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CN108504346A - A kind of antifreeze clean fracturing fluid and preparation method thereof - Google Patents

A kind of antifreeze clean fracturing fluid and preparation method thereof Download PDF

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Publication number
CN108504346A
CN108504346A CN201810410231.8A CN201810410231A CN108504346A CN 108504346 A CN108504346 A CN 108504346A CN 201810410231 A CN201810410231 A CN 201810410231A CN 108504346 A CN108504346 A CN 108504346A
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fracturing fluid
antifreeze
surfactant
clean fracturing
water
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CN108504346B (en
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殷鸿尧
冯玉军
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Sichuan University
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Sichuan University
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Priority to CA3093615A priority patent/CA3093615C/en
Priority to PCT/CN2019/079425 priority patent/WO2019210750A1/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/62Compositions for forming crevices or fractures
    • C09K8/66Compositions based on water or polar solvents
    • C09K8/68Compositions based on water or polar solvents containing organic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/602Compositions for stimulating production by acting on the underground formation containing surfactants
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/62Compositions for forming crevices or fractures
    • C09K8/66Compositions based on water or polar solvents
    • C09K8/665Compositions based on water or polar solvents containing inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2208/00Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/26Gel breakers other than bacteria or enzymes

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Abstract

Antifreeze clean fracturing fluid of the present invention, including component and each component mass percent it is as follows:Surfactant 2.0~15.0%, water soluble salt 1.0~20.0%, alcohol 28.0~55.0%, water 36.0~55.0%.According to the difference of selected surfactant, clean fracturing fluid of the present invention is divided into two kinds.The mass percent of the first antifreeze clean fracturing fluid, each component and each component is:Surfactant 2.0~5.0%, water soluble salt 2.0~20.0%, alcohol 28.0~55.0%, water 38.0~55.0%, the surfactant are at least one of the zwitterionic surfactant that hydrophobic tail chain is unsaturated 22 carbon hydrocarbyl chains.Second of component for including and the mass percent of each component are:Surfactant 9.0~15.0%, water soluble salt 3.0~15.0%, alcohol 33.0~52.0%, water 36.0~50.0%, the surfactant are at least one of the zwitterionic surfactant that hydrophobic tail chain is unsaturated 18 carbon hydrocarbyl chains.The present invention reduces fracturing fluid solidification point, improves low temperature resistant performance so that remain to use safely under less than zero degree working environment while ensureing fracturing fluid property.

Description

A kind of antifreeze clean fracturing fluid and preparation method thereof
Technical field
The invention belongs to oilfield chemistry and fracturing yield increasing technical fields, more particularly to a kind of to be suitable for severe cold area oil-gas reservoir The low temperature resistant antifreeze clean fracturing liquid system of exploitation.
Background technology
As Reservoir Development constantly carries out, oil and gas production continuously decreases, and it is to improve Oil & Gas Productivity to implement hydraulic fracturing With the important well stimulation of oil recovery.Hydraulic fracturing refers to utilizing ground high-tension apparatus, is noted to stratum by oil, gas well cylinder It is more than the viscoelastic fluid (i.e. fracturing fluid) with certain prop-carrying capacity of formation absorption energy to enter, when strata pressure is more than that rupture is pressed It just will produce the crack with certain flow conductivity when power, after removing geostatic pressure, the sand grains branch entrained by fracturing fluid cracks Seam ensures oil, flow of air channel, to realize well production increment purpose.
The effect of pressing crack construction depends on Multiple factors, such as geostatic pressure, ground environment etc., the wherein performance of fracturing fluid It is crucial.Fracturing fluid needs that there is higher viscosity can effectively carry proppant, and after fracturing fluid reaches target zone, again Needing it, rapid break is discharged to earth's surface to ensure to return to the maximum extent within a certain period of time, to reduce the injury to reservoir.Base It is that current domestic and international application obtains most commonly used system in the fracturing fluid for including natural plant and synthetic polymer.However, Polymer solubility is poor, dissolving takes compared with long, water-insoluble is more, and easily forms " flake ", greatly reduces the profit of polymer With rate.On the other hand, for polymer fracturing fluid, peroxide is added typically in fracturing fluid as gel breaker.Work as pressure break After liquid reaches the stratum of certain depth, under the action of high temperature and peroxide, polymer molecular chain is gradually broken, and is caused quickly Broken glue.However in the case where well depth is shallower, well temperature is usually relatively low, and gel breaking time is longer or is difficult to brokenly glue, it is easy to make At fracturing fluid recovery (backflow) difficulty.Such case can cause reservoir greatly to injure, and volume increase purpose not only be not achieved, it is also possible to reduce Production capacity.In addition, the fracturing fluid of polymer especially natural polymer usually requires to be cross-linked to form gel before being pumped into, it is good to ensure Good solid-carrying performance, but the gellike is higher in the required pump injection pressure power of earth's surface, and be difficult to break glue completely after entering stratum, Left residue can damage reservoir.
