CN108753267A - Drilling fluid and completion fluid anti-superhigh temperature anionic polymer fluid loss additive and preparation method thereof - Google Patents
Drilling fluid and completion fluid anti-superhigh temperature anionic polymer fluid loss additive and preparation method thereof Download PDFInfo
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- CN108753267A CN108753267A CN201810560677.9A CN201810560677A CN108753267A CN 108753267 A CN108753267 A CN 108753267A CN 201810560677 A CN201810560677 A CN 201810560677A CN 108753267 A CN108753267 A CN 108753267A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/38—Esters containing sulfur
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/38—Esters containing sulfur
- C08F220/385—Esters containing sulfur and containing nitrogen
Abstract
The present invention relates to drilling fluid and completion fluid anti-superhigh temperature anionic polymer fluid loss additives and preparation method thereof, the anti-superhigh temperature salt-resistant polymer fluid loss additive is by alkenyl monomer acrylamide, the terpolymer that strongly hydrophilic anion alkenyl monomer 2- acrylamide-2-methyl propane sulfonics and alkenyl monomer dimethylaminoethyl methacrylate are generated through aqueous solution polymerization reaction, molar ratio shared by anion alkenyl monomer 2- acrylamide-2-methyl propane sulfonics contained in its molecule chain element reaches 35%-42.5%, with extremely strong hydrophily and dissolubility, contain 1 in polymer molecular chain, 400-2, 000 structural unit, weight average molecular weight 650, 000-850, 000, number-average molecular weight 600, 000-700, 000.The fluid loss additive of the present invention has good dissolubility energy in superhigh temperature water base drilling fluid, temperature resistance ability is up to 248 DEG C, a small amount of be added just can significantly reduce the filter loss of water-base drilling fluid completion fluid under ultra-high temperature condition, and drilling fluid and completion fluid can be made to keep good colloidal stability under ultra-high temperature condition.
Description
Technical field:
The present invention relates to a kind of anti-superhigh temperature anionic polymer fluid loss additives and preparation method thereof, belong to oil and day
Drilling and completion fluids technical field in right gas drilling engineering, Earth resource exploration and exploitation and geothermal well drilling engineering.
Background technology:
As whole world oil and gas exploration and development is gradually to the expansion of Hydrocarbon Resource of The Deep Formation, the deep resource in China
The lasting propulsion of the great deep ground project such as exploration, Continental Scientific Drilling, Earth survey plan and geothermal energy resources
Exploration and development with utilize, superhigh temperature water base drilling fluid completion fluid technology already become such drilling project in core technology it
One.Currently, the widely used superhigh temperature water base drilling fluid completion fluid system in the whole world is mainly based on " sulphonated polymer mud ", wherein
Polymerization species product is a kind of indispensable superhigh temperature water base drilling fluid completion solution additive, and hydrophily is strong, has after aquation
Larger hydrodynamic volume can play the role of drilling fluid and completion fluid good colloid protecting action and filtrate reducing.But mesh
Before can resist 220 DEG C or more of the drilling fluid and completion fluid negligible amounts of polymerization species fluid loss additive, practical application at the scene
There is also certain deficiencies in the process, are mainly manifested in the anti-superhigh temperature (> 220 of now widely used polymer filtrate reducer
DEG C) filtrate loss controllability under performance is poor, anti-complex salt performance is insufficient and hyperthermal environments can be still undesirable etc. with shield colloidality.
In the past when researching and developing high-temperature resistant polymer fluid loss additive, the temperature resistance comonomer often selected needs to have more
Aquation group and adsorption group, thus having developed a batch has the multiple copolymer of certain heat-resisting property and anti-salt property,
Mainly think that the high molecular polymer with more aquation group and adsorption group can effectively make up under the high temperature conditions
High molecular polymer hydrating capacity reduces the decrease with high temperature adsorption characteristic caused by polymer high temperature dehydration.But by
The multiple copolymer prepared containing the comonomer of more aquation group and adsorption group still cannot meet when temperature is more than 220
DEG C when superhigh temperature water base drilling fluid completion fluid to the requirement of the technology of polymer treatment agent, main cause is still can not be by polymer
Inorganic agent is in temperature less than 220 DEG C of performances below and when the performance in the hyperthermal environments that temperature is more than 220 DEG C reaches coordination
It is unified, the physicochemical properties in water-base drilling fluid as the water of continuous phase under the conditions of superhigh-temperature and-pressure were especially ignored in the past
Change confrontation superhigh temperature polymer treatment agent directly or indirectly influence, lead to the polymer treatment agent under hyperthermal environments
Efficiency substantially reduces.
