CN108504346B - 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 PDFInfo
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- CN108504346B CN108504346B CN201810410231.8A CN201810410231A CN108504346B CN 108504346 B CN108504346 B CN 108504346B CN 201810410231 A CN201810410231 A CN 201810410231A CN 108504346 B CN108504346 B CN 108504346B
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- C09K8/62—Compositions for forming crevices or fractures
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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 first antifreeze clean fracturing fluid, the mass percent of each component and each component are as follows: 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.The mass percent of second of component for including and each component are as follows: 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 freezing point, improves low temperature resistant service performance while guaranteeing fracturing fluid property, so that remaining to use safely in the case where being lower than zero degree working environment.
Description
Technical field
The invention belongs to oilfield chemistry and fracturing yield increasing technical fields, in particular 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 technique
As Reservoir Development constantly carries out, oil and gas production is gradually decreased, and implementing hydraulic fracturing is to improve Oil & Gas Productivity
With the important well stimulation of oil recovery.Hydraulic fracturing refers to using ground high-tension apparatus, is infused by oil, gas well cylinder to stratum
Entering is more than the viscoelastic fluid (i.e. fracturing fluid) with certain prop-carrying capacity of formation absorption energy, when strata pressure is more than rupture pressure
The crack with certain flow conductivity will be generated when power, after removing geostatic pressure, sand grains branch entrained by fracturing fluid is cracked
Seam guarantees 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., wherein the performance of fracturing fluid
It is crucial.Fracturing fluid needs viscosity with higher that can effectively carry proppant, and after fracturing fluid reaches target zone, again
Needing it, rapid break to guarantee to return to the maximum extent is discharged to earth's surface 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 including natural plant and synthetic polymer.However,
Polymer solubility is poor, dissolution takes a long time, water-insoluble is more, and easily forms " flake ", greatly reduces the benefit of polymer
With rate.On the other hand, for polymer fracturing fluid, peroxide is added usually 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 pump injection pressure power required for earth's surface higher for the gellike, and is difficult to break glue completely behind entrance stratum,
Left residue can damage reservoir.
Clean fracturing fluid based on Surfactant Used in Viscoelastic Fracturing Fluids then can be avoided the above problem.For polymer,
The molecular weight of surfactant is extremely low, therefore dissolubility is preferable, will not generate 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 outer portion 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 freezing 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 will increase fracturing fluid with 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, time-consuming 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 being 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 freezing point, this problem could be solved from the root by developing low temperature resistant antifreeze fracturing fluid.
Summary of the invention
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 freezing point, improves low temperature resistant service performance while guaranteeing fracturing fluid property, so that being lower than zero degree
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 for the effect for giving full play to 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 first antifreeze clean fracturing fluid, the mass percent of each component and each component are as follows: 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- (cis- 22 carbon -13- enoic base propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, N-
(cis- 22 carbon -13- enoic base propyl)-N, N- dimethyl-N-hydroxysultaine, N- (cis- 22 carbon -
9- enoic base propyl)-N, at least one of N- dimethyl carboxylic acid glycine betaine, preferably N- (cis- 22 carbon -13- alkene
Sour amidopropyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine 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 preferred are as follows: 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, the mass percent of the component and each component that include are as follows: 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 Acid
Amidopropyl)-N, N- dimethyl-N-hydroxysultaine.
Above-mentioned second of antifreeze clean fracturing fluid, the mass percent of the component and each component that include are preferred are as follows: surface is living
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 both
Object, preferably sodium chloride or potassium chloride.
In antifreeze clean fracturing fluid of the present invention, the alcohol is in the binary or polynary alkylol of carbon atom number 2~5
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
Range is -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 freezing point of the present invention is lower than -40 DEG C, does not tie under most of extreme low temperature environment
Ice, and good fluidity can satisfy the construction requirement of extreme low temperature environment, provide 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 are wanted with meeting the construction of different temperatures range
It asks.
Detailed description of the invention
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 embodiment
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
17:295-301 ErucylAmidobetaines.J Surfact Deterg, the salt and alcohol are the purchase of market Reagent Company
It buys.
