CN108251085A - A kind of salt-resisting high-temperature-resisting fluid loss additive and preparation method thereof - Google Patents
A kind of salt-resisting high-temperature-resisting fluid loss additive and preparation method thereof Download PDFInfo
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- CN108251085A CN108251085A CN201711468464.5A CN201711468464A CN108251085A CN 108251085 A CN108251085 A CN 108251085A CN 201711468464 A CN201711468464 A CN 201711468464A CN 108251085 A CN108251085 A CN 108251085A
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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
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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
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
Abstract
This application discloses a kind of salt-resisting high-temperature-resisting fluid loss additives and preparation method thereof, purpose is, for polymerization species fluid loss additive under the conditions of stratum high-temperature high content of salt, under the premise of filtrate reducing effect is ensured, the high temperature resistance and salt-resistance of fluid loss additive are improved, used technical solution is：Fluid loss additive is made after copolymerization under conditions of initiator and chain-transferring agent by monomer；The monomer includes the N that mass fraction is 5~25 parts, the N vinylpyrrolidones that N dimethacrylamide, mass fraction are 2~5 parts, the acrylic acid that mass fraction is 20~60 parts, 2 acrylamide, 2 methyl propane sulfonic acid that mass fraction is 10~50 parts and the dimethyl diallyl ammonium chloride that mass fraction is 2~10 parts.
Description
Technical field
This application involves petroleum drilling technology fields, and in particular to a kind of salt-resisting high-temperature-resisting fluid loss additive and its preparation side
Method, for polymerization species fluid loss additive degrade under the conditions of stratum high-temperature, high content of salt failure and viscosity effect it is big etc. actually
Problem.
Background technology
With the increasing of deep formation oil-gas exploration and development dynamics, the Special Drilling Operations ring such as high temperature, high pressure and high content of salt
Border brings the challenge of bigger to drilling fluid construction.One of the core processing agent of fluid loss additive as drilling fluid, the height of performance
It is low often to determine that construction carry out safe, fast, efficiently.Polymerizeing species fluid loss additives has that environmental protection, dosage be low, sexual valence
Than high advantage, but during practice of construction, high temperature degradation failure, high density well slurry medium viscosity effect is big, affects it
Promote the use of, also limit the development of high-temperature high-density drilling fluid to a certain extent.
The method for improving polymerization species fluid loss additive performance at present mainly has：
(1) it introduces to clay adsorption compared with strong, the firm sulfonic acid group of hydration shell (- SO3H)；
(2) cation is introduced, improves the adsorption capacity of inorganic agent and clay；
(3) while polymeric water-soluble is not changed, surfactant is introduced, changes clay surface wettability；
(4) the strong group of hydrolytic stability is introduced, improves the heat-resisting property of product, such as n-vinyl pyrrolidone (NVP),
While temperature resistance is improved, there is certain inhibition.
At present, natural products is modified and polymerization species fluid loss additive is two more commonly used major class fluid loss additives, using than
It is wide.Wherein, the fluid loss additive formed by the modification of the natural products such as starch, cellulose and tannin, raw material sources enrich, price
Relative moderate, production technology is also easier, ripe, but such fluid loss additive temperature resistance ability and contamination resistance are poor, and scene should
Drilling fluid rheology is caused to be deteriorated with vulnerable in the process, filter loss is substantially increased.Synthesized polymer species fluid loss additive has
Certain temperature resistance and contamination resistance, water-disintegrable good, performance is stablized, and has been widely used in oil field development.It polymerize species drop filter
It loses agent active group under the higher alkaline condition of temperature and irreversible hydrolysis, degradation easily occurs, water middle-jiao yang, function of the spleen and stomach when salinity is higher
Ion can generate compression double electric layer effect, and polymer molecular chain is made to curl degree increase, and filtrate reducing effect is deteriorated.In ground floor height
Under the conditions of temperature, high content of salt, there are the practical problems such as degradation is failed and viscosity effect is big in polymerization species fluid loss additive, therefore grind
The polymerization species fluid loss additive for studying carefully high temperature resistance and salt-resistance has practical application value.
