CN106883831B - A kind of novel oil base drilling fluid organic sepiolite and preparation method thereof - Google Patents

A kind of novel oil base drilling fluid organic sepiolite and preparation method thereof Download PDF

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CN106883831B
CN106883831B CN201710236093.1A CN201710236093A CN106883831B CN 106883831 B CN106883831 B CN 106883831B CN 201710236093 A CN201710236093 A CN 201710236093A CN 106883831 B CN106883831 B CN 106883831B
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sepiolite
organic
drilling fluid
oil base
base drilling
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CN106883831A (en
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张泽朋
庄官政
廖立兵
吕国诚
梅乐夫
谭建杰
欧阳东红
刘卫湘
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Xiangtan Sepiolite Technology Co Ltd
China University of Geosciences Beijing
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Xiangtan Sepiolite Technology Co Ltd
China University of Geosciences Beijing
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    • 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
    • C09K8/02Well-drilling compositions
    • C09K8/03Specific additives for general use in well-drilling compositions
    • 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
    • C09K8/02Well-drilling compositions
    • C09K8/32Non-aqueous well-drilling compositions, e.g. oil-based

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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Silicates, Zeolites, And Molecular Sieves (AREA)
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Abstract

The invention discloses a kind of novel oil base drilling fluid organic sepiolites and preparation method thereof, the preparation method includes will be after the abundant aquation of sepiolite, it is organically-modified to sepiolite progress that specific quaternary ammonium salt cationic surfactant is added, oil base drilling fluid organic sepiolite can be prepared.This preparation method condition is simple, low to the device requirement of production, is conducive to the popularization of industrialization, organic sepiolite lipophilicity obtained is good, and rheological property is excellent in oil base drilling fluid, mention it is viscous, mention and cut significant effect, thixotropy is prominent, and high temperature resistant property is excellent, can use under the conditions of 200 DEG C.

Description

A kind of novel oil base drilling fluid organic sepiolite and preparation method thereof
Technical field
The present invention relates to oilfield drilling field, in particular to a kind of lipophilicity is good, rheological characteristic and high temperature resistant property are excellent Oil base drilling fluid organic sepiolite and preparation method thereof.
Background technique
Sepiolite is aqueous magnesium silicate, and it is viscous to belong to 2:1 layers of chain for the transiens structure feature with chain and stratiform Soil.Its general structure is Mg8Si12O30(OH)4(OH2)4·8H2O is made of oxygen-octahedron and magnesia octahedron.Constitute silicon oxygen The oxygen on tetrahedron basis constitutes the continuous crystal layer of interval about 0.65nm, and apex angle oxygen is alternately directed to this continuous crystal layer Up and down.Crystal layer is connected with each other by octahedral coordination magnesium ion.Therefore, there is continuous four sides in the crystal structure of sepiolite Body piece, and octahedral sheet is then channel discontinuous, that formation size is about 0.37nm × 1.06nm.Structure based on sepiolite Feature, with biggish specific surface area, adsorptivity, the cationic properties such as exchangeability and rheological characteristic.The cation of sepiolite is handed over Changing capacity is 20~45mmol/100g.
The wide range of applications of sepiolite, these applications are mainly based upon the adsorptivity, optical property, stream of sepiolite The features such as denaturation and molecular sieve effect.The main application fields of sepiolite include adsorbent, cleanser, catalyst carrier, drug Sustained release agent and rheology control agent etc..Haden(Attapulgite:properties and uses[J].Clays Clay Miner, 1963,10:284-290.) application of palygorskite and sepiolite is divided into colloidal type and non-colloid class two major classes.Colloid The application of class is primarily referred to as the fibrous structure using sepiolite, makes its dispersion in the liquid phase, utilizes the dispersion liquid of formation, colloidal sol The even performance of gel rubber system.The application of non-colloid class refers to using the crystal structure of sepiolite itself, property or utilizes sea The performance of afrodite particle itself.