In multiple polymers mixed solution, under a certain steady temperature and pressure, the heat of multicomponent polymeric solution system
Mechanical equilibrium condition is front and back free enthalpy changes delta G≤0 of each polymer solution mixing.Due to mixed between high molecular polymer
Entropy very little is closed, so only when there are the repulsion between very strong interaction or component itself segment to be more than group between polymer
It, could be fully compatible when the repulsion of/segment.And it is thermodynamically incompatible between most polymers or only portion
Split-phase is held.In general, the relative molecular mass for participating in polymer in multicomponent polymeric solution is bigger, then more it is difficult to meet multicomponent
The thermodynamical equilibrium condition of polymer solution system, this new knowledge just demonstrate why high molecular polymer fluid loss additive exists
Dissolubility in water becomes indissoluble solution with the increase of relative molecular mass and from can dissolve, while being also able to verify that drilling fluid and completion fluid
Water-soluble inorganic agent is formed super due to crosslinked action caused by high temperature or Raolical polymerizable under high temperature or hyperthermal environments
The effect of macromolecular or build cross-linked polymer compound eventually lead to dissolubility variation, lose water soluble drilliong inorganic agent,
Even react on drilling fluid and completion fluid.In addition, the interaction of different high molecular polymer molecule interchains is to influence multicomponent
The important factor in order of polymer solution thermodynamic compatibility, the interaction between high molecular polymer macromolecular chain is bigger, such as
Hydrogen bond, the effect of strong dipole, ionization etc. are formed, then its compatibility is more preferable.Hydrogen bond action, interionic interaction, π-π
Intermolecular electric charge transfer is will produce when electron conjugated effect and polymer blended with electron rich group and short of electricity subbase group
Effect etc. can promote the compatibility of multicomponent macromolecule polymer solution.
Chinese patent document CN105733524A (application numbers:201610150092.0) disclose a kind of high temperature resistance, salt tolerant
Fluid loss additive and preparation method thereof.In terms of parts by weight, the raw material composition of the fluid loss additive includes 3-10 parts of acrylamide, 2-
15-25 parts of acrylamide-2-methyl propane sulfonic, 20-40 parts of sodium styrene sulfonate, 3-8 parts of maleic anhydride, sodium hydrate aqueous solution
220 parts of 27-52 parts, 3-6 parts of ammonium persulfate aqueous solution and pure water.The preparation method of the fluid loss additive includes:It is added into container pure
Water purification, acrylamide, 2- acrylamide-2-methyl propane sulfonics, sodium styrene sulfonate and maleic anhydride, hydroxide is added after dissolving
Sodium water solution and ammonium persulfate aqueous solution, isothermal reaction obtain fluid loss additive.The fluid loss additive can effectively reduce high temperature saturation
The filter loss of brine water base drilling fluid system, but when persulfate is as initiator, by sodium styrene sulfonate, maleic anhydride
When both reaction monomers and both monomer tools of acrylamide, 2- acrylamide-2-methyl propane sulfonics, due to each reaction
The dramatically different of monomer reactivity ratio will cause the variation of product property with the variation of reaction process and otherness is larger, meanwhile, such as
The activity of the maleic anhydride comonomer similar with sodium styrene sulfonate etc. is not high, thus causes the conversion ratio of reaction monomers not
Height further causes field application temperature of its product in drilling fluid and completion fluid to be generally below to influence product property
220℃。
Chinese patent document CN104388061A (application numbers:201410513354.6) disclose a kind of water-base drilling fluid use
High-temperature resisting and salt-resisting polymer filtrate reducer and preparation method thereof, the component and proportioning of the fluid loss additive are N- ethylene in parts by weight
8~39 parts of base caprolactam, 20~100 parts of 2- acrylamide-2-methylpro panesulfonic acids, 20~50 parts of acrylic acid, N, N-2 methyl
10~45 parts of acrylamide, 100~200 parts of water;Specific preparation method is to neutralize acid monomer with sodium hydroxide, control system
PH value adds non-ionic monomer and stirs to dissolving 7.0~11.0, using oxidation-reduction trigger system as initiator, is dividing
Aqueous solution polymerization is carried out in the presence of son amount conditioning agent to form, reaction temperature is 25~60 DEG C, and the reaction time is 4~6h, is obtained
Gum-like product drying, crush after obtain polymer filtrate reducer.The fluid loss additive can effectively be promoted in deep-well, ultradeep well
After drilling fluid temperature resistance, salt resistance, high temperature ageing the problems such as viscosity retention ratio.But the catalyst used in the patent document is still
It is oxidation-reduction trigger system traditionally, the efficiency of initiation of the initiation system is relatively low, and required initiation temperature is higher, reaction
It is unfavorable for being effectively controlled to the relative molecular mass of product again in the process, for the alkenyl for being prone to polymerisation
" sudden and violent poly- " phenomenon then easily occurs for reaction monomers, meanwhile, it is the time required to reaction or relatively long, and or the reaction time it is extremely short;Separately
Outside, the product synthesized using the initiation system is influenced generally drop in high temperature and high pressure environment by subcritical water change of properties
The filter loss of low drilling fluid 50-80%.
