CN104403645A - Fluid loss agent and preparation method thereof - Google Patents
Fluid loss agent and preparation method thereof Download PDFInfo
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- CN104403645A CN104403645A CN201410617819.2A CN201410617819A CN104403645A CN 104403645 A CN104403645 A CN 104403645A CN 201410617819 A CN201410617819 A CN 201410617819A CN 104403645 A CN104403645 A CN 104403645A
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- 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
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
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- 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
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
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Abstract
The invention discloses a high temperature resistant fluid loss agent for drilling fluids, and a preparation method thereof. The fluid loss agent is formed by copolymerizing 2-methyl-2-acrylamidopropylsulfonic acid, acrylamide, N,N-dimethyldiallylammonium chloride and sodium p-styrene sulfonate according to a molar ratio of 3-6:6-9:1-2:1-2. The preparation method comprises the following steps: blending four monomers, mixing, introducing nitrogen to remove oxygen, adding an initiator in a dropwise manner when a specified temperature is reached to initiate a copolymerization reaction in order to obtain a sticky jelly, repeatedly extracting with anhydrous ethanol, and carrying out Soxhlet extraction and organic solvent dissolving to remove impurities in order to obtain the pure and dry copolymer fluid loss agent. The fluid loss agent has good rheological performance and filtration loss performance in freshwater drilling fluids and brine drilling fluids, and has a good temperature resistance; and an adsorption hydration group in the molecular structure of the fluid loss agent reacts with clay, so the particle size of clay particles is changed, the zeta potential of the surface of clay micelles is changed, and a formed filter cake is thin and compact and has a low permeability, thereby the filtration loss is effectively reduced.
Description
Technical field
The present invention relates to a kind of filtrate reducer for drilling fluid, particularly relate to a kind of drilling fluid high temperature resistance copolymer analog fluid loss agent and preparation method thereof.
Background technology
Fast development along with modern petroleum industry and the continuous increase to petroleum demand amount, drilling strata is increasingly sophisticated, bore meet deep-well, ultra deep well get more and more, bottom temperature even reach 200 DEG C and more than, this proposes huge challenge to modern drilling process technology.
Fluid loss agent, as one of most important treatment agent of drilling fluid, plays an important role to the safe, fast, efficient drilling well of guarantee.And the deep-well subsurface environment of High Temperature High Pressure make typical well liquid fluid loss agent generation high-temperature cross-linking, high temperature degradation, high-temperature thickening etc. make its leak-off and rheological out of hand, typical well liquid fluid loss agent can not meet deep & ultra-deep well drilling well needs, therefore, the research and development of high temperature resistant drilling fluids fluid loss agent are most crucial contents.
At present, existing heat resisting fluid loss reducing agent is mainly divided into natural/flocculation compound and synthetic polymer class fluid loss agent.Natural/flocculation compounds fluid loss agent (mainly comprising Mierocrystalline cellulose, starch, humic acid and modified product thereof) is mainly used in boring meets the deep-well that bottom temperature is no more than 180 DEG C, and therefore its use range is restricted.And polymer class fluid loss agent is obtained by the mutual addition of carbon bond that is unsaturated or ring-type, generally using-C-C-key as the main chain of copolymer molecule, the functional groups on monomer is generally on the side chain of multipolymer.In multipolymer polymer, the fracture of-C-C-key needs very high energy, even if envrionment temperature is very high, also not easily ruptures.Therefore, the main chain of this type of fluid loss agent is more stable compared with the fluid loss agent of other types, and temperature resistance ability is stronger, and use temperature is higher.
On the whole, the polymer filtrate reducer relative molecular weight that prior art uses is higher, under high temperature and high salt condition, better filtrate reducing effect is played for making it, its consumption must be strengthened, the unfavorable factor brought like this or cause drilling fluid system viscosity to increase or make its rheological wayward due to polymkeric substance high-temperature thickening, high temperature degradation, high-temperature cross-linking etc.Drilling well needs within existing High Temperature High Pressure fluid loss agent sulfonated phenol formaldehyde resin (SMP-1 and SMP-2) can meet 200 DEG C substantially, but the control of salt solution and saturated brine high temperature and high pre ssure filtration and rheological under ultra-high temperature condition can not be met.