Sepiolite is microcosmic upper in threadiness, with { 110 } cleavage for being parallel to fiber axis, in water and highly polar solvent easily In dispersion, mixed and disorderly fibrous suspension system is formed, rheological characteristic is fabulous.Therefore, application of the sepiolite in water-base drilling fluid It can protrude very much, there is good salt-resistance and high temperature resistance, commonly bored in salt water, seawater drilling well and high-temperature drilling field Well liquid rheology control agent.
With the development of drilling engineering, the Holes of Complicated Wells such as high temperature deep well, horizontal well and offshore drilling for being faced in drilling practice It is more and more.The performance that can drilling fluid keep stable and excellent under high temperature, high pressure, conditions of high density is most important.Oil base Drilling fluid is widely used in excellent properties such as its excellent high temperature resistance, lubricity, borehole wall stability, salt-resistance and low-permeabilities In such complex drilling engineering.
Organic clay is widely used in oil base drilling fluid because of its excellent gelling performance in oil based system and thixotropy Rheology control agent.Currently, widely used rheology control agent is organobentonite in oil base drilling fluid.Bentonite is with montmorillonite For the clay rock of essential mineral.Organobentonite is usually that organic cation is inserted into montmorillonite in the way of cation exchange Interlayer supports big interlamellar spacing, enhances the lipophilicity of the surface and interface of organic montmorillonite.Organobentonite is added in oil based system, lamella Structure disperses, expansion, removing and form the network structure on different scale, provide good thixotropy and gelling for drilling fluid Intensity can effectively adjust rheological property of oil base drilling fluid.However, high temperature resistance of the organobentonite in oil base drilling fluid is past Toward the demand for being insufficient for actual well drilled, usually it is difficult to bear by the oil base drilling fluid of rheology control agent of organobentonite 180 DEG C or more of high temperature.This is because the lamellar structure of organic montmorillonite at high temperature can atrophy, network structure, which is destroyed, to be caused 's.
Sepiolite forms network structure by the mixed and disorderly dispersion of its fiber in aqueous based systems, and creates excellent rheology Performance.It is contemplated that changing the surface property of sepiolite by organically-modified, makes its lipophilicity enhancing, also can achieve similar Effect in aqueous based systems.
Currently, modification and product development in relation to sepiolite mainly surround adsorbent, cleanser, catalyst carrier, height What the rheological agent in molecular composite material and aqueous based systems was unfolded.Organically-modified for sepiolite is studied fewer, at present The modified organic sepiolite of the only useful cetyl trimethylammonium bromide of organic sepiolite report, mainly applies and controls in environment Reason and the preparation etc. of macromolecule/sepiolite composite material.And organic sepiolite made from other types organic modifiers with And its research of the application aspect in oil base drilling fluid rarely has document report.
Since the thermal stability of cetyl trimethylammonium bromide modifying agent is poor, it is difficult to meet the work of oil base drilling fluid It is required that being seldom used as modifying agent application in bentonite preparation, therefore cetyl trimethyl bromination is used currently on the market The modified organic sepiolite of ammonium is equally difficult to meet the requirement of organic drilling mud.
Therefore, insufficient in order to solve existing organobentonite thermal stability, especially in solution complex drilling practice The problem of rheological characteristic and the high temperature resistance deficiency of oil base drilling fluid is badly in need of studying and develops that rheological property is prominent, high temperature resistance is good Rheology control agent, and modified organic sepiolite is expected to become this excellent rheologic controlling agent.
Summary of the invention
To solve the above-mentioned problems, present inventor has performed sharp studies, as a result, it has been found that: use specific quaternary table Face activating agent is organically-modified to sepiolite progress, can prepare lipophilic oil base good, that rheological characteristic and high temperature resistant property are excellent and bore Well liquid organic sepiolite.This preparation method condition is simple, low to the device requirement of production, thereby completing the present invention.
The purpose of the present invention is to provide following aspect:
(1) a kind of preparation method of novel oil base drilling fluid organic sepiolite, comprising the following steps:
Step 1, sepiolite raw material is mixed with solvent;
Step 2, modifying agent is added in Xiang Shangshu system, is reacted;
Step 3, after reaction, post-treated, obtain organic sepiolite.