Clean fracturing fluid based on Surfactant Used in Viscoelastic Fracturing Fluids can then avoid the above problem.For polymer, The molecular weight of surfactant is extremely low, therefore dissolubility is preferable, not will produce water-insoluble, and surfactant fracturing fluid encounters Glue can be broken after oil or gas in stratum automatically, viscosity is caused to drastically reduce, stratum will not be damaged.Therefore, it sticks in recent years The research of elastic surface activating agent clean fracturing fluid is more and more.
The hydraulic fracturing construction of winter severe cold area has become the thorny problem in domestic and international part oil field.These regional winters Temperature is generally at 0 DEG C hereinafter, even as low as -30 DEG C.And conventional fracturing fluid system, either clean fracturing fluid or polymer Fracturing fluid, main component are all water, although imparting the preferable viscoelasticity of fracturing fluid, this also results in its solidification point (knot The temperature of ice) it is higher, in the difficulty that low temperature environment can not construct by icing.Fracturing fluid not only be easy to cause frozen block after freezing, Increase construction risk coefficient, but also can increase fracturing fluid match liquid " Fu Zuoliang ", waste a large amount of fracturing fluid.Such as it is located at China Soviet Union's Sulige gas field temperature in winter of Sulige area is usually less than -10 DEG C, and large-scale fractured horizontal well needs a large amount of pressure Liquid is split, is taken long with liquid, fracturing fluid, which can freeze, blocks valve, causes construction that can not carry out.Solve fracturing fluid ice formation issues, one It is to add insulating layer to flow container, wraps up thick and heavy coldproof material, such as rock wool, mineral wool, polyurethane foam tile fragment, but this method Insulation effect in short-term can be only played, tolerance to cold is limited.Second is that heated to fracturing fluid, but time-consuming for this method, and consume Energy is big, can not be applied on a large scale.Above two method is all difficult to solve the problems, such as the pressing crack construction of severe cold area oil gas field, only greatly Amplitude reduction fracturing fluid solidification point, this problem could be solved from the root cause by developing low temperature resistant antifreeze fracturing fluid.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of antifreeze clean fracturing fluid and its preparation side Method reduces fracturing fluid solidification point, improves low temperature resistant performance so that less than zero degree while ensureing fracturing fluid property It remains to use safely under working environment.
Antifreeze clean fracturing fluid of the present invention, including component and each component mass percent it is as follows:
Surfactant 2.0~15.0%, water soluble salt 1.0~20.0%, alcohol 28.0~55.0%, water 36.0~ 55.0%.
It is more preferable to obtain using effect to give full play to the effect of each component according to the difference of selected surfactant Fracturing fluid, clean fracturing fluid of the present invention is divided into two kinds, both fracturing fluids belong to same inventive concept.
The mass percent of the first antifreeze clean fracturing fluid, each component and each component is:Surfactant 2.0~ 5.0%, water soluble salt 2.0~20.0%, alcohol 28.0~55.0%, water 38.0~55.0%, the surfactant is hydrophobic Tail chain is at least one of the zwitterionic surfactant of unsaturated 22 carbon hydrocarbyl chains.
The first above-mentioned antifreeze clean fracturing fluid, the hydrophobic tail chain are the amphoteric ion of unsaturated 22 carbon hydrocarbyl chains Surfactant is N- (Gadoleic Acid amidopropyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, N- (Gadoleic Acid amidopropyl)-N, N- dimethyl-N -s hydroxysultaine, N- (cis- 22 carbon- 9- enoic bases propyl)-N, at least one of N- dimethyl carboxylic acid glycine betaines, preferably N- (cis- 22 carbon -9- alkene Sour amidopropyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaines or N- (Gadoleic Acid amidopropyl)- N, N- dimethyl carboxylic acid glycine betaine.
