CN108676129A - A kind of comb-type structure amphoteric ion polymer fluid loss additive and preparation method thereof - Google Patents
A kind of comb-type structure amphoteric ion polymer fluid loss additive and preparation method thereof Download PDFInfo
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- CN108676129A CN108676129A CN201810525580.4A CN201810525580A CN108676129A CN 108676129 A CN108676129 A CN 108676129A CN 201810525580 A CN201810525580 A CN 201810525580A CN 108676129 A CN108676129 A CN 108676129A
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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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- 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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Abstract
The present invention relates to a kind of comb-type structure amphoteric ion polymer fluid loss additives and preparation method thereof.Fluid loss additive is copolymerized by the monomer of following parts by weight：20~40 parts of 2 acrylamide, 2 methyl propane sulfonic acid, 5~30 parts, N of monomethyl polyethylene glycol acrylate ester, 10~60 parts of N dimethacrylamide, 5~20 parts of dimethyl diallyl ammonium chloride.The fluid loss additive contains point subbase group such as quaternary ammonium, amide groups, sulfonic group, and there is wherein sulfonic group stronger hydration capability, amide groups and quaternary ammonium salt to have strong adsorption capacity to clay, improve the absorption stability under fluid loss additive hot conditions；It is in combed special construction by the product that macromonomer monomethyl polyethylene glycol acrylate ester and other monomers graft copolymerization obtain, it can further improve anti-shear performance and high-temperature stability, while ensureing filtrate loss controllability, heat and salinity tolerance effect is good, can be efficiently applied in the drilling fluid of high temperature bad ground environment.
Description
Technical field
The invention belongs to drilling fluid additive agent fields, and in particular to a kind of comb-type structure amphoteric ion polymer filtrate reducing
Agent and preparation method thereof.
Background technology
Development with petroleum industry and the continuous growth to oil demand, drilling depth are continuously increased, encounter therewith
High temperature bad ground and down hole problem are also more and more.Drilling fluid is referred to as " blood " of drilling technology, is drilling technology
Important component, increasingly important role is played in drilling process with the drilling fluid of high-temperature resisting and salt-resisting performance.
Fluid loss additive is one of important dose of kind of drilling fluid, and effect is that low-permeability, flexible, thin and compact filter are formed on the borehole wall
Cake reduces the filter loss of drilling fluid, to maintain wellbore stability, to ensure downhole safety as far as possible.
How emphasis one of that fluid loss additive with good temperature resistance and salt-resistance be oil worker research is prepared.Shen
Please publication No. be CN101864030A patent disclose a kind of preparation method of high-temperature resisting and salt-resisting fluid loss additive, this method be with
C6-C10 alkane is continuous phase, is soluble in the aqueous phase with three kinds of acrylamide, acrylic acid and sodium styrene sulfonate monomers and emulsification is added
The method of agent conversed phase micro emulsion copolymerization obtains high-temperature resisting and salt-resisting both sexes fluid loss additive；In the preparation method, three kinds of initial monomers
It should be strict controlled in certain proportion range, if conversed phase micro emulsion copolymerization ratio is improper, system is difficult to form microemulsion or meeting
The performance of polymer is reduced, the stability of industrial mass production is difficult to be protected.
Authorization Notice No. is that the patent of CN100595254C discloses a kind of preparation of amphoteric ion polymer fluid loss additive
Method, the preparation method are to obtain high-temperature resisting and salt-resisting both sexes fluid loss additive in the method for aqueous solution polymerization, but production technology is multiple
It is miscellaneous, low production efficiency, it is difficult to meet the condition of large-scale production.Authorization Notice No. is that the patent of CN104926986B discloses one
Kind for drilling fluid amphoteric ion polymer preparation method, the preparation method be with dimethylaminoethyl methacrylate,
1,3-propane sultone and acrylamide are prepared for the aggregated reaction of monomer, though the amphoteric ion polymer has preferably
Anti-calcium and anti-salt ability, but temperature resistance ability is poor, can not be applied in high-temperature stratum.
