CN108342188A - A kind of heat resisting fluid loss reducing agent and preparation method thereof and a kind of water-base drilling fluid - Google Patents
A kind of heat resisting fluid loss reducing agent and preparation method thereof and a kind of water-base drilling fluid Download PDFInfo
- Publication number
- CN108342188A CN108342188A CN201810367916.9A CN201810367916A CN108342188A CN 108342188 A CN108342188 A CN 108342188A CN 201810367916 A CN201810367916 A CN 201810367916A CN 108342188 A CN108342188 A CN 108342188A
- Authority
- CN
- China
- Prior art keywords
- fluid loss
- water
- reducing agent
- heat resisting
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- 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
- C08F220/56—Acrylamide; Methacrylamide
-
- 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 present invention provides a kind of heat resisting fluid loss reducing agents and preparation method thereof.The present invention strictly controls preparation condition, obtain polymer made of being copolymerized by various of monomer, due to the statistical property of the polymer forming process, the inhomogenous characteristic of the fluid loss additive molecular weight i.e. Polydispersity is formd, the rheological property of drilling fluid under the high temperature conditions and heat and salinity tolerance ability are greatly improved；And also contains phenyl ring in heat resisting fluid loss reducing agent molecular structure, there is stronger rigidity than linear molecule chain, enhance the rigid nature of strand, improve the thermal stability of the fluid loss additive, improve heat-resisting property of the fluid loss additive in drilling fluid.The present invention also provides the water-base drilling fluids for including the heat resisting fluid loss reducing agent；Fluid loss additive provided by the invention remains to keep good filtration reduction under 200 DEG C of hot conditions in fresh water-based slurry, and good filtration reduction can be also kept under 160 DEG C of hot conditions in compound salt-water basic slurry.
Description
Technical field
The present invention relates to petroleum drilling fluid technical field more particularly to a kind of heat resisting fluid loss reducing agent and preparation method thereof and
A kind of water-base drilling fluid.
Background technology
Drilling fluid quality is the key that determine entire drilling engineering success, and the height of drilling liquid technology is also to weigh to bore
The important indicator of the flat height of well water.With the continuous development of petroleum exploration and development technology, the exploration and development of oil gas is increasingly turned to surpass
Deep stratum.During deep-well and ultradeep well exploration and development, the stratum for boring chance becomes increasingly complex, and the requirement to property of drilling fluid is more
It is harsh.
As the increase of well depth, downhole temperature can be higher and higher in drilling process, pressure also can be increasing, temperature and
The change of pressure can all have an impact the stability of water-base drilling fluid rheological characteristic, and the drilling fluid that rheological characteristic is stablized is for drilling well
Being smoothed out for journey is most important.In order to ensure being smoothed out for deep drilling engineering, deep-well water-base drilling fluid must have height
Temperature stability.
Fluid loss additive is the important component of drilling fluid, and the good and bad of fluid loss additive high-temperature stability directly determines drilling fluid
High-temperature stability.Currently, the fluid loss additive type used in oilfield drilling is more, but its temperature resistant capability is poor, deep-well,
Particularly evident in ultradeep well operation process, existing fluid loss additive is easily easy to decompose at relatively high temperatures, and filtrate reducing effect subtracts
It is weak；If under the conditions of saliferous, the case where fluid loss additive pyrolytic, is even more serious.
Invention content
In view of this, the present invention provides a kind of heat resisting fluid loss reducing agent and preparation method thereof and a kind of water-base drilling fluid,
Fluid loss additive provided by the invention has excellent high-temperature stability, to improve the high temperature stability performance of drilling fluid.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The present invention provides a kind of preparation methods of heat resisting fluid loss reducing agent, include the following steps：
Comonomer water-soluble liquid is provided；The comonomer includes acrylic acid, acrylamide, 2- acrylamidos -2-
Methyl propane sulfonic acid, sodium styrene sulfonate and acrylonitrile；
It is molten to obtain alkaline monomer to 8~9 for the pH value for adjusting the comonomer water-soluble liquid using alkaline pH adjuster
Solve liquid；
The alkaline monomer lysate is mixed with oxidized form initiator, reduced form initiator, molecular weight regulator, is carried out
Polymerisation obtains jel product；
The dry jel product, obtains heat resisting fluid loss reducing agent.
Preferably, acrylic acid, acrylamide, 2- acrylamido -2- methyl-prop sulphurs in the comonomer water-soluble liquid
Acid, sodium styrene sulfonate, acrylonitrile and water mass ratio be (310~330)：(310~330)：(140~160)：(230~
260)：(130~160)：(130~160).
Preferably, the quality of the molecular weight regulator be alkaline monomer lysate in comonomer gross mass 0.05~
0.2%；The molecular weight regulator includes one or more in thioglycolic, thioacetic acid, mercaptopropionic acid and sodium formate.
Preferably, the quality of the oxidized form initiator be alkaline monomer lysate in comonomer gross mass 1~
2%；The oxidized form initiator includes one or more in ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate and hydrogen peroxide.
Preferably, the quality of the reduced form initiator be alkaline monomer lysate in comonomer gross mass 1~
2%；The reduced form initiator includes one kind or more in sodium hydrogensulfite, sodium sulfite, potassium sulfite and sodium thiosulfate
Kind.
Preferably, the temperature of the polymerisation is 60~65 DEG C, and the time of polymerisation is 5~7h.
Preferably, after the drying heat resisting fluid loss reducing agent moisture content≤15wt%.