Summary of the invention
The present invention is directed to above-mentioned shortcoming, from the mechanism of action of polymer filtrate reducer, provide a kind of heat resisting fluid loss reducing agent and preparation method thereof for this technical barrier of high temperature resistance simultaneously.
The invention discloses a kind of fluid loss agent, it is that raw material reaction is prepared from primarily of 2-methyl-2-acryamidopropanesulfonic acid, acrylamide, N, N-dimethyl diallyl ammonium chloride, sodium p styrene sulfonate, and reaction formula is:
The mol ratio of described raw material 2-methyl-2-acryamidopropanesulfonic acid, acrylamide, N, N-dimethyl diallyl ammonium chloride and sodium p styrene sulfonate is 3 ~ 6:6 ~ 9:1 ~ 2:1 ~ 2.
The invention also discloses a kind of method of fluid loss agent, comprise the following steps:
A. described 2-methyl-2-acryamidopropanesulfonic acid is dissolved in distilled water, then adds in ice-water bath and the equimolar sodium hydroxide of described 2-methyl-2-acryamidopropanesulfonic acid;
B. the pH of regulating step solution A is 4 ~ 13, adds described acrylamide, described N, N-dimethyl diallyl ammonium chloride and described sodium p styrene sulfonate afterwards successively, and passes into the continuous mix and blend of nitrogen and heat;
Wherein, as preferably, be 4 ~ 13 with the pH of one or more regulating step solution A in sodium hydroxide, potassium hydroxide, ammonium hydroxide.
C. when temperature reaches 50 ~ 120 DEG C, initiator is dripped in mixing solutions, described initiator dosage is 2-methyl-2-acryamidopropanesulfonic acid, acrylamide, N, 0.1% ~ 1.0% of N-dimethyl diallyl ammonium chloride and sodium p styrene sulfonate four kinds of material total masses, carry out insulation reaction afterwards and obtain thick jelly in 5 ~ 7 hours; Wherein, described initiator is ammonium persulphate.
D. by described viscous gum organic solvent extraction, carry out separating-purifying, and obtain described fluid loss agent 40 ~ 70 DEG C of vacuum drying oven dryings;
Wherein in steps A, the consumption of distilled water controls between 10% ~ 35% for making total monomer concentration.
Wherein, as preferably, the organic solvent extraction 2 ~ 4 times of viscous gum described in step D.
In the present invention, the product apparatus,Soxhlet's after described extraction is carried out separating-purifying.Be specially, the product after described extraction soaked 24 ~ 72h at organic solvent, then in apparatus,Soxhlet's, uses dehydrated alcohol extracting.
As preferably in the present invention, described organic solvent is one or more in dehydrated alcohol, Virahol, ethyl acetate, acetone, chloroform, ether, tetrahydrofuran (THF), benzene, toluene, hexanaphthene.
The present invention adopts solution polymerization process easy, simple to operate, and condition is easy to control, and cost is low, and productive rate is high; This fluid loss agent high temperature resistance, salt resistant character are better, all have stream preferably to become and filtration property in fresh-water drilling fluid, 4% salt-water drilling fluid, saturated salt-water drilling fluid; The filter cake formed is thin, and fine and close, rate of permeation low energy effectively reduces filter loss; Better with drilling fluid compatibleness, be applicable to deep-well and ultra-deep well drilling needs.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the invention will be further described:
Fig. 1 is the infrared spectrogram of fluid loss agent prepared by the embodiment of the present invention 1;
Fig. 2 is the proton nmr spectra of fluid loss agent prepared by the embodiment of the present invention 1.
