CN106432632A - Amido polymer filtrate loss reducer for water-based drilling fluid resistant to high temperature, salt and calcium and preparation method and application thereof - Google Patents
Amido polymer filtrate loss reducer for water-based drilling fluid resistant to high temperature, salt and calcium and preparation method and application thereof Download PDFInfo
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- C09K8/02—Well-drilling compositions
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Abstract
The invention provides an amido polymer filtrate loss reducer for water-based drilling fluid resistant to high temperature, salt and calcium and a preparation method and application thereof. The filtrate loss reducer is prepared from acrylamide, 2-acrylamido-2-methyl propanesulfonate, allyl polyethylene glycol and ammonium triethoxylallylbromide, wherein the molar ratio of the four monomers is (8.1-20.2):(9-15.2):(2.1-4.3):(8-10). The filtrate loss reducer can be effectively adsorbed on clay particles, meanwhile, hydration groups, namely sulfo groups and hydroxyl groups can bring an adsorbed hydration layer to the clay particles, steric stability of a disperse system is enhanced, the situation that fine particles aggregate to form dense mud cakes is effectively suppressed, and therefore the effect of filtrate loss reduction is achieved. Vander Waals force and electrostatic attraction exist between cationic quaternary ammonium groups and the clay particles with negative charges on surfaces, and therefore the filtrate loss reducer can be firmly adsorbed on the surfaces of the clay particles; steric hindrance generated by long side chains of polyoxyethylene groups can enhance the rigidity of main chains, and therefore the temperature resistance of a polymer is improved.
Description
Technical field
The present invention relates to drilling liquid technology field, particularly relate to a kind of high-temperature resisting and salt-resisting calcium water-base drilling fluid amido and be polymerized
Thing fluid loss additive and its preparation method and application, this amine based polymer fluid loss additive is applied to petroleum vapour drilling process and bores chance deeply
In the drilling fluid on portion HTHP stratum.
Background technology
Due to China's oil and natural gas resource demand increase sharply and the shallow hydrocarbon stratum energy increasingly exhausted, deeply
The exploitation of the layer oil gas energy is the main outlet of China Petroleum future development, wherein it is essential that deep-well, ultradeep well
Drilling technique.High-temperature resistant water-based drilling fluid technology is the key technology of probing high temperature deep well, always world-famous puzzle.
During deep drilling exploration, due to geothermal gradient effect, vertical depth is deeper, and bottom pit shaft interior temperature degree is higher.Plus brill
Well liquid stops in down-hole and the time of circulation also extends.Therefore it is required that Deal With Drilling Fluid keeps good performance at high temperature.Separately
Meeting bad ground outer deep-well, ultradeep well, such as salt deposit, saline bed or high pressured slatwater layer etc. more.Salt calcium intrusion can affect drilling well fluidity
Energy.Under high temperature, the impact of salt calcium invasion can aggravate.It is therefore desirable to filtrate reducer for drilling fluid can be with high temperature resistance, salt resistance calcium contamination.
The molecular weight of polymerization species fluid loss additive is often higher, using the rheological characteristic to drilling fluid in low density drilling fluid
Impact is less.But use in high density drilling fluid, because the solid concentration of drilling fluid is high, adds and run into mud shale mud making formation,
Leading to amine based polymer fluid loss additive to be difficult to be added in drilling fluid, even if adding a small amount of fluid loss additive, also resulting in drilling fluid
Viscosity shear force significantly rise, drilling fluid rheology performance rises and falls big, finally can not use this kind of fluid loss additive.Therefore, study
High temperature resistance, salt resistance calcium drilling fluid amido fluid loss additive have urgent realistic meaning.
Content of the invention
It is an object of the invention to provide a kind of amine based polymer fluid loss additive of loss additive for drilling calcium, this fall
Fluid loss agents have good heat-resisting property (temperature resistance ability reaches 180 DEG C), and salt resistance calcium ability is strong, low to the viscosity effect of drilling fluid.
It is a further object to provide the preparation method of this amine based polymer fluid loss additive, the method operation letter
Single, mild condition, yield is higher.
For solving above-mentioned technical problem, the present invention employs the following technical solutions and is achieved：
A kind of high-temperature resisting and salt-resisting calcium water-base drilling fluid amine based polymer fluid loss additive, this amine based polymer fluid loss additive
General structure is as follows：
Wherein, m=40%～45%, n=40%～45%, p=1-m-n-q, q=8%～10%, K is 9～20, m,
N, p, q represent molar content.
