CN106543377B - A kind of copolymer fluid loss agent and preparation method thereof - Google Patents
A kind of copolymer fluid loss agent and preparation method thereof Download PDFInfo
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- CN106543377B CN106543377B CN201610550442.2A CN201610550442A CN106543377B CN 106543377 B CN106543377 B CN 106543377B CN 201610550442 A CN201610550442 A CN 201610550442A CN 106543377 B CN106543377 B CN 106543377B
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- fluid loss
- loss agent
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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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
- 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
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/22—Synthetic organic compounds
- C09K8/24—Polymers
Abstract
The invention discloses a kind of copolymer fluid loss agent, the main chain of the copolymer fluid loss agent is made of following repetitive units (I),
Description
Technical field
The present invention relates to a kind of copolymer fluid loss agents and preparation method thereof.More particularly it relates to a kind of siliceous
The copolymer fluid loss agent and preparation method thereof of oxygen alkane.
Background technique
Fluid loss additive is one of most common inorganic agent in oilfield drilling, and in drilling process, drilling fluid filtrate is invaded
Membership causes shale hydration to expand, and hole instability and various complex situations is caused to occur, and boring also will cause oil when meeting payzone
Gas-bearing formation damage, these features are especially prominent in deep-well, ultradeep well probing, and the effect of fluid loss additive is to control wellbore fluid
Be filter loss, reduce and enters the amount of filtrate on stratum because of differential pressure action, thus damage of the reduction to stratum, be drilling fluid system not
The crucial inorganic agent that can or lack.Current water-base drilling fluid fluid loss additive both domestic and external is broadly divided into flocculation class, closes
At polymerization species and synthetic resin.
Natural polymer subclass fluid loss additive has the characteristics that cheap, from a wealth of sources, mainly includes cellulose, wooden
Element, humic acid, starch, lignite, tannin etc..The not strong disadvantage of its generally existing heat-resisting property, needs to be modified it, to reach
Temperature-resistant anti-salt effect.
Synthetic polymer fluid loss additive is many kinds of, function admirable, has the characteristics that some natural polymers are incomparable,
It is to study most widely used fluid loss additive at present.It is formed by various monomer addition polymerizations so that the fluid loss additive synthesized is with various
Different comprehensive performances, are widely applied.Synthetic resin fluid loss additive be based on phenolic resin, it is sulfonated or introduce it
His functional group and be made, the most commonly used with sulfonated-pheno-formoldehyde resin, although such fluid loss additive has good high-temperature resisting and salt-resisting to drop
Filtration property, but its dosage is larger, easily causes problem of environmental pollution.
Researchers have found after study, can be in the feelings of smaller dosage using the polymer filtrate reducer containing siloxanes
Preferable filtrate loss controllability is obtained under condition, and the polymer filtrate reducer containing siloxanes contains siloxane group, siloxanes
The general molecular formula of group is Si-OR, which is easily hydrolyzed to Si-OH, and then is generated securely by polycondensation reaction to each other
Si-O-Si key, and the clay particle surface after aquation is rich in silicone hydroxyl, therefore the polymer filtrate reducer containing siloxanes can
Condensation occurs with the silicone hydroxyl on clay particle surface and forms Si-O-Si key, fluid loss additive macromolecular can securely be adsorbed by this key
In on clay particle.Due to foring new chemical bond in adsorption process, therefore belong to chemisorption scope, and Si-O-Si key
Bond energy is high, does not act on and scission of link vulnerable to high temperature and salt calcium, imparts the good suction of the polymer filtrate reducer containing siloxanes
Attached stability.
