CN110079293A - Nano-cellulose base fracturing fluid and preparation method thereof - Google Patents
Nano-cellulose base fracturing fluid and preparation method thereof Download PDFInfo
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- CN110079293A CN110079293A CN201910445292.2A CN201910445292A CN110079293A CN 110079293 A CN110079293 A CN 110079293A CN 201910445292 A CN201910445292 A CN 201910445292A CN 110079293 A CN110079293 A CN 110079293A
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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
- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
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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
- C09K8/90—Compositions based on water or polar solvents containing organic compounds macromolecular compounds of natural origin, e.g. polysaccharides, cellulose
- C09K8/905—Biopolymers
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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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/08—Fiber-containing well treatment fluids
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Abstract
The invention belongs to nano-cellulose fields, and in particular to a kind of nano-cellulose base fracturing fluid and preparation method thereof, preparation method includes the following steps: 1) dispersion liquid that guar gum powder is dissolved into 1-10%；2) gel or dispersion liquid of the nano-cellulose of the guar gum dispersion liquid and 0.6-25% that obtain step 1)；Mixed liquor is formed after mixing, and the crosslinking agent of mixed liquor 1-5% is added；Post-crosslinking reaction 1-30min；System pH is 9.5-10.0, and temperature is 20-40 DEG C；Wherein, the dry weight of the guar gum and nano-cellulose ratio are as follows: 100:10-25.Cellulose nano-fibrous addition can improve the gel strength after guar gum crosslinking, improve its apparent viscosity, enhance sediment carrying capacity；Meanwhile after fibrous nanofiber and guar gum crosslinking, the salt tolerant temperature resistant capability of Guar fracturing fluid can be improved, promote fracturing effect.
Description
Technical field
The invention belongs to nano-cellulose fields, and in particular to a kind of nano-cellulose base fracturing fluid and preparation method thereof.
Background technique
Cellulose nano-fibrous is a kind of native cellulose fibre isolated by plant fiber, and length dimension is several
Hundred nanometers to tens microns, a kind of filamentary fibers cellulose fiber that diameter is tens nanometers.Conventional method is prepared cellulose and receives
Rice fiber is similar to the gel of jelly, and concentration is 10% or less.It is cellulose nano-fibrous due to its special fiber size, make
It makes it possess higher surface-active with huge specific surface area, a large amount of hydroxyl in surface, and special fluid behaviour makes it
There is potential application value in petroleum industry.Cellulose nano-fibrous its size of element is rich in hydroxyl on micro-nano rank, surface, easily
In modification, therefore it in stratum high-temperature hypersaline environment, fibrous nanofiber has advantage outstanding.
Guar gum and modified guar are widely used in the pressure break of petroleum drilling and mining process, such as guar gum, hydroxypropyl at present
The guar derivative of base guar gum, carboxymethyl guar gum and functional modification.Guar gum is in natural cluster bean
It extracts, belongs to polysaccharose substance, contain a large amount of hydroxyl, apparent viscoplasticity with higher in strand.Oil fracturing mistake
Cheng Zhong, it will usually be crosslinked the hydroxyl between guar gum different molecular chain using crosslinking agents such as boraxs, to become
Jelly and be applied to pressure break.
Summary of the invention
The purpose of the present invention is to provide a kind of nano-cellulose base fracturing fluids and preparation method thereof.
The present invention to achieve the above object, using following technical scheme:
A kind of preparation method of nano-cellulose base fracturing fluid, includes the following steps:
1) guar gum powder is dissolved into the dispersion liquid of 1-10%；
2) gel or dispersion liquid of the nano-cellulose of the guar gum dispersion liquid and 0.6-25% that obtain step 1)；It is mixed
Mixed liquor is formed after closing uniformly, the crosslinking agent of mixed liquor 1-5% is added；Post-crosslinking reaction 1-30min；System pH is 9.5-
10.0, temperature is 20-40 DEG C；Wherein, the absolute dry mass of the guar gum and nano-cellulose ratio are as follows: 100:10-25.