Invention content
In order to solve the problems in the prior art, present applicant proposes a kind of salt-resisting high-temperature-resisting fluid loss additive and its preparation sides
Method under the premise of filtrate reducing effect is ensured, improves the high temperature resistance and salt-resistance of fluid loss additive.
In order to achieve the goal above, technical solution is used by the application：
A kind of salt-resisting high-temperature-resisting fluid loss additive, the fluid loss additive be by monomer under conditions of initiator and chain-transferring agent
It is made after copolymerization；The monomer includes the N,N-DMAA that mass fraction is 5~25 parts, mass fraction 2
~5 parts of N- vinylpyrrolidones, the acrylic acid that mass fraction is 20~60 parts, the 2- acryloyls that mass fraction is 10~50 parts
Amine -2- methyl propane sulfonic acids and the dimethyl diallyl ammonium chloride that mass fraction is 2~10 parts.
The initiator is potassium peroxydisulfate and sodium hydrogensulfite.
The chain-transferring agent is sodium formate.
A kind of preparation method of salt-resisting high-temperature-resisting fluid loss additive, includes the following steps：
1) 2- acrylamide-2-methyl propane sulfonics and acrylic acid is taken to be dissolved in deionized water and obtain solution A, and in cooling
Under the conditions of the pH value of solution A is adjusted to 8~10；
2) N,N-DMAA, N- vinylpyrrolidones, dimethyl diallyl ammonium chloride and chain-transferring agent are taken
Solution is added in solution A and is sufficiently stirred, and obtains solution B；
3) solution B is put into after leading to nitrogen deoxygenation in reactor and initiator solution is added dropwise, under nitrogen protection constant temperature to 80
~95 DEG C of reactions, obtain sticky flowable liquids C；
4) after sticky flowable liquids C being dried in vacuo and crushed successively, it is filtrate reducing to obtain pulverulent solids
Agent.
2- acrylamide-2-methyl propane sulfonics, acrylic acid, N,N-DMAA, N- ethylene pyrroles in the solution B
The total mass concentration of pyrrolidone and dimethyl diallyl ammonium chloride is 15~25%.
2- acrylamide-2-methyl propane sulfonics, acrylic acid, N,N-DMAA, N- ethylene pyrroles in the solution B
The total mass concentration of pyrrolidone and dimethyl diallyl ammonium chloride is preferably 20%.
The fluid loss additive includes the N,N-DMAA that mass fraction is 5~25 parts, mass fraction be 2~
5 parts of N- vinylpyrrolidones, the acrylic acid that mass fraction is 20~60 parts, the 2- acryloyls that mass fraction is 10~50 parts
Amine -2- methyl propane sulfonic acids and the dimethyl diallyl ammonium chloride that mass fraction is 2~10 parts.
Sodium formate solution of the chain-transferring agent solution for a concentration of 0.1mol/L, the addition mass fraction of sodium formate solution
It is 1.5~10 parts.
The initiator solution is a concentration of 0.1mol/L mixed solutions prepared by potassium peroxydisulfate and sodium hydrogensulfite, is drawn
The addition mass fraction for sending out agent solution is 1~5 part.
Sodium hydrate aqueous solution that mass concentration is 30% is added in solution A in the step 1) by the pH value of solution A
It is adjusted to 8~10.
Compared with prior art, the application is made by monomer after copolymerization under conditions of initiator and chain-transferring agent,
The polymer of synthesis introduces N- vinylpyrrolidones (NVP), N,N-DMAA (DMAM), dimethyl two in the molecule
Allyl ammonium chloride (DMDAAC) etc. not facile hydrolysis, degradation nonhydratable group, the five-ring heterocycles of N- vinylpyrrolidones (NVP)
And the methyl side groups of N,N-DMAA (DMAM) improve molecule chain rigidity and have hydrophobic shielding action, improve
The hydrolysis degradation resistant ability of product, cationic introducing, improves product in dimethyl diallyl ammonium chloride (DMDAAC)
Adsorption capacity on bentonite surface.Acrylic acid (AA), 2- acrylamide-2-methyl propane sulfonics (AMPS) have carboxyl and sulphur
Two kinds of aquation groups of acidic group, the proper ratio of the two assign product saline-alkaline tolerance, and the fluid loss additive of the application passes through infrared spectrum
Analysis, thermogravimetic analysis (TGA), filtrate loss controllability analysis etc., the fluid loss additive for demonstrating the application has very low viscosity effect,
Under the premise of ensureing filtrate reducing effect, the high temperature resistance and salt-resistance of fluid loss additive are improved, fluid loss additive still has before 280 DEG C
Good thermal stability also has good filtrate reducing effect under saturated sodium-chloride saltwater environment.