(2) a kind of novel oil base drilling fluid organic sepiolite obtained using preparation method described in above-mentioned (1), it is described Organic sepiolite includes the component of following proportion:
10 parts by weight of sepiolite,
0.5~8 parts by weight of modifying agent, preferably 1.5~5 parts by weight,
Preferably, the modifying agent is quaternary ammonium salt cationic surfactant, preferably dodecyl trimethyl ammonium chloride, 14 Alkyl trimethyl ammonium chloride, hexadecyltrimethylammonium chloride, octadecyltrimethylammonium chloride, octadecyl dimethyl benzyl Any one or more in ammonium chloride, dioctadecyl dimethyl ammonium chloride;
It is highly preferred that the organic sepiolite 2 θ be 7.30 °, 19.71 °, 23.71 ° and 35.02 ° place presence (110), (060), (260) and (371) crystallographic plane diffraction peak;
Especially preferably, for 17 ° of sepiolite raw material, contact angle can increase to the organic sepiolite 100% or more, even up to 200%;Compared with the colloidity (only 2.0%) of sepiolite raw material, colloidity be can reach 100.0%;Apparent viscosity, plastic viscosity and shear force of the drilling fluid prepared by it at 150 DEG C can be respectively greater than 20.0mPa S, 18.0mPas and 2.0Pa, the thixotropic loop area at 66 DEG C, 150 DEG C, 180 DEG C and 200 DEG C are respectively greater than 1.5Pas-1、 23.0Pa·s-1、14.5Pa·s-1And 8.5Pas-1
(3) a kind of oil base drilling fluid includes organic sepiolite described in above-mentioned (2) in the oil base drilling fluid, described to have The concentration of organic sepiolite is 10~100g/L, preferably 20~50g/L.
A kind of novel oil base drilling fluid organic sepiolite provided according to the present invention and preparation method thereof has with following Beneficial effect:
1) in entire preparation method, using water as solvent, organic solvent is not introduced, it is at low cost, green safe;
2) sepiolite low in raw material price, be easy to get, use is safe, reduces production cost;
3) entire preparation method simple process, the solvent used is cheap, of less demanding to the production equipment used, It while easily operated, reduces costs, these factors are conducive to the popularization of industrialization;
4) the organic sepiolite lipophilicity that middle preparation method obtains through the invention is good, and contact angle is relative to sepiolite original For 17 ° of material, 100% or more, even up to 200% can be increased to;Its colloidity and sepiolite raw material (only 2.0%) phase Than can reach 100.0%;Apparent viscosity, plastic viscosity and shear force of the drilling fluid prepared by it at 150 DEG C can be respectively greater than 20.0mPas, 18.0mPas and 2.0Pa;Thixotropic loop area at 66 DEG C, 150 DEG C, 180 DEG C and 200 DEG C is respectively greater than 1.5Pa·s-1、23.0Pa·s-1、14.5Pa·s-1And 8.5Pas-1;Thus rheological property is excellent in oil base drilling fluid, mentions It glues, mention and cut significant effect, thixotropy is prominent, and high temperature resistant property is excellent, can use under the conditions of 200 DEG C.
Detailed description of the invention
Fig. 1 is the XRD spectra of the organic sepiolite prepared in Examples 1 to 3 in the present invention, and with sepiolite raw material XRD spectra is compared.
Specific embodiment
Present invention will now be described in detail, and the features and advantages of the invention will become more with these explanations It is clear, clear.
According to an aspect of the present invention, a kind of preparation method of novel oil base drilling fluid organic sepiolite is provided, including Following steps:
Step 1, sepiolite raw material is mixed with solvent;
Step 2, modifying agent is added in Xiang Shangshu system, is reacted;
Step 3, after reaction, post-treated, obtain organic sepiolite.
In step 1, sepiolite raw material is weighed in reaction kettle, and solvent, stirring is added.
In the present invention, the sepiolite is the sepiolite after purification, and the sepiolite that can be selected from originating from Hunan purifies to obtain, The purity of sepiolite raw material is about 20 (weight) % before purifying, and the purity of sepiolite raw material is greater than 70 (weight) % after purification.It mentions Sepiolite impurity after pure is few, and effective component is high, and the effect in oil base drilling fluid is more prominent.