The present invention also provides the heat resisting fluid loss reducing agents that preparation method described in above-mentioned technical proposal is prepared；It is described anti-
The weight average molecular weight of high temperature fluid loss additive is 5~3,000,000；
The heat resisting fluid loss reducing agent has structural formula shown in Formulas I：
In Formulas I, x：y：z：m：N=(31~33)：(23~26)：(14~16)：(31~33)：(13~16).
The present invention provides a kind of water-base drilling fluid, including water based slurry and fluid loss additive, the fluid loss additive is above-mentioned
Heat resisting fluid loss reducing agent described in technical solution；The quality of the heat resisting fluid loss reducing agent is the 1~5% of drilling fluid gross mass.
Preferably, in terms of mass parts, the water based slurry includes 3~4 parts of sodium bentonites, 0.25 part of natrium carbonicum calcinatum and
100 parts of water.
The present invention provides a kind of preparation methods of heat resisting fluid loss reducing agent, provide comonomer water-soluble liquid first；Institute
It includes acrylic acid, acrylamide, 2- acrylamide-2-methylpro panesulfonic acids, sodium styrene sulfonate and acrylonitrile to state comonomer；
It uses the pH value that alkaline pH adjuster adjusts the comonomer water-soluble liquid to 8~9 again, obtains alkaline monomer lysate
Afterwards, the alkaline monomer lysate is mixed with molecular weight regulator, oxidized form initiator, reduced form initiator, is polymerize
Reaction, obtains jel product；The dry jel product, obtains heat resisting fluid loss reducing agent.The present invention is copolymerized defined by using
The effect of monomer combination alkaline pH adjuster, in the effect of oxidized form initiator, reduced form initiator and molecular weight regulator
Under, polymer made of being copolymerized by various of monomer is obtained, due to the statistical property of the polymer forming process, forms drop filter
Lose the inhomogenous characteristic, that is, Polydispersity of agent molecule amount, the very big rheological characteristic for improving drilling fluid under the high temperature conditions
It can be with heat and salinity tolerance ability；And also contains phenyl ring in heat resisting fluid loss reducing agent molecular structure, have than linear molecule chain stronger
Rigidity, enhance the rigid nature of strand, improve the thermal stability of the fluid loss additive, improve the fluid loss additive
Heat-resisting property in drilling fluid.Embodiment the result shows that, fluid loss additive provided by the invention 200 DEG C of height in fresh water-based slurry
It remains to keep good filtration reduction under the conditions of temperature, can also keep good under 160 DEG C of hot conditions in compound salt-water basic slurry
Filtration reduction.
Description of the drawings
Fig. 1 is the infrared spectrogram for the heat resisting fluid loss reducing agent that embodiment 1 obtains.
Specific implementation mode
The present invention provides a kind of preparation methods of heat resisting fluid loss reducing agent, include the following steps：
Comonomer water-soluble liquid is provided；The comonomer includes acrylic acid, acrylamide, 2- acrylamidos -2-
Methyl propane sulfonic acid, sodium styrene sulfonate and acrylonitrile；
It is molten to obtain alkaline monomer to 8~9 for the pH value for adjusting the comonomer water-soluble liquid using alkaline pH adjuster
Solve liquid；
The alkaline monomer lysate is mixed with oxidized form initiator, reduced form initiator, molecular weight regulator, is carried out
Polymerisation obtains jel product；
The dry jel product, obtains heat resisting fluid loss reducing agent.
In the present invention, unless otherwise specified, the raw material used in the preparation method is those skilled in the art institute
Well known commercial goods.
In this application, unless otherwise specified, when arriving the dosage of raw material involved in the preparation method, the base of unit mass
Standard is identical.
The present invention provides comonomer water-soluble liquid.In the present invention, the comonomer includes acrylic acid, acryloyl
Amine, 2- acrylamide-2-methylpro panesulfonic acids, sodium styrene sulfonate and acrylonitrile.In the present invention, the comonomer is water-soluble
Solve the quality of acrylic acid, acrylamide, 2- acrylamide-2-methylpro panesulfonic acids, sodium styrene sulfonate, acrylonitrile and water in liquid
Than preferably (310~330)：(310~330)：(140~160)：(230~260)：(130~160)：(130~160), into
One step is preferably (320~325)：(320~330)：(150~160)：(250~260)：(140~160)：(140~160),
More preferably 320:320:160:250:150:150.In the present invention, the dosage of the 2- acrylamide-2-methyl propane sulfonics
Less, the cost of raw material propylene acid, acrylamide, sodium styrene sulfonate and acrylonitrile is low and derives from a wealth of sources.
In the present invention, the preparation method of the comonomer water-soluble liquid preferably include by acrylic acid, acrylamide and
Water mixes, and obtains primary solubilization liquid；2- acrylamide-2-methylpro panesulfonic acids, styrene are added in the primary solubilization liquid
Sodium sulfonate and acrylonitrile, the mixed dissolution under water bath condition obtain comonomer water-soluble liquid.In the present invention, the propylene
The mixing of acid, acrylamide and water preferably carries out under agitation；The present invention does not have the specific implementation mode of the stirring
Particular/special requirement uses agitating mode well-known to those skilled in the art can realize dissolving；In the embodiment of the present invention
In, the rate of the stirring is preferably 300rpm, and the time of stirring is preferably 30min.In the present invention, the mixed dissolution mistake
Water bath condition preferably is selected from room temperature to keeping the temperature 30min after 60 DEG C in journey.The present invention by the way of step-wise dissolution comonomer,
Each monomer is promoted fully to dissolve.