Preferably, described amine based polymer fluid loss additive is mainly by acrylamide, 2- acrylamido -2- methyl-prop
Sulfonic acid, allyl polyglycol, trihydroxyethyl allylic bromination ammonium are prepared from for raw material, and acrylamide, 2- acrylamido-
2- methyl propane sulfonic acid, allyl polyglycol, the mol ratio of trihydroxyethyl allylic bromination ammonium are 8.1～20.2：9～15.2：
2.1～4.3：8～10, and the molecular weight of allyl polyglycol is between 400～1000.
The above-mentioned high-temperature resisting and salt-resisting calcium water-base drilling fluid preparation method of amine based polymer fluid loss additive, walks including following
Suddenly：
(1) acrylamide, 2- acrylamide-2-methylpro panesulfonic acid, allyl polyglycol, trihydroxyethyl pi-allyl are pressed
The mol ratio of ammonium bromide is 8.1～20.2：9～15.2：2.1～4.3：8～10 weigh raw material monomer；
(2) 2- acrylamide-2-methylpro panesulfonic acid is dissolved in deionized water, regulation solution ph to 7～8, then
Successively acrylamide, allyl polyglycol, trihydroxyethyl allylic bromination ammonium are added in solution, stirring and dissolving is uniform, and
Add molecular weight regulator, logical nitrogen deoxygenation；
(3) lead to nitrogen be warming up to 40 DEG C～60 DEG C after 30 minutes, add initiator, to total monomer concentration be 12.5%～
25%, reaction obtains gel solution in 4～6 hours；
(4) will extract in molten for gel solution use organic solvent, shear granulation dries pulverizing after purification, obtain final product quarternary copolymerized product
Thing.
Preferably, in described step (2), adjust pH value and pass through to add potassium hydroxide solution to realize.
Preferably, in described step (2), molecular weight regulator is C3～C12In sulfur alcohol compound or isopropanol
At least one, its addition is the 0.1wt%～1.0wt% of polymerized monomer total amount.
Preferably, in described step (3), initiator is the oxidant in redox initiation system, and initiator
At least one in potassium peroxydisulfate, ammonium persulfate, hydrogen peroxide；Reducing agent in initiator is selected from sodium hydrogensulfite, thio
At least one in sodium sulphate, tetramethylethylenediamine, the addition of initiator is acrylamide, 2- acrylamido -2- methyl
Propane sulfonic acid, allyl polyglycol, the 0.2wt%～0.6wt% of trihydroxyethyl allylic bromination ammonium gross mass.
Preferably, the organic solvent in described step (4) is absolute ethyl alcohol.
The invention allows for application in drilling fluid for the above-mentioned amine based polymer fluid loss additive.
The adsorption groups such as amide groups, ehter bond, hydroxyl, quaternary ammonium group are had on the molecular structure of the fluid loss additive that the present invention is obtained
Can effectively adsorb on clay particle, meanwhile, aquation group sulfonic group, hydroxyl can bring absorption hydrated sheath to clay particle,
Enhancing the spatial stability of dispersion, effectively inhibit the coalescence of subparticle, forming fine and close mud cake, thus reaching fall
The effect of leak-off.
Do not only exist Van der Waals power between the negatively charged clay particle of cationic quaternary ammonium groups and surface, also have higher
Electrostatic attraction, therefore can firmly adsorb on clay particle surface, even if being also not easy desorption at high temperature.In addition,
Quaternary ammonium ion group can ionize in water completely, can increase polymer molecular chain extension degree in aqueous.Polyoxy
It is sterically hindered that the long side chain of vinyl produces, and can strengthen main chain rigidity, be difficult to roll up and be wound around, also can reduce amide groups water
Solution speed, thus improve the heat-resisting property of polymer.Sulfonic group has good stability, to high temperature action and extraneous cation
Attack is insensitive, is conducive to strengthening high temperature resistance, the salt resistance calcium performance of copolymer.Amine based polymer fluid loss additive is with carbon carbon backbone chain
For skeleton, macromolecule side chain, as side chain, slow down fluid loss additive degraded at high temperature, is conducive to playing its fall filter under high temperature
The effect lost.
The molecular weight of amine based polymer fluid loss additive is moderate, the viscosity of drilling fluid is not affected greatly after addition.I.e.
When adding the density that the heavy weight additive such as barite improves drilling fluid, the viscosity amplification of drilling fluid is little.