It in the present invention, further include crushing the sepiolite raw material in step 1, sieving obtains sepiolite powder, preferably 200 meshes are crossed on ground, and the maximum particle diameter of sepiolite raw material is less than 75 microns after sieving.Pulverization process is carried out to sepiolite raw material, is increased Its big surface area, convenient for the dispersion of sepiolite raw material in a solvent.
In the present invention, the solvent is water, and sepiolite raw material can be formed in water by the mixed and disorderly dispersion of its fiber Network structure, i.e. step 1 are the aquation of sepiolite raw material.The mass concentration of sepiolite raw material is 15% (weight)~60 (weight Amount) %, preferably 25 (weight) %~50 (weight) %.The mass concentration of sepiolite raw material is lower than 15 (weight) %, water resource Consumption is big, production low efficiency;Mass concentration is higher than 60 (weight) %, and the time needed for fully dispersed and aquation is longer.
In the present invention, sepiolite raw material adjoint stirring in dispersion process, so that sepiolite raw material sufficiently connects with solvent Rate of dispersion is accelerated in touching, saves the operating time.Mixing time is less than 20min, sepiolite raw material it is dispersible in solvent, but not The abundant aquation of energy, influences subsequent reactions;Reaction time be greater than 3h, sepiolite raw material aquation is abundant, but the time is long, increase manpower and Equipment use cost, thus, select mixing time for 20min~3h, preferably 30min~2h.
In the present invention, sepiolite stock dispersion in a solvent when temperature be 10 DEG C~50 DEG C, as the temperature rises, Rate of dispersion is accelerated, however consumes energy and increase when high temperature, the high requirements on the equipment, increases production cost, thus determines that dispersion temperature is low In 50 DEG C.
In step (2), modifying agent is added in Xiang Shangshu system, is reacted.
In the present invention, the modifying agent be quaternary ammonium salt cationic surfactant, preferably dodecyl trimethyl ammonium chloride, Tetradecyl trimethyl ammonium chloride, hexadecyltrimethylammonium chloride, octadecyltrimethylammonium chloride, octadecyldimethyl Any one or more in benzyl ammonium chloride, dioctadecyl dimethyl ammonium chloride.
In addition to dioctadecyl dimethyl ammonium chloride, above-mentioned quaternary ammonium salt cationic surfactant is water-soluble at normal temperature, Dioctadecyl dimethyl ammonium chloride is dispersed in water under heating, on the sepiolite raw material after can be coupled to aquation in water, Since above-mentioned surfactant has long carbon chain structure, the organic modification of sepiolite raw material is realized, thus Hai Pao can be increased The dispersibility of stone in the oil.
In the present invention, the weight proportion of the sepiolite raw material and modifying agent be 10:0.5~10:8, preferably 10: 1.5~10:5.When the weight proportion of sepiolite raw material and modifying agent is less than 10:0.5, the modifying agent that sepiolite raw material is integrated to has Limit, dispersibility of the modified sepiolite in oil base drilling fluid be not good enough;When weight proportion is greater than 10:8, modifying agent is in sepiolite Adsorption saturation, on first layer modifying agent, polar end stretches out excessive modifying agent reverse adsorption, equally reduces organic Hai Pao The dispersibility of stone in the oil, and modifying agent consumption is big, it is at high cost, it is not suitable for industrialization production.
In the present invention, the mass concentration of the modifying agent in the reaction system is 2 (weight) %~15 (weight) %.Change Property agent concentration be lower than 2 (weight) % when, it is lower with the reaction rate that organises of sepiolite raw material;Concentration is higher than 15 (weight) % When, reaction rate is no longer significantly raised, and additional amount can exceed that aequum, causes modifying agent excessive, and performance decline, cost mentions It rises.
Modifying agent can be directly added into step 1 in sepiolite stock suspension, can also be dissolved in solvent II again into Row is added, and is preferably dissolved in being added again in solvent II, it is highly preferred that solvent used in the solvent II and step 1 It is identical.The modifying agent that dissolves in advance is added to be more convenient for contact of the sepiolite raw material with modifying agent, accelerates reaction speed.
