CN108727536A - A kind of shale gas reservoir slippery water fracturing fluid polymer drag reducer and preparation method thereof - Google Patents
A kind of shale gas reservoir slippery water fracturing fluid polymer drag reducer and preparation method thereof Download PDFInfo
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- CN108727536A CN108727536A CN201810558937.9A CN201810558937A CN108727536A CN 108727536 A CN108727536 A CN 108727536A CN 201810558937 A CN201810558937 A CN 201810558937A CN 108727536 A CN108727536 A CN 108727536A
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- structural unit
- drag reducer
- monomer
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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
- C08F220/56—Acrylamide; Methacrylamide
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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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/882—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
A kind of shale gas reservoir slippery water fracturing fluid polymer drag reducer, using acrylamide and salt resistant function monomer, it is made by inverse emulsion polymerization method, simple production process, low production cost, reaction efficiency is high, product belongs to acrylamide quadripolymer, viscosity average molecular weigh 3,000,000~15,000,000, with outstanding resistance to high salinity effect, the adaptability of drag reducer has been significantly greatly increased, in turn, highly mineralized formation brines may be used in preparing fracturing fluid, return draining in stratum, it is allowed to be utilized effectively, to reduce onsite application cost, take full advantage of water resource, it is effectively protected environment, in addition to this, drag reducer emulsion-stabilizing, dissolubility is good, easily anti-row.
Description
Technical field
The invention belongs to the fracturing fluid additive fields of shale gas fracturing technique, and in particular to a kind of shale gas reservoir slippery water
Fracturing fluid polymer drag reducer and preparation method thereof.
Technical background
The region of shale gas rich content is often the very poor area of water resource, such as according to the number of world resource association
According to shown, China possess the world it is most exploit shale gas resource, but these resources be mainly all distributed in as Tarim Basin,
The place that water resource extremely lacks in this way such as Sichuan Basin.And there is 15%~75% to return in shale gas reservoir slippery water fracturing process
Draining, which is returned, is discharged to ground, and direct emission is seriously polluted, emission scenary complex treatment process after processing, and cost is higher.To respond state
Family's environmental protection and the call for saving water resource, using returning draining or water flooding is carried out with liquid scheme in Sichuan Fuling Weiyuan
Etc. being implemented.But since inorganic salts are affected to drag reducer performance, and return draining and formation water salinity is higher, part
Regional formation water salinity is up to 20 × 104Mg/L, what is be used repeatedly returns drain salinity and can also gradually increase, and needs pair
Water quality carries out multistep treatment, and inorganic salt treatment is complex.According to related research shows that when calcium ion concentration is more than 200mg/L,
When magnesium ion concentration is more than 100mg/L, drag reduction by polymer water viscosity, drag reduction can be adversely effected, or even flocculate
Or precipitation.And 8500~24000mg/ of draining calcium ion content is returned for the water quality of high calcium-containing magnesium ion, such as areas Marcellus
L, 933~1790mg/L of magnesium ion, common drag reducer can not adapt to, and also not find temporarily to be directed to high calcium-containing magnesium ion in the market
Drag reducer.Although Kemira companies have been developed that a kind of polyacrylamide emulsion system drag reducer, molecular weight are up to 2~4
×108, can be 23 × 104Mg/L salt still has higher drag reducing efficiency under water, but under the conditions of excessively high calcium ions and magnesium ions, performance according to
So it is a greater impact.So while research and development one kind having resistance to high-salinity water quality, to the specific condition of high calcium-containing magnesium ion
The drag reducer that water quality still adapts to is compeled required.To make drag reducer that there is high drag-reduction effect, spy to propose in concentrated water
The invention.
Invention content
The object of the present invention is to provide a kind of shale gas reservoir slippery water fracturing fluid polymer drag reducer and preparation method thereof,
The emulsion polymer drag reducer solution rate of preparation is fast, and Efficient Adhesive Promotion is good, and resistance reducing performance is excellent, and rock core adsorbance is low, easily the row of returning,
Salt tolerant effect is good, and industrial manufacture process is simple, mainly for pit shaft drop resistance in shale gas reservoir slippery water fracturing technology.