Embodiment
Below in conjunction with the embodiment in the present invention and accompanying drawing, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
Be dissolved in 95mL deionized water by 2-methyl-2-acryamidopropanesulfonic acid (AMPS) 20.72g, in ice-water bath, with 4.0g NaOH, AMPS be converted into equimolar sodium salt, be 10 with sodium hydrate regulator solution pH simultaneously.Again by acrylamide (AM) 9.95g, N, N-dimethyl diallyl ammonium chloride (DMDAAC) 10.8mL, sodium p styrene sulfonate (SSS) 4.12g mix with the AMPS solution after neutralization, add in the four-hole boiling flask of band thermometer, reflux, stir, logical nitrogen deoxygenation.Temperature of reaction is set as 75 DEG C.Logical nitrogen is after 30 minutes, and when temperature rises to 75 DEG C, add 0.33g ammonium persulfate initiator in flask, insulation reaction 6 hours, obtains thick jelly, then with dehydrated alcohol, this jelly is extracted 3 times repeatedly; Again extraction product to be soaked in acetone 48h to remove residual impurity, and then in apparatus,Soxhlet's with dehydrated alcohol extracting to remove unreacted monomer and initiator; At finally products therefrom being placed in 50 DEG C, vacuum-drying removes dehydrated alcohol, obtains final product, and productive rate is 88.7%.
Embodiment 2
Be dissolved in 700mL deionized water by 2-methyl-2-acryamidopropanesulfonic acid (AMPS) 31.09g, in ice-water bath, with 6.0g NaOH, AMPS be converted into equimolar sodium salt, be 4 with potassium hydroxide regulator solution pH simultaneously.Again by acrylamide 21.3g, N, N-dimethyl diallyl ammonium chloride 13.5mL, sodium p styrene sulfonate 15.45g mix with the AMPS solution after neutralization, add in the four-hole boiling flask of band thermometer, reflux, stir, logical nitrogen deoxygenation.Temperature of reaction is set as 120 DEG C.Logical nitrogen is after 30 minutes, and when temperature rises to 120 DEG C, add 0.76g ammonium persulfate initiator in flask, insulation reaction 5 hours, obtains thick jelly, then with dehydrated alcohol, this jelly is extracted 2 times repeatedly; Again extraction product to be soaked in acetone 24h to remove residual impurity, and then in apparatus,Soxhlet's with dehydrated alcohol extracting to remove unreacted monomer and initiator; At finally products therefrom being placed in 40 DEG C, vacuum-drying removes dehydrated alcohol, obtains final product, and productive rate is 83.4%.
Embodiment 3
Be dissolved in 500mL deionized water by 2-methyl-2-acryamidopropanesulfonic acid (AMPS) 62.17g, in ice-water bath, with 12.0g NaOH, AMPS be converted into equimolar sodium salt, be 13 with ammonium hydroxide regulator solution pH simultaneously.Again by acrylamide 31.95g, N, N-dimethyl diallyl ammonium chloride 27.0mL, sodium p styrene sulfonate 20.6g mix with the AMPS solution after neutralization, add in the four-hole boiling flask of band thermometer, reflux, stir, logical nitrogen deoxygenation.Temperature of reaction is set as 50 DEG C.Logical nitrogen is after 30 minutes, and when temperature rises to 50 DEG C, add 0.22g ammonium persulfate initiator in flask, insulation reaction 7 hours, obtains thick jelly, then with dehydrated alcohol, this jelly is extracted 4 times repeatedly; Again extraction product to be soaked in acetone 72h to remove residual impurity, and then in apparatus,Soxhlet's with dehydrated alcohol extracting to remove unreacted monomer and initiator; At finally products therefrom being placed in 70 DEG C, vacuum-drying removes dehydrated alcohol, obtains final product, and productive rate is 79.8%.
The above-mentioned fluid loss agent structural characterization produced is as follows:
Fig. 1 is the infrared spectrogram of fluid loss agent, is analyzed as follows:
3437.69cm
-1the N-H stretching vibration absorption peak of the primary amine in corresponding acrylamide, 3196.69cm
-1the N-H stretching vibration absorption peak of secondary amine in corresponding 2-methyl-2-acryamidopropanesulfonic acid, 2931.90cm
-1-CH in corresponding 2-methyl-2-acryamidopropanesulfonic acid and N, N-dimethyl diallyl ammonia chloride
3c-H stretching vibration absorption peak, 1666.79cm
-1the stretching vibration absorption peak of C=O in corresponding 2-methyl-2-acryamidopropanesulfonic acid and acrylamide, 1553.72cm
-1and 1458.50cm
-1the charateristic avsorption band of phenyl ring in corresponding sodium p styrene sulfonate, 1416.84cm
-1and 1387.08cm
-1the stretching vibration absorption peak 1366.25cm of five-membered ring is produced after the polymerization of corresponding N, N-dimethyl diallyl ammonia chloride
-1-CH in corresponding 2-methyl-2-acryamidopropanesulfonic acid and N, N-dimethyl diallyl ammonia chloride
3middle C-H in-plane bending vibration absorption peak, 1303.77cm
-1for N-H in-plane bending vibration in amide group, 1190.70,1122.26,1038.94,1006.21cm
-1-SO in corresponding 2-methyl-2-acryamidopropanesulfonic acid and sodium p styrene sulfonate
3-charateristic avsorption band, and at 1650-1620cm
-1do not have absorption peak to prove not C=C, can be obtained by analysis, synthetic product is the tetrapolymer of AMPS/AM/DMDAAC/SSS.