The guar gum is hydroxypropyl guar gum, non-modified guar gum, one of carboxymethyl guar gum or several
Kind.
The nano-cellulose is the mixing of one or more of cellulose nanometer fibril and Cellulose nanocrystal body.
The cellulose nanometer fibril diameter is 5-20nm, length 700nm-20um；The cellulose Nanowire
Silk includes anion-modified cellulose nanometer fibril, TEMPO system oxycellulose nanofibrils, carboxymethyl-modification fiber
Plain nanofibrils and the cellulose nanometer fibril of surface free chemical modification；
The Cellulose nanocrystal body is that length is 100-300nm, diameter 4-20nm, stick of the crystallinity greater than 85%
Shape crystal；The Cellulose nanocrystal body includes the Cellulose nanocrystal body that sour water solution obtains, and TEMPO oxidation system obtains
Cellulose nanocrystal body.
The crosslinking agent is borax, boric acid, sodium tetraborate, sodium borohydride, organic borate cross-linker, titanium tetrachloride, tetrachloro
Change one of zirconium or several.
The invention also includes a kind of nano-cellulose base fracturing fluids, are obtained using the preparation method.
Compared with prior art, the beneficial effects of the present invention are:
Nano-cellulose, consisting of the glucose unit that Isosorbide-5-Nitrae-β-glycosidic bond is formed by connecting, fiber surface contains largely
Hydroxyl, lesser size can be crosslinked under the action of inorganic crosslinking agent with guar gum strand.On the one hand, cellulose is received
The addition of rice fiber can improve the gel strength after guar gum crosslinking, improve its apparent viscosity, enhance sediment carrying capacity；Another party
After face, fibrous nanofiber and guar gum crosslinking, the salt tolerant temperature resistant capability of Guar fracturing fluid can be improved, promote pressure
Split effect.
The present invention utilizes cellulose nano-fibrous nano-scale, biggish draw ratio and surface hydroxyl abundant, through handing over
Join agent and is mutually cross-linked to form jelly with guar gum.The fracturing fluid of the method preparation has preferable apparent viscosity, and gel strength is big, takes
Sand ability is strong, and salt tolerant temperature tolerance is good, can significantly improve fracturing effect, and more traditional guar gum dosage will be lacked.The present invention is simple, passes through
Ji, strong applicability, effect are efficient.
Detailed description of the invention:
Fig. 1 shows the apparent schematic diagram of the cellulose nano-fibrous gel of embodiment 2；
Fig. 2-3 shows the apparent schematic diagram of 2 nano-cellulose base fracturing fluid of embodiment.
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, implement below with reference to best
The present invention is described in further detail for example.In the application unless otherwise specified, percentage composition refers both to mass percentage.
Embodiment 1
Hydroxypropyl guar gum 50g is taken, is added in the water of 5L, is kept stirring in adition process, until guar gum is completely molten
Solution, forms 1% dispersion liquid；Cellulose nanocrystal body (length 200nm, the diameter of the sulphuric acid hydrolysis of 1% concentration is then added
For 7nm) dispersion liquid, additive amount is 10% relative to guar gum dry weight: being kept stirring the adjustment until two kinds of material mixings are uniform
System pH to 9.5.The aqueous solution of 4% sodium borohydride is weighed in mixed liquor, the additional amount of sodium borohydride is the 1% of mixed liquor；
Jelly can be hung by being kept stirring to formation, and carry out performance evaluation.Jelly will be obtained and carry out temperature resistant capability, the anti-shearing survey of heatproof
It is fixed, the measurement of crosslinking time and filtration property.Wherein temperature resistant capability is detection 170S-1Shear rate under, increase temperature to table
See temperature achieved when viscosity is reduced to 50mPas；Heatproof is anti-shearing to be referred in 170S-1Shear rate under, in certain temperature
Apparent viscosity after spending lower continuous shear stress 60min；Filtration property refers to tests in high-temperature and high-pressure filter press, and wherein pressure is kept
In 3.5Mpa.Testing result is shown as obtaining its gelation time of fracturing fluid with upper type as 120s, and temperature resistant capability can reach
145℃；When temperature is 100 DEG C, in 170S-1Shear rate under shear 60min when, when shear time be greater than 18min after, viscosity
It tends towards stability, viscosity is all larger than 250mpas after 18min；Leak-off the results show that 100 DEG C at a temperature of, filter in 30min
Indecorous product is 24ml.