Invention content
The purpose of the present invention is to provide a kind of comb-type structure amphoteric ion polymer fluid loss additives, to solve existing drop
Fluid loss agents cannot have both the problem of excellent filtrate loss controllability and heat and salinity tolerance performance.
Second object of the present invention is to provide the preparation method of above-mentioned fluid loss additive.
To achieve the above object, the technical solution adopted in the present invention is：
A kind of comb-type structure amphoteric ion polymer fluid loss additive, is copolymerized by the monomer of following parts by weight：2- propylene
20~40 parts of amide -2- methyl propane sulfonic acids, 5~30 parts of monomethyl polyethylene glycol acrylate ester, N,N-DMAA 10
~60 parts, 5~20 parts of dimethyl diallyl ammonium chloride.
Monomethyl polyethylene glycol acrylate ester is due to its polyethylene glycol segment with excellent compatibility, in various medical lifes
The surface of object material is modified and extensive use in the research of the materials synthesis such as new and effective water-reducing agent.Using this macromonomer as comb
The branch of type polymer ensures that drilling fluid has preferable rheological property and high temperature resistance to enhance the integrally-built rigidity of molecule
Energy.Its structural formula is as follows：
The comb-type structure amphoteric ion polymer fluid loss additive of the present invention, 2- acrylamide-2-methyl propane sulfonics, poly- second two
Alcohol monomethyl ether acrylate, N, N- dimethacrylamide, dimethyl diallyl ammonium chloride in aqueous solution graft copolymerization and
At a kind of multiple copolymer, gained copolymer contains point subbase group such as quaternary ammonium, amide groups, sulfonic group, and wherein sulfonic group has
Stronger hydration capability (especially high temperature anticalcium, magnesium pollution capacity), amide groups and quaternary ammonium salt have strong adsorption capacity to clay,
Improve the absorption stability under fluid loss additive hot conditions；Product is in combed special construction, can further improve shear resistant
Energy and high-temperature stability, while ensureing filtrate loss controllability, heat and salinity tolerance effect is good, can be efficiently applied to high temperature bad ground
In the drilling fluid of environment.
The preparation method of above-mentioned comb-type structure amphoteric ion polymer fluid loss additive, includes the following steps：
1) by 2- acrylamide-2-methyl propane sulfonics, monomethyl polyethylene glycol acrylate ester, N, N- dimethyl allene acyls
Amine, dimethyl diallyl ammonium chloride are soluble in water, obtain monomer solution；
2) under protective atmosphere, be added initiator carry out copolyreaction to get.
In step 1), first 2- acrylamide-2-methyl propane sulfonics are dissolved in water, add poly glycol monomethyl ether propylene
Acid esters stirs evenly, and adds N,N-DMAA and dimethyl diallyl ammonium chloride, in N235~50 DEG C of protection
Under stir evenly to get the monomer solution.
In step 1), it is 6~8 that pH adjusting agent regulation system pH value is added into monomer solution.PH adjusting agent is hydrogen
One or more combinations in sodium oxide molybdena, hydrogen-oxygen agent, ammonium hydroxide.
In step 1), in monomer solution, the sum of mass concentration of each monomer is 20~45%.
In step 2), the initiator is the mixing of at least one of ammonium persulfate, potassium peroxydisulfate with sodium hydrogensulfite
Object.Preferably, mass percent of the sodium hydrogensulfite in initiator is 25%~50%.
In step 2), initiator in polymerization system a concentration of 0.5%~5%.
In step 2), the copolyreaction is first polymerase 10 .5~1.5h at 35~50 DEG C, then is polymerize at 75~85 DEG C
2.5~3.5h.
It in step 2), is filtered after copolyreaction, collects filtration product, washing, drying are to get the fluid loss additive.Washing
Washing lotion used is acetone；The drying is 8~12h of vacuum drying at 100~110 DEG C.