The technical solution adopted by the present invention is that：
A kind of shale gas reservoir slippery water fracturing fluid polymer drag reducer, belongs to acrylamide quadripolymer, contains
Structural unit A, structural unit B, structural unit C, structural unit D, the structural formula of each structural unit are as follows：
On the basis of the gross mass of each structural unit in the acrylamide quadripolymer, the structural unit A's
Quality accounts for the 50~90% of gross mass, and the quality of the structural unit B accounts for the 10~30% of gross mass, the structural unit C's
Quality accounts for the 5~20% of gross mass, and the quality of the structural unit D accounts for the 0.1~2% of gross mass；
In structural unit A, R1For one kind in H, methyl, ethyl, n-propyl or isopropyl；
In structural unit B, M Li, Na, K, Rb or Cs；
In structural unit C, R2And R3Selected from H, methyl, ethyl, n-propyl or isopropyl, n1 >=1, S are sulfonic acid foundation
Group；
In structural unit D, R4Selected from H, methyl, ethyl, n-propyl or isopropyl, R5Selected from methyl, ethyl, propyl, fourth
Base, amyl, hexyl, heptyl, octyl, nonyl, decyl, C11~C16, polyoxyethylene ether long-chain, R6Selected from methyl, ethyl, third
Base, butyl, amyl, hexyl, heptyl, octyl, nonyl, decyl, C11~C16, polyoxyethylene ether long-chain.
Further, the viscosity average molecular weigh of the acrylamide quadripolymer is 3,000,000~15,000,000.
A kind of preparation method of shale gas reservoir slippery water fracturing fluid polymer drag reducer, includes the following steps：
The first step mixes each monomer and deionized water, and after being uniformly dissolved, it is 7~9 to adjust pH value with sodium hydroxide,
Obtain water phase mixed liquor；
Emulsifier is dissolved in oil phase, stirred by second step, obtains oil phase mixed solvent；
Third walks, and water phase mixed liquor prepared by the first step is slowly dropped to the oil phase in the mixed solvent of second step preparation,
It is sufficiently stirred emulsification；
Initiator is added under the conditions of 30~60 DEG C of temperature, high-speed stirreds after leading to 30~60min of nitrogen deoxygenation in 4th step,
High-speed stirred is reacted 2~4 hours, and polymer drag reducer is obtained；
Wherein, the monomer includes monomer E, monomer F, monomer G, monomer H, and each monomer structure formula is as follows：
In the raw material for preparing polymer drag reducer, emulsifier mass percent is 4%~10%, and oil phase mass percent is
40%-60%, initiator quality percentage are 0.01%-0.1%, remaining is water phase mixed liquor, wherein monomer E, monomer F, list
Body G, monomer H are respectively 15~30%, 3%~9%, 2%~6%, 0.01%~1% with the mass ratio of deionized water.
Further, the emulsifier be Span20, Span40, Span60, Span65, Span80, Span85,
Tween20, Tween40, Tween60, Tween65, Tween80, Tween85, OP-4, OP-7, OP-9, OP-10, OP-13,
It is one or more in OP-15, OP-20, OP-30, OP-40, OP-50.
Further, the oil phase is one or more mixing in diesel oil, white oil, hexamethylene.
Further, the initiator includes oil-soluble initiator and water soluble starter, and the two is according to 1:1~1:1.2
Mass ratio composition, the total dosage of initiator accounts for the 0.005%-0.02% of lotion gross mass, wherein oil-soluble initiator is azo
Two different heptonitriles (AIBN), tert-butyl hydroperoxide, one or more mixing in peroxidized t-butyl perbenzoate；Water solubility causes
Agent is potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate, azo-bis-isobutyrate hydrochloride (AIBA), two isobutyl imidazoline hydrochloric acid of azo
One or more mixing in salt (AIBI), azo-bis-isobutyl cyanide.