Description of the drawings
In order to illustrate more clearly of the technical solution of the application, letter will be made to attached drawing needed in the embodiment below
Singly introduce.
Fig. 1 is the infrared spectrum analysis figure of the fluid loss additive of the application；
Fig. 2 is the thermogravimetic analysis (TGA) figure of the fluid loss additive of the application.
Specific embodiment
The application is further explained with reference to specific embodiment and Figure of description.
Attached drawing herein is incorporated into specification and forms the part of this specification, shows the implementation for meeting the application
Example, and for explaining the principle of the application together with specification.
Embodiment 1：
Fluid loss additive is made after copolymerization under conditions of initiator and chain-transferring agent by monomer；Monomer includes quality
N,N-DMAA that number is 5 parts, the N- vinylpyrrolidones that mass fraction is 2 parts, mass fraction are 20 parts
The 2- acrylamide-2-methyl propane sulfonics that acrylic acid, mass fraction are 10 parts and the dimethyl diallyl that mass fraction is 2 parts
Ammonium chloride.Initiator is potassium peroxydisulfate and sodium hydrogensulfite.Chain-transferring agent is sodium formate.
Based on above proportioning, the present embodiment preparation method includes the following steps：
1) 2- acrylamide-2-methyl propane sulfonics and acrylic acid is taken to be dissolved in deionized water and obtain solution A, and in cooling
Under the conditions of add in mass concentration be 30% sodium hydrate aqueous solution the pH value of solution A is adjusted to 8；
2) N,N-DMAA, N- vinylpyrrolidones, dimethyl diallyl ammonium chloride and chain-transferring agent are taken
Solution is added in solution A and is sufficiently stirred, and obtains solution B；Chain-transferring agent solution is the sodium formate solution of a concentration of 0.1mol/L,
The addition mass fraction of sodium formate solution is 1.5 parts.
3) solution B is put into after leading to nitrogen deoxygenation in reactor and initiator solution is added dropwise, under nitrogen protection constant temperature to 80
~95 DEG C of reactions, obtain sticky flowable liquids C；Initiator solution is a concentration of to be prepared by potassium peroxydisulfate and sodium hydrogensulfite
0.1mol/L mixed solutions, the addition mass fraction of initiator solution is 1 part.
4) after sticky flowable liquids C being dried in vacuo and crushed successively, it is filtrate reducing to obtain pulverulent solids
Agent.
2- acrylamide-2-methyl propane sulfonics, acrylic acid, N,N-DMAA, N- vinyl pyrrolidines in solution B
The total mass concentration of ketone and dimethyl diallyl ammonium chloride is 15%.
Embodiment 2：
Fluid loss additive is made after copolymerization under conditions of initiator and chain-transferring agent by monomer；Monomer includes quality
N,N-DMAA that number is 10 parts, the N- vinylpyrrolidones that mass fraction is 3 parts, mass fraction are 30 parts
The 2- acrylamide-2-methyl propane sulfonics that acrylic acid, mass fraction are 20 parts and the dimethyl diallyl that mass fraction is 4 parts
Ammonium chloride.Initiator is potassium peroxydisulfate and sodium hydrogensulfite.Chain-transferring agent is sodium formate.
Based on above proportioning, the present embodiment preparation method includes the following steps：
1) 2- acrylamide-2-methyl propane sulfonics and acrylic acid is taken to be dissolved in deionized water and obtain solution A, and in cooling
Under the conditions of add in mass concentration be 30% sodium hydrate aqueous solution the pH value of solution A is adjusted to 9；
2) N,N-DMAA, N- vinylpyrrolidones, dimethyl diallyl ammonium chloride and chain-transferring agent are taken
Solution is added in solution A and is sufficiently stirred, and obtains solution B；Chain-transferring agent solution is the sodium formate solution of a concentration of 0.1mol/L,
The addition mass fraction of sodium formate solution is 3 parts.