Embodiment 2
Hydroxypropyl guar gum 60g is taken, is added in the water of 1L, is kept stirring in adition process, until guar gum is completely molten
Solution, forms 6% dispersion liquid；Cellulose nano-fibrous (the length 0.8- of the TEMPO oxidation of 0.6% concentration is then added
2um, diameter 15nm) gel (Fig. 1 is shown), additive amount is 15% relative to guar gum dry weight, is kept stirring until two kinds
Material mixing is uniform, and sodium hydroxide solution adjusts system pH to 9.0.Borax (aqueous solution of 4.0% concentration) is weighed in mixed liquor
In, the additional amount of borax is the 5% of mixed liquor；Jelly can be hung to formation by, which being kept stirring, obtains nano-cellulose base fracturing fluid
(Fig. 2-3 is shown), and carry out performance evaluation.Jelly will be obtained and carry out temperature resistant capability, the anti-shearing measurement of heatproof, crosslinking time and filter
Lose the measurement of performance.Wherein temperature resistant capability is detection 170S-1Shear rate under, increase temperature to apparent viscosity be reduced to
Temperature achieved when 50mPas；Heatproof is anti-shearing to be referred in 170S-1Shear rate under, continuous shear stress at a certain temperature
Apparent viscosity after 60min；Filtration property refers to tests in high-temperature and high-pressure filter press, and wherein pressure is maintained at 3.5Mpa.Inspection
Surveying and obtaining its gelation time of fracturing fluid in the above manner as the result is shown is 94s, and temperature resistant capability can reach 151 DEG C；Temperature is
At 120 DEG C, in 170S-1Shear rate under shear 60min when, when shear time be greater than 20min after, viscosity tends towards stability,
Viscosity is all larger than 289mpas after 20min；Leak-off the results show that 120 DEG C at a temperature of, the filtrate volume in 30min is
28ml。
Embodiment 3
Hydroxypropyl guar gum 100g is taken, is added in the water of 1L, is kept stirring in adition process, until guar gum is completely molten
Solution, forms 10% dispersion liquid；Cellulose nano-fibrous (the length 0.8- of the carboxymethyl-modification of 25% concentration is then added
5um, diameter 20nm) dispersion liquid, additive amount relative to guar gum dry weight 25%, be kept stirring until two kinds of material mixings it is equal
It is even, adjust system pH to 10.0.Organic borate cross-linker (aqueous solution of 5.0% concentration) is weighed in mixed liquor, organic boron adds
Enter 2.5% that amount is mixed liquor；Jelly can be hung by being kept stirring to formation, and carry out performance evaluation.Jelly will be obtained to carry out
Temperature resistant capability, the anti-shearing measurement of heatproof, the measurement of crosslinking time and filtration property.Wherein temperature resistant capability is detection 170S-1Cut
Under cutting speed rate, temperature achieved when temperature to apparent viscosity is reduced to 50mPas is increased；Heatproof is anti-shearing to be referred in 170S-1
Shear rate under, the apparent viscosity after continuous shear stress 60min at a certain temperature；Filtration property refers in high temperature and pressure dehydration
It is tested in instrument, wherein pressure is maintained at 3.5Mpa.Testing result is shown as obtaining its gelation time of fracturing fluid with upper type
81s, temperature resistant capability can reach 138 DEG C；When temperature is 120 DEG C, in 170S-1Shear rate under shear 60min when, work as shearing
After time is greater than 25min, viscosity tends towards stability, and viscosity is all larger than 398mpas after 25min；Leak-off is the results show that at 120 DEG C
At a temperature of, the filtrate volume in 30min is 31ml.