Fig. 2 is the hydrogen nuclear magnetic resonance spectrogram of fluid loss agent, is analyzed as follows:
H
1in NMR, the absorption peak of the proton in the corresponding sodium p styrene sulfonate of 7.56ppm, 7.18ppm on phenyl ring, the multiple proton uptake peak of N-H in primary amide in the corresponding acrylamide of 5.85-5.92ppm, the multiple proton uptake peak of N-H in the corresponding 2-methyl of 5.51-5.59ppm-2-acryamidopropanesulfonic acid secondary amide, the corresponding solvent D of 4.50-4.79ppm
2the complicated absorption peak of O, 3.47, the corresponding N of 3.50ppm, the proton uptake peak of N-dimethyl diallyl ammonia chloride neutralization, proton uptake peak in the corresponding 2-methyl of 1.60ppm-2-acryamidopropanesulfonic acid, proton uptake peak in the corresponding 2-methyl of 2.86ppm-2-acryamidopropanesulfonic acid, 2.98ppm correspondence connects the proton uptake peak of phenyl ring, in the corresponding molecular backbone chain structure of 1.47ppm proton uptake peak, other absorption peaks may be due to introduce in the polishing purification process of polymkeric substance ethanol impurity etc. completely removing cause.Can draw in conjunction with Infrared spectroscopy, tetrapolymer is successfully prepared.
Embodiment 4
Above-mentioned copolymer fluid loss agent is in fresh-water drilling fluid, 4% salt-water drilling fluid, saturated salt-water drilling fluid aging front and back rheological property and filtration property.
According to SYT56211993 test procedure for drilling fluids method
A. fresh-water drilling fluid
Copolymer fluid loss agent dosage affects in table 1 fresh-water drilling fluid rheological property and filtration property
Table 1
In above-mentioned table 1, AV-apparent viscosity; PV-plastic viscosity; YP-yield value; FL
(API)press filtration vector in-normal temperature
FL
(HTHP)-high temperature and high pre ssure filtration; Wherein high temperature and high pre ssure filtration test condition is: (180 DEG C, 3.5MPa)
From above-mentioned table 1, along with the increase of polymer content, aging front and back apparent viscosity, plastic viscosity, yield value all present ascendant trend, but ascensional range is not too large, illustrate that the Efficient Adhesive Promotion of tetrapolymer fluid loss agent is not obvious, the rheological of drilling fluid is easily controlled.But its rheological parameter declines all to some extent after aging.When polymkeric substance dosage is 1.2% time, can control aging front API filtration is 6.4mL, and after 180 DEG C of aging 16h, API filtration is 9.6mL, and high temperature and high pre ssure filtration controls at about 20mL.
B.4% salt-water drilling fluid
Copolymer fluid loss agent dosage on 4% salt-water drilling fluid rheological property and filtration property impact in table 2
Table 2
From above-mentioned table 2, along with the increase of copolymer fluid loss agent content, aging front API filtration entirety is in the trend reduced, the aging front API filtration of 4% salt-water drilling fluid is up to 80mL, after adding fluid loss agent, API filtration declines obviously, when dosage is 1.0%, can be controlled in below 10mL, continue the content F L increasing fluid loss agent
(API)change less, substantially tend towards stability.The salt-water drilling fluid of 4% is after 180 DEG C of aging 16h, and viscosity and shear force decline all to some extent, its FL
(API)and FL
(HTHP)all reduce gradually with the increase of copolymer fluid loss agent dosage, when dosage is 1.5%, FL
(API)for and FL
(HTHP)all can be effectively controlled.