After obtaining comonomer water-soluble liquid, the present invention adjusts the comonomer water dissolution using alkaline pH adjuster
The pH value of liquid obtains alkaline monomer lysate to 8~9.In the present invention, the alkaline pH adjuster preferably includes hydroxide
Potassium or sodium hydroxide；The alkaline pH adjuster provides preferably in the form of alkaline pH adjuster solution；The alkaline pH
The mass fraction that value adjusts agent solution is preferably 15%.In the present invention, the alkaline pH adjuster solution is preferably to be added dropwise
Mode add；The present invention does not have particular/special requirement to the dosage of the alkaline pH adjuster, can obtain being total to for target ph
Polycondensation monomer water-soluble liquid.In the present invention, the pH value of comonomer water-soluble liquid is 8~9 after pH value is adjusted, preferably
8.2~8.8, most preferably 8.5.The present invention can adjust the pH value regulated value target zone of comonomer water-soluble liquid anti-
Speed is answered, the initiation effect of initiator is promoted, plays the role of promoting to accelerate reaction speed, under pH value adjusting, causes effect
Most preferably.
After obtaining alkaline monomer lysate, by the alkaline monomer lysate and oxidized form initiator, reduced form initiator,
Molecular weight regulator mixes, and carries out polymerisation, obtains jel product.In the present invention, the quality of the oxidized form initiator
The 1~2%, further preferably 1.2~1.8% of comonomer gross mass preferably in alkaline monomer lysate, more preferably
1.5%.In the present invention, the oxidized form initiator preferably includes ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate and hydrogen peroxide
In it is one or more.When the oxidized form initiator is two kinds in above-mentioned substance, three or at four kinds, the present invention is to each object
The additive amount of matter does not have special restriction, using arbitrary proportioning.
In the present invention, the quality of the reduced form initiator is preferably comonomer gross mass in alkaline monomer lysate
1~2%, further preferably 1.2~1.8%, more preferably 1.5%.In the present invention, the reduced form initiator is preferred
Including one or more in sodium hydrogensulfite, sodium sulfite, potassium sulfite and sodium thiosulfate.When the reduced form initiator
For two kinds in above-mentioned substance, three or four kinds when, the present invention does not have the additive amount of each substance special restriction, using arbitrary
Proportioning.
In the present invention, the quality of the molecular weight regulator is preferably comonomer gross mass in alkaline monomer lysate
0.05~0.2%, further preferably 0.1~0.15%.In the present invention, the molecular weight regulator preferably includes thio
It is one or more in ethyl alcohol, thioacetic acid, mercaptopropionic acid and sodium formate.When the molecular weight regulator is in above-mentioned substance
When two kinds, three or four kinds, the present invention does not have the additive amount of each substance special restriction, using arbitrary proportioning.At this
In invention, molecular weight regulator plays the role of adjusting the size of polymer molecular weight, adjusts the molecular weight after polymerization, is coagulated
Glue product.
In the present invention, the alkaline monomer lysate and oxidized form initiator, reduced form initiator, molecular weight regulator
Mixed process preferably carry out in a nitrogen atmosphere, for raw material mixing and polymerization process oxygen-free environment is provided.The present invention couple
The mixing specific implementation mode of the alkaline monomer lysate and oxidized form initiator, reduced form initiator and molecular weight regulator
There is no particular/special requirement, using feed liquid hybrid mode well-known to those skilled in the art.
After the mixing for completing alkaline monomer lysate, molecular weight regulator, oxidized form initiator and reduced form initiator, this
The mixed liquor is carried out polymerisation by invention, obtains jel product.In the present invention, the temperature of the polymerisation is preferred
It is 60~65 DEG C, further preferably 61~62 DEG C；The time of the polymerisation is preferably 5~7h, further preferably 6h.
Redox initiator polymerisation has occurred in polymerization process in the present invention, and when effect of molecular weight regulator adjusts poly-
The effect of the size of adduct molecule amount, initiator is initiated polymerization.In the present invention, the oxidized form initiator, reduction
Single electron transfer between type initiator has caused redox reaction and has generated free radicals, to occur chain initiation, chain growth,
The series reactions such as chain termination.The decomposition activation energy that peroxide can both be reduced in this way causes single under lower temperature conditions
Body polymerize, and can also increase the decomposition rate of peroxide, to increase rate of polymerization.
After obtaining jel product, the jel product is dried in the present invention, obtains heat resisting fluid loss reducing agent.In this hair
In bright, the moisture content of the dried product exhibited is preferably smaller than equal to 15%；In the present invention, the temperature of the drying is preferably 60
~70 DEG C, further preferably 65 DEG C；The present invention does not have particular/special requirement to the time of the drying, can obtain meeting moisture content
It is required that desciccate.
After the drying, obtained desciccate is preferably crushed processing by the present invention, obtains powdered high temperature resistance drop
Fluid loss agents.In the present invention, the grain size of the powdered high temperature resistance fluid loss agents is preferably 60~80 mesh.The present invention is to the crushing
The specific implementation mode of processing does not have particular/special requirement, uses well-known to those skilled in the art can obtain the powder of target grain size
Last shape heat resisting fluid loss reducing agent.
The present invention also provides preparation methods described in above-mentioned technical proposal, and heat resisting fluid loss reducing agent is prepared.
