CN106883834A - A kind of fracturing fluid for shale gas pressure break and preparation method thereof - Google Patents
A kind of fracturing fluid for shale gas pressure break and preparation method thereof Download PDFInfo
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
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Abstract
The invention discloses a kind of fracturing fluid for shale gas pressure break and preparation method thereof, belong to shale gas exploitation technical field.Counted with the quality of fracturing fluid as 100%, fracturing fluid includes the component of following mass percent：Crosslinking agent, 0.3~2.0%；Gelling agent, 0.5~2.0%；PH adjusting agent, 1.0~2.5%；Reinforcing agent, 3.0~8.5%；Gel breaker, 0.2~1.5%；Low-carbon alkanes, surplus；Crosslinking agent is the mixture of ferric sulfate, ethylene glycol and monoethanolamine；Gelling agent is the product with phosphorus pentoxide, triethyl phosphate and mixed alcohol as raw material, counted with the gross mass of phosphorus pentoxide, triethyl phosphate and mixed alcohol as 100%, the mass percent of the phosphorus pentoxide is 25.1%~32.8%, the mass percent of the mixed alcohol is 41.3%~45.9%, and the mass percent of triethyl phosphate is 21.3%~33.6%；Mixed alcohol is the mixture of hexanol, amylalcohol, octanol and decyl alcohol；Low-carbon alkanes are at least one in methane, propane and butane.The fracturing fluid heat resistance can reach more than 135 DEG C, and crosslinking time is adjustable, and the easily row of returning.
Description
Technical field
The present invention relates to shale gas exploitation technical field, more particularly to a kind of fracturing fluid for shale gas pressure break
And preparation method thereof.
Background technology
Shale gas are natural gas of the preservation in rammell, belong to Unconventional gas, are entered by fracturing process
Row exploitation.The fracturing fluid commonly used in pressing crack construction mainly includes aqueous fracturing fluid and oil base fracturing fluid.But by
Belong to compact reservoir in shale gas reservoir, it is necessary to carry out pressure break using big liquid measure, huge discharge volume fracturing pattern.
The waste of water resource, and aqueous fracturing fluid can be caused to be also easy to damage reservoir using aqueous fracturing fluid.
And can effectively solve above-mentioned water resource waste and to storage using the lower carbon number hydrocarbons oil base fracturing fluid that lower carbon number hydrocarbons substitutes water
The problem that layer is damaged.
The formula of current lower carbon number hydrocarbons fracturing fluid has a lot, and such as US7341103B2 discloses a kind of liquefied petroleum
Air pressure splits formula of liquid, is made up of liquefied petroleum gas, alkyl phosphate iron Polyvalent metal complexes.
US8408289B2 discloses a kind of liquified petroleum gas fracturing formula of liquid, by liquefied petroleum gas, alkyl phosphate
Iron Polyvalent metal complexes are constituted.US2002/0165101A1 discloses a kind of liquified petroleum gas fracturing formula of liquid,
By alkene, diesel oil, kerosene, fuel oil, diesel oil, petroleum distillate, phosphate iron multivalent metal salt and broken glue
Agent is constituted.Chinese patent literature CN101395340A discloses a kind of liquified petroleum gas fracturing system, the liquid
Liquefied oil gas fracturing fluid is made up of propane, butane or propane and butane mixture, gelling agent and aluminum sulfate.In
State patent document CN104232072A discloses a kind of liquid phosphoric acid ester waterless fracturing fluid, the anhydrous fracturing fluid by
Pentane, phosphate, sodium metaaluminate are constituted.Chinese patent literature CN104371694A discloses a kind of nothing
Water phase fracturing fluid system, anhydrous phase fracturing fluid system is by propane, iso-butane or n-hexane, alkyl phosphate aluminium
Constitute.Chinese patent literature CN103468236A discloses a kind of fracturing fluid containing butane, fracturing liquid
System is made up of butane, phosphate and crosslinking agent.Chinese patent literature CN104004506A discloses a kind of suitable
Close the anhydrous fracturing fluid of unconventional reservoir pressure break, the fracturing fluid system by alkyl hydro carbons, dialkyl phosphate iron,
Organic complex and sulfamic acid or DBSA containing trivalent metal ion are constituted.