3) solution B is put into after leading to nitrogen deoxygenation in reactor and initiator solution is added dropwise, under nitrogen protection constant temperature to 80
~95 DEG C of reactions, obtain sticky flowable liquids C；Initiator solution is a concentration of to be prepared by potassium peroxydisulfate and sodium hydrogensulfite
0.1mol/L mixed solutions, the addition mass fraction of initiator solution is 2 parts.
4) after sticky flowable liquids C being dried in vacuo and crushed successively, it is filtrate reducing to obtain pulverulent solids
Agent.
2- acrylamide-2-methyl propane sulfonics, acrylic acid, N,N-DMAA, N- vinyl pyrrolidines in solution B
The total mass concentration of ketone and dimethyl diallyl ammonium chloride is 20%.
Embodiment 3：
Fluid loss additive is made after copolymerization under conditions of initiator and chain-transferring agent by monomer；Monomer includes quality
N,N-DMAA that number is 15 parts, the N- vinylpyrrolidones that mass fraction is 4 parts, mass fraction are 40 parts
The 2- acrylamide-2-methyl propane sulfonics that acrylic acid, mass fraction are 30 parts and the dimethyl diallyl that mass fraction is 6 parts
Ammonium chloride.Initiator is potassium peroxydisulfate and sodium hydrogensulfite.Chain-transferring agent is sodium formate.
Based on above proportioning, the present embodiment preparation method includes the following steps：
1) 2- acrylamide-2-methyl propane sulfonics and acrylic acid is taken to be dissolved in deionized water and obtain solution A, and in cooling
Under the conditions of add in mass concentration be 30% sodium hydrate aqueous solution the pH value of solution A is adjusted to 10；
2) N,N-DMAA, N- vinylpyrrolidones, dimethyl diallyl ammonium chloride and chain-transferring agent are taken
Solution is added in solution A and is sufficiently stirred, and obtains solution B；Chain-transferring agent solution is the sodium formate solution of a concentration of 0.1mol/L,
The addition mass fraction of sodium formate solution is 5 parts.
3) solution B is put into after leading to nitrogen deoxygenation in reactor and initiator solution is added dropwise, under nitrogen protection constant temperature to 80
~95 DEG C of reactions, obtain sticky flowable liquids C；Initiator solution is a concentration of to be prepared by potassium peroxydisulfate and sodium hydrogensulfite
0.1mol/L mixed solutions, the addition mass fraction of initiator solution is 3 parts.
4) after sticky flowable liquids C being dried in vacuo and crushed successively, it is filtrate reducing to obtain pulverulent solids
Agent.
2- acrylamide-2-methyl propane sulfonics, acrylic acid, N,N-DMAA, N- vinyl pyrrolidines in solution B
The total mass concentration of ketone and dimethyl diallyl ammonium chloride is 25%.
Embodiment 4：
Fluid loss additive is made after copolymerization under conditions of initiator and chain-transferring agent by monomer；Monomer includes quality
N,N-DMAA that number is 20 parts, the N- vinylpyrrolidones that mass fraction is 5 parts, mass fraction are 60 parts
The 2- acrylamide-2-methyl propane sulfonics that acrylic acid, mass fraction are 40 parts and the dimethyl diallyl that mass fraction is 8 parts
Ammonium chloride.Initiator is potassium peroxydisulfate and sodium hydrogensulfite.Chain-transferring agent is sodium formate.
Based on above proportioning, the present embodiment preparation method includes the following steps：
1) 2- acrylamide-2-methyl propane sulfonics and acrylic acid is taken to be dissolved in deionized water and obtain solution A, and in cooling
Under the conditions of add in mass concentration be 30% sodium hydrate aqueous solution the pH value of solution A is adjusted to 9；
2) N,N-DMAA, N- vinylpyrrolidones, dimethyl diallyl ammonium chloride and chain-transferring agent are taken
Solution is added in solution A and is sufficiently stirred, and obtains solution B；Chain-transferring agent solution is the sodium formate solution of a concentration of 0.1mol/L,
The addition mass fraction of sodium formate solution is 8 parts.