Brief description
Fig. 1 is the infrared spectrum analysis figure of the fluid loss additive of the present invention.
Specific embodiment
It is to allow those skilled in the art to become apparent from getting information about the present invention, below in conjunction with accompanying drawing, to the present invention
It is further described.
Embodiment 1
A kind of high-temperature resisting and salt-resisting calcium water-base drilling fluid amine based polymer fluid loss additive, by acrylamide, 2- acrylamide
Base -2- methyl propane sulfonic acid, allyl polyglycol, trihydroxyethyl allylic bromination ammonium are prepared from for raw material, acrylamide, 2-
Acrylamide-2-methylpro panesulfonic acid, allyl polyglycol, trihydroxyethyl allylic bromination ammonium mol ratio be 8.1～
20.2：9～15.2：2.1～4.3：8～10, its reaction equation is：
Wherein, m=40%～45%, n=40%～45%, p=1-m-n-q, q=8%～10%, and the poly- second of pi-allyl
The molecular weight of glycol is between 400～1000, and K is 9～20, m, and n, p, q represent molar content.
The preparation method of this amine based polymer fluid loss additive comprises the steps：By acrylamide, 2- acrylamido -2-
Methyl propane sulfonic acid, allyl polyglycol, the mol ratio of trihydroxyethyl allylic bromination ammonium are 8.1～20.2：9～15.2：2.1
～4.3：8～10 weigh raw material monomer；2- acrylamide-2-methylpro panesulfonic acid is dissolved in deionized water, uses potassium hydroxide
The pH value of solution, to 7～8, puts into acrylamide, allyl polyglycol, trihydroxyethyl pi-allyl successively after pouring reaction vessel into
Ammonium bromide, stirring and dissolving is uniform；Add C3～C12Sulfur alcohol compound or the molecular weight regulator of isopropanol, its addition is poly-
Close the 0.1wt%～1.0wt% of monomer total amount, then lead to nitrogen deoxygenation；Logical nitrogen is warming up to 40 DEG C～60 DEG C after 30 minutes, plus
Enter the initiator of redox initiation system, its addition is the 0.2wt%～0.6wt% of raw material gross mass, makes total monomer dense
Spend for 12.5%～25%, reaction obtains gel solution in 4～6 hours；Gel solution is purified with absolute ethanol washing, shearing is made
Grain dries pulverizing, obtains final product quarternary copolymerized product.
The structural characterization of the amine based polymer fluid loss additive of embodiment 2 gained
As shown in Figure 1,1044.28cm-1For-SO3-Characteristic absorption peak, contain in the molecular structure that polymerizate is described
Sulfonic acid group；2920.67cm-1For CH2The flexural vibrations absworption peak of group；1660.47cm-1C=O stretching vibration for amide groups
Absworption peak；1544.04cm-1Stretching vibration absworption peak for the N-H bond bending vibration in secondary amide-CONH- group and C-N key；
1397.41cm-1Locate as-CH3Characteristic absorption peak；1277.38cm-1Locate as C-N stretching vibration absworption peak；982.24cm-1Locate be
RCH=CH2In=flexural vibrations peak of C-H；3400.21cm-1Shrink vibration absorption peak for non-association N-H；1174.31cm-1Place
There is characteristic absorption peak, illustrate to contain ether epoxide in product molecule.3262.82cm-1For the stretching vibration peak of hydroxyl, 954.26cm-1
For quaternary ammonium salt ion N+Stretching vibration absworption peak.1444.04cm-1For-CH2Stretching vibration peak.Illustrate to contain in product molecule
TAAC.Additionally, in 1680～1620cm-1The characteristic absorption peak of no carbon-carbon double bond, illustrates that polymerisation is complete.Analyzing polymers
Infrared spectrogram, contains the functional group of design in polymer molecular chain, understand accordingly, target product structure and Molecular Design
It is consistent.
The aqueous solution performance study of the amine based polymer fluid loss additive of embodiment 3 gained
Table 1：The rheological characteristic of amine based polymer fluid loss additive
| Fluid loss additive addition (wt%) | 0.5 | 1.0 | 1.5 | 2 |
| Apparent viscosity (mPa s) | 2.5 | 4.5 | 7.0 | 8.5 |
| Plastic viscosity (mPa s) | 2.0 | 4.0 | 6.5 | 8.5 |
As can be seen from Table 1, increasing with fluid loss additive addition, the viscosity of polymer solution is gradually increased.When
When solution concentration is 2%, its apparent viscosity and plastic viscosity are only 8.5mPa s, and what fluid loss additive was described carries viscous limited use.