Realize it is of the invention during, the inventors discovered that at least there is problems with the prior art：It is existing
Some lower carbon number hydrocarbons fracturing fluid heat resistances are less than 130 DEG C, and the deeper shale gas reservoir temperature of buried depth generally exists
More than 130 DEG C, therefore existing lower carbon number hydrocarbons fracturing fluid is not suitable for the exploitation of deep layer shale gas.And it is existing
Lower carbon number hydrocarbons fracturing fluid crosslinking time is uncontrollable, and site operation frictional resistance is high.Additionally, existing lower carbon number hydrocarbons fracturing fluid
It is not easy the row of returning after into reservoir.
The content of the invention
In order to solve above-mentioned technical problem, when present invention offer one kind can be resistant to 130 DEG C of high temperature above, crosslinking
Between controllable and the easily row of returning the fracturing fluid for shale gas pressure break and preparation method thereof.
First aspect present invention provides a kind of fracturing fluid for shale gas pressure break, with the quality of the fracturing fluid
It is 100% meter, the fracturing fluid includes the component of following mass percent：
Crosslinking agent, 0.3~2.0%；
Gelling agent, 0.5~2.0%；
PH adjusting agent, 1.0~2.5%；
Reinforcing agent, 3.0~8.5%；
Gel breaker, 0.2~1.5%；
Low-carbon alkanes, surplus；
Wherein,
The crosslinking agent is the mixture of ferric sulfate, ethylene glycol and monoethanolamine；
The gelling agent is obtained for phosphorus pentoxide, triethyl phosphate and mixed alcohol according to following preparation method
Product, the preparation method is：Under inert gas atmosphere, first by the triethyl phosphate and five oxygen
Change two phosphorus stirring reaction 1.5~2.5 hours under the conditions of 75~85 DEG C, after reaction system is cooled into 55~65 DEG C
The mixed alcohol is added, 115 DEG C~125 DEG C reactions is then heated to and is obtained final product the gelling agent in 4~5 hours；
Counted with the gross mass of the phosphorus pentoxide, triethyl phosphate and mixed alcohol as 100%, five oxygen
It is 25.1%~32.8% to change the mass percent of two phosphorus, and the mass percent of the mixed alcohol is
41.3%~45.9%, the mass percent of the triethyl phosphate is 21.3%~33.6%；
The mixed alcohol is the mixture of hexanol, amylalcohol, octanol and decyl alcohol；
The reinforcing agent is glycine betaine or octadecyl ammonium chloride or combinations thereof；
The pH value of the fracturing fluid is 3.0~4.5.
The low-carbon alkanes are at least one in methane, propane and butane.
Preferably, the ferric sulfate, ethylene glycol and monoethanolamine mol ratio are 9:(2.5~5.5):(3~6).
Preferably, hexanol, amylalcohol, octanol and decyl alcohol mol ratio are 3 in the mixed alcohol:1:1:2~2:1:1:1.
Preferably, the pH adjusting agent is sodium bicarbonate solution or sodium hydroxide solution or combinations thereof.
Preferably, the mass concentration of the sodium bicarbonate solution is 23%, and the quality of the sodium hydroxide solution is dense
Spend is 8%.
Preferably, the gel breaker is sodium thiosulfate or sodium acetate or combinations thereof.
Preferably, the low-carbon alkanes are the mass ratio of the mixture of methane and propane, the methane and propane
Example be：(1~2):(1~6).
Preferably, the low-carbon alkanes are the mixture of methane, propane and butane, the methane, propane
And the mass ratio of butane is：(1~2):(5~6):(3~5).
Preferably, the low-carbon alkanes are the mass ratio of the mixture of propane and butane, the propane and butane
Example be：(5~8):(1~3).
Second aspect present invention provides a kind of preparation method of the fracturing fluid of first aspect present invention, the preparation
Method is comprised the following steps：
Step 1, under inert gas atmosphere, by triethyl phosphate and phosphorus pentoxide under the conditions of 75~85 DEG C
Stirring reaction 1.5~2.5 hours, mixed alcohol is added after reaction system is cooled into 55~65 DEG C, is then heated to
115 DEG C~125 DEG C reactions obtain gelling agent in 4~5 hours；The mixed alcohol is hexanol, amylalcohol, octanol and the last of the ten Heavenly stems
The mixture of alcohol；
Step 2, under normal temperature airtight condition, by crosslinking agent, step 1 gained gelling agent, pH adjusting agent,
Reinforcing agent and gel breaker are added in low-carbon alkanes, and the fracturing fluid is obtained final product after being well mixed.