3) solution B is put into after leading to nitrogen deoxygenation in reactor and initiator solution is added dropwise, under nitrogen protection constant temperature to 80
~95 DEG C of reactions, obtain sticky flowable liquids C；Initiator solution is a concentration of to be prepared by potassium peroxydisulfate and sodium hydrogensulfite
0.1mol/L mixed solutions, the addition mass fraction of initiator solution is 4 parts.
4) after sticky flowable liquids C being dried in vacuo and crushed successively, it is filtrate reducing to obtain pulverulent solids
Agent.
2- acrylamide-2-methyl propane sulfonics, acrylic acid, N,N-DMAA, N- vinyl pyrrolidines in solution B
The total mass concentration of ketone and dimethyl diallyl ammonium chloride is 18%.
Embodiment 5：
Fluid loss additive is made after copolymerization under conditions of initiator and chain-transferring agent by monomer；Monomer includes quality
N,N-DMAA that number is 25 parts, the N- vinylpyrrolidones that mass fraction is 5 parts, mass fraction are 60 parts
The 2- acrylamide-2-methyl propane sulfonics that acrylic acid, mass fraction are 50 parts and two allyl of dimethyl that mass fraction is 10 parts
Ammonium chloride.Initiator is potassium peroxydisulfate and sodium hydrogensulfite.Chain-transferring agent is sodium formate.
Based on above proportioning, the present embodiment preparation method includes the following steps：
1) 2- acrylamide-2-methyl propane sulfonics and acrylic acid is taken to be dissolved in deionized water and obtain solution A, and in cooling
Under the conditions of add in mass concentration be 30% sodium hydrate aqueous solution the pH value of solution A is adjusted to 8；
2) N,N-DMAA, N- vinylpyrrolidones, dimethyl diallyl ammonium chloride and chain-transferring agent are taken
Solution is added in solution A and is sufficiently stirred, and obtains solution B；Chain-transferring agent solution is the sodium formate solution of a concentration of 0.1mol/L,
The addition mass fraction of sodium formate solution is 10 parts.
3) solution B is put into after leading to nitrogen deoxygenation in reactor and initiator solution is added dropwise, under nitrogen protection constant temperature to 80
~95 DEG C of reactions, obtain sticky flowable liquids C；Initiator solution is a concentration of to be prepared by potassium peroxydisulfate and sodium hydrogensulfite
0.1mol/L mixed solutions, the addition mass fraction of initiator solution is 5 parts.
4) after sticky flowable liquids C being dried in vacuo and crushed successively, it is filtrate reducing to obtain pulverulent solids
Agent.
2- acrylamide-2-methyl propane sulfonics, acrylic acid, N,N-DMAA, N- vinyl pyrrolidines in solution B
The total mass concentration of ketone and dimethyl diallyl ammonium chloride is 20%.
Embodiment 6：
Fluid loss additive is made after copolymerization under conditions of initiator and chain-transferring agent by monomer；Monomer includes quality
N,N-DMAA that number is 22 parts, the N- vinylpyrrolidones that mass fraction is 4 parts, mass fraction are 50 parts
The 2- acrylamide-2-methyl propane sulfonics that acrylic acid, mass fraction are 30 parts and the dimethyl diallyl that mass fraction is 9 parts
Ammonium chloride.Initiator is potassium peroxydisulfate and sodium hydrogensulfite.Chain-transferring agent is sodium formate.
Based on above proportioning, the present embodiment preparation method includes the following steps：
1) 2- acrylamide-2-methyl propane sulfonics and acrylic acid is taken to be dissolved in deionized water and obtain solution A, and in cooling
Under the conditions of add in mass concentration be 30% sodium hydrate aqueous solution the pH value of solution A is adjusted to 9；
2) N,N-DMAA, N- vinylpyrrolidones, dimethyl diallyl ammonium chloride and chain-transferring agent are taken
Solution is added in solution A and is sufficiently stirred, and obtains solution B；Chain-transferring agent solution is the sodium formate solution of a concentration of 0.1mol/L,
The addition mass fraction of sodium formate solution is 7 parts.