Invention content:
In view of the deficiencies of the prior art, the present invention, which provides one kind, can resist superhigh temperature (being more than 248 DEG C), saline-alkaline tolerance strong,
Strong to the shield glue ability of water-base drilling fluid completion fluid under superhigh-temperature and-pressure environment, filtrate reducing effect is good, with other inorganic agent compatibilities
Property it is good, while have concurrently inhibit deep layer complexity shale hydration peptizaiton polymer filtrate reducer.
Technical scheme is as follows:
The anti-superhigh temperature anionic polymer fluid loss additive of a kind of drilling fluid and completion fluid, with the structure described in formula (I):
The fluid loss additive is by alkenyl reaction monomers acrylamide, strongly hydrophilic anion alkenyl monomer 2- acrylamides-
The terpolymer that 2- methyl propane sulfonic acids and alkenyl monomer dimethylaminoethyl methacrylate are generated through aqueous solution polymerization reaction;
In formula (I), x, y and z respectively represent acrylamide, 2- acrylamide -2- methyl-propanesulfonic acids and methacrylic acid two
The molal quantity of methylamino ethyl ester, molar ratio x ﹕ y ﹕ z=(4.75-5.25) ﹕ (3.5-4.25) ﹕ (1.0-3.0).
, according to the invention it is preferred to, anion alkenyl monomer 2- third contained in the fluid loss additive molecule chain element
Molar ratio shared by acrylamide -2- methyl propane sulfonic acids is 35%-42.5%, has extremely strong hydrophily and dissolubility;
Preferably, Isosorbide-5-Nitrae 00-2,000 structural unit, weight average molecular weight 650,000- are contained in fluid loss additive strand
850,000, number-average molecular weight 600,000-700,000.
, according to the invention it is preferred to, 1,600-1,700 structural units are contained in the fluid loss additive strand, are rubbed
You are than x ﹕ y ﹕ z=(4.95-5.05) ﹕ (3.75-4.05) ﹕ (1.0-1.5);For weight average molecular weight 690,000-740,000, number is equal
Molecular weight is in 620,000-650,000.
According to the present invention, the preparation side of the anti-superhigh temperature anionic polymer fluid loss additive of above-mentioned drilling fluid and completion fluid
Method, including steps are as follows:
Reactant acrylamide, 2- acrylamide-2-methyl propane sulfonics and dimethylaminoethyl methacrylate are dissolved
In a solvent, it is fitted into reaction kettle, with the concentration of solvent adjustment reactant mixed liquor, pH is adjusted with alkali, catalyst, heating is added
Mixed liquor in reaction kettle maintains the reaction time, reaction is terminated, through drying, crushing, sieving to get anti-superhigh temperature anionic
Polymer filtrate reducer.
, according to the invention it is preferred to, the solvent is water;
Preferably, the catalyst is two NSC 18620 oxazoline hydrochloride of azo, azo diisobutyl amidine hydrochloride, azo
One or both of dicyano valeric acid or azo dicyclohexyl formonitrile HCN combine;
Preferably, the alkali is sodium hydroxide or potassium hydroxide;
Preferably, pH value is adjusted to 5-9, further preferably 6.5-7.5.
, according to the invention it is preferred to, reactant monomer total weight accounts for the 8- for the total solution weight that reactant is formed with solvent
20wt%, further preferably 12-16wt%;
Preferably, the weight of required catalyst accounts for the 0.05-0.5wt% of reactant total weight, further preferably 0.15-
0.30wt%;
Preferably, reaction temperature is 35-80 DEG C, further preferably 40-60 DEG C;
Preferably, the reaction time is -8 hours 2 hours, further preferably -4.5 hours 3.5 hours;
Preferably, drying temperature is 105-345 DEG C;
Preferably, the rear fine particulate product granularity that pulverizes and sieves is 10-40 mesh, further preferably 20-40 mesh;Fine grained
The granularity of product is 0.9mm sieve pore screen over-sizes < 15%;The contents on dry basis > 90% of fine grained product.
The present invention is the solubility property and compatibility for improving polymer filtrate reducer under hyperthermal environments, and creative is logical
Cross molecular structure optimization design, the excellent alkenyl reaction monomers 2- of optimum option alkenyl reaction monomers acrylamide, anti-salt property
Acrylamide-2-methyl propane sulfonic and novel alkenyl polymerization reaction monomer methyl-prop with multiple methyl, methylene and ester group
Olefin(e) acid dimethylaminoethyl.Meanwhile in polymerization catalyzed method, optimum option new type water-solubility azo-initiator is as reaction
Catalyst, obtain a kind of anti-superhigh temperature salt-resistant polymer fluid loss additive of New drilling fluid completion fluid, the polymer filtrate reducing
Agent can enable its its molecule interchain under hyperthermal environments to pass through interionic by carrying part hydrophobic grouping by itself
Or intermolecular interaction etc. forms associative structure, and it is molten under superhigh-temperature and-pressure environment to significantly increase high molecular polymer
Xie Xing enhances its function and effect under hyperthermal environments, and more conventional drilling fluid and completion fluid polymer filtrate reducer is super
Colloid protecting action and filtrate reducing effect under high temperature and high pressure environment is more excellent.