Chinese patent application CN102174318A discloses a kind of fluid loss additive containing organosilicon, though have preferable anti-
High temperature and anti-salt property, but be somebody's turn to do the polymer filtrate reducer containing siloxanes and need to be added heterocyclic type polyamine segment to increase drop
The high temperature resistant property of fluid loss agents, being added has ionizable polymer segment to enhance its dissolubility and salt-resistance.It is well known that
Heterocyclic type polyamine monomers are costly, and unfriendly to environment;Ionizable monomer will usually first pass through the step of deprotonation,
It is converted into salt to be polymerize again, so that preparation process is relatively complicated.Therefore, a kind of polymer for being able to solve these problems is needed
Fluid loss additive, that is, need one kind without containing heterocyclic type monomer and ionizable monomer, and there is good high temperature resistant property and resist
The polymer filtrate reducer of the silicone-containing of salt.
Summary of the invention
It is an object of the invention to overcome the above-mentioned deficiency in the presence of the prior art, a kind of copolymer fluid loss agent is provided
And preparation method thereof.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical schemes:
The main chain of a kind of copolymer fluid loss agent, the copolymer fluid loss agent is made of following repetitive units (I),
In formula, the integer that M is 400~8000, (70~90) X: Y: Z=: (5~12): (5~20).
Copolymer fluid loss agent according to the present invention is a kind of copolymer, the copolymer be by AM, APEG-M and and
Polymer made of tri- kinds of monomer copolymerization of KH570, the amount accounting of the substance of the monomer account for 5~12%, AM for APEG-M and account for 70
~90%, KH570 account for 5~20%.Wherein the monomer AM is acrylamide;APEG-M is that polyethylene glycol chain segment molecular weight is M
Allyl polyglycol, such as APEG-1000 be polyethylene glycol chain segment molecular weight be 1000 allyl polyglycol;
KH570 is gamma-methyl allyl acyloxypropyl trimethoxysilane.Copolymer fluid loss agent according to the present invention, in chemical formula (I)
" PEG-M " refers to that molecular weight is the polyethylene glycol segment of M, such as " PEG-1000 " refers to that molecular weight is 1000 polyglycol chain
Section.Copolymer fluid loss agent according to the present invention, preferably M=500~5000, further preferred M=600~3000, more preferable M
=700~2400, most preferably M=600~2000.
Another object of the present invention is to provide a kind of each methods processed of copolymer fluid loss agent, comprising the following steps:
S1, acrylamide, allyl polyglycol are mixed and are heated in a solvent;
S2, when reaction temperature is 65~85 DEG C, gamma-methyl allyl acyloxypropyl trimethoxysilane is added, it is then logical
Enter nitrogen deoxygenation;
S3, to acrylamide, allyl polyglycol and gamma-methyl allyl acyloxypropyl trimethoxysilane mixing it is molten
Initiator is added in liquid and causes polymerization, reaction obtained gelling material after 4~12 hours, will obtain after gelling material purification
Copolymer fluid loss agent.
The copolymer fluid loss agent of above-mentioned preparation is a kind of copolymer, and main chain is made of following repetitive units (I),
In formula, the integer that M is 400~8000, (70~90) X: Y: Z=: (5~12): (5~20).
The preparation method of the copolymer fluid loss agent provided according to the present invention, wherein the AM is acrylamide;APEG-M
It is the allyl polyglycol that polyethylene glycol chain segment molecular weight is M, such as APEG-1000 is that polyethylene glycol chain segment molecular weight is
1000 allyl polyglycol;KH570 is gamma-methyl allyl acyloxypropyl trimethoxysilane.It provides according to the present invention
The each method processed of copolymer fluid loss agent, the solvent are atent solvents, such as ethers, amide solvent, such as tetrahydrofuran
(THF), n,N-Dimethylformamide (DMF) etc., preferably tetrahydrofuran (THF), n,N-Dimethylformamide (DMF), more preferably
DMF.The preparation method of the copolymer fluid loss agent provided according to the present invention, the initiator are oil-soluble heat decomposition type free radicals
Initiator, such as azo, peroxide initiator, such as azodiisobutyronitrile (AIBN), cumyl peroxide and peroxidating two
Tert-butyl etc.;It is preferred that azo-initiator, more preferable AIBN.