C. saturated salt-water drilling fluid
Copolymer fluid loss agent dosage affects in table 3 saturated salt-water drilling fluid rheological property and filtration property
Table 3
From above-mentioned table 3, along with the increase of copolymer fluid loss agent content, aging front API filtration entirety is in the trend reduced, the aging front API filtration of saturated salt-water drilling fluid is up to 130mL, after adding fluid loss agent, API filtration declines obvious, when dosage is 1.0%, can be controlled in below 10mL, continue the content F L increasing fluid loss agent
(API)change relatively little, even when AMPS/AM/DMDAAC/SSS massfraction is 2.0%, within normal temperature API filtration can be controlled in 5mL, saturated salt-water drilling fluid is after 180 DEG C of aging 16h, viscosity and shear force decline all to some extent, but downtrending is not obvious, the rheological of aging front and back saturated salt-water drilling fluid still can all control effectively.Its FL
(API)and FL
(HTHP)all reduce gradually with the increase of copolymer fluid loss agent dosage, when dosage is 2.0%, FL
(API)for and FL
(HTHP)all can be effectively controlled.
Embodiment 5
Above-mentioned copolymer fluid loss agent heat-resisting property test
Multipolymer-drilling fluid system, the rheological property of drilling fluid system and filtration property under different aging temperatures.The concrete steps of this evaluation experimental are: the AM/AMPS/DMDAAC/SSS tetrapolymer fluid loss agent of 2.0% is added 400ml tri-kinds of drilling fluid bases slurry (wilkinite massfraction is 4.0%).Keep agitation is after copolymer fluid loss agent dissolves completely, by drilling fluid 120 DEG C, 150 DEG C, 180 DEG C, 200 DEG C high temperature ageings 16 hours, test the rheological of aging rear drilling fluid, API filtration and high temperature and high pre ssure filtration (180 DEG C, 3.5MPa), experimental result sees the following form 4.
Table 4
From above-mentioned table 4, between 120-200 DEG C, AV, PV, YP of three kinds of drilling fluid systems all raise with temperature and constantly reduce; Especially between 180-200 DEG C, AV, PV downtrending is obvious, illustrates that copolymer fluid loss agent decomposed causes caused by viscosity degradation when temperature is higher than 180 DEG C, but the filter loss (FL of 3 kinds of drilling fluid systems
(API)and FL
(HTHP)) all increase with the rising of temperature, after fresh-water drilling fluid adds polymer filtrate reducer process, aging 16h at 200 DEG C, can control aging after FL
(API)be only 13mL, high temperature and high pre ssure filtration FL can be controlled
(HTHP)within 50mL; After 4% salt-water drilling fluid adds polymer filtrate reducer process, aging 16h at 200 DEG C, can control aging after FL
(API)at about 25mL, high temperature and high pre ssure filtration FL can be controlled
(HTHP)within 80mL; After saturated salt-water drilling fluid adds polymer filtrate reducer process, aging 16h at 200 DEG C, can control aging after FL
(API)within 30mL, high temperature and high pre ssure filtration FL can be controlled
(HTHP)within 100mL.Illustrate that the multipolymer water retaining of synthesis has stronger temperature resistance ability thus.Temperature resistance can reach about 200 DEG C.
Above test result result shows, the heat resisting fluid loss reducing agent of the present embodiment has good rheological property and filtrate loss controllability at fresh-water drilling fluid, 4.0wt% salt-water drilling fluid, saturated salt-water drilling fluid base slurry, and property of drilling fluid changes after 200 DEG C of aging 16h, but substantially effectively can also control filter loss, be applicable to deep drilling needs.
Above-mentioned embodiment is intended to illustrate that the present invention can be professional and technical personnel in the field and realizes or use; modifying to above-mentioned embodiment will be apparent for those skilled in the art; therefore the present invention includes but be not limited to above-mentioned embodiment; any these claims or specification sheets of meeting describes; meet and principle disclosed herein and novelty, the method for inventive features, technique, product, all fall within protection scope of the present invention.