The reaction process of the present invention is as follows:
The present invention anti-superhigh temperature anionic polymer fluid loss additive the mechanism of action and have the beneficial effect that:
(1) viscosifying mechanisms, after a small amount of polymer filtrate reducer is added, the viscosity of water-base drilling fluid completion fluid will obviously rise
Height, the viscosity conservation rate of drilling fluid and completion fluid is relatively high after high temperature ageing, that is, improves the filtrate viscosity of drilling fluid and completion fluid,
Fine and close mud cake can be formed again, to reduce filter loss.
(2) under hot environment, the sulfonic group in polymer filtrate reducer strand can be adsorbed on clay particle surface and be formed
Thicker hydration shell reduces the content of Free water, to enhance the thermal stability of drilling fluid.
(3) polymer filtrate reducer with higher relative molecular mass can effectively be coated with drilling cuttings, be bored to reduce
The aquation dispersibility of bits.
(4) the more methyl and methylene energy contained in dimethylaminoethyl methacrylate chain link in polymer molecular chain
Enough make it that there is good compatibility under superhigh-temperature and-pressure environment.
(5) fluid loss additive of the invention has good dissolubility energy in superhigh temperature water base drilling fluid, and other water base
The compatibility of drilling fluid and completion fluid inorganic agent is good, and temperature resistance ability is up to 248 DEG C, and can be significantly reduced under ultra-high temperature condition water base
The filter loss of drilling fluid and completion fluid, while good shield colloidality energy can be kept under ultra-high temperature condition again.
Description of the drawings:
Fig. 1 is the anti-superhigh temperature anionic polymer fluid loss additive of drilling fluid and completion fluid made from the embodiment of the present invention 1
Infrared spectrum characteristic spectrum.
Specific implementation mode:
Below by specific embodiment, the present invention will be further described, but not limited to this.
In embodiment unless otherwise specified, raw materials used is regular market purchase product.
Polymer filtrate reducer in embodiment, with the structure described in formula (I):
The fluid loss additive is by alkenyl reaction monomers acrylamide, strongly hydrophilic anion alkenyl monomer 2- acrylamides-
The terpolymer that 2- methyl propane sulfonic acids and alkenyl monomer dimethylaminoethyl methacrylate are generated through aqueous solution polymerization reaction;
In formula (I), x, y and z respectively represent acrylamide, 2- acrylamide -2- methyl-propanesulfonic acids and methacrylic acid two
The molal quantity of methylamino ethyl ester.
Embodiment 1:
It is 2.5 to the capacity equipped with blender, reflux condenser, nitrogen protection device, temperature sensor and heating device
64.8 grams of acrylamide and 43.0 grams of dimethylaminoethyl methacrylate are weighed respectively in the reaction kettle risen, pour into reaction
In kettle, 500 milliliters of tap water are added, high-speed stirred makes it dissolve fully;Weigh 132.2 grams of 2- acrylamide -2- methyl-props
Sulfonic acid is dissolved in 300 milliliters of tap water, is then used the NaOH solution of 10-14 mol/Ls to adjust pH to 7, is poured into reaction kettle;
The reactant mixed liquor being sufficiently stirred in reaction kettle.It weighs 0.72 gram of azo diisobutyl amidine hydrochloride and is dissolved in 100 milliliters
In tap water, stirring, which is completely dissolved, to be placed in reaction kettle;For supplement tap water dosage to 1600 milliliters, control is anti-in a kettle
It is 15% to answer object total concentration, the solution in quick stirred autoclave 5 minutes.High-speed stirred rises after 30 minutes under the protection of nitrogen
Temperature to 55 DEG C, take out the jelly in reaction kettle, be placed in 105 DEG C of vacuum drying ovens and dry 8 by 4 hours postcoolings of reaction to room temperature
Hour, it then crushes, crosses 20 mesh sieve to get anti-superhigh temperature anionic polymer fluid loss additive of the present invention.
3.5 ﹕ 1.5 of molar ratio x ﹕ y ﹕ z=5.0 ﹕ of each reaction monomers, the weight average molecular weight of polymer are about in this polymer
73.4 ten thousand, number-average molecular weight is about 64.6 ten thousand, and structural unit number is about 1680.
Embodiment 2:
It it is 3-3.5 tons to the capacity equipped with blender, reflux condenser, nitrogen protection device, thermometer and heating device
The corrosion-resistant reaction kettle of stainless steel in be first added 1000 kilograms of tap water, turn on agitator is added with 25 kg/min of rate
2- acrylamide -2- methyl-propanesulfonic acids are 211.8kg, are stirred 10 minutes, and it is solid that sodium hydroxide is added with 5 kg/min of rate
Body, adjusting pH value are 7-7.5, tap water are added in a kettle to 1500 kilograms, control temperature is less than 40 DEG C;With 25 kilograms/
It is 96.3 kilograms that acrylamide, which is added, in the rate of minute, and 500 kilograms of tap water is added, and is stirred 10 minutes;Add 53.2 kilograms
Dimethylaminoethyl methacrylate, stir 5 minutes;The azo diisobutyl amidine hydrochloride for weighing 1.038 kilograms, is dissolved in
In 25 kilograms of tap water, pour into reaction kettle.Continue that tap water to tap water total weight is added in a kettle to be 2400kg,
Logical nitrogen, stirring are warming up to 55-58 DEG C after 30 minutes, 4 hours postcoolings of reaction to room temperature take out the jelly in reaction kettle,
(spray drying process) is dried through drying equipment, then crushed 20 mesh sieve to get anti-superhigh temperature anion of the present invention
Type polymer filtrate reducer.