The preparation method of copolymer fluid loss agent according to the present invention, " PEG-M " refers to that molecular weight is M's in chemical formula A
Polyethylene glycol segment, such as " PEG-1000 " refer to that molecular weight is 1000 polyethylene glycol segment.Copolymer according to the present invention
The preparation method of fluid loss additive, preferably M=500~5000, further preferred M=600~3000, more preferable M=700~
2400, most preferably M=600~2000.
The preparation method of the copolymer fluid loss agent provided according to the present invention, preferably by KH570 in mixed uniformly condition
Under be added dropwise in the solution of AM and APEG.The preparation method of the copolymer fluid loss agent provided according to the present invention, the deoxygenation
Step can be carried out by leading to the method for nitrogen.The each method processed of the copolymer fluid loss agent provided according to the present invention, described " by
The step of gelling material purification ", can carry out by the following method: for example the gelling material being put into a large amount of acetone
It impregnates 12~36 hours, is filtered to remove liquid, again with methanol extracts 4~8 hours, re-dry.
Compared with prior art, beneficial effects of the present invention:
Copolymer fluid loss agent preparation method provided by the invention has simple process, and monomer is cheap and easy to get, reaction condition
Mildly, easily controllable advantage;Its starting monomer do not contain heterocyclic type monomer and ionizable monomer, but still have it is good,
Even more excellent high temperature resistant property and salt-resistance;Copolymer fluid loss agent provided by the invention contains siloxane group,
Facile hydrolysis forms silicone hydroxyl, and condensation occurs with the silicone hydroxyl on clay particle surface and forms Si-O-Si key, is securely adsorbed by this key
In on clay particle, filtrate reducing effect is preferable in fresh water-based slurry.
Specific embodiment
Below with reference to test example and specific embodiment, the present invention is described in further detail.But this should not be understood
It is all that this is belonged to based on the technology that the content of present invention is realized for the scope of the above subject matter of the present invention is limited to the following embodiments
The range of invention.
Embodiment 1
2.00g AM is dissolved in and is had in reflux unit three-necked flask equipped with 53.37gDMF, to after completely dissolution will
3.03gAPEG-700 is added in three-necked flask, is warming up to 70 DEG C, and 0.90g organic silicon monomer KH570 is added dropwise under agitation,
Lead to nitrogen deoxygenation in 30 minutes after being added dropwise, the initiator A IBN of monomer gross mass 0.4% is then added, and whole logical in reaction
Nitrogen protection, reaction obtained gelling material (i.e. the thick finished product of AM/APEG-700/KH570 ternary polymerization product) after 8 hours.It will coagulate
Jelly, which pours into a large amount of acetone, to be impregnated 24 hours, and liquid is filtered to remove, and is then extracted 4 hours with methanol, then at 35 DEG C
Copolymer fluid loss agent I is made to remove methanol in lower vacuum drying.
Embodiment 2
3.00g AM is dissolved in and is had in reflux unit three-necked flask equipped with 32.00gDMF, to after completely dissolution will
3.69gAPEG-2400 is added in three-necked flask, is warming up to 65 DEG C, and 1.31g organic silicon monomer KH570 is added dropwise under agitation,
Lead to nitrogen deoxygenation in 30 minutes after being added dropwise, the initiator A IBN of monomer gross mass 0.2% is then added, and whole logical in reaction
Nitrogen protection, reaction obtained gelling material (i.e. the thick finished product of AM/APEG-2400/KH570 ternary polymerization product) after 12 hours.It will
Gelling material, which pours into a large amount of acetone, to be impregnated 24 hours, and liquid is filtered to remove, and is then extracted 8 hours with methanol, then at 35 DEG C
Copolymer fluid loss agent II is made to remove methanol in lower vacuum drying.