Claims (8)
1. a fluid loss agent, is characterized in that, it is that raw material reaction is prepared from primarily of 2-methyl-2-acryamidopropanesulfonic acid, acrylamide, N, N-dimethyl diallyl ammonium chloride, sodium p styrene sulfonate;
The mol ratio of described raw material 2-methyl-2-acryamidopropanesulfonic acid, acrylamide, N, N-dimethyl diallyl ammonium chloride and sodium p styrene sulfonate is 3 ~ 6:6 ~ 9:1 ~ 2:1 ~ 2.
2. prepare a fluid loss agent method as claimed in claim 1, it is characterized in that, comprise the following steps:
A. described 2-methyl-2-acryamidopropanesulfonic acid is dissolved in distilled water, then in ice-water bath, adds the sodium hydroxide with described 2-methyl-2-acryamidopropanesulfonic acid equimolar amount;
B. the pH of regulating step solution A is 4 ~ 13, adds described acrylamide, described N, N-dimethyl diallyl ammonium chloride and described sodium p styrene sulfonate afterwards successively, and passes into the continuous mix and blend of nitrogen and heat;
C. when temperature reaches 50 ~ 120 DEG C, initiator is dripped in mixing solutions, described initiator dosage is described 2-methyl-2-acryamidopropanesulfonic acid, described acrylamide, described N, 0.1% ~ 1.0% of N-dimethyl diallyl ammonium chloride and described sodium p styrene sulfonate four kinds of material total masses, carry out insulation reaction afterwards and obtain thick jelly in 5 ~ 7 hours;
D. by described viscous gum organic solvent extraction, carry out separating-purifying, and obtain described fluid loss agent 40 ~ 70 DEG C of vacuum drying oven dryings;
Wherein in steps A, the consumption of distilled water controls between 10% ~ 35% for making total monomer concentration.
3. the preparation method of fluid loss agent according to claim 2, is characterized in that, with sodium hydroxide, potassium hydroxide in step B, the pH of one or more regulating step solution A in ammonium hydroxide is 4 ~ 13.
4. the preparation method of fluid loss agent according to claim 2, is characterized in that, described initiator is ammonium persulphate.
5. the preparation method of fluid loss agent according to claim 2, is characterized in that, the organic solvent extraction 2 ~ 4 times of viscous gum described in step D.
6. the preparation method of fluid loss agent according to claim 2, is characterized in that, the product apparatus,Soxhlet's after described extraction is carried out separating-purifying.
7. the preparation method of fluid loss agent according to claim 6, is characterized in that, the product after described extraction is soaked 24 ~ 72h at organic solvent, then in apparatus,Soxhlet's, uses dehydrated alcohol extracting.
8. the preparation method of the fluid loss agent according to claim 2, any one of 5-7, it is characterized in that, described organic solvent is the mixture of one or more arbitrary proportions in dehydrated alcohol, Virahol, ethyl acetate, acetone, chloroform, ether, tetrahydrofuran (THF), benzene, toluene, hexanaphthene.
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| CN106432632A (en) * | 2016-09-27 | 2017-02-22 | 西南石油大学 | Amido polymer filtrate loss reducer for water-based drilling fluid resistant to high temperature, salt and calcium and preparation method and application thereof |
| CN108264890A (en) * | 2018-01-22 | 2018-07-10 | 中国石油大学(华东) | A kind of preparation method of micro-cross-linked water-base drilling fluid fluid loss additive |
| CN108641683A (en) * | 2018-03-30 | 2018-10-12 | 中国石油大学(华东) | A kind of high temperature resistance high salinity high-density water-based drilling fluid and its application |
| GB2568777A (en) * | 2017-09-25 | 2019-05-29 | China Petroleum & Chem Corp | Random copolymer, preparation method and use thereof, and drilling fluid |
| CN111621271A (en) * | 2020-05-11 | 2020-09-04 | 中国石油大学(北京) | Saturated saline drilling fluid of salt response type intelligent polymer and preparation method thereof |
| CN115677900A (en) * | 2022-11-05 | 2023-02-03 | 西南石油大学 | High-temperature high-density saturated salt water drilling fluid and preparation method thereof |
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