3.75 ﹕ 1.25 of molar ratio x ﹕ y ﹕ z=5.0 ﹕ of each reaction monomers in this polymer, the weight average molecular weight of polymer is about
It is 72.4 ten thousand, number-average molecular weight is about 62.6 ten thousand, and structural unit number is about 1640.
Comparative example 1:
Amide groups in acrylamide has very strong suction-operated to clay mineral, thus it is poly- to be commonly used as synthesis
One of the critical functionality monomer of object fluid loss additive is closed, however hydrolysis easily occurs under the high temperature conditions for amide groups, generates carboxylic
Base affects the filtrate reducing effect of fluid loss additive, traditionally the polymer drop containing acrylamide chain link in polymer molecular chain
Its temperature resistance ability of fluid loss agents is generally less than 180 DEG C.However, when acrylamide and dimethylaminoethyl second in the present invention
When ester and other anion alkenyl reaction monomers are copolymerized, the laboratory test results of products therefrom show to contain propylene in strand
Its heat-resisting property of the polymer of amide monomer is significantly improved.For this purpose, during synthesizing the fluid loss additive, x ﹕ are set
Y=5.0 ﹕ 3.75, control other Variable Conditions it is constant under conditions of, by change dimethylaminoethyl methacrylate polymerizeing
Shared molar ratio in object, synthesis comparative example 1-1 (dimethylaminoethyl methacrylate chain element is free of in product),
Comparative example 1-2 (mole accounting of dimethylaminoethyl methacrylate is 0.5 in product), comparative example 1-3 (products
Mole accounting of middle dimethylaminoethyl methacrylate be 0.75), comparative example 1-4 (dimethylaminoethyl acrylate methyls in product
Mole accounting of amino ethyl ester be 1.0), comparative example 1-5 (mole accountings of dimethylaminoethyl methacrylate in product
For 1.25).
The water base slurry of saturated salt is prepared:Stir in cup addition 400mL tap water in height, under 8000 revs/min of mixing speeds according to
Secondary addition 0.8g natrium carbonicum calcinatums and 16g drilling fluids two level bentonite stir 2 hours, and closed standing 24 was as a child added afterwards
NaCl is stirred evenly to saturated concentration to get the water base slurry of saturated salt.
Test the preparation and test of slurry:1.5% comparative example is added into the water base slurry of saturated salt respectively, 8000 turns/
High-speed stirred is uniform under the mixing speed of minute, surveys the rheological characteristic and leak-off of each experiment slurry.Experiment is starched and is packed into high temperature ageing
Tank, heat rolling aging 16 hours under 180 DEG C of environment, the rheological characteristic and leak-off of each experiment slurry is tested with same method, as a result
As shown in table 1.
Test result of the table 1 in the water base slurry of saturated salt
Comparative example 2:
It is poly- with this is compared shared by acrylamide and anionic monomer 2- acrylamide -2- methyl-propanesulfonic acids in the present invention
The influence for closing the high-temperature resisting and salt-resisting effect of object fluid loss additive is more notable.When acrylamide and 2- acrylamide -2- the-the third sulphurs of methyl
When the molar ratio of acid is excessive, the heat and salinity tolerance filtrate loss controllability of products therefrom is undesirable;When acrylamide and 2- acrylamides-
When the molar ratio of 2- methyl-propanesulfonic acids is too small, the heat and salinity tolerance filtrate loss controllability of products therefrom is also undesirable.For this purpose, synthesizing
During the fluid loss additive, mole accounting of dimethylaminoethyl methacrylate is set as 1.25, controls other variable items
Under conditions of part is constant, by changing matching shared by acrylamide and anionic monomer 2- acrylamide -2- methyl-propanesulfonic acids
Than, synthesis comparative example 2-1 (x ﹕ y=5.0 ﹕ 3.75 in product), comparative example 2-2 (x ﹕ y=6.0 ﹕ 3.75 in product),
Comparative example 2-3 (x ﹕ y=7.0 ﹕ 3.75 in product), comparative example 2-4 (x ﹕ y=5.0 ﹕ 4.75 in product), comparative example
Sample 2-5 (x ﹕ y=5.0 ﹕ 5.75 in product).
It is consistent described in the preparation method of the water base slurry of saturated salt, the preparation of experiment slurry and test method and comparative example 1, as a result such as
Shown in table 2.