In the present invention, the heat resisting fluid loss reducing agent has structural formula shown in Formulas I：
In Formulas I, x：y：z：m：N=(31~33)：(23~26)：(14~16)：(31~33)：(13~16), further
Preferably 32:(24~25):15:32:(14~15).
In the present invention, the weight average molecular weight of the heat resisting fluid loss reducing agent is 5~3,000,000, preferably 10~2,000,000,
Most preferably 15~200,000.
In the present invention, the heat resisting fluid loss reducing agent is by acrylic acid, acrylamide, 2- acrylamido -2- methyl
Propane sulfonic acid, sodium styrene sulfonate and acrylonitrile are used as copolymer list after oxidized form initiator, the initiation of reduced form initiator is added
Member, the copolymer of formation；The heat resisting fluid loss reducing agent is as polymer made of being copolymerized by various of monomer, due to the polymer
The statistical property of forming process forms the inhomogenous characteristic of the fluid loss additive molecular weight i.e. Polydispersity, described anti-
The dispersibility of high temperature fluid loss additive molecular weight reaches the ability for the rheological characteristic for adjusting drilling fluid system, very big to improve in height
The rheological property of drilling fluid and heat and salinity tolerance ability under the conditions of temperature.
In the present invention, amide group and sulfonic acid group, molecular structure are contained in the structure of the heat resisting fluid loss reducing agent
In sulfonic acid group be strongly hydrophilic group, while there is stronger hydration, improve fluid loss additive in saline solution
Dissolubility, improve salt resistant character of the fluid loss additive in drilling fluid, make it that can effectively control leak-off in brine mud
Amount；And also contains phenyl ring in the heat resisting fluid loss reducing agent molecular structure, there is stronger rigidity, enhancing than linear molecule chain
The rigid nature of strand, improves the thermal stability of the fluid loss additive, improves the fluid loss additive in drilling fluid
Heat-resisting property.
In the present invention, the heat resisting fluid loss reducing agent still has filtration reduction under the conditions of 200 DEG C.In the present invention,
Temperature resistance ability of the heat resisting fluid loss reducing agent in fresh water-based slurry reaches 200 DEG C, the heat and salinity tolerance energy in compound salt-water basic slurry
Power reaches 160 DEG C.
The present invention provides a kind of drilling fluids, including heat resisting fluid loss reducing agent described in water based slurry and above-mentioned technical proposal.
In the present invention, the quality of the fluid loss additive is the 1~5%, preferably 0.3~3% of drilling fluid gross mass, further preferably
It is 0.5~2.5%, more preferably 0.6~2%, most preferably 0.7~1.0%.Heat resisting fluid loss reducing agent provided by the present invention
Only need less additive amount, you can the requirement for ensureing the filtration reduction of drilling fluid helps to reduce cost.The present invention is to the water
The concrete composition of based slurries does not have particular/special requirement, and drilling fluid raw material components well-known to those skilled in the art can be used.At this
In invention, in terms of mass parts, the water based slurry preferably includes 3~4 parts of sodium bentonites, 0.25 part of natrium carbonicum calcinatum and 100 parts
Water.
With reference to embodiment to heat resisting fluid loss reducing agent provided by the invention and preparation method thereof and a kind of water-based drilling
Liquid is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
In terms of mass parts, into the four-hole boiling flask equipped with blender, reflux condenser, thermometer and heating device, it is added
130 parts of distilled water, 315 parts of acrylic acid and 315 parts of acrylamides, start blender, and stirring to monomer is all dissolved.It adds
145 parts of 2- acrylamide-2-methylpro panesulfonic acids, 235 parts of sodium styrene sulfonate, heating water bath are warming up to 60 DEG C of heat preservations to monomer
Dissolving, obtains comonomer water-soluble liquid.
PH value 8~9 is adjusted with NaOH solution.Logical nitrogen flooding oxygen simultaneously, 1.5 parts of initiator ammonium persulfates are added at 60 DEG C
5min is reacted, 1.5 parts of sodium hydrogensulfite reaction 40min is added, 1.3 parts of molecular weight regulator thioglycolic acids is then added,
4h is reacted, gel-like product is obtained.
65 DEG C of dryings of steady temperature in drying box by obtained gel-like product, it is to be dried to moisture content be less than 15%
Afterwards, desciccate is crushed, 60 mesh sieve is crossed, obtains the fluid loss additive of white powder.
For the group on the fluid loss additive strand of verification synthesis, the sample A synthesized in embodiment 1 is mixed into pressure with KBr
Piece tests it using Fourier Transform Infrared Spectrometer, and gained infrared spectrogram is as shown in Figure 1.
It is learnt from infrared spectrum analysis, 3425cm-1For-NH2Absorption peak, 3208cm-1For the absorption peak of-NH,
2936cm-1For-CH3Asymmetric stretching vibration peak, 2900cm-1For-CH2Stretching vibration peak, 1672cm-1For in acyl group
- stretching vibration peak of C=0,1040cm-1、1220cm-1For the symmetrical and asymmetric vibration absorption peak of-S03-, 699cm-1
For the absorption peak of monomer substituted benzene ring, show in polymer containing groups such as amide groups, sulfonic group and phenyl ring.
Embodiment 2
In terms of mass parts, into the four-hole boiling flask equipped with blender, reflux condenser, thermometer and heating device, it is added
150 parts of distilled water, 325 parts of acrylic acid and 325 parts of acrylamides, start blender, and stirring to monomer is all dissolved.It adds
150 parts of 2- acrylamide-2-methylpro panesulfonic acids, 250 parts of sodium styrene sulfonate, it is molten that heating water bath to 60 DEG C is warming up to monomer
Solution, obtains comonomer water-soluble liquid.