The beneficial effect of technical scheme provided in an embodiment of the present invention is：
(1), in fracturing fluid provided in an embodiment of the present invention, gelling agent is with phosphorus pentoxide, tricresyl phosphate second
The dialkyl phosphate that ester and mixed alcohol are prepared for raw material, by the composition and proportioning that control mixed alcohol
To control the structure of final dialkyl phosphate, so as to improve the heat resistance of fracturing fluid.Meanwhile, by control
The ratio of pH adjusting agent processed controls the pH value of fracturing fluid, makes the ratio of iron ion and dialkyl phosphate most
It is good, the most strong heat resistance to improve fracturing fluid of binding ability.Fracturing fluid provided in an embodiment of the present invention
Heat resistance can reach more than 135 DEG C.
(2), in fracturing fluid provided in an embodiment of the present invention, by controlling ferric sulfate and monoethanolamine in crosslinking agent
Ratio control iron ion rate of release, so as to control the crosslinking time of fracturing fluid, reduce fracturing work and apply
Work frictional resistance.The crosslinking time of fracturing fluid provided in an embodiment of the present invention can be adjusted in the range of 60s~200s
Section.
(3), in fracturing fluid provided in an embodiment of the present invention, formed in lower carbon number hydrocarbons fracturing fluid by reinforcing agent
Mesh network, strengthens the intensity and viscoplasticity of frozen glue, while reinforcing agent can form a tunic on frozen glue surface,
Suppress lower carbon number hydrocarbons and flee from frozen glue, enhancing gel strength, heat resistance.
(4), in fracturing fluid provided in an embodiment of the present invention, lower carbon number hydrocarbons used includes methane, propane and fourth
At least one in alkane, lower carbon number hydrocarbons combination low boiling point, surface tension is low, and density is low, and fracturing fluid enters storage
The easy gasification row of returning after layer, to reservoir fanout free region.Experiment shows, fracturing fluid pair provided in an embodiment of the present invention
The infiltration recovery rate of shale reservoir can reach 99.99%.
Brief description of the drawings
Technical scheme in order to illustrate more clearly the embodiments of the present invention, institute in being described to embodiment below
The accompanying drawing for needing to use is briefly described, it should be apparent that, drawings in the following description are only the present invention
Some embodiments, for those of ordinary skill in the art, on the premise of not paying creative work,
Other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the heatproof curve map of the fracturing fluid for shale gas pressure break that the embodiment of the present invention 1 is provided.
Specific embodiment
To make technical scheme and advantage clearer, below in conjunction with accompanying drawing to embodiment party of the present invention
Formula is described in further detail.
The embodiment of the present invention provides a kind of fracturing fluid for shale gas pressure break, and the quality with the fracturing fluid is
100% meter, the fracturing fluid includes the component of following mass percent：
Crosslinking agent, 0.3~2.0%；
Gelling agent, 0.5~2.0%；
PH adjusting agent, 1.0~2.5%；
Reinforcing agent, 3.0~8.5%；
Gel breaker, 0.2~1.5%；
Low-carbon alkanes, surplus；
Wherein,
Crosslinking agent is the mixture of ferric sulfate, ethylene glycol and monoethanolamine；
Gelling agent is the product that phosphorus pentoxide, triethyl phosphate and mixed alcohol are obtained according to following preparation method
Thing, the preparation method is：
Under inert gas atmosphere, triethyl phosphate and phosphorus pentoxide are stirred under the conditions of 75~85 DEG C first
Reaction 1.5~2.5 hours, mixed alcohol is added after reaction system is cooled into 55~65 DEG C, is then heated to
115 DEG C~125 DEG C reactions obtain final product gelling agent in 4~5 hours；
Counted with the gross mass of phosphorus pentoxide, triethyl phosphate and mixed alcohol as 100%, phosphorus pentoxide
Mass percent is 25.1%~32.8%, and the mass percent of mixed alcohol is 41.3%~45.9%, triethyl phosphate
Mass percent be 21.3%~33.6%；
Mixed alcohol is the mixture of hexanol, amylalcohol, octanol and decyl alcohol；
Low-carbon alkanes are at least one in methane, propane and butane.