Beneficial effects of the present invention：
The present invention obtains high molecular emulsion polymer using acrylamide and salt resistant function monomer, by inverse emulsion polymerization
Drag reducer, simple production process, low production cost, and also with outstanding resistance to high salinity effect, (0.1% drag reducer is total
Salinity is 10 × 104The high calcium-containing magnesium ion (5 × 10 of mg/L3mg/L Ca2+, 2 × 103mg/L Mg2+) have in brine
65.82% drag reduction efficiency (Fig. 2)；0.2% drag reducer is 20 × 10 in total salinity4Mg/L high calcium-containing magnesium ion (2 ×
104mg/L Ca2+, 2 × 103mg/L Mg2+) drag reduction efficiency (Fig. 3) that 63.83% is kept in brine, drag reducer has been significantly greatly increased
Adaptability, in turn, highly mineralized formation brines may be used in preparing fracturing fluid, draining is returned on stratum, is allowed to be utilized effectively, from
And onsite application cost is reduced, water resource is taken full advantage of, environment is effectively protected.
Drag reducer prepared by the present invention also has the advantages that dissolubility is good, shear resistant is good, and in clear water, drag reducer can be
It is completely dissolved within 3 minutes, in concentrated water, drag reducer is completely dispersed dissolving within 5 minutes；In 1000s-1~
7000s-1Under shear rate, resistance reducing performance gradually increases (Fig. 2 and Fig. 3).
In addition to this, initiator of the invention selection is stability and product based on polymerized emulsion in emulsion polymerization process
Quality requirement, uses oil-soluble initiator and water soluble starter dual-split causes the method polymerizeing and prepares drag reducer, because
And reaction efficiency higher.
Description of the drawings
Fig. 1 is the drag reducer polymer product infared spectrum of embodiment 1；
1 drag reducer of embodiment that Fig. 2 is 0.1% is 10 × 104(different calcium ion contents) salt tolerant drag reduction is imitated in ppm brine
Fruit；
2 drag reducer of embodiment that Fig. 3 is 0.2% is 20 × 104(different calcium ion contents) salt tolerant drag reduction is imitated in ppm brine
Fruit.
Specific implementation mode
Embodiment 1
A kind of shale gas reservoir slippery water fracturing fluid polymer drag reducer, by following material quality composition of proportions：
Water phase：Monomer E, monomer F, monomer G, monomer H mass ratios are：70:20:10:0.5；Monomer gross mass 3kg；Water
7kg；
Oil phase：White oil 7.5kg；Emulsifier：The blended emulsifier of Span80/Twee-60, wherein Span-80 dosages
0.738kg, Twee-60 dosage 0.095kg；
Initiator：Water soluble starter is potassium peroxydisulfate, and dosage accounts for the 0.01% of overall reaction system, and oil-soluble initiator is
Azobisisoheptonitrile (AIBN), dosage are the 0.01% of overall reaction system；
Preparation method includes the following steps：
The first step, by monomer and deionized water mixed dissolution it is uniform after, with sodium hydroxide solution adjust pH value be 7, obtain
Water phase mixed liquor；
Emulsifier is dissolved in oil phase, stirred by second step, obtains oil phase mixed solvent；
Third walks, and grease mixes, and the water phase mixed liquor that the first step is prepared is slowly dropped to second step preparation
Oil phase in the mixed solvent is sufficiently stirred emulsification, not occur being layered as standard within one week；
After leading to nitrogen deoxygenation 30min, azobisisoheptonitrile (AIBN) is added in 4th step under the conditions of 35 DEG C, high-speed stirred,
Potassium peroxydisulfate is added after 30min, high-speed stirred is reacted 2 hours, and polymer drag reducer is obtained.