Embodiment 3
2.00g AM is dissolved in and is had in reflux unit three-necked flask equipped with 37.85gDMF, to after completely dissolution will
5.12gAPEG-1000 is added in three-necked flask, is warming up to 85 DEG C, and 1.00g organic silicon monomer KH570 is added dropwise under agitation,
Lead to nitrogen deoxygenation in 30 minutes after being added dropwise, the initiator A IBN of monomer gross mass 0.3% is then added, and whole logical in reaction
Nitrogen protection, reaction obtained gelling material (i.e. the thick finished product of AM/APEG-1000/KH570 ternary polymerization product) after 4 hours.It will coagulate
Jelly, which pours into a large amount of acetone, to be impregnated 24 hours, and liquid is filtered to remove, and is then extracted 6 hours with methanol, then at 35 DEG C
Copolymer fluid loss agent III is made to remove methanol in vacuum drying.
Test case 1
For evaluation the embodiment of the present invention preparation fluid loss additive filtrate reducing effect, first, in accordance with GB/T16783-1997 state
Family's standard configuration base slurry.20g bentonite and 1g natrium carbonicum calcinatum are added i.e. in 500ml water, it is close after high-speed stirred 30 minutes
It closes standing 24 hours, obtains the fresh water-based slurry that bentonite content is 4%.The 400ml fresh water-based slurry solution is taken to be put into ZNS-2 type
It presses in filter press, measures the filter loss in its 0.7MPa pressure lower 30 minutes;The as filter loss of fresh water-based slurry.
The copolymer fluid loss agent I for accounting for quality of mud fluid score 1% is added in the fresh water-based slurry of 400ml, then stirring is equal
It is even, it is put into ZNS-2 type and presses in filter press, measure the filter loss in its 0.7MPa pressure lower 30 minutes and dropped to get to copolymer
Filter loss of the fluid loss agents I in fresh water-based slurry;Measure copolymer fluid loss agent II and copolymer filtrate reducing respectively according to above method
Filter loss of the agent III in fresh water-based slurry.Experimental result is as follows:
The filtrate reducing effect of product in 1 fresh water-based slurry of table
As can be seen from Table 1,1% copolymer fluid loss agent according to the present invention is added in fresh water-based slurry, can make to filter
Vector is reduced to 8.7ml~10.5ml by 27.4ml, illustrates that the filtrate reducer for drilling fluid of Examples 1 to 3 preparation can be effectively reduced
Fresh water-based slurry filter loss.
Test case 2
The copolymer fluid loss agent III for accounting for quality of mud fluid score 1% is added in the fresh water-based slurry of 400ml, then stirs
Uniformly, after 160 DEG C of high temperature ageing 16h, filter press is pressed to measure the leak-off in its 0.7MPa pressure lower 30 minutes in ZNS-2 type
Amount, i.e., middle filter pressing loss are 14.5ml, and GGS71-A type high-temperature and high-pressure filter press measures it 30 under the conditions of 160 DEG C and 3.5MPa
The filter loss of minute, twice for surveying 30 minutes filter losses is high temperature and high pressure filter loss, result 42ml, it follows that closing
At fluid loss additive high temperature resistant property it is preferable.Compare the prior art, it is seen that copolymer fluid loss agent according to the present invention is even
With than containing the better high temperature resistance of heterocyclic type monomer copolymer fluid loss additive.
Test case 3
The copolymer fluid loss agent III for accounting for quality of mud fluid score 4% is added in the fresh water-based slurry of 400ml, then stirs
Uniformly, pressing filter press to measure the filter loss in its 0.7MPa pressure lower 30 minutes in ZNS-2 type is 4ml, and addition accounts for quality of mud fluid
After the calcium chloride of score 1%, measuring middle filter pressing loss is 9ml, it is seen that the copolymer fluid loss agent tool of preparation of the embodiment of the present invention
There is preferable salt-resistance.