PH value 8~9 is adjusted with NaOH solution.Logical nitrogen flooding oxygen simultaneously, 1.55 parts of initiator persulfuric acid are added at 60 DEG C
Ammonium reacts 3min, adds 1.55 parts of sodium hydrogensulfite reaction 30min, 1.3 parts of molecular weight regulator thioglycolics are then added
Acid reacts 4h, obtains gel-like product.
65 DEG C of dryings of steady temperature in drying box by obtained gel-like product, it is to be dried to moisture content be less than 15%
Afterwards, desciccate is crushed, 60 mesh sieve is crossed, obtains the fluid loss additive of white powder.
Embodiment 3
In terms of mass parts, into the four-hole boiling flask equipped with blender, reflux condenser, thermometer and heating device, it is added
160 parts of distilled water, 330 parts of acrylic acid and 330 parts of acrylamides, start blender, and stirring to monomer is all dissolved.It adds
160 parts of 2- acrylamide-2-methylpro panesulfonic acids, 255 parts of sodium styrene sulfonate, heating water bath be warming up to 60 DEG C it is molten to monomer
Solution, obtains comonomer water-soluble liquid.
PH value 8~9 is adjusted with NaOH solution.Logical nitrogen flooding oxygen simultaneously, 1.6 parts of initiator ammonium persulfates are added at 60 DEG C
2min is reacted, 1.6 parts of sodium hydrogensulfite reaction 35min is added, 1.5 parts of molecular weight regulator thioglycolic acids is then added,
5h is reacted, gel-like product is obtained.
65 DEG C of dryings of steady temperature in drying box by obtained gel-like product, it is to be dried to moisture content be less than 15%
Afterwards, desciccate is crushed, 60 mesh sieve is crossed, obtains the fluid loss additive of white powder.
Embodiment 4
Fresh water-based slurry is prepared to prepare：Addition 400mL tap water in cup is stirred in height, 16g sodium swellings are added under constant stirring
Soil, 1.0g natrium carbonicum calcinatums, with 12000r/min high-speed stirred 20min, curing in airtight condition for 24 hours, obtains the light of prehydration at room temperature
Water base slurry.
Experiment slurry is prepared：The fresh water-based slurry of three parts of prehydrations is taken, under constant agitation to the fresh water-based slurry of prehydration
In be separately added into the fluid loss additive that the Examples 1 to 3 of 0.3wt.% obtains, high-speed stirred is uniform, is denoted as A fluid loss additives-fresh water
Base slurry, B fluid loss additives-fresh water-based slurry and C fluid loss additives-fresh water-based slurry.Respectively to A fluid loss additives-fresh water-based slurry, B filtrate reducings
Agent-fresh water-based slurry and C fluid loss additives-fresh water-based slurry and fresh water-based slurry carry out rheological characteristic and filter loss test, as a result such as 1 institute of table
Show.
Rheological characteristic and filter loss test result of the table 1 in different fluid loss additives in fresh water-based slurry
| Experiment slurry | AV(mPa·s) | PV(mPa·s) | YP(Pa) | FLAPI(mL) |
| Fresh water-based slurry | 7 | 4 | 3 | 23 |
| A fluid loss additives-fresh water-based slurry | 11 | 10 | 1 | 11 |
| B fluid loss additives-fresh water-based slurry | 20 | 15 | 5 | 7 |
| C fluid loss additives-fresh water-based slurry | 18 | 14 | 4 | 9 |
In table 1, AV refers to apparent viscosity, and PV refers to plastic viscosity, and YP refers to yield value, FLAPIRefer to normal temperature and pressure wellbore liquid leaching loss
Amount.(similarly hereinafter) as shown in Table 1, fluid loss additive of the invention just has good filtrate loss controllability in the case of dosage very little.
Embodiment 5
Prepare 15% brine mud：It is stirred in cup in height and the fresh water sodium bentonite slurry for corresponding to component is added in embodiment 4
60gNaCl is added in 400mL under constant stirring, stirs 20min, for 24 hours, the salt for obtaining prehydration is water base for curing in airtight condition at room temperature
Slurry.
Experiment slurry is prepared：Take 3 parts of prehydration brine muds, be stirred continuously it is lower respectively into the brine mud of prehydration respectively
The heat resisting fluid loss reducing agent that 1.5% Examples 1 to 3 obtains is added, high-speed stirred is uniform, is denoted as A fluid loss additives-brine respectively
Base slurry, B fluid loss additives-brine mud and C fluid loss additives-brine mud.Respectively to A fluid loss additives-brine mud, B filtrate reducings
Agent-brine mud and C fluid loss additives-brine mud and 15% brine mud carry out rheological characteristic and filter loss test, as a result such as
Shown in table 2.
Rheological characteristic and filter loss test result of the table 2 in different fluid loss additives in 15% brine mud
| Experiment slurry | AV(mPa·s) | PV(mPa·s) | YP(Pa) | FLAPI(mL) |
| 15% salt slurries | 5 | 3 | 2 | 60 |
| A fluid loss additives-brine mud | 49 | 38 | 11 | 7.6 |
| B fluid loss additives-brine mud | 49 | 36 | 13 | 9 |
| C fluid loss additives-brine mud | 46 | 34 | 12 | 7 |
As shown in Table 2, fluid loss additive of the invention has more good filtrate loss controllability in 15% brine mud, and
Dosage is small.