Embodiment 1
In the present embodiment, the formula of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon-
13- enoic base propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, stirring to N- (cis- 22 carbon -13- olefin(e) acid acyl
Aminocarbonyl propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, which is sufficiently 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 of test, 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 greater than 400mPas, and as the temperature rises, fracturing fluid viscosity gradually 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 of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon-
13- enoic base propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, stirring to N- (cis- 22 carbon -13- olefin(e) acid acyl
Aminocarbonyl propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, which is sufficiently 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 of test, 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 greater than 500mPas, but as the temperature rises, fracturing fluid viscosity gradually 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 of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon-
13- enoic base propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, stirring to N- (cis- 22 carbon -13- olefin(e) acid acyl
Aminocarbonyl propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, which is sufficiently 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 of test, 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 greater than 400mPas, but as the temperature rises, fracturing fluid viscosity gradually 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 of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon-
13- enoic base propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, stirring to N- (cis- 22 carbon -13- olefin(e) acid acyl
Aminocarbonyl propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, which is sufficiently 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 of test, 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 greater than 400mPas, but as the temperature rises, fracturing fluid viscosity gradually 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 of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon-
13- enoic base propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, stirring to N- (cis- 22 carbon -13- olefin(e) acid acyl
Aminocarbonyl propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, which is sufficiently 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 of test, 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 greater than 400mPas, but as the temperature rises, fracturing fluid viscosity gradually 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 of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon-
9- enoic base propyl)-N, N- dimethyl carboxylic acid glycine betaine, stirring to N- (Gadoleic Acid amide groups third
Base)-N, N- dimethyl carboxylic acid glycine betaine, which is sufficiently 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 of test, 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 the viscosity of fracturing fluid is greater than 400mPas, but as the temperature rises, pressure in initial temperature
Liquid viscosity is split to gradually 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 of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon-
9- enoic base propyl)-N, N- dimethyl carboxylic acid glycine betaine, stirring to N- (Gadoleic Acid amide groups third
Base)-N, N- dimethyl carboxylic acid glycine betaine, which is sufficiently 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 of test, 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 greater than 400mPas, but as the temperature rises, fracturing fluid viscosity gradually 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 of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and potassium chloride are added to the water at room temperature, add N- (cis- Linolenic Acid-
Enoic base propyl)-N, N- dimethyl-N-hydroxysultaine, stirring to N- (cis- Octadec-9-enoic Acid amide groups
Propyl)-N, N- dimethyl-N-hydroxysultaine, which is sufficiently 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 of test, 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 greater than 900mPas, but as the temperature rises, fracturing fluid viscosity gradually 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 of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- Linolenic Acid-
Enoic base propyl)-N, N- dimethyl-N-hydroxysultaine, stirring to N- (cis- Octadec-9-enoic Acid amide groups
Propyl)-N, N- dimethyl-N-hydroxysultaine, which is sufficiently 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 of test, 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 greater than 1000mPas, but as the temperature rises, fracturing fluid viscosity gradually 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 of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- Linolenic Acid-
Enoic base propyl)-N, N- dimethyl-N-hydroxysultaine, stirring to N- (cis- Octadec-9-enoic Acid amide groups
Propyl)-N, N- dimethyl-N-hydroxysultaine, which is sufficiently 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 of test, 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 greater than 900mPas, but as the temperature rises, fracturing fluid viscosity gradually 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 of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- Linolenic Acid-
Enoic base propyl)-N, N- dimethyl-N-hydroxysultaine, stirring to N- (cis- Octadec-9-enoic Acid amide groups
Propyl)-N, N- dimethyl-N-hydroxysultaine, which is sufficiently 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 of test, 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 greater than 900mPas, but as the temperature rises, fracturing fluid viscosity gradually 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 alcohol is added in the fracturing fluid into embodiment 1 at room temperature, and shakes, and discovery fracturing liquid ties up in 10s
Can rapid break, viscosity is substantially reduced.
It is carried out followed by rheological property of the rotational rheometer (Anto Paar, MCR 301) to system after addition n-octyl alcohol
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 alcohol is added in the fracturing fluid into embodiment 2 at room temperature, and shakes, and discovery fracturing liquid ties up in 10s
Can rapid break, viscosity is substantially reduced.