The preparation method of the comb-type structure amphoteric ion polymer fluid loss additive of the present invention, preparation process is simple, to equipment
Requirement it is low, production stability is good, of low cost, large-scale industrial production easy to implement.
Specific implementation mode
Embodiments of the present invention are described further with reference to specific embodiment.In following embodiment, poly- second two
The number-average molecular weight of alcohol monomethyl ether acrylate is 400-2000.
Embodiment 1
The comb-type structure amphoteric ion polymer fluid loss additive of the present embodiment, is copolymerized by the monomer of following parts by weight：
40 parts of 2- acrylamide-2-methyl propane sulfonics, 20 parts of monomethyl polyethylene glycol acrylate ester, N,N-DMAA 30
Part, 10 parts of dimethyl diallyl ammonium chloride；Preparation process is as follows：
1) 40 parts of 2- acrylamide-2-methyl propane sulfonics and 300 parts of distilled water are added in reactor, are stirred to abundant
Dissolving；20 parts of monomethyl polyethylene glycol acrylate esters are added, are stirred evenly, it is molten that the sodium hydroxide that mass concentration is 20% is added
Liquid, regulation system pH value are 6；Then 30 parts of N,N-DMAAs and 10 parts of dimethyl diallyl ammonium chlorides are added,
It is stirred evenly at 40 DEG C, obtains the monomer solution that the sum of each monomer mass concentration is 25%；
2) lead to nitrogen protection 30min, initiator is then added, and (ammonium persulfate is 2 with sodium hydrogensulfite mass ratio：1 it is mixed
Object is closed, 3%) a concentration of in system of initiator polymerize 1h at 40 DEG C, then heat to 80 DEG C of polyase 13 h, reacted
Product；
3) reaction product is washed with acetone, filters and collect filtration product, 10h is dried in vacuo at 105 DEG C, crushing is
Obtain white powder fluid loss additive.
Embodiment 2
The comb-type structure amphoteric ion polymer fluid loss additive of the present embodiment, is copolymerized by the monomer of following parts by weight：
30 parts of 2- acrylamide-2-methyl propane sulfonics, 10 parts of monomethyl polyethylene glycol acrylate ester, N,N-DMAA 50
Part, 10 parts of dimethyl diallyl ammonium chloride；Preparation process is as follows：
1) 30 parts of 2- acrylamide-2-methyl propane sulfonics and 400 parts of distilled water are added in reactor, are stirred to abundant
Dissolving；10 parts of monomethyl polyethylene glycol acrylate esters are added, are stirred evenly, it is molten that the sodium hydroxide that mass concentration is 20% is added
Liquid, regulation system pH value are 7；Then 50 parts of N,N-DMAAs and 10 parts of dimethyl diallyl ammonium chlorides are added,
It is stirred evenly at 35 DEG C, obtains the monomer solution that the sum of each monomer mass concentration is 20%；
2) lead to nitrogen protection 30min, initiator is then added, and (potassium peroxydisulfate is 3 with sodium hydrogensulfite mass ratio：2 it is mixed
Object is closed, 1%) a concentration of in system of initiator polymerize 1.5h at 35 DEG C, then heat to 75 DEG C of polyase 13 .5h, obtain
Reaction product；
3) reaction product is washed with acetone, filters and collect filtration product, 11h is dried in vacuo at 100 DEG C, crushing is
Obtain white powder fluid loss additive.