Test result of the table 2 in the water base slurry of saturated salt
The heat and salinity tolerance performance and filtrate loss controllability of Inventive polymers fluid loss additive are commented below by test example
Valence.
Test method in test example:①GB/T 32198-2015:IR spectrum quantitative analysis technology general rule;2. using GB/
T16738-1997:Water-base drilling fluid On-Site Test Procedure.
Test example 1:To the infrared spectrum point of anti-superhigh temperature anionic polymer fluid loss additive described in the embodiment of the present invention 1
Analysis.
Using Fourier Transform Infrared Spectrometer, anti-superhigh temperature anionic polymer has been measured by pellet technique
The infrared spectrum characteristic spectrum of fluid loss additive, as shown in Figure 1.
Test example 2:The relative molecular mass of anti-superhigh temperature anionic polymer fluid loss additive described in testing example 1.
Using gel permeation chromatograph, analysis has obtained the average molecular of anti-superhigh temperature anionic polymer fluid loss additive
Quality, as shown in table 3.
The relative molecular mass of 3 embodiment of table, 1 sample is analyzed
Test example 3:Inhibit the test of shale hydration dispersion performance
A concentration of 0.5% 2 sample aqueous solution of embodiment, the 0.5% anti-height of import polymer for drilling fluid are made respectively
Warm salt resistant filter loss reduction agent Driscal D aqueous solutions, 0.5% drilling fluid polyacrylamide sylvite KPAM aqueous solutions, 0.5%
Drilling fluid amphoteric ion polymer tackifier 80A51 aqueous solutions select deep bad ground mud shale rock sample to carry out mud shale
Dispersion experiment is rolled, the results are shown in Table 4.
Table 4 inhibits shale hydration dispersion test results
Title | The rate of recovery/% |
Tap water | 47.3 |
0.5% embodiment, 2 sample | 81.7 |
0.5%Driscal D | 70.1 |
0.5%KPAM | 56.8 |
0.5%80A51 | 66.0 |
Test example 4:It is tested in fresh water-based slurry
Base slurry is prepared:Addition 400mL tap water in cup is stirred in height, is sequentially added under 8000 revs/min of mixing speeds
0.8g natrium carbonicum calcinatums and 16g drilling fluids two level bentonite stir 2 hours, and 24 hours as prehydrations of closed standing are good
Fresh water-based slurry.
Test the preparation and test of slurry:0.3% evaluation sample (embodiment is added into the good fresh water-based slurry of prehydration respectively
2 samples, Driscal D), high-speed stirred is uniform under 8000 revs/min of mixing speed, with Brookfield DV-2 rheometers
Test the apparent viscosity of each experiment slurry at different temperatures;Experiment is starched and is packed into high temperature ageing tank, heat rolling is old under 180 DEG C of environment
Change 16 hours, tests each experiment slurry in 20 DEG C of leak-off, the results are shown in Table 5.
Test result of the table 5 in fresh water-based slurry
Test example 5:It is tested in brine mud
Brine mud is prepared:Addition 400mL tap water in cup is stirred in height, is added successively under 8000 revs/min of mixing speeds
Enter 0.8g natrium carbonicum calcinatums and 16g drilling fluid two level bentonites, stir 2 hours, closed standing 24 is as a child added 4% afterwards
NaCl stirs 20 minutes to get brine mud.
Test the preparation and test of slurry:Respectively into brine mud be added 1.5% evaluation sample (2 sample of embodiment,
Driscal D), high-speed stirred is uniform under 8000 revs/min of mixing speed, surveys the rheological characteristic and leak-off of each experiment slurry.
Experiment is starched and is packed into high temperature ageing tank, each experiment slurry is tested in heat rolling aging 16 hours under 180 DEG C of environment with same method
Rheological characteristic and leak-off, the results are shown in Table 6.
Test result of the table 6 in brine mud
Test example 6:It is tested in the water base slurry of saturated salt
The preparation method that the water base slurry of saturated salt is prepared is as described in comparative example 1.
Test the preparation and test of slurry:Respectively into the water base slurry of saturated salt be added 1.5% evaluation sample (2 sample of embodiment,
DriscalD), high-speed stirred is uniform under 8000 revs/min of mixing speed, surveys the rheological characteristic and leak-off of each experiment slurry.It will
Experiment slurry is packed into high temperature ageing tank, and heat rolling aging 16 hours under 180 DEG C of environment test the stream of each experiment slurry with same method
Denaturation and leak-off, the results are shown in Table 7.