3) solution B is put into after leading to nitrogen deoxygenation in reactor and initiator solution is added dropwise, under nitrogen protection constant temperature to 80
~95 DEG C of reactions, obtain sticky flowable liquids C；Initiator solution is a concentration of to be prepared by potassium peroxydisulfate and sodium hydrogensulfite
0.1mol/L mixed solutions, the addition mass fraction of initiator solution is 3 parts.
4) after sticky flowable liquids C being dried in vacuo and crushed successively, it is filtrate reducing to obtain pulverulent solids
Agent.
2- acrylamide-2-methyl propane sulfonics, acrylic acid, N,N-DMAA, N- vinyl pyrrolidines in solution B
The total mass concentration of ketone and dimethyl diallyl ammonium chloride is 20%.
The synthesis material and dosage of the application：
N,N-DMAA (DMAM), dosage are 5~25 mass parts；N- vinylpyrrolidones (NVP), dosage are
2~5 mass parts；Acrylic acid (AA), dosage are 20~60 mass parts；2- acrylamide-2-methyl propane sulfonics (AMPS), dosage are
10~50 mass parts；Dimethyl diallyl ammonium chloride (DMDAAC), dosage are 2~10 mass parts.Initiator is potassium peroxydisulfate
And sodium hydrogensulfite, 0.1mol/L solution is configured to, dosage is 1~5 mass parts；Chain-transferring agent is sodium formate, is configured to
0.1mol/L solution, dosage are 1.5~10 mass parts；After raw material mixing, the mass concentration of monomer is 20%.
Synthesis technology：Acid monomer (AMPS, AA) is dissolved in appropriate amount of deionized water, under cooled conditions with appropriate
PH value is adjusted to 8~10 by 30% sodium hydrate aqueous solution, is then added in remaining monomer, chain-transferring agent and is sufficiently stirred, solution
It adds in the four-hole boiling flask with blender, condenser and thermometer, initiator solution is added dropwise after logical nitrogen deoxygenation 30min,
The lower constant temperature of nitrogen protection is reacted 2 hours to 80~95 DEG C, obtains sticky flowable liquids, vacuum drying crushes, and obtains solid powder
Last shape product is high-temperature resisting and salt-resisting fluid loss additive.
The fluid loss additive that the application obtains carries out infrared spectrum analysis：
The fluid loss additive outturn sample ethyl alcohol of the application synthesis is taken off repeatedly and is washed after purification with potassium bromide mixed pressuring plate, is made
It is tested with Fourier transformation infrared spectrometer, the result is shown in Figure 1.In figure, 3408cm-1 and 1662cm-1 are the spies of amide groups
Levy peak；1041cm-1 and 1180cm-1 is the characteristic peak of SO32- in AMPS；1317cm-1 is the stretching vibration absworption peak of carboxyl；
Absorption peak near 1450cm-1 is pentacyclic stretching vibration peak in NVP；958cm-1,1400cm-1 and 1554cm-1 are
The characteristic absorption peak of DMDAAC, for analysis result with expected consistent, the application fluid loss additive has good filtrate reducing effect.
The fluid loss additive that the application obtains carries out thermogravimetic analysis (TGA)：
Sample is done into thermal weight loss experiment with identical heating rate (8 DEG C/min), its thermal stability is investigated, as a result sees Fig. 2.
Fluid loss additive is can be seen that from Fig. 2 data, a small amount of weightlessness less than 20% has occurred before 150 DEG C, this is because in product
Containing 10~15% moisture, therefore remaining moisture and residual monomer volatilization or decomposition can cause on a small quantity.After 280 DEG C,
Fast decoupled has occurred in product.As can be seen that product has good thermal stability before 280 DEG C.
The fluid loss additive that the application obtains carries out filtrate loss controllability evaluation：
1st, fresh water slurry evaluation：
Test the application fluid loss additive FLOTHIN in 5% calcium soil aquation slurry, the front and rear rheological characteristic of 200 DEG C of heat rollings with
And filter loss, hot rolling condition are 200 DEG C × 16h.It the results are shown in Table 1：
As can be seen from Table 1, as the dosage of inorganic agent increases, filter loss is greatly lowered, and dosage reaches
When 0.5%, filter loss reduces nearly 50%, when dosage reaches 1.5% before and after heat rolling, and filter loss is less than 10mL before and after heat rolling, simultaneously
The rheological characteristic of experiment slurry does not vary widely, and viscosity effect is small, convenient for on-site maintenance.