In fracturing fluid provided in an embodiment of the present invention, gelling agent be with phosphorus pentoxide, triethyl phosphate and
The dialkyl phosphate that mixed alcohol is prepared for raw material.When pressing crack construction is carried out, fracturing fluid is injected and is stored up
Layer, the iron ion provided by ferric sulfate in crosslinking agent and dialkyl phosphate are crosslinked generation and freeze by complex reaction
Glue；After pressing crack construction terminates, in the presence of gel breaker, the frozen glue for generating under certain condition becomes again
Ground is flow back to for flowable liquid is returned.In the embodiment of the present invention, by the structure to gelling agent, crosslinking agent
Composition, the composition of low-carbon alkanes and crosslinking agent, gelling agent, pH adjusting agent, reinforcing agent, gel breaker and
Proportioning between low-carbon alkanes optimizes improvement, obtained that a kind of heat resistance is good, crosslinking time is controllable,
The fracturing fluid of the easy row of returning.Specific Optimal improvements are as follows：
(1), be used to preparing in the embodiment of the present invention alcohol of dialkyl phosphate for hexanol, amylalcohol, octanol with
And the mixture of decyl alcohol, the frozen glue tool that the dialkyl phosphate prepared with the mixture of these four alcohol is cross-linked to form
There is intensity higher, therefore with good heat resistance.Meanwhile, also by control in the embodiment of the present invention
The ratio of pH adjusting agent controls the pH of fracturing fluid, makes the pH of fracturing fluid 3.0~4.5, in the pH scopes
Interior, the ratio of iron ion and dialkyl phosphate is optimal, and binding ability is most strong, also has fracturing fluid good
Heat resistance.
(2), the middle ferric sulfate of crosslinking agent is used to provide iron ion, and iron ion passes through network with dialkyl phosphate
Close reaction generation frozen glue.When crosslinking agent does not mix with fracturing fluid other components, in iron ion and crosslinking agent
Monoethanolamine is combined.When after crosslinking agent mixes with fracturing fluid other components and enter reservoir during,
With the change of pH value and temperature, iron ion and monoethanolamine dissociate, so as to be complexed with dialkyl phosphate.By
The regular hour is needed in iron ion and monoethanolamine dissociation, after crosslinking agent mixes with fracturing fluid other components
Crosslinking will not be immediately begun to, therefore can be according to actual working conditions such as different tube diameters, different well depths by control
The ratio of Sulphuric acid iron and monoethanolamine controls the crosslinking time of fracturing fluid, to reduce fracturing work construction friction.
Ethylene glycol in crosslinking agent can improve dispersive property of the crosslinking agent in fracturing fluid, enable crosslinking agent in pressure
Split dispersed in liquid, prevent partial cross-linked, and the mobile performance of fracturing fluid can be improved.
(3), in fracturing fluid provided in an embodiment of the present invention, formed in lower carbon number hydrocarbons fracturing fluid by reinforcing agent
Mesh network, strengthens the intensity and viscoplasticity of frozen glue, while reinforcing agent can form a tunic on frozen glue surface,
Suppress the frozen glue of fleeing from of lower carbon number hydrocarbons, enhancing gel strength, heat resistance.
(4), the lower carbon number hydrocarbons in the embodiment of the present invention includes at least one in methane, propane and butane,
The lower carbon number hydrocarbons combines low boiling point, and surface tension is low, and density is low, fracturing fluid into the easy gasification row of returning after reservoir,
To reservoir fanout free region.
To sum up, by above-mentioned Optimal improvements, the heat resistance of fracturing fluid provided in an embodiment of the present invention can reach
To more than 135 DEG C, crosslinking time can be adjusted in the range of 60s~200s, the infiltration to shale reservoir
Recovery rate can reach 99.99%, it is adaptable to shale gas pressing crack construction.