Test result of the table 7 in the water base slurry of saturated salt
Test example 7:Test in superhigh temperature water base drilling fluid completion fluid
The preparation of superhigh temperature water base drilling fluid completion liquid-based slurry:400mL fresh water-based slurrys are measured, in 8000 revs/min of height
High-speed stirred 20 minutes on fast blender, then sequentially add 0.3-0.5 parts of sodium hydroxides, 0.3-1 parts of anti-superhigh temperature resist it is compound
The amphoteric ion hydrophobic associated polymer fluid loss additive of salt, 3-5 parts of II types of sulfonated-pheno-formoldehyde resin, 3-5 parts of sulfonated lignite resins,
2-4 parts of sulfonated gilsonite powder, 1-2 parts of modified graphites, 1-2 parts of polymeric alcohols, 3-5 parts of high temperature resistance sealing agents, 20-50 grammes per square metre spar, often
High-speed stirred 20 minutes after a kind of inorganic agent are added, it is complete superhigh temperature water base drilling fluid of the present invention can be made according to the above method
Well liquid base is starched, density 1.10-1.30g/cm3。
Test method:Superhigh temperature water base drilling fluid completion liquid-based is taken to starch 400mL, under 8000 revs/min of mixing speed
High-speed stirred is uniform, and 0.5-1 parts of 2 samples of embodiment are added, and high-speed stirred 20 minutes is to get superhigh temperature water base drilling fluid completion fluid
System surveys the rheological characteristic and leak-off of experiment slurry.Experiment is starched and is packed into high temperature ageing tank, the heat rolling in 248 DEG C of high temp roller furnaces
The rheological characteristic and leak-off of experiment slurry are tested in aging 16 hours with same method, and the results are shown in Table 8.
Test result of the table 8 in superhigh temperature water base drilling fluid completion fluid
Note:No. 1 is formulated as the superhigh temperature water base drilling fluid completion fluid system of embodiment sample is added, and No. 2 formulas are not add
Enter the superhigh temperature water base drilling fluid completion liquid-based slurry of embodiment sample, the test condition of HTHP filter losses is 180 DEG C/3.5MPa.
Test example 8:Test in superhigh temperature ultrahigh-density water-base drilling fluid completion fluid
The preparation of low solid phase fresh water-based slurry:Addition 400mL tap water in cup is stirred in height, in 8000 revs/min of mixing speeds
Under sequentially add 0.3-0.5g natrium carbonicum calcinatums and 6-10g drilling fluid two level bentonites, stir 2 hours, closed to stand 24 small
When the as good low solid phase fresh water-based slurry of prehydration.
The preparation of superhigh temperature ultrahigh-density water-base drilling fluid completion liquid-based slurry:The low solid phase fresh water-based slurrys of 400mL are measured,
Then high-speed stirred 20 minutes on 8000 revs/min of homogenizer sequentially add the 0.1-0.5 parts of anti-anti- complex salts of superhigh temperature
Amphoteric ion hydrophobic associated polymer fluid loss additive, 2-4 parts of I types of sulfonated-pheno-formoldehyde resin, 3-8 parts of sulfonated lignite resins, 2-9
Part sulfonated gilsonite powder, 3-7 parts of potassium chloride, 900-1000 grams of compound heavy weight additive (Iron Ore Powder and barite mass ratio 2:1 compounding), often
High-speed stirred 20-30 minutes after a kind of inorganic agent are added, superhigh temperature ultra high density of the present invention can be made according to the above method
Water-base drilling fluid completion liquid-based is starched, density 2.40-2.55g/cm3。
Test method:Superhigh temperature ultrahigh-density water-base drilling fluid completion liquid-based is taken to starch 400mL, in 8000 revs/min stir
It is uniform to mix high-speed stirred under speed, 0.1-0.3 parts of 2 samples of embodiment are added, high-speed stirred 30 minutes is to get superhigh temperature ultra high density
Water-base drilling fluid completion fluid system surveys the rheological characteristic and leak-off of experiment slurry.Experiment is starched and is packed into high temperature ageing tank, 240
Heat rolling aging 16 hours, the rheological characteristic and leak-off of experiment slurry are tested with same method, as a result such as in DEG C high temp roller furnace
Shown in table 9.
Test result of the table 9 in superhigh temperature ultrahigh-density water-base drilling fluid completion fluid
Note:For the superhigh temperature ultrahigh-density water-base drilling fluid completion fluid system of 2 sample of embodiment is added, No. 2 are matched No. 1 formula
The superhigh temperature ultrahigh-density water-base drilling fluid completion liquid-based slurry of 2 sample of embodiment, the test-strips of HTHP filter losses are added in Fang Weiwei
Part is 180 DEG C/3.5MPa.
Interpretation of result:
Show anti-superhigh temperature anionic polymer fluid loss additive of the present invention from the test result of test example 1 to 2
It is by three kinds of acrylamide, 2- acrylamide-2-methyl propane sulfonics and alkenyl monomer dimethylaminoethyl methacrylate alkenyls
Monomer occurs polymerisation and generates, and weight average molecular weight is about 730,000 or so, and number-average molecular weight is about 640,000 or so.
Show anti-superhigh temperature anionic polymer fluid loss additive tool of the present invention from the test result of test example 3
There is the performance of good inhibition shale hydration dispersion.