2nd, saturated salt water slurry is evaluated：
In 5% calcium soil aquation slurry, the application fluid loss additive FLOTHIN is added in, adds sodium chloride to saturation, test examination
The front and rear rheological property of slurry heat rolling and filter loss are tested, hot rolling condition is 200 DEG C × 16h.It the results are shown in Table 2：
As can be seen from Table 2, with the increase of fluid loss additive FLOTHIN dosages, experiment is starched from paste coagulation
Solution flocculation, restores mobility, when dosage reaches 2.0%, while tests slurry and gluing due to the excessive appearance of inorganic agent dosage does not occur
The phenomenon that high is spent, filter loss shows that product has very low viscosity effect, well by losing the 9.0mL after being reduced to heat rolling entirely
Heat and salinity tolerance ability.
The fluid loss additive and the comparative evaluation of similar product that the application obtains：
Under the same conditions, the drop that contrast test similar product Driscal D, Driscal TEMP is synthesized with the application
The rolling of fluid loss agents FLOTHIN heat front and rear rheological characteristic and filter loss.Base is starched：2% calcium soil+0.25% soda ash+10% evaluation soil+
+ 2.0% fluid loss additive of 15% sodium chloride.Hot rolling condition is 200 DEG C × 16h.As a result such as table 3：
As can be seen from Table 3, identical base slurry under the conditions of, dosage be 2% when, with similar product Driscal D,
DriscalTEMP is compared, and the application, which synthesizes fluid loss additive FLOTHIN, not to be occurred significantly viscosifying, and rheological characteristic is opposite before and after heat rolling
Stablize, filter loss is smaller than similar product, more than similar products at home and abroad level.
Performance evaluation of the fluid loss additive that the application obtains in potassium chloride high density system：
Have rated leak-off wave making machines of the application polymer filtrate reducer FLOTHIN in potassium chloride high density system and
Rheological characteristic, base slurry：3% soil paste+3%SPNH sulfonated lignite resins+4%SMP-, II sulfonated phenol formaldehyde resin+7%KCl+4%KFT change
+ 4% emulsified asphalt of property lignite fluid loss additive+0.3%NaOH+3% fluid lubricants+barite (is exacerbated to 2.0g/cm3).Heat
Rolling condition：200℃×16h；High temperature and pressure test temperature：150℃.Data are shown in Table 4：
As can be seen from Table 4, after 2% polymer filtrate reducer FLOTHIN being added in potassium chloride high density system,
Viscosity does not increase considerably, and rheological characteristic is stablized relatively before and after heat rolling, convenient for on-site maintenance.After adding in 2% polymer,
Filter loss is also greatly lowered, and high temperature and high pressure filter loss is reduced to 12.8mL from 22.4mL.It can be seen that the polymer filtrate reducing
Agent and system compatibility are good, and the addition of inorganic agent improves the thermal stability of system and leak-off wall building property.
The fluid loss additive of the application synthesis has very low viscosity effect, under the premise of filtrate reducing effect is ensured, improves
The high temperature resistance and salt-resistance of fluid loss additive, fluid loss additive still has good thermal stability before 280 DEG C, in saturated sodium-chloride
Also there is good filtrate reducing effect under saltwater environment.
The above is only the specific embodiment of the application, is made skilled artisans appreciate that or realizing this Shen
Please.A variety of modifications of these embodiments will be apparent to one skilled in the art, it is as defined herein
General Principle can in other embodiments be realized in the case where not departing from spirit herein or range.Therefore, the application
The embodiments shown herein is not intended to be limited to, and is to fit to and the principles and novel features disclosed herein phase one
The most wide range caused.
It should be understood that the content that the application is not limited to be described above and be shown in the drawings, and can
To carry out various modifications and change without departing from the scope.Scope of the present application is only limited by appended claim.
Claims (10)
1. a kind of salt-resisting high-temperature-resisting fluid loss additive, which is characterized in that the fluid loss additive is in initiator and chain tra nsfer by monomer
It is made after copolymerization under conditions of agent；The monomer includes the N,N-DMAA that mass fraction is 5~25 parts, matter
It is 10~50 parts to measure N- vinylpyrrolidones, the acrylic acid that mass fraction is 20~60 parts, mass fraction that number is 2~5 parts
2- acrylamide-2-methyl propane sulfonics and mass fraction be 2~10 parts of dimethyl diallyl ammonium chloride.