Embodiment 4
Hydroxypropyl guar gum 100g is taken, is added in the water of 1L, is kept stirring in adition process, until guar gum is completely molten
Solution, forms 10% dispersion liquid；Cellulose nano-fibrous (the length 0.8- of the carboxymethyl-modification of 25% concentration is then added
5um, diameter 20nm) dispersion liquid, additive amount relative to guar gum dry weight 5%, 10%, 15%, 20% and 25%, keep stirring
Mix until two kinds of material mixings it is uniform, adjust system pH to 10.0.Weigh organic borate cross-linker (aqueous solution of 5.0% concentration) in
In mixed liquor, additional amount is the 5% of mixed liquor；Jelly can be hung by being kept stirring to formation, and carry out performance evaluation.It will obtain
Jelly carries out temperature resistant capability, the anti-shearing measurement of heatproof, the measurement of crosslinking time and filtration property.Wherein temperature resistant capability is detection
170S-1Shear rate under, increase temperature achieved when temperature to apparent viscosity is reduced to 50mPas；Heatproof is anti-shearing to be
Refer in 170S-1Shear rate under, the apparent viscosity after continuous shear stress 60min at a certain temperature；Filtration property refers in height
It is tested in high-temperature and high-pressure filter press, wherein pressure is maintained at 3.5Mpa.Table 1 shows the cellulose nano-fibrous of carboxymethyl-modification and adds
Influence of the dosage to fracturing fluid property parameter
Table 1
The above is only a preferred embodiment of the present invention, for those of ordinary skill in the art, according to the present invention
Thought, there will be changes in the specific implementation manner and application range, and the content of the present specification should not be construed as to the present invention
Limitation.
Claims (6)
1. a kind of preparation method of nano-cellulose base fracturing fluid, which is characterized in that include the following steps:
1) guar gum powder is dissolved into the dispersion liquid of 1-10%；
2) gel or dispersion liquid of the nano-cellulose of the guar gum dispersion liquid and 0.6-25% that obtain step 1)；Mixing is equal
Mixed liquor is formed after even, and the crosslinking agent of mixed liquor 1-5% is added；Post-crosslinking reaction 1-30min；System pH is 9.5-10.0,
Temperature is 20-40 DEG C；Wherein, the dry weight of the guar gum and nano-cellulose ratio are as follows: 100:10-25.
2. the preparation method of nano-cellulose base fracturing fluid according to claim 1, which is characterized in that the guar gum
For hydroxypropyl guar gum, non-modified guar gum, one or more of carboxymethyl guar gum.
3. the preparation method of nano-cellulose base fracturing fluid according to claim 1, which is characterized in that the Nanowire
Dimension element is one of cellulose nanometer fibril and Cellulose nanocrystal body or mixing.
4. the preparation method of nano-cellulose base fracturing fluid according to claim 3, which is characterized in that the cellulose
Nanofibrils diameter is 5-20nm, length 700nm-20um；The cellulose nanometer fibril includes anion-modified fibre
Tie up plain nanofibrils, TEMPO system oxycellulose nanofibrils, carboxymethyl-modification cellulose nanometer fibril and surface
Cellulose nanometer fibril without chemical modification；
The Cellulose nanocrystal body is that length is 100-300nm, diameter 4-20nm, rodlike crystalline substance of the crystallinity greater than 85%
Body；The Cellulose nanocrystal body includes that the Cellulose nanocrystal body that sour water solution obtains or TEMPO oxidation system obtain
Cellulose nanocrystal body.