The property of drilling fluid research of case study on implementation 4 amine based polymer fluid loss additive
Base is starched：4% calcium bentonite is added (to meet oil and gas industry standard SY/T 5060- in 1000ml warm water
93 regulation), add 2.4g soda ash, high-speed stirred 2h, maintenance 24h at room temperature after stirring, obtain final product base slurry.
Weigh different amounts of fluid loss additive successively, be dissolved in 400ml fresh water bentonite slurry, after high-speed stirred 20min, airtight
Maintenance 24h, heat rolling under the conditions of 180 DEG C was taken out after 16 hours, after being cooled to room temperature, tested its rheological characteristic, API filtration and height
Warm high pressure (HTHP) filter loss.Result is as shown in table 2.
Table 2：The impact to drilling fluid rheology and filtration property for the amine based polymer addition of filtrate reducer
From experimental data, the addition of amine based polymer fluid loss additive can effectively reduce the dehydration of fresh water-based slurry
Amount, with the increase of temperature, API filtration and HTHP (HTHP) filter loss gradually decrease.
By contrasting apparent viscosity and plastic viscosity, with the increase of copolymer concentration, the apparent viscosity of drilling fluid
It is gradually increased with plastic viscosity, but increasing degree is less, illustrates that copolymer is less to the viscosity of drilling fluid system.
The property of drilling fluid research of case study on implementation 5 amine based polymer fluid loss additive
Add the fluid loss additive of 1.5wt% in base slurry, after stirring, add the barite of certain mass to increase
Agent, measures its density using densitometer, and measures the various performance parameters of weighted drilling fluid.Result is as shown in table 3.
Table 3：Fluid loss additive concentration is rheological characteristic and the filtration property of 1.5wt% drilling fluid
Table 3 understands, the addition of fluid loss additive does not increase considerably apparent viscosity and the plastic viscosity of drilling fluid.Even if
In weighted drilling fluid, the addition of fluid loss additive does not cause the surge of drilling fluid viscosity yet.
The anti-salt property research of case study on implementation 6 amine based polymer fluid loss additive
Add the fluid loss additive of 1.5wt% in base slurry, after stirring, add the NaCl of variable concentrations, research
The anti-salt property of amine based polymer fluid loss additive.Result is as shown in table 4.
Table 4：The anti-salt property of amine based polymer fluid loss additive
By in table as can be seen that drilling fluid aging before and after viscosity reduce with the increase of NaCl.The addition of electrolyte
Compression double electric layer, clay particle is susceptible to coalesce, and the decentralization of drilling fluid reduces, and therefore macro manifestations drop for drilling fluid viscosity
Low.The API filtration of drilling fluid increases with the increase of NaCl, but pernicious leak-off, it can be said that the polymerization of bright amido
Thing fluid loss additive has stronger saline-alkaline tolerance.Because the anion of sulfonic acid group is very stable, affected by extraneous metal ion
Less, thus salt-resistance is stronger.Meanwhile, even if sulfonic acid group and polyoxyethylene base side chain have very strong hydrophily in electrolyte
Still enough hydration shells can be brought to clay it is ensured that drilling fluid system has preferable anti-salt property in environment.
The anticalcium performance study of case study on implementation 7 amine based polymer fluid loss additive
Add the fluid loss additive of 1.5wt% in base slurry, after stirring, add the CaCl of variable concentrations2, research
The anticalcium performance of amine based polymer fluid loss additive.Result is as shown in table 5.
Table 5：The anticalcium performance of amine based polymer fluid loss additive
The viscosity of drilling fluid is with CaCl as can be seen from the table2The increase of concentration and reduce, API filtration increase.Explanation
CaCl2Addition exacerbate the coalescence of clay particle, the decentralization of drilling fluid reduces.But pernicious leak-off does not occur, illustrates to be polymerized
Thing drilling fluid has good anticalcium performance.
Although, above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (8)
1. a kind of high-temperature resisting and salt-resisting calcium water-base drilling fluid with amine based polymer fluid loss additive it is characterised in that this amine based polymer
The general structure of fluid loss additive is as follows：
Wherein, m=40%～45%, n=40%～45%, p=1-m-n-q, q=8%～10%, K is 9～20.