In above-mentioned fracturing fluid, the ratio of monoethanolamine is higher in crosslinking agent, with reference to iron ion it is more,
The time that iron ion whole release is carried out into cross-linking reaction is also more long；Similarly, in crosslinking agent monoethanolamine ratio
Example is smaller, with reference to iron ion it is just smaller, by iron ion, all release carries out time of cross-linking reaction and also gets over
It is short.Ferric sulfate, ethylene glycol and monoethanolamine mol ratio preferably 9:(2.5~5.5):(3~6), more preferably 9:4:5.
In above-mentioned fracturing fluid, hexanol, amylalcohol, octanol and decyl alcohol mol ratio are preferably in mixed alcohol
3:1:1:2~2:1:1:1.Wherein, hexanol, amylalcohol, octanol and decyl alcohol can be n-hexyl alcohol, n-amyl alcohol, just
Octanol and Decanol, or other isomers.
In above-mentioned fracturing fluid, pH adjusting agent be preferably sodium bicarbonate solution or sodium hydroxide solution or
Combinations thereof.Wherein, the mass concentration of sodium bicarbonate solution preferably 23%, the quality of sodium hydroxide solution is dense
Degree preferably 8%.It will be appreciated to those of skill in the art that sodium acid carbonate and NaOH can also directly with
The solid form of equivalent is added.
In above-mentioned fracturing fluid, the species of gel breaker does not have a considered critical, this area conventional break agent,
But should select with the preferable gel breaker of other components compatibility in fracturing fluid, preferably sodium thiosulfate or
Sodium acetate or combinations thereof.
In above-mentioned fracturing fluid, the preferably following several combinations of low-carbon alkanes：
(1) mixture of methane and propane, wherein, the mass ratio of methane and propane is：(1~2):(1~6),
It is preferred that 1:1.
(2) mixture of methane, propane and butane, wherein, the mass ratio of methane, propane and butane
Example be：(1~2):(5~6):(3~5), preferably 1:5:3.
(3) mixture of propane and butane, wherein, the mass ratio of propane and butane is：(5~8):(1~3),
It is preferred that 5:1.
Above-mentioned fracturing fluid can be prepared using following preparation method：
Step 1, the preparation of gelling agent under inert gas atmosphere, triethyl phosphate and phosphorus pentoxide is existed
Stirring reaction 1.5~2.5 hours under the conditions of 75~85 DEG C, add by oneself after reaction system is cooled into 55~65 DEG C
The mixed alcohol of alcohol, amylalcohol, octanol and decyl alcohol composition, then heats to 115 DEG C~125 DEG C and reacts 4~5 hours
Obtain gelling agent；
Step 2, under the conditions of normal temperature pressure-tight, in proportion by crosslinking agent, step 1 gained gelling agent, pH
Conditioning agent, reinforcing agent and gel breaker are added in low-carbon alkanes, are obtained final product after being well mixed and are obtained above-mentioned fracturing fluid.
In above-mentioned preparation method, inert gas in step 1 can be nitrogen or argon gas, preferably pure
The smart nitrogen of degree 99.99%.
The mixing speed during gelling agent is prepared in above-mentioned preparation method, in step 1 can be
100r/min~500r/min.20s~10min is stirred in step 2 is well mixed fracturing fluid each component.
The technical scheme of the embodiment of the present invention is made further specifically below by specific pressure break formula of liquid
It is bright.
Embodiment 1
The present embodiment provides a kind of fracturing fluid for shale gas pressure break, is counted with the quality of fracturing fluid as 100%,
The fracturing fluid includes the component of following mass percent：
Crosslinking agent, 0.8%；
Gelling agent, 1.0%；
23% sodium bicarbonate solution that mass concentration is, 1.5%；
Glycine betaine, 3.0%；
Sodium thiosulfate, 0.5%；
Propane, 93.2%.
Wherein,
Crosslinking agent is the mixture of ferric sulfate, ethylene glycol and monoethanolamine, ferric sulfate, ethylene glycol and ethanol
Amine mol ratio is 9:4:5.
The pH value of the fracturing fluid of the present embodiment is 3.5.