It is carried out followed by rheological property of the rotational rheometer (Anto Paar, MCR 301) to system after addition n-octyl alcohol
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 alcohol is added in the fracturing fluid into embodiment 3 at room temperature, and shakes, and discovery fracturing liquid ties up in 10s
Can rapid break, viscosity is substantially reduced.
It is carried out followed by rheological property of the rotational rheometer (Anto Paar, MCR 301) to system after addition n-octyl alcohol
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, 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 alcohol is added in the fracturing fluid into embodiment 7 at room temperature, and shakes, and discovery fracturing liquid ties up in 10s
Can rapid break, viscosity is substantially reduced.
It is carried out followed by rheological property of the rotational rheometer (Anto Paar, MCR 301) to system after addition n-octyl alcohol
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, shows just pungent
Alcohol makes original fracturing fluid system rapid break after being added.
Embodiment 16
In the present embodiment, the formula of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon-
13- enoic base propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, stirring to N- (cis- 22 carbon -13- olefin(e) acid acyl
Aminocarbonyl propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, which is sufficiently dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
It is measured according to People's Republic of China (PRC) petrochemical industry standard SH/T 0090-91, the solidification of the antifreeze fracturing fluid
Point is lower than -45 DEG C
Embodiment 17
In the present embodiment, the formula of the antifreeze clean fracturing fluid is as follows:
Preparation: the glycerine of formula ratio and sodium chloride are added to the water at room temperature, add N- (cis- 22 carbon-
9- enoic base propyl)-N, N- dimethyl carboxylic acid glycine betaine, stirring to N- (Gadoleic Acid amide groups third
Base)-N, N- dimethyl carboxylic acid glycine betaine, which is sufficiently dissolved and is uniformly mixed, obtains antifreeze fracturing fluid.
It is measured according to People's Republic of China (PRC) petrochemical industry standard SH/T 0090-91, the solidification of the antifreeze fracturing fluid
Point is lower than -45 DEG C.
Claims (4)
1. a kind of antifreeze clean fracturing fluid, it is characterised in that the mass percent of each component and each component are as follows: 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 N-
(cis- 22 carbon -13- enoic base propyl)-N, N- dimethyl-N-propyl sulfonic acid glycine betaine, N- (cis- 22 carbon -
13- enoic base propyl)-N, N- dimethyl-N-hydroxysultaine, N- (cis- 22 carbon -13- enoic base
Propyl)-N, at least one of N- dimethyl carboxylic acid glycine betaine；The salt is sodium chloride or potassium chloride；The alcohol is glycerine
Or ethylene glycol.
2. antifreeze clean fracturing fluid according to claim 1, it is characterised in that the hydrophobic tail chain is unsaturated 22 hydrocarbon
The zwitterionic surfactant of base chain is N- (cis- 22 carbon -13- enoic base propyl)-N, N- dimethyl-N-propyl
Sulphonic acid betaine or N- (cis- 22 carbon -13- enoic base propyl)-N, N- dimethyl carboxylic acid glycine betaine.
3. a kind of antifreeze clean fracturing fluid, it is characterised in that the mass percent of the component and each component that include are as follows: surface-active
Agent 9.0~15.0%, water soluble salt 3.0~15.0%, alcohol 33.0~52.0%, water 36.0~50.0%, the surface-active
Agent is N- (cis- Octadec-9-enoic Acid amidopropyl)-N, N- dimethyl-N-hydroxysultaine；The salt is chlorination
Sodium or potassium chloride；The alcohol is glycerine or ethylene glycol.
4. the preparation method of antifreeze clean fracturing fluid described in any claim in claims 1 to 3, it is characterised in that in room temperature
It is lower that water, alcohol, salt are mixed evenly by formula ratio, then be mixed and stirred for the surfactant of formula ratio to being completely dissolved.