Embodiment 6
Prepare compound brine：45g sodium chloride, 3g anhydrous magnesium chlorides, 5.0g anhydrous calcium chlorides are added in every liter of distilled water,
It stirs evenly, it is spare.
Prepare compound alkali slurry：It is stirred in height and the compound brine of 400mL is added in cup, under high-speed stirred, the anhydrous carbon of 3.6g is added
Sour sodium, 60g sodium bentonites, high-speed stirred 20min, at room temperature curing in airtight condition for 24 hours, obtain prehydration compound alkali slurry.
Experiment slurry is prepared：Three parts of compound alkali slurries are taken, under constant stirring respectively into the good compound salt slurries of prehydration
The heat resisting fluid loss reducing agent that 1.5% Examples 1 to 3 obtains is added, high-speed stirred is uniform, and it is compound to be denoted as A fluid loss additives-respectively
Alkali slurry, B fluid loss additives-compound alkali slurry and C fluid loss additives-compound alkali slurry.A fluid loss additives-compound alkali is starched respectively,
B fluid loss additives-compound alkali slurry and C fluid loss additives-compound alkali slurry and compound alkali slurry progress rheological characteristic and leak-off measure
Examination, the results are shown in Table 3.
Rheological characteristic and filter loss test result of the table 3 in different fluid loss additives in compound alkali slurry
| Experiment slurry | AV(mPa.s) | PV(mPa.s) | YP(Pa) | FLAPI(mL) |
| Compound alkali slurry | 6 | 4 | 2 | 65 |
| A fluid loss additives-compound alkali slurry | 26 | 23 | 3 | 12 |
| A fluid loss additives-compound alkali slurry | 18 | 16 | 2 | 14 |
| A fluid loss additives-compound alkali slurry | 15 | 14 | 1 | 7 |
As shown in Table 3, fluid loss additive product of the invention has more good filtrate loss controllability in compound salt-water basic slurry.
Embodiment 7
Fresh water-based slurry is prepared in the way of embodiment 4, obtains prehydration fresh water-based slurry.
Experiment slurry is prepared：Three parts of prehydration fresh water-based slurrys are taken, under constant stirring respectively to the good fresh water-based slurry of prehydration
The heat resisting fluid loss reducing agent that the embodiment 2 of middle addition 0.3%, 0.5% and 1.0% obtains, high-speed stirred are uniform.It is old to be packed into high temperature
Change tank, 16h is rolled at 200 DEG C, surveys its rheological characteristic and filter loss respectively, the results are shown in Table 4.
Rheological characteristic and filter loss test result of the fluid loss additive in fresh water-based slurry under 4 hot conditions of table
| Experiment slurry | AV(mPa.s) | PV(mPa.s) | YP(Pa) | FLAPI(mL) |
| + 0.3% fluid loss additive of fresh water-based slurry | 23.5 | 20 | 3.5 | 11.5 |
| + 0.5% fluid loss additive of fresh water-based slurry | 11.5 | 10 | 1.5 | 14.8 |
| + 1.0% fluid loss additive of fresh water-based slurry | 6.5 | 5 | 1.5 | 8.4 |
As shown in Table 4, fluid loss additive product of the invention still has the filter of good drop under the conditions of fresh water-based slurry, 200 DEG C
Performance is lost, illustrates that the fluid loss additive has preferable high temperature resistant property.
Embodiment 8
Compound alkali slurry is prepared in the way of embodiment 6, obtains the compound alkali slurry of prehydration.
Experiment slurry is prepared：The compound alkali slurry of three parts of prehydrations is taken, under constant stirring respectively to the good complex salt of prehydration
The heat resisting fluid loss reducing agent that 0.5%, 1.0% and 1.5% embodiment 2 obtains is added in base slurry, high-speed stirred is uniform.Continuous
0.5%~2.5% evaluation sample is added into the good compound salt-water basic slurry of prehydration under stirring, high-speed stirred is uniform.It is transferred to
High temperature ageing tank rolls 16h at 160 DEG C, surveys its rheological characteristic and filter loss, the results are shown in Table 5.
Rheological characteristic and filter loss test result of the fluid loss additive in compound alkali slurry under 5 hot conditions of table
| Experiment slurry | AV(mPa.s) | PV(mPa.s) | YP(Pa) | FLAPI(mL) |
| Compound alkali starches+0.5% fluid loss additive | 6 | 5 | 1 | 59 |
| Compound alkali starches+1.0% fluid loss additive | 6.5 | 5 | 1.5 | 48.8 |
| Compound alkali starches+1.5% fluid loss additive | 15 | 8 | 7 | 24.8 |
As shown in Table 5, fluid loss additive product of the invention starch in compound alkali, 160 DEG C under the conditions of, still there is good drop
Filtration property illustrates that the fluid loss additive has preferable high-temperature resisting and salt-resisting performance.
Embodiment 9
Fresh water-based slurry is prepared in the way of embodiment 4, obtains prehydration fresh water-based slurry.