2. amine based polymer fluid loss additive according to claim 1 is it is characterised in that described amine based polymer fluid loss additive
Mainly by acrylamide, 2- acrylamide-2-methylpro panesulfonic acid, allyl polyglycol, trihydroxyethyl allylic bromination ammonium
It is prepared from for raw material, acrylamide, 2- acrylamide-2-methylpro panesulfonic acid, allyl polyglycol, trihydroxyethyl allyl
The mol ratio of base ammonium bromide is 8.1～20.2：9～15.2：2.1～4.3：8～10, and the molecular weight of allyl polyglycol is
Between 400～1000.
3. the preparation method of amine based polymer fluid loss additive according to claim 1 and 2 is it is characterised in that include as follows
Step：
(1) acrylamide, 2- acrylamide-2-methylpro panesulfonic acid, allyl polyglycol, trihydroxyethyl allylic bromination are pressed
The mol ratio of ammonium is 8.1～20.2：9～15.2：2.1～4.3：8～10 weigh raw material monomer；
(2) 2- acrylamide-2-methylpro panesulfonic acid is dissolved in deionized water, regulation solution ph to 7～8, then successively
Acrylamide, allyl polyglycol, trihydroxyethyl allylic bromination ammonium are added in solution, stirring and dissolving uniformly, and adds
Molecular weight regulator, logical nitrogen deoxygenation；
(3) lead to nitrogen and after 30 minutes, be warming up to 40 DEG C～60 DEG C, add initiator, be 12.5%～25% to total monomer concentration,
Reaction obtains gel solution in 4～6 hours；
(4) will extract in gel solution organic solvent, shear granulation dries pulverizing after purification, obtain final product quarternary copolymerized product.
4. the preparation method of amine based polymer fluid loss additive according to claim 3 is it is characterised in that described step (2)
In, adjust pH value and pass through to add potassium hydroxide solution to realize.
5. the preparation method of amine based polymer fluid loss additive according to claim 3 is it is characterised in that described step (2)
In, molecular weight regulator is C3～C12At least one in sulfur alcohol compound or isopropanol, its addition is that polymerized monomer is total
0.1wt%～the 1.0wt% of amount.
6. the preparation method of amine based polymer fluid loss additive according to claim 3 is it is characterised in that described step (3)
In, initiator is for the oxidant in redox initiation system, and initiator in potassium peroxydisulfate, ammonium persulfate, hydrogen peroxide
At least one；Reducing agent in initiator be selected from sodium hydrogensulfite, sodium thiosulfate, in tetramethylethylenediamine at least one
Kind, the addition of initiator is acrylamide, 2- acrylamide-2-methylpro panesulfonic acid, allyl polyglycol, trihydroxyethyl
0.2wt%～the 0.6wt% of allylic bromination ammonium gross mass.
7. the preparation method of amine based polymer fluid loss additive according to claim 3 is it is characterised in that described step (4)
In organic solvent be absolute ethyl alcohol.
8. application in drilling fluid for the amine based polymer fluid loss additive according to claim 1 and 2.
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| CN109810679A (en) * | 2019-02-28 | 2019-05-28 | 西安石油大学 | A kind of oligomeric clay hydrate inhibiter of deepwater drilling liquid polyhydroxy and its synthetic method |
| CN109837073A (en) * | 2019-03-21 | 2019-06-04 | 西安石油大学 | A kind of shale gas horizontal well drilling shale closure inhibitor and preparation method thereof |
| CN113527575A (en) * | 2021-07-29 | 2021-10-22 | 长江大学 | Hyperbranched polymer filtrate reducer synthesized from pentaerythritol polyene monomer and preparation method thereof |
| CN114574177A (en) * | 2022-03-25 | 2022-06-03 | 库尔勒同益工贸有限责任公司 | Mud cake synergist for drilling fluid and preparation method thereof |
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| CN109810679A (en) * | 2019-02-28 | 2019-05-28 | 西安石油大学 | A kind of oligomeric clay hydrate inhibiter of deepwater drilling liquid polyhydroxy and its synthetic method |
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| CN109837073B (en) * | 2019-03-21 | 2021-01-19 | 西安石油大学 | Shale plugging inhibitor for drilling shale gas horizontal well and preparation method thereof |
| CN113527575A (en) * | 2021-07-29 | 2021-10-22 | 长江大学 | Hyperbranched polymer filtrate reducer synthesized from pentaerythritol polyene monomer and preparation method thereof |
| CN114574177A (en) * | 2022-03-25 | 2022-06-03 | 库尔勒同益工贸有限责任公司 | Mud cake synergist for drilling fluid and preparation method thereof |
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Application publication date: 20170222 |