Show anti-superhigh temperature anionic polymer fluid loss additive of the present invention from the test result of test example 4 to 6
Thickening property in drilling fluid and completion fluid is slightly less than the thickening property of contrast product Driscal D, meanwhile, in fresh water-based
Good high-temperature resisting and salt-resisting filtrate loss controllability is all had in slurry, brine mud and the water base slurry of saturated salt.
Show from the test result of test example 7 to 8 water base in superhigh temperature water base drilling fluid system and superhigh temperature ultra high density
The stream of drilling fluid and completion fluid after anti-superhigh temperature anionic polymer fluid loss additive of the present invention is added in drilling fluid system
Become performance and filtration property to stablize, the heat-resisting property of drilling fluid and completion fluid system can be made at least to improve to 248 DEG C, meanwhile, again
The middle filter pressing loss of superhigh temperature water base drilling fluid completion fluid and superhigh temperature ultrahigh-density water-base drilling fluid completion fluid can be controlled
Within 5mL, high temperature and high pressure filter loss controls within 20mL.
The test result of compbined test example 1 to 8 shows anti-superhigh temperature anionic polymer filtrate reducing of the present invention
Agent have good heat-resisting property, the heat-resisting property in drilling fluid and completion fluid system up to 248 DEG C, while its also have it is good
Salt resistance filtrate loss controllability.
Claims (10)
1. a kind of anti-superhigh temperature anionic polymer fluid loss additive of drilling fluid and completion fluid, which is characterized in that the fluid loss additive
With the structure described in formula (I):
The fluid loss additive is by alkenyl reaction monomers acrylamide, strongly hydrophilic anion alkenyl monomer 2- acrylamide -2- first
The terpolymer that base propane sulfonic acid and alkenyl monomer dimethylaminoethyl methacrylate are generated through aqueous solution polymerization reaction;
In formula (I), x, y and z respectively represent acrylamide, 2- acrylamide -2- methyl-propanesulfonic acids and dimethylaminoethyl acrylate methyl ammonia
The molal quantity of base ethyl ester, molar ratio x ﹕ y ﹕ z=(4.75-5.25) ﹕ (3.5-4.25) ﹕ (1.0-3.0).
2. anti-superhigh temperature anionic polymer fluid loss additive according to claim 1, which is characterized in that the drop filter
It is 35%- to lose molar ratio shared by anion alkenyl monomer 2- acrylamide-2-methyl propane sulfonics contained in agent molecule chain element
42.5%,
Contain Isosorbide-5-Nitrae 00-2 in fluid loss additive strand, 000 structural unit, weight average molecular weight 650,000-850,000, number is
Molecular weight 600,000-700,000.
3. anti-superhigh temperature anionic polymer fluid loss additive according to claim 1, which is characterized in that the drop filter
It loses in agent molecule chain and contains 1,600-1,700 structural units, molar ratio x ﹕ y ﹕ z=(4.95-5.05) ﹕ (3.75-4.05) ﹕
(1.0-1.5);Weight average molecular weight is 690,000-740,000, and number-average molecular weight is 620,000-650,000.
4. claim 1-3 any one of them drilling fluid and completion fluid system of anti-superhigh temperature anionic polymer fluid loss additive
Preparation Method, including steps are as follows:
Reactant acrylamide, 2- acrylamide-2-methyl propane sulfonics and dimethylaminoethyl methacrylate are dissolved in molten
It in agent, is fitted into reaction kettle, with the concentration of solvent adjustment reactant mixed liquor, pH is adjusted with alkali, catalyst, heating reaction is added
Mixed liquor in kettle maintains the reaction time, reaction is terminated, through drying, crushing, sieving to get anti-superhigh temperature anionic polymerization
Object fluid loss additive.
5. preparation method according to claim 4, which is characterized in that the solvent is water;
The catalyst is two NSC 18620 oxazoline hydrochloride of azo, azo diisobutyl amidine hydrochloride, azo dicyano valeric acid
Or one or both of azo dicyclohexyl formonitrile HCN combination;
The alkali is sodium hydroxide or potassium hydroxide.
6. preparation method according to claim 4, which is characterized in that pH value is adjusted to 5-9, preferably 6.5-7.5.
7. preparation method according to claim 4, which is characterized in that reactant monomer total weight accounts for reactant and solvent shape
At total solution weight 8-20wt%, preferably 12-16wt%.
8. preparation method according to claim 4, which is characterized in that the weight of required catalyst accounts for reactant total weight
0.05-0.5wt%, preferably 0.15-0.30wt%.
9. preparation method according to claim 4, which is characterized in that reaction temperature is 35-80 DEG C, preferably 40-60 DEG C;
Reaction time is -8 hours 2 hours, preferably -4.5 hours 3.5 hours.
10. preparation method according to claim 4, which is characterized in that drying temperature is 105-135 DEG C;
The rear fine particulate product granularity that pulverizes and sieves is 10-40 mesh;The granularity of fine grained product is 0.9mm sieve pore screen over-sizes <
15%;The contents on dry basis > 90% of fine grained product.
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