2. a kind of salt-resisting high-temperature-resisting fluid loss additive according to claim 1, which is characterized in that the initiator is persulfuric acid
Potassium and sodium hydrogensulfite.
3. a kind of salt-resisting high-temperature-resisting fluid loss additive according to claim 1, which is characterized in that the chain-transferring agent is formic acid
Sodium.
4. a kind of preparation method of salt-resisting high-temperature-resisting fluid loss additive, which is characterized in that include the following steps：
1) 2- acrylamide-2-methyl propane sulfonics and acrylic acid is taken to be dissolved in deionized water and obtain solution A, and in the condition of cooling
It is lower that the pH value of solution A is adjusted to 8~10；
2) N,N-DMAA, N- vinylpyrrolidones, dimethyl diallyl ammonium chloride and chain-transferring agent solution are taken
It adds in solution A and is sufficiently stirred, obtain solution B；
3) solution B is put into after leading to nitrogen deoxygenation in reactor and initiator solution is added dropwise, under nitrogen protection constant temperature to 80~95
DEG C reaction, obtain sticky flowable liquids C；
4) after sticky flowable liquids C being dried in vacuo and crushed successively, it is fluid loss additive to obtain pulverulent solids.
A kind of 5. preparation method of salt-resisting high-temperature-resisting fluid loss additive according to claim 4, which is characterized in that the solution
2- acrylamide-2-methyl propane sulfonics, acrylic acid, N,N-DMAA, N- vinylpyrrolidones and dimethyl two in B
The total mass concentration of allyl ammonium chloride is 15~25%.
A kind of 6. preparation method of salt-resisting high-temperature-resisting fluid loss additive according to claim 5, which is characterized in that the solution
2- acrylamide-2-methyl propane sulfonics, acrylic acid, N,N-DMAA, N- vinylpyrrolidones and dimethyl two in B
The total mass concentration of allyl ammonium chloride is preferably 20%.
A kind of 7. preparation method of salt-resisting high-temperature-resisting fluid loss additive according to claim 4, which is characterized in that the drop filter
It loses agent and includes the N,N-DMAA that mass fraction is 5~25 parts, the N- ethylene pyrroles that mass fraction is 2~5 parts
Acrylic acid that alkanone, mass fraction are 20~60 parts, the 2- acrylamide-2-methyl propane sulfonics that mass fraction is 10~50 parts and
Mass fraction is 2~10 parts of dimethyl diallyl ammonium chloride.
8. the preparation method of a kind of salt-resisting high-temperature-resisting fluid loss additive according to claim 4, which is characterized in that the chain turns
The sodium formate solution that agent solution is a concentration of 0.1mol/L is moved, the addition mass fraction of sodium formate solution is 1.5~10 parts.
A kind of 9. preparation method of salt-resisting high-temperature-resisting fluid loss additive according to claim 4, which is characterized in that the initiation
Agent solution is a concentration of 0.1mol/L mixed solutions prepared by potassium peroxydisulfate and sodium hydrogensulfite, the addition matter of initiator solution
It is 1~5 part to measure number.
A kind of 10. preparation method of salt-resisting high-temperature-resisting fluid loss additive according to claim 4, which is characterized in that the step
It is rapid 1) in solution A add in mass concentration be 30% sodium hydrate aqueous solution the pH value of solution A is adjusted to 8~10.
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| CN113150754A (en) * | 2021-04-01 | 2021-07-23 | 西南石油大学 | Temperature-resistant and salt-resistant water-based drilling fluid filtrate reducer and preparation method thereof |
| CN113214817A (en) * | 2021-05-14 | 2021-08-06 | 西南石油大学 | Ultrahigh-temperature fracturing fluid thickening agent and preparation method thereof |
| CN115960314A (en) * | 2023-03-15 | 2023-04-14 | 克拉玛依友联实业有限责任公司 | Preparation method of environment-friendly filtrate reducer and application of environment-friendly filtrate reducer in drilling fluid |
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