Embodiment 2
A kind of shale gas reservoir slippery water fracturing fluid polymer drag reducer, is made of following material quality ratio：
Water phase：Monomer E, monomer F, monomer G, monomer H mass ratios are：80:15:5:0.5；Monomer gross mass 3kg；Water
9kg；
Oil phase：Hexamethylene 7.2kg；Emulsifier：The blended emulsifier of Span80/OP-10, wherein Span-80 dosages
0.7448kg, OP-10 dosage 0.055kg；
Initiator：Water soluble starter is two isobutyl imidazoline hydrochloride (VA-044) of azo, oil-soluble initiator azo
Two different heptonitriles (AIBN), VA-044 dosages are 0.002kg, AIBN dosages 0.0018kg；
A kind of production technology of shale gas reservoir slippery water fracturing fluid polymer drag reducer, includes the following steps：
The first step, by monomer and deionized water mixed dissolution it is uniform after, with sodium hydroxide solution adjust pH value be 8, obtain
Water phase mixed liquor；
Emulsifier is dissolved in oil phase, stirred by second step, obtains oil phase mixed solvent；
Third walks, and the water phase mixed liquor that the first step is prepared is slowly added dropwise to the oil phase mixed solvent of second step preparation
In, it is sufficiently stirred emulsification, not occur being layered as standard within one week；
4th step, after leading to nitrogen deoxygenation 30mins, be successively added at 60 DEG C, under the conditions of high-speed stirred oil-soluble initiator and
Water soluble starter, high-speed stirred are reacted 4 hours, and polymer drag reducer is obtained.
Infared spectrum analysis is carried out to drag reducer polymer prepared by embodiment 1, as shown in Figure 1, in 3420cm-1That locates is strong
Absorption peak is-NH in acyl group amido (- CONH2)2Stretching vibration peak, show that monomer E is successfully introduced into polymer.1660cm-1The peak at place is that C=O stretches peak, is the blending surface flexural vibrations peak of C-N at 1396cm-1.In 3233cm-1It is stretched for N-H at place
Contracting vibration peak, it was demonstrated that monomer F is successfully introduced into polymer chain.1186cm-1, 1112cm-1And 1038cm-1Place is-SO1-In it is right
Title and nonsymmetrical vibration absorption peak, show that monomer G is successfully introduced into polymer chain.In 2913cm-1~2852cm-1It observes at place
Peak by the asymmetric stretching vibration peak for-CH3, show that monomer H has been successfully introduced into polymer.Peak is in 619cm-1Place,
Corresponding to the out-of-plane bending vibration of the superposition absorption peak and-NH2 (- CONH2) of-SO3 stretching vibrations.
Claims (6)
1. a kind of shale gas reservoir slippery water fracturing fluid polymer drag reducer, which is characterized in that quarternary copolymerized for acrylamide
Object, containing structural unit A, structural unit B, structural unit C, structural unit D, the structural formula of each structural unit is as follows：
On the basis of the gross mass of each structural unit in the acrylamide quadripolymer, the quality of the structural unit A
The 50~90% of gross mass are accounted for, the quality of the structural unit B accounts for the 10~30% of gross mass, the quality of the structural unit C
The 5~20% of gross mass are accounted for, the quality of the structural unit D accounts for the 0.1~2% of gross mass；
In structural unit A, R1For one kind in H, methyl, ethyl, n-propyl or isopropyl；
In structural unit B, M Li, Na, K, Rb or Cs；
In structural unit C, R2And R3Selected from H, methyl, ethyl, n-propyl or isopropyl, n1>=1, S are sulfonate group；
In structural unit D, R4Selected from H, methyl, ethyl, n-propyl or isopropyl, R5Selected from methyl, ethyl, propyl, butyl,
Amyl, hexyl, heptyl, octyl, nonyl, decyl, C11~C16, polyoxyethylene ether long-chain, R6Selected from methyl, ethyl, propyl, fourth
Base, amyl, hexyl, heptyl, octyl, nonyl, decyl, C11~C16, polyoxyethylene ether long-chain.
2. shale gas reservoir slippery water fracturing fluid polymer drag reducer as described in claim 1, which is characterized in that the propylene
The viscosity average molecular weigh of amide system quadripolymer is 3,000,000~15,000,000.
