthen the high temperature seal-off effect of mud cake.
The experiment of 3 property of drilling fluid of experimental example
Property of drilling fluid experiment, by the high temperature thermal response bentonite drilling fluid of embodiment 5 and the common bentonite of comparative example 1
Drilling fluid is placed in heat rolling aging in ageing can, later with rotational viscometer measurement drilling fluid rheology variation, experimental result such as Fig. 4
It is shown.Fig. 4 reflects the viscosity change curve of two types drilling fluid following temperature change, and wherein SSDWX represents high temperature thermal response
Bentonite drilling fluid, DWX represent common bentonite drilling fluid, and conventional bentonite base drilling fluid following temperature increases as seen from the figure
Viscosity gradually decreases, and drilling fluid rheology performance is unstable.Although high temperature thermal response bentonite drilling fluid is increased with temperature, early period is glutinous
Degree reduces, but Drilling Fluid Viscosity gradually gos up after temperature is greater than 120 DEG C, shows self-healing properties, and drilling fluid rheology is stablized.
Then, by the common bentonite drilling fluid of the high temperature thermal response bentonite drilling fluid of upper embodiment 5 and comparative example 1
It is respectively placed in 150 DEG C of high-temperature high pressure dilatometers and 150 DEG C of high temperature and pressure diafiltration instrument, measures the high temperature seal-off effect of drilling fluid, it is real
It is as shown in Figure 5 to test result.In figure, SSDWX represents high temperature thermal response bentonite drilling fluid, and DWX represents common bentonite drilling fluid,
Fig. 5 can be seen that under hot environment (150 DEG C), and the seal-off effect of high temperature thermal response bentonite drilling fluid is significantly stronger than bentonite
The linear expansion rate of drilling fluid, shale is down to 2.3% by 6.3%, and API filtration is down to 1.4mL by 7.2mL.Experimental result is tested
The thermo-responsive of high temperature thermal response bentonite drilling fluid is demonstrate,proved.
Technical solution provided by the invention, is not restricted to the described embodiments, it is all by structure of the invention and in the way of,
By converting and replacement is formed by technical solution, all within the scope of the present invention.
Claims (9)
1. a kind of high temperature thermal response bentonite, it is characterised in that: high temperature thermal response bentonite core is rigid bentonite clay particle, outside
Portion is flexible high temperature thermal response molecular brush.
2. high temperature thermal response bentonite according to claim 1, it is characterised in that: flexible high temperature thermal response molecular brush is poly-
(benzyl acrylic ester).
3. high temperature thermal response bentonite according to claim 2, it is characterised in that: the molecule of thermal response polymer molecule brush
Measuring Mn is 5000~60000.
4. high temperature thermal response bentonite according to claim 2, it is characterised in that: the molecule of thermal response polymer molecule brush
Measuring Mn is 5000~25000.
5. a kind of high temperature thermal response preparation method for bentonite as described in Claims 1-4 is any, it is characterised in that including with
Lower step:
Step 1, bentonite acid activation, building activation site
By bentonite mixing aqueous hydrochloric acid solution, clay duct is dredged, building hydroxyl adsorbs point, improves bentonite adsorption；
Step 2 is dried
It is dried the bentonite of step 1, removes hydrochloric acid and moisture in bentonite；
Step 3, ATRP are modified
Activated bentonite and 0.5~1mL (3- aminopropyl) trimethoxy silane (ATMS) and 10~40mL methanol is miscible, 35~
12~16h of magnetic agitation under the conditions of 45 DEG C provides ATRP modified active site；
Then, 10~20mL methylene chloride (containing 3~5% (v/v) arsenic pyridines) is added and the 2- bromine isobutyl acylbromide of 5~10mL carries out
ATRP is modified, during ATRP is modified, is added and (contains 0.5~1g containing 5~10g phenyl methacrylate and 5~10mL paraxylene
The N of copper bromide and 0.3~0.5mL, N, N', N ", N "-pentamethyldivinyltriamine), under the conditions of 80~100 DEG C, nitrogen is protected
Shield stirring 8~10 hours, it is modified to complete ATRP；
Step 4 rinses drying
After modification, drying is rinsed, high temperature thermal response bentonite is made.
6. high temperature thermal response preparation method for bentonite according to claim 5, it is characterised in that the following steps are included:
Step 1, bentonite acid activation, building activation site
By 10~15wt% aqueous hydrochloric acid solution of 1~3g bentonite mixing 100mL, clay duct is dredged, building hydroxyl adsorbs point
Bentonite adsorption is improved in position；
Step 2 is dried
120~150 DEG C be dried step 1 bentonite, drying time be 10~for 24 hours, remove bentonite in hydrochloric acid and
Moisture；
Step 3, ATRP are modified
Activated bentonite and 0.5~1mL (3- aminopropyl) trimethoxy silane (ATMS) and 10~40mL methanol is miscible, 35~
12~16h of magnetic agitation under the conditions of 45 DEG C provides ATRP modified active site；
Then, 10~20mL methylene chloride (containing 3~5% (v/v) arsenic pyridines) is added and the 2- bromine isobutyl acylbromide of 5~10mL carries out
ATRP is modified, during ATRP is modified, is added and (contains 0.5~1g containing 5~10g phenyl methacrylate and 5~10mL paraxylene
The N of copper bromide and 0.3~0.5mL, N, N', N ", N "-pentamethyldivinyltriamine), under the conditions of 80~100 DEG C, nitrogen is protected
Shield stirring 8~10 hours, it is modified to complete ATRP；
Step 4 rinses drying
After modification, bentonite methylene chloride and ethyl alcohol rinse 3 times or more, then, nitrogen protection is dry, and high warm is made and rings
Answer bentonite.
7. application of the high temperature thermal response bentonite in drilling fluid as described in Claims 1-4 is any, it is characterised in that: use
In the bentonitic high temperature thermal response bentonite drilling fluid of high temperature thermal response that preparation includes described in Claims 1-4 is any.
8. application of the high temperature thermal response bentonite as claimed in claim 7 in drilling fluid, it is characterised in that: the high warm
It responds bentonite drilling fluid ingredient and proportion is,
8~12g of high temperature thermal response bentonite；
3~4.5g of sodium chloride；
Anionic carboxymethyl cellulose (Lv-PAC) 2~3g；
1~2g of amphoteric ion polymer FA367；
Calcium carbonate superfine powder powder (partial size is 2000 mesh) 10~15g；
Water 300mL；
Weighting material (blanc fixe, 200 mesh) is adjusted to required density.
9. a kind of high temperature thermal response bentonite drilling fluid, it is characterised in that: high temperature thermal response bentonite drilling fluid ingredient and proportion
It is as follows,
8~12g of high temperature thermal response bentonite；
3~4.5g of sodium chloride；
Anionic carboxymethyl cellulose (Lv-PAC) 2~3g；
1~2g of amphoteric ion polymer FA367；
Calcium carbonate superfine powder powder (partial size is 2000 mesh) 10~15g；
Water 300mL；
Weighting material (blanc fixe, 200 mesh) is adjusted to required density.
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