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| CA3093615A CA3093615C (en) | 2018-05-02 | 2019-03-25 | Anti-freezing clear fracturing fluid and preparation method thereof |
| PCT/CN2019/079425 WO2019210750A1 (en) | 2018-05-02 | 2019-03-25 | Anti-freezing and cleaning fracturing fluid and preparation method therefor |
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| CN108504346B (en) * | 2018-05-02 | 2019-06-11 | 四川大学 | A kind of antifreeze clean fracturing fluid and preparation method thereof |
| CN110616067B (en) * | 2018-06-20 | 2022-06-07 | 中国石油化工股份有限公司 | Low-temperature-resistant clean polymer fracturing fluid crosslinking agent and preparation method thereof |
| CN110684520A (en) * | 2019-09-11 | 2020-01-14 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | Anti-freezing fracturing fluid and construction method thereof |
| CN110845372A (en) * | 2019-11-26 | 2020-02-28 | 陕西科技大学 | Multiolefin hook type surfactant gel fracturing fluid and preparation and gel breaking methods thereof |
| CN110938419A (en) * | 2019-12-09 | 2020-03-31 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | Low-freezing-point liquid recoverable clean fracturing fluid thickening agent and preparation method thereof |
| US20210380867A1 (en) * | 2020-06-08 | 2021-12-09 | Saudi Arabian Oil Company | Methods and compositions for downhole diversion of well treatment fluid |
| CN114195927B (en) * | 2020-09-18 | 2023-08-22 | 中国石油天然气集团有限公司 | Thickening agent, composition for forming thickening agent, emulsion polymer, fracturing fluid system and application of fracturing fluid system |
| CN112410015B (en) * | 2020-12-16 | 2022-07-19 | 陕西延长石油（集团）有限责任公司 | Low-temperature integrated clean fracturing fluid and preparation method thereof |
| US12071838B2 (en) | 2022-10-07 | 2024-08-27 | Saudi Arabian Oil Company | Viscoelastic surfactants for acid diversion in downhole operations |
| US11959017B1 (en) | 2022-10-07 | 2024-04-16 | Saudi Arabian Oil Company | Methods and materials for wellbore fluid diversion using visco-elastic surfactants |
| CN117164472A (en) * | 2023-08-16 | 2023-12-05 | 碳中能源科技(北京)有限公司 | Viscoelastic amphoteric surfactant and high-temperature-resistant fracturing fluid prepared from viscoelastic amphoteric surfactant |
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| US6605570B2 (en) * | 2001-03-01 | 2003-08-12 | Schlumberger Technology Corporation | Compositions and methods to control fluid loss in surfactant-based wellbore service fluids |
| CN101812290A (en) * | 2010-05-11 | 2010-08-25 | 陕西科技大学 | Acid clean fracturing fluid and preparation method thereof |
| CN102093874B (en) * | 2010-12-28 | 2012-11-07 | 中国石油大学(华东) | Anion type nano compound clean fracturing fluid and preparation method thereof |
| CN102277152B (en) * | 2011-05-16 | 2013-03-13 | 陕西科技大学 | Acid-triggered thickening agent and preparation method thereof |
| CN102559166B (en) * | 2011-12-28 | 2014-01-15 | 中国石油天然气股份有限公司 | Amphoteric surfactant fracturing fluid and preparation method thereof |
| CN103305205B (en) * | 2012-03-09 | 2016-04-06 | 中国石油天然气股份有限公司 | Preparation method of polyhydroxy alcohol fracturing fluid crosslinking agent |
| CN102851017A (en) * | 2012-08-16 | 2013-01-02 | 四川西普化工股份有限公司 | Viscous-elastic clean fracturing fluid containing erucic acid betaines |
| US10759990B2 (en) * | 2014-01-16 | 2020-09-01 | Wilmar Trading Pte Ltd. | Use of olefinic ester compositions in oil and gas fields |
| CN103773354A (en) * | 2014-02-21 | 2014-05-07 | 亿城淄博石油陶粒制造有限公司 | Thickening agent applicable to surfactant fracturing liquid and online cross-linking factory operation method |
| US9624418B2 (en) * | 2014-04-15 | 2017-04-18 | Baker Hughes Incorporated | Antifreeze proteins for use in downhole fluids |
| CN104073235A (en) * | 2014-06-19 | 2014-10-01 | 西安石油大学 | Long-carbon-chain amide glycine betaine clean fracturing fluid and preparation method thereof |
| CN108504346B (en) * | 2018-05-02 | 2019-06-11 | 四川大学 | A kind of antifreeze clean fracturing fluid and preparation method thereof |
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