The mass percent of the first above-mentioned antifreeze clean fracturing fluid, each component and each component is preferably:Surfactant 2.0~4.0%, water soluble salt 2.5~15.0%, alcohol 29.0~53.0%, water 39.0~54.0%.
Second of antifreeze clean fracturing fluid, including component and the mass percent of each component be:Surfactant 9.0~ 15.0%, water soluble salt 3.0~15.0%, alcohol 33.0~52.0%, water 36.0~50.0%, the surfactant is hydrophobic Tail chain is at least one of the zwitterionic surfactant of unsaturated 18 carbon hydrocarbyl chains.
Above-mentioned second of antifreeze clean fracturing fluid, the zwitterionic surfactant are N- (cis- Octadec-9-enoic Acids Amidopropyl)-N, N- dimethyl-N-hydroxysultaines.
Above-mentioned second of antifreeze clean fracturing fluid, including component and the mass percent of each component be preferably:It lives on surface Property agent 10.0~12.0%, water soluble salt 3.0~14.0%, alcohol 34.0~39.0%, water 41.0~46.0%.
In antifreeze clean fracturing fluid of the present invention, the salt is the mixing of water-soluble inorganic salt or organic salt or the two Object, preferably sodium chloride or potassium chloride.
In antifreeze clean fracturing fluid of the present invention, the alcohol is in the binary of carbon atom number 2~5 or polynary alkylol At least one, preferably glycerine.
The present invention provides the preparation method of above-mentioned antifreeze clean fracturing fluid, at room temperature mixes water, alcohol, salt by formula ratio It stirs evenly, then is mixed and stirred for the surfactant of formula ratio to being completely dissolved.
Antifreeze clean fracturing fluid of the present invention, the first temperature limit are -40~90 DEG C, and second using temperature Ranging from -40~50 DEG C, wherein surfactant selected in second of fracturing fluid is oleic acid by preparing used raw material, Oleic acid is cheap and easy to get, therefore cost is relatively low.
1, antifreeze clean fracturing fluid solidification point of the present invention is less than -40 DEG C, is not tied under most of extreme low temperature environment Ice, and good fluidity disclosure satisfy that the construction requirement of extreme low temperature environment, be provided for the fracturing yield increasing construction under low temperature environment A kind of novel antifreeze clean fracturing fluid.
2, antifreeze clean fracturing fluid composition of the present invention is simple, and preparation process is simple, can be mass-produced and uses.
3, antifreeze clean fracturing fluid of the present invention is free of any polymer, meet oil can rapid break, and without residue, over the ground Layer injury is small.
4, the used surfactant of antifreeze clean fracturing fluid of the present invention contains unsaturated double-bond and amphoteric ion head base, It is degradable, therefore there is environment friendly.
5, in the formula of antifreeze clean fracturing fluid of the present invention, type and content, the type of salt of change alcohol can be passed through And content and surface-active contents, adjusting of the realization to fracturing fluid rheological property, the construction to meet different temperatures range are wanted It asks.
Description of the drawings
Fig. 1 is that fracturing liquid ties up to 170s in embodiment 1-1Under viscosity and temperature and time and relational graph.
Fig. 2 is that fracturing liquid ties up to 170s in embodiment 2-1Under viscosity and temperature and time and relational graph.
Fig. 3 is that fracturing liquid ties up to 170s in embodiment 3-1Under viscosity and temperature and time and relational graph.
Fig. 4 is that fracturing liquid ties up to 170s in embodiment 4-1Under viscosity and temperature and time and relational graph.
Fig. 5 is that fracturing liquid ties up to 170s in embodiment 5-1Under viscosity and temperature and time and relational graph.
Fig. 6 is that fracturing liquid ties up to 170s in embodiment 6-1Under viscosity and temperature and time and relational graph.
Fig. 7 is that fracturing liquid ties up to 170s in embodiment 7-1Under viscosity and temperature and time and relational graph.
Fig. 8 is that fracturing liquid ties up to 170s in embodiment 8-1Under viscosity and temperature and time and relational graph.