Six parts of prehydration fresh water-based slurrys are taken, are added 0.5% into the good fresh water-based slurry of prehydration under constant stirring respectively
The fluid loss additive for preparing of embodiment 2 and other 5 kinds of traditional fluid loss additives, wherein LV-PAV is low adhesive aggregation anionic cellulose,
HV-PAV is PAC HV, and PMHC is composite metal zwitterionic polymer, and PAMS-900 is multi-component copolymer
Object fluid loss additive, SF-1 are acrylate copolymer fluid loss additives, and high-speed stirred is uniform.This six classes product is tested respectively in fresh water
In use, rheological characteristic and filter loss at room temperature and 200 DEG C after aging 16h, the results are shown in Table 6 in base slurry.
Rheological characteristic and filter loss test result of the different fluid loss additives of table 6 under room temperature and hot conditions
As can be seen from Table 6, the heat resisting fluid loss reducing agent that prepared by the present invention and other 5 kinds traditional fluid loss additive progresses pair
Than fluid loss additive of the invention drop dehydration effect is optimal, while the front and back rheological property variation of heat rolling is small, and heat-resisting property is good.
As seen from the above embodiment, there is fluid loss additive of the present invention stronger heat and salinity tolerance ability, high temperature resistance can reach
200℃；160 DEG C can be reached in compound salt-water basic slurry drilling fluid and keep preferable filtrate loss controllability, meet its heat-resistant salt-resistant
The requirement of performance.Therefore, which has preferable heat and salt resistance
Energy.
The preparation method of heat resisting fluid loss reducing agent provided by the invention is simple and feasible, and preparation temperature is no more than 70 DEG C, condition
It is mild controllable.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of heat resisting fluid loss reducing agent, includes the following steps：
Comonomer water-soluble liquid is provided；The comonomer includes acrylic acid, acrylamide, 2- acrylamido -2- methyl
Propane sulfonic acid, sodium styrene sulfonate and acrylonitrile；
The pH value for adjusting the comonomer water-soluble liquid using alkaline pH adjuster obtains alkaline monomer dissolving to 8~9
Liquid；
The alkaline monomer lysate is mixed with oxidized form initiator, reduced form initiator, molecular weight regulator, is polymerize
Reaction, obtains jel product；
The dry jel product, obtains heat resisting fluid loss reducing agent.
2. preparation method according to claim 1, which is characterized in that acrylic acid, third in the comonomer water-soluble liquid
Acrylamide, 2- acrylamide-2-methylpro panesulfonic acids, sodium styrene sulfonate, acrylonitrile and water mass ratio be (310~330)：
(310~330)：(140~160)：(230~260)：(130~160)：(130~160).
3. preparation method according to claim 1 or 2, which is characterized in that the quality of the molecular weight regulator is alkalinity
The 0.05~0.2% of comonomer gross mass in monomer lysate；The molecular weight regulator includes thioglycolic, sulfydryl second
It is one or more in acid, mercaptopropionic acid and sodium formate.
4. preparation method according to claim 1 or 2, which is characterized in that the quality of the oxidized form initiator is alkalinity
The 1~2% of comonomer gross mass in monomer lysate；The oxidized form initiator includes ammonium persulfate, potassium peroxydisulfate, over cure
It is one or more in sour sodium and hydrogen peroxide.
5. preparation method according to claim 1 or 2, which is characterized in that the quality of the reduced form initiator is alkalinity
The 1~2% of comonomer gross mass in monomer lysate；The reduced form initiator includes sodium hydrogensulfite, sodium sulfite, Asia
It is one or more in potassium sulfate and sodium thiosulfate.
6. preparation method according to claim 1, which is characterized in that the temperature of the polymerisation is 60~65 DEG C, is gathered
The time for closing reaction is 5~7h.
7. preparation method according to claim 1, which is characterized in that the moisture content of heat resisting fluid loss reducing agent after the drying
≤ 15wt%.
8. the heat resisting fluid loss reducing agent that any one of claim 1~7 preparation method is prepared；The high temperature resistance filtrate reducing
The weight average molecular weight of agent is 5~3,000,000；
The heat resisting fluid loss reducing agent has structural formula shown in Formulas I：
In Formulas I, x：y：z：m：N=(31~33)：(23~26)：(14~16)：(31~33)：(13~16).
9. a kind of water-base drilling fluid, including water based slurry and fluid loss additive, which is characterized in that the fluid loss additive is claim
Heat resisting fluid loss reducing agent described in 8；The quality of the heat resisting fluid loss reducing agent is the 1~5% of drilling fluid gross mass.