It is mentioned in step 1, the mass concentration of sepiolite raw material is 15 (weight) %~60 (weight) %, preferably 25 (weights Amount) %~50 (weight) %.It is added in step 1 in sepiolite stock suspension if modifying agent is dissolved in solvent II, step 2 After middle modifying agent and solvent II are added, mass concentration of the sepiolite raw material in whole system is 5 (weight) %~60 (weight Amount) %, preferably 15 (weight) %~50 (weight) %.
In the present invention, with stirring during addition modifying agent.With the progress of stirring, modifying agent is dispersed in rapidly In reaction system, it is excessive to avoid local concentration, accelerates reaction and carries out.
In the present invention, the temperature of system is 10 DEG C~80 DEG C, preferably 15 DEG C~35 DEG C when modifying agent is added.Along with The addition of modifying agent, reaction starts to carry out, and in this lower temperature range, modifying agent addition is finished, and continues insulation reaction.This hair Reaction temperature described in bright is low, even if also achievable at normal temperature, substantially reduces to equipment requirement, has saved production cost, just It is used in large-scale promotion.
The inventors discovered that organic modification reaction carried out is not enough, body when the time of insulation reaction is less than 0.5h More free modifier raw material is still deposited in system, reduces the organic degree of product, while causing the waste of modifying agent.Heat preservation When the time of reaction is greater than 5h, product organic degree is no longer significantly improved, and takes a long time simultaneously, and improving people's force-summing device makes Use cost.Therefore, the present invention selects the reaction time for for 0.5~5h, preferably 1h~3h.
It is after reaction, post-treated in step (3), obtain organic sepiolite.
In the present invention, the organic sepiolite suspension in step 2 is post-processed, the post-processing includes solid-liquid point From the solid-liquid separation method is centrifugation or filtering, is preferably centrifuged.
Filter type is any one in natural filtration or pressure filtration, the preferably mode of pressure filtration, to reduce Filter the time.However, due in suspension sepiolite be threadiness, increase the difficulty of filtering, easily block filter cloth on filter opening, because And separative efficiency is higher by the way of centrifugation.
In the present invention, the post-processing further includes drying, and drying temperature is 60 DEG C~120 DEG C, and preferably 80 DEG C~105 ℃.Optionally, it is crushed after drying, crosses 200 meshes, the maximum particle diameter of product is less than 75 microns after crushing.
It is a further object of the present invention to provide a kind of organic sepiolites, are made according to above-mentioned method, organic sea Afrodite includes the component of following proportion:
10 parts by weight of sepiolite,
0.5~8 parts by weight of modifying agent, preferably 1.5~5 parts by weight,
Preferably, the modifying agent is quaternary ammonium salt cationic surfactant, preferably dodecyl trimethyl ammonium chloride, 14 Alkyl trimethyl ammonium chloride, hexadecyltrimethylammonium chloride, octadecyltrimethylammonium chloride, octadecyl dimethyl benzyl Any one or more in ammonium chloride, dioctadecyl dimethyl ammonium chloride, more preferable stearyl dimethyl benzyl ammonium chloride;
It is highly preferred that the organic sepiolite 2 θ be 7.30 °, 19.71 °, 23.71 ° and 35.02 ° exist (110), (060), (260) and (371) crystallographic plane diffraction peak;
Especially preferably, for 17 ° of contact angle of sepiolite raw material, contact angle can increase the organic sepiolite Add to 100% or more, even up to 200%;Colloid compared with sepiolite raw material colloidity (only 2%), in oily phase Rate can reach 100.0%;Apparent viscosity, plastic viscosity and shear force of the drilling fluid prepared by it at 150 DEG C can be respectively greater than 20mPas, 18mPas and 2Pa, the thixotropic loop area at 66 DEG C, 150 DEG C, 180 DEG C and 200 DEG C are respectively greater than 1.5Pa s-1、23.0Pa·s-1、14.5Pa·s-1And 8.5Pas-1
It is a further object of the present invention to provide a kind of oil base drilling fluid, have in the oil base drilling fluid including described above Organic sepiolite, wherein the concentration of organic sepiolite is 10~100g/L, preferably 20~50g/L in the oil base drilling fluid.