Fig. 9 is that fracturing liquid ties up to 170s in embodiment 9-1Under viscosity and temperature and time and relational graph.
Figure 10 is that fracturing liquid ties up to 170s in embodiment 10-1Under viscosity and temperature and time and relational graph.
Figure 11 is that fracturing liquid ties up to 170s in embodiment 11-1Under viscosity and temperature and time and relational graph.
Figure 12 is 170s when fracturing liquid ties up to 90 DEG C in embodiment 12-1Lower viscosity and time and relational graph.
Figure 13 is 170s when fracturing liquid ties up to 90 DEG C in embodiment 13-1Lower viscosity and time and relational graph.
Figure 14 is 170s when fracturing liquid ties up to 90 DEG C in embodiment 14-1Lower viscosity and time and relational graph.
Figure 15 is 170s when fracturing liquid ties up to 90 DEG C in embodiment 15-1Lower viscosity and time and relational graph.
Specific implementation mode
Antifreeze clean fracturing fluid of the present invention and preparation method thereof is described further below by embodiment.
In following embodiment, surfactant used is laboratory self-control, preparation method referring to Wang Y, Zhang Y, Liu X,Wang J,Wei L,Feng Y(2014)Effect of a Hydrophilic Head Group on Krafft Temperature,Surface Activities and Rheological Behaviors of ErucylAmidobetaines.J Surfact Deterg 17:295-301, the salt and alcohol are the purchase of market Reagent Company It buys.
Embodiment 1
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon- 9- enoic bases propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaines, stirring to N- (Gadoleic Acid amides Base propyl)-N, N- dimethyl-N-propyl sulfonic acids glycine betaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 90 DEG C, then constant temperature shears 60min, and test result is shown in Fig. 1.As shown in Figure 1, in initial temperature When, the viscosity of fracturing fluid is more than 400mPas, and with the raising of temperature, fracturing fluid viscosity continuously decreases.When being warming up to 90 DEG C Afterwards, system viscosity is about 50mPas, and after continuing shearing one hour, system viscosity stablization shows the present embodiment in 38mPas Gained fracturing fluid meets clean fracturing fluid requirement, while having excellent resistance to low temperature.
Embodiment 2
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon- 9- enoic bases propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaines, stirring to N- (Gadoleic Acid amides Base propyl)-N, N- dimethyl-N-propyl sulfonic acids glycine betaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 90 DEG C, then constant temperature shears 60min, and test result is shown in Fig. 2.As shown in Figure 2, in initial temperature When, the viscosity of fracturing fluid is more than 500mPas, but with the raising of temperature, fracturing fluid viscosity continuously decreases.When being warming up to 90 DEG C Afterwards, system viscosity drop is down to 32mPas, and after continuing shearing one hour, system viscosity stablization shows this implementation in 24mPas Example gained fracturing fluid meets clean fracturing fluid requirement, while having excellent resistance to low temperature.
Embodiment 3
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon- 9- enoic bases propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaines, stirring to N- (Gadoleic Acid amides Base propyl)-N, N- dimethyl-N-propyl sulfonic acids glycine betaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 90 DEG C, then constant temperature shears 60min, and test result is shown in Fig. 3.From the figure 3, it may be seen that in initial temperature When, the viscosity of fracturing fluid is more than 400mPas, but with the raising of temperature, fracturing fluid viscosity continuously decreases.When being warming up to 90 DEG C Afterwards, system viscosity is about 58mPas, and after continuing shearing one hour, system viscosity stablization shows the present embodiment in 43mPas Gained fracturing fluid meets clean fracturing fluid requirement, while having excellent resistance to low temperature.
Embodiment 4
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon- 9- enoic bases propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaines, stirring to N- (Gadoleic Acid amides Base propyl)-N, N- dimethyl-N-propyl sulfonic acids glycine betaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 90 DEG C, then constant temperature shears 60min, and test result is shown in Fig. 4.As shown in Figure 4, in initial temperature When, the viscosity of fracturing fluid is more than 400mPas, but with the raising of temperature, fracturing fluid viscosity continuously decreases.When being warming up to 90 DEG C Afterwards, system viscosity drop is down to 50mPas, and after continuing shearing 1 hour, system viscosity stablization shows the present embodiment in 70mPas Gained fracturing fluid meets clean fracturing fluid requirement, while having excellent resistance to low temperature.