10. water-base drilling fluid according to claim 9, which is characterized in that in terms of mass parts, the water based slurry includes 3
~4 parts of sodium bentonites, 0.25 part of natrium carbonicum calcinatum and 100 parts of water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810367916.9A CN108342188A (en) | 2018-04-23 | 2018-04-23 | A kind of heat resisting fluid loss reducing agent and preparation method thereof and a kind of water-base drilling fluid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810367916.9A CN108342188A (en) | 2018-04-23 | 2018-04-23 | A kind of heat resisting fluid loss reducing agent and preparation method thereof and a kind of water-base drilling fluid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108342188A true CN108342188A (en) | 2018-07-31 |
Family
ID=62955433
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810367916.9A Pending CN108342188A (en) | 2018-04-23 | 2018-04-23 | A kind of heat resisting fluid loss reducing agent and preparation method thereof and a kind of water-base drilling fluid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108342188A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112175135A (en) * | 2019-07-01 | 2021-01-05 | 中国石油化工股份有限公司 | High-molecular polymer 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 |
| CN114773539A (en) * | 2022-05-06 | 2022-07-22 | 中国石油大学(华东) | High-temperature-resistant high-salt-resistant micro-crosslinking hydrophobic association tackifying filtrate reducer for water-based drilling fluid and preparation method thereof |
| CN115124667A (en) * | 2022-03-24 | 2022-09-30 | 中石化石油工程技术服务有限公司 | Preparation method of filtrate reducer for high-temperature high-density brine drilling fluid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643632A (en) * | 2012-04-06 | 2012-08-22 | 茂名市三元化工有限公司 | High-temperature salt-resistant fluid loss agent and production method thereof |
| CN104829784A (en) * | 2015-05-25 | 2015-08-12 | 西南石油大学 | Dissoluble polymeric microsphere deep profile modifying and flooding agent and preparation method thereof |
| CN105884954A (en) * | 2016-06-15 | 2016-08-24 | 中国海洋石油总公司 | Temperature-resistant and salt-resistant latex blocking agent and preparation method thereof |
-
2018
- 2018-04-23 CN CN201810367916.9A patent/CN108342188A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643632A (en) * | 2012-04-06 | 2012-08-22 | 茂名市三元化工有限公司 | High-temperature salt-resistant fluid loss agent and production method thereof |
| CN104829784A (en) * | 2015-05-25 | 2015-08-12 | 西南石油大学 | Dissoluble polymeric microsphere deep profile modifying and flooding agent and preparation method thereof |
| CN105884954A (en) * | 2016-06-15 | 2016-08-24 | 中国海洋石油总公司 | Temperature-resistant and salt-resistant latex blocking agent and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112175135A (en) * | 2019-07-01 | 2021-01-05 | 中国石油化工股份有限公司 | High-molecular polymer and preparation method and application thereof |
| CN112175135B (en) * | 2019-07-01 | 2023-03-21 | 中国石油化工股份有限公司 | High-molecular polymer 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 |
| CN113563510B (en) * | 2021-08-09 | 2022-09-06 | 建平天正矿业有限公司 | Temperature-resistant salt-resistant comb polymer fluid loss additive for drilling mud bentonite |
| CN115124667A (en) * | 2022-03-24 | 2022-09-30 | 中石化石油工程技术服务有限公司 | Preparation method of filtrate reducer for high-temperature high-density brine drilling fluid |
| CN115124667B (en) * | 2022-03-24 | 2023-11-03 | 中石化石油工程技术服务有限公司 | Preparation method of filtrate reducer for high-temperature high-density brine drilling fluid |
| CN114773539A (en) * | 2022-05-06 | 2022-07-22 | 中国石油大学(华东) | High-temperature-resistant high-salt-resistant micro-crosslinking hydrophobic association tackifying filtrate reducer for water-based drilling fluid and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108342188A (en) | A kind of heat resisting fluid loss reducing agent and preparation method thereof and a kind of water-base drilling fluid | |
| DE19909231C2 (en) | Water-soluble copolymers based on AMPS and their use as drilling aids | |
| CN105462568B (en) | A kind of drilling fluid resinae nano-particle latex sealing agent and preparation method | |
| CN106479457B (en) | A kind of drilling fluid heat and salinity tolerance thinner and its preparation and use | |
| JP2019501988A (en) | Crosslinked polymers derived from monomers having acryloyl and lactam and sulfonic acid / sulfonate comonomers, compositions thereof and applications thereof | |
| EP1045869A1 (en) | Cementation auxiliary agent | |
| CN107245329B (en) | Deep-well sulphonated polymer mud and preparation method thereof | |
| CN104312548B (en) | A kind of phosphorous high temperature resistant drilling fluids thinner and preparation method thereof | |
| CN108774509A (en) | A kind of drilling fluid heat and salinity tolerance high temperature and pressure fluid loss additive and preparation method thereof | |
| DE102005051906A1 (en) | Mixed polymer based on olefinic sulfonic acids | |
| CN104388063B (en) | Micro-crosslinked polymer fluid loss additive for drilling fluid and preparation method thereof | |
| CN102433107A (en) | Low-molecular-weight polymer type filtrate loss reducer for drilling fluid and preparation method for same | |
| CN101712865B (en) | Viscoelastic weak gel profile control agent | |
| CN104357030B (en) | A kind of drilling fluid branched polymer inorganic agent and preparation method thereof | |
| CN104558217A (en) | Cross-linked starch for drilling fluid and preparation method thereof | |
| CN108753267A (en) | Drilling fluid and completion fluid anti-superhigh temperature anionic polymer fluid loss additive and preparation method thereof | |
| CN108587580A (en) | Drilling fluid high-temperature salt-resistant fluid loss additive modified gum resin and preparation method thereof | |
| CN109054782B (en) | Thermo-sensitive polymer rheological regulator suitable for ocean and constant-current modified water-based drilling fluid | |
| CN106758392A (en) | A kind of new dye stamp synthetic thickening agent and preparation method thereof, application | |
| CN106905937A (en) | A kind of oil base drilling fluid extracting and cutting agent and preparation method thereof | |
| CN107629768A (en) | A kind of superhigh temperature resistant water-base drilling fluid | |
| CN104910330A (en) | High-density fluid loss additive for drilling fluids and preparation method thereof | |
| CN106519136A (en) | Inverse emulsion polymer and preparation method and application thereof in preparation of water-based drilling fluid | |
| CN106366243A (en) | Method for synthesizing betaine copolymer filtrate loss reducer for drilling fluid | |
| CN104152130B (en) | AM/NaAA/NIDA hydrophobic associated polymer oil displacement agent and synthetic method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180731 |