Apparent viscosity, plastic viscosity and shear force of this oil base drilling fluid at 150 DEG C can be respectively greater than 20mPas, 18mPas and 2Pa, the thixotropic loop area at 66 DEG C, 150 DEG C, 180 DEG C and 200 DEG C are respectively greater than 1.5Pas-1、 23.0Pa·s-1、14.5Pa·s-1And 8.5Pas-1, rheological property is excellent, mention it is viscous, mention and cut significant effect, thixotropy is prominent, Its high temperature resistant property is excellent, can meet the drilling well demand of 200 DEG C of hot conditions.
Embodiment
The present invention is further described below by way of specific example.But these examples are only exemplary, not to this The protection scope of invention constitutes any restrictions.
Embodiment 1
Step (1) weighs the sepiolite powder of 100g purification, is scattered in 100mL water, stirs 30min, obtains sepiolite point Dispersion liquid;
Step (2) weighs 25g octadecyltrimethylammonium chloride and is dissolved in 100mL water, is added in sepiolite dispersion liquid, Continue to stir 1h at 30 DEG C;
Suspension is centrifuged 5min by step (3) under the conditions of 4500rpm, separates organic sepiolite and supernatant liquid, and 80 DEG C Under the conditions of organic sepiolite is dried, crush, cross 200 meshes, obtain the powdered organic sepiolite product of yellowish-brown mobility, contain Water 2.8%.
Embodiment 2
Step (1) weighs the sepiolite powder of 100g purification, is scattered in 100mL water, stirs 1h, obtains sepiolite dispersion Liquid;
Step (2), weighs 35g stearyl dimethyl benzyl ammonium chloride, is added in sepiolite dispersion liquid, at 25 DEG C after Continuous stirring 1h;
Suspension is centrifuged 5min by step (3) under the conditions of 4500rpm, separates organic sepiolite and supernatant liquid, and 80 DEG C Under the conditions of organic sepiolite is dried, crush, cross 200 meshes, obtain the powdered organic sepiolite product of yellowish-brown mobility, contain Water 2.3%.
Embodiment 3
Step (1) weighs the sepiolite powder of 100g purification, is scattered in 300mL water, stirs 1h, obtains sepiolite dispersion Liquid;
Step (2) weighs 15g dioctadecyl dimethyl ammonium chloride and is scattered in 200mL water, and sepiolite dispersion liquid is added In, continue to stir 2h at 35 DEG C;
Suspension is centrifuged 5min by step (3) under the conditions of 4500rpm, separates organic sepiolite and supernatant liquid, and 80 DEG C Under the conditions of organic sepiolite is dried, crush, cross 200 meshes, obtain the powdered organic sepiolite product of yellowish-brown mobility, contain Water 1.8%.
Experimental example
X-ray diffraction experiment
Using German Bruker D8Advance type X-ray powder diffraction instrument (Cu target KαRay), in λ=0.15406nm, Sample is analyzed under the conditions of operating voltage 40kV, operating current 40mA in step width=0.02.
Contact angle test
Distillation is used by sample in the pressure lower sheeting 1min of 15MPa using upper marine morning JC200D contact angle measurement Water droplet is fallen in sample strip, records the contact angle of sample and water.
The preparation of oil base drilling fluid
12g organic sepiolite sample is weighed, is added in 400mL white oil, high-speed stirred 20min under the conditions of 10000rpm adds Enter in ageing can, is placed in aging 16h in 66 DEG C, 150 DEG C, 180 DEG C and 200 DEG C of heat rolling furnace, takes out, be cooled to 25 DEG C, High speed agitator 5min under the conditions of 10000rpm is tested after standing 5min.