Embodiment 5
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon- 9- enoic bases propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaines, stirring to N- (Gadoleic Acid amides Base propyl)-N, N- dimethyl-N-propyl sulfonic acids glycine betaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 90 DEG C, then constant temperature shears 60min, and test result is shown in Fig. 5.As shown in Figure 5, in initial temperature When, the viscosity of fracturing fluid is more than 400mPas, but with the raising of temperature, fracturing fluid viscosity continuously decreases.When being warming up to 90 DEG C Afterwards, system viscosity drop is down to 220mPas, and after continuing shearing 1 hour, system viscosity stablization shows this implementation in 195mPas Example gained fracturing fluid meets clean fracturing fluid requirement, while having excellent resistance to low temperature.
Embodiment 6
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon- 9- enoic bases propyl)-N, N- dimethyl carboxylic acid glycine betaines, stirring to N- (Gadoleic Acid amide groups third Base)-N, N- dimethyl carboxylic acid glycine betaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 90 DEG C, then constant temperature shears 60min, and test result is shown in Fig. 6.
It will be appreciated from fig. 6 that in initial temperature, the viscosity of fracturing fluid is more than 400mPas, but with the raising of temperature, pressure Liquid viscosity is split to continuously decrease.After being warming up to 90 DEG C, system viscosity drop continues after shearing 1 hour, system down to 220mPas Viscosity stablization shows that fracturing fluid obtained by the present embodiment meets clean fracturing fluid requirement in 195mPas, while having excellent resistance to Cryogenic property.
Embodiment 7
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon- 9- enoic bases propyl)-N, N- dimethyl carboxylic acid glycine betaines, stirring to N- (Gadoleic Acid amide groups third Base)-N, N- dimethyl carboxylic acid glycine betaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 90 DEG C, then constant temperature shears 60min, and test result is shown in Fig. 7.As shown in Figure 7, in initial temperature When, the viscosity of fracturing fluid is more than 400mPas, but with the raising of temperature, fracturing fluid viscosity continuously decreases.When being warming up to 90 DEG C Afterwards, system viscosity drop is down to 68mPas, and after continuing shearing one hour, system viscosity stablization shows this implementation in 73mPas Example gained fracturing fluid meets clean fracturing fluid requirement, while having excellent resistance to low temperature.
Embodiment 8
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and potassium chloride are added to the water at room temperature, add N- (cis- Linolenic Acids- Enoic base propyl)-N, N- dimethyl-N-hydroxysultaines, stirring to N- (cis- Octadec-9-enoic Acid amide groups Propyl)-N, N- dimethyl-N -s hydroxysultaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 50 DEG C, then constant temperature shears 60min, and test result is shown in Fig. 8.As shown in Figure 8, in initial temperature When, the viscosity of fracturing fluid is more than 900mPas, but with the raising of temperature, fracturing fluid viscosity continuously decreases.When being warming up to 50 DEG C Afterwards, system viscosity drop is down to 56mPas, and after continuing shearing 1 hour, system viscosity stablization shows the present embodiment in 35mPas Gained fracturing fluid meets clean fracturing fluid requirement, while having excellent resistance to low temperature.
Embodiment 9
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- Linolenic Acids- Enoic base propyl)-N, N- dimethyl-N-hydroxysultaines, stirring to N- (cis- Octadec-9-enoic Acid amide groups Propyl)-N, N- dimethyl-N -s hydroxysultaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 50 DEG C, then constant temperature shears 60min, and test result is shown in Fig. 9.As shown in Figure 9, in initial temperature When, the viscosity of fracturing fluid is more than 1000mPas, but with the raising of temperature, fracturing fluid viscosity continuously decreases.When being warming up to 50 After DEG C, system viscosity drop is down to 53mPas, and after continuing shearing one hour, system viscosity stablization shows this reality in 42mPas It applies fracturing fluid obtained by example and meets clean fracturing fluid requirement, while there is excellent resistance to low temperature.