Embodiment 3
The comb-type structure amphoteric ion polymer fluid loss additive of the present embodiment, is copolymerized by the monomer of following parts by weight：
30 parts of 2- acrylamide-2-methyl propane sulfonics, 5 parts of monomethyl polyethylene glycol acrylate ester, 60 parts of N,N-DMAA,
5 parts of dimethyl diallyl ammonium chloride；Preparation process is as follows：
1) 30 parts of 2- acrylamide-2-methyl propane sulfonics and 300 parts of distilled water are added in reactor, are stirred to abundant
Dissolving；5 parts of monomethyl polyethylene glycol acrylate esters are added, are stirred evenly, it is molten that the sodium hydroxide that mass concentration is 20% is added
Liquid, regulation system pH value are 8；Then 60 parts of N,N-DMAAs and 5 parts of dimethyl diallyl ammonium chlorides are added,
50 DEG C stir evenly, and obtain the monomer solution that the sum of each monomer mass concentration is 25%；
2) lead to nitrogen protection 30min, initiator is then added, and (ammonium persulfate is 1 with sodium hydrogensulfite mass ratio：1 it is mixed
Close object, initiator in system it is a concentration of 4%), the polymerase 10 .5h at 50 DEG C, then heat to 85 DEG C polymerization 2.5h, obtain
Reaction product；
3) reaction product is washed with acetone, filters and collect filtration product, 8h is dried in vacuo at 110 DEG C, crushing is
Obtain white powder fluid loss additive.
Test example
This test example detect embodiment 1 filtrate loss controllability of the fluid loss additive in compound salt-water basic slurry and brine mud and
High-temperature behavior.Comparative example is commercially available acrylamide copolymer fluid loss additive.
Compound salt-water basic slurry is formulated as：1000mL distilled water+45.0g sodium chloride+7.0g calcium chloride+15g magnesium chlorides are made
For compound brine, the compound brine of 350mL is taken, it is complex salt that 3.15g sodium carbonate and 52.50g calcium bentonites are added under stiring
Water base slurry；Brine mud is formulated as：The brine 350mL of different sodium chloride concentrations is taken, 35g evaluations soil and 1g are added under stiring
Sodium bicarbonate continues after stirring 20min, obtains brine mud, and control base starches filter loss in 80-90mL.
The fluid loss additive of embodiment 1 is as shown in table 1 in the Evaluation results of compound salt-water basic slurry, surveys room temperature filter loss
When, the addition mass fraction of fluid loss additive is 0.7%, when pyrometry aging filter loss, addition of filtrate reducer 1.5%, specifically
Process is as follows：
(1) room temperature filter loss measures：The compound salt-water basic slurry conserved is taken, under certain rotating speed, 0.7% is added thereto
Fluid loss additive, stir 20min, room temperature conserve for 24 hours.It is stirred for 20min, surveys API filtration.
(2) high temperature filter loss measures：The compound salt-water basic slurry conserved is taken, under certain rotating speed, 1.5% is added thereto
Fluid loss additive, stir 20min, room temperature conserve 6h.It is stirred for 20min, is put into stainless steel ageing can after 200 DEG C of aging 16h,
Cooling is taken out, 20min is stirred, surveys API filtration.
Benchmark test data of the fluid loss additive of 1 embodiment 1 of table in compound salt-water basic slurry
| Serial number | Room temperature API filtration/mL | API filtration/mL after 200 DEG C of agings |
| Embodiment 1 | 6.2 | 8.9 |
| Comparative example | 13.5 | 25.4 |
The fluid loss additive of embodiment 1 is as shown in table 2 in the Evaluation results of brine mud, takes the chlorine of five kinds of various concentrations
Change each two parts of the water base slurry 350mL of sodium salt, is separately added into the fluid loss additive stirring 30min of 2.45g and 5.25g embodiments 1；Wherein five
Part conserves for 24 hours at room temperature, and another five parts after room temperature conserves 6h, are packed into high-temperature tank, and heat rolling 16h, is cooled to room at 200 DEG C
Temperature；After base to be measured is starched high-speed stirred (6000r/min) 5min, the API filtration after the mild 200 DEG C of agings of measuring cell.
Benchmark test data of the fluid loss additive of 2 embodiment 1 of table in brine mud
By the Evaluation results of Tables 1 and 2 it is found that in compound salt-water basic slurry and brine mud, the drop of embodiment 1 is filtered
It loses agent to show under 200 DEG C of high temperature well, there is excellent heat and salinity tolerance and filtrate loss controllability.