Rheology testing
Using six fast viscosimeters of Qingdao Sen Xin mechanical & electronic equipment corporation, Ltd production.Apparent viscosity AV=1/2 θ600600For The reading of six fast viscosimeters under 600rpm revolving speed), plastic viscosity PV=θ600–θ300, yield value YP=1/2 (θ300-PV)。
Dynamic rheological property curve test
The HAAKE RV1 type rotary viscometer produced using U.S. Thermo Scientific, test program are as follows: 5min In in, shear rate is from 0~100s-1It gradually increases, immediately after from 100~0s-1It gradually decreases, time 5min, to dynamic Rheological curve is integrated, and the area of thixotropic loop is calculated.
Experimental example 1XRD analysis
In the present invention, organic sepiolite made from embodiment 1-3 is subjected to XRD test, as a result as shown in Figure 1.
As seen from Figure 1, the sepiolite raw material in embodiment 1, process is organically-modified, the crystalline substance of obtained organic sepiolite Body structure is (110), (060), (260) and (371) crystal face occur at 7.30 °, 19.71 °, 23.71 ° and 35.02 ° in 2 θ Diffraction maximum, it is essentially identical with sepiolite raw material through comparing, show that the crystal structure of sepiolite remains unchanged, mainly realizes pair The modification on sepiolite raw material surface.
The crystal structure of organic sepiolite and sepiolite raw material are essentially identical in embodiment 2 and embodiment 3, although showing to change Property agent it is different, but mainly realize the modification to sepiolite raw material surface.
2 contact angle test of experimental example
Contact angle test is carried out to the organic sepiolite prepared in Examples 1 to 3, to determine the hydrophobe of organic sepiolite Property.In embodiment 1, contact angle increases to 41 ° of organic sepiolite by 17 ° of sepiolite raw material;In embodiment 2, contact angle by 17 ° of sepiolite raw material increase to 43 ° of organic sepiolite;In embodiment 3, contact angle is increased to organic by 17 ° of sepiolite raw material 51 ° of sepiolite.
Have greatly by the contact angle of modified organic sepiolite compared to sepiolite raw material in Examples 1 to 3 It improving, for organic sepiolite for sepiolite raw material, contact angle can increase to 100% or more, even up to 200%, Illustrate the surface of solids of organic sepiolite have it is hydrophilic simultaneously, water increases the wetability difficulty of the surface of solids, solid Surface hydrophobic is greatly improved.
The analysis of 3 colloidity of experimental example
Organic sepiolite prepared by the sepiolite raw material of phase homogenous quantities and experimental example 1~3 is added in white oil, before modified Sepiolite raw material is distributed in white oil with graininess, poor with the compatibility of white oil, a large amount of to settle after standing for 24 hours;It is modified Organic sepiolite may be homogenously dispersed in white oil, form colloidal liquid, after standing for 24 hours, no sedimented particle.
The colloidity of sepiolite raw material before modified is only 2.0%, and the colloidity of organic sepiolite is in embodiment 1 100.0%, the colloidity of organic sepiolite is 100.0% in embodiment 2, and the colloidity of organic sepiolite is in embodiment 3 100.0%.
It follows that modified by surface, the polarity of organic sepiolite is reduced, and lipophilicity increases, and enhances organic Hai Pao Dispersibility of the stone in base oil (white oil).
The rheological property of 4 drilling fluid sample of experimental example
The rheological property for the drilling fluid sample that organic sepiolite in Examples 1 to 3 is prepared is tested, as a result such as table 1 It is shown.
The rheological property data of 1 drilling fluid sample of table
Q/SYZJG0022-2011 standard is index of the property of drilling fluid after 150 DEG C of aging 16h.
The drilling fluid sample that organic sepiolite is prepared in embodiment 1, at 150 DEG C, apparent viscosity, the plasticity of drilling fluid are viscous Degree and shear force respectively reach 24.0mPas, 21.0mPas and 3.0Pa, and apparently glue within the temperature range of 150 DEG C~200 DEG C Degree, plastic viscosity and shear force kept stable, are superior to China Petroleum Group Drilling Engineering Technology Research Institute company standard Q/ The performance index value of SYZJG0022-2011.
The drilling fluid sample that organic sepiolite is prepared in embodiment 2, at 150 DEG C, apparent viscosity, plastic viscosity and shear force Respectively reach 30.5mPas, 24.0mPas and 6.5Pa.In the range of 150 DEG C~200 DEG C, as the temperature rises, Though apparent viscosity and shear force have a degree of decline, performance is still substantially better than company standard Q/SYZJG0022-2011's Performance indicator.