Gelling agent is prepared according to following preparation method：
Counted with the gross mass of triethyl phosphate, phosphorus pentoxide and mixed alcohol as 100%, first by 22% phosphorus
Triethylenetetraminehexaacetic acid ester, 35.3% phosphorus pentoxide are added in three-necked bottle, then to being passed through smart nitrogen (i.e. purity in three-necked bottle
Nitrogen for 99.99%), stirred with 100r/min-500r/min speed at 80 DEG C, reaction 2 hours, so
After cool to 60 DEG C, add the mixture of 42.7% n-hexyl alcohol, n-amyl alcohol, n-octyl alcohol and Decanol, rise
Temperature obtains final product above-mentioned gelling agent in 4.5 hours to 120 DEG C of reactions.Wherein, n-hexyl alcohol, n-amyl alcohol, n-octyl alcohol, just
The mol ratio of decyl alcohol is 3:1:1:2.
In normal temperature pressure-tight environment, according to above-mentioned composition and proportioning, by crosslinking agent, gelling agent, quality
23% sodium bicarbonate solution, glycine betaine and the sodium thiosulfate that concentration is are added in propane, stir 1min
Make each component that the fracturing fluid of the present embodiment is obtained final product after being well mixed.
Using MARS rheometer test frozen glue temperature and shearing sustainabilities, the fracturing fluid of the present embodiment is as a result shown
The frozen glue formed after crosslinking can 135 DEG C of heatproof (referring to Fig. 1).
The crosslinking time of the fracturing fluid of the present embodiment is 60s.
Embodiment 2
The present embodiment provides a kind of fracturing fluid for shale gas pressure break, is counted with the quality of fracturing fluid as 100%,
The fracturing fluid includes the component of following mass percent：
Crosslinking agent, 1.5%；
Gelling agent, 1.0%；
8% sodium hydroxide solution that mass concentration is, 1.0%；
Octadecyl ammonium chloride, 5.0%；
Sodium acetate, 1.0%；
Ratio is 1:1 methane and the mixture of propane, 90.5%.
Wherein,
Crosslinking agent is the mixture of ferric sulfate, ethylene glycol and monoethanolamine, ferric sulfate, ethylene glycol and ethanol
Amine mol ratio is 9:4:5.
The pH value of the fracturing fluid of the present embodiment is 4.5.
Gelling agent is prepared according to following preparation method：
Counted with the gross mass of triethyl phosphate, phosphorus pentoxide and mixed alcohol as 100%, first by 25% phosphorus
Triethylenetetraminehexaacetic acid ester, 32.3% phosphorus pentoxide are added in three-necked bottle, then to being passed through smart nitrogen (i.e. purity in three-necked bottle
Nitrogen for 99.99%), stirred with 100r/min-500r/min speed at 80 DEG C, reaction 2 hours, so
After cool to 60 DEG C, add the mixture of 42.7% n-hexyl alcohol, n-amyl alcohol, n-octyl alcohol and Decanol, rise
Temperature obtains final product above-mentioned gelling agent in 4.5 hours to 120 DEG C of reactions.Wherein, n-hexyl alcohol, n-amyl alcohol, n-octyl alcohol, just
The mol ratio of decyl alcohol is 3:1:1:1.
In normal temperature pressure-tight environment, according to above-mentioned composition and proportioning, by crosslinking agent, gelling agent, quality
23% sodium bicarbonate solution, octadecyl ammonium chloride and the sodium thiosulfate that concentration is are added to methane and third
In the mixture of alkane, stirring 5min makes to obtain final product the fracturing fluid of the present embodiment after each component is well mixed.
Using MARS rheometer test frozen glue temperature and shearing sustainabilities.Result shows the fracturing fluid of the present embodiment
The frozen glue formed after crosslinking can 134.1 DEG C of heatproof.
The crosslinking time of the fracturing fluid of the present embodiment is 100s.
Embodiment 3
The present embodiment provides a kind of fracturing fluid for shale gas pressure break, is counted with the quality of fracturing fluid as 100%,
The fracturing fluid includes the component of following mass percent：
Crosslinking agent, 2.0%；
Gelling agent, 2.0%；
23% sodium bicarbonate solution that mass concentration is, 1.0%；
Octadecyl ammonium chloride, 5.0%；
Sodium thiosulfate, 1.5%；
Ratio is 5:1 propane and the mixture of butane, 88.5%.
Wherein,
Crosslinking agent is the mixture of ferric sulfate, ethylene glycol and monoethanolamine, ferric sulfate, ethylene glycol and ethanol
Amine mol ratio is 9:4:5.
The pH value of the fracturing fluid of the present embodiment is 4.0.