Although specific embodiment has been combined to be described in detail the present invention, those skilled in the art are come
It says, it is obvious for making various changes and modifications under the premise of without departing from the scope to it.Implementation described herein
Mode is only exemplary, and is not intended to be limiting of the invention.Many change and modification of the invention disclosed herein are
It is possible, and fall into the scope of the present invention.Therefore, protection scope is not limited by description set out above, only
It is limited by the attached claims, range includes all equivalents of claim theme.Each claim is incorporated to
Bright book is as embodiments of the present invention.Thus, claim is further instruction book, and is that the present invention is preferably implemented
The increase of mode.The disclosure of all patents referred to herein, patent application and publication is incorporated herein by reference, packet
It includes in exemplary, program that they are provided or other detailed supplements.
Claims (5)
1. a kind of copolymer fluid loss agent, which is characterized in that the main chain of the copolymer fluid loss agent is by following repetitive units (I)
It constitutes,
In formula, the integer that M is 400~8000, (70~90) X: Y: Z=: (5~12): (5~20).
2. copolymer fluid loss agent according to claim 1, which is characterized in that the integer that M is 500~5000.
3. the method for preparing copolymer fluid loss agent described in claim 1, which comprises the following steps:
S1, acrylamide, allyl polyglycol are mixed and are heated in a solvent;
S2, reaction temperature be 65~85 DEG C when, be added gamma-methyl allyl acyloxypropyl trimethoxysilane, be subsequently passed nitrogen
Gas deoxygenation;
S3, into the mixed solution of acrylamide, allyl polyglycol and gamma-methyl allyl acyloxypropyl trimethoxysilane
Initiator is added and causes polymerization, reaction obtained gelling material after 4~12 hours, will be copolymerized after gelling material purification
Object fluid loss additive.
4. preparation method according to claim 3, which is characterized in that the solvent is tetrahydrofuran, glycol dimethyl ether
One or more of with n,N-Dimethylformamide.
5. preparation method according to claim 3, which is characterized in that purification operations described in the step S3 include that will coagulate
Jelly, which is put into acetone, to be impregnated 12~36 hours, and liquid is filtered to remove, and again with methanol is extracted 4~8 hours, is subsequently dried.
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CN108774508A (en) * | 2018-05-31 | 2018-11-09 | 广西大学 | A kind of starch base organosilicon fire-resistant fluid loss additive and preparation method thereof |
CN108774507A (en) * | 2018-05-31 | 2018-11-09 | 钦州学院 | A kind of mixing fluid loss additive and preparation method thereof |
CN109097008B (en) * | 2018-08-09 | 2020-12-15 | 中国石油集团渤海钻探工程有限公司 | Filtrate reducer for soil-phase-free high-density saturated salt water drilling fluid and preparation method thereof |
CN108774505A (en) * | 2018-08-16 | 2018-11-09 | 张建华 | A kind of fluid loss additive for boring fluid and its preparation method and application |
CN115109269B (en) * | 2021-03-18 | 2023-06-02 | 中国石油化工股份有限公司 | Filtrate reducer and preparation method and application thereof |
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CN1528796A (en) * | 2003-09-28 | 2004-09-15 | 石油大学(华东) | Silicone modified polyacrylamide and preparing method thereof |
CN103289658A (en) * | 2013-05-24 | 2013-09-11 | 西南石油大学 | Drilling fluid loss agent and preparation method thereof |
CN105693925A (en) * | 2016-04-13 | 2016-06-22 | 中国石油大学(华东) | Sand prevention multi-branched polymer for oil-water well and preparation method of sand prevention multi-branched polymer |
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Patent Citations (3)
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CN1528796A (en) * | 2003-09-28 | 2004-09-15 | 石油大学(华东) | Silicone modified polyacrylamide and preparing method thereof |
CN103289658A (en) * | 2013-05-24 | 2013-09-11 | 西南石油大学 | Drilling fluid loss agent and preparation method thereof |
CN105693925A (en) * | 2016-04-13 | 2016-06-22 | 中国石油大学(华东) | Sand prevention multi-branched polymer for oil-water well and preparation method of sand prevention multi-branched polymer |
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