3. a kind of preparation method of shale gas reservoir slippery water fracturing fluid polymer drag reducer, which is characterized in that including following step
Suddenly：
The first step mixes each monomer and deionized water, and after being uniformly dissolved, it is 7~9 to adjust pH value with sodium hydroxide, is obtained
Water phase mixed liquor；
Emulsifier is dissolved in oil phase, stirred by second step, obtains oil phase mixed solvent；
Third walks, and water phase mixed liquor prepared by the first step is slowly dropped to the oil phase in the mixed solvent of second step preparation, fully
Stirring and emulsifying；
Initiator is added under the conditions of 30~60 DEG C of temperature, high-speed stirreds after leading to 30~60min of nitrogen deoxygenation in 4th step, high speed
It is stirred to react 2~4 hours, obtains polymer drag reducer；
Wherein, the monomer includes monomer E, monomer F, monomer G, monomer H, and each monomer structure formula is as follows：
In the raw material for preparing polymer drag reducer, emulsifier mass percent is 4%~10%, and oil phase mass percent is
40%-60%, initiator quality percentage are 0.01%-0.1%, remaining is water phase mixed liquor, wherein monomer E, monomer F, list
Body G, monomer H are respectively 15~30%, 3%~9%, 2%~6%, 0.01%~1% with the mass ratio of deionized water.
4. a kind of preparation method of shale gas reservoir slippery water fracturing fluid polymer drag reducer as claimed in claim 3, special
Sign is, the emulsifier is Span20, Span40, Span60, Span65, Span80, Span85, Tween20, Tween40,
Tween60, Tween65, Tween80, Tween85, OP-4, OP-7, OP-9, OP-10, OP-13, OP-15, OP-20, OP-30,
It is one or more in OP-40, OP-50.
5. a kind of preparation method of shale gas reservoir slippery water fracturing fluid polymer drag reducer as claimed in claim 3, special
Sign is that the oil phase is one or more mixing in diesel oil, white oil, hexamethylene.
6. a kind of preparation method of shale gas reservoir slippery water fracturing fluid polymer drag reducer as claimed in claim 3, special
Sign is that the initiator includes oil-soluble initiator and water soluble starter, and the two is according to 1:1~1:1.2 mass ratio group
At the total dosage of initiator accounts for the 0.005%-0.02% of lotion gross mass, wherein oil-soluble initiator is azobisisoheptonitrile
(AIBN), tert-butyl hydroperoxide, one or more mixing in peroxidized t-butyl perbenzoate；Water soluble starter is over cure
Sour potassium, sodium peroxydisulfate, ammonium persulfate, azo-bis-isobutyrate hydrochloride (AIBA), two isobutyl imidazoline hydrochloride (AIBI) of azo,
One or more mixing in azo-bis-isobutyl cyanide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265605A (en) * | 2018-11-26 | 2019-01-25 | 西南石油大学 | A kind of low adsorption salt tolerant friction reducer suitable for shale reservoir fracturing reform |
| CN112410013A (en) * | 2020-10-15 | 2021-02-26 | 德仕能源科技集团股份有限公司 | Suspension liquid drag reducer and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104250339A (en) * | 2013-06-28 | 2014-12-31 | 中国石油化工股份有限公司 | Acrylamide copolymer and its preparation method and use |
| CN104403656A (en) * | 2014-11-27 | 2015-03-11 | 胜利油田胜利化工有限责任公司 | Novel zwitterionic slickwater fracturing fluid and preparation method thereof |
-
2018
- 2018-06-01 CN CN201810558937.9A patent/CN108727536A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104250339A (en) * | 2013-06-28 | 2014-12-31 | 中国石油化工股份有限公司 | Acrylamide copolymer and its preparation method and use |
| CN104403656A (en) * | 2014-11-27 | 2015-03-11 | 胜利油田胜利化工有限责任公司 | Novel zwitterionic slickwater fracturing fluid and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265605A (en) * | 2018-11-26 | 2019-01-25 | 西南石油大学 | A kind of low adsorption salt tolerant friction reducer suitable for shale reservoir fracturing reform |
| CN109265605B (en) * | 2018-11-26 | 2020-12-04 | 西南石油大学 | Low-adsorption salt-resistant resistance-reducing agent suitable for shale reservoir fracturing transformation |
| CN112410013A (en) * | 2020-10-15 | 2021-02-26 | 德仕能源科技集团股份有限公司 | Suspension liquid drag reducer and preparation method and application thereof |
| CN112410013B (en) * | 2020-10-15 | 2022-08-02 | 德仕能源科技集团股份有限公司 | Suspension liquid drag reducer and preparation method and application thereof |
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Application publication date: 20181102 |