Embodiment 10
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- Linolenic Acids- Enoic base propyl)-N, N- dimethyl-N-hydroxysultaines, stirring to N- (cis- Octadec-9-enoic Acid amide groups Propyl)-N, N- dimethyl-N -s hydroxysultaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 50 DEG C, then constant temperature shears 60min, and test result is shown in Figure 10.As shown in Figure 10, in initial temperature When, the viscosity of fracturing fluid is more than 900mPas, but with the raising of temperature, fracturing fluid viscosity continuously decreases.When being warming up to 50 DEG C Afterwards, system viscosity drop is down to 62mPas, and after continuing shearing 1 hour, system viscosity stablization shows the present embodiment in 45mPas Gained fracturing fluid meets clean fracturing fluid requirement, while having excellent resistance to low temperature.
Embodiment 11
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- Linolenic Acids- Enoic base propyl)-N, N- dimethyl-N-hydroxysultaines, stirring to N- (cis- Octadec-9-enoic Acid amide groups Propyl)-N, N- dimethyl-N -s hydroxysultaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
The rheological property of configured solution is tested using rotational rheometer (Anto Paar, MCR 301).It is cutting Cutting speed rate is 170s-1Lower mini-frac liquid viscosity is with temperature, the variation relation of time.- 25 DEG C of initial temperature is tested, with 3 DEG C min-1Heating rate be warming up to 50 DEG C, then constant temperature shears 60min, and test result is shown in Figure 11.As shown in Figure 11, in initial temperature When, the viscosity of fracturing fluid is more than 900mPas, but with the raising of temperature, fracturing fluid viscosity continuously decreases.When being warming up to 50 DEG C Afterwards, system viscosity drop is down to 102mPas, and after continuing shearing 1 hour, system viscosity stablization shows this implementation in 75mPas Example gained fracturing fluid meets clean fracturing fluid requirement, while having excellent resistance to low temperature.
The gel breaking test of antifreeze clean fracturing fluid during the following examples illustrate the invention and evaluation.
Embodiment 12
1mL n-octyl alcohols are added in the fracturing fluid into embodiment 1 at room temperature, and shake, it is found that fracturing liquid ties up in 10s Can rapid break, viscosity is substantially reduced.
The rheological property of system after addition n-octyl alcohol is carried out followed by rotational rheometer (Anto Paar, MCR 301) Test.At 90 DEG C with 170s-1Rate shear 35min, test result is shown in Figure 12.As seen from the figure, after n-octyl alcohol being added, system Viscosity is greatly lowered, only 3mPas or so, and as the increase of shear time does not change significantly, shows n-octyl alcohol Make original fracturing fluid system rapid break after addition.
Embodiment 13
1mL n-octyl alcohols are added in the fracturing fluid into embodiment 2 at room temperature, and shake, it is found that fracturing liquid ties up in 10s Can rapid break, viscosity is substantially reduced.
The rheological property of system after addition n-octyl alcohol is carried out followed by rotational rheometer (Anto Paar, MCR 301) Test.At 90 DEG C with 170s-1Rate shear 35min, test result is shown in Figure 13.As seen from the figure, after n-octyl alcohol being added, system Viscosity is greatly lowered, only 3mPas or so, and as the increase of shear time does not change significantly, shows n-octyl alcohol Make original fracturing fluid system rapid break after addition.
Embodiment 14
1mL n-octyl alcohols are added in the fracturing fluid into embodiment 3 at room temperature, and shake, it is found that fracturing liquid ties up in 10s Can rapid break, viscosity is substantially reduced.
The rheological property of system after addition n-octyl alcohol is carried out followed by rotational rheometer (Anto Paar, MCR 301) Test.At 90 DEG C with 170s-1Rate shear 35min, test result is shown in Figure 14.As seen from the figure, after n-octyl alcohol being added, system Viscosity is greatly lowered, only 3.8mPas or so, and as the increase of shear time does not change significantly, and shows just pungent Alcohol makes original fracturing fluid system rapid break after being added.
Following embodiment verifies the freezing point of the antifreeze clean fracturing fluid down to -40 DEG C
Embodiment 15
1mL n-octyl alcohols are added in the fracturing fluid into embodiment 7 at room temperature, and shake, it is found that fracturing liquid ties up in 10s Can rapid break, viscosity is substantially reduced.