5. the preparation method of nano-cellulose base fracturing fluid according to claim 4, which is characterized in that the crosslinking agent
For borax, boric acid, sodium tetraborate, sodium borohydride, organic borate cross-linker, titanium tetrachloride, one of zirconium chloride or several.
6. a kind of nano-cellulose base fracturing fluid, which is characterized in that obtained using the described in any item preparation methods of claim 1-5
It arrives.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257041A (en) * | 2019-06-26 | 2019-09-20 | 滨州学院 | Fracturing fluid guar gum-nano-cellulose fiber crosslinked thickening agent and preparation method |
| CN111205848A (en) * | 2020-02-07 | 2020-05-29 | 西南石油大学 | Cellulose nanocrystal hybrid fracturing fluid and preparation method thereof |
| CN112251204A (en) * | 2020-10-19 | 2021-01-22 | 中国石油大学(华东) | Nano-cellulose cross-linking agent for high-temperature-resistant fracturing fluid and preparation method and application thereof |
| CN112646560A (en) * | 2020-12-24 | 2021-04-13 | 中国地质大学（北京） | Method for simulating petroleum recovery by using cellulose nanocrystals |
| CN112850715A (en) * | 2021-01-06 | 2021-05-28 | 江苏福瑞士电池科技有限公司 | Nitrogen-boron co-doped nano silicon-carbon powder material, preparation method and application thereof |
| CN113956862A (en) * | 2021-10-29 | 2022-01-21 | 中国石油大学(华东) | Guanidine gum fracturing fluid gel capable of reducing pH dependence, guanidine gum fracturing fluid system, and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257041A (en) * | 2019-06-26 | 2019-09-20 | 滨州学院 | Fracturing fluid guar gum-nano-cellulose fiber crosslinked thickening agent and preparation method |
| CN110257041B (en) * | 2019-06-26 | 2021-05-14 | 滨州学院 | Guar gum-nano cellulose fiber crosslinking thickener for fracturing fluid and preparation method thereof |
| CN111205848A (en) * | 2020-02-07 | 2020-05-29 | 西南石油大学 | Cellulose nanocrystal hybrid fracturing fluid and preparation method thereof |
| CN112251204A (en) * | 2020-10-19 | 2021-01-22 | 中国石油大学(华东) | Nano-cellulose cross-linking agent for high-temperature-resistant fracturing fluid and preparation method and application thereof |
| CN112251204B (en) * | 2020-10-19 | 2022-08-09 | 中国石油大学(华东) | Nano-cellulose cross-linking agent for high-temperature-resistant fracturing fluid and preparation method and application thereof |
| CN112646560A (en) * | 2020-12-24 | 2021-04-13 | 中国地质大学（北京） | Method for simulating petroleum recovery by using cellulose nanocrystals |
| CN112646560B (en) * | 2020-12-24 | 2021-10-08 | 中国地质大学（北京） | Method for simulating petroleum recovery by using cellulose nanocrystals |
| CN112850715A (en) * | 2021-01-06 | 2021-05-28 | 江苏福瑞士电池科技有限公司 | Nitrogen-boron co-doped nano silicon-carbon powder material, preparation method and application thereof |
| CN113956862A (en) * | 2021-10-29 | 2022-01-21 | 中国石油大学(华东) | Guanidine gum fracturing fluid gel capable of reducing pH dependence, guanidine gum fracturing fluid system, and preparation method and application thereof |
| WO2023071333A1 (en) * | 2021-10-29 | 2023-05-04 | 中国石油大学华东 | Guanidine gum fracturing fluid gel capable of reducing ph dependence, guanidine gum fracturing fluid system and preparation method therefor and application thereof |
| EP4202007A4 (en) * | 2021-10-29 | 2024-03-13 | Univ China Petroleum East China | Guanidine gum fracturing fluid gel capable of reducing ph dependence, guanidine gum fracturing fluid system and preparation method therefor and application thereof |
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Application publication date: 20190802 |