The drilling fluid sample that organic sepiolite is prepared in embodiment 3, at 150 DEG C, apparent viscosity, plastic viscosity and shear force 23.0mPas, 18.0mPas and 5.0Pa are respectively reached.It, as the temperature rises, should within the scope of 150 DEG C~200 DEG C Though the viscosity and shear force of drilling fluid have faint decline, performance kept stable is still substantially better than company standard Q/ The performance indicator of SYZJG0022-2011 fully meets the application requirement of oil base drilling fluid at relatively high temperatures.
Therefore, apparent viscosity, plasticity of the drilling fluid sample that organic sepiolite is prepared in Examples 1 to 3 at 150 DEG C are viscous Degree and shear force can be respectively greater than 20mPas, 18mPas and 2Pa, fully meet the application of oil base drilling fluid at relatively high temperatures It is required that high temperature up to 200 DEG C even more than.
Further, rheological curve test is carried out to the drilling fluid sample that organic sepiolite in Examples 1 to 3 is prepared.
It is good that the dynamic rheological property curve graph for the drilling fluid that organic sepiolite is prepared in embodiment 1 shows that drilling fluid sample has Good thixotropy is stablized in 150 DEG C~200 DEG C of high temperature section viscosity and thixotropy.At 66 DEG C, 150 DEG C, 180 DEG C and 200 DEG C When thixotropic loop area be respectively 1.72Pas-1、23.48Pa·s-1、14.68Pa·s-1And 9.14Pas-1
The dynamic rheological property curve graph for the drilling fluid that organic sepiolite is prepared in embodiment 2 and embodiment 3 shows embodiment 2 Thixotropic loop area of the middle drilling fluid sample at 66 DEG C, 150 DEG C, 180 DEG C and 200 DEG C is respectively 12.52Pas-1、 68.08Pa·s-1、91.81Pa·s-1And 20.98Pas-1;In embodiment 3 drilling fluid sample at 66 DEG C, 150 DEG C, 180 DEG C and Thixotropic loop area at 200 DEG C is respectively 1.52Pas-1、37.35Pa·s-1、19.72Pa·s-1And 8.8Pas-1.Implement Drilling fluid sample has excellent thixotropy in example 2 and embodiment 3, in 150 DEG C~200 DEG C of high temperature section viscosity and thixotropy Stablize.
It can be seen from the above, the organic sepiolite of Examples 1 to 3 preparation, the touching at 66 DEG C, 150 DEG C, 180 DEG C and 200 DEG C Become anchor ring product and is respectively greater than 1.5Pas-1、23.0Pa·s-1、14.5Pa·s-1And 8.5Pas-1, as oil base drilling fluid Rheology control agent can meet the drilling well demand of 200 DEG C of hot conditions.
It is described the invention in detail above in conjunction with detailed description and exemplary example, but these explanations are simultaneously It is not considered as limiting the invention.It will be appreciated by those skilled in the art that without departing from the spirit and scope of the invention, Can be with various equivalent substitutions, modifications or improvements are made to the technical scheme of the invention and its embodiments, these each fall within the present invention In the range of.Scope of protection of the present invention is subject to the appended claims.

Claims (1)

1. a kind of preparation method of oil base drilling fluid organic sepiolite, comprising the following steps:
Step (1) weighs the sepiolite powder of 100g purification, is scattered in 100mL water, stirs 30min, obtains sepiolite dispersion Liquid;
Step (2) weighs 25g octadecyltrimethylammonium chloride and is dissolved in 100mL water, is added in sepiolite dispersion liquid, 30 Continue to stir 1h at DEG C;
Suspension is centrifuged under the conditions of 4500rpm 5min, separates organic sepiolite and supernatant liquid, 80 DEG C of conditions by step (3) It is lower to dry organic sepiolite, it crushes, crosses 200 meshes, obtain the powdered organic sepiolite product of yellowish-brown mobility, water content 2.8%.
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