The rheological property of system after addition n-octyl alcohol is carried out followed by rotational rheometer (Anto Paar, MCR 301) Test.At 90 DEG C with 170s-1Rate shear 35min, test result is shown in Figure 15.As seen from the figure, after n-octyl alcohol being added, system Viscosity is greatly lowered, only 2.2mPas or so, and as the increase of shear time does not change significantly, and shows just pungent Alcohol makes original fracturing fluid system rapid break after being added.
Embodiment 16
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon- 9- enoic bases propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaines, stirring to N- (Gadoleic Acid amides Base propyl)-N, N- dimethyl-N-propyl sulfonic acids glycine betaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
It is measured according to People's Republic of China (PRC) petroleum chemical industry standard SH/T 0090-91, the solidification of the antifreeze fracturing fluid Point is less than -45 DEG C
Embodiment 17
In the present embodiment, the formula such as following table of the antifreeze clean fracturing fluid:
It prepares:The glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon- 9- enoic bases propyl)-N, N- dimethyl carboxylic acid glycine betaines, stirring to N- (Gadoleic Acid amide groups third Base)-N, N- dimethyl carboxylic acid glycine betaine, which is fully dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
It is measured according to People's Republic of China (PRC) petroleum chemical industry standard SH/T 0090-91, the solidification of the antifreeze fracturing fluid Point is less than -45 DEG C.

Claims (10)

1. a kind of antifreeze clean fracturing fluid, it is characterised in that including component and each component mass percent it is as follows:
Surfactant 2.0~15.0%, water soluble salt 1.0~20.0%, alcohol 28.0~55.0%, water 36.0~55.0%.
2. antifreeze clean fracturing fluid according to claim 1, it is characterised in that the mass percent of each component and each component is: Surfactant 2.0~5.0%, water soluble salt 2.0~20.0%, alcohol 28.0~55.0%, water 38.0~55.0%, the table Face activating agent is at least one of the zwitterionic surfactant that hydrophobic tail chain is unsaturated 22 carbon hydrocarbyl chains.
3. antifreeze clean fracturing fluid according to claim 2, it is characterised in that the hydrophobic tail chain is unsaturated 22 carbon The zwitterionic surfactant of hydrocarbyl chain is N- (Gadoleic Acid amidopropyl)-N, N- dimethyl-N -s third Base sulphonic acid betaine, N- (Gadoleic Acid amidopropyl)-N, N- dimethyl-N -s hydroxysultaine, At least one of N- (Gadoleic Acid amidopropyl)-N, N- dimethyl carboxylic acid glycine betaine.
4. antifreeze clean fracturing fluid according to claim 3, it is characterised in that the hydrophobic tail chain is unsaturated 22 hydrocarbon The zwitterionic surfactant of base chain is N- (Gadoleic Acid amidopropyl)-N, N- dimethyl-N-propyl Sulphonic acid betaine or N- (Gadoleic Acid amidopropyl)-N, N- dimethyl carboxylic acid glycine betaine.
5. antifreeze clean fracturing fluid according to claim 1, it is characterised in that the quality percentage of the component and each component that include Than for:Surfactant 9.0~15.0%, water soluble salt 3.0~15.0%, alcohol 33.0~52.0%, water 36.0~50.0%, The surfactant is at least one of the zwitterionic surfactant that hydrophobic tail chain is unsaturated 18 carbon hydrocarbyl chains.
6. antifreeze clean fracturing fluid according to claim 5, it is characterised in that the zwitterionic surfactant is N- (cis- Octadec-9-enoic Acid amidopropyl)-N, N- dimethyl-N-hydroxysultaines.
7. according to antifreeze clean fracturing fluid described in any claim in claim 1-6, it is characterised in that the salt is water-soluble The mixture of property inorganic salts or organic salt or the two.
8. according to antifreeze clean fracturing fluid described in any claim in claim 1-6, it is characterised in that the alcohol is that carbon is former At least one of the binary of subnumber 2~5 or polynary alkylol.
9. antifreeze clean fracturing fluid according to claim 8, it is characterised in that the polyalcohol is glycerine.
10. the preparation method of antifreeze clean fracturing fluid described in any claim in claims 1 to 3, it is characterised in that in room Water, alcohol, salt are mixed evenly by formula ratio under temperature, then are mixed and stirred for completely molten with the surfactant of formula ratio Solution.
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