Gelling agent is prepared according to following preparation method：
Counted with the gross mass of triethyl phosphate, phosphorus pentoxide and mixed alcohol as 100%, first by 33% phosphorus
Triethylenetetraminehexaacetic acid ester, 29.5% phosphorus pentoxide are added in three-necked bottle, then to being passed through smart nitrogen (i.e. purity in three-necked bottle
Nitrogen for 99.99%), stirred with 100r/min-500r/min speed at 80 DEG C, reaction 2 hours, so
After cool to 60 DEG C, add the mixture of 37.5% n-hexyl alcohol, n-amyl alcohol, n-octyl alcohol and Decanol, rise
Temperature obtains final product above-mentioned gelling agent in 4.5 hours to 120 DEG C of reactions.Wherein, n-hexyl alcohol, n-amyl alcohol, n-octyl alcohol, just
The mol ratio of decyl alcohol is 2:1:1:1.
In normal temperature pressure-tight environment, according to above-mentioned composition and proportioning, by crosslinking agent, gelling agent, quality
23% sodium bicarbonate solution and sodium thiosulfate that concentration is are added in the mixture of propane and butane, are stirred
Mixing 10min makes to obtain final product the fracturing fluid of the present embodiment after each component is well mixed.
Using MARS rheometer test frozen glue temperature and shearing sustainabilities.Result shows the fracturing fluid of the present embodiment
The frozen glue formed after crosslinking can 134.3 DEG C of heatproof.
The crosslinking time of the fracturing fluid of the present embodiment is 120s.
Embodiment 4
The present embodiment provides a kind of fracturing fluid for shale gas pressure break, is counted with the quality of fracturing fluid as 100%,
The fracturing fluid includes the component of following mass percent：
Crosslinking agent, 1.0%；
Gelling agent, 2.0%；
Glycine betaine, 3.0%；
23% sodium bicarbonate solution that mass concentration is, 2.5%；
Sodium thiosulfate, 1.5%；
Ratio is 1:5:The mixture of 3 methane, propane and butane, 90%.
Wherein,
Crosslinking agent is the mixture of ferric sulfate, ethylene glycol and monoethanolamine, ferric sulfate, ethylene glycol and ethanol
Amine mol ratio is 9:4:5.
The pH value of the fracturing fluid of the present embodiment is 4.2.
Gelling agent is prepared according to following preparation method：
Counted with the gross mass of triethyl phosphate, phosphorus pentoxide and mixed alcohol as 100%, first by 33% phosphorus
Triethylenetetraminehexaacetic acid ester, 29.5% phosphorus pentoxide are added in three-necked bottle, then to being passed through smart nitrogen (i.e. purity in three-necked bottle
Nitrogen for 99.99%), stirred with 100r/min-500r/min speed at 80 DEG C, reaction 2 hours, so
After cool to 60 DEG C, add the mixture of 37.5% n-hexyl alcohol, n-amyl alcohol, n-octyl alcohol and Decanol, rise
Temperature obtains final product above-mentioned gelling agent in 4.5 hours to 120 DEG C of reactions.Wherein, n-hexyl alcohol, n-amyl alcohol, n-octyl alcohol, just
The mol ratio of decyl alcohol is 2:1:1:1.
In normal temperature pressure-tight environment, according to above-mentioned composition and proportioning, by crosslinking agent, gelling agent, quality
23% sodium bicarbonate solution, glycine betaine and the sodium thiosulfate that concentration is are added to methane, propane and fourth
In the mixture of alkane, stirring 20s makes to obtain final product the fracturing fluid of the present embodiment after each component is well mixed.
Using MARS rheometer test frozen glue temperature and shearing sustainabilities.Result shows the fracturing fluid of the present embodiment
The frozen glue formed after crosslinking can 135 DEG C of heatproof.
The crosslinking time of the fracturing fluid of the present embodiment is 75s.
To sum up, fracturing fluid provided in an embodiment of the present invention has good resistance to elevated temperatures, and crosslinking time
Can be adjusted according to actual condition very much to reduce the frictional resistance of fracturing work, easily the gasification row of returning, it is adaptable to shale
Gas pressing crack construction.And the pressure break formula of liquid is simple, is easy to field operation.