Claims (9)
1. a kind of comb-type structure amphoteric ion polymer fluid loss additive, which is characterized in that by the monomer copolymerization of following parts by weight
At：20~40 parts of 2- acrylamide-2-methyl propane sulfonics, 5~30 parts, N of monomethyl polyethylene glycol acrylate ester, N- dimethyl propylenes
10~60 parts of acrylamide, 5~20 parts of dimethyl diallyl ammonium chloride.
2. a kind of preparation method of comb-type structure amphoteric ion polymer fluid loss additive as described in claim 1, feature exist
In including the following steps：
1) by 2- acrylamide-2-methyl propane sulfonics, monomethyl polyethylene glycol acrylate ester, N, N- dimethacrylamide, two
Methyl diallyl ammonium chloride is soluble in water, obtains monomer solution；
2) under protective atmosphere, be added initiator carry out copolyreaction to get.
3. the preparation method of comb-type structure amphoteric ion polymer fluid loss additive as claimed in claim 2, which is characterized in that step
It is rapid 1) in, first 2- acrylamide-2-methyl propane sulfonics are dissolved in water, it is equal to add monomethyl polyethylene glycol acrylate ester stirring
It is even, N,N-DMAA and dimethyl diallyl ammonium chloride are added, is stirred evenly at 35~50 DEG C to get institute
State monomer solution.
4. the preparation method of comb-type structure amphoteric ion polymer fluid loss additive as claimed in claim 2, which is characterized in that step
It is rapid 1) in, into monomer solution be added pH adjusting agent regulation system pH value be 6~8.
5. the preparation method of comb-type structure amphoteric ion polymer fluid loss additive as claimed in claim 2, which is characterized in that single
In liquid solution, the sum of mass concentration of each monomer is 20~45%.
6. the preparation method of comb-type structure amphoteric ion polymer fluid loss additive as claimed in claim 2, which is characterized in that step
It is rapid 2) in, the initiator is the mixture of ammonium persulfate, at least one of potassium peroxydisulfate with sodium hydrogensulfite.
7. the preparation method of comb-type structure amphoteric ion polymer fluid loss additive as claimed in claim 6, which is characterized in that sub-
Mass percent of the niter cake in initiator is 25%~50%.
8. the preparation method of comb-type structure amphoteric ion polymer fluid loss additive as claimed in claims 6 or 7, feature exist
In, initiator in polymerization system a concentration of 0.5%~5%.
9. the preparation method of comb-type structure amphoteric ion polymer fluid loss additive as claimed in claim 2, which is characterized in that step
It is rapid 2) in, the copolyreaction be first at 35~50 DEG C polymerase 10 .5~1.5h, then at 75~85 DEG C polymerize 2.5~3.5h.
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Cited By (4)
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| CN113563539A (en) * | 2021-07-21 | 2021-10-29 | 中国石油大学(华东) | Water-based drilling fluid surface hydration inhibitor and preparation method and application thereof |
| CN113563510A (en) * | 2021-08-09 | 2021-10-29 | 建平天正矿业有限公司 | Temperature-resistant salt-resistant comb polymer fluid loss additive for drilling mud bentonite |
| CN115672261A (en) * | 2022-10-31 | 2023-02-03 | 江苏海洋大学 | Polymer-modified attapulgite containing sulfhydryl Schiff base side group and preparation method thereof |
| CN117645869A (en) * | 2024-01-29 | 2024-03-05 | 广饶县盛泉化工厂 | Emulsion polymer composite fracturing fluid and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113563539A (en) * | 2021-07-21 | 2021-10-29 | 中国石油大学(华东) | Water-based drilling fluid surface hydration inhibitor and preparation method and application thereof |
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| CN117645869A (en) * | 2024-01-29 | 2024-03-05 | 广饶县盛泉化工厂 | Emulsion polymer composite fracturing fluid and preparation method thereof |
| CN117645869B (en) * | 2024-01-29 | 2024-04-12 | 广饶县盛泉化工厂 | Emulsion polymer composite fracturing fluid and preparation method thereof |
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