The above is for only for ease of it will be understood by those skilled in the art that technical scheme, and without
To limit the present invention.All any modifications within the spirit and principles in the present invention, made, equivalent,
Improve etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of fracturing fluid for shale gas pressure break, it is characterised in that the quality with the fracturing fluid is
100% meter, the fracturing fluid includes the component of following mass percent：
Crosslinking agent, 0.3~2.0%；
Gelling agent, 0.5~2.0%；
PH adjusting agent, 1.0~2.5%；
Reinforcing agent, 3.0~8.5%；
Gel breaker, 0.2~1.5%；
Low-carbon alkanes, surplus；
Wherein,
The crosslinking agent is the mixture of ferric sulfate, ethylene glycol and monoethanolamine；
The gelling agent is obtained for phosphorus pentoxide, triethyl phosphate and mixed alcohol according to following preparation method
Product, the preparation method is：
Under inert gas atmosphere, first by the triethyl phosphate and phosphorus pentoxide under the conditions of 75~85 DEG C
Stirring reaction 1.5~2.5 hours, reaction system is cooled to the mixed alcohol is added after 55~65 DEG C, then
It is warming up to 115 DEG C~125 DEG C reactions and obtains final product the gelling agent in 4~5 hours；
Counted with the gross mass of the phosphorus pentoxide, triethyl phosphate and mixed alcohol as 100%, five oxygen
It is 25.1%~32.8% to change the mass percent of two phosphorus, and the mass percent of the mixed alcohol is
41.3%~45.9%, the mass percent of the triethyl phosphate is 21.3%~33.6%；
The mixed alcohol is the mixture of hexanol, amylalcohol, octanol and decyl alcohol；
The reinforcing agent is glycine betaine or octadecyl ammonium chloride or combinations thereof；
The low-carbon alkanes are at least one in methane, propane and butane；
The pH value of the fracturing fluid is 3.0~4.5.
2. fracturing fluid according to claim 1, it is characterised in that the ferric sulfate, ethylene glycol and
Monoethanolamine mol ratio is 9:(2.5~5.5):(3~6).
3. fracturing fluid according to claim 1, it is characterised in that hexanol in the mixed alcohol, amylalcohol,
Octanol and decyl alcohol mol ratio are 3:1:1:2~2:1:1:1.
4. fracturing fluid according to claim 1, it is characterised in that the pH adjusting agent is sodium acid carbonate
Solution or sodium hydroxide solution or combinations thereof.
5. fracturing fluid according to claim 4, it is characterised in that the quality of the sodium bicarbonate solution
Concentration is 23%, and the mass concentration of the sodium hydroxide solution is 8%.
6. fracturing fluid according to claim 1, it is characterised in that the gel breaker is sodium thiosulfate
Or sodium acetate or combinations thereof.
7. fracturing fluid according to claim 1, it is characterised in that the low-carbon alkanes are methane and third
The mass ratio of the mixture of alkane, the methane and propane is：(1~2):(1~6).
8. fracturing fluid according to claim 1, it is characterised in that the low-carbon alkanes are methane, third
The mixture of alkane and butane, the mass ratio of the methane, propane and butane is：(1~2):(5~6):
(3~5).
9. fracturing fluid according to claim 1, it is characterised in that the low-carbon alkanes are propane and fourth
The mass ratio of the mixture of alkane, the propane and butane is：(5~8):(1~3).
10. a kind of preparation method of the fracturing fluid described in any one of claim 1~9, it is characterised in that institute
Preparation method is stated to comprise the following steps：
Step 1, under inert gas atmosphere, by triethyl phosphate and phosphorus pentoxide under the conditions of 75~85 DEG C
Stirring reaction 1.5~2.5 hours, mixed alcohol is added after reaction system is cooled into 55~65 DEG C, is then heated to
115 DEG C~125 DEG C reactions obtain gelling agent in 4~5 hours；The mixed alcohol is hexanol, amylalcohol, octanol and the last of the ten Heavenly stems
The mixture of alcohol；
Step 2, under normal temperature airtight condition, by crosslinking agent, step 1 gained gelling agent, pH adjusting agent,
Reinforcing agent and gel breaker are added in low-carbon alkanes, and the fracturing fluid is obtained final product after being well mixed.
